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Copyright Agilent Technologies 2001 All rights reserved. Reproduction, adaption, or translation without prior written permission is prohibited, except as allowed under the copyright laws. Part No. NONE 09/2001 Printed in Germany
Warranty
The information contained in this document is subject to change without notice. Agilent Technologies makes no warranty of any kind with regard to this material, including, but not limited to, the implied warranties or merchantability and fitness for a particular purpose. Agilent Technologies shall not be liable for errors contained herein or for incidental or consequential damages in connection with the furnishing, performance, or use of this material.
IMPORTANT NOTE This version of the 1050 service manual includes all sections from the 01050-90102 edition 4 (1995). The series I opticals information (79854A MWD and G1306A DAD) and the 79853A VWD information has been removed (products went out of support during 2000). Part numbers have been updated as of 09/2001. Contact your local Agilent support office in case of part number issues or upgrades. The latest version of this manual is available as Adobe Acrobat Reader (PDF) version only and can be downloaded from the Agilent Technolgies web page www.agilent.com.
Contents
1 Common: General Information This chapter provides general information about the 1050 Series of HPLC Modules 29 Safety Information 30
General 30 Operation 30 Safety Symbols 32
33
33 33
35 36
1050 Introduction
2 Common: Electronic Information This chapter provides common electronic information about the 1050 Series of HPLC Modules 39 Overview 41 Common Main Processor Board (CMP) 42
Common 1050 Functions CMP Details 44 Remote Control 47 42
Contents
53 55
Fluorescent Indicator Module (FIP) External Contacts 56 Power Supply (DPS-B / DPS-A) 57
General Description 57 Base Supply (DPS-B) 58 Lamp Supply (DPS-A) 60
64
3 Common: Cable Information This chapter provides information on cables for the 1050 Modules 67 Overview 68 Analog Cables 70 Remote Cables 72 BCD Cables 77
4 Pumps: General Information This chapter provides general information about the 1050 Pumps 83 Introduction 84 About this Manual 84 About the Pumps 85 Repair Policy 85 Product Structure 86
Contents
Capillaries 87 Specifications 88
5 Pumps: Hardware Information This chapter provides hardware information about the 1050 Pumps 91 Overview 93 How does the Pump Work? 95
Isocratic Operation Gradient Operation 95 96
Multi Channel Gradient Valve (MCGV) Metering Drive Assembly 103 Pump Head Assembly 104 Continuous Seal Wash 105 Active Inlet Valve 107 Outlet Ball Valve 108 Frit Adapter Assembly 109 Purge Valve 110 High Pressure Damper 111 Column Holder 112
102
Contents
6 Pumps: Electronic Information This chapter provides electronic information about the 1050 Pumps 113 Overview 115 Pump Drive Control Board (PDC2) 118 Relative A/D Converter Board (RAD) 123 Firmware Board (SFW) 127 HRI Board - Heater Isocratic Board 128 Heater Quaternary Board (HRQ) 131 High Pressure Transducer Board (HPT) 134 Connector Board (CON) 136 Pump Motherboard (HPS) 138
7 Pumps: Diagnostic Information This chapter provides information on error messages and diagnostic features of the 1050 Pumps 143 How to use the Diagnostic Test Functions Pump Pressure Ripple 146 Flow (Pressure) Tests 147
Prerequisites for the Pressure Tests 148 Normal Pressure Test 149 The Modified Pressure Test 150 Flow Test Method 151 Flow Test Method - Firmware Rev. 1.0 152 Flow Test Method - Firmware Rev. 3.0 and above
145
157
159
159
Prerequisites for the Gradient Test Method Running the Gradient Test Method 159
Contents
162
Panic Error / Bus Error Address Error 164 Common 1050 Error Messages 165 Pump Initialization Error Messages 167 Normal Operation Error Messages 171 Column Heater Error Messages 175 Online Monitor Messages 177 Troubleshooting Hints 180 Standard Pressure Tests with different Solvents 181
Modified Pressure Tests 181 Pressure Tests - Firmware Revision 1.0 182 Pressure Tests - Firmware Revision 3.0 and above Pressure Tests - Leak at Piston Seal 1 186 Pressure Tests - Leak at Piston Seal 2 189 Pressure Tests - Defective Piston 1 192 Pressure Tests - Defective Piston 2 196 Pressure Tests - Defective Active Inlet Valve 184
200
8 Pumps: Maintenance Information This chapter provides provide procedures for service and maintenance of the 1050 Pumps 203 Solvent Cabinet and Column Heater
Replacing the Heat Exchanger 205 Replacing the Cable Assembly 206
205
207
Contents
Replacing the Outlet Ball Valve 209 Maintaining the Frit Adapter Assembly Maintaining the Purge Valve 211
210
Maintaining the Pump Head Assembly 212 Procedure 1: Pump Head with old Plunger Housing
Stage 1: Removing the Pump Head Assembly 213 Stage 2: Disassembling the Pump Head assembly 213 Stage 3: Replacing the Seals 214 Stage 4: Disassembling the Plunger Housing 215 Stage 5: Reassembling the Plunger Housing 216 Stage 6: Reassembling the Pump Head Assembly 217 Stage 7: Mounting the Pump Head Assembly 217
213
218
Continuous Seal Wash Option 221 Replacing the Fan 222 Removing the Metering Drive Assembly
223
9 Pumps: Parts Information This chapter provides information on parts of the 1050 Pumps 225 Electronic Boards 227 Complete List of Ti-Parts 229 Solvent Cabinet 230
Contents
Solvent Cabinet with Helium Degassing 232 Solvent Cabinet with Column Heater and Manual Injection Valve 234 Overall Diagram 236 Hydraulic Flow Path 240 Metering Drive Assembly 243 Pump Head Assembly (old version) 244 Pump Head Assembly (new version) 245 Pump Head Assembly with Seal Wash 246 Active Inlet Valve 248 Outlet Ball Valve 249 Frit Adapter Assembly 250 Purge Valve Assembly 251 Column Holder Assembly 252 Special Tools 253
10Pumps: Additional Information This chapter provides additional information about the 1050 Pumps 255 Product History 257 Firmware History 259
Revision 1.0 Revision 3.0 Revision 3.1 Revision 3.2 259 259 260 260
Contents
267
275
11Sampler: General Information This chapter provides general information about the 1050 Autosampler 281 About this Manual 282 About the Autosampler 282 Repair Policy 283
10
Contents
12Sampler: Hardware Information This chapter provides hardware information about the 1050 Autosampler 287 Overview 289 Solvent Flow Path 290 How Does The Autosampler Work? 291 The Injection Sequence 293 What happens when the 18596L/M Sample Tray is connected? 294 Overview of the Electronics 295 Sampling Unit 297 Metering Drive 299 Analytical Head Assembly 300 High Pressure Switching Valve 301 Pneumatic Assembly 302
Actuator Air Solenoids 303
304
13Sampler: Electronic Information This chapter provides electronic information about the 1050 Autosampler 307 Overview 309
11
Contents
Max Tray Drive Board (MTD) 312 Needle Mini Tray Drive Board (NMD) 316 Valve Metering Drive Board (VMD) 320 Firmware Board (FIM) 324 Autosampler Motherboard (ALM) 325 Extender Test Board (ET) 330
14Sampler: Diagnostic Information This chapter provides information on error messages and diagnostic features of the 1050 Autosampler 333 Single Steps 335
335
Single Steps For The 21 Sample Tray 336 Single Steps for the 100 Sample Tray 338
Entering the Additional Single Steps Entering Diagnostic Mode 340 Z Test (Gripper Assembly) 340 R Test (radial arm movement) 341 Theta Test (angular movement) 341 338
340
Common 1050 Error Messages 344 Error Messages for Firmware Revision 4.0 and greater 346 Injector Program Error Messages 350 Normal Operation Messages for Firmware Revision 3.1 and below 351 Events Messages 354
12
Contents
355
15Sampler: Maintenance Information This chapter provides provide procedures for service and maintenance of the 1050 Autosampler 357 Sampling Unit 359
Stage 1: Removing the Sampling Unit 359 Stage 2: Removing the Needle 360 Stage 3: Installation of the Needle 361 Stage 4: Removing the Seat Capillary 361 Stage 5: Disassembling the Needle Arm 362 Stage 6: Reassembling the Needle Arm 362 Stage 7: Disassembling the Tray Mechanic 363
Metering Device
365
Removing the Metering Device 365 Removing the Gear Belt 365 Analytical Head Assembly 366 Procedure 1: Analytical Head Assembly with old Adapter Housing Procedure 2: Analytical Head with new Adapter Housing 369 Reassembling the Metering Device 371
366
372
13
Contents
16Sampler: Parts Information This chapter provides information on parts of the 1050 Autosampler 381 Electronic Boards and Fuses 383
Electronic Boards Fuses 383 383
Complete List of Ti-Parts 384 Overall Diagram 79855A/B 385 Hydraulic Flow Path 389 Sampling Unit 391
Arm Assembly Spare Parts 395
396
17Sampler: Additional Information This chapter provides additional information about the 1050 Autosampler 403 Product History 405 Firmware Revisions 406
Firmware Revision 1.0 Firmware Revision 2.0 Firmware Revision 2.1 Firmware Revision 3.0 Firmware Revision 3.1 Firmware Revision 4.0 406 406 407 408 409 410
14
Contents
Firmware Revision 4.1 411 Firmware Revision 4.2 411 If you update the firmware to revision 4.0 and greater 412 If you add a 100 vial tray to the autosampler 412 If you have Intermittant E17: Needle cannot move out of vial If you have to update the autosampler with a fan 413 If the fan in the autosampler does not work properly 413 If the needle lifts the vial out of the tray 414 If the injections are not reproducible (grooved needle) 414
413
18DAD/MWD: General Information This chapter provides general information about the 1050 Diode Array and Multiple Wavelength Detectors 419 About the Detector 420
General 420 Repair Policy 420 Identification 421 Compatibility 421
15
Contents
19DAD/MWD: Hardware Information This chapter provides hardware information about the 050 Diode Array and Multiple Wavelength Detectors 433 Overview: Optical System 435 Overview: Electronics 436 Optical Unit 438
Flow Cell Assemblies 439 Slit Assembly 441 Deuterium Lamp Assembly 442 Heat Exchanger Assembly 444 Shutter Assembly 445 Leak Sensor Assembly 446
Fans 447
20DAD/MWD: Electronic Information This chapter provides electronic information about the 1050 Diode Array and Multiple Wavelength Detectors 449 Overview 451 Array Signal Conversion Board (ASC) 454 Data Acquisition Board (AQB) 459 Firmware Board (FIM) 463 Common Main Processor Board (CMP) 464
Remote Control 466
Communication Interface (CRB) 467 Digital to Analog Conversion Board (DAC) Fluorescent Indicator Module (FIP) 472 Motherboard (LUM) 473 LPC Board 477
468
16
Contents
478
21DAD/MWD: Diagnostic & Troubleshooting Information This chapter provides information on error messages and diagnostic features of the 1050 Diode Array and Multiple Wavelength Detectors 483 STATUS Information
Status Modes 485 Status LEDs 486 Warnings 486
485
Common 1050 Error Messages 488 1050 DAD/WMD Error Messages 490 Diagnostic Features 493
Entering the Test Functions 493
Measure Intensity Profile 494 Lamp Intensity Test 496 Measure Holmium Spectrum 498 D/A Converter Test 500 Electronic Noise Test 502 Check of Wavelength Calibration 504 ASC Test 505 Shutter Position 506 ROM/RAM/DISPLAY Tests 507 Using the Built-in Test Chromatogram 508
How to print the DAD Profiles 510
17
Contents
22DAD/MWD: Maintenance Information This chapter provides provide procedures for service and maintenance of the 1050 Diode Array and Multiple Wavelength Detectors 513
Tools Needed 514 Warnings and Notes
515
522
Replacing the Achromat 524 Replacing Fans 525 Replacement of Shutter or LPC Board 526 Replacement of Leak Sensor 527 Upgrade to from 79854A MWD to G1306A DAD 528 Upgrade MWD with Series II Optical 529 Verifying the Performance 530
Specifications 530 What You Need 530 Preparations 530 Scaling Factors 532
23DAD/MWD: Parts Information This chapter provides information on parts of the 1050 Diode Array and Multiple Wavelength Detectors 533
18
Contents
Overall Diagram 535 Optical Unit 538 Heat Exchanger and Flow Cell 540 Flow Cell Parts (STD-SST) 541 High Pressure Flow Cell Parts (HP-STD-SST) 542 High Pressure Flow Cell Parts (HP-Micro-SST) 543 Cell Repair Kits 544 Lamp Housing 545 Upgrade Parts MWD to DAD 546 Upgrade Parts MWD to Series II Optical 547 List of Accessories 548
24DAD/MWD: Additional Information This chapter provides additional information about the 1050 Diode Array and Multiple Wavelength Detectors 549 Product History
Hardware Changes
551
551
25VWD: General Information This chapter provides general information about the 1050 Variable Wavelength Detectors 559 About the Detector 561 Versions vs. Support Periods (EOS) 561
19
Contents
79853A 79853C
561 561
26VWD: Hardware Information This chapter provides hardware information about the 1050 Variable Wavelength Detectors 565 Overview 566 Optical System Overview 568 Leak Interface Assembly 569 Leak Sensor Assembly 570 Fan Assemblies 571 Optical Unit 572
Flow Cells 573 Deuterium Lamp 576 Photodiodes Assemblies 579 Filter Assembly 580 Grating Assembly and Motor 581 Mirrors 582 Slit Assemblies 582 Beam Splitter 582
27VWD: Electronic Information This chapter provides electronic information about the 1050 Variable Wavelength Detectors 585
20
Contents
Location of Electronic Assemblies 587 Interconnection Diagram 589 Detector Controller Board (DCB) 590
Digital Section 592 Analog Sections 594
601
603
Pre-Amplifier Boards 605 Power Supply Connection Board (PSC) 606 GPIB Communication Interface 607
GPIB Firmware Revisions 608
28VWD: Diagnostic & Troubleshooting Information This chapter provides information on error messages and diagnostic features of the 1050 Variable Wavelength Detectors 609 Self Diagnosis 611
During Power On 611 During Normal Operation At Power ON 612 611
612
Error Messages After Lamp Ignition 616 Error Messages During Normal Operation 617 Error Messages During Use of Control Functions 619 User Control Functions 620 Service Control Functions 622
Entering the Service Mode 622 Zero Order Calibration 624
21
Contents
Wavelength Calibration 626 Wavelength Calibration Check 628 SET WL Parameter 629 Fix Signal 631 Leak Sensor Voltage 634 Voltage Test 635 ADC Noise 636 Grating Photo Sensor 637 Filter Photo Sensor 638 Remote Test 639 Filter Check 640 Zero Order Test 641 DAC Test 642 Pre-amplifier Gain 644 EEROM Test 645 DAC Calibration 646 Wavelength Compensation 647
29VWD: Maintenance Information This chapter provides provide procedures for service and maintenance of the 1050 Variable Wavelength Detectors 649 Warnings 650 Securing for Transport 651 Replacement of Deuterium Lamp
Step 1: Replacement 652 Step 2: 0th Order Calibration 653 Step 3: WL CALIBRATION 654
652
655
655
22
Contents
656
Using the Cuvette Holder 658 Replacing DCB Board and Firmware
DCB Board 661 DCB Firmware 661
661
665
Removing the Optical Unit 666 Replacing the PSC Board 667 Replacing Pre-amplifiers or Photodiodes 667 Replacing Grating Assembly Parts 668 Replacing Filter Assembly Parts 670 Replacing Mirrors, Beamsplitter and Slits 670
Cleaning of Optical Unit Parts 675 Upgrade to GPIB 676 Performance Verification 677
What you need 677 Preparations 677 Starting a run 678 Scaling Factors 679
30VWD: Parts Information This chapter provides information on parts of the 1050 Vari-
23
Contents
able Wavelength Detectors Overall Diagram 683 Front Panel Parts 686
Leak Interface 686 Font Panel 687
681
Optical Unit C
688
Optical Unit C Inner Parts Top 689 Optical Unit C Inner Parts Bottom 690
Grating Assembly 691 Filter Assembly 692 Standard Flow Cell C (SST/Ti) 693 Semi-Micro Flow Cell (SST) 695 High Pressure Flow Cell (SST) 696 Ultra High Pressure Flow Cell (SST) 697 Preparative Flow Cell (Ti) 698 Cuvette Holder 700 Accessories 701 Screws 702
31VWD: Enhanced Optical Unit Information This chapter provides information about the enhanced optical unit D 705 Compatibility 706 Support of Previous Optical Units Introduction 707 Support Considerations 708
Prefix Change 708 Identification 708
706
24
Contents
Compatibility Matrix
708
Part Numbers for Enhanced D Optical Unit 709 Standard Flow Cell D Repair Parts 710 Repair and Mainenance 711
Tools required: 711 Pre-requisites: 711
Additional Information 712 Replacements and Calibrations 712 Installing the Test Slit 713 Replacing Mirror #1 Assembly 715 Replacing Mirror #3 or #4 Assembly 716 Replacing the Grating or Grating Motor 718 Replacing the Beam Splitter 720 Cleaning or Replacing the Lens 721 Unlocking the Reference Aperture 723 Optimizing the Reference Readings 725 Installing the Standard Slit 726
32VWD: Additional Information This chapter provides additional information about the 1050 Variable Wavelength Detectors 727 Product History
Prefix Changes
729
729
DCB ROM Firmware Revisions 731 GPIB ROM Firmware Revisions 733 Hardware Changes and Service Notes 734
Modified Pre-Amplifier Gain 734 Important Service Note 734
25
Contents
26
Copyright Agilent Technologies 2001 All rights reserved. Reproduction, adaption, or translation without prior written permission is prohibited, except as allowed under the copyright laws. Part No. NONE 11/2001 Printed in Germany
Warranty
The information contained in this document is subject to change without notice. Agilent Technologies makes no warranty of any kind with regard to this material, including, but not limited to, the implied warranties or merchantability and fitness for a particular purpose. Agilent Technologies shall not be liable for errors contained herein or for incidental or consequential damages in connection with the furnishing, performance, or use of this material.
IMPORTANT NOTE This version of the 1050 service manual includes all sections from the 01050-90102 edition 4 (1995) and G1306-90102 edition 2 (May 1994). It merges both sections, the MWD and the DAD. The series I opticals information (79854A MWD) information has been removed (product went out of support during 2000). Part numbers have been updated as of 11/2001. Contact your local Agilent support office in case of part number issues or upgrades. The latest version of this manual is available as Adobe Acrobat Reader (PDF) version only and can be downloaded from the Agilent Technolgies web page www.agilent.com.
Safety Information
The following general safety precautions must be observed during all phases of operation, service, and repair of this instrument. Failure to comply with these precautions or with specific warnings elsewhere in this manual violates safety standards of design, manufacture, and intended use of the instrument. Agilent Technologies assumes no liability for the customers failure to comply with these requirements.
General
This is a Safety Class I instrument (provided with terminal for protective earthing) and has been manufactured and tested according to international safety standards.
Operation
Before applying power, comply with the installation section. Additionally the following must be observed. Do not remove instrument covers when operating. Before the instrument is switched on, all protective earth terminals, extension cords, auto-transformers, and devices connected to it must be connected to a protective earth via a ground socket. Any interruption of the protective earth grounding will cause a potential shock hazard that could result in serious personal injury. Whenever it is likely that the protection has been impaired, the instrument must be made inoperative and be secured against any intended operation. Make sure that only fuses with the required rated current and of the specified type (normal blow, time delay, and so on.) are used for replacement. The use of repaired fuses and the short-circuiting of fuseholders must be avoided. Some adjustments described in the manual, are made with power supplied to the instrument, and protective covers removed. Energy available at many points may, if contacted, result in personal injury. Any adjustment, maintenance, and repair of the opened instrument under voltage should be avoided as much as possible. When inevitable, this should be carried out by a skilled person who is aware of the hazard involved. Do not attempt internal service or adjustment unless another person, capable of
30
rendering first aid and resuscitation, is present. Do not replace components with power cable connected. Do not operate the instrument in the presence of flammable gases or fumes. Operation of any electrical instrument in such an environment constitutes a definite safety hazard. Do not install substitute parts or make any unauthorized modification to the instrument. Capacitors inside the instrument may still be charged, even though the instrument has been disconnected from its source of supply. Dangerous voltages, capable of causing serious personal injury, are present in this instrument. Use extreme caution when handling, testing and adjusting. When working with solvents please observe appropriate safety procedures (for example, goggles, safety gloves and protective clothing) as described in the material handling and safety data sheet by the solvent vendor, especially when toxic or hazardous solvents are used.
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Safety Symbols
Table 1 shows safety symbols that are used on the instrument and in the manuals.
Table 1
Safety Symbols Symbol Description The apparatus is marked with this symbol when the user should refer to the instruction manual in order to prevent risk of harm to the operator and protect the apparatus against damage. Indicates dangerous voltages.
Eye damage may result from directly viewing the light produced by the deuterium lamp used in this product. Always turn off the deuterium lamp before opening the metal lamp door on the side of the instrument. WA R N I N G A warning alerts you to situations that could cause physical injury or damage to the equipment. Do not proceed beyond a warning until you have fully understood and met the indicated conditions.
C A UT I O N
A caution alerts you to situations that could cause a possible loss of data. Do not proceed beyond a caution until you have fully understood and met the indicated conditions.
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Radio Interference
Manufacturers Declaration
This is to certify that this equipment is in accordance with the Radio Interference Requirements of Directive FTZ 1046/1984. The German Bundespost was notified that this equipment was put into circulation, the right to check the series for compliance with the requirements was granted. Test and Measurement If test and measurement equipment is operated with equipment unscreened cables and/or used for measurements on open set-ups, the user has to assure that under operating conditions the radio interference limits are still met within the premises.
Sound Emission
Manufacturers Declaration
This statement is provided to comply with the requirements of the German Sound Emission Directive of 18 January 1991. This product has a sound pressure emission (at the operator position) < 70 dB. Sound Pressure Lp < 70 dB (A) At Operator Position Normal Operation According to ISO 7779:1988/EN 27779/1991 (Type Test)
33
UV-Radiation
Emissions of ultraviolet radiation (200-315 nm) from this product is limited such that radiant exposure incident upon the unprotected skin or eye of operator or service personnel is limited to the following TLVs (Threshold Limit Values) according to the American Conference of Governmental Industrial Hygienists:
Table 2
UV-Radiation Limits Exposure/day 8 hours 10 minutes Effective Irradiance 0.1 W/cm2 5.0 W/cm2
Typically the radiation values are much smaller than these limits:
Table 3
UV-Radiation Typical Values Position Lamp installed, 50-cm distance Lamp installed, 50-cm distance Effective Irradiance average 0.016 W/cm2 maximum 0.14 W/cm2
34
Solvent Information
Observe the following recommendations on the use of solvents.
Flow Cell
Long term operation at pH > 11 should be avoided. Never leave strongly alkaline solutions in the flow cell without flow.
Solvents
Always filter solvents through 0.4 m filters, small particles can permanently block the capillaries. Avoid the use of the following steel-corrosive solvents: Solutions of alkali halides and their respective acids (for example, lithium iodide, potassium chloride, and so on). High concentrations of inorganic acids like sulfuric acid, especially at higher temperatures (replace, if your chromatography method allows, by phosphoric acid or phosphate buffer which are less corrosive against stainless steel). Halogenated solvents or mixtures which form radicals and/or acids, for example: 2CHCl3 + O2 2COCl2 + 2HCl This reaction, in which stainless steel probably acts as a catalyst, occurs quickly with dried chloroform if the drying process removes the stabilizing alcohol. Chromatographic grade ethers, which can contain peroxides (for example, THF, dioxane, di-isopropylether) such ethers should be filtered through dry aluminium oxide which adsorbs the peroxides. Solutions of organic acids (acetic acid, formic acid, and so on) in organic solvents. For example, a 1-% solution of acetic acid in methanol may attack steel. Mixtures of carbon tetrachloride with 2-propanol or THF dissolve stainless steel.
35
1050 Introduction
The Modules Overview
1050 is a series of HPLC products based on a modular concept. The necessary functions are broken down into independent stand-alone modules with standardized external design hydraulic- and external interfaces. Following modules will be available at introduction:
Table 4
1050 Modules Module 1050 Isocratic Pump 1050 Quaternary Pump 1050 Quaternary Pump (bio compatible) 1050 Variable Wavelength Detector 1050 Multiple Wavelength Detector 1050 Diode Array Detector 1050 Autosampler 1050 Autosampler (bio compatible) Product Number 79851A 79852A 79852B 79853C 79854A G1306A 79855A 79855B
36
Figure 1
1050 Modules
37
1050 Identification
Each module is identified by a 5 digit product number and a 10 unit serial number on a label attached to the wall inside the module. The first four digits of the serial number are the serial prefix. The letter identifies the country of origin. The last five digits are an identification number unique to each module. Any changes to the modules will be covered initially by Service Notes. They will be sent out to all Service personnel prior to implementation of the change to the instrument. With every reprint these changes will be incorporated into the documentation.
Repair Policy
Major mechanical and electrical assemblies inside the 1050 modules will be repaired on an assembly-exchange level. All other items have to be repaired on board/component level. Repair procedures are given in the respective sections of this manual (refer to Table of Contents). Assemblies can be set up to the Blue Stripe Exchange system or can be removed. If in doubt contact Waldbronn Product Support (Europe/ICON) or Little Falls Product Support (USA/Canada).
38
This chapter gives information about the common electronics used in more than one of the 1050 Series of modules: Overview Common Main Processor (CMP) Remote Control Firmware Boards (FIM, SFW) Fluorescent Indicator Module (FIP) External Contacts Poweer Supplies (DPS-B, DPS-A) Communication Interfaces (CIB, CRB)
40
Overview
Some of the electronic boards are used in more than one 1050 module. The following table shows common electronic assemblies:
Table 5
41
Table 6
Part Numbers for CMP Board Item CMP Board (Exchange) CMP Board (NEW) Part Number 01050-69580 5061-3380
42
Figure 2
Blockdiagram CMP
43
According to the above functions the main processor board contains some basic hardware which is common to all 1050 modules: 68008 main processor running at 8 MHz; 64 kByte RAM (32 kbyte RAM with battery back-up for parameter storage. The data will be lost when CMP is removed from the slot); interrupt logic for system communication; 3 channel software controlled timer; interface to keyboard/display module; remote I/O hardware; leak sensor electronics; interface to backplane bus; watchdog hardware. Firmware is not part of this board, because parts of the main processors software are module specific. The main processor firmware will be located on the personality module (AQB-, RAD, VMD-Board) or on an optional board.
CMP Details
Interrupt system There are one non-maskable interrupt six high priority hardware interrupt lines and seven low priority mail interrupt lines. The non-maskable interrupt is connected to the powerfail line of the power supplies (DPS-A/B). The high priority interrupt lines are: One from timer 6840 for hardware synchronization and five from remaining slots (these lines are disabled by SOK- = HIGH (system not ok). The low priority interrupt lines are: Five lines from all slots except power supply used for communication with local processors via dual port RAMs and two lines for CMP controlled software interrupts. Watchdog timer (Test for CPU hang-up) This circuitry is software retriggerable and is disabled during CPU initialization. In case of CPU hang-up SOK line is set the CPU is halted and the remote line shutdown is set.
44
LED on board There is a RED LED on the board which is the output of the watchdog circuit. It is ON during initialization and when the processor has a hang-up (LD 101). Programmable timer It includes 3 independent timers: Timer 1 is connected to the backplane bus its free for module special use. Timer 2 is used as software timer for the CMP. Timer 3 is used to generate the BUS ERROR signal. Reset system A harware reset is performed at power manually by on-board switch Hardware reset will reset all devices connected to the bus but main processor can reset these devices by software too. Reset for display unit The latch for the status LEDs and the brigthness control will not be reseted by power on or by software reset. The alphanumeric display is reseted at power on. I/O Two remote connectors are at the rear panel. They provide start, stop, not ready, shutdown, prepare-run and power on signals. The remote lines are input and output and are decoupled for EMC. The shutdown line is set by hardware in the case of leak or CPU hang-up. System control The POK (peripheral OK) is driven from all devices. The SOK- (system OK) is outputted from main processor to all devices; is hardware and software controlled disables/enables all devices by main software; disables all devices if main processor watchdog becomes active (main processor hang-up); Service Handbook for 1050 Series of HPLC Modules - 11/2001 45
All devices are enabled after initialization. Bus control After bus request the main processor will pass bus control to the requesting external controller. The local main processor areas including I/O are accessible too. This may be a feature for diagnostics or if data rate is increasing to much with later options. For this second case an external fast transfer hardware (for example DMA device) could do the transfers after set-up by the main processor. Leak sensing The leak detection circuit is located on the CMP board and checks continuously for presence and leak conditions. If the sensor is missing (defect) or in leak condition the PTC is cooled down the error message appears. When the module is turned on the leak message is disabled for some time to allow the sensor to reach its working range. Working condition of the PTC Normal: Error: Actions: Check for leak. Check connector of the sensor. Check resistance of leak sensor. Change leak sensor. Change CMP board. Change FIM board. about 75C below 55C 400...500 Ohm about 150 Ohm
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Remote Control
The CMP board provides two remote connectors. Remote control allows easy connection between single instruments or systems to ensure coordinated analysis with simple coupling requirements. When 1050 System is started from the autosampler the following signals can be measured at the remote lines. The START REQUEST signal is only available when the autosampler was started from any other module (remote configuration set to HPSystem). Figure 3 Remote Control Analysis
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For the 1050 Series of HPLC Modules the subminiatur D connector is used. Each module provides two remote connectors which are both parallel and inputs/outputs (wired-or technique). To provide maximum safety within a distributed analysis system one line is dedicated to SHUT DOWN the systems critical parts in case any module detects a serious problem. To detect whether all participating modules are switched on or properly powered one line is defined to summarize the POWER ON state of all connected modules. Control of analysis is maintained by signal readiness READY for next analysis followed by START of run and optional STOP of run triggered on the respective lines. In addition PREPARE and START REQUEST may be issued. Signal description
SHUT DOWN POWER ON READY PREPARE START REQUEST START STOP (L) System has serious problem (e.g. leak: stops pump). Receiver is any module capable to reduce safety risk. (H) All modules connected tosystem are switched on. Receiver is any module relying on operation of others. (H) System is ready for next analysis. Receiver is any sequence controller. (L) Request to prepare for analysis (e.g. calibration detector lamp on). Receiver is any module performing preanalysis activities. (L) Request to start injection cycle (e.g. by start key on any module). Receiver is the autosampler. (L) Request to start run / timetable. Receiver is any module performing runtime controlled activities. (L) Request to reach system ready state as soon as possible (e.g. stop run abort or finish and stop injection). Receiver is any module performing runtime controlled activities.
The signal level are defined as standard TTL levels (0 V is logic true, + 5 V is logic false). The remote lines can be input or output (wired or technique). Fan-out is 10 Input Load 2 kOhm against + 5 V Outputs are open collector type
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The REMOTE Connector To help you make the correct connections the signals carried on each pin are listed in the table below (the colors refer to wires of remote cable 01046-60201). Figure 4 APG Remote Connector
Table 7
Remote Signals
Pin 1 2 3 4 5 6 7 8 9 Signal Digital ground Prepare run Start Shut down Reserved Power ON Ready Stop Start request HIGH HIGH LOW LOW LOW LOW LOW Active Color white brown gray blue pink yellow red green black
Remote Configuration The 1050 Series provides three remote configurations: HPsystem GLOBAL LOCAL Start of automatic operation from any modules start key. Start request is outputted. Synchronized start of several modules for a single run. Start / Stop is outputted. Single modules start. No pulses outputted.
49
Figure 5
Notes Y1 is done by balance key of MWD only. Y2 BALANCE on detectors is performed. Y3 is not used in the module. The remote line SHUT DOWN will always be active. The remote line POWER ON will not be processed.
50
Figure 6
N OT E
Above schematic is for Pump, Autosampler, MWD and DAD. The signal level are defined as standard TTL levels (0 V is logic true, +5 V is logic false). The remote lines can be input or output (wired or technique). Fan-out is 10 Input Load >=2.2 kOhm against + 5 V Outputs are open collector type
51
Figure 7
52
Table 8
Part Numbers for Firmware Boards Item for Pumps (79851/2A/B) on RAD Board for Autosamplers (79855A/B) on VMD Board for Multiple Wavelength Detectors (79854A) on AQB Board for Diode ArrayDetectors (G1306A) on AQB Board Part Number Exchange 01018-66518 no 01078-66504 no 01048-66504 no G1306-66524 no
Firmware Description
Figure 3-7 shows the firmware structure for the 1050 Series of modules (pump, autosampler, multiple wavelength detector and diode array detector). As many as possible tasks use the same core firmware and only special routines for each module are developed seperate (control of the hardware sensors motors and so on). This common structure gives maximum flexibility for later development of similar products. It is obvious that also in the common firmware different commands display contents method parameters and so on. appear (Dialog, Method Handler, Parameter Handler). But nevertheless the structure is the same. In each part of the firmware there exist tables which hold the module specific commands parameters and so on, which are all handled under the same conditions. The firmware works with a foreground background mode. All time critical tasks (timetable execution, sensor and motor information) are working in the foreground mode and have highest priority. All other tasks share the remaining time in the background. If there are no tasks running the processor goes into the idle state. The firmware per module has approxmiately 300 kByte, where 170 kByte is Common and 130 kByte module specific).
53
The firmware is located on the module specific firmware board which is piggy back on the personality board of each module (AQB-, RAD- or VMD-board) and can be exchanged easily. Figure 8 Firmware Structure
54
Table 9
Part Numbers for FIP Board Item FIP Board Fuse 1 A Part Number 5061-3376 2110-0099 used for pumps, autosampler, MWD amd DAD
The FIP module is located behind the keyboard module of pump, autosampler and multiple wavelength detector. The function of the FIP module is to provide an interface between a host system and the user. Messages can be displayed with up to 32 characters (2 lines x 16 characters/line). A matrix keyboard is scanned for numeric or special function input and status information is displayed through 4 LEDs. The characters are displayed in a 5 x 7 dot matrix. In case of a dark display, check the on board fuse ICP1 (1 A) which is soldered in close to the connector P1/P2. Figure 9 Board Layout FIP
55
External Contacts
The personality boards of the 1050 modules (MWD/DAD: AQB, Pumps: RAD and Autosampler: VMD) have two external conacts at the rear. 1 contact without supply (contact closure) <newline>max. 30 V/250 mA (fused with 250 mA) 1 contact with internal 24 V supply (max. 250 mA output with fuse) The schematic for all three boards (AQB, NMD and RAD) is in general the same. Only the values of the components vary from board to board due to internal specifications. Figure 10 External Contacts
Table 10
56
Table 11
Part Numbers for LUC/LPC Board Item DPS-B (Exchange) DPS-B (New) DPS-A (Exchange) DPS-A (New) Fuse for 110 V operation 3 A Fuse for 220 V operation 2 A Part Number 01050-69374 5061-3374 01050-69375 5061-3375 2110-0003 2110-0002 used for Pumps and Autosamplers Pumps and Autosamplers MWD, DAD, VWD MWD, DAD, VWD
General Description
The power supply is a primary switching regulated type. It consists of two parts. the Base Supply and the Lamp Supply. The Base Supply provides outputs of +5 V, 19 V, +24 V and +36 V. In addition the Lamp Supply provides all circuits necessary for the operation of a deuterium lamp.
57
58
Figure 11
59
60
Figure 12
61
Figure 13
62
Lamp Ignition To ignite the deuterium lamp a 0.5 F capacitor loaded with 600 V is discharged via a 10 kOhm resistor to the anode. These 600 V are generated by a separate winding. The lamp status output signal shows "OK" if the lamp current has the selected value. Otherwise an error message is generated. The heater output made by a series regulator is in the pre-heating status 2.5 V always. After ignition a different output voltage is selected depending on the lamp type used: In the 79853C VWD, 79854A MWD and the G1306A DAD, the heater is switched off after ignition. The 12 V low noise output is made by a series regulator connected to the +19 V output.
63
Table 12
Part Numbers for CRB Board Item CIB Board (NEW) CRB Board (NEW) Part Number 5061-3382 5062-2482 used for Pumps and Autosampler 79854A MWD / G1306A DAD
N OT E
This section describes the communication interface for the 1050 Pumps (79851/2A/B), Autosamplers (79855A/B), Multiple Wavelength Detectors (79854A) and Diode Array Detector (G1306A) only. The communication interface for the 1050 Variable Wavelength Detector (79853C) is described in the chapter of the 1050 VW Detector. The communication interface board is necessary for the control by a Personal Computer and to connect printer or plotter devices. The communication interface board provides one GPIB and one RS-232 interface. The CRB for the 1050 MWD/DAD has a 96 kbyte runbuffer for the data/spectrum operation with the Multiple Wavelength Detector. The interface is located in Slot #2 of the module.
64
Compatibilities
Table 13
CIB/CRB Compatibility Instrument 1050 Pump 1050 Sampler 1050 MWD 1050 DAD R P C CIB R R C C CRB P P R R Firmware REV 3.1 REV 3.1 REV 3.1 REV 1.0
recommended configuration possible but not neccessary only for instrument control
Firmware To use the communication interface board it is mendatory to have the 1050 Modules equipped with the latest firmware revisions (see Table 13). Baud rate The board contains a baudrate generator. The baudrate is setable up to 19200 baud from the keyboard. The transmitter and receiver baudrate are independent adjustable. RS-232 Interface The implemented serial interface is a subset of the RS-232 standard only. It contains at PIN 2 PIN 3 PIN 4 RxD receive data (data input) TxD transmit data (data output) GND (Ground)
The 1050 modules are designed as DCE (data communication equipment) without hardware handshake.
65
66
Overview
The 1050 Modules provide Analog Signal Output (Pumps, Detectors) Remote Control Connector (all) BCD Connector (Autosampler) WA R N I N G Never use cables other than the ones supplied by Agilent Technologies to ensure proper functionality and compliance with safety or EMC regulations.
68
Table 14
Cables Overview Type Analog cables Description 3390/2/3 integrators 3394/6 integrators, 35900A A/D converter General purpose (spade lugs) Remote cables 3390 integrator 3392/3 integrators 3394 integrator 3396A (Series I) integrator 3396 Series II / 3395A integrator, see page 74 3396 Series III / 3395B/96C/97A integrator 1100 / 1050 modules / 1046A FLD / 35900A A/D converter 1040 DAD / 1090 liquid chromatographs / SDM BCD cables 3392/3 integrators 3396 integrator General purpose (spade lugs) GP-IB cable 1100 module to ChemStation, 1 m 1100 module to ChemStation, 2 m 1100 module to ChemStation, 5 m 03396-61010 5061-3378 01046-60202 obsolete 03396-60560 18594-60520 10833A 10833B 10833D Part Number 01040-60101 35900-60750 01046-60105 01046-60203 01046-60206 01046-60210 03394-60600
69
Analog Cables
One end of these cables provides a BNC connector to be connected to 1050 Series modules. The other end depends on the instrument to which connection is being made. 1050 to 3390/2/3 Integrators
Connector 01040-60101 Pin 3390/2/3 1 2 3 4 5 6 7 8 Shield Center Pin 1050 Shield
Signal Name Ground Not connected Signal + Connected to pin 6 Analog Connected to pin 4 Key Not connected
70
71
Remote Cables
One end of these cables provides a Agilent Technologies APG (Analytical Products Group) remote connector to be connected to 1050 Series modules. The other end depends on the instrument to be connected to. 1050 to 3390 Integrators
Connector 01046-60203 Pin 3390 2 NC 7 NC NC NC NC NC NC Pin 1050 1 - White 2 - Brown 3 - Gray 4 - Blue 5 - Pink 6 - Yellow 7 - Red 8 - Green 9 - Black Active (TTL)
Signal Name Digital ground Prepare run Start Shut down Not connected Power on Ready Stop Start request
72
Signal Name Digital ground Prepare run Start Shut down Not connected Power on Ready Stop Start request
Signal Name Digital ground Prepare run Start Shut down Not connected Power on Ready Stop Start request Not connected
N OT E
START and STOP are connected via diodes to pin 3 of the the 3394 connector.
73
Signal Name Digital ground Prepare run Start Shut down Not connected Power on Ready Stop Start request Not connected
1050 to 3396 Series II / 3395A Integrators Use the cable 03394-60600 and cut pin #5 on the integrator side. Otherwise the integrator prints START; not ready.
74
Signal Name Digital ground Prepare run Start Shut down Not connected Power on Ready Stop Start request Not connected
Signal Name Digital ground Prepare run Start Shut down Not connected Power on Ready Stop Start request
75
1050 to 1090 LC, 1040 DAD or Signal Distribution Module Connector 01046-60202 Pin 1090
1 NC 4 7 8 NC 3 6 5 - Key NC
Pin 1050
1 - White 2 - Brown 3 - Gray 4 - Blue 5 - Pink 6 - Yellow 7 - Red 8 - Green 9 - Black
Signal Name Digital ground Prepare run Start Shut down Not connected Power on Ready Stop Start request
76
BCD Cables
One end of these cables provides a 15-pin BCD connector to be connected to the 1050 Series modules. The other end depends on the instrument to be connected to. 1050 to 3392/3 Integrators (Obsolete)
Connector 18584-60510 Pin 3392/3 10 11 3 9 7 5 12 4 6 - Key 1 2 Pin 1050 1 2 3 4 5 6 7 8 9 15
Signal Name BCD 5 BCD 7 BCD 6 BCD 4 BCD 0 BCD 3 BCD 2 BCD 1 Digital ground +5V
BCD Digit 20 80 40 10 1 8 4 2
Low
77
Signal Name BCD 5 BCD 7 BCD 6 BCD 4 BCD 0 BCD 3 BCD 2 BCD 1 Digital ground +5V
BCD Digit 20 80 40 10 1 8 4 2
Low
Wire Color Green Violet Blue Yellow Black Orange Red Brown Gray White
Signal Name BCD 5 BCD 7 BCD 6 BCD 4 BCD 0 BCD 3 BCD 2 BCD 1 Digital ground +5 Vt
BCD Digit 20 80 40 10 1 8 4 2
Low
78
In This Book This manual contains technical information about the Agilent 1050 liquid chromatographs. This manual is available as electronic version (Adobe Acrobat Reader file) only.
Copyright Agilent Technologies 2001 All rights reserved. Reproduction, adaption, or translation without prior written permission is prohibited, except as allowed under the copyright laws. Part No. NONE 11/2001 Printed in Germany
Warranty
The information contained in this document is subject to change without notice. Agilent Technologies makes no warranty of any kind with regard to this material, including, but not limited to, the implied warranties or merchantability and fitness for a particular purpose. Agilent Technologies shall not be liable for errors contained herein or for incidental or consequential damages in connection with the furnishing, performance, or use of this material.
IMPORTANT NOTE This version of the 1050 service manual includes all sections from the 01050-90102 edition 4 (1995) and G1306-90102 edition 2 (May 1994). It merges both sections, the MWD and the DAD. The series I opticals information (79854A MWD) information has been removed (product went out of support during 2000). Part numbers have been updated as of 11/2001. Contact your local Agilent support office in case of part number issues or upgrades. The latest version of this manual is available as Adobe Acrobat Reader (PDF) version only and can be downloaded from the Agilent Technolgies web page www.agilent.com.
Introduction
This chapter gives general information on about this pump repair policy product structure capillaries specifications
84
Repair Policy
The 1050 Pumps are designed that all components are easy accessible Customers are able to repair certain parts of the 1050 Pumps see Operators Handbook. For details on repair policy refer to Repair Policy on page 38.
85
Product Structure
The 1050 Series of HPLC modules are available in two versions. In the standard version most of the parts used are stainless steel. In the 1050 Ti Series the flow path of the quaternary pump consists solely of corrosion resistant materials such as titanium, tantalum, quartz, sapphire, ruby, ceramic and fluorocarbon polymers. It is recommended for use with mobile phases containing high salt concentrations, extreme pH solutions and other aggressive mobile phases. Isocratic Pump Quaternary Pump Ti - Quaternary Pump N OT E 79851A 79852A 79852B
The isocratic pump was also introduced as Ti - version (79851B) but due to the insufficient orders it became obsolete end of FY 91.
86
Capillaries
In the 1050 Pumps the capillary shipped with the module will have a plastic color coating for identification in terms of material and internal diameter. All capillaries before the injector have a internal diameter of 0.25 mm. From the injector the internal diameter is reduced to 0.17 mm.
Table 15
Capillary Color Code color blue green red white Internal Diameter 0.25 mm 0.17 mm 0.12 mm tantalum Material
N OT E
For the Ti pumps the fittings are always titanium with a titanium nitrite coating and the front and back ferrules are gold plated. The Ti capillaries have two color coatings. One for identifying the material covering the main part of the capillary and a small one for the internal diameter.
87
Specifications
Table 16
Specifications of 1050 Pumps Hydraulic System Dual-pistons in-series with proprietary servo-controlled variable stroke drive floating pistons and active inlet valve. Setpoint from 0.001 to 9.999 ml/min in 0.001 ml/min increments. 20 to 100 l, automatic matched to flow rate or user-selectable. <0.3% RSD (typically <0.15%) based on retention time at 0.5 ml/min and 2.5 ml/min. Operating range from 0-400 bar (5880 psi) up to 5 ml/min; from 0-200 bar (2950 psi) up to 10 ml/min. Display in bar, psi or MPa. <2% amplitude (typically <1%), 1 ml/min isopropanol at all pressures >10 bar.
Pressure Pulsation
Compressibility Compensation User-selectable, based on mobile phase compressibility. Recommended pH Range 2.3 to 12.5 (stainless steel version). Solvents with pH below 2.3 should not contain acids which attack stainless steel. 1.0 to 14 (TI series). Low pressure quaternary mixing/gradient capability using proprietary high-speed proportioning valve. Delay Volume 900 to 1100 l dependent on back pressure. 0 to 100% in 0.1% increments from four independent channels. 0.25% absolute (typically 0.15%) peak to peak, binary mixed water/acetonitrile from 0.5 ml/min to 5.0 ml/min without mixer. Four 1 liter bottles each with individually-regulated helium sparger, cap and filter.
Gradient Formation
Solvent Preparation
88
Table 16
Specifications of 1050 Pumps Oven Temperature Range Oven Temperature Stability Oven Capacity Control Parameters Ambient +5C to ambient +60C in 0.1C increments.Display in C, F or K. 0.15C Two 25-cm or three 20-cm columns. Integrated keyboard with function keys; parameter editing during run possible; keyboard lock; optional control by PC. Flow rate, compressibility, stroke volume, upper and lower pressure limits, 2 external contacts; %B, %C, %D (for quaternary pump). Time-programmable Parameters: Flow rate, upper pressure limit, external contacts; %B, %C, %D. Battery-backed storage of up to 10 methods. Automatic start up and shut down methods. Editing of stored methods possible in run. For pressure monitoring, 2 mV/bar. Outputs: ready signal and two external outputs (one 24 V relay and one 30V (AC/DC) contact closure, both with 0.25 A. In-and outputs: start, stop and shut down signals. Optional interface for GPIB and RS-232C. Extensive diagnostics, error detection and display via front-panel LED's and status logbook. User-definable shutdown method activated in case of error. Leak detection and safe leak handling. Low voltages in major maintenance areas. Column pressure protection with maximum rate of pressure change of <20 bar/sec after a setpoint change. 4C to 55C (constant temperature) with <95% humidity (non-condensing). Line voltage: 100-120 or 220-240 VAC 10% Line frequency: 48-66 Hz Power consumption: 120 VA max.
Methods
Safety Aids
89
Table 16
Specifications of 1050 Pumps Dimensions Height: 208 mm (8.2 in) Width: 325 mm (12.8 in) Depth: 560 mm (22.0 in)
For complete description of test conditions used to obtain specifications, see Owners Manual.
90
This chapter gives general and technical information about the hardware components of the 1050 Pumps. Solvent Cabinet Pump Hardware Multi Channel Gradient Valve (MCGV) Metering Drive Assembly Pump Head Assembly Continuous Seal Wash Active Inlet Valve Outlet Ball Valve Frit Adapter Assembly Purge Valve High Pressure Damper Column Holder
92
Overview
The 1050 Pump is based on a dual piston series design which comprises all essential functions a solvent delivery system has to fulfill. Metering of solvent and delivery to the high pressure side are performed by one metering assembly which can generate pressure up to 400 bar. The basic system (isocratic) comprises the metering assembly including an active inlet valve, an outlet valve, a frit adapter assembly and a damping unit. The gradient operation system includes a highs peed proportioning valve allowing quaternary operation and a solvent cabinet with separate Helium degassing for each solvent channel. Since the introduction of the G1303A Online Degasser (December 1,1991) the Helium degassing might be replaced by the degasser module. A purge valve is installed on the pump head for convenient priming of the pump. An continuous seal wash is available when the pump is used with buffer solutions. It is mandatory in the Ti - pump and can be ordered as an option for the standard version. The solvent cabinet for the 1050 Pumps can be equipped with a manual injection valve and a column heater.
93
Figure 14
94
Isocratic Operation
When turned on the pump runs through a initialization procedure to determine the upper dead center of the first piston. The first piston moves slowly upwards into the mechanical stop of the pump head and from there it moves back a predetermined path length. The controller stores this piston position in memory. After this initialization the pump starts operation with the set parameters. The active inlet valve is opened and the down moving piston draws solvent into the first pump head. At the same time the second piston is moving upwards delivering into the system. After a controller defined stroke length (depending on the flow rate) the drive motor is stopped and the active inlet valve is closed. The motor direction is reversed and moves the first piston up until it reaches the stored upper limit and at the same time moving the second piston downwards. Then the sequence starts again moving the pistons up and down between the two limits.
95
During the up movement of the first piston the solvent in the pump head is pressed through the outlet ball valve and the damping unit into the second pumping unit. The second piston draws in half of the volume displaced by the first piston and the remaining half volume is directly delivered into the system. During the drawing stroke of the first piston the second piston delivers the drawn volume into the system.
Gradient Operation
For gradient operation the multi channel gradient valve (MCGV) connected to solvent containers A, B, C and D is required. The controller makes sure that each intake stroke of the first piston contains the required solvent composition. The controller divides the length of the intake stroke in certain fractions in which the MCGV connects the specified solvent channel to the pump input.
96
The communication interface board (CIB) provides an GPIB and RS232C interface. With the CIB installed the pump can be controlled via the ChemStation or via the 3396B integrator. Figure 15 Block Diagram 1050 Pumps
97
98
Solvent Cabinet
Repair Level: Component
Table 17
Product Numbers for Solvent Cabinet Item Solvent Cabinet Ti - Solvent Cabinet Part Number 79856A 79856B
The solvent cabinet allows storage of 4 four 1 liter solvent bottles. It is designed to hold the following options: Helium degassing; later it was replaced by 1050 online degassing Manual injection valve Column Heater Manual injection valve and column heater
Helium Degassing
N OT E For low pressure mixing degassing is a must. Therefore the Helium degassing or the Online Degasser G1303A is mandatory for the quaternary pump. If the Helium degassing is selected a internal tubing guides the Helium from the back of the solvent cabinet to an on/off valve and from there to four regulators. Each of the regulator supplies helium to one bottle head assembly for separate sparging of each bottle. The bottle head assembly consists of a sintered glass sparger, stainless steel or titanium filter and a cap with vent position. It is designed for the provided standard bottle, but allows also operation with supply bottles from certain vendors. The bottle head assembly has also a connection for a fume hood tubing (see also Helium Degassing Principle on page 269).
99
N OT E
The connected helium pressure has to be in the range 2 to 4 bar (30 to 60 psi). With pressures below 2 bar the helium degassing system may not work correctly. Pressure above 4 bar might damage the helium regulators.
Column Heater
The column heater fits into the recess of the cabinet. Electronic control is done via the pump module. The column heater can hold up to 25 cm long columns. The flow path of the column heater is stainless steel even in the Ti version. The heater uses a heating foil which is attached to a aluminum heating block where the solvent capillaries are leading through (heat exchanger). The column rests in the U-shaped heat exchanger. When turned on, the heat exchanger will heat up the solvent, the column and the surrounding air in the compartment. Temperature is monitored on the heating block via a Pt. 100. A multi (3) color LED shows the actual status of the column heater. The power consumption of the heater is reduced by heat recycling. Incoming and outgoing capillaries of the heat exchanger are in close thermal contact allowing radial heat exchange while the solvent is streaming through.
100
Figure 17
101
Table 18
Part Numbers MCGV Item MCGV Ti - MCGV Part Number 79835-67701 01019-67701 Exchange 79835-69701
The multi channel gradient valve (MCGV) works like a multi position switch. Depending on the timing of the control electronic the Heater Quaternary Board (HRQ) activates one of the four solenoids connecting the selected channel to the output of the valve. In the Ti-version of the gradient valve only the materials have been changed.
Table 19
Technical Data of MCGV Switching Time: Solenoid Voltage: Ti Series Materials in contact with solvent: PFA, PTFE, sapphire, ruby, ceramic, Titanium approximately 2 ms +12 V (+36 V Chopper Drive)
Figure 18
MCGV
102
Table 20
Part Numbers Metering Drive Assembly Item Metering Drive Assembly Part Number 01018-60001 Exchange 01018-69100
The metering drive assembly is identical for the stainless steel and the Ti version. The metering pump system is driven by a variable reluctance motor (servo) and electrically controlled by the Pump Drive Control Board (PDC). Feedback about actual movement is sensed by a shaft encoder mounted on top of the motor. In order to achieve required flow resolution a gear is used to transmit motor movement to the two pistons. The gears for the ball screw drives have different circumferences (ratio 2:1) allowing the first piston a twice as large stroke volume as the second piston. The second piston operates with a fixed 180 difference relative to the first piston. A sensor on the motor surface checks for over temperature conditions (90C).
Table 21
Figure 19
103
Table 22
Part Numbers Pump Head Assembly Item Pump Head Assembly Ti - Pump Head Assembly Part Number 01018-60004 01019-60002
Two identical piston move inside the solvent filled chamber in the pump head assembly. The piston are ball loaded on the spindles and center itself in the seal. The built in spring prevents clearances of the plunger affecting flow accuracy (see also Pump Head Assembly on page 271).
Table 23
Technical Data of Pump Head Maximum displacement volume: Ti - Series Materials in contact with solvents titanium, gold, sapphire, ceramic 108 l
Figure 20
104
Table 24
Part Numbers Seal Wash Item Seal Wash Kit Velocity regulator 3/pk Part Number 01018-68722 5062-2486
Bioscience application do very often use high concentrated buffer solutions. Therefore the seal wash is installed in each Ti pump. For the stainless steel version it is available as an option and should be used when buffer solutions are used in the instrument. If high buffer concentration are used in the pump the continuous seal wash will maintain the life time of the pump seal. Buffer solutions below 0.1mol normally do not require the seal wash option. The option is customer installable. The option consists of a support ring (1) a secondary seal (2) and a gasket (3) for both piston sides. A wash bottle filled with water/isopropanol (90/10) will be placed above the pump module and gravity will maintain a flow through the pump head removing all possible buffer crystals from the back of the pump seal. N OT E Running dry is the worst case for a seal and drastically reduces the life time of it. Therefore the tubings of the wash option should always be filled with solvent to maintain the life time of the wash seal. Use always a mixture of distilled water (90%) and isopropanol (10%) as wash solvent. The mixture prevents bacteria growth in the wash bottle and reduces also the surface tension of the water. The flow rate should be regulated to approximately 20 drops/minute (velocity regulator 5062-2486).
105
Figure 21
106
Table 25
Part Numbers Active Inlet Valve Item Active Inlet Valve Ti - Active Inlet Valve Part Number 01018-60010 01019-60010
The active inlet valve is a solenoid driven check valve. In the Ti version all parts in contact with solvents are corrosion resistant. The solenoid is controlled by the Pump Drive Control Board (PDC). A spring loaded ruby ball sitting in a sapphire seat closes or opens the flow path. If the solenoid is deactivated the keeper of the magnet presses the ruby ball down opening the flow path. At the same time the down moving first piston draws solvent into the pump head. The activated solenoid enables the spring to press the ruby ball in its seat and the flow path is blocked. Older versions do have a solvent protection cover installed.
Table 26
Figure 22
107
Table 27
Part Numbers Outlet Ball Valve Item Outlet Ball Valve Part Number G1311-60012
The outlet ball valve is made of corrosion resistant materials and can be used in both pump versions. The outlet valve cartridge contains two seat / ball pairs with the necessary seals. A slight weight on top of each ball limits the movement of the ball and maintains a small delay volume. The cartridge (3) is fixed with adhesive and the valve will be damaged if opened. The valve should always be tightened at the housing screw (2) and never at the cartridge (3) itself.
Table 28
Figure 23
108
Table 29
Part Numbers Seal Wash Item Frit Adapter Assembly Part Number 01018-60007
The housing of the frit adapter assembly is made from titanium and is suitable for both pump versions. The frit adapter assembly is installed in each isocratic pump. It is the interface to the following system components (for example autosampler) and holds a PTFE frit. The capacity of the frit when installed correctly is large enough to collect all the particles during the normal life time of the piston seal. It is recommended to replace the frit each time the seal has to be replaced as part of the normal pump maintenance. The second criteria for replacing the frit is the pressure across over it. If the pressure drop is more then approximately 10 bar with 5ml/min H2O the frit should be changed.
Table 30
Figure 24
109
Purge Valve
Repair Level:Assembly except of PTFE frit and gold seal (item 1 to 3)
Table 31
Part Numbers Purge Valve Item Purge Valve (replacement) Purge Valve Update Kit Part Number G1311-60009 01018-68723
The purge valve was introduced in November 1990. The purge valve is made from corrosion resistant materials and is suitable for both pump versions. The purge valve will be installed on all quaternary pumps and can be ordered as an option to the isocratic pump. The lower part of the purge valve is designed like the frit adapter assembly and holds the PTFE frit. A ball seat combination builds the purge valve. When opened at the thumb screw the ball is lifted out of its seat allowing the solvent to flow through the waste outlet. When the thumbscrew is turned down the internal springs press the ball into the seat. Flow is directed to the following system components.
Table 32
Figure 25
110
Table 33
Part Numbers High Pressure Damper Item Damper Ti - Damper Part Number 79835-60005 01019-60005
For the Ti version of the high pressure damper all parts which are in contact with solvents are gold plated. Two functions are obtained from the High Pressure Damper. Flow is damped (flow ripple reduction) and the pressure in the system is measured. The damping function is provided by an aluminum housing partly filled with water as the compressible medium and a solid steel block (3) which compensates for different coefficients of expansion of water and the aluminum housing. A protection plate (2) mounted between cover and housing prevents membrane (1) damage resulting from pressure excess or pressure shocks. Pressure is measured with a pressure transducer. The electrical circuit that outputs a voltage proportional to the pressure measured is mounted directly to the pressure transducer.
Table 34
Figure 26
111
Column Holder
Repair Level:Assembly
Table 35
Part Numbers High Pressure Damper Item Column Holder Assembly Part Number 5062-2469
The column holder is standard for the 1050 Ti Pumps. It is designed for use with any of the 1050 Series modules either separately or in a stack. A 1050 module will fit onto the column holder base (1) and the stand (2) can be used to attach columns which do not fit into the solvent module compartment using the clamp (3). Possible leaks will be collected in the groove (5). The support block (4) maintains the correct height adjustment of the autosampler foot support (100 vial tray). WA R N I N G The column holder is not intended for use with solvents which are flammable or toxic. If such solvents are used you must use a leak tray or equivalent. You must also position the column so that any leaking solvent is collected by the leak tray. Column Holder
Figure 27
112
This chapter gives information about the electronic of the pumps: Overview Pump Drive Control Board (PDC) Relative A/D Converter Board (RAD) Firmware Board (SWF) Heater Isocratic Board (HRI) Heater Quaternary Board (HRQ) High Pressure Transducer Board (HPT) Connector Board (CON) Pump Motherboard (HPS)
114
Overview
All electronic boards (except the FIP, behind the keyboard and the CON, above the MCGV) are located in the rear part of the module and they are connected to the Motherboard (HPS). Excess to the boards is from the back of the instrument. Slot numbers for the boards (as shown in the status screen) are counted from left to right. The power supply board is located in slot 1 and the common main processor is located in slot 7. In the 1050 pumps the following electronic assemblies are available:
Table 36
Electronic Boards Description Power Supply (DPS-B) Common Main Processor (CMP) Pump Drive Control (PDC2) Relative A/D Converter (RAD) Firmware Board (SFW) Heater Isocratic Board (HRI) Heater Quaternary Board (HRQ) Connector Board (CON) Motherboard (HPS) Display Interface Board (FIP) Communication Interface (CIB) Part Number 5061-3374 5061-3380 01018-66532 01018-66503 01018-66506 01018-66517 01018-66518 01018-66505 01018-66501 5061-3376 5061-2482 01018-69518 01018-69503 Exchange 01050-69374 01050-69580
N OT E
For information about Power Supply, Common Processor and Fluorescent Interface refer to Common: Electronic Information on page 39.
115
Figure 28
116
Figure 29
117
Table 37
Part Numbers for ASC Board Item PDC2 PDC Fuse: F16 (PDC), F481 (PDC2) 1.5 A Fuse F891, F892 (PDC); F112, F113 (PDC2) on board 500 mA U78 (MC78L15ACP) U79 (MC79L15ACP) Part Number 01018-66532 replaced by PDC2 2110-0304 2110-0934 1826-0274 1826-0281
The main functions of the PDC board are the control of the pump motor and the active inlet valve. For the quaternary system the PDC board has also to generate the control signals for the gradient valve circuit on the Heater Quaternary Board (HRQ). The PDC2 board succeeds the PDC board. For standardization and cost reduction reasons part of the circuit has been implemented in ASIC (Application Specific Integrated Circuit). The board size was reduced the board is also used in the other APG products and a stainless steel plate extends the board to 1050 board size. Fuses Fuse F16 (PDC) or F481 (PDC2) (1.5 A) protects the +36 V for servo motor and active inlet valve for overcurrent conditions on the old PDC board. F891 (PDC) or F113 (PDC2) (500 mA) protects the active inlet valve for overcurrent conditions while F892 (PDC) or F112 (PDC2) is for future use (space for additional connector on CON board).
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Figure 30
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U78, U79 PDC Boards revision A need an replacement of U78 and U79 when the metering drive (01018-69100) of the instrument has to be changed. Clock Generator The clock generator provides the clocks for the different pump boards. The pump control chip needs the 2 MHz clock and the pump control logic on the Relative A/D Board (RAD) and the Gradient Valve Driver Board (GVD) need the 1 MHz clock. Filter and Logic The filter and logic circuit disables the operation of the control chip in case of malfunctions in the system. Input signals for the block is the system OK (SOK) signal from the common main processor (CMP) which is active when the processor has locked up. The second signal connected to the circuit comes from the over temperature sensor on the surface of the pump motor. The TOK signal is active when the motor temperature exceeds 90C. 12 V Check The +12 V voltage will be checked for under voltage conditions. In case the voltages drops below approximately +10 V a proper working of the pump is no longer possible and the pump control chip will be disabled. Pump Control Chip The pump control chip is the brain of the PDC board. It handles all time critical and time consuming tasks for the digital position control of the pumping system. The chip works independent from the processor which supplies only the pump parameters (for example flow, stroke, compensation, gradient information and so on). All parameter changes will be transferred directly to the pump control chip. The feedback from the motor comes to the chip via the shaft encoder and allows accurate control of the motor (speed, direction and so on). The control chip sends the signals for the motor driver to energize the various motor windings. The control chip influences the current through the motor windings by changing the pulse width and by an amplification factor (Gain). The actual value of the current is supplied by the current amplifier and comparator circuit.
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The active inlet valve gets its control signals from the control chip. The optional gradient valve driver board (GVD), which controls the MCGV works under the supervision of the control chip. Motor Driver The motor driver circuit block contains the power stages for the motor. The motor is a three phase variable reluctance motor. Current Amplifier and Comparator One task of this circuit block is to measure the current through all the windings and to feed this signal into the control chip. From the control chip the circuit gets the pulse width (PW) and gain (GA) signals. With the pulse width the current value through the windings is determined. If the gain signal is active the amplifier multiplies the current with a factor (1.4). This is necessary to assure a constant torque at all motor positions. Active Inlet Valve The control chip provides the signals to activate or deactivate the active inlet valve. Figure 31 shows the control signal from the control chip and the current in the solenoid valve. The high current allows fast switching of the valve while the holding current reduces the heat dissipation of the solenoid. Figure 31 Inlet Valve Control
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Figure 32
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Table 38
Part Numbers for ASC Board Item RAD Fuse: F12, F22, 250 mA Part Number 01018-66503 2110-0004 Exchange 01018-69503
The main function of the board is the relative A/D conversion with an analog pressure output and overpressure measurement for the flow reduction. In addition the RAD board controls the two external contacts and checks for the status of active inlet valve and motor temperature. The firmware board (SFW) which contains the module firmware is attached to the RAD board and is used by the common main processor (CMP). Control Logic The control logic synchronizes the communication between the RAD and the main processor. Status Register The status register sends information about board identification motor temperature and active inlet valve to the main processor. Via the board identification the main processor identifies the board in the card cage. In case of a wrong board position the processor does not allow signals to the board. The over temperature sensor on the pump motor surface generates an error message when the motor temperature exceeds 90C (fan defective?). If the active inlet valve is not connected an error message is generated (when pump will be turned on) and the operation of the pump is inhibited.
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Figure 33
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Relay Contact Register The relay contact register activates the two relay contact circuits on request of the processor. When activated contact 1 provides fused (250 mA) +24 V while contact 2 provides a fused (250 mA) 30 V (AC/DC) rated contact closure. For more technical information about the relay contacts see External Contacts on page 56. Relative A/D Conversion The relative A/D conversion consist of a A/D converter a D/A converter with differential amplifier and a divider and filter. In addition a filter and amplifier for the pressure signal is needed and a comparator for the overpressure signal. The relative A/D converter delivers a binary data word which is independent from the absolute value of the signal. The output data word shows the % difference of the actual value compared to a reference value. The 8 bit D/A converter and the differential amplifier provide the reference voltage URef. The dynamic range for the relative measurement represents 6.4% of the absolute value of the signal. The divider and filter stage determines the Reference signal which is Ref=URef x 12.8%. The pressure signal from the high pressure damper is filtered and amplified. The outlet of this stage is the input voltage (UIn) for the A/D converter. The same signal is directly fed to the BNC output which has a resolution of 2 mV/bar for the range between 0 to 440 bar. The output has an offset of 30 mV (typical value) for offset compensation of the damping unit. The comparator compares reference signal and actual pressure signal. In case of overpressure conditions the flow will be reduced via the PDC board. The A/D converter allows different operation modes. Measurements of the difference between URef - UIn in relation to the reference (Ref) value or the absolute measurement of UIn - AGND in relation to Ref is possible. The results will be used by the processor to show the pressure ripple and the actual pressure on the display. It is also used to reduce the flow in case of overpressure conditions and for the online diagnostic (for example gas bubble detector, ball valve check, and so on). The BNC output is an additional diagnostic tool for checking the performance of the pump. For normal operation the use of the displayed pressure ripple is sufficient.
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Figure 34
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Table 39
Part Numbers for FIM Board Item Firmware Board (SWF) Part Number 01018-66506
The SFW board is a piggy back board, placed on RAD board (personality module). The programmed SFW contains the firmware of the 1050 pump module. The board is designed for on board programming. The FIM contains 128K x 8bit EPROMs. All inputs/outputs are pulled down for electrostatic discharge protection. Figure 35 Layout of SFW Board
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Table 40
Part Numbers for HRI Board Item HRI Fuse: F4, 2.5 A Part Number 01018-66517 2110-0083
The main function of the board is to control the column heater in the solvent conditioning module of the 1050 Isocratic Pump. Fuse Fuse F4 (2.5A) protects the +24V for the heater foil for overcurrent conditions. Control Logic The control logic synchronizes the communication between the HRI and the main processor. Status Register The register provides the main processor with the board identification. Synchronization The circuit receives the timing for the D/A converter from the main processor via the control logic. Synchronization adapts the timing to the needs of the 12 bit D/A converter. Pulse Width Modulator When the column heater is turned on the main processor provides control signals to the pulse width modulator. The output is a TTL signal with a duty cycle which depends on the temperature difference (error signal) between actual and setpoint temperature.
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Figure 36
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Temperature Measurement The temperature of the heat exchanger is measured with a Pt. 100 temperature sensor. (Resistance 1000 Ohm; at 0C and approximately 1400 Ohm; at 100C). The temperature converter circuit provides an analog signal (0V to +5V) correlating to the temperature of the heating block. The chosen setpoint temperature is converted in a reference voltage via the 12 bit A/D converter. Actual and setpoint temperature are then compared in the comparator. The derived error signal is send via Latch 1 to the main processor which updates the necessary signals for the heating section. The sensor check circuit provides information whether the temperature sensor is installed or not. Heater Driver The heater driver circuit contains the power stages for the heater foil. If the temperature of the heater block exceeds 100C a over-temperature switch on the heater foil interrupts the connection to the heater driver. Latch 2 The latch provides the signals to the multi color LED which gives visible information about the heater status. The LED shines green when the heater is on and at correct temperature. When maintaining the temperature the LED flashes yellow indicating the percentage of power used. The LED shines yellow when the heater is on and is at correct temperature but the not ready time has not been elapsed. During the heating up phase the LED flashes yellow. A red LED appears in case of error conditions. The system ok signal (SOK) of the processor is connected to the latch. In case of problems Latch 1 and the PWM are disabled and the heating process is interrupted. Board Layout Refer to Board Layout HRI/HRQ on page 133.
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Table 41
Part Numbers for HRQ Board Item HRQ Fuse: F4, 2.5 A Fuse: F16, 1 A Part Number 01018-66518 2110-0083 2110-0007 Exchange 01018-69518
The main function of the board is the control of the column heater as well as the multi channel gradient valve (MCGV). The board comprises the function of the HRI Board. Therefore only the multi channel gradient control has been described. The HRQ board replaced the gradient valve driver board (GVD) which controlled the MCGV. Block Diagram Refer to Block Diagram HRI/HRQ Board on page 129. Fuses Fuse F16 (1A) protects the +36V for the multi channel gradient valve (MCGV) for overcurrent conditions. Originally the fuse had 500 mA which was a incorrect value. Control Logic The control logic synchronizes the communication between the HRQ and the main processor. Valve Sequence Register The valve sequence register contains the information about the sequence in which the solenoids of the MCGV should be activated (for example A, B, C, D or A, C, D and so on).
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4 Bit Counter The control chip divides the piston path length for one stroke into four parts. The length for each part is depending on the flow composition. The four bit counter gets a pulse each time the portion is changed. The output is a 2 bit data word for the valve select memory. Valve Select Memory The following figure shows an example for the input and output of the valve select memory circuit. The channel number information comes from the 4 bit counter. The pump drive control board (PDC) supplies the gradient power pulse (GPP) and the blank out pulse (BOP). GPP delivers the power switching signals for the multi channel gradient valve (MCGV). BOP makes sure that all solenoids of the MCGV are switched off before opening the next one. Valve sequence register gives the relation between the four piston portions and the solvent channels. Output of the valve select memory is the accurate timing for the four solenoids of the MCGV. Figure 37 Valve Select Memory Signals
Valve Driver The valve Driver contains the power stages for the multi channel gradient valve (MCGV).
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Common Valve Switch Fast switching of the four valves without any interference between the channels is achieved with the common valve switch. One side of all the four valves is connected together and is opened each time before switching to the next valve (BOP). Figure 38 Board Layout HRI/HRQ
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Figure 39
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Figure 40
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Table 42
Part Numbers for CON Board Item CON (NEW) Fuse: F2, 375 mA Part Number 01018-66505 2110-0421
The connector board (CON) allows easy access to plugs for the multi channel gradient valve (MCGV) active inlet valve and the leak sensor. The connector cable transmits the signals to the motherboard and from there it is fed to the various boards. The fuse protects the active inlet valve circuit for overcurrent conditions (only on board revisions B and greater). Figure 41 Board Layout CON
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Table 43
CON Connectors Connector J1 J2 J3 J4 J5 J1 Function MCGV not used Active Inlet Valve Leak Sensor Cable MCGV
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Table 44
Part Numbers for LUM Board Item HPS Board Part Number 01018-66501
The Motherboard connects the various boards of the pump to each other and supplies the signals for the front parts like metering drive, damper, MCGV, fan and keyboard. Figure 42 shows the location of all connectors, Figure 43 to Figure 45 show the main signals of the pump. Figure 42 Layout of Pump Motherboard
J1 - Power Supply J2 - PDC Board J3 - RAD/SFW Board J4 - not used yet J5 - HRI/HRQ Board
J11 - Fan J12 - High Pressure Damper J13 - Connector Board Cable J14 - Metering Drive Motor J15 - Shaft Encoder
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Figure 43
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Figure 44
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Figure 45
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This chapter provides information about: Test Functions Flow (Pressure) Tests Pump Pressure Ripple Normal Pressure Test Modified Pressure Test Flow Test Method - Firmware Revision 1.0 Flow Test Method - Firmware Revision 3.0 and above Gradient Test Error Messages Selftest Common 1050 Messages Pump Initialization Normal Operation Column Heater Online Monitor Troubleshooting Hints (Pressure Tests) Pressure Tests with water and methanol Pressure Tests when the pump is broken
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Explanations to Plot The plot shows a typical pressure profile of a normal performing 1050 Pump. With the flow of 1 ml/min the pressure in the system raises until the pump stops via the overpressure condition at 400 bar. After one minute wait time the pressure drop should not exceed 5 bar/min.
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Explanations to the Modified Pressure Plot The plot shows a typical pressure profile of a normal performing 1050 Pump. The pressure in the system rises as seen in the previous test. When switched to the reduced flow rate the pressure increases with a lower slope. During the time until the system pressure limit will be reached piston I and II deliver alternately into the system. A straight line as seen indicates that both piston chambers are leak free. After switched off at 400 bar and one minute wait time the pressure drop should not exceed 5 bar/min.
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Explanations to Pressure Plot The plot shows a typical pressure profile of a normal performing 1050 Pump. Following are some remarks to the various steps in the plot. N OT E The pump displaces approximately 150 l until the first plateau will be reached at a pressure of 120 to 130 bar. After pump initialization the 1. piston is in its upper position which means the 2. piston starts delivering into the system. With the given stroke length of 70 l strokes of both pistons (II-I-II- I)| are necessary to reach the 1. plateau. Drastic leaks at active inlet valve outlet ball valve or seals will disturb the intake stroke of the 1. piston. The result might be a pressure drop when the 1. piston takes over to deliver into the system at a pressure between 20 to 40 bar. If the pressure test does not reach the first plateau the pressure plot cannot give any reliable diagnostic or troubleshooting hints.
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1 From the predefined position the pistons start moving with a flow of 150 | and rises the pressure in the pump. 2 At the first plateau the firmware makes sure that the first piston is delivering into the pump. With the very small flow rate of 2 l the pump pressure should remain stable. During the 1min at this plateau a maximum pressure drop of 5 bar is allowed (pressure display). At this position the tightness of the whole system is measured. 3 Pressure is increased until the second piston is delivering. 4 At the second plateau the second piston is delivering into the system with a flow of 2 l. Again a straight line is expected. A pressure drop of 5 bar during the 1min is allowed. 5 The pistons move now with a higher speed (flow 500 l/min) increasing the pressure in the system. 6 While increasing system pressure the pistons move with a stroke volume of 4 l. The system pressure must reach a value of 330 bar 30 bar. This part of the test checks for the mechanical tolerances from system to system and is of minor interest for system troubleshooting. 7 The system pressure is increased until the system shows an overpressure condition (>400 bar) which turns the pump off. 1 min after turning off the pump pressure drop should not exceed 5 bar/min. Possible Failure Modes The most relevant service information are obtained from the plot of the first (2) and second (4) plateau of the pressure plot. Three major failure modes are possible. For troubleshooting the system both plateaus should be seen together and not separately. The following plots show the different failure modes.
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Straight line at first plateau but negative slope at second plateau Figure 49 Negative Slope at second Plateau
The plot shows a leak free system when the first piston provides the flow. But during the stroke of the second piston the pressure drops down indicating a internal leak. The pump seals are definitely ok. Possible failure: Contaminated outlet ball valve (backflow).
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Negative slope at first plateau and stable plot at second plateau Figure 50 First Plateau unstable
Plot shows malfunction in the system when the first piston maintains the pressure in the system. The delivery stroke of the second piston is separated from the first one via the outlet ball valve and shows no problem. Possible failure: leak at first piston seal leak at active inlet valve no tight connection at outlet ball valve.
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Plot shows same failure mode on both pistons when maintaining the pressure in the pump. Under the assumption that the slope has the same angle for both plateaus it can be said that the problem is probably coming from the second piston chamber. Different angles indicate more than one leak in the pump. Possible failure Blank nut not tight enough Fittings at frit adapter assembly or damper not tight Leaking piston seal at second piston.
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Explanations to Pressure Plot N OT E This flow test method is pressure controlled. The actual pressure has to exceed at least 270 bar for the first step otherwise the test cannot reach the following steps. 1 Starting with a flow of 500 l/min and a stroke of 20 l the pump starts delivering into the system. The pressure rises until the damper detects a system pressure of more than 270 bar. The pump continues to deliver with the same parameters until piston I reaches its upper limit. At this position the stroke is changed to 80 l and piston II delivers one stroke with the larger stroke volume. 2 Now the flow is changed to 100 l/min (stroke 80 l) and piston I continues with this parameters for about 1/3 of its stroke. 3 At the plateau piston I delivers for approximately 1 minute with a very low flow rate (4 l) into the system. A straight line or a slight pressure increase is expected for a normal performing pump. A pressure drop during this minute indicates a problem in the pump.
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4 Piston II delivers into the system. At the end of the first plateau the flow is increased back to 500 l until piston II reaches approximately 1/3 of its stroke. At the second plateau piston II delivers with a very low flow rate (4 l) into the system. A straight line or a slight pressure increase is expected for a normal performing pump. A pressure drop during this minute indicates a problem in the pump. 5 The flow is increased to 250 l and the pumps works with this rate until the damper detects more than 390 bar. The flow is set to zero and the test is finished. It might happen that the system stops with a pressure slightly below 400 bar. This allows to restart the pump without reset. In most of the cases the pressure will exceed the upper pressure limit of 400 bar and will show the error message. 1 minute after reaching the maximum pressure of the test the pressure drop should not exceed 5 bar/min. Possible Failure Modes The plateaus (3, 4) of the pressure test provide the same information like in the previous test (Rev. 1.0). The only difference is that the two plateaus are moved to higher pressure values. The section pressure plots of this manual will provide additional pressure tests under failure conditions of the pump.
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5 Set integrator parameters (339X). Zero = 5 Att 2^ = ** CHT SP = 1.0 PK WD = 0.01 THRSH = 11 AT 12 min Att 2^ = ** AT 12 min CHT SP = 0.5 AT 45 min STOP ** The tracer concentration may vary from mixture to mixture. Therefore check for the appropriate integrator attenuation. Start the integrator manually change %B = 7 observe the plot and adjust the attenuation to a value which gives the highest deflection without exceeding the paper range. Proceed in the same way with %B = 100. Set the pump parameters back to start values (%B = 0). 6 Load gradient test method. 7 Press START, then ENTER to run the test method. Figure 53 Gradient Test Method (part 1)
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Figure 54
Explanations to Gradient Test In the first part of the test the step reproducibility will be tested. The steps should have all the same height except the last two steps. The last steps (from 2% to 1% to 0%) will not have the same step height because of a too small solvent volume versus the switching time at this positions. In addition the composition precision can be tested. The noise on each of the steps should not exceed 50% of the step height. Typically values of 30% representing a composition precision of 0.15% are reached. In the second part of the test the gradient linearity will be verified. Except of the bump at the upper end of the gradient the curve should show a straight line indicating a good linearity of the system. Be aware that the performance of the detector (linearity, stray light, and so on) will have a significant impact on the results.
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Error Messages
The error messages will help to locate and repair a failure. In case an error message appears the Error LED will be turned on and the message will be written into the system logbook. Reset Pump or switching on the pump again will reset the error. The entry in the logbook remains. The error messages can be divided into the following blocks: Selftest PANIC Error Common 1050 Messages Pump Initialization Normal Operation Column Heater Online Monitor
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Selftest
ROM/RAM Test
RAM and display can be tested via the build in selftest. The selftest will be performed when CRTL will be pressed while the module is turned on at the LINE~ switch. In case of a failure one of the following messages appears. The complete test requires approximately two minutes. ROM test failed ( ROM test failed ) The ROMs on the SFW board are tested. In case of a checksum error the ROM test fails. Replace the SFW board. RAM test failed ( RAM test failed ) The RAMs on the CMP board will be tested. In case of a failure the error message appears and the CMP has to be replaced. Replace the CMP board.
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Actions: Check for leaks in the pump module. Check connector of the sensor. Check resistance of leak sensor. Change leak sensor. Change CMP board. Change SFW board. E02 : Shutdown In Other Module E02 HH:MM DDMMM shut down > error in other module An external device pulled the shut down line of the remote connector down. This forces the pump to stop the pump motor inhibiting a flow into the system. Probably a leak appeared in one of the connected modules. E03 : Error Method loaded E03 HH:MM DDMMM error method > error method has been loaded The operator may define a method as a error method. The event message indicates that the module detected an error and that the error method was loaded. E04 : Time Out E04 HH:MM DDMMM time out The operator may define a time after which the instruments stops all further actions. Mainly two cases will lead to the time out message. First if a normal run is finished the pump is turned off after the specified time (only if no new start command appears during this time). Second a not ready condition in a sequence mode or in multiple run mode will start the time out timer eventually leading to the message.
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E13 HH:MM DDMMM init failed > pump timeout After restart the pump will move the first piston to its upper position. The upper position is recognized when the piston touches the mechanical stop rising drive power for the blocked motor. If the piston will not reach the upper limit within one minute the initialization will be stopped and the error message appears. Check gears of the drive assembly (broken coupler?). Change PDC board. Change the drive assembly.
The following three error messages use the same measurement principle with different limits. During the pump initialization the first piston hits the upper dead center of the pump head and stops there. To make sure that the piston will not run into this mechanical stop during normal operation the index hole of the motor shaft encoder wheel is used as the initialization reference. From the upper center the piston travels back until it reaches the index hole. There will be no reinitialization during normal operation (initialization only during pump on procedure or pump reset command). The Index position is expected in a certain range from the upper dead center. If the Index does not appear in this range one of the three messages will show up on the display. E14 HH:MM DDMMM init failed > home position not found After the piston has hit the upper limit it will move down to find the first Index hole of the encoder. If the Index is not found in the maximum allowed number of steps this error message appears. The communication to the shaft encoder index hole is missing. Check cable and connector of the encoder. Check PDC board connection. Change PDC board. Change Drive Assembly.
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E15 HH:MM DDMMM init failed > home position out of limit When the motor is stopped for reversing the direction the moment of inertia of motor and spindle will continue the movement for certain steps until it finally stops. Therefore an minimum number of steps is necessary until the Index should be reached. In case the number is to small this error message appears. Changed adjustment or sticking movement of the system can be the reason for this. Check drive system for smooth movement. Change motor drive assembly. Change PDC board.
E16 HH:MM DDMMM init failed > pump head missing The mechanical tolerances from one system to the other need an offset compensation to make sure that the piston reverses its direction always at the same position. If the distance between the upper limit and the first index exceeds the compensation range but is still below the maximum limit (E14) the error message will show up. Reason can be that the pump head is missing or not mounted in the right way. Mount pump head correctly. Check drive system for smooth movement. Change motor drive assembly. Change PDC board.
E17 HH:MM DDMMM init failed > idle power exceeded The PDC board measures the actual electrical current. If the motor needs more then a defined current for a pressure free pump it indicate a failure in the system. Reason is either an tight mechanical system or a defective motor. Check drive system for smooth movement. Check PDC board.
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E18 HH:MM DDMMM init failed > stroke length misadjusted This error message appears only when the pump is running in DIAGNOSE LEVEL 3 which is a manufacturing test. The error indicates a incorrect spindle position adjustment. Hint: If error message E27 occurs when pump works with 100 l stroke volume diagnose level 3 allows a quick check of the pump. Set diagnose level 3 and turn on pump. If E18 occurs the metering drive is mis-adjusted and generates the E27 problem. Metering drive has to be changed.
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E21 HH:MM DDMMM press too low > pressure below lower limit The lower limit value function is firmware controlled. In case the system pressure drops once below a user defined value the pump motor will be turned off or the specified error method will be activated and the error message appears. The error message allows to check the system for empty solvent bottles, broken capillaries, fitting leakage and so on. Check flow value and solvent composition. Check all seals and fittings in the complete LC system.
E22 HH:MM DDMMM sensor failed > temperature sensor failed While the pump is turned on the firmware checks for the presence of the temperature sensor. In case the sensor is disconnected defective or the sensor is activated (switch open) by an over temperature condition the error message appears. The temperature sensor switch opens at 90C and the pump motor will be turned off. Check fan. Check air filters. Check sensor with meter. Change metering drive. Change RAD board.
E23 HH:MM DDMMM overtemperature> motor temp exceeded limit The highest power consumption in the module is inside the variable reluctance motor. High system back pressure at low flow rates results in maximum heat dissipation. A fan and a special designed foam part make sure that the heat of the motor is brought out of the instrument. In case the airstream of the module is interrupted or the fan fails the motor temperature will rise above allowed limits. A thermal switch is mounted on the surface of the motor and turns off the pump when the temperature exceeds 90C. The error event circuit reacts immediately on the PDC board and turns off the pump motor power. The same signal line on the PDC board is also used from the system ok command (SOK). This means that the error also appears in case of a SOK error. The SOK is set when the processor has locked up
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preventing damage of pump or others or one of the boards holds the signal down. Check fan. Check air flow path. Check temperature of the motor. Change PDC board. Check all other boards in the system. Change CMP board. E24 : Inlet valve disconnected E24 HH:MM DDMMM valve missing > inlet valve disconnected If the active inlet valve is disconnected and the first piston is delivering solvent the valve may be damaged. Therefore the presence of the active inlet valve is controlled. In case the active inlet valve is not connected during the initialization of the pump the pump motor is turned off and the message occurs. Check Connector of the valve. Check the connector cable to the motherboard. Change RAD board. E25 : Adjust pressure offset E25 HH:MM DDMMM pressure offset> adjust pressure offset The high pressure damping unit measures the system pressure in the range from 0 to 400 bar. Thermal drift of the electronic components may cause drift to negative values. If the pressure offset is below -15 bar the error message appears on the display. Incorrect adjustment may influence the pump performance (pressure ripple measurement and so on). Perform offset adjustment. Check connector of damping unit. Change RAD board. Change damping unit.
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E26 HH:MM DDMMM init lost pump drive lost init values The reference position for the upper limit of the piston is reached during each pump cycle. In case the difference of the actual value in relation to the value of the initialization is too large the system will turn off the pump and the error message appears. Check connector and cable of the encoder. Change PDC board. Change motor drive assembly.
E27 : Max motor drive E27 HH:MM DDMMM power use high> power exceeded max motor drive power exceeded The power consumption of the motor drive will be monitored. In case of servo failures or blockages of the ball screw drive the motor current will exceed the maximum limit and the processor will turn off the pump. Check motor drive for smooth movement. Check the +12 V on the PDC board. Change PDC board. Change motor drive assembly. Check outlet ball valve for blockages. E28 : Secondary Powerfail E28 HH:MM DDMMM Sec Powerfail > +12 V analog supply failed The +12 V generated on the PDC board will be continuously checked for under voltage conditions. In case the voltages drops below approximately +10 V the pump will shut down and the error message will appear. The +12 V will be also used on the RAD board and the pressure transducer board of the damping unit. Change the PDC Board. Change the RAD Board. Change the Damping Unit.
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E35 HH:MM DDMMM column heater > overtemperature The column temperature is normally checked with the Pt. 100. In case of malfunctions the temperature may exceed the normal working range. At 90C the firmware disables the heater circuit, sets the error message and turns on the red error LED at the pump and the column heater. In case the heater transistor is defective and still heats up the heat exchanger the over temperature switch on the heater foil opens at 100C and interrupts heating. Change the HRI/HRQ board.
E36 HH:MM DDMMM column heater > fuse blown With the column heater turned on the firmware checks for the presence of the +24 V on the HRI/HRQ board. If fuse F4 is blown, the +24 V is missing and the instrument shows the error message, turns on the red error LED on the pump and the column heater module. The fuse blows in case of a shortage on the +24 V line. Replace fuse F4.
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M04 / M05 : 1st piston M04 HH:MM DDMMM 1st piston leak> leak check seals or inlet valve M05 HH:MM DDMMM 1st piston ok > problem solved leak in range If the online monitor function detects a leak in the first piston chamber the above message M4 appears. If the instrument returns to normal operation (problem solved by user) the message M5 indicates a good working instrument. The occurrence of M4 is a very good indicator when the seals should be changed. Check for leaks a fittings. Check for tight connection of the active inlet valve. Change seals. Change active inlet valve. M06 / M07 : Valve backflow M06 HH:MM DDMMM valve backflow> check outlet valve M07 HH:MM DDMMM valve tight > problem solved no backflow M06 indicates that the pump detected a backflow in the outlet valve which indicates that the valve has been closed but is not tight. M07 indicates that the problem was solved. Clean outlet valve. Change outlet ball valve. M08 / M09 : Outlet Valve M08 HH:MM DDMMM outlet valve > clean outlet valve M09 HH:MM DDMMM outlet valve ok> problem solved outlet valve ok M08 appears when the outlet ball valve shows a time delay before it blocks the flow path in the correct way. This is an indication that the valve sticks and need to be cleaned. Clean outlet ball valve. Change outlet ball valve.
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M11 HH:MM DDMMM purging > purge mode activated This message shows when the instrument was purged the last time.
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Troubleshooting Hints
This section gives practical hints in troubleshooting the pumps according to the pressure plots: Pressure Tests with different Solvents (water methanol) Pressure Tests when the Pump is broken
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Figure 56
With methanol the pressure drop at 400 bar is larger than with isopropanol because of the lower viscosity.
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Figure 57
Figure 58
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Figure 60
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185
The flow is reduced to 0.1 ml/min at approximately 240 bar. From this point both piston deliver with a constant value and increase the pressure to <nobreak|320 bar|. From this point the pressure moves up to 400 bar in an oscillating curve. This means that one of the two pistons has a leak rate when delivering into the system. At the upper pressure limit (400 bar) the pressure is stable. The outlet ball valve is closed in this position and indicates that the leak is probably on the first piston side. In this case it is a defective piston seal. Firmware revision 3.0 allows to identify the leaky piston side via the current active piston display.
186
Figure 62
The flow test method shows a quite normal pressure profile. Only on the slope to reach the upper limit some pressure fluctuations can be seen. The modified pressure test showed that the seal leaked at more than 320 bar. Therefore the flow test method cannot detect this defective seal.
187
Figure 63
The flow test method reduces the flow to 100 l at approximately 320 bar. The pressure drops and when the piston I delivers with its small flow rate a continuous pressure drop can be observed at the first plateau. The second plateau shows a slight pressure increase and the upper limit shows stable conditions. The pressure drop at the first plateau indicates a leak on the first piston side. In this case a leaky piston seal.
188
The flow is reduced to 0.1 ml/min at approximately 240 bar. From this point both piston deliver into the system with a constant rate. At 360 bar to <nobreak|370 bar| the curve is bent. With both pistons still delivering into the system the pressure cannot exceed more than 380 bar. The fact that both piston cannot increase the pressure above a certain value point to a leak on the second piston side. In this case a leaky piston seal.
189
Figure 65
The pressure profile shows a pressure drop at the upper limit. The modified test showed that the leak appears at more than 370 bar. Therefore the two plateaus cannot show the malfunction. At the upper limit the outlet ball valve is closed which indicates that the problem is on the second piston side. In this case the flow test method cannot clearly identify the leaky seal. The modified test is needed in addition.
190
Figure 66
Both plateaus for piston 1 and piston 2 and the upper limit of the test show a certain pressure drop. Here it is very obvious that the problem is on the second piston side. In this case it is the second piston seal.
191
The pump is working with the default stroke (AUTO) setting. The flow is reduced to 0.1 ml/min at approximately 260 bar. The pressure moves up to the upper pressure limit in a oscillating curve. At the upper limit the pressure remains stable. One of the two pistons generates a small leak when delivering (pressure drop). The stable pressure line at 400 bar points to a problem on the first piston side. Firmware revision 3.0 allows to verify that the pressure drop appears on piston 1. N OT E When the piston is scratched in a certain part the failure cannot be always detected when using the default stroke setting. Therefore the test should be done also with a stroke of 100 l.
192
Figure 68
Here the pressure test has been done with a stroke of 100 l. The pressure profile gives additional information to the previous plot. When delivering with the small flow rate the pressure increases for a long time but drops only for a relatively short time. With the currently active display of firmware revision 3.0 it can be seen that the pressure drops while the first piston is in the middle of its stroke. This indicates that the piston itself is the source of the problem. The test checks the pressure tightness of the seal over the full length of the piston.
193
Figure 69
Before the pressure reaches the two plateaus there is always a pressure dip when the piston change there direction. Before the pressure reaches the upper limit an oscillating curve can be seen. At the upper limit the pressure is stable. All this indicates that the pump is not working correctly but it is very difficult to locate the source of the problem.
194
Figure 70
The pressure increases in an oscillating curve. When exceeding 270 bar piston 2 delivers with one large stroke into the system and increases the pressure by more than 40 bar. This points already to a problem on the first piston side. Now piston 1 delivers into the system increases the pressure for a short time and then the pressure decreases for the whole plateau. The second plateau looks quite normal and also the upper value when reached after some pressure dips is stable. It is quite obvious that the problem is on the first piston side. In this case the piston is defective.
195
Even with the reduced flow of 0.1 ml/min the pistons deliver with constant rate into the system. After reaching the upper pressure value a continuous pressure drop occurs. This indicates a problem. Therefore the test was repeated with a stroke of 100 l.
196
Figure 72
This pressure profile shows a totally different behavior then the previous one. There are already pressure drops when the flow is 1.0 ml/min and the piston change there directions. When the flow is reduced to 0.1 ml/min the pressure drops with each stroke of the pistons until it is zero. With firmware revision 3.0 it can be checked that the pressure drops appear on both pistons but that the slight pressure increase is generated by piston 1. The piston is scratched in its lower part. Delivering with a small stroke volume into the system generates no problem. With the maximum flow rate of 100 l the scratched part has to move through the seal and is obviously leaking.
197
Figure 73
The both pressure plateaus cannot be reached but when switching to the part where the instrument uses a stroke volume of 4 l the pressure increases up to its normal value. At the upper limit a slight leak rate is visible. The scratches in the lower part of the piston are not visible when the pump is working with its small stroke volume.
198
Figure 74
The pressure profile looks very strange. In the first part the pressure increases up to approximately 320 bar and than it drops down to about 100 bar with normal behavior of the two plateaus and afterwards an increase of the pressure to 400 bar with a slight pressure decrease at the upper limit. Before reaching the first plateau the second piston performs one large (80 l) stroke. At this point the pressure drops. When the piston is moving only with the upper part through the seal no leak can be seen. But when the scratched part of the piston moves through the seal the system is no longer tight and the pressure drops. At the low pressure value the system is still tight and therefore the plateaus show no problem. The pump then reaches the upper limit with 250 l and a stroke volume of 20 l. Here the piston uses again only the unscratched part of the piston.
199
With the reduced flow rate of 0.1 ml/min the pressure increases slowly in an oscillating curve until the upper limit is reached. At the upper limit the pressure is stable pointing onto a problem on the first piston side. The actively current piston display of firmware revision 3.0 shows that the pressure drop is on the first piston side.
200
Figure 76
The test fails completely. The pressure in the system cannot be increased to reach the plateaus at a pressure of more than 100 bar. Also the rest of the test does not reach useful pressure values. Therefore the test provides no information about the problem in the system. N OT E In such a case the pump can be troubleshooted in the following way. Move the solvent inlet tubing out of the bottle and let the pump draw a large air bubble (for example 5 cm in the tubing). In a normal working pump the bubble will move during the intake stroke of piston 1 and will stop when the first piston is delivering into the system. If the active inlet valve is internally leaky the air bubble will move forwards during the intake stroke and the whole time backwards when the piston is delivering into the system.
201
Figure 77
Also the new version of the test fails. The pressure in the system cannot be increased to the two plateaus (>270 bar). The pressure in the system stabilizes below that value. The pump can be troubleshooted as described before.
202
This section provides information on the procedures used for maintenance replacement and alignment of assemblies in the pump. You will find procedures for: Solvent Cabinet and Column Heater Heat Exchanger Solvent Cabinet Cable Assembly Pump Mainframe Active Inlet Valve Outlet Ball Valve Frit Adapter Assembly Purge Valve Pump Head Assembly Continuous Seal Wash Fan Metering Drive Assembly
204
205
Pumps: Maintenance Information Solvent Cabinet and Column Heater Slide the front base back into its guiding slits. Assure that the front edge of the plastic heat shield is guided into the gap between the front panel and the connected metal panel. Tighten the two solvent cabinet screws. Reinstall all capillaries at the column heater assembly.
206
207
Pumps: Maintenance Information Replacing the Active Inlet Valve Using the 12 mm wrench tighten the screw of the valve by turning the assembly in its final position (should not be more than a quarter turn). Make sure that the ESD cover and the solvent sucking tube can be installed with the valve in its position. Fix the spade lug of the shield cable in its position and reconnect the solenoid cable to the connector board. N OT E If the active inlet valve is installed in an instrument without connection for the shield connector connect the spade lug to the holding screw of the connector board. Connect the valve inlet tube to the active inlet valve. Install the ESD cover Perform the pressure tests to verify tightness of the system.
208
209
210
211
There are two different versions of the pump head available. In the latest version the spring is integrated in the plunger housing. The following table shows the serial number prefix at introduction of the new plunger housing design.
Table 45
Pump Head Versions Pump 79851A 79852A/B 79851A 79852A/B SN Prefix 3447 G ..... 3447 G ..... 3448 A ..... 3448 A ..... Procedure 2 2 2 2
212
Pumps: Maintenance Information Procedure 1: Pump Head with old Plunger Housing
N OT E
Since introduction of the new plunger housing design the old plunger housing parts are no longer available. The new parts are fully compatible to all existing pump heads.
213
Pumps: Maintenance Information Procedure 1: Pump Head with old Plunger Housing
214
Pumps: Maintenance Information Procedure 1: Pump Head with old Plunger Housing
215
Pumps: Maintenance Information Procedure 1: Pump Head with old Plunger Housing
216
Pumps: Maintenance Information Procedure 1: Pump Head with old Plunger Housing
217
Pumps: Maintenance Information Procedure 2: Pump Head with new Plunger Housing
218
Pumps: Maintenance Information Procedure 2: Pump Head with new Plunger Housing
219
Pumps: Maintenance Information Procedure 2: Pump Head with new Plunger Housing
220
221
222
223
224
This chapter gives complete parts listings and exploded views for the HP 1050 (Ti) Pumps. Electronic Boards All Ti - Parts Solvent Cabinet Overall Diagram Flow Path Metering Drive Assembly Pump Head Assemblies Active Inlet Valve Outlet Ball Valve Frit Adapter Assembly Purge Valve Assembly Special Tools
226
Electronic Boards
For fuses refer to Table 47 on page 228.
Table 46
Electronic Boards Item Description 1 Power Supply Board 2 Pump Drive Control 2 Board # U 78 MC78L15ACP # U 79 MC79L15ACP 3 Relative A/D Converter 4 Firmware Board 5 Heater Isocratic Board 6 Heater Quaternary Board 7 Communication Interface Board 8 Common Main Processor Board 9 Fluorescent Indicator Module 10 Connector Board 11 Motherboard RAD SFW HRI HRQ CIB CMP FIP CON HPS Part Number DPS-B 5061-3374 PDC2 01018-66532 1826-0274 1826-0281 01018-66503 01018-66506 01018-66517 01018-66518 5061-3382 5061-3380 5061-3376 01018-66505 01018-66501 01018-69518 01050-69582 01050-69580 01018-69503 Exchange PN 01050-69374
# U 78 and U 79 have to be replaced when a new metering device 01018-60001/-69100 (parts included) is installed in a pump with PDC board revision A.
227
Table 47
Fuses Description Fuse 110V operation (3 A) Fuse 220V operation (2 A) Fuse F16 (PDC); F481 (PDC2) 1.5 A Fuse F891, F892 on board 500 mA Fuse F112, F113 on board 500 mA Fuse F12, F22 250 mA Fuse F4 2.5 A Fuse F15 1 A Fuse ICP1 1 A Fuse F1 375 mA Board DPS-B DPS-B PDC2 PDC PDC2 RAD HRI, HRQ HRQ FIP CON Part Number 2110-0003 2110-0002 2110-0304 2110-0934 2110-0934 2110-0004 2110-0083 2110-0007 2110-0099 2110-0421
228
Ti - Pump Head Assembly Ti - Pump Chamber Housing Ti - Active Inlet Valve Ti - Piston Seal Ti - Damping Unit Ti - MCGV Ti - Manual Injection Valve Ti - Rotor Seal Tefzel Ti - Stator Ti - Loop Capillary 20 l Ti - Bottle Head Assembly Ti - Bushing Solvent Glass Filter Adapter Ti - He - Sparge Assembly Ti - Screw Tube Ti - Name Plate Ti - Capillary Piston 1 260 mm lg Ti - Capillary Piston 2 210 mm lg Ti - Tubing ID 0.25 mm 700 mm lg Ti - Sucking Tube
01019-60002 01019-25205 01019-60010 0905-1199 01019-60005 01019-67701 obsolete 0101-0620 0101-0663 0101-0655 obsolete 01019-21734 5041-2168 5062-8517 01019-82702 01019-23232?
Ti - Capillary ID 0.17 35 cm lg
01019-87608
Ti - Maintenance Kit includes: Ti - Piston Seal (2x) PTFE Frits 5/PK Gasket Seal Wash (2x) 6/pk Seal Wash (2x) Seal Gold Outlet (5x) Cap Outlet (5x) 4/pk
01019-68724
01019-68709
Ti - Capillary ID 0.25 13 cm lg Ti - Fitting Insert (2x) Fitting Nut (1x) Fitting Screen (1x) Fitting Insert (1x)
229
Solvent Cabinet
Table 49
Item Description
1 Solvent Compartment incl. (2) 2 Bottle Tub 3 Front Panel Cover Cap, no injection valve Cover Cap, no Helium on/off valve
11 Holder He-Valves 12 Washer 13 Screw 14 Injector Tub 15 Screw M3 4 mm lg 16 Capillary ID 0.17 400 mm lg 16 Ti - Capillary ID 0.17 35 cm lg
Cover Cap, no Helium Regulators 6960-0028 4 Front Base 5 Oven Door 6 Bolt 7 Door Hinge 8 Name Plate 9 Tubing Flexible ID 4 mm OD 5 mm 10 Funnel Leak 01018-43211 01018-40512 01018-60302 01018-43701 01018-45101 5041-2170
17 Accessory Kit, includes following 01018-68704 items Angle Injection Position (part of Sensor Assembly) Sensor Assembly Screw lock female (2x) Washer M4 (2x) 01018-00511 5062-2432 1251-7788 3050-0893
230
Figure 85
Solvent Cabinet
231
1 Solvent Compartment, incl. (2) 2 Front Panel 3 Holder He-Valves 4 Screw 5 Washer 6 Regulator Knob A Regulator Knob B Regulator Knob C Regulator Knob D 7 Knob On/Off 8 Helium Regulator Assembly, includes item 6 an 7 9 Tubing PTFE ID 1/16 OD 1/8 10 Fitting 11 Tubing Flexible ID 0,156 12 Fitting Filter Disc (part of 12) 13 Air Tubing Flexible 5 m
01018-60019 no PN 01018-05501 0624-0045 5001-3746 01018-47413 01018-47414 01018-47415 01018-47416 01018-47412 01018-67001 0890-0746 0100-1430 0890-0581 0100-1047
14 Solvent Bottle, 1 liter 15 Bottle Head Assembly, includes item 16 to 25 15 Ti - Bottle Head Assembly, includes item 16 to 25 16 Bottle Head Cap 17 Bottle Head Shaft 18 Bottle Head Washer Helium Sparge Assembly, includes item 19 and 20
19 Connector Helium Sparger (6/pk) 5062-8515 20 Helium Sparger 10-16 l 21 Solvent Filter SST 21 Solvent Glass Filter Adapter 22 Tube Bushing Teflon 22 Ti - Bushing 23 Tube Screw 24 Tubing FEP ID 1.5 mm OD 3 mm 5 m 25 Tubing PTFE ID 1.45 mm OD 2.5 mm 5 m 5041-8339 01018-60025 5041-2168 5062-8517 79835-21734 01019-21734 5041-2163 5062-2483 5062-2461
5021-7127
232
Figure 86
233
Pumps: Parts Information Solvent Cabinet with Column Heater and Manual Injection Valve
Table 51
Item Description 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21
Solvent Compartment, incl. (2) Front Panel Plug Cable Assembly Heater Washer Screw M4 6 mm lg Heater Assembly Washer Screw M3 16 mm lg Insulation Heat Shield Front Base Oven Door Bolt Door Hinge Waste Vial Vial Holder Holder He-Valves Screw Washer Angle Injection Position
234
Pumps: Parts Information Solvent Cabinet with Column Heater and Manual Injection Valve
Figure 87
235
Overall Diagram
Table 52
Item Description
Overall Diagram
Part Number Item Description Part Number
1 Fan Grill 2 DC Fan 3 Cooling Drain 4 Push Button, white 5 Power Actuator 6 Spring Compression 7 Cover Hinge 8 Sheet Metal Kit 9 Foot Front 10 Cable to Connector Board 11 Connection Tube 150 mm lg 12 MCGV Exchange 13 Connector Board 14 Front Plate 15 Leakage Tray, left 16 Leak Sensor 17 Logo Base 18 Name Plate 19 Front Door 20 Power Switch Base
3160-0544 01048-68500 01018-47706 5041-1203 5041-2162 1460-1510 5041-2147 01018-68701 5041-2161 5062-2416 G1311-67304 79835-67701 79835-69701 01018-66505 01018-04106 01018-44501 5061-3356 5041-2144 5041-2170 01018-60301 5041-2145
35 Screw (plastic) for MCGV 36 no longer used 37 no longer used 38 no longer used 39 Leakage Tray right 40 High Pressure Damper 41 Active Inlet Valve 42 Frit Adapter Assembly 42 Purge Valve 43 Adapter short 44 Outlet Ball Valve 45 Metering Drive Assembly 46 Pump Head Assembly includes item 41 to 44 47 Pump Plate
0515-1256 no PN no PN no PN 01018-44502 79835-60005 01018-60010 01018-60007 G1311-60009 01018-23207 G1311-60008 01018-60001 01018-60004 01018-04704
48 Capillary Piston 1 ID 0.5 27 cm lg 01018-67309 49 Capillary Piston 2 ID 0.5 21 cm lg 01018-67302 50 Power Supply (DPS-B) Exchange 51 PDC2 Board 52 SFW Board (Firmware) 53 RAD Board Exchange 5061-3374 01050-69374 01018-66532 01018-66506 01018-66503 01018-69503
236
Table 52
Item Description
Overall Diagram
Part Number Item Description Part Number
01018-44106 5001-3736
54 HRI Board 54 HRQ Board 56 Motherboard 57 Cover Plate P/S 58 Top Cover 59 Plate Cover, 1.5 inch 60 Plate Cover, 1.3 inch 61 Card Cage 62 Screw M3.5 6 mm lg also for AIV ground cable Screw, ESD cover
23 Leak Assembly, includes item 24, 5062-8551 25, 26 27 Keyboard Module 28 Fluorescent Interface 29 Cable to Display Board 30 Screw M3.5 6 mm lg 31 Bumper 32 Screw M4 6 mm lg 33 Screw M4 20 mm lg (special) 34 Screw M3 8 mm lg 01018-60201 5061-3376 5061-3400 0515-0889 0403-0427 0515-0898 0515-1918 0515-0912
237
Figure 88
238
Figure 89
239
no PN 01018-60025 5041-8339
Gripper MCGV Connector MCGV Ferrule, inlet valve 20/pk Gripper, inlet valve 20/pk Male, inlet valve 20/pk Buffer Disc, inlet valve 40/pk
Connector Helium Sparger (6/pk) 5062-8515 Tubing FEP ID 1.5 mm OD 3 mm 5 m Tube Bushing Teflon Screw Tube 5062-2483 79835-21734 5041-2163
1 Ti - Drawing Tubing, consists of Solvent Glass Filter Adapter Tubing FEP ID 1.5 mm OD 3 mm 5 m Ti - Bushing Screw Tube 2 Connection Tube, consists of
4 Capillary Piston 2 ID 0.5 21 cm lg 01018-67302 4 Ti - Capillary Piston 2 210 mm lg 01019-67302 5 Tubing ID 0.25 mm 700 mm lg 01018-67305
5 Ti - Tubing ID 0.25 mm 700 mm lg 01019-67305 6 Teflon Tubing ID 1 mm OD 3 mm 0890-1764 7 Tubing PTFE ID 1.45 mm OD 2.5 mm 5 m 5062-2461
240
Table 54
Item Description
2 Drawing Tubing, consists of Solvent Filter SST Tubing FEP ID 1.5 mm OD 3 mm 5 m Nut Screw Tube
2 Ti - Drawing Tubing, consists of Solvent Glass Filter Adapter Tubing FEP ID 1.5 mm OD 3 mm 5 m Nut Ti - Screw Tube
241
Figure 90
Hydraulic Path
242
3 Metering Drive Assembly Exchange Assembly, includes item 1, 2, 4, U78 and U79 for PDC board rev. A 1 Cover 2 Screw M2.5 6 mm lg 4 Stay Bolt Figure 91
01018-60001 01018-69100
5021-1839 0515-0887
01018-04704 5021-1841
243
Figure 92
244
Complete Assembly 1 Sapphire Plunger 2 Screw M4 40 mm lg 3 Plunger Housing 4 Support Seal Assembly 5 Plunger Seal (2/Pk) 6 Wear Retainer (10/pk) 7 Outlet Ball Valve 8 Pump Chamber Housing Figure 93
9 Adapter short 10 Active Inlet Valve 11 Screw M5 50 mm lg Tools Wrench 12 mm Wrench 14 mm Insert Tool seals
Teflon Grease
79841-65501
245
Complete Assembly Ti - Complete Assembly 1 Screw M5 50 mm lg 2 Active Inlet Valve 2 Ti - Active Inlet Valve 3 Adapter short 4 Pump Chamber Housing 4 Ti - Pump Chamber Housing 5 Outlet Ball Valve 6 Wear Retainer (10/pk) 7 Plunger Seal (2/Pk) 7 Ti - Seal 8 Seal Keeper 9 Gasket, seal wash (6/Pk) 10 Seal Wash 11 Support Ring Seal Wash
01018-60005 01019-60002 0515-1220 01018-60010 01019-60010 01018-23207 01018-25203 01019-25205 G1311-60008 5064-8249 5063-6589 0905-1199 5001-3743 5062-2484 0905-1175 5062-2465
5063-6586 no PN 01018-60006
Tools Wrench 12 mm Wrench 14 mm Insert Tool, seals Teflon Grease 8710-1841 8710-1924 01018-23702 79841-65501
Accessories Seal Wash Option Update Kit includes tubing, seals (2x), support ring (2x) and items # # Syringe # Adapter Luer (3x) # Abrasive Paper TP 240 # Insert Tool Seal # Seal Keeper (item 8) (2x) 01018-23702 5001-3743 01018-68722
9301-0411 0100-1681
12 Teflon Tubing ID 1 mm OD 3 mm 0890-1764 13 Set Screw M3 8 mm lg 14 Plunger Housing (old version) 15 Screw M4 40 mm lg 16 Spring Compression 0515-1917 order 19 0515-0850 1460-2220
5062-2486
246
Figure 94
247
Table 59
Active Inlet Valve # Description AIV Assembly, complete Ti - AIV Assembly, complete 1 Cap Inlet Valve 2 Gold Seal 3 Retainer Ring, gold coated Part Number 01018-60010 01019-60010 01018-21207 5001-3708 5021-1874
Figure 95
248
Table 60
Outlet Ball Valve # Description Outlet Ball Valve Assembly, complete Ti - Outlet Ball Valve Assembly, complete 1 Socket Cap 2 Housing Screw 3 Outlet Valve Cartridge 4 Gold Seal, Outlet 5 Cap Part Number G1311-60008 01018-60032 5042-1345 01018-22410 no PN 5001-3707 5062-2485
Figure 96
249
Table 61
Frit Adapter Assembly # Description Frit Adapter Assembly, complete 1 O-ring (12/Pk) 2 Housing Screw 3 Adapter 4 PTFE Frit (5/Pk) 5 Gold Seal 6 Cap (4/pk) Part Number 01018-60007 5180-4167 01018-22410 01018-23209 01018-22707 5001-3707 5062-2485
Figure 97
250
Table 62
Purge Valve Assembly # Description Purge Valve Assembly, complete 1 Gold Seal 2 Cap (4/pk) 3 PTFE Frit (5/Pk) 4 Tubing PTFE ID 1.45 mm OD 2.5 mm 5 m Part Number G1311-60009 5001-3707 5062-2485 01018-22707 5062-2461
Figure 98
251
Table 63
Column Holder Assembly # Description Column Holder Assembly 1 Holder Brass 2 Stand 3 Clamp 4 Support Block Part Number 5062-2469 no PN 5001-3738 no PN no PN
Figure 99
252
Special Tools
Table 64
Special Tools # Description Wrench, 12 mm Wrench, 14 mm Insert Tool, Seals Teflon Grease Part Number 8710-1841 8710-1924 01018-23702 79841-65501
253
254
10
10
This section gives information about: Pumps Prefix History Pumps Firmware History Online Monitor Operational Hints Helium Degassing Principle Isocratic Pumps Pump Head Assembly PDC Board HRQ Board Wear Retainer Outlet Ball Valve Flow Test Method Method Loading Flow Gradients Manual Injection Valve
256
Product History
Since introduction of the 1050 Pumps in 1988 a couple of hardware and firmware changes have been implemented in production. With most of this changes the serial number prefix has been changed too. Following is a list of all prefix changes done in Waldbronn and Little Falls.
Table 65
Product History 79851A and 79852A/B S/N Prefix 2813 G ..... 2913 G ..... Changes Introduction of the 1050 Pumps ESD cover added to the gradient valve. Hardware changes of extrusion and holding bracket for the MCGV. Wear retainer installed in front of each seal. Introduction of the current pump head version. In the meantime all old pump heads have been updated. Introduction of firmware revision 3.0 and introduction of column heater. Introduction of HRI/HRQ Board (HRQ replaces GVD board).
2949 G ..... 2949 A..... 3010 G ..... 3012 A ..... 3016 G ..... 3019 A .....
3031 G ..... 3034 A ... (51A) or Introduction of firmware revision 3.1 3032 A ... (52A) 3045 G ..... Purge Valve added to all quaternary pumps
3106 G ..... 3106 A ... (51A) or New voltage regulators on PDC board (rev B), 3107 A ... (52A) exchange metering drives require a PDC update. 3117 G ..... 3117 A ... (51A) or Introduction of firmware revision 3.2 3118 A ... (52A) 3206 G ..... 3243 G .....3244 A...(51A) or 3145 A...(52A) Introduction of dedicated seal and hardware modifications of pump chamber and seal keeper Introduction of PDC2 board.
257
Table 65
Product History 79851A and 79852A/B S/N Prefix 3312 G ..... 3334 G ..... Changes Integrated spindle for metering drive assembly 01018-60001 Support seal assembly replaces support ring and seal keeper
3404 G ..... 3404 A ... (51A) or Introduction of Damper with new pressure sensor and 3405 A ... (52A) electronic board (Rev. G) 3447 G ..... 3448 A ..... June 1996 March 1998 November 1998 September 2001 Spring integrated in plunger housing Active Inlet Valve with Exchangeable Valve Cartridge Plunger Housing with new springs available Part Number Change for DC-Fans End of Support of 1050 Isocratic Pump 79851B TI ends September 30, 2001
Table 66
Product History Solvent Cabinet S/N Prefix 3019 G ..... 3205 G ..... 3216G... Changes Solvent Cabinet 79856A/B serialized Improvement of Helium Regulators; better regulation range and tightening behavior. Modification of Bottle Head Shaft of the Bottle Head Assembly.
258
Firmware History
Revision 1.0
Revision 1.0 was the firmware at introduction of the 1050 Pumps. Known Problems In purge mode flow values above 5 ml/min will not be shown on the display. At higher values the display remains at 5 ml/min but the pump is purging with the set value.
Revision 3.0
Europe/ICON US/Canada SN 3016 G..... SN 3019 A .....
Revision 3.0 incorporates: Communication with the GPIB communication interfaces. Support of the column heater. Improved flow test method. Known Problems 1 If a gradient test method is started directly after running the build in flow test method the gradient might be distorted. Switching the pump off and on again after a pressure test solves the problem. 2 For applications with system pressures below 30 to 40 bar the lower pressure limit is not applicable. 3 Internal tests of the DOS workstation (Phoenix) revealed a couple of bugs in the communication part of the firmware.
259
Revision 3.1
Europe/ICON US/Canada SN 3031 G..... SN 3034 A ..... (for 79851A/B) SN 3033 A ..... (for 79852A/B) This firmware revision fixes the bugs encountered with the ChemStation. Known Problems Due to an internal timing problem relay contact 1 and 2 may switch incorrectly when used together in the timetable. Relay contact 2 might be activated together with contact 1 even when the timetable shows only an entry for contact 1.
Revision 3.2
Europe/ICON US/Canada SN 3117 G..... SN 3117 A .....
260
261
Normal Operation
The figure below shows the normal pressure profile of the instrument. The curve is ideal and can only be recorded with a very fast transient recorder. A normal integrator (339X) is too slow to record the very fast changes of the curve and shows a smoothed one. However occurring operation problems can be also seen on a integrator plot. During the delivering strokes of the two pistons the instrument measures the pressure at the points D1 to D10. Failure conditions like leaks or gas bubbles influence the pressure curve from which the processor can determine certain failure modes. Figure 100 Online Diagnostic: Normal Operation
262
M2 Gas Bubble
The following figure shows the pressure profile when a gas bubble was drawn from the bottle. During the delivery phase of piston I the gas bubble will be compressed first before solvent can be delivered into the second chamber. This means the pressure will drop during the compression phase of the air bubble before it returns to normal behavior. The pressure profile of the second piston shows no deviation. The pressure drop at the beginning of the stroke generates a higher pressure ripple which is used to determine a gas bubble problem. The pressure ripple is depending on various parameters like solvent, flow, compressibility and so on. For this reasons the pressure ripple has to exceed a certain range before a gas bubble can be detected. The relation between pressure ripple and compressibility setting is shown in the respective figure. N OT E Drastic pressure changes (for example suddenly no more solvent to pump due to empty bottle) can not be detected under all circumstances. To make sure that the system will stop in such a case (for example running out of solvent during an unattended sequence) a lower pressure limit should be set. Online Diagnostic: Gas Bubble
Figure 101
263
Figure 102
264
265
M6 Valve Backflow
The following figure shows the pressure profile when the outlet ball valve is not working correctly. Delivery stroke of piston I shows normal behavior while during the stroke of piston II the pressure drops because of the internally leaking ball valve. Figure 104 Online Diagnostic: Outlet Ball Valve Backflow
266
267
268
Helium Regulators
The helium regulators allow the regulation of the helium flow. The regulator design does not allow to set the helium stream to zero. A small flow of helium is still possible.
269
Isocratic Pumps
Isocratic pumps are often sold without the solvent conditioning module option. The bottle is then placed beside the instrument. Tests have shown that best results in regards of pressure ripple stability, air sensitivity and so on are reached when the solvent bottle is placed on top of the module or even higher (for example on top of a stack of modules). The slight gravity pressure reduces the under pressure the pump requires to draw solvent from the solvent bottle.
270
PDC Board
When exchanging the metering drive assembly 01018-69100 in a pump with PDC Board revision A installed (see Product History on page 257), the voltage regulators U78 and U79 on the board have to be replaced. Parts are included in the exchange metering drive. PDC Board revision B and greater and the PDC2 Board do not have the new type voltage regulator already installed. A short in the active inlet valve cable (for example cable squeezed between pump head and metering drive) will generate excessive current on the components of the PDC board. This overcurrent will at least damage (unsolder) one resistor on the board. The fuse added to the CON board (introduction approximately January 1992) will prevent damage of the PDC board.
PDC2 Board
In a standardization (board will also be used in other APG products) and cost reduction program part of the circuit was implemented in ASIC (Application Specific Integrated Circuit) which allowed a reduction in board size. A stainless steel plate and the cover plate assure compatibility to the 1050 board.
271
HRQ Board
Originally the fuse F16 on the HRQ board was a 500 mA type. Evaluation of returned defective exchange boards showed that the fuse was blown in most of the cases. The fuse was to weak and could be blown without circuit failure. Therefore the fuse was changed to a 1 A type.
GVD Board
At introduction of the 1050 Pumps the Gradient Valve Driver (GVD) board controlled the multi channel gradient valve (MCGV). During the design phase of the column heater option it was decided that the control of the heater should be also done via the same board. Therefore the GVD was replaced by the HRQ board for control of column heater and gradient valve (see Product History on page 257).
Wear Retainer
The abrasion of the seal is a very well known fact. The wear retainer is a device which keeps the departed particles around the seal instead of allowing to move immediately into the flow path. The retainer consist of a small porous Teflon disc placed directly in front of the seal. When installed the retainer disc deflects and with the piston diameter slightly bigger than the one of the Teflon disc a recess for the seal material is build. With the operation time the plunger will widen the diameter of the disc allowing part of the particles to move into the flow system. Therefore the wear retainer should always be changed together with the seal. The high pressure filter in the purge valve will collect all this materials without problem. When changing the seals also the high pressure filter should be changed too.
272
Method loading
If a method will be loaded while pumping, the pump might be switched off when there is a lower pressure limit set in the new method.
Flow Gradients
Timetables containing flow gradients with a starting point of 0 ml/min will not be executed. Gradient parameter changes will always be executed at the culmination point of the first piston. With a flow set to zero, this point will never be reached.
273
274
275
PANIC Errors
Intermittent PANIC errors are mostly generated by spikes (disturbances) on the bus lines. A dynamic bus termination has been added to the FIM board to suppress the spikes and to reduce the possibility of this failure mode. All firmware boards with revision C and higher do have the dynamic bus termination installed (RC-network instead of a R-network). In case of intermittent PANIC errors replace FIM boards (rev A or B) with the current version.
276
In This Book This manual contains technical information about the Agilent 1050 liquid chromatographs. This manual is available as electronic version (Adobe Acrobat Reader file) only.
Copyright Agilent Technologies 2001 All rights reserved. Reproduction, adaption, or translation without prior written permission is prohibited, except as allowed under the copyright laws. Part No. NONE 11/2001 Printed in Germany
Warranty
The information contained in this document is subject to change without notice. Agilent Technologies makes no warranty of any kind with regard to this material, including, but not limited to, the implied warranties or merchantability and fitness for a particular purpose. Agilent Technologies shall not be liable for errors contained herein or for incidental or consequential damages in connection with the furnishing, performance, or use of this material.
IMPORTANT NOTE This version of the 1050 service manual includes all sections from the 01050-90102 edition 4 (1995) and G1306-90102 edition 2 (May 1994). It merges both sections, the MWD and the DAD. The series I opticals information (79854A MWD) information has been removed (product went out of support during 2000). Part numbers have been updated as of 11/2001. Contact your local Agilent support office in case of part number issues or upgrades. The latest version of this manual is available as Adobe Acrobat Reader (PDF) version only and can be downloaded from the Agilent Technolgies web page www.agilent.com.
11
11
This chapter gives general information on about this autosampler repair policy product structure capillaries specifications
282
Repair Policy
The 1050 Autosampler is designed that all components are easy accessible. Customers are able to repair certain parts of the 1050 Autosampler, see Operators Handbook. For details on repair policy refer to Repair Policy on page 38.
Product Structure
The 1050 Series of HPLC modules are available in two versions. In the standard version most of the parts in the flow path are stainless steel. In the 1050 Ti Series the flow path of the autosampler consists solely of corrosion resistant materials such, as titanium, tantalum, quartz, sapphire, ruby and fluorocarbon polymers. It is recommended for use with mobile phases containing high salt concentrations, extreme pH solutions and other agressive mobile phases. Autosampler Ti - Autosampler 79855A 79855B
283
Capillaries
In the 1050 Series all capillary shipped with the modules will have a plastic colour coating for identification in terms of material and internal diameter.
Table 67
Capillary Color Code color blue green red white Internal Diameter 0.25 mm 0.17 mm 0.12 mm tantalum Material
N OT E
The capillaries for the 1050 Series will have only one color coating for the internal diameter. The capillaries for the 1050 Ti Series have two color coatings. One for identifying the material, covering the main part of the capillary, and a small one for the internal diameter. For the 1050 Ti Series the fittings are always titanium with a titanium nitrite coating and the front and back ferrules are gold plated.
284
Specifications
Table 68
Specifications of 1050 Autosampler Injection Range Programmable from 0.1 to 100 l in 0.1 l increments without hardware change required. Up to 1.8 ml with larger injection valve capillary. 1-99 from one vial. Typically <0.5% RSD of peak areas from 5-100 l and <1% from 2-5 l 1 l can be sampled from 5 l in 100 l micro vial or 10 l in 300 l micro vial. <0.1% typically None required, sample path flushed continuously with mobile phase during normal operation. 0.2 - 50 cp 21 or 34 in standard trays, with additional 100 in external tray (less two positions for access). <4 seconds from standard tray. 20 seconds typically, depending on injection volume and drawing speed. 2.3 to 9.5 standard; 1.0 to 12.5 optional (TEFZEL replaces VESPEL rotor). Solvent with pH below 2.3 should not contain acids which attack stainless steel. Ti-Series pH 1 to 14. Integrated keyboard with function keys; parameter editing possible during run; keyboard lock. Optional control by PC or 3396 Series II integrator. Injection volume, draw offset, sample draw/eject speed, 2 external contacts, stop time, post time, injector program.
Replicate Injections Precision Minimum Sample Volume Carryover Wash Cycle Sample Viscosity Range Sample Capacity Random Vial Access Injection Cycle Time Recommended pH Range
Control
Method Parameters
285
Table 68
Specifications of 1050 Autosampler Methods Battery-backed storage of up to 10 methods. Automatic startup and shutdown methods. Editing of stored methods possible during run. Up to 10 parameter sets, each with keyboard setup of: first- and last sample vial, # of injections per sample vial, first- and last calibration vial, # of injections per calibration vial, re-calibration frequency and injection method. Editing of stored parameter sets possible during run. Inputs: start request. Outputs: BCD for bottle number; start; two external relay contacts (one 24 V relay, one 30 V (AC/DC) contact closure, both 0.25A). In- and Outputs: stop, ready, shut, down. Optional interface for GPIB and RS-232C. Extensive diagnostics, error detection and display via front-panel LEDs and status logbook. User-definable shutdown method activated in case of error. Leak detection, safe leak handling, leak output signal to shutdown pump. Low voltages in major maintenance areas. 4C to 55C (constant temperature) with <95% humidity (non-condensing) 1C to 60C using external circulating bath with thermostat. Line voltage: 100-120 or 220-240 VAC 10% Line frequency: 48-66 Hz Power consumption: 120 VA max. Autosampler Dimensions Height: 208 mm (8.2 in) Width: 325 mm (12.8 in) Depth: 560 mm (22.0 in) Weight: 16 kg (35 lb)
Sequence Parameters
Communications
Safety Aids
286
12
12
This chapter gives general and technical information about the hardware components of the 1050 Autosampler. Overview about the Autosampler Autosampler hardware Sampling Unit Metering Drive Analytical Head Assembly High Pressure Switching Valve Pneumatic Assembly Additional 100 vial capacity
288
Overview
The 79855A/B Autosampler is a fully programmable module and is controlled via the user interface. The operator sets the parameters at the user interface which provides also the required analytical information. The processor controlled electronic drives the mechanic of the 79855A/B Autosampler consisting of sampling unit metering device and high pressure valve unit. The pump delivers flow to a six port high pressure valve unit in which a sampling unit and a metering device take the place of a sample loop. In normal mode the needle of the sampling unit is held firm in its seat forming a leak free seal. The valve unit directs the solvent through the metering device and the sampling unit to the column. During injection the flow is bypassed and the metering device loads the sample. Needle and metering device are always flushed and ready for the next injection.
289
290
291
1 Injection Sequence I
2 Injection Sequence II
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293
Sampler: Hardware Information What happens when the 18596L/M Sample Tray is connected?
294
295
Figure 107
296
Sampling Unit
Repair Level: Component (see Parts ID)
Table 69
Part Numbers Sampling Unit Item Sampling Unit Ti - Sampling Unit Part Number 01078-60001 01079-60001
The Sampling Unit comprises two functions, control of needle movement and positioning the respective vial under the needle. The sampling unit is controlled by the needle mini tray drive board (NMD). The stepper motor for the needle movement is connected to a lead screw which moves the needle arm with the needle up and down. Lightswitches at the needle arm check for upper and lower limit of the needle and also check the presence of a vial during the injection cycle. The second stepper motor drives the coupler which holds the sample tray. The home position of the tray is determined when a little magnet in the tray is located directly above the home sensor. Standard sample tray with 21 vials or micro tray with 34 vials are identified by the polarity of the tray magnet (north pole for standard tray and south pole for the micro tray). A quadrature encoder on the coupler shaft allows accurate positioning of the tray.
297
Table 70
Technical Data Sampling Unit Number of spindle motor steps between upper and lower limit Number of spindle motor steps between upper limit and needle in vial position Needle speed Spindle Number of encoder wheel slits Resolution of the tray Reproducibility of tray position Tray speed Sealing Force Ti Series Materials in contact with solvent: tantalum, titanium, Peek, gold 5867 steps (44 mm) 5334 steps (40 mm) 20 mm/sec 200 steps (1.5 mm)/revolution 500 2000 steps/revolution 1 mm 2.3 seconds/revolution 50-55 N
Figure 108
Sampling Unit
298
Metering Drive
Repair Level: Assembly or component level for given parts (see Parts ID)
Table 71
Part Numbers Metering Drive Item Metering Drive Part Number 01078-60002
The Metering Drive is responsible for drawing the sample into the sample loop. The stepper motor controlled by the Valve Metering Drive Board (VMD) drives the spindle via a belt. The circular movement of the spindle is transformed in a linear movement for the piston via a bronze nut. A light sensor determines the home position of the piston.
Table 72
Technical Data Metering Drive Resolution of mechanical system Number of steps between extension limits 7 nl/step of motor 15000
Figure 109
299
Table 73
Part Numbers Metering Drive Item Analytical Head assembly Ti - Analytical Head assembly Part Number 01078-60003 01079-60003
The sapphire piston moves up or down the spindle on a bronze nut. The built in spring prevents clearance affecting drawing accuracy. Piston movement in the analytical head is guided by a sapphire ring. On the backward stroke the piston draws sample from the vial.
Table 74
Technical Data Analytical Head Maximum stroke Ti Series Materials in contact with solvent Filled Teflon, sapphire, titanium 100 l
Figure 110
300
Table 75
Part Numbers Metering Drive Item High Pressure Switching Valve Ti - High Pressure Switching Valve Part Number 01078-60004 01079-60004 Exchange 01078-69004 01079-69004
The High Pressure Switching Valve bypasses the flow direct to the column during the injection cycle. The valve is air driven. The switching positions of the valve are sensed with a light switch that provides a status signal to the Valve Metering Drive (VMD) indicating proper execution of any movement.
Table 76
Technical Data High Pressure Switching Valve Ti Series Materials in contact with solvent Tefzel, titanium, ceramic
Figure 111
301
Pneumatic Assembly
Repair Level: Component (see Parts ID)
Table 77
Part Numbers Pneumatic Assembly Item Pneumatic Assembly Part Number 01078-66101
Air supply is connected from the rear of the module to a self latching solenoid valve. Pressure is sensed for an under pressure condition (<5 bar) with a sensor that provides an electrical status signal. Air pressure is applied to the SUP connector of the valve. In normal position pressure is connected to connector CYL1.When the solenoid is activated by a pulse, the air stream is directed to outlet CYL2 and the air pressure moves the 6 port valve and forces it to stay there. Air pressure is applied to the SUP connector of the valve. In normal position pressure is switched to connector CYL1 and when the valve is switched it moves to CYL2. Both exhaust outlets (EXH1/EXH2) are connected together at the rear of the module. The air leaves through a filter to reduce the noise during the switching. Electrical control of the valve is from the Valve Metering Drive (VMD). Figure 112 Valve Connections
302
For test reasons the actuator air solenoid may be switched manually.
Table 78
Switching of Solenoids Screw A Screw B Cyl #1 0 1 0 0 0 0 0 0 1 0 SUP SUP SUP EXH EXH Cyl #2 EXH EXH EXH SUP SUP Solenoid ready for next switch Solenoid ready for next switch Comment Relaxed Position
Figure 113
Pneumatic Assembly
303
Table 79
For access of the additional vials the firmware adds 100 to each tray position so that the 100 sample tray holds the positions 101 to 200. The arm of the 100 sample tray moves the selected bottle into position 16 of the 21 sample tray. Position 15 has to be empty for the undisturbed movement of the tray arm. After the injection the vial is placed back into its original position in the large tray. The remaining vial range of the 21 sample tray (1 to 14 and 17 to 21) is fully accessible. The firmware automatically skips vial 15 and 16. N OT E Service Information about the 18696A/B can be obtained from the 7673 Service Manual for the A tray and for the B tray.
304
Figure 114
305
306
13
13
This chapter gives information about the electronic of the 1050 autosampler: Overview Max Tray Drive Board (MTD) Needle Mini Tray Drive Board (NMD) Valve Metering Drive Board (VMD) Firmware Board (FIM) Autosampler Motherboard (ALM)
308
Overview
All electronic boards (except the FIP, behind the keyboard) are located in the rear part of the module and they are connected to the Motherboard (ALM). Excess to the boards is from the rear of the instrument. Slot numbers (for example in the status display) are counted from left to right. The Power Supply (DPS-B) is located in slot 1 and the common main processor is located in slot 7. The rear of the autosampler is shown in Figure 115 on page 310. In the Autosampler the following electronic assemblies are available:
Table 80
Electronic Boards
Description Part Number Exchange
Power Supply (DPS-B) Common Main Processor (CMP) # Max Tray Drive Assembly (18596A/L) (MTD)
## Max Tray Drive Assembly (18596B/M) (MTD) 01078-66513 # Rotor Reader Drive Assembly (G1926A) (RRC) 01078-66507 Valve Metering Drive (VMD) Needle Mini Tray Drive (NMD) Firmware Board (SFW) Motherboard (ALM) Display Interface Board (FIP) Communication Interface (CIB) # Optional board 01078-66501 01078-66502 01018-66506 01078-66504 5061-3376 5061-2482
01078-69501 01078-69502
## Optional board, attached to the MTD board (not described in this manual)
309
N OT E
For information about Power Supply, Common Processor and Fluorescent Interface refer to chapter 1050 Common Information. Rear of 1050 Autosampler
Figure 115
N OT E
310
Figure 116
311
Table 81
Part Numbers for MTD Board Item MTD Board 18596M MTD Board 18596L RRC Board for both versions Part Number 01078-66513 01078-66503 01078-66507 Exchange 01078-69513 01078-69503
N OT E
The RRC board will be attached to the MTD board when Rotor Reader Option (G1926A) for the 100 vial tray is installed. The function of the board is to control the 18596L/M sample tray and to provide the electrical interface to the common main processor (CMP). The 18596L/M is part of the 7673A product family. I/O Control The I/O control circuit enables the common main processor (CMP) and the maxi tray drive (MTD) to exchange data. This is done via a bidirectional I/O buffer. A board identification (a resistor network) allows the processor to identify the board and to address. Sensor Status Via the sensors interface circuit the sensor status is transferred to the sensor status latch. The sensor status latch transfers the information via the common bus to the CMP.
312
Data Conversion While the common main processor bus has a parallel data structure the Main Processor Unit (MPU) uses a serial data bus. The data conversion section performs the parallel to serial and serial to parallel conversion for the different bus structures. Figure 117 Block Diagram MTD Board
Clock The clock circuit provides all necessary frequencies for the main processor unit (MPU) and the data conversion section. It uses a 4.9152 MHz clock generator.
313
Main Processor Unit (MPU) The MPU is the heart of the MTD board and controls all the functions of the 18596L sample tray. All the necessary memory needed to run the 100 tray resides inside the MPU chip. The MPU chip provides all the signals for the motor drivers and sends a tray fault signal out in case of malfunctions. To control all the steps of the tray the MPU reads the sensor status from the sensor interface. Reset and Watchdog This circuit checks for proper operation of the Main Processor Unit (MPU). In case of malfunctions (for example timing problems and so on), the reset and watchdog resets the system preventing any damage of the 18956L tray. The System OK Signal (SOK) from the Common Main Processor (CMP) is also fed into the reset and watchdog block. In case of 79855A processor problems or problems which influence the SOK status, the reset and watchdog will also reset the MTD board. Motor Drivers Three motors control all the movements of the 18596L 100 sample tray. The radial arm drives (R-Motor) and the gripper drives (Z-Motor) are similar. To keep the position of the arm or the gripper mechanism when not turning the motors are powered down to maintain a standby torque. The angular driver (Theta-Motor) provides a constant standby current in chopper mode and normal on/off switching of the motor windings at standard speed. Sensor Interface Three position sensors are located in the tray to provide feedback as to the position of the tray arm. An additional sensor in the gripper on the arm to indicates the presence of a bottle. The bottle sensor is simply a micro switch which provides a short ground when the bottle is present. The two position sensors that are used to sense the home positions for radial (R) axis and gripper (Z) axis are hall sensors that provide a logic low output when they encounter a suitable magnetic field. Small permanent magnets are placed in the appropriate positions in the tray. The angular (Theta) axis position sensor is an optical photo diode transistor pair. The photo diode is turned on only when the motor is being actuated. The interlock is a sense line which identifies whether the sample tray (cable) is installed or not.
314
Figure 118
315
Table 82
Part Numbers for NMD Board Item NMD Board Capacitor 100 pF (between pin 5 and 7 of U26) Part Number 01078-66502 0160-4801 Exchange 01078-69502
The main function of the NMD board is the control of needle motor and tray motor. Capacitor 100pF Firmware revision 4.0 and above require a modification of the NMD board. Otherwise incorrect positioning of the 21 or 34 vial tray may occur. The 100 pF capacitor soldered between pin 5 and 7 of U26 solves the problem. Instruments with serial number prefix 3117 G ..... or 3121 A ..... do have this capacitor. I/O Control The I/O control circuit enables the common main processor and the needle mini tray drive (NMD) to exchange data. This is done via a bidirectional I/O buffer. A board identification circuit allows the processor to identify the board and to address it. BCD Output The circuit codes the bottle number into BCD and provides the signal to the connector on the back of the NMD board. The BCD code is implemented in positive true logic. Firmware REV 2.0 and above allow configuration of the output for either 2 digit BCD coded or 8 bit binary (HEX) coded information.
316
Figure 119
317
Sensor Status The hall sensor, the bottle sensor and the needle sensor are connected to this circuit block. The hall sensor checks the presence of the sample tray and is used to set the home position. The bottle sensor checks for the presence of a bottle during injection cycle. The needle sensor checks upper and lower position of the needle. The status information from the sensors are transferred directly to the processor. Control Logic The control logic provides the motor parameters to the motor driver. The parameters are the direction, resolution and current for the motors. The control logic starts the timer and stops it under two conditions. In case a light sensor detects the home position or the number of steps of the motor have been elapsed, the timer will be stopped. To increase the life time of the sensors the control logic activates the light sensors only during the injection cycle and switches it off afterwards. Timer The timer chip of the timer circuit consist of three independent timer/counter stages from which only two are used. One timer generates the speed (step frequency) of needle and sample tray motor. The second timer defines the number of steps the motor has to perform to reach its selected destination (needle position). Motor Driver The motor driver delivers the power to the two motors. A bipolar phase controller allows a high torque at high frequency for the movement. Quadrature Decoder The quadrature encoder on the tray coupler senses the movement of the sample tray. The derived signals contain information of the direction and the actual position of the tray motor. The decoder reads the signals and transfers the information to the processor.
318
Figure 120
319
Table 83
Part Numbers for NMD Board Item Valve Metering Drive (VMD) Fuse F12, F14 250 mA Part Number 01078-66501 2110-0004 Exchange 01078-69501
The main functions of the board is to control the Metering Drive and the High Pressure Switching Valve. In addition the VMD board holds also the firmware for the common main processor (CMP).The firmware is attached to the VMD board but has no functional connection to the board. I/O Control The I/O control circuit enables the common main processor and the Valve Metering Drive (VMD) to communicate data. This is done via a bidirectional I/O buffer. A board identification circuit allows the processor to identify the board and to address it. Control Logic The control logic provides the motor parameters to the motor driver circuit. The parameters are the direction, resolution and current for the metering drive motor. The control logic starts the timer. It stops it in case the home position light switch is activated or the motor steps have been elapsed. To increase the life time of the sensors the control logic activates the light sensors only during the injection cycle and switches it off afterwards. The pneumatic valve will be switched via the valve driver circuit to change the position of the high pressure switching valve.
320
Figure 121
321
Relay Contact Control Two relay contacts are controlled. When activated, contact 1 provides fused (250 mA) +24 V, while contact 2 provides a fused (250 mA) 30 V maximum (AC/DC) rated contact closure. For more information about the relay contacts see External Contacts on page 56 in the chapter 1050 Common Information. Timer The timer chip of the timer circuit consist of three independent timer/counter stages from which only two are used. One timer generates the speed (step frequency) of the metering motor. The second timer defines the number of steps the motor has to perform to reach its selected destination (volume). Motor Driver The motor driver delivers the power to the motor. A bipolar phase driver allows a high torque for the movement. Sensor Status The metering home sensor the valve position sensor and the air pressure switch are connected to the sensor status circuit. The home position sensor checks whether the piston of the metering unit is in the maximum front position or not. The valve position sensor checks the switching of the bypass valve. The air pressure switch senses low air pressure in the system and inhibits further injections. The metering motion status signal gives the information whether the metering drive motor is running or not. The signal is derived from the timer circuit. The switch (S28) is not used so far and is reserved for future use.
322
Figure 122
323
Table 84
Part Numbers for FIM Board Item Firmware Board (New) Part Number 01078-66506
The FIM board is a piggy back board, placed on VMD board (personality module). The programmed FIM contains the firmware of the 1050 Autosampler. The board is designed for on board programming. The FIM contains 128K x 8bit EPROMs. All inputs/outputs are pulled down for electrostatic discharge protection. Figure 123 Layout of FIM Board
324
Table 85
Part Numbers for ALM Board Item ALM Board Part Number 01078-66504
The motherboard contains all connectors for the boards and the assemblies in the front part, like sampling unit, metering drive, high pressure switching valve, pneumatic valve and keyboard. Figure 124 on page 326 shows the location of all connectors. A mechanical Injection Counter displays the actual number of injections counted by switching valve transitions.
325
Figure 124
Table 86
ALM Connectors J1 - Power Supply J2 - TAR Board J3 - VMD/FIM Board J4 - NMD Board J5 - Not used J6 - Not used J7 - CMP J8 - FIP Keyboard J9 - DGND J10 - Bottle Sensor J11 - future option J12 - Needle Motor J13 - Tray Motor J14 - Shaft Encoder J15 - Hall Sensor J16 - Needle Sensor J17 - Leak Sensor J18 - Home Sensor J19 - Metering Motor J20 - Valve Position J21 - Low Pressure Switch J22 - Pneumatic Solenoid Valve
Figure 125 on page 327 to Figure 127 on page 329 show the main signals and voltages of the various boards and connectors.
326
Figure 125
327
Figure 126
328
Figure 127
329
Table 87
Part Numbers for Extender Test Board Item Extender Test Board Cable Assembly Part Number 01078-66509 01078-61609
The extender test board in combination with the cable assembly allows the operation of sampling unit metering drive and high pressure switching valve taken out of the autosampler module. The test board contains all the connectors for the different items and holds some electronic for troubleshooting and sensor adjustment. Figure 128 shows the circuit diagram of the test board. The LEDs CR1 to CR7 show the actual status of the sensors. An LED which is ON indicates that the sensor is either blocked or deactivated. The sensors are only activated during the injection cycle. Figure 128 Extender Test Board
330
Figure 129
331
332
14
14
This chapter provides information about diagnostic steps error messages additional information
334
Single Steps
The autosampler has several test functions which are part of the control section. The test functions provides access to the single steps of the injection sequence. If the 18596L/M sample tray (100 sample tray) is installed the firmware provides also single steps for this tray.
335
SINGLE STEP 1
336
SINGLE STEP 5
SINGLE STEP 5 NEEDLE INTO VIAL Sampling unit lowers needle into vial. The stepper motor executes a defined number of steps to lower the needle. No sensor is involved in this action. Do not execute this step a second time. Otherwise the needle will be lowered again by the same number of steps. This means that the needle hits either the bottom of the vial or the plastic of the sample tray (if no vial is present). No error message will occur.
SINGLE STEP 6
SINGLE STEP 6 DRAW UP Metering device withdraws plunger drawing up sample according to selected injection volume. For each injection volume the metering device motor performs certain steps to withdraw the plunger. Multiple execution of this step will withdraw the plunger until it reaches the maximum position. No error will occur.
SINGLE STEP 7
SINGLE STEP 7 NEEDLE OUT Sampling unit raises needle out of vial. The needle motor is activated until stopped by the interrupter sensor, which is activated at upper position. Multiple execution of the step are possible without any problem (needle moves always up until it reaches the upper position and is moved back).
SINGLE STEP 8
SINGLE STEP 8 MINITRAY HOME Sample tray moves back to home position. The number of encoder steps performed under step 4 will be executed in opposite direction. The home sensor is not involved in this action. Multiple execution of this step are possible without any problem (tray remains in home position).
SINGLE STEP 9
SINGLE STEP 9 NEEDLE DOWN Sampling unit lowers needle into needle seat. Lower position is determined by the activation of the interrupter sensor. Multiple execution will create an error message (E19) because light path of sensor is already blocked.
SINGLE STEP 10
SINGLE STEP 10 MAINPASS Switches switching valve to direct mobile phase through metering device and sampling unit and then into column. Light switch recognizes the change of the position. Multiple execution of this step will create an error message (E20) because the light switch will not be activated again.
337
Sampler: Diagnostic Information Single Steps for the 100 Sample Tray
C A UT I O N
Single steps can be performed in any order and the step sequence is under the control of the operator. In case of incorrect step sequences damage of gripper assembly tray arm and other parts of the instrument might be possible. Multiple execution of the steps should be avoided, because of occurring error messages or possible damage of the instrument. SINGLE STEP 1 INIT 100 TRAY 100 sample tray performs an initialization. Multiple execution of this step causes no problem.
SINGLE STEP 1
SINGLE STEP 2
SINGLE STEP 2 MOVE TO POS 101 From the home position the tray arm moves to the position 1 of the 100 sample tray. The firmware does not support access to other vials. Do not execute the step a second time. Otherwise the arm performs the same number of steps again and moves into the mechanical stop.
SINGLE STEP 3
SINGLE STEP 3 PICK UP VIAL The gripper assembly moves down, picks up the bottle and the gripper moves up to home position (determined by a hall sensor). Second execution of this step will lead to incorrect position in step 4.
338
Sampler: Diagnostic Information Single Steps for the 100 Sample Tray
SINGLE STEP 4
SINGLE STEP 4 MOVE TO 21 TRAY Tray arm moves vial to the 21 sample tray position and stops above vial position 16 of the tray. Do not execute this step a second time, because the arm would move into the mechanical stop.
SINGLE STEP 5
SINGLE STEP 5 INSERT VIAL Gripper assembly moves down and places the vial into the 21 sample tray and gripper returns to home position. Down position of the gripper can be influenced via the teach tray mode. Do not execute the step a second time. Otherwise incorrect positioning of the tray arm will occur and the following steps might show incorrect results.
SINGLE STEP 6
SINGLE STEP 6 REMOVE VIAL Gripper assembly picks up the vial from the 21 tray. Step is similar to step 2.
SINGLE STEP 7
SINGLE STEP 7 MOVE TO POS 101 From the 21 sample tray the arm moves back to the position 1 of the 100 sample tray. Second execution should be avoided, otherwise the tray arm moves into the mechanical stop.
SINGLE STEP 8
SINGLE STEP 8 INSERT VIAL The gripper assembly moves down and replaces the vial into its original position.
SINGLE STEP 9
SINGLE STEP 9 HOME 100 TRAY The tray arm is moved back to the home position. This step is not identical with the initialization of the tray arm.
339
340
341
Error Messages
The error messages will help to locate and repair a possible failure. In case an error message appears the Error LED will be turned on and the message will be written into the system logbook. RESET INJECTOR clears the error message. The entry in the logbook remains. The error messages are divided into the following blocks: Selftest PANIC Error Common 1050 Messages Error Messages for Firmware Revision 4.0 and greater Injector Program Error Messages for Firmware Revision 3.1 and below Events 18596L/M vial tray
342
Selftest
RAM and display can be tested via the build in selftest. The selftest will be performed when CTRL will be pressed while the module is turned on at the LINE ~ switch. In case of a failure one of the following messages appears. The complete test requires approximately two minutes. ROM test failed ( ROM test failed ) The ROMs on the FIM board are tested. In case of a checksum error the ROM test fails. Replacement of the FIM board will probably fix the problem. RAM test failed ( RAM test failed ) The RAMs on the CMP board will be tested. In case of a failure the error message appears and the CMP has to be replaced.
Panic Error
Bus Error Address Error PANIC: XXXXXXH BUS ERROR PANIC: XXXXXXH Address ERROR The panic error messages should not appear under normal operation conditions. In case of hardware or firmware problems the instrument might try to access a wrong or not existing address which results in the error message on the display. The instrument is locked up and has to be switched off/on. Reason for the PANIC error message can be any disturbance on the bus lines due to bad contacts (high resistance) or defective IC on any of the boards. Check boards for good connections or corrosions at the contacts (clean contact pins). Check firmware revision of the firmware board (SWF). It should be revision C or higher. Boards with revision C do have a dynamic bus termination for spike suppression on the bus lines. Replace one board at a time to identify the faulty one. If board replacement will not cure the problem, replace the motherboard.
343
344
E02 HH:MM DDMMM shut down > error in other module An external device pulled the shut down line of the remote connector down. This forces the autosampler to stop all further injections.
E03 HH:MM DDMMM error method > error method has been loaded The operator may define an method as a error method. The event message gives the information that the instrument detected an error and that the error message has been loaded.
E04 HH:MM DDMMM time out > The operator may define a time period after which the instruments stops all further actions. In case the instrument is in a sequence and a not ready has been detected in one of the other modules the instrument will stop the sequence after time out time has been elapsed.
345
Sampler: Diagnostic Information Error Messages for Firmware Revision 4.0 and greater
346
Sampler: Diagnostic Information Error Messages for Firmware Revision 4.0 and greater
E13 HH:MM DDMMM inject failed > needle has not been raised The motor is activated and moves the needle arm out of the seat or vial. In the upper position the interrupter pin blocks the light path of the interrupter sensor. The motor is stopped and the interrupter pin is moved out of the lights witch. Both positions upper limit and lower limit are determined by the same lights witch (interrupter sensor). Check for blockages of the sensor. Check for proper connection of motor and sensor. Check for smooth movement of the spindle system. Check for smooth movement of the bottle vane (bottle sensor). Check drive nut. Change NMD board. Change interrupter sensor.
E14 : Vial position not E14 HH:MM DDMMM inject failed > found vial position not found During the initialization, the sample tray determines its home position (magnet above home sensor). The shaft encoder mounted onto the tray coupler provides the information to reach the various vial positions of the tray. If the selected position cannot be reached the error message will appear. Possible failure modes are blockages of the mechanical system, defective encoder or a electronic problem. Check for mechanical blockages of the mechanical system (sample tray, tray coupler, belt and so on). Check all cable connections. Change NMD board. Change encoder.
347
Sampler: Diagnostic Information Error Messages for Firmware Revision 4.0 and greater
E18 : Home position of E18 HH:MMDDMMM inject failed > tray not found home position of tray not found After moving the requested vial to the injection position the sample tray moves back to its home position. The encoder checks the movement of the tray. If the tray cannot be moved the error message will appear. Failure modes might be mechanical blockages of the tray or problems from the encoder. Check for blockages of the system. Check Encoder signal. Check Home sensor signal. Change NMD board. E19 : Needle has not been lowered E19 HH:MM DDMMM inject failed > needle has not been lowered From the upper position the needle gets the command to move down into the seat or vial. In case of malfunctions the error appears. A defective bottle in place sensor might also generate the error. Check the needle motor and sensor connection. Check for blockages of the mechanical system. Check sensor signal. Check for smooth movement of the bottle vane (bottle sensor). Lubricate bottle vane. Change NMD board. Check bottle in place sensor. E20 : Valve not moved E20 HH:MM DDMMM inject failed > to mainpass valve not moved to mainpass Last step in the injection sequence is to turn back the high pressure switching valve into its main pass position. Problems in the air supply, sensor or board problems may cause the error message to appear. Check the pneumatic assembly. Check cable connections. Check sensor adjustment. Change VMD board.
348
Sampler: Diagnostic Information Error Messages for Firmware Revision 4.0 and greater
E22 HH:MM DDMMM inject failed > plunger home pos not found The plunger of the metering device is moved forward until the home position sensor indicates the maximum allowed front position. In case the home sensor cannot be recognized the plunger moves into the mechanical stop. The motor will be stopped after the programmed time out has been elapsed. Second possibility is that the motor does not start and the plunger will not move at all. After time out the error message appears. Possible failure modes are a misadjusted or defective sensor or a defective motor. Check for proper connection of motor and sensor. Change VMD board. Check alignment of sensor. Change sensor.
E24 HH:MM DDMMM inject failed > tray home pos not found During the initialization the sample tray determines its home position (magnet above home sensor). If the home position could not be recognized the error appears (for example sample tray not installed). At the begin of an injection the system checks for the presence of the home sensor. If this cannot be recognized the tray will be positioned incorrectly and the error will show up. Check the magnet of the sample tray. Check for mechanical blockages of the mechanical system (sample tray, tray coupler and so on). Check tray motor. Change encoder. Change NMD board.
349
350
Sampler: Diagnostic Information Normal Operation Messages for Firmware Revision 3.1 and below
351
Sampler: Diagnostic Information Normal Operation Messages for Firmware Revision 3.1 and below
E16 : Plunger failed to E16 HH:MM DDMMM inject failed > draw sample plunger failed to draw sample From the home position the plunger is moved back a certain number of steps to draw the requested volume. Failure mode is the electronics of the VMD board. Check connections of metering motor. Change VMD board. E17 : Needle did not move out of vial E17 HH:MM DDMMM inject failed > needle did not move out of vial The needle motor is activated to move the needle in its upper position. If this action fails the error appears. Possible failure mode is the interrupter sensor, spindle motor or the NMD board. Check interrupter sensor. Change NMD board. E23 : Needle has not been raised E23 HH:MM DDMMM init failed > needle has not been raised During this step the needle is raised from any position. In case this step fails the error message appears. Check for blockages of the sensor. Check for proper connection of motor and sensor. Check for smooth movement of the spindle system. Check drive nut. Change NMD board. Change interrupter sensor.
352
Sampler: Diagnostic Information Normal Operation Messages for Firmware Revision 3.1 and below
E25 HH:MM DDMMM init failed > needle has not been lowered From the upper position the needle driver gets the command to move the needle down into the seat. In case of malfunctions the error appears. Firmware revision 2.0 and above connect the functioning of the needle sensor and the bottle in place sensor. If the bottle in place sensor is defective the error will also appear. Check the needle motor and sensor connection. Check for blockages of the mechanical system. Check for smooth movement of the bottle vane (bottle sensor). Lubricate bottle vane. Check sensor signal of interrupter and bottle in place sensor. Change NMD board.
353
Events Messages
Event messages give the operator informations about the performed action of the instrument. Messages will appear in the logbook. E26 : No vial in sam[ple tray E26 HH:MM DDMMM missing vial > no vial in sample tray During the injection sequence the bottle in place sensor checks for the presence of a vial. If no vial is in the tray the message appears in the logbook. Depending on the system configuration (stop/cont/skip at missing vial), the message is interpreted as an error or a event message. If the vial sensor is not connected or defective error message E19 will appear. Place a bottle into vial position. Check bottle in place sensor. Check cabling of sensor board. Change sensor. Change NMD board. E29 : Sequence done E29 HH:MM DDMMM sequ done > sequ exec finished Sequence finished is an event message. It records the correct termination of an automated operation. E30 : Sequence aborted E30 HH:MM DDMMM sequ aborted > sequ exec aborted Sequence either stopped by operator or error occurred during operation. In case of an error the Error lamp will be on. Check next logbook line for more information.
354
355
E34 HH:MM DDMMM inject failed > serious error in 100 vialtray Error appears when the tray arm is not able to move to its selected position. Reset autosampler. Check cable connection. Change MTD board. Check tray arm.
E35 : Teach of 100 vial E35 HH:MM DDMMM teach done > tray done teach of 100 vialtray done Event message indicating use of the teach tray function. E36 : Vial number for unknown device E35 HH:MM DDMMM teach done > teach of 100 vialtray done This error appears when an incorrect vial range has been set. Example: The vial range was specified 1 to 30 for the 34 vial tray. When the 21 vial tray is installed the autosampler will show error E36 when reading 22 or greater. E38 : Barcode verification failed E38 HH:MM:DDMMM verified failed barcode verification failed The error can only be seen when the DOS workstation is connected to the autosampler with 100 vial tray and barcode reader. The label from the vial will be verified with the setting for the analyzed vial position. A mismatch will generate the error message. Check vial label and computer information for correctness. Check/replace barcode reader and driver board. E39 : Error state of 100 E39 HH:MM:DDMMM injector aborted > vial tray error state of 100 vial tray The error appears when a previous error on the 100 vial tray is still present (error LED blinking) and a new action for the 100 vial tray has been started.
356
15
15
This chapter describes the procedures that have to be performed during servicing and maintenance of the 1050 Autosampler. You will find procedures for: Sampling Unit Metering Device Analytical Head High Pressure Switching Valve Sensor Adjustments
358
Sampling Unit
N OT E Needle and needle seat changes can be performed without removing the sampling unit. For stage 2 it is necessary that the needle is in the needle change position.
359
360
361
362
363
Figure 131
364
Metering Device
N OT E Move the plunger into the plunger change position before removing the metering device from the instrument.
365
Table 88
New Analytical Head Assembly Autosampler 79855A/B 79855A/B SN Prefix 3404 G ..... 3406 A ..... Version new; Procedure2 new; Procedure 2
N OT E
Follow this instruction when either changing Plunger Seal or Plunger. Do not forget to use the plunger change position in the control section before removing the analytical head assembly. The numbers in brackets refer to Figure 132 on page 367.
366
Stage 2: Changing the Seal Remove the seal keeper (11) from the head (13). Using the three millimeter hexagonal key remove the seal (12). Clean the head chamber (13) from all seal particles. Best is to use a degreaser spray (for example 8500-0232). Insert a new seal (12). Stage 3: Disassembling the Body Remove the support ring (10) or the support seal assembly. Hold the body down on a flat surface loosen the setscrew (15) and carefully release the tension of the spring. WA R N I N G Figure 132 The spring will catapult the body up if released without holding it. Analytical Pump Head Assembly (old)
367
Stage 4: Reassembling the Analytical Head Assembly Place sapphire plunger (7) and spring (8) into the spring support (6). Place the adapter (9) on a flat surface and insert the parts from the previous step. Hold the adapter (9) from one side with the thumb and press the spring support (9) with plunger and spring with the fingers into the body. Hold the spring support (6) with one hand in place and fix the setscrew. Slide the support ring (10) or the support seal assembly onto the plunger. N OT E If the support ring (10) or the support seal assembly sticks at the body when sliding down the plunger push the plunger (7) slightly from the bottom. This will center the plunger and the ring keeper slides into its position. Place the seal keeper (11) on the seal (12) of the head. N OT E In this position the seal keeper guides the plunger into the seal and reduces the possibility to break the plunger. Carefully place the head (13) onto the adapter (9). Turn the assembly upside-down insert the screws (14) and fix them stepwise with increased torque. N OT E It is important that the surface of head and adapter are parallel to each other to obtain a good seal.
368
369
Figure 133
Stage 3: Reassembling the Analytical Head Assembly Prepare the head (6) as described beforehand. Place the adapter housing (3) without the piston (1) onto the head (6). Insert the two screws (2) and tighten until hand tight. N OT E Tightening the screws fully will require much more force to push the piston into its position in the seal. Insert the piston (1) into the adapter housing (3) and carefully push it into the seal. Tighten the two screws (2) stepwise with increasing torque. Make sure that head and adapter surfaces are in parallel.
370
371
Stage 2: Disassembling
Loosen and remove the three socket head stator screws (4). Remove the stator (2) from the top of the valve. Remove the stator ring from the valve. Take special care not to lose the stop pins in the stator ring. Using the blade of a screwdriver, release the rotor seal from the valve.
372
Figure 134
373
374
N OT E
EXECUTE STEP allows the performance of the step commands (Test Functions) by entering the step number. #1 Switch Valve Unit to bypass. #2 Initialize Metering Device. #3 Raise needle. #4 Move vial underneath needle. #5 Lower needle. #6 Draw sample up from sample vial. #7 Raise needle. #8 Move vial to home position. #9 Lower needle. #10 Switch Valve Unit to flow through sample loop. INSTR# allows to read the position of the various sensors and can be used for adjustment of sensors. An negative number (for example -2) writes the actual value into the processor memory for adjustment calculations. For more information see chapter sensor adjustment. #1 Reads the position of the shaft encoder. for example INSTR# 1 VAL 1 ; 0 #2 Reads the left stop of the sample tray. for example INSTR# 2 VAL -56 ; -56 #3 Reads the right stop of the sample tray. for example INSTR# 3 VAL 53 ; 53 #4 Calculate correction value for measurement performed under #2 and #3. The result is shown in m. for example INSTR# 4 VAL 251 ; 251 #5 Reads the data which represents the actual sensor status for the complete sampling unit (interrupter home and bottle sensor). for example INSTR# 5 VAL 227 ; 227 after initialization. Depending on the sensor which is activated or not the value changes in increments of 1, 4, 8. 8 for the sample tray 4 for the bottle in place sensor 1 for interrupter sensor.
375
N OT E
#6 Reads the data which represents the actual sensor status for the metering home sensor and the valve position sensor. Readings can be used for sensor adjustment or troubleshooting. for example INSTR# 6 VAL 240 ; 240 after initialization. Depending on the sensor which is activated or not the value changes in increments of 1 or 8. 8 for the metering device home sensor. 1 for the valve position sensor.
N OT E
Interrupter Sensor: Initializes a signal to stop the needle motor at upper and lower limit. The adjustment ensures a defined force for the needle into the seat and determines the position of the needle in the sample vial during the injection cycle. Home Sensor: Determines the home position of the sample tray. The processor counts the selected vial number relative to the home position. Adjustment ensures that the needle hits the septa of the sample vial in each vial position. Bottle in Place Sensor Checks for presence of a vial during the injection cycle. No adjustment required. Quadrature Decoder Checks the actual position of the 21 sample tray for adjustment of the 21 vial tray. If the 34 vial tray is installed the more precise procedure should be selected. No adjustment required. The home sensor will be adjusted with the build in service level test features. For the interrupter sensor there are two adjustment procedures available. Adjustment can be done via the extender test board which is the easiest way because of the accessibility of the sensor. If the test board is not available the features of the service level also allow adjustment of the sensor.
376
Adjustment of Interrupter Sensor with test board With the test functions commands move the needle into upper position. By turning the motor coupler move the needle arm downwards until the interrupter pin just touches the upper plate. Now move the needle arm upwards 1 mm. N OT E One revolution of the spindle moves the needle arm 1.5 mm up. Therefore 240 represent 1 mm. Position the sensor that the LED on the extender board just changes its state from on to off (should remain off) and fix it in this position. Adjustment of Interrupter Sensor via Service Only Level Follow steps 1 to 3 of the previous described procedure. Enter SERVICE ONLY level. Move to the Instr# and enter #5 to get the following display. INSTR# 5 VAL 239 ; 239 (without sample tray) Position the interrupter sensor that the value just changes to 238. Move it back until you reach 239 and fix it in this position. Adjustment of Home Sensor - procedure for 21/34 vial tray N OT E During RESET of the autosampler the processor finds the home position of the sample tray and stores the actual dehydrator encoder reading as zero position. The position of vial #1 is used as reference for the adjustment. With INSTR# 1 the processor reads the steps from the home position to the actual position. If the tray is aligned correctly the encoder should read the following values for the position of vial #1: 21 vial tray: VAL 0;-200 tolerance 1 34 vial tray: VAL 0;-191 tolerance 1 The above values can be obtained from the SERVICE ONLY level.
377
Adjustment Procedure Remove door, inner cabinet and the top cover from the autosampler. Make sure that the tray is installed correctly and that the vial is in position #1. Using the CTRL functions of the instrument RESET the autosampler. Enter the TEST FUNCTIONS. Use single steps 3 to raise the needle. In the display SINGLE STEP 4 POS. TRAY AT 10 change the vial position to 1 (use > ) and press 1 ENTER. They tray moves to position #1. The needle should point to the center of the vial. If not, turn the tray manually until the position is correct. *Enter the service only level and select the following display INSTR# 1 VAL 0; -XXX. N OT E XXX is the value for the actual position of the tray. If the home sensor is adjusted correctly, the value should be -191 1 for the 34 vial tray or -200 1 for the 21 vial tray. If XXX differs from the above values the sensor has to be adjusted. 6 counts represent approximately 1mm. Remove the tray, loosen the sensor screws and move the sensor Towards the front of the autosampler (ccw) when the actual values of XXX are larger then the nominal (for example -199 for 34 vial tray; or -205 for 21 vial tray). Towards the back of the autosampler (cw) when the actual value of XXX is smaller then the nominal (for example -185 for 34 vial tray; or -195 for the 21 vial tray). Verify the correct position. Insert the tray, RESET the injector and repeat step 4 to 8 of this procedure.
378
379
380
16
16
This chapter gives diagrams for parts identification and the complete parts listings respectively for the 1050 (Ti) Autosampler. Electronic Boards Ti - Parts Overall Diagram Solvent Flow Path Sampling Unit Metering Drive and Analytical Head High Pressure Switching Valve Pneumatic Valve Assembly
382
3 Maxi Tray Drive Board for 18596B/M MTD 4 Rotor Reader Drive Board 5 Valve Metering Drive Board 6 Firmware Board 7 Needle Mini Tray Drive Board 8 Communication Interface Board 9 Common Main Processor Board 10 Fluorescent Indicator Module 11 Motherboard RRC VMD FIM
NMD 01078-66502 CIB CMP FIP ALM 5061-3382 50613380 5061-3376 01078-66504
Fuses
Table 90 Fuses Description Fuse 110V operation (3 A) Fuse 220V operation (2 A) Fuse F12, 250 mA Fuse: ICP1 1 A Board DPS-B DPS-B VMD FIP Part Number 2110-0003 2110-0002 2110-0004 2110-0099
383
Table 91
Description
Ti - Needle Ti - ZDV Fitting Ti - Loop Capillary 100 l ID 0.5 1.08 m lg Ti - Valve Metering Capillary ID 0.25 140 mm lg Ti - Seat Capillary ID 0.17 180 mm lg Ti - Capillary 500 l Volume ID 0.5 2.8 m lg Ti - Capillary 2 ml Volume ID 0.94 2.8 m lg Ti - Flush Union
High Pressure Switching Valve Exchange Ti - Rotor Seal TEFZEL pH 12.5 Ti - Pump Capillary ID 0.25 70 cm lg Ti - Sampling Unit Ti - Needle Seat (Peek)
384
Overall Diagram
Part Number Item Description Part Number
1 Foot Support 2 100 Sample Tray 3 Tray Support Assembly 4 Screw M3.5 6 mm lg 5 Cover Hinge 6 Screw M3.5 6 mm lg 7 Fan Holder 8 Fan Assembly
21 Flexible Tubing (12ft) 22 Press Switching Cable 23 Nut M4 24 Pneumatic Assembly 25 Screw M4 35 mm lg 26 Name Plate 27 Logo Base 28 Front Panel 29 Inner Cabinet 30 Screw M3.5 8 mm lg 31 Power Switch Base 32 Leak Assembly, includes 33, 34, 35 36 Sample Tray 37 Sample Tray 34 vials 38 Sampling Unit 39 Screw M3.5 6 mm lg 40 Flexible Tubing (12ft) 41 Connector 42 Muffler 43 Adapter 44 Connector, long
5021-7127 01078-61601 0535-0056 01078-66101 0515-1666 5041-2170 5041-2144 01078-60301 01078-64401 5021-1862 5041-2145 5062-8551 01078-44501 01078-44511 01078-60001 0515-0887 5021-7127 0100-1175 0100-1176 79846-23202 0100-1047
Fan Upgrade Kit (for ALS without 01078-68720 fan) 9 Screw M4 20 mm lg (special) 10 Sheet Metal Kit 11 Screw M3.5 6 mm lg 12 Bumper 13 Foot Front 14 Push bottom, white 15 Actuator 16 Spring Compression 17 Front Plate 18 Leak Sensor 19 Screw M3 10 mm lg 20 Leak Tub 0515-1918 01078-68701 0515-0889 0403-0427 5041-2161 5041-1203 5041-2162 1460-1510 5001-3725 5061-3356 0515-1105 01078-44502
385
Table 92
Item Description
Overall Diagram
Part Number Item Description Part Number
45 Valve Metering Capillary ID 0.25 140 mm lg 46 Top Cover 47 Loop Capillary 100 l ID 0.5 1.08 m lg 48 DPS-B 49 Plate Cover P/S 50 MTD Board (18596A/L) Exchange 50 MTD Board (18596B/M) Exchange 51 Cover large (3 inch) 52 FIM Board 53 Screw M3 6 mm lg 54 VMD Board Exchange 55 NMD Board Exchange 56 Cover small (1.3 inch) 57 CMP Board Exchange 58 Screw M5 10 mm lg
01078-87301 01078-04110 01078-87302 5061-3374 5001-3728 01078-66503 01078-69503 01078-66513 01078-69513 01078-04115 01078-66506 0515-0912 01078-66501 01078-69501 01078-66502 01078-69502 5001-3721 5061-3380 01050-69580 0515-1117
59 Screw M4 6 mm lg 60 Analytical Head Assembly 61 Metering Drive 62 Cable; FIP to ALM 63 HPS Valve Exchange 64 Valve Waste Capillary ID 0.5 130 mm lg 65 Screw M4 6 mm lg 66 Screw M5 6 mm lg 67 Valve Base Plate 68 Valve Holder Plate 69 Card Cage 70 Keyboard Module 71 Fluorescent Interface 72 ALM
0515-0898 01078-60003 01078-60002 5061-3400 01078-60004 01078-69004 01078-87304 0515-1963 0515-1117 part of (10) 01078-02310 part of (10) 01078-60201 5061-3376 01078-66504
386
Figure 135
387
Figure 136
388
1 Pump Capillary ID 0.25 70 cm lg 1 Ti - Pump Capillary ID 0.25 70 cm lg 2 Valve Metering Capillary ID 0.25 140 mm lg 2 Ti - Valve Metering Capillary ID 0.25 140 mm lg 3 Loop Capillary 100 l ID 0.5 1.08 m lg 3 Ti - Loop Capillary 100 l ID 0.5 1.08 m lg 4 ZDV Fitting 4 Ti - ZDV Fitting 5 Needle (fitting laser welded) 5 Ti - Needle 5 Needle Grooved 6 Seat Capillary ID 0.17 180 mm lg 6 Ti - Seat Capillary ID 0.17 180 mm lg
01078-87306 01079-87306 01078-87301 01079-87301 01078-87302 01079-87302 0100-0900 5021-1871 01078-67200 01079-67201 01078-67202 01078-87303 01079-87303
6 Multi Draw Kit, includes 500 l Volume ID 0.5 2.8 m lg 2 ml Volume ID 0.94 3.1 m lg Flush Union 6 Ti - Multi Draw Kit, incudes Ti - Capillary 500 l Volume ID 0.5 2.8 m lg Ti - Capillary 2 ml Volume ID 0.94 2.8 m lg Ti - Flush Union
7 Column Capillary ID 0.17 80 cm lg 7 Ti - Column Capillary ID 0.17 70 cm lg 8 Valve Waste Capillary ID 0.5 130 mm lg
389
Figure 137
390
Sampling Unit
Table 94
Item Description
Sampling Unit
Part Nmber Item Description Part Nmber
Complete Assembly Complete Ti - Assembly 1 2 3 4 5 6 6 7 8 9 10 11 12 13 14 15 16 17 Tray Motor Assembly Screw M3 12 mm lg Washer Screw M2.5 6 mm lg BOS Board Screw M3.5 6 mm lg (older version) Screw M3.0 6 mm lg Washer Cable Clamp Retaining Ring Washer Spring Bearing Sleeve Sampler Body Screw M2.5 6 mm lg Washer Home Sensor Traction Relief Tray Coupler
01078-60001 01079-60001 01078-64702 0515-1110 3050-0890 0515-0894 01078-66505 0515-0887 0515-0886 3050-0892 1400-0082 0510-1310 3050-1299 1410-1261 no PN 0515-0894 3050-0890 5180-0861 5001-3752 01078-43201
18 19 20 21 22 23 24 25 26 27 28 28 29 29 30 31 32 33 34 35
Lubrication Ring Coupler Assembly Plug Hole Motor Coupler Set Screw M5 10 mm lg Belt Belt Roller Bearing Sleeve Washer Screw M3 25 mm lg Needle Seat Ti - Needle Seat (Peek) Seat Capillary ID 0.17 180 mm lg Ti - Seat Capillary ID 0.17 180 mm lg Socket Shock Mount Screw M3 6 mm lg Spindle Motor Assembly Spring Needle Arm Assembly
5001-3749 01078-63201 6960-0076 1500-0796 0515-1741 1500-0698 01078-22501 1410-1253 3050-0891 0515-1060 79846-67101 01079-67101 01078-87303 01079-87303 01078-25201 1520-0260 0515-0886 01078-64703 1460-2365 01078-60000
391
Table 94
Item Description
Sampling Unit
Part Nmber Item Description Part Nmber
36 37 38 39 40 41 41 42 42 43
43 44 45 46 47 48 49 49
Ti - ZDV-Fitting Needle (fitting laser welded) Connector Cable Traction Relief Quadrature Encoder Screw M2.5 25 mm lg Screw M3.5 6 mm lg (older version) Screw M3.0 6 mm lg Gear Cover Bumper Foott
5021-1871 01078-67200 01078-61602 5001-3752 1990-1265 0515-1640 0515-0887 0515-0886 01078-04101 0403-0282
Screw M3.5 6 mm lg (old version) 0515-0887 Screw M3.0 6 mm lg Needle (old design) Ti - Needle ZDV-Fitting 01079-67201 0100-0900 0515-0886
50 51
392
Figure 138
Sampling Unit I
393
Figure 139
Sampling Unit II
394
Arm Spare Part Kit 1 Bottle Vane Screw 2 Screw M3.5 10 mm lg Figure 140
01078-68706 no PN no PN
no PN no PN
395
Metering Drive
Part Nmber Item Description Part Nmber
01078-60002 no PN 1500-0697
Analytical Head Assembly Ti - Analytical Head Assembly 6 Spring Support 7 Sapphire Plunger 8 Spring 9 Adapter 10 Support Ring 10a Support Seal Assembly
01078-60003 01079-60003 no PN 5063-6586 1460-2220 see new version order (10a) 5001-3739
11 Seal Keeper 12 Seal (2/pk) 12 Ti-Seal 13 Head Body 13 Ti - Head Body 14 Screw M4 40 mm lg 15 Set Screw M3 5 mm lg 16 Screw M5 60 mm lg
396
Figure 141
397
Analytical Head Assembly Ti - Analytical Head Assembly 1 Sapphire Plunger 2 Screw M4 40 mm lg 3 Adapter with spring 4 Support Seal Assembly Figure 142
398
High Pressure Switching Valve Assembly Exchange Assembly excluding items 11 to 17 Ti - New Assembly Exchange Assembly excluding items 11 to 17 1 Rotor Seal VESPEL Ti - Rotor Seal TEFZEL pH 12.5 2 Stator 3 Isolation Seal 4 Stator Screw 5 Stator Set Screw 6 Bearing Ring
01078-60004 01078-69004 01079-60004 01079-69004 0101-0626 0101-0627 1535-4044 1535-4046 1535-4857 no PN 1535-4045
7 Valve Sensor Board 8 Bracket Actuator 9 Screw M5 6 mm lg 10 Elbow Fitting 11 Valve Waste Capillary ID 0.5 130 mm lg 12 Valve Holder Plate 13 Valve Base Plate 14 Screw M5 6 mm lg 15 Screw M4 6 mm lg (flat head) 16 Screw M3.5 8 mm lg 17 Screw M2.5 6 mm lg
79846-66504 79846-01206 0515-1510 0100-1408 01078-87304 01078-02310 part of 01078-68701 0515-1510 0515-1963 0515-1105 0515-0894
399
Figure 143
400
Pneumatic Assembly
Part Nmber Item Description Part Nmber
Complete Assembly excluding items 5, 6 and 7 1 Solenoid Valve 2 Low Air Pressure Switch 1/8 3 Push-in Fitting Male Figure 144
401
402
17
17
This section gives the following informations: Autosampler Prefix History Autosampler Firmware History Update to Firmware Revision 4.0 Adding the 100 vial tray Intermittant E17 Update the autosampler with a fan
404
Product History
Since introduction of the 1050 Autosampler in 1988 a couple of hardware and firmware changes have been implemented into the production. With most of this changes the serial number prefix has been changed too. Following is a list of all prefix changes done in Waldbronn and Little Falls.
Table 101
Changes
Introduction of the 1050 Autosampler Introduction of firmware revision 2.0 Introduction of firmware revision 2.1 #024 (add 100 vial capacity) for support of 18596B/M tray Fan Assembly added to the autosampler Introduction of 1050 Ti Autosampler Introduction of firmware revision 3.1 Introduction of firmware revision 4.0 Support Ring for Analytical Head with Ceramic Insert Introduction of firmware revision 4.1 New Revision of High Pressure Switching Valve Modification of ALM board to increase fan voltage Introduction of support seal assembly Introduction of firmware rev. 4.2 Analytical Head - Spring integrated in the adapter Needle with integrated Fitting Adapter (Analytical Head) with new spring Sampling Unit - ZDV Fitting Laser welded to the Needle
405
Firmware Revisions
Firmware Revision 1.0
Rev 1.0 was the firmware at introduction of the 79855A Autosampler. Known Problem: Time table execution Problem is in the timetable execution, if there is more then one entry in the timetable. Manually stop of the run (before elapsing the stoptime) may lead to wrong behavior of the relay contacts in the next run. Workaround/Solution 1 To stop a run manually reduce the stoptime to a value lower then the actual run time. 2 Other 1050 modules do not show this problem and can be used as an alternative to control the relay contacts.
Firmware revision 2.0 incorporates: Support of 18596A/L sample tray. Configuration of BCD output (either 2 digit BCD or 8 bit binary coded) Draw Offset Position for the needle. Fix of revision 1.0 bug.
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Revision 2.1 incorporates: Support of 18596B/M sample tray (Killer Bee). N OT E The 18596B/M sample tray is not compatible to the 18596A/L tray. It does requires a change in firmware and hardware (MTD board). Nevertheless firmware revision 2.1 support both versions of the tray. Known Problem: Intermittant BUS ADDRESS ERRORS Intermittant BUS ADDRESS ERRORS or similar lock ups of the autosampler may occur when the 100 vial tray is connected. A firmware bug in combination with a weak air supply genereates the problem. During the injection cycle a underpressure condition may be detected. This condition might be misinterpreted and then leads to the error.
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Revision 3.0 incorporates: Communication with the HPIB communication interfaces. Support of the Roto Reader of the 18596A/B tray. Support of the 34 vial tray in the autosampler. Introduces the AUTO-ON feature. Known Problems Serious Problem with 21 vial tray. If the 21 vial tray is not in home position at the begin of an injection, the tray will be recognized as 34 vial tray and positioned accordingly. Damage of the needle can be the result. Any time the 21 vial tray has been moved or replaced, perform a RESET INJECTOR prior to starting an injection. Reset during injection Break. If the injection cycle is interrupted (injection break-stop during injection) and followed by a RESET INJECTOR hardware crashes may appear. It was observed that either the syringe piston was forced into the mechanical stop or the tray was moved against the needle arm. Swtching off and on the autosampler will cure the problem. Do not use the RESET INJECTOR during injection break. Teach Mode If one of the possible teach modes (tray or bar code reader) is done without a vial in position 101 the autosampler is forced into an error mode. The error LED is blinking and the display shows the value 3000. ESCAPE and RESET INJECTOR brings the autosampler back into the normal operation mode.
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The final tests for the DOS workstation revealed some firmware bugs in the autosampler firmware. Revision 3.1 fixes these communication bugs. Known Problems Problems with Relay Contact 2. Relay Contact 2 generates a double pulse each time it is turned on or off. Intermittant E26, E32, E33 or E34: 100 vial tray arm moves two vials into position #16 of the 21 vial tray. A firmware bug in the synchronization between the autosampler and the 100 vial tray generates the problem. The firmware expects that the metering syringe is already in home position before the 100 vial tray places its vial into the 21 vial tray. With large injection volumes (for example100 l) and lower eject speed (for example <200 l) the initialization of the syringe takes longer then the movement of the tray arm. Set the EJECT SPEED to at least 300 when using larger injection volumes.
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Revision 4.0 incorporates: Support of Injector Program. Introduction of additional displays. Changes in tray movement. Addition of error messages. Fixes of known bugs. N OT E Autosamplers with serial number prefix below 3117 G ..... and 3121 A ..... need a modification of the NMD board when updated to revision 4.0. A capacitor (100 pF part number 0160-4801) has to be soldered between pin 5 and 7 of U26 on the NMD board. Known Problems Incorrect BCD output for vials in 100 vial tray. When working from the 100 vial tray the transfer position is always used as output for the BCD output. Therefore the bottle number displayed on the integrator is always 16 for BCD, or 10 for BIN, if the bottle number is transfered via a BCD cable. PHOENIX and LC APPAC do not show the problem. Using the injector program feature allows a work around for the problem. {{ 10 DRAW def l from SMPL SPEED def l/min OFFSET def mm}} {{ 20 UTILITY OUTPUT SMPL }} Intermittant hang-up of a sequence that uses overlap and return mode for the 100 vial tray. Adjustment of the sampling unit home (hall) sensor via the service only is not possible. INSTR# 4 gives incorrect values.
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Revision 4.1 incooperates: Fix of the three known bugs of revision 4.0 The default transfer position is redifined (better position). The utility tray move command of the injector program allows to use the sample vial option now. The wait after a post time represents a seperate event (for future workstation only). Keep/Return configuration changes during the injection are possible now.
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Table 102
Compatibility Table 18596A/L Firmware SN Prefix MTD Board MTD firmware (U33) 2.0 or higher 2848 G / 2902A 01078-66503 / -69503 18596B/M 2.1 or higher 2944 G / 2950 A 01078-66513 / -69513 18594-80295
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Update of existing Autosampler Check wether the fan of the autosampler is running or not. Make also sure that the fan will start at turn on of the module. If not, replace R1 on the motherboard with the 33.2 Ohm resistor. Identify R1 which is located next to the connector J8 for the keyboard cable. Cut the wires of the 100 Ohm resistor close to its body. This allows you to solder the new 33.2 Ohm resistor (0757-0995) to the existing wires without removing the ALM board from the card cage.
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In This Book This manual contains technical information about the Agilent 1050 liquid chromatographs. This manual is available as electronic version (Adobe Acrobat Reader file) only.
1050 Series of HPLC Modules Service Handbook Diode Array Detector (G1306A) and Multiple Wavelength Detector (79854A)
Copyright Agilent Technologies 2001 All rights reserved. Reproduction, adaption, or translation without prior written permission is prohibited, except as allowed under the copyright laws. Part No. NONE 11/2001 Printed in Germany
Warranty
The information contained in this document is subject to change without notice. Agilent Technologies makes no warranty of any kind with regard to this material, including, but not limited to, the implied warranties or merchantability and fitness for a particular purpose. Agilent Technologies shall not be liable for errors contained herein or for incidental or consequential damages in connection with the furnishing, performance, or use of this material.
IMPORTANT NOTE This version of the 1050 service manual includes all sections from the 01050-90102 edition 4 (1995) and G1306-90102 edition 2 (May 1994). It merges both sections, the MWD and the DAD. The series I opticals information (79854A MWD) information has been removed (product went out of support during 2000). Part numbers have been updated as of 11/2001. Contact your local Agilent support office in case of part number issues or upgrades. The latest version of this manual is available as Adobe Acrobat Reader (PDF) version only and can be downloaded from the Agilent Technolgies web page www.agilent.com.
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This chapter gives general information on about this detector repair policy features user-interfaces specifications
Repair Policy
The 1050 DAD/MWD is designed that you can access all components easily. Customers are able to repair certain parts of the 1050 DAD/MWD described in the User Handbooks. For details on repair policy refer to Repair Policy on page 38 in chapter 1050 Common Information.
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Identification
The module is identified by a 5 digit product number (G1306A or 79854A) and a 10 unit serial number on a label attached to the wall inside the module. The first four digits of the serial number are the serial prefix. The letter identifies the country of origin. The last five digits are an identification number unique to each module. Any changes to the modules will be covered initially by Service Notes. They will be sent out to all Service personnel prior to implementation of the change to the instrument. With every reprint these changes will be incorporated into the service documentation.
Compatibility
The replacement parts of the 1050 MWD are usable in the 1050 DAD and vice versa. The 1050 MWD can be upgraded to a 1050 DAD.
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DAD Differences
The G1306A Diode Array Detector (DAD) is basically the 1050 Multiple Wavelength Detector (MWD). The DAD has the same hardware as the 1050 MWD with two exceptions: keyboard and firmware are different. The 1050 DAD is NO replacement for the 1050 MWD. The 1050 DAD adds spectra capabilities to the existing 1050 MWD, necessary for workstation controlled 3D detection systems. The 1050 DAD needs control by the HPLC DOS ChemStation (PHOENIX 3D-PLUS) to become operable. Upgrade from 1050 MWD to 1050 DAD will need new firmware and a new user interface (keyboard).
Added features
The following features are new (compared to the 1050 MWD): up to five independent signals (sample and reference wavelength each) up to 5 spectra/second (time programmed, periodically or peak controlled) temporary storage of up to 90 spectra in internal run buffer up to 1 spectrum/second for monitor output lamp-on time information
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The signal multiplication factor has been removed from signal parameter set points. no max monitor screen.
Compatibility
The replacement parts of the 1050 MWD are usable in the 1050 DAD and vice versa. The 1050 MWD can be upgraded to a 1050 DAD. An upgrade kit will contain the necessary hardware and instructions (see section Parts Identification). The 1050 DAD cannot be operated properly in an integrator based system. The LC APPACK software will not recognize the 1050 DAD as a module to control.
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The following functions remain the same as for the 79854A MWD (same keys): LAMP ON/OFF Pressing NEXT LAMP ON FOR n hours and RESET LAMPHOURS (enter)are displayed. BALANCE START and STOP Status line including signal A monitor, not ready conditions, logbook, installed options and firmware revisions. The following functions are hidden behind the STATUS key for maintenance purpose): DATE&TIME REVISION CONFIGURATION remote configuration. set GPIB address. autobalance on/off. lamp current setting. set wavelength calibration factor. set analog output voltage. TEST FUNCTIONS measure intensity. Holmium spectrum. lamp intensity. gain (ASC). D/A converter. electronics noise. shutter position. wavelength calibration check.
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Workstation Interface
The 1050 DAD must be operated with the LC ChemStation. Rawdata File The run buffer within the detector is shared by signal and spectra data. In case the run buffer is going to overflow, the signal data will have the higher priority: the last stored spectrum is removed from the run buffer. This will guarantee useful signal data but may cause loss of interesting spectral data. The run buffer can hold up to 30000 signal data points or about 90 spectra. Peak Detector The peak detector (PD) always uses signal A as the pilot signal. The PD is adjusted by means of the two set points peak width and threshold. Both setpoint are time programmable. Whereas the PD-threshold is a method parameter of its own, the PD-peak width parameter is derived from the general peak width (PKWD) parameter. At start of the run the value for the PD-peak width is set equal to the PKWD setpoint. During the run the PD-peak width parameter can be changed by time programming. Spectra Acquisition Modes The spectra acquisition mode allows automatic storage of spectra during a run. The mode can be changed during the run by time programming. Compared to the 1040 DAD the 1050 DAD will have two new features storing spectra at the baseline before the begin of a peak periodically store spectra during a peak and at a reduced data rate. The modes in detail are:
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Table 103
Spectra Acquisition Modes Mode none apex apex + baselines Details no spectra is stored top of peak spectra is stored last baseline spectrum before peak, top of peak spectrum and first baseline spectrum after peak is stored. spectrum in peak upslope, at top of peak and in peak downslope is stored. combined apex + slopes and apex + baselines. compared to storing all spectra periodically, only stores spectra within a peak at doubled period. Starts with last baseline spectrum before peak and ends with first baseline spectrum after peak. If baseline spectra are not detected, the spectrum before the first spectrum in peak or the spectrum after the last spectrum within the peak is stored instead. periodically all spectra are stored. The period depends on the peak width setting. For peak width setting=0 (narrowest peak), the spectrum data rate would be 20 Hz
all
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Test Functions
The 1050 DAD has a reduced user interface and no analog output (DAC board is optional). It has no means to display (plot) the spectra (or intensity scans) of some of the built-in tests. These plots can be retrieved with the Workstation.
Options
Because the 1050 DAD is only operable together with the workstation, the Communication Interface Board (CRB) is mandatory. Because the 1050 DAD typically needs no analog output signals, the Digital to Analog Conversion Board (DAC) is optional. For complete description of test conditions used to obtain specifications, see Owners manual.
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Specifications DAD/MWD
Table 104
Specification of the 1050 DAD/MWD (Series II Optical) Detection Type Signals Double beam photometer Up to 3 (MWD) or 5 (DAD), each defined by a sample wavelength and bandwidth and an optional reference wavelength and bandwidth. Sum of two signals; difference of two signals; ratio of two signals, with definable range and threshold; window plot with definable ratio, range and threshold. < 2.0 x 10-5 AU peak-to-peak, at 254 nm with 4 nm bandwidth, flowing water at 1 ml/min, 1 second response time (10-90%). < 2 x 10-3 AU/hour, at 254 nm, after warm-up. 190-600 nm, selectable in 1 nm increments. 2-400 nm, selectable in 1 nm increments. 1 nm. Better than 1% up to 1.5 AU, using acetone at 265 nm. 8 choices, ranging from 0.1 to 20 seconds (10-90%). Storage of at least 8 spectra, with definable wavelength range from 190-600 nm (total number of spectra depends on range defined). Post-run plotting of original or subtracted spectra possible. depends on slit width. < 5 x 10-6 AU 12.5 ms from 190 to 600 nm; according to the response time settings scans are accumulated for one data point for improved sensitivity.
Signal Combinations
Noise
Drift Wavelength Range Bandwidth Range Wavelength Accuracy Linear Absorbance Range Response Time Spectra
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Table 104
Specification of the 1050 DAD/MWD (Series II Optical) Light Source Flow Cell (Series II) Deuterium lamp. SST cell, 8 l volume with 6 mm path length or 13 l volume with 10 mm path length and 120 bar (1760 psi) maximum pressure. Optional high-pressure cells (400 bar). 2 line by 16 character fluorescent display with real-time display of operating parameters or absorbance and wavelength of maximum absorbance. Integrated keyboard with function keys; parameter editing during run possible; keyboard lock. External control via GPIB with ChemStation or RS-232. Integrated keyboard with function keys; limited functionality and control on DAD. Signal definitions (wavelengths/bandwidths), attenuation, response time, zero offset, balance; spectra definitions; external contacts; analog outputs. Wavelengths/bandwidths, attenuation, spectra acquisition, external contacts. Battery-backed storage of up to ten methods (depends on length of method), including initial and time-programmed parameters. Automatic startup and shutdown methods. Editing of stored methods possible during run. Two analog outputs are available (on DAD optional) for output of signals and/or signal combinations; both 1 V/2 AU or 100 mV/2 AU, user-selectable. START (in- and output), STOP (in- and output), READY (output), SHUTDOWN (output) for synchronization with other LC modules; two external contacts including: 1 relay with 24 V and 250 mA; 1 contact closure with maximum 30 V and 250 mA.
Display
Control
Parameters
Analog Outputs
Communications
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Table 104
Specification of the 1050 DAD/MWD (Series II Optical) Safety Aids Extensive diagnostics, error detection and display via front-panel LEDs and status logbook. User-definable shutdown method activated in case of error. Leak detection, safe leak handling, leak output signal to shutdown the pump. Temperature range: 5 to 55 C Humidity: < 85% (non-condensing) Line voltage: 100-120 or 220-240 VAC 10% Line frequency: 48-66 Hz Power consumption: 150 VA max. Height: 208 mm (8.2 inch) Width: 325 mm (12.8 inch) Depth: 560 mm (22.0 inch) Weight: 16 kg (35 lb.)
Dimensions
For complete description of test conditions used to obtain specifications, see Owners manual.
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19
This chapter gives general and technical information about the hardware components of the 1050 Diode Array and Multiple Wavelength Detectors. overview about the optical system overview about the electronics detector hardware optical units flow cells heat exchanger lamp shutter assembly leak sensor fans N OT E This chapter describes the Series II optical unit hardware only.
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1 - deuterium lamp 2 - windows 3 - shutter 4 - achromat 5 - flow cell 6 - slit assembly 7 - lens 8 - grating 9 - array
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Overview: Electronics
Figure 147 shows a block diagram of the 1050 DAD/MWD. The Common Main Processor (CMP) controls all functions of the module. The CMP communicates with the AQB, controls directly the shutter of the optical unit and the power supply. If a leak is detected inside the optical unit, this leak message is connected to the CMP. The CMP also provides the I/O Remote connections. To the CMP the common main processor BUS is connected which allows the communication with the user interface (keyboard), Digital to Analog Converter (DAC) and GPIB/RS232 interface. The Digital to Analog Converter interface is optional. Because of the structure of the 1050 Series the module specific controller firmware is piggy-back loaded to the Data Acquisition Board (AQB). The AQB controls the Analog to Digital Conversion Board (ASC) and the Photo Diode Array (PDA).
436
Figure 147
437
Optical Unit
The main areas of the optical unit are: Optical housing flow cell same for use in 1050 MWD and 1040/90 DAD (different flow cell, cover and slit). available as stainless steel (SST) with different path lengths (6/10 mm, 8/13 l) for high pressure use (120 bar). Additional high-pressure cells (400 bar) are also available. available with optical slit width of 2, 4 and 8 nm slit. interface between leak sensor/shutter assembly and main electronics.
Due to this separation of flow cell and slit and the availability of flow cells with different path lengths and slit assemblies with different optical slit width, it is now possible to optimize the signal-to-noise and the spectral resolution. The optical unit is optimized for the flow cell with 6 mm path length together with the 4 nm slit assembly. Figure 148 Optical Unit
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Table 105
Flow Cell Data STD Volume Path length Maximum pressure in the cell Inlet capillary id Outlet capillary id recommended pH range STD HP-STD HP-Micro Standard Flow Cell High Pressure Cell with 13 l volume High Pressure Cell with 1.7 l volume 8 or 13 6 or 10 120 0.17 0.17 HP-STD 13 10 400 0.17 0.17 >2.3 to 9.5 HP-Micro 1.7 6 400 0.12 0.12 l mm bar mm mm
C A UT I O N
Because the very small inner diameter (0.17 or 0.12 mm) of the inlet capillary only very clean solvents should be used.
439
Additional Information of High Pressure Cells Typical applications of the high-pressure flow cells are: Hyphenated systems (LC-MS) Super Critical Fluid Chromatography (SFC) Multi-detector systems Narrow-bore column applications The main difference between the standard and high-pressure flow cells is the design of the window assemblies. The high-pressure flow cells have a different window screw, window and seal ring, washer, and a different number and orientation of conical disk (bevelled) springs, see Figure 150. The seal rings support and hold the window and at the same time form the high-pressure seal. Figure 150 Cross-section of Window Assembly
Windows
Washer
The following materials are in contact with solvents: Stainless steel (AISI 316) Quartz Vespel (polyamide) Vespel is a registered trademark of DuPont.
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Under standard conditions (1 ml/min water flow, 254 nm detection wavelength, 4 nm bandwidth, 1 s response time) the noise of the high-pressure micro flow cell might increase. The high-pressure micro flow cell is supplied with an additional 0.12 mm i.d. capillary, allowing you to bypass the heat exchanger.
Slit Assembly
The separation of the slit from the flow cell allows to change the slits according the needs to optimize signal-to-noise and spectral resolution. Available slit sizes are 2, 4 and 8 nm. Figure 151 Slit Assembly
441
Two versions were used: 79880-60002 was the original lamp 79883-60002 with 20% higher initial energy
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Figure 153
Measured wavelength is 230 nm initial intensity about 20% higher than 79880-60002 should be used with 2 nm slit initially top prevent overload of photo diodes (if intensity is to high). decrease in intensity is less with use N OT E The lamp should be replaced only if the following two criteria are both fulfilled: Baseline Noise (with test cell) has increased significantly. Amount of counts of the lamp (with test cell) has decreased to less than 50% of the count record of this same lamp when newly installed). The decision to replace the lamp due to criteria 2 alone is not relevant, because the signal/noise may be still within instrument specifications.
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Shutter Assembly
The Shutter Assembly is located in the cell compartment of the optical unit. The stepper motor is responsible for moving the shutter into one of three possible positions: 3 Shutter not in light path (normal operation) 4 Shutter in filter mode (a holmium filter is moved into the light), refer to TEST FUNCTIONS, see Shutter Position on page 506. 5 Shutter in dark position (no light is coming through the cell; this is necessary for dark current measurements carried out for calibration purposes). Figure 155 Shutter Assembly
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Fans
Two DC-fans are located between the optical unit and the motherboard, inserted in a set of foam. The left one provides air for the lamp housing and power supply and the right one provides air for the electronics in the rear. For replacement refer to section Procedures. In May 1994, a protection cover for the left fan (close to the lamp connector) was introduced for safety reasons (not shown in Figure 157). Figure 157 Fans
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This chapter gives information about the electronic of the 1050 Diode Array
450
Overview
All electronic boards (except the FIP, behind the keyboard and the LPC, in the optical unit) are located in the rear part of the module and they are connected to the Motherboard (LUM). The rear of the detector is shown in Figure 158 on page 452. In the 1050 DAD the following electronic assemblies are available:
Table 106
Electronic Boards Description Power Supply (DPS-A) Common Main Processor (CMP) Array Signal Conversion (ASC) Digital/Analog Conversion (DAC) (optional) Data Acquisition (AQB) Firmware Board (FIM) for DAD Firmware Board (FIM) for MWD Leak/Shutter Interface (LPC) Motherboard (LUM) Display Interface Board (FIP) Communication Interface (CRB) Part Number 5061-3375 5061-3380 01048-66501 01048-66502 01048-66543 G1306-66524 01048-66504 79883-66509 01048-66510 5061-3376 5062-2482 Exchange 01050-69375 01050-69380
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Figure 158
N OT E
452
The system consists of the Photo Diode Array (PDA) with 211 elements, the Array Front End Board (AFE), the Analog Signal Conversion Board (ASC) and the Acquisition Processor Board (AQB). The PDA detects a spectrum of incident light in the wavelength from 190...600 nm with 2 nm increments. The AFE Board consists of a Readout Amplifier, which transfers the accumulated charge from the diodes and generates the PDA signal. The ASC Board consists of a variable gain amplifier, a 16-bit A/D converter, a microprocessor interface and a control logic to control the PDA, the amplifier and the microprocessor interface. Figure 159 Block Diagram of Electronics
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Table 107
Part Numbers for ASC Board Item ASC board Part Number 01048-66501
The two main functions of the ASC board are: providing of control signals for the readout routine of the photo diode array; analog to digital conversion of the array signal. Photo Diode Array Readout Routine The readout cycle (12.5 ms) is divided into 225 time slots each 55.55 s.
Time Slot 0 1 2 3...211 212 213 214 215 216 217 218...224 Function not used dummy diode, not used Bit 1 of shift register, not used information of intensity Bit 213 of shift register, not used dummy diode, not used not used Offset value, Gain = 1 Offset value, Gain = 2 Offset value, Gain = 4 not used
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Figure 160
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The analog ARRAY SIGNAL coming from the AFE board is in the range of -5 V to - 10 V depending on the intensity of the light falling on to the photo diodes. Analog/Digital Conversion The principle of conversion is based on the Triple-Slope technique see Figure 161. During the TRACK phase the integration capacitor is loaded by a constant voltage Uc. This voltage is proportional to the ARRAY SIGNAL voltage. The voltage Uc is in the range of 0...10 V and is present for 12.37 s. Figure 161 Triple Slope Integration
During the HOLD phase (the ARRAY Signal voltage is disconnected). Uc is discharged by two constant bipolar currents I1 and I2 and the discharge time is measured. U c is discharged with I1 until the zero passage is reached. The time used for this down slope is counted with the clock (18.432 MHz) and will represent the upper 9 bits of the 16 bit data word. After the zero passage I1 is switched off with the next active clock and the negative residual charge is discharged with I 2 until the zero passage is reached the second time. The time between both zero passages represent the lower 7 bits of the 16 bit data word. In reality only I 1 is switched and I2 is on permanent to avoid failures due to multiple switching.
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The cycle for the conversion takes 55.55 s (18 kHz) and is divided into 1024 steps of 54.2 ns (18.432 MHz) which is the internal clock on the board. During steps 0...227 the amplified input voltage (ARRAY SIGNAL) is switched through and the integration capacitor is charged. The gain level can be 1, 2 or 4 depending on the instrument characteristic of the light source. These amplification factors are measured for each diode at the begin of a chromatographic run when a BALANCE is made. The values are put as a table into memory on the AQB Board. Starting with step 228 the input voltage is disconnected from the capacitor and a RESET pulse resets all flip-flops and counters. Current I1 is switched on. The conversion starts. Up to this point the described timing sequence is independent of the input voltage. The following processes are controlled by the zero passages. The 9-bit counter counts the clock pulses until the comparator sees a zero passage of the integrator voltage. Then I1 and the 9-bit counter are switched off. I 2 and a 8-bit counter are now active discharging the negative integrator voltage until the next zero passage. The 8-bit counter stops. During steps 1012...1016 the 16 bit data word is build. The 16 bit word is moved into the output registers from where the AQB Board takes the information. Because of the long availability of the data word (55.55 s) the AQB processor has enough time to get the data. Input Amplifier and Integrator The ARRAY SIGNAL coming from the AFE Board is in the range of +0.1 V (dark) and -5.1 V (bright). A input amplifier transfers this voltage into the range of -0.7 V to -11.1 V which is the input of an amplification switch. This switch changes the amplification factor of the integrator stage (gain factor 1, 2 or 4). The adjustment of the separate photo diodes is done by the AQB Board. Ramp Amplifier and Comparator The ramp amplifier is used to increase the slope speed of the integrator voltage. The comparator looks for the zero passage and provides the signals COMP and COMP- for the time and control logic.
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DC-Voltages The internal reference voltages +10 V and -10 V are derived from the +15 V. Input voltages: +19 V, -19 V, AGND +5 V, DGND Output Voltages: +15 V, -15 V, AGND +5 V, DGND Digital Sections This section provides all timing and control signals used on the ASC Board. The timing is done with a Programmable Array Logic (PAL) that gets 8 synchronous input signals in the range of 2.304 MHz and 18 KHz all derived out of the 18.432 MHz main clock. A SYNC signal is used for synchronization of the switching power supply. The comparator signals COMP and COMP- (generated in the analog part) control the 9-bit and 8-bit counter. The 16-bit data word is transferred to the Data Acquisition Board (AQB) via the 16-bit Data Register. Status information is transferred to the Data Acquisition Board (AQB) via the Status Register.
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Table 108
Part Numbers for AQB Board Item AQB Board Firmware Board DAD/CE Firmware Board MWD Fuse F11, F12 (250 mA) Part Number also used for
The Data Acquisition Board (AQB) is the personality module. It contains the firmware for the main processor system. Firmware including address decoder will be located piggy back on the FIM board. But the main purpose of this board is to hold special hardware only necessary for the DAD/MWD. This is frontend control hardware and a data reduction processor system including dual port RAM for data transfer to main processor. Main Functions max. four EPROM main firmware on FIM board FIM board piggy back on AQB board lamp control hardware stepper motor driver hardware for shutter 2 external contacts 2 connectors on rear panel 1 contact without supply (only contact closure) max. 30 V (fused with 250 mA) 1 contact with internal 24 V supply (fused with 250 mA)
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Figure 162
460
Frontend Processor Area 6809 running at 2 MHz A/D converter interface frontend firmware 512 byte 8 Kilobyte dual port RAM including interrupt register Main Processor Area max. four EPROM main firmware on FIM board FIM board piggy back on AQB board lamp control hardware lamp on/off (anode voltage) heater on/off lamp start (600 V ignition) 2 lines for lamp current select status stepper motor driver hardware for light shutter motor on/off 4 bit step pattern lines bus buffer for backplane bus connection 2 external contacts Input / Output 2 external contacts 2 connectors on rear panel 1 contact without supply (only contact closure) max. 30 V/250 mA 1 contact with internal 24 V supply (max. 250 mA output with fuse) via motherboard stepper motor lines to optical unit lamp control to power supply connection to ASC board backplane bus Service Handbook for 1050 Series of HPLC Modules - 11/2001 461
Figure 163
462
Table 109
Part Numbers for FIM Board Item Firmware Board DAD/CE Firmware Board MWD Part Number also used for
The FIM board is a piggy back board, placed on AQB board (personality module). The programmed FIM contains the firmware of the 1050 DAD module. The board is designed for on board programming. The FIM contains up to four 128K x 8bit EPROM (U4 to U7). All inputs/outputs are pulled down for electrostatic discharge protection. Figure 164 Layout of FIM Board
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Table 110
Part Numbers for CMP Board Item CMP Board Part Number 5061-3380/01050-69580 also used for G1600A CE
Common 1050 functions for the main processor are: display handling keyboard polling remote control input and output leak sensing option interfacing time programming method storage module configuration memory switching 32 kilobyte RAM with battery back-up for parameter storage. Firmware is not part of this board, because parts of the main processors software are module specific. The main processor firmware will be located on the personality module (AQB Board) or on an optional board.
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Figure 165
465
Remote Control
The CMP board provides two remote connectors. Remote Signals
Table 111
Pin 1 2 3 4 5 6 7 8 9 Signal Digital ground Prepare run Start Shut down Reserved Power ON Ready Stop Start request HIGH HIGH LOW LOW LOW LOW LOW Active Color white brown gray blue pink yellow red green black
Remote Configuration The 1050 Series provides three remote configurations: HPsystem GLOBAL LOCAL Start of automatic operation from any modules start key. Start request is outputted. Synchronized start of several modules for a single run. Start / Stop is outputted. Single modules start. No pulses outputted.
The signal level are defined as standard TTL levels (0 V is logic true, + 5 V is logic false). The remote lines can be input or output (wired or technique). Fan-out is 10 Input Load 2 kOhm against + 5 V Outputs are open collector type 466 Service Handbook for 1050 Series of HPLC Modules - 11/2001
Table 112
Part Numbers for CRB Board Item CRB Board Part Number 5062-2482 also used for G1600A CE
The communication interface board is necessary for the control by a Personal Computer and to connect printer or plotter devices. The communication interface board provides one GPIB and one RS232 interface. The CRB for the 1050 DAD has a 96 kilobyte run buffer for the data/spectrum operation with the Multiple Wavelength Detector. The interface is located in Slot #2 of the module. The board contains a baud rate generator. The baud rate is selectable up to 19200 baud from the keyboard. The transmitter and receiver baud rate are independent adjustable. The implemented serial interface is a subset of the RS232 standard only. It contains at PIN 2 PIN 3 PIN 4 RxD receive data (data input) TxD transmit data (data output) GND (Ground)
The 1050 modules are designed as DCE (data communication equipment) without hardware handshake.
467
Table 113
Part Numbers for DAC Board Item DAC Board Part Number 01048-66502 also used for G1600A CE
The main functions of the DAC board are: conversion of digital data into analog signals compatible with external integrators; provide two independent analog outputs. The DAC board comprises two independent pulse-width modulated 16 bit D/A converters with noise <1/4 LSB (peak to peak). The repetition rate for the data per channel is 90 Hz. The two analog outputs can be used for integrators and recorders. The rise time and the offset voltage is selectable per software. Output voltage: Scale factor: Rise Time (10/90%): Noise (0.1 s rise time): -4 ... 996 mV (1 V) or -0.4 mV ... 99.6 mV (100 mV) 0.5 V/AU or 0.05 V/AU (for multiplication factor =1) 0.1/0.3/1/3 s < 4 V (< 0.008 mAU)
468
Figure 166
469
Address Decoder and Data Storage The digital signal prepared for conversion is sent from AQB through LUM data bus in 8 bit portions. The appropriate address is available on LUM address bus. This address is decoded by the address decoder and the data storage circuit is activated and the digital word is stored. The two channels are separated only through the appropriate address recognized by the address decoder. Timers Three 16 bit timers are available on the DAC. One is fixed as a divider (6.555 MHz/90 Hz) and provides the 90 Hz clock for the control logic. The other two timers work as Pulse width Modulator for channel 1 and 2. They are loaded with the digital word stored in the data storage and activated with a 90 Hz clock. Starting with the loaded word each counter will count downwards with the 6.555 MHz cycle. Pulse Width Modulator The pulses generated in the counter section are fed to diode switches that are responsible to switch the constant current source on or off to the low pass filter section. Low Pass Filter All low pass filters should suppress the 90 Hz cycle. The cutoff frequency is <4 Hz and suppresses the 90 Hz with >100 dB. The second low pass filter is a variable low pass filter dependent on the rise time (0.1/0.3/1/3 s). The third low pass filter has a variable gain which allows a scale factor for the analog output voltage at 50 mV/AU or 0.5 V/AU. Rise time The rise time is software selectable to 0.1 s, 0.3 s, 1 s, or 3 s. This rise time is varied in combination with the peak width setting. The default setting is 1 s. Refer to Operating Manual for more details. Power Supply The 19 V from the Power Supply is used to generate 15 V and + 10 V as a reference voltage for the constant current source.
470
Board Diagnostics There are two possibilities to troubleshoot the DAC board: output voltage check, see User Manual D/A converter test, see D/A Converter Test on page 500 Both of these tests can be done on both output channels. Figure 167 Layout of DAC Board
471
Table 114
Part Numbers for FIP Board Item FIP Board Fuse 1 A Part Number 5061-3376 2110-0099
The FIP module is located behind the keyboard module of pump, autos ampler and multiple wavelength detector. The function of the FIP module is to provide an interface between a host system and the user. Messages can be displayed with up to 32 characters (2 lines x 16 characters/line). A matrix keyboard is scanned for numeric or special function input and status information is displayed through 4 LEDs. The characters are displayed in a 5 x 7 dot matrix. In case of a dark display, check the on board fuse ICP1 which is soldered in close to the connector P1/P2. Figure 168 Board Layout FIP
472
Motherboard (LUM)
Repair Level: Board
Table 115
Part Numbers for LUM Board Item LUM Board Part Number 01048-66510
The Motherboard contains all connectors for the boards and the assemblies in the front part, like fans, optical unit and keyboard. Figure 169 shows the location of all connectors. Figure 169 Layout of Motherboard
J10 - Shutter/Leak J11 - Lamp J12 - not used J13 - Fan (left) J14 - Fan (right)
473
Figure 170
474
Figure 171
475
Figure 172
476
LPC Board
Repair Level: Board
Table 116
Part Numbers for LUC/LPC Board Item LPC Board Part Number 79883-66509 also used for G1600A CE
The board routes the signals from the leak sensor and signals to the shutter assembly. Via J3 it is connected to J10 of the LUM board (Motherboard). Figure 173 LPC Board Assembly
477
Table 117
Part Numbers for LUC/LPC Board Item DPS-A Fuse for 110 V operation 3 A Fuse for 220 V operation 2 A Part Number 5061-3375/01050-69375 2110-0003 2110-0002 also used for G1600A CE
For detailed information refer to the 1050 Service Handbook, Chapter Common Information. General Description The power supply is a primary switching regulated type. It consists of two parts. the Base Supply and the Lamp Supply. The Base Supply provides outputs of +5 V, 19 V, +24 V and +36 V. In addition the Lamp Supply provides all circuits necessary for the operation of a deuterium lamp. Lamp Ignition The heater output made by a series regulator is in the pre-heating status 2.5 V always. After ignition the heater voltage is switched off (DAD/MWD). Figure 174 Deuterium Lamp Ignition
478
Figure 175
479
Figure 176
480
Figure 177
481
482
21
21
The 1050 DAD/MWD provides STATUS information during the normal operation (e.g. conditions errors); ERROR MESSAGES that identify the problem; DIAGNOSTIC features on special request to allow troubleshooting of the module.
484
STATUS Information
Status Modes
Status Modes Status LEDs Warnings SYSTEM INIT initializing ..... After turning on the module runs through an initialization. STANDBY 1050 STANDBY 01:A 0.00mAU All LEDs and the deuterium lamp are off. Edit of all parameters is possible (if PARAMETER LOCK is off). LAMP IGNITION LAMP ON <lamp is off> ENTER LAMP IGNITION 01:A 0.00mAU During the ignition process the NOT READY LED is on. PRERUN PRERUN 01:A 0.00mAU The same as in STANDBY mode except that the deuterium lamp is on now. Transition to RUN only possibly by pressing START (LOCAL) or via REMOTE. RUN timeprogram starting is displayed for 2 seconds. Then actual display shows RUN 01:A 0.00mAU. The RUN LED is on and the timetable commands are executed. The deuterium lamp cannot be switched to off. timeprogram stopped POSTRUN POSTRUN 01:A 0.00mAU The RUN LED is blinking. If post time has elapsed or STOP occurs the instrument switches to BALANCE mode (calibration) if auto calibration parameter is ON else to PRERUN mode.
485
BALANCE
SYSTEM TEST
This mode is normally skipped and has to be called up through the TEST functions or during power on by pressing STATUS and LINE~ switch. Then ROM- RAM- and DISPLAY Test is performed. For details see ROM/RAM/DISPLAY Tests on page 507.
Status LEDs
ERROR LED ON This state indicates an error condition and requires an interaction of the user. A message will be written into the system logbook. The display will be overwritten with a messages: This state indicates a NOT READY condition (action not yet finished see also mode description). A logbook entry is made. The following reasons may be reported on display for 2 seconds: lamp ignition in progress amp test in progress balancing LAMP LED ON RUN LED ON Deuterium lamp on. Instrument in RUN mode. If instrument is in POSTRUN mode the RUN LED is blinking.
Warnings
A warning is written into the logbook if a problem occurs which doesnt cause the user to stop analysis. A message is written to the display for 2 seconds. Possible warnings can be: lamp below intensity test limit; excessive leakage current of one of the photo diodes (non-linear); intensity too high (wrong calibration at gradient run); temporary memory overflow.
486
Error Messages
This section describes the troubleshooting of the 1050 DAD/MWD according to the error messages. The error messages will help to locate and repair a failure. In case an error message appears the Error LED will be turned on and the message will be written into the system logbook.
Selftest
ROM RAM and display can be tested via the build in selftest. The selftest will be performed when STATUS will be pressed while the module is turned on at the LINE~ switch. In case of a failure one of the following messages appears. The complete test requires approximately two minutes. ROM test failed ( ROM test failed ) The ROMs on the FIM board are tested. In case of a checksum error the ROM test fails. Replacement of the FIM board will probably fix the problem. RAM test failed ( RAM test failed ) The RAMs on the CMP board will be tested. In case of a failure the error message appears and the CMP has to be replaced.
487
488
E02 HH:MM DDMMM shut down > serious error in other module An external device pulled the shut down line down (pins 1 and 4 of REMOTE connector), for example when a leak is detected.
E03 HH:MM DDMMM error method > error method has been loaded An error has come up in the DAD and this caused to load an error method (if specified) and turned off the lamp.
E04 HH:MM DDMMM time out > lamp turned off automatically If the time after finishing the last run or a not ready condition exceed the value of set time-out time the deuterium lamp is turned off automatically. A time out occurs (pin 1 and 7 of REMOTE connector).
E05 HH:MM DDMMM lamp has been > turned on automatically If the lamp was programmed to be turned on automatically this message is displayed.
489
490
E15 HH:MM DDMMM ignition failed> lamp failed during ignition Actions: Turn lamp on. Check lamp connector. Perform lamp test. Change lamp. Replace AQB. Replace power supply.
E16 HH:MM DDMMM intensity test> low intensity make lamptest Actions: Perform lamp test. Change lamp. Change flow cell.
E17 HH:MM DDMMM data overflow > intensity too high Actions: Check whether cell is inserted correctly. Reduce lamp current. Change lamp.
E18 HH:MM DDMMM data underflow> ASC data too low Actions: Check whether cell is inserted correctly. Increase lamp current. Change lamp. Change ASC, cable, AFE.
491
E19 HH:MM DDMMM lamp turned on> lamp turned on automatically The lamp has been switched on per time program.
492
Diagnostic Features
The instrument offers several built-in test features. Some are limited to ChemStation operation (for details see descriptions of tests): intensity test holmium oxide test lamp intensity test ASC test D/A-Converter test electronic noise test close/open shutter check wavelength calibration RAM test ROM test Display test N OT E When using these test functions the 1050 DAD/MWD must not be in RUN MODE. Press BALANCE prior to perform the test. When test cell is mentioned, remove cell and insert 4 nm slit for Series II optical
493
494
Find Maximum of Spectrum (MWD only) Press SPECTR, DOWN and RIGHT. MAX. 01 REF -- ;ints 0.00min You can change now the wavelength range (190...600 nm) and the output channel if necessary. The maximum is shown after pressing ENTER. max 17805cts at 234nm ; 0.00min Figure 178 Intensity Profile with Test Cell
495
Figure 179
496
On local keyboard If performed locally the display shows: LAMP INTENSITY TEST ; 0 ENTER LAMP INTENSITY TEST ; 14296 On ChemStation If performed on the ChemStation this test is part of the DAD Test, see Figure 179 on page 496. The profile (190 to 600 nm) is stored on the ChemStation. Select Instrument, More DAD, DAD Tests... Press Measure and the instrument will perform the Lamp Intensity Test and the Holmium Test automatically. Press Save to store both profiles. To print the profile refer to How to print the DAD Profiles, page 5-29.
497
Figure 180
N OT E
At least one point should be >3000 mAU in the range of 190...300 nm.
498
On ChemStation On the ChemStation this test is part of the DAD Test, see Figure 180. The profile (190 to 600 nm) is stored on the ChemStation. Select Instrument, More DAD, DAD Tests... Press Measure and the instrument will perform the Lamp Intensity Test and the Holmium Test automatically. Press Save to store both profiles. To print the profile refer to How to print the DAD Profiles, page 5-29. On local keyboard MAX. 01 REF -- ;holm 0.00min ENTER max 3912mAU at 228nm ; 0.00min
499
If the D/A converter and the plotting device are in specification then the noise is depending on the peak width (5 V are equal to 1 x 10-5 AU).
500
When the function is switched on start the plotter (ATTN -5, ZERO=50) and zero it.
Table 118
501
With this test non-logarithmic intensity is measured. Result of test must not exceed a given limit. If test fails the ASC DAC or optical unit may be defective. If DAC test is OK then ASC or optical unit may be the problem.
502
Table 119
Limits of Electronic Noise Test Limit 3390/2/3 13.5 mm 13.5 mm 15.0 mm 18.0 mm 18.0 mm 12.0 mm 12.0 mm 12.0 mm
Peak width < 0.01 > 0.01 > 0.03 > 0.05 > 0.10 > 0.20 > 0.40 > 0.85
Rise time 0.1 s 0.2 s 0.3 s 1.0 s 1.3 s 2.6 s 5.2 s 10.0 s
Vpp 90 90 50 30 30 20 20 20
Measurement conditions Any sample wavelength, bandwidth 4 nm, reference is switched off automatically, 1 V full scale. NOISE 1: NOISE 2: Test as described. Test as described under NOISE 1 but with PDA/LUM cable disconnected
Table 120
Noise Test Results Result System OK Electrical Problem Optical Problem Explanation If NOISE 1 > NOISE 2 and in specification. If NOISE 1 > limit and NOISE 2 >= limit. If NOISE 1 > limit and NOISE 2 < NOISE 1
503
504
ASC Test
N OT E This function is available from local keyboard only! ASC TEST WITH GAIN 0 ; 0 ASC TEST WITH GAIN 0 ; 3871 ASC TEST WITH GAIN 1 ; 4462 ASC TEST WITH GAIN 2 ; 4654 The ASC board is tested by closing the shutter and measuring the dark current of the photo diodes with three possible gains (0, 1, 2). Start test with minimum gain first. High values may reflect in a non-linearity. (Default is minimum gain = 0). The value that is shown is the average dark current counts of a all photo diodes. A value between 2500...5500 is the limit measured with gain 0. The value in gain 1 and 2 may have a difference of 1500 compared to the value from gain 0. N OT E High values may reflect in a non-linearity. The scan (190 to 600 nm) is stored. You can change now the wavelength range (190...600 nm) and the output channel if necessary. Now you can retrieve the plots or the maximum information. MAX. 01 REF -- ;tasc 0.00min ENTER max 3885cts at 475nm ; 0.00min N OT E If the difference between average and maximum is >100 then the array has a problem at this particular wavelength. This might be no problem if the customer is using a different wavelength.
505
Shutter Position
N OT E This function is available from local keyboard only! SHUTTERPOSITION OPEN SHUTTERPOSITION HOLMIUM/CLOSED The shutter can be positioned manually to OPEN, HOLMIUM and CLOSED (dark current). Leave this function by switching to OPEN.
506
ROM/RAM/DISPLAY Tests
The following functions are also performed during power on when both STATUS and the LINE~ switch are pressed. ROM TEST (enter) The ROM checksum is compared with a stored value and the firmware revision is displayed. ROM TEST <executing> ( ROM test failed ) Action: Replace the FIM board. RAM TEST (enter) The RAM is tested. RAM TEST <executing> ( RAM test failed ) Action: Replace CMP board. DISPLAY TEST (enter) The 32 characters of the display and the LEDs are tested. This test is the same as performed during power on. DISPLAY TEST <executing> Action: If the display shows nothing, check first the soldered in on-board fuse, see Fluorescent Indicator Module (FIP) on page 472.
507
DAD/MWD: Diagnostic & Troubleshooting Information Using the Built-in Test Chromatogram
508
DAD/MWD: Diagnostic & Troubleshooting Information Using the Built-in Test Chromatogram
Figure 184
Figure 185
509
DAD/MWD: Diagnostic & Troubleshooting Information Using the Built-in Test Chromatogram
Using Paintbrush Press ALT and Print Screen keys to make screen capture. Leave the DAD Test and enter Paintbrush from the Program Manager. Select View and click Zoom Out. Select Edit and Paste (2x). Select View and click Zoom In. Select File, Print and [[OK]].
510
DAD/MWD: Diagnostic & Troubleshooting Information Using the Built-in Test Chromatogram
Using the Data Editor Select View, Data Analyses. Select View, Review DAD Test... Select from the table the spectrum of interest see Figure 187 or Figure 188. Press [[Show Selected Spectrum]] and select the window. At this point you may zoom a certain part of the profile. Select File, Print, Selected Window for print. Figure 187 DAD Test: Lamp Intensity
511
DAD/MWD: Diagnostic & Troubleshooting Information Using the Built-in Test Chromatogram
Figure 188
512
22
22
This chapter describes the following procedures that have to be performed during servicing and maintenance of the 1050 DAD. removing the optical unit; flow cell maintenance; cleaning the quartz window; replacing fans; replacing shutter assembly or LUC/LPC board; replacing the leak sensor; upgrade to new optical unit; performance verification.
Tools Needed
Screw driver flat 6 mm Hex wrench 6 mm Hex wrench 4 mm and length of 200 mm Pozidriv small cleaning tissue
514
N OT E
DO NOT open the screws of the large cover of the optical unit. This may result in misalignments of the optical path. exchange lamp housing. They are matched to the optical and replacement may result in a misalignment of the optical path. return defective exchange optical without information about the problem (use attached info-note). return flooded optical without information about the last used solvents (this is needed for recycling).
N OT E
The lamp housing may be hot when you have to work at the optical unit.
515
1 - deuterium lamp 2 - union holder 3 - waste tube 4 - bolts 5 - connector shutter 6 - connector PDA
516
517
Replacing Window Assembly Parts Take out the flow cell window assembly (Figure 190, item 1). Take out the quartz window carefully by pressing it out of the window holder. N OT E If the washers have fallen out of the assembly they have to be inserted in the correct order. Otherwise the window may break or will be leaky see. Clean or replace the window. Fix the window assembly.
518
519
Windows
Washer
520
Stage 1: Disassembling the Window Assembly Take flow cell out of optical unit. Unscrew window assembly (see Figure 191) using a 4 mm hexagonal key--use a 20 mm open-ended wrench to hold the flow cell. Carefully take out window using a toothpick or a 4 mm hexagonal key. Take out the conical disk springs and discard them. Clean window in ultrasonic bath filled with methanol or ethanol. Stage 2: Assembling the Window Assembly Put conical disk springs in window screw see Figure 191. Always use new conical disk springs. Press window and seal rings together using tweezers. Put window and seal rings in window screw. Keep window facing upwards to prevent it falling out. Screw window assembly into flow cell until finger tight. Tighten window assembly using a 4 mm hexagonal key, use a 20 mm open-ended wrench to hold flow cell. Check flow cell for leaks. If you have an 1050 Series pumping system use flow test method described in Installing and Maintaining Your Pumping System. Connect inlet capillary of flow cell to pump outlet. Connect blank nut to outlet capillary of flow cell. If flow cell leaks tighten window screw and check again for leaks. Put flow cell in optical unit.
521
522
Figure 192
523
524
Replacing Fans
Remove top cover and disconnect ALL cables from Motherboard. Figure 194 Removing Fans
Take out the foam part which contains the fans completely. N OT E Take care that no connector on the Motherboard breaks when removing or inserting the foam part. Note the position of the fan and replace it (arrow on the fan). Replace foam part carefully into the module. Connect ALL cables at the Motherboard and replace top cover.
525
Remove the main cover to have access to optical unit. Disconnect flow cell and remove it. Remove slit assembly. Remove the cover of the optical compartment (5 screws). Disconnect LPC board from shutter assembly. Replace shutter assembly or LPC board. Replace all parts in correct order.
526
Remove the main cover to have access to optical unit. Disconnect flow cell and remove it. Remove slit assembly. Remove the cover of the optical compartment (5 screws). Disconnect leak sensor from LPC board using a pliers. Replace leak sensor. Replace all parts in correct order.
527
528
529
Preparations
Prime the pump and ensure there are no air bubbles in the system. Thoroughly degas about 300 ml of bi-distilled water. Set pump to deliver bi-distilled water at a flow rate of 1 ml/min. Set the attenuation of the recording device to about 35 cm/mV. Set run time to 6.0 minutes. Turn ON detector and allow intensity of emitted radiation from radiation source to stabilize. Set detection wavelength to 254 nm and bandwidth to 4 nm. Set reference wavelength to 450 nm and bandwidth to 100 nm. Set peak width to >0.05 minutes. Set output signal so that 1 AU is equivalent to 0.5V. Start a run, press [[START]] [[ENTER]].
530
DAD/MWD: Maintenance Information Verifying the Performance The baseline noise should not exceed 20 V (4 x 10-5 AU) equivalent to 12 mm at attenuation - 3 on a3390/2/3 integrator and equivalent to 24 mm at attenuation - 3 on a 3394/6 integrator. Figure 197 Example of Noise Plot
531
Scaling Factors
The table below shows the scaling factors for the 339XA family of integrators. The 3390A, 3392A and 3393A have a full scale deflection of 75 mm. The 3394A and the 3396A have a full scale deflection of 150 mm, they also have an attenuation range between -8 and 36.
Table 121
Scaling Factors on 339X integrators ATTN -3 -2 -1 0 1 2 3 4 5 6 7 8 9 10 mV full scale 0.125 0.25 0.5 1 2 4 8 16 32 64 128 256 512 1024 mAU full scale 0.25 0.5 1 2 4 8 16 32 64 128 256 512 1024 2048
532
23
23
This chapter gives diagrams for parts identification and the complete parts listings respectively. Overall Diagram Optical Unit Heat Exchanger and Flow Cell Flow Cell Kits Upgrade Parts MWD to DAD Accessory Kit
534
Overall Diagram
Table 122
Item Description 1 Fan Base (set of two) 2 Fan DC Axial Fan Cover # 3 Mainframe 4 Screw M4 20 mm lg 5 Screw M3.5 8 mm lg 6 Foot Rear 7 Foot Front 8 Cover Hinge 9 PWR Switch Actuator 10 PWR Switch Spring 11 PWR Switch Push Button #12 Frame + Cover Keyboard (42) 13 Filter 14 Ring Filter 15 Logo Base/Name Plate 16 Front Panel (incl. 13, 14) 17 Power Switch Base 18 Leak Interface TOP 19 Leak Interface BOTTOM 20 Leak Interface Adapter 21 Tube Flexible 6.5 mm i.d. (5 m) 22 Tube Flexible 0.7 mm i.d. (5 m) 23 Bolt Part of 16 Part of 16 5041-2144/n.a. 01048-60301 5041-2145 5062-8551 Part of 18 Part of 18 5062-2463 5062-2462 5041-2164 0515-0175 0515-0889 0403-0427 5041-2161 5041-2147 5041-2162 1460-1510 G1600-47400
Overall Diagram
Part Number 01048-47701 01048-68500 3160-0544 Item Description 24 Keyboard Module (DAD) Keyboard Module (MWD) 25 FIP Board 26 Cable FIP/LUM 27 Optical Unit 28 Cable PDA/SHUTTER-LUM 29 Heat Exchanger/Flow Cell 30 Cable Lamp/LUM # 31 Cover Power Supply 32 Power Supply Assembly 33 ASC Board Assembly 34 AQB Board Assembly 35 FIM Board Assembly (DAD) FIM Board Assembly (MWD) Screw M3 6 mm lg 36 DAC Board Assembly 37 Plate Cover (33 mm width) 38 CMP Board Assembly 39 Top Cover # 40 Card Cage Assembly 41 LUM Mother Board Assembly Part Number 01048-60202 01048-60201 5061-3376 5061-3400 see page 538 5062-2410 see page 540 01048-61603 01048-04104 01050-69375 01048-66501 01048-69543 G1306-66524 01048-66504 0515-0886 01048-66502 5001-3721 01050-69580 5001-3724 01048-84501 01048-66510
43 Communication Interface Board CRB 5062-2482 # These items are part of Sheet Metal Kit 01048-68701
535
Figure 198
536
Figure 199
537
Optical Unit
Table 123
Item Description
Optical Unit
Part Number Item Description Part Number
# Optical Unit - New # Optical Unit - Exchange # 1 Shutter Assembly 2 Screw M3 6mm lg # 3 LPC Board Assembly 4 Screw M2.5 6mm lg 5 Bolt 6 RFI Strip 7 Damper 8 Deuterium Lamp Assembly 9 Screw M3 10mm lg 10 Union Holder 11 Screw M3 8mm lg 12 Set Screw M3 6mm lg 13 Union # 14 Slit Assembly 2 nm Slit Assembly 4 nm Slit Assembly 8 nm
01048-60024 01048-69024 79883-61901 0515-0886 79883-66509 0515-0894 5021-1853 01048-09101 5041-2165 79883-60002 0515-0757 01048-02321 0515-1430 0515-0031 0100-0900 79883-80002 79883-80004 79883-80008
# 15 Flow Cell Assembly STD Flow Cell Assembly HP-STD Flow Cell Assembly HP-Micro Cell Clamp Assembly Screw M2.5 6mm lg # 16 Capillary IN 0.17 # 17 Capillary OUT 0.17 18 Union 19 Clamp Union # 20 Screw 21 Heat Exchanger Assembly 22 Screw M3 8mm lg 23 Tubing Flexible 80mm lg 24 Elbow Fitting (Plastic) 25 Leak Sensor Assembly 26 Nut M3 27 Screw M3 8mm lg # 28 Cover Illum Compartment # 29 Achromat Assembly
see page 541 see page 542 see page 543 79883-85001 0515-1056 79883-87303 79883-87304 0100-0900 79883-00502 0515-0922 01048-87305 0515-0897 0890-0581 0100-1428 5061-3356 0535-0004 0515-1430 79883-04101 79883-60000
# These parts are not interchangeable with the previous optical unit design (Series I).
538
Figure 200
Optical Unit
29
539
1 Heat Exchanger 2 Screw M3 8mm lg 3 Flow Cell STD Flow Cell High Pressure STD Flow Cell High Pressure Micro 4 Capillary IN Figure 201
01048-87305 0515-0897 see page 541 see page 542 see page 543 see flow cell Heat Exchanger and Flow Cell
540
Flow cell SST 6 mm, 8 l Flow cell SST 10 mm, 13 l Cell Repair Kits Capillary IN 0.17, 100 mm lg Capillary OUT 0.17, 150 mm lg 1 Window Assembly consists of 3, 4, 5, 6, 7 2 Cell Gasket 3 Window Quartz 4 Window Holder Figure 202
5 Compression Washer 6 Washer (pack of 10) 7 Window Screw 8 Cell Clamp Assembly
Screw M2.5 x 4 mm lg (cell body) 0515-1056 Clamp Union Screw M2.5 x 8 mm lg (clamp) 79883-00502 0515-0922 8710-1534 8710-2023
541
High Pressure Flow Cell Cell Repair Kits 1 Window Assembly consists of 2, 3, 4, 5, 6 Seal ring HP Window Quartz HP Compression Washer HP
5 6
Washer (pack of 10) Window Screw SST Cell IN 50 .17, 100 mm lg Cell OUT 50 .17, 150 mm lg
2 3 4
Figure 203
542
Micro Flow Cell 1.7 l Cell Repair Kits 1 Window Assembly consists of 2, 3, 4, 5, 6 2 Seal ring HP 3 Window Quartz 4 Compression Washers HP Figure 204
5 Washer (pack of 10) 6 Window Screw SST Cell IN 50 .17, 100 mm lg Cell IN .12, 100 mm lg
Cell OUT 50 .12, 370 mm lg Hex Key 6 mm for cell screw Wrench 4 mm for fittings
543
Table 128
Cell Repair Kits Description Cell Repair Kit Seal Kit Cell Screw Kit Seal Kit Cell Screw Kit Window Quartz (2) Compression Washers (2) Window Holder (2) Window Screw (1) Spring Washers (10) Cell Kit High Pressure Window Quartz HP (1) Spring Washers (10) Seal ring HP (2) Cell Gasket (12) contains (Qty) Part Number 79883-68701 79883-68702 79883-68703 79883-68702 79883-68703 1000-0488 79883-28801 79883-22301 79883-22402 5062-8553 79883-68700 1000-0953 5062-8553 79883-27101
544
Lamp Housing
Table 129
Lamp Housing # Description 1 Retaining Ring 2 Spring Compression 3 Aperture 4 Window Part Number 0510-1219 1460-2254 79883-24601 79880-28111
Figure 205
Lamp Housing
545
Table 130
1050 Upgrade Parts MWD to DAD Description Firmware Board FIM Keyboard (plastics) Installation Note Part Number G1306-66524 01048-60202 see Upgrade to from 79854A MWD to G1306A DAD on page 528
546
Table 131
Upgrade Parts MWD to Series II Optical Description Optical Unit Firmware Board FIM Slit assemblies as required Flow cell as required Resistor for AQB board modification 220 Ohm 5% 2W AQB board (latest version)
*
Part Number 79883-60024 01048-66504 * see Optical Unit on page 538 see Flow Cells 0698-3628 ** or
01048-69543
Only required, if firmware revision is < 3.1. Only required if AQB board does not have the resistor that is located between fuse F22 and the rear connector J1 (SN 01050-016).
**
547
List of Accessories
The following list shows parts that were part of the STD Accessory Kit. Please order by item if required.
Table 132
Accessories Description Hex Key for flow cell Capillary Column/MWD 0.17 mm i.d. 800 mm lg Crimp Terminals Screw M3 6 mm lg Tube Flexible 0.7 mm i.d. (re-order 5 m) CONT CONN UTIL F CONN UTIL 2PIN F Fuse 2 A 250 V NTD Fuse 3 A Fuse 250 V 0.25 A NB Ferrule Gripper Male Buffer Disc Wrench 5/16-1/4 Screwdriver POZI 1 PT 3 Hex Key 3 mm Hex Key 6 mm for cell screw Part Number 8710-2023 01048-87302 0362-0321 0515-0886 5062-2462 1251-3911 1251-4782 2110-0002 2110-0003 2110-0004 5041-2121 5041-2122 5041-2123 5041-2124 8710-0510 8710-0899 8710-0911 8710-2023
548
24
24
This section gives the following informations: Hardware changes Firmware changes Known Problems
550
Product History
The introduction of the 79854A Multiple Wavelength Detector was in 1988. The introduction of the G1306A Diode Array Detector was in 1993. The following hardware and firmware changes have been implemented.
Hardware Changes
Table 133 Hardware Changes Date 1990 Jul 1992 Serial Number 3016G.... Change Introduction of Series II optical Introduction of new cell screw design for Series II flow cells. 6 mm hexagonal key instead of screw with slit. Introduction of High Pressure Cell with 13 l and 1.7 l for 400 bar operation (for Series II). 3343G00938 New AQB board, same for 79854A MWD, G1306A DAD and G1600A CE. Introduction of Fan Cover and new part number for fans 3414G00321 3423G../3423A... New Firmware 1.10 (see Firmware Changes on page 552). Introduction of n-MOS optical units. Change on ASC board (delay time of amplifier), revision D-3444. DAD DAD New Firmware 1.20 (see Firmware Changes on page 552). New Firmware 1.30 (see Firmware Changes on page 552).
Nov 1992 Oct 1993 Apr 1994 Apr 1994 May 1994 Jul 1994 Dec 1995 May 1997
551
Firmware Changes
Table 134
DAD Firmware Revisions Revision Major Changes 1.00 1.10 Instrument checks for lamp overflow before WL calibration and returns an error message (RE3001) if lamp overflow occurs. Comments First official release for G1306A Essential for optical used in Capillary Electrophoresis instruments. FIM board same in G1306A and G1600A (CE)
1.20 1.30
added fraction collection for G1600A same in G1306A and G1600A (CE) (CE) for use with new ChemStation Software same in G1306A and G1600A (CE)
Table 135
MWD Firmware Revisions Revision Major Changes 1.00 3.00 No GPIB communication GPIB communication for HPLC ChemStation. Comments First official release for 79854A Showed some GPIB communication problems. Should be replaced with revision 3.1 (01048-66504).
3.10
552
Known Problems
Panic Errors
Intermittent PANIC errors are mostly generated by spikes (disturbances) on the bus lines. A dynamic bus termination has been added to the FIM board to suppress the spikes and to reduce the possibility of this failure mode. All FIM boards with revision C and higher do have the dynamic bus termination installed (RC-network instead of R-network). In case of intermittent PANIC errors replace FIM boards (revision A or B) with the current version.
553
554
In This Book This manual contains technical information about the Agilent 1050 liquid chromatographs. This manual is available as electronic version (Adobe Acrobat Reader file) only.
1050 Series of HPLC Modules Service Handbook Variable Wavelength Detector (79853C)
Copyright Agilent Technologies 2001 All rights reserved. Reproduction, adaption, or translation without prior written permission is prohibited, except as allowed under the copyright laws. Part No. NONE 11/2001 Printed in Germany
Warranty
The information contained in this document is subject to change without notice. Agilent Technologies makes no warranty of any kind with regard to this material, including, but not limited to, the implied warranties or merchantability and fitness for a particular purpose. Agilent Technologies shall not be liable for errors contained herein or for incidental or consequential damages in connection with the furnishing, performance, or use of this material.
IMPORTANT NOTE This version of the 1050 service manual includes all sections from the 01050-90102 edition 4 (1995). The series I opticals information (79854A MWD) and the 79853A VWD information has been removed (products went out of support during 2000). Part numbers have been updated as of 11/2001. Contact your local Agilent support office in case of part number issues or upgrades. The latest version of this manual is available as Adobe Acrobat Reader (PDF) version only and can be downloaded from the Agilent Technolgies web page www.agilent.com.
25
25
This chapter gives general information on about this detector repair policy specifications
560
79853C
The 79853C VWD replaced the model 79853A VWD in January 1992. The end of support (EOS) will be August 1, 2006 with all 1050 series HPLC modules. The 79853C VWD got a redesigned optical unit (D enhanced optical, see VWD: Enhanced Optical Unit Information on page 705) that replaced the original C optical unit in June 1995. The end of support (EOS) for the C optical unit parts will be August 1, 2006 with all 1050 series HPLC modules.
561
Repair Policy
The 1050 VWD is designed that you can access all components easily. You can recalibrate wavelength using control functions. Customers are able to maintain certain parts of the 1050 VWD see Operators Handbook. For details on repair policy refer to Repair Policy on page 38 in chapter 1050 Common Information.
562
Specifications
Table 136
Specifications of 79853C VWD Detection Type Noise Double beam photometer. < 1.5 x 10-5 AU peak-to-peak at 254 nm, flowing water at 1 ml/min, 1 second response time (10-90%), standard flow cell. < 5 x 10-4 AU/hour at 254 nm after warm-up. 190 - 600 nm, settable in 1 nm increments. 2 nm. 0.3 nm. 6.5 nm. Better than 1% up to 1.2 AU using acetone at 265 nm. 0.25, 1 or 4 seconds (10-90%); user-selectable. Storage of 1 spectrum during run; scan rate 10 nm/sec; range from 190 to 600 nm, selectable. Post-run plotting speed from 1 to 50 nm/sec selectable; plotting of background-corrected spectrum. Deuterium lamp from 1090/40/50 DAD. Standard 14 l volume, 8 mm pathlength cell with 40 bar (588 psi) pressure maximum. Optional micro, preparative, high-pressure cells are available. Single line, 16 character fluorescent display with real time display of operating parameters and/or absorbance. Integrated keyboard with function keys; parameter editing during run possible; keyboard lock; optional control by computer or 3396 Series II integrator.
Drift Wavelength Range Wavelength Accuracy Wavelength Reproducibility Bandwidth Linear Absorbance Range Response Time Spectra
Display
Control
563
Table 136
Specifications of 79853C VWD Parameters Diagnostic Aids Time-programs Analog Output Wavelength, output range, response time, zero, offset, balance, spectrum acquisition. Wavelength calibration check with Holmium oxide filter. Time-programmable wavelength and output range; storage of up to 5 time-programs. One output user-configurable as recorder or integrator. For recorder: 100 mV or 1 V output range from 0.001 to 4 AU, user-selectable; for integrator: 100 mV/2 AU full scale or 1 V/2 AU full scale, user-selectable. START (input/output), STOP (input/output), READY (output), SHUTDOWN (output) for synchronization with other LC modules. Extensive diagnostics, error detection and display via front-panel LEDs. Leak detection, safe leak handling, leak output signal for shutdown pumping system. Low voltages in major maintenance areas. Temperature range: 5 to 55C Humidity: < 95% (non-condensing) Power Requirements Line voltage: 100-120 or 220-240 VAC 10% Line frequency: 48-66 Hz Power consumption: 150 VA max. Dimensions Height: 133 mm ( 5.2 inch) Width: 325 mm (12.8 inch) Depth: 545 mm (21.5 inch) Weight: 14 kg ( 31 lb)
Communications
Safety Aids
Environment
564
26
26
Overview
N OT E The information in this chapter is based on the original optical unit (version C). In June 1995 this optical was replaced by the enhanced version D to overcome baseline stability problems in unstable environments. For details on this D version refer to section Enhanced Optical Unit Information VWD: Enhanced Optical Unit Information on page 705. Figure 206 on page 567 shows the block diagrams of the 1050 VWD 79853C. The main components are:
Table 137
Main Components Overview Component Power Supply (DPS-A) Detector Controller Board (DCB) Purpose provides all voltages within the instruments controls power supply, grating stepper motor, cutoff filter, keyboard, display and GPIB interface. It processes the signals coming from the pre-amplifier boards (sample and reference), the information from the grating and filter position sensor, leak sensor, remote control lines and the GPIB interface. contains all optical parts entry and display of parameter communication with external controllers via GPIB
566
Figure 206
567
568
569
570
Fan Assemblies
The instrument is equipped with two fans. On the 79853C VWD, the fans are of different type: HIGH type LOW type this fan is located close to the lamp housing and runs with a higher speed this fan is located at the rear under the GPIB interface and runs with a lower speed
571
Optical Unit
N OT E The information in this chapter is based on the original optical unit (version C). In June 1995 this optical was replaced by the enhanced version D to overcome baseline stability problems in unstable environments. For details on this D version refer to section Enhanced Optical Unit Information VWD: Enhanced Optical Unit Information on page 705. The Optical Unit houses all parts, from the deuterium lamp to the photodiode pre-amplifiers. N OT E The repair level is component. The optical unit is also available as assembly. Figure 210 Optical Unit
572
Flow Cells
There are several flow cells available as stainless steel or as titanium version, see Table 138 on page 574. The flow cell (Figure 211) can be exchanged easily. No adjustments are necessary. After disassembling of the flow cell, gaskets and windows can be replaced (refer to section Flow Cell Maintenance on page 655). There are several kits set up with replacement parts like gaskets and windows, see Standard Flow Cell C (SST/Ti) on page 693 and the following pages. Figure 211 STD Flow Cell
N OT E
At the outlet of the flow cell a defined peek capillary (from the accessories must be connected to build up a certain back pressure (noise reduction). See Standard Flow Cell C (SST/Ti) on page 693 and the following pages for parts.
573
Table 138
Flow Cell Data STD (SST) Maximum Pressure Pathlength Volume Inlet i.d. Inlet length Outlet i.d. Outlet length Outer diameter 40 8 14 0.25 555 0.25 67 1/16 UHP MICRO (SST) (SST) 400 8 14 0.25 555 0.25 67 1/16 40 5 1 0.10 555 0.25 67 1/16 STD (TI) 40 8 14 0.25 555 0.25 67 1/16 PREP (TI) 40 VAR VAR 0.80 67 0.80 100 1/16 bar mm l mm mm mm mm inch
Used materials for SST flow cells: SST, quartz and PTFE or Polyimide HP cell Used materials for TI flow cells: STD HP UHP Standard Flow Cell High Pressure Flow Cell (replaced by UHP early 1993) Ultra High-Pressure Flow Cell (replaces HP early 1993), see details on Ultra High-Pressure Flow Cell on page 575. Variable Preparative Flow Cell with volume of 0.9, 1.8, 4.4 or 8.8 l depending on which gasket is used. Semi Micro Flow Cell TI, quartz and PTFE
PREP MICRO N OT E
The gaskets, windows and rings are not compatible with the high pressure Cell (79853-60009 - OBSOLETE) that has been replaced by the ultra high pressure Cellflow cell (79853-60013). See Ultra High Pressure Flow Cell (SST) on page 697 for details.
574
Table 139
Correction factors for 79853C flow cells Path length (nominal) 8 mm 8 mm 5 mm 8 mm Path length (actual) 8.00 0.19 mm 8.00 0.19 mm 5.00 0.19 mm 8.00 0.19 mm Correction factor 8/8.05 8/8.00 5/5.00 8/8.00
Flow cell type Standard flow cell Standard flow cell TI Micro flow cell Ultra High pressure flow cell
Ultra High-Pressure Flow Cell Typical applications of the high-pressure flow cells are: Hyphenated systems (LC-MS) Supercritical Fluid Chromatography (SFC) Multidetector systems Narrow-bore column applications The main difference between the standard and high-pressure flow cells is the design of the window assemblies. The high-pressure flow cells have different windows, seal ring and gaskets, see Figure 212. The seal rings support and hold the window and at the same time form the high-pressure seal. N OT E The gaskets, windows and rings are not compatible with the high pressure Cell (79853-60009 - OBSOLETE) that has been replaced by the ultra high pressure Cellflow cell (79853-60013). See Ultra High Pressure Flow Cell (SST) on page 697 for details. The following materials are in contact with solvents: Stainless steel (AISI 316), Quartz, Kapton polyimide (Kapton is a registered trademark of DuPont). Recommended pH range: 2.3 to 9.5
575
Figure 212
Deuterium Lamp
On the 79853C VWD, the deuterium lamp (Figure 213) is the high intensity lamp (79883-60002), which is same as in the 1040/90/50 series Diode Array Detectors. The reduction of energy emission of the lamp (Figure 214 on page 577) is time and wavelength dependent and is significantly higher within the first days and for wavelengths in the ultra violet range compared to the visible range (change in transmission of lamp glass). Usually, the response maximum of the lamp is near 230 nm, but can be shifted to a higher wavelength for an aged lamp. It has no relevance for intensity degradation at other wavelengths. The deuterium lamp filament is heated only during the ignition phase. The deuterium lamp can be exchanged easily. The lamp needs no adjustments.
576
Figure 213
Deuterium Lamp
Figure 214
Measured wavelength is 230 nm initial intensity about 20% higer than 79880-60002 decrease in intensity is less with use
577
N OT E
The lamp should be replaced only if the following two criterias are both fulfilled: Baseline Noise (with test cell) has increased significantly. Amount of counts of the lamp (with test cell) has decreased to less than 50% of the count record of this same lamp when newly installed). The decision to replace the lamp due to criterium 2 alone is not relevant, because the signal/noise may be still within instrument specifications.
578
Photodiodes Assemblies
Two photodiode assemblies (Figure 215) are installed in the optical unit. The sample diode assembly is located at the right side of the optical unit. The reference diode assembly is located in the front of the optical unit. N OT E Neither, the diodes nor the pre-amplifier boards are interchangeable.
N OT E Figure 215
Refer to Replacing Pre-amplifiers or Photodiodes on page 667 for cleaning. Photodiode Assemblies
sample diode
reference diode
579
Filter Assembly
On the 79853C VWD (Figure 216), the Filter Assembly has a three filters [1] installed and is processor controlled. It can move into four positions: OPEN CUTOFF DARK HOLMIUM nothing in lightpath at wavelength < 370 nm cut off filter in lightpath at wavelength > 370 nm 0 order calibration filter to reduce the light throughput to the photodiode during grating calibration at 0 order light holmium filter for grating motor alignment
A photo sensor [3] determines the correct position. N OT E Figure 216 Refer to Replacing Filter Assembly Parts on page 670 for cleaning. Filter Assembly
580
N OT E
The grating is coated with magnesium fluoride. The grating surface should not be touched or cleaned (see also Replacing Grating Assembly Parts on page 668). This will destroy the surface and reduce the light reflection.
581
Mirrors
The instrument contains four mirrors (M1, M2, M3, M4). Three of them are spherical type, one plane. On M2, M3 and M4 the beam height is adjustable. Mirror M3 and M4 are identical. N OT E The mirrors are coated with magnesium fluoride. They should not be touched or cleaned (see also Replacing Mirrors, Beamsplitter and Slits on page 670). This will destroy the surface and reduce the light reflection.
Slit Assemblies
The instrument has two slit assemblies. The first slit is located at the light entry into the main optical compartment and focused the light on mirror M3. The second slit is in front of the reference diode.
Beam Splitter
The beam splitter splits the light beam. One part goes directly to the sample diode. The reference diode gets the other part. The height of the light beam is adjustable. Refer to Replacing Mirrors, Beamsplitter and Slits on page 670 for cleaning.
582
583
584
27
27
This chapter gives information about the electronic of the 1050 Variable Wavelength Detector: Overview Interconnection Diagram Detector Controller Board (DCB) Power Supply (DPS-A) Keyboard/-electronics Pre-amplifier Boards Power Supply Connection Board (PSC) GPIB Communication Interface
586
Table 140
Electronic Assemblies Item Description 1 GPIB Interface Firmware ROM GPIB 2 Fan Assembly (LOW) 3 Fan Assembly (HIGH) 4 Connection Board (PSC) 5 Deuterium Lamp Assembly 6 Sample Diode Assembly (SDA) 6 Pre-Amplifier Board SAMP 7 Display Interface Board (KDI) 7 Display Module (VFD) 8 Leak Sensor Assembly 9 Reference Diode Assembly (RDA) 9 Pre-Amplifier Board REF 10 Controller Board (DCB) 11 Firmware ROM DCB 12 Power Supply Assembly (DPS-A)
587
Figure 218
Location of Electronic
588
Interconnection Diagram
Figure 219 Interconnection Diagram
589
Table 141
Part Numbers for DCB tem DCB (Exchange) DCB DCB Firmware ROM DCB Part Number 79853-69511 79853-66511 Comment for use with PSC -66512 for use with PSC -66512
N OT E
If the DCB board is replaced by 79853-66511 version, the PSC board MUST be changed to 79853-66512. The main functions of the Detector Controller Board (DCB) are: CPU signal processing display analog output digital input/output A/D conversion D/A conversion control of Optical Unit deuterium lamp ignition grating movement filter movement leak detector remote control
Main Functions
590
Figure 220
591
Digital Section
CPU A 8-bit 1-chip Microprocessor 7810 is used as CPU. The 7810 includes 256 byte-RAM, 8 channel 8-bit A/D Converter, 16-bit timer/event counter, 2-channel 8-bit timer and two 8-bit I/O Ports. The Data Bus is 8-bit multiplexed with the address. The ROM contains the firmware of the the detector and can be exchanged separately. In addition to the built-in functions, the 7810 has 64 Kbyte| of external memory address and 32 Kbyte-ROM, 8 Kbyte-SRAM and 2 Kbyte-EEPROM are added. The EEPROM contains: the time program; the grating calibration constant; D/A converter calibration constant; parameters set by key input (wavelength, range, response time, mode). Clock The main clock (24 MHz) is divided and distributed to: 24 MHz 12 MHz 6 MHz 3 MHz 1.2 KHz A/D Converter Count Pulse CPU Clock D/A Converter Count Pulse GPIB Controller, Key/Display Controller Clock A/D Converter Integration period
ROM/RAM/EEPROM
After the power turns on, for about 100 ms the RESET signal is supplied to CPU, GPIB Controller and Key/Display controller. Also, anytime when power voltage becomes less than 4.7 V, the RESET signal is generated. The CPU controls directly the Buzzer and the Stepper Motor Driver to move the filters on the filter assembly. The stepper motor for the grating, the input and the output port are connected to the internal BUS (DATA ADDRESS and CONTROL) and are controlled by the CPU. The grating motor and the filter motor are driven by a motor controller IC and phase pattern are coming from CPU.
592
Figure 221
593
Analog Sections
Signal Processing The light beam from the SAMPLE and REFERENCE enters the photodiode respectively. Its current output is converted into a voltage by pre-amplifier. The gain of the pre-amplifier can be changed into four stages with CPU control. The voltage signal from the pre-amplifiers are multiplexed and converted into digital form by a 18-bit A/D Converter. The conversion time of A/D Converter is 25 ms and is performed cyclically in the order of Zero Sample-Reference (Zero=GNDA) Electrically zero calibration is done while balancing. Digital data is transmitted to the CPU, digitally filtered based on response time and converted into the absorbance unit using the equation shown below:
AU = log
10
( REF ) log
10
( SAMP )
594
Figure 222
595
A/D Converter
Method for the A/D conversion is feedback type Pulse Width Modulation (PWM). A/D Converter
Figure 223
Positive or negative reference voltage is alternately added to the integrator. Duty cycles of each reference voltage is controlled by the output of a comparator connected to the output of integrator. Input voltage (U1) is converted to pulse width so that sum of both reference voltages is balanced with the U1. Clock voltage and ES control this system and determines the period. The sum of clock voltage in one cycle is set to zero. Pulse width, which is proportional to input voltage U1, is counted and is converted into a digital output. The A/D converter has 18 bits resolution with 25 ms conversion time. D/A Converter D/A converter combines a Pulse Width Modulator (PWM) and a 12-bit DAC. The lower 4 bits of the DAC pulse width modulated with 12 bit resolution is added to the upper 8 bits of the DAC. The upper 8 bits are also modulated by fixed pulse width so that the lower 4 bits balances to LSB of the upper 8 bits (pulse width is 15/16). The lower 4 bits are scaled to each bit of the upper 8 bits when using 44:DAC CALIBRATION. The output of the 12-bit DAC is passed through a low-pass filter and 20-bit resolution analog signal is outputted to the BNC Connector. The cutoff frequency of a low-pass filter is set at 17 Hz while conversion frequency is 183 Hz.
596
Figure 224
D/A Conversion
The signal output is classified into three types: Display Out, Analog Out, Digital In/Out. The display module receives ASCII codes via Keyboard Interface Board via the Data Bus. On the Display Module, the ASCII code is converted to display code and gives output on fluorescent display with 5 x 7 dots and 16 characters. The Signal (Analog) Out is available at a BNC connector at the rear of the instrument. It is generated by 20-bit D/A converter. The conversion cycle of the D/A converter is about 5.5 ms. The output of the D/A converter is filtered by a low-pass filter. The output can be switched to: Full Scale 1V 0.1 V Output Impedance 1000 Ohm 100 Ohm
The digital signal is delivered to the GPIB Interface (option) via the Data Bus and is converted into an GPIB signal. The deuterium lamp is ignited using Anode Current, Trigger Voltage and Heater Voltage supplied from the Power Supply Unit. The ignition procedures are controlled by the CPU signal. The heater voltage is switched from 2.5 V during ignition to 0 V after ignition.
597
The wavelength is set by rotating the grating with a 2-phase stepper motor. The step angle of the stepper motor rotation (1 step angle 3.75) and is reduced to 1/300 by a gear. The stepper motor is controlled and driven by DCB. The CPU contrls the motor controller IC that drives the motor. Stepper Motor reference position is determined by a plate fitted on the swing arm interrupting a beam of photo interrupter. The output signal of the photo interrupter is read by a 8-bit ADC of the CPU. The rotation of stepper motor controls the insertion of a diffterent filters into the light path (cutoff, holmium, light reduction). The stepper motor is controlled and driven by DCB. The CPU controls the motor controller IC that drives the motor.
Remote Control
The REMOTE connectors communicate start or stop, error and not ready signal inputs and outputs. For detailed description of remote control refer to the 1050 Service Handbook, chapter Common Information.
N OT E
When the 79853C VWD is used in a system which is connected via remote, the VWD should be switched on as first module. Otherwise it may influence other modules at power on. The leakage from a flow cell is detected by change of Thermal Radiation Constant of NTC thermistor. Wheatstone bridge is constructed from NTC thermistor and resistors on the DCB. Its supply voltage is varied by controlling 24 V-power with Switching Regulator controller. The supply voltage is controlled to keep the thermistor at about 150 Ohm (150C) constantly. If leakage occurs and the thermistor is soaked in the leaked liquid, the thermal radiation constant are changed and gives higher supply voltage at both ends of wheatstone bridge. This change is read by the CPU and compensated with ambient temperature. Error condition is when LS > LL. The values are visable with 33:LEAK TEST.
Leak Detection
598
Figure 225
Change in Thermal Radiation Constant with surrounding temperature change is compensated by second NTC thermistor having same characteristics.
599
Figure 226
Table 142
Photocurrent 2 REF +5 V 7
Analog GND 10
600
Table 143
Part Numbers for DPS-A Item DPS-A (Exchange) DPS-A (New) Fuse for 110 V operation 3 A Fuse for 220 V operation 2 A Part Number 01050-69375 5061-3375 2110-0003 2110-0002
For detailed information on the power supply refer the 1050 Service Handbook, chapter 1050 Common Information. Lamp Ignition The heater output made by a series regulator is in the pre-heating status 2.5 V always. After ignition a different output voltage is selected depending on the lamp type used: In the 79853C VWD the heater is switched off after ignition.
601
Keyboard
The flat keys at the front panel is composed of 6 x 4 matrix. Data is read by scanning at Key/Display Controller on the Keyboard Display Interface Board. Key entry is checked by reading the status of the controller by the CPU at every 10 ms. The Key/Display Controller also controls LED lamp lighting. Figure 227 Keyboard
602
Table 144
Part Numbers for Keyboard Electronics Item Keyboard Display Interface (KDI) Display Module Board (VFD) Part Number 79853-66502 79853-66503
Behind the frontpanel two electronic boards are located: Keyboard Interface Board (KDI) and the Display Module Board (VFD). Keyboard Display Interface The Keyboard Interface Board (KDI) is connected to the DCB board and contains: interface between key-matrix (6 x 4) and DATA bus LED driver for the status messages ERROR, NOT READY, LAMP and RUN buzzer. Display Module The Display Module Board (VFD) is connected to the KDI and contains: CPU for control of latch driver latch driver for the Vacuum Fluorescence Display (FLD) DC/DC converter to provide the voltages for the FLD. Refer to Replacing Display Boards on page 662, when replacing this board.
603
Figure 228
604
Pre-Amplifier Boards
Repair Level: Board
Table 145
Part Numbers for Pre-Amplifiers Item Pre-Amplifier Board Sample Pre-Amplifier Board Reference Sensor Sample Sensor Reference Part Number 79853-66507 79853-66508 79853-61109 79853-61110
The light (absorbtion) from the deuterium lamp (flow cell) is detected by the sample and the reference photodiode. Its current is then amplified by the pre-amplifiers. The signal then is routed to the DCB. The wires from the photodiodes are soldered onto the board. Figure 229 Photodiode Assemblies
Sample
Reference
605
Table 146
Part Numbers for PSC Board Item PSC Board (for DCB -66511) PSC Board (for DCB -66506 OBSOLETE) Part Number 79853-66512 79853-66509 OBSOLETE
N OT E
If the DCB board is replaced by 79853-66511 version, the PSC board MUST be changed to 79853-66512. This board connects the Power Supply DPS-A with the DCB and the Deuterium Lamp Assembly. The wires of the lamp cable are soldered in.
Figure 230
606
Table 147
Part Numbers for GPIB Interface Board Item GPIB Board (with cable) GPIB Cable to DCB Board Firmware ROM GPIB 79853-13004 Part Number 79853-68711
Parallel Interface
Dual direction transceiver for data bus between master and slave CPUs. 8 bit aux code from DCB to GPIB board. 3 bit control code from GPIB board to DCB Single chip microprocessor with 1 Mbyte address capability, 512 byte internal RAM and 32 I/O ports. 32 Kbyte of ROM for program memory and 128 Kbyte RAM for the run buffer.
Microprocessor Memories
Firmware Description The GPIB board performs all interruption processing from the GPIB controller. DCB and GPIB board communicate with hardware interrupts. Receiving GPIB commands the GPIB board passes them to the DCB with 3 bit control code. This control code shows the kind of bus data such as GPIB commands, error codes or requesting data code and whether the data ended or not. During run or monitor mode the DCB send chromatogram data immediately to the GPIB board with 8 bit aux code. This aux code shows the kind of bus data such as chromatogram data, parameters, time tables, remote line status or GPIB board control code and whether the data ended or not. The GPIB board writes the received data into the run buffer. The GPIB sends out the formatted data adding the start and the end record. GPIB Address Setting The GPIB address setting is done with a switch (1) at the rear of the GPIB board. The factory setting is 10 (position A).
607
Figure 231
608
28
28
This section provides information on the diagnostic routines error messages user contol functions service control functions
610
Self Diagnosis
At power on and after lamp ignition the instrument checks itself for correct operation. In case of malfunctions, error messages will inform the operator on the fault.
During Power On
The following tests are done automatically during power on. They are descibed on the next pages together with the error message: Vaccuum Fluorescent display ROM and RAM Display Leak sensor Voltages A/D Converter EEROM Data Grating Drive
611
VWD: Diagnostic & Troubleshooting Information Error Messages Before Lamp Ignition
At Power ON
During power on the instrument run automatically through different selftest routines. If all test are passed, the display shows HP 1050 VWD. While initializing the CPU checks the response of the Vaccuum Fluorescent Display (VFD) module. If there is no problem, SELF DIAGNOSIS IN PROGRESS is displayed. If there is no response from the VFD, the ERROR lamp will light, the buzzer is heard for 2 seconds and is halted. Check connection DCB/KDI and KDI/VFD module. Replace VFD Module. Replace KDI Board. Replace DCB Board. Replace DPS. ROM TEST FAILED The ROM Test calculates the checksum and compares it with a stored value. If a differrence is found, ERROR LED lights, ROM TEST FAILED is displayed and the CPU is halted. Otherwise ROM TEST OK is displayed. Replace EPROM. Replace DCB. RAM TEST FAILED During RAM Test, firstly every RAM address is uniformly written. Then in ascending order, each address is tested for contents and then the data is inverted and written. Then the same procedure is repeated in decending order with the inverted data. This cycle is repeated twice. If an error is found, RAM TEST FAILED is displayed and further operation is prohibited. Otherwise, RAM TEST OK is displayed. Replace DCB.
612
VWD: Diagnostic & Troubleshooting Information Error Messages Before Lamp Ignition
Display Test
During Display Test every dot on the VFD module is set and you have to confirm it by yourself. If display is black or shows missing dots Check connection of flat ribbon cable DCB to KDI. Replace KDI.
L.SENSOR TROUBLE
The Leak Sensor Test checks the leak sensor and the leak sensor circuit, but not for a leak resulting from the cell. The voltage applied is measured using built-in 8 bit ADC (A/D Converter) of the CPU as well as temperature compensation voltage from a second thermistor. If the LS > LL, L.SENSOR TROUBLE is displayed. The range during turn on should be: LS:0.63..4.06 V and LL:2.82..4.00 V. Use 33:LEAK S.VOLT to verify the values, (see message LEAK DETECTED. Check connection of leak sensor to DCB. Replace leak sensor. Replace DCB.
POWER FAILURE
During Voltage Test this message is displayed if the voltages exceeds the tolerance. If a voltage is not correct, it is displayed for a short moment, for example +24V TROUBLE. Check voltages using function 34:VOLTAGE TEST:
Table 148
DC Voltages Voltages + 12 V (1 V) - 15 V, + 15 V (1 V) + 24 V ( 4.8V) Replace DCB. Replace Power Supply. Used for filter and grating motor analog circuits leak sensor, fans
613
VWD: Diagnostic & Troubleshooting Information Error Messages Before Lamp Ignition
ADC TROUBLE
During the A/D Converter Test the 18 bit ADC for photocurrent acquisition is tested with multiplexer channel fixed at analog ground. Pulse count for ground input is measured 20 times and calculate the average and the fluctuations. If the value exceeds the pre-determined value ADC TROUBLE is displayed. Replace DCB.
During EEROM Data Test various parameters such as monochrometer parameter and time table are stored in EEROM (Electrically Erasable Read Only Memory) in order to save the value in absence of power. At initializing those values are checked using checksum. If an error is found, EEROM DATA LOST is displayed and default values are set. Different types of EEROM DATA LOST messages are possible:
The key settable parameters (wavelength, responsetime, and so on) or time time tables are lost. They are replaced by default values. Re-enter the values. Replace DCB.
Wavelength parameter (zero order) are lost. They are replaced by default values. The monochromater parameters are differrent for each instrument. Execute 20:0th CALIB. or enter the 0th order parameter directly using 31:SET WL PARAM. Execute 45:WL COMPENSATE.
The DAC parameters are lost. The parameters are the scaling factors for each DAC bit and ZERO SPAN factors. The lost parameters are recoverable. Execute 44:DAC CALIB.
The DAC parameters are lost. The parameters are the offset parameter of the ADC reading for the output of each DAC bit (used for DAC calibration). These parameters can be re-written at the factory only. Perform 41:DAC TEST. If OK, then leave it as it is. If NOT OK, then continue.
N OT E
614
VWD: Diagnostic & Troubleshooting Information Error Messages Before Lamp Ignition Perform 44:DAC CALIB. The default values of the offset parameters are taken now. Perform 41:DAC TEST. If OK, then leave it as it is. If NOT OK, then replace DCB board. WL SET TROUBLE During the initialization of the grating motor position, the motor moves backward to the home position where position sensor detects the limit. If it is not able to detect the limit, WL SET TROUBLE is displayed. Check connection of position sensor and grating drive motor. Switch OFF lamp, remove top cover of optical unit to observe movement of grating mirror (changing wavelength). If grating will not rotate after changing the wavelength, replace DCB or the Grating Driver Assy. Using 36:GRATING P.S. you can move the grating shaft automatically or stepwise by pressing the down/up key. Normally in the position of about -200 steps, the output voltage of the position sensor will change from LOW to HIGH, detecting the limit position. If the output voltage will never change, the position sensor is defective or the grating drive assembly has a problem and has to be replaced.
615
VWD: Diagnostic & Troubleshooting Information Error Messages After Lamp Ignition
616
VWD: Diagnostic & Troubleshooting Information Error Messages During Normal Operation
Table 149
If there is no leakage, check the connection leak sensor to DCB. Replace Leak Detector board. Replace Leak Sensor. DATA UNDERFLOW This message may come up only during BALANCING when the sample or referrence voltage is lower than 1 mV. Check, whether the flow cell is in correct position and the screws are tightened. Check the connection of pre-amplifier sample to DCB. Clean cell windows. Replace photo diode assembly. Replace DCB. DATA OVERFLOW This message may come up only during BALANCING when the sample or referrence voltage exceeds 9.4 V. Check, whether the flow cell is in correct position and the screws are tightened. Replace DCB.
617
VWD: Diagnostic & Troubleshooting Information Error Messages During Normal Operation Execute BALANCE, so that the proper pre-amplifier gain is selected. Check, whether the flow cell is in correct position and the screws are tightened. Is apature gasket installed in flow cell? Replace DCB. No response for HPIB set address switch correct. check connection to DCB and GPIB cable. change GPIB board.
ADC OVERFLOW
618
VWD: Diagnostic & Troubleshooting Information Error Messages During Use of Control Functions
619
Table 150
User Control Functions # 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 Display 1:SAMPLE SCAN 2:REF. SCAN 3:SPECTRUM OUT 4:SCAN FROM 5:SCAN TO 6:ZERO OFFSET 7:RESPONSETIME 8:AUTO LAMPOFF 9:AUTO LAMP ON 10:OUTP. DEVICE 11:OUTPUT VOLT 12:STATUS 13:START MODE 14:OUTPUT CHECK 15:RESET 16:PHOTOCURRENT 17:PARAM. LOCK 18:WL SHIFT 19:POLARITY 20:0th CALIB. Used for takes a sample scan takes a reference scan plots the spectrum defines scan range from defines scan range to zero offset in % choices 0.25, 1 and 4 s automatic lamp off automatic lamp on integrator or recorder 1 V or 100 mV FW revision, errors or status local, remote, hpsystem checks the output voltage reset to default sample and reference diodes current locks certain parameters WL change on display polarity of signal (analog/GPIB) 0th order calibration
620
Table 150
User Control Functions # 21 22 Display 21:WL CALIBRATION 22:HOLMIUMCHECK Used for 656 nm calibration WL Calibration check
621
622
The functions 20, 21 and 22 are part of the User Functions, but they are described in this section.
Table 151
Service Control Functions # 20 21 22 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 Display 20:0th CALIB. 21:WL CALIBRATION 22:HOLMIUMCHECK 31:SET WL PARAM. 32:FIX SIGNAL 33:LEAK S. VOLT 34:VOLTAGE TEST 35:ADC NOISE 36:GRATING P.S. 37:FILTER P.S. 38:REMOTE TEST 39:FILTER CHECK 40:0TH TEST OFF 41:DAC TEST 42:PREAMP GAIN 43:EEROM TEST 44:DAC CALIB . 45:WL COMPENSATE Used for Zero Order calibration 656 nm calibration Wavelength Calibration check Parameter Set for Zero Order and 656 nm Fixed voltage to sample or reference path Shows leak sensor voltages Shows DC Voltages Check of ADC noise Check of Grating Sensor Check of Filter Sensor Check of Remote linesChecks movement of Filter Positions the Zero Order Beam Checks DAC Checks linearity of gains Checks EEROM data Calibrates the DAC Compensates non-lineraties of grating
C A UT I O N
Important parameters might be lost. DO NOT use control functions 31 through 45 until you have read this paragraph and fully understand the functions and result of operation. Some functions may change the monochrometer parameters and misuse of these functions leads to inaccurate wavelength setting.
623
Table 152
Control Function: Zero Order Calibration Key Operation Display 20:0th CALIB. ENTER ENTER or CLEAR nn step CHANGE? Description Select function. display current parameter or change to 200. to continue calibration or to abort. wait appr. 20 seconds. nn step x.xxxV starts the calibration scan from 150 step to 250step No key entry is allowed here. Possible error message at this point may be: CALIB. FAILURE DATA OVERFLOW Indicates that the lamp is OFF. Indicates that too much light reaches the sample photo diode. Reduce light and insert paper between cell and sample diode
624
Table 152
Control Function: Zero Order Calibration Key Operation Display DATA UNDERFLOW Description Indicates that not enough light reaches the sample photo diode. Check light path. The next line will be shown, if no error message occured. nn step y.yyyV ENTER ENTER CLEAR ENTER nnn step nnn step OK ? Displays the step that gave the maximum light intensity. Promps for confirmation, to change the parameter. Takes the displayed step number. Rejects the displayed step number. New parameter is written in EEROM and monochrometer is reset with new parameter. End of Zero order beam calibration. You may repeat the procedure again.
20:0th CALIB.
625
Wavelength Calibration
21:WL CALIBRATION This control function is used for the calibration of the monochrometer using the 656 nm line emission from the deuterium lamp. The step number appeared in this control function is the number of steps of stepper motor from the 0 order beam to the 656 nm emission line. Maximum light intensity is searched between 50 steps of 656 nm value. If the maximum peak is found, the step number is written into EEROM and corresponds to the value in 31:SET WL PARAM.
Table 153
Control Function: WL Calibration Key Operation Display 21:WL CALIBRATION ENTER 656nm xxxx step Description Select function. Displays the wavelength for calibration and steps based on present PARAM.WL 656. To continue calibration or to abort. Wait appr. 30 seconds. xxxxstep y.yyyV Starts the calibration scan from 656 nm 50 steps and seeks for maximum light intensity. No key entry is allowed here. Possible error message at this point may be: CALIB. FAILURE Indicates that there was no maximum found (see CALIB FAILURE on page 619). Indicates that not enough light reaches the sample photodiode (<30 mV). The next line will be shown, if no error message occured.
ENTER or CLEAR
DATA UNDERFLOW
626
Table 153
Control Function: WL Calibration Key Operation Display xxxxstep y.yyyV ENTER 656nm xxxx step Description Displays the step that gave the maximum light intensity. Displays the wavelength and step that gave the maximum light intensity. Displays the new parameter at 546 nm and prompts the confirmation. Takes the displayed step number. Rejects the displayed step 656 yyyystepOK New parameter is written in EEROM and monochrometer is reset with new parameter. End of calibration. You can repeat the procedure again.
after 2 seconds
656nm xxxxstep
after 2 seconds
21:WL CALIBRATION
627
Table 154
Control Function: HOLMIUMCHECK Key Operation Display 22:HOLMIUMCHECK ENTER CLEAR ENTER 360.8nm 418.5nm 536.4nm HOLMIUM CHECK OK CLEAR DOWN DOWN DOWN CLEAR 360.8nm 360.7nm 418.5nm 418.4nm 536.4nm 536.4nm 22:HOLMIUMCHECK CHECK? to leave function. to start the calibration check. automatic verification automatic verification automatic verification if within specification to leave function. displays measured value displays measured value displays measured value to leave function. Description Select function.
If this test was not successful, perform 20:0th CALIB. and 21:WL CALIBRATION.
628
SET WL Parameter
31:SET WL PARAM. This control function is used for the confirmation of monochrometer parameters or for changing them directly. PARM.WL0 is the number of steps of stepper motor from the position sensor, while PARM.WL656 is the number of steps from 0 order beam. As these values changes slightly from instrument to instrument, they are originally calibrated and written into EEROM. The parameter 360.8 nm, 418.5 nm, 486 nm and 536.4 nm cannot be changed. These four parameters set with 45:COMPENSATE are used to compensate non-linearity of the grating drive. If PARM.WL656 is changed, these four parameters are automatically shifted.
Table 155
Control Function: SET WL PARAM. Key Operation Display 31:SET WL PARAM. ENTER value found with 20:0th CALIB. . UP Parm. 656yyyy Select the parameter WL656 nm. Displays the step number at 656 nm (same value found with 21:WL CALIBRATION. Enter the parameter using numeric keys. UP UP UP UP Parm.360.8yyyy Parm.418.5yyyy Parm. 486 yyyy Parm.536.4yyyy Displays the step number at 360.8 nm. Displays the step number at 418.5 nm. Displays the step number at 486 nm. Displays the step number at 536.4 nm. Parm.WL0 200 Description Select function. Displays the 0 order light parameter (same
629
Table 155
Control Function: SET WL PARAM. Key Operation ENTER CLEAR Display 31:SET WL PARAM. Description Control function is displayed again. On WL0 or WL656 parameter, reenters the displyed value.
In order to change both parameters you have to repeat the above procedure for both wavelengths.
630
Fix Signal
32:FIX SIGNAL If the 1050 VWD shows noise or drift problems, this function can help to isolate the cause. The reference or the sample diode can be set to an fixed electrical value to remove influences from the light path. This function can also be used to retrieve the instrument profile of the instrument.
Table 156
Control Function: FIX SIGNAL Key Operation Display 32:FIX SIGNAL ENTER REF. CH. FIXED Description Select function. The photocurrent of reference photo diode is a fixed electrical value. Select the parameter. NORMAL-NOT FIXED Return to normal condition (neither photocurrrent is fixed.) The photocurrent of sample photo diode is a fixed value. Control function is displayed again.
DOWN or UP
N OT E
If either channel is fixed, the ERROR status lamp is blinking even after returning to analysis mode from service control mode. This is an alarm to show that the instrument is abnormal condition. You can return to normal condition by executing NORMAL-NOT FIXED or switching off the power.
631
Use this function for checking the noise of both sides separately; taking the instrument profile of both sides separately. With fixed signal, either the reference or the sample side is supplied with a constant current. So influences from the lamp effects only that side which is not fixed. Influence due to a drifting or defective photo diode effects both, a scan and the signal (noise). Small wavelength variations between fixed sample and reference scans are caused by the characteristics of the photo diodes. Noise with Reference Signal Fixed: If the noise is large, the problem may be caused by light path, flow cell or sample diode/pre-amplifier. Noise with Sample Signal Fixed: If the noise is large, the problem may be caused by light path, lamp or reference diode/pre-amplifier. To take an instrument profile proceed as follows: Enter 32:FIX SIGNAL and set SMP. CH. FIXED . Press [ENTER] and leave function. Press [BALANCE]. Take a reference scan 2:REF SCAN . Take a sample scan 1:SAMPLE SCAN . Set integrator to ATTN9, CS10 and Zero10%. Press [BALANCE]. Enter 3:SPECTRUM OUT , press [ENTER] [ENTER]. Start plot on integrator and press [ENTER]. The intensity profile is now plotted on the integrator. Perform above steps with REF. CH. FIXED to check the light through put of the cell. Figure 233 on page 633 shows both plots.
632
Figure 233
633
Table 157
Control Function: Leak Sensor Voltage Key Operation Display 33:LEAK S.VOLT ENTER LS:2.70 LL:3.30 Description Select function. Displays LS (Leak Sensor Voltage) and LL (Temperature compensation voltage). Error condition is when LS > LL. The normal ranges are: LS signal 2.35..2.85 V, LL signal 2.95..3.45 V Leaves function.
CLEAR
33:LEAK S.VOLT
634
Voltage Test
34:VOLTAGE TEST You can check some (but not all) voltages with this contol function.
Table 158
Control Function: Voltage Test Key Operation Display 34:VOLTAGE TEST ENTER DOWN or UP CLEAR 15.0 22.9 12.1 -15.0 34:VOLTAGE TEST Description Select function. Displays first set of voltages. Displays second set of voltages. Leaves function.
Table 159
DC Voltages Voltages + 12 V (1 V) - 15 V, + 15 V (1 V) + 24 V ( 4.8V) Used for filter and grating motor analog circuits leak sensor, fans
635
ADC Noise
35:ADC NOISE The output signal of the ADC noise corresponds to 196 AD counts at the Analog Output with 1 V full scale setting. The ADC noise must be within 10 counts (50 mV) over a time of 10 minutes (Figure 234).
Table 160
Control Function: ADC Noise Key Operation Display 35:ADC NOISE ENTER TESTING ADC Description Select function. ADC noise is outputted. Start plotter in ATTN 7, ZERO 50, Chartspeed 1 (on HP 339X) Leaves function.
35:ADC NOISE
636
Table 161
Control Function: Grating Photo Sensor Key Operation Display 36:GRATING P.S. ENTER STPxxx PS0.11 Description Select function. Present step of stepper motor and photo sensor voltage is displayed. You can move the stepper motor and observe the voltage. Starts automatically the search for the home position and displays the step number (nnn) and the corresponding voltage. Leaves function.
DOWN or UP
STPxxx PSy.yy
ENTER
STP-nnn PS3.90
CLEAR
36:GRATING P.S.
637
Table 162
Control Function: Filter Photo Sensor Key Operation Display 37:FILTER P.S. ENTER STP0 PS4.98 Description Select function. Move to home position and shows steps and photo sensor voltage. You can move the stepper motor and observe the voltage. When the motor leaves the photo sensor, then PS changes to 0.01. Leaves function.
DOWN or UP
STPxxx PSy.yy
37:FILTER P.S.
rotates the filter 1 step (7.5) to the left. rotates the filter 1 step (7.5 to the right.
638
Remote Test
38:REMOTE TEST This control function is to test the remote control line. Disconnect the remote cables to avoid interferrence to and from other instruments. Remote lines tested are: START, SHUT DOWN, POWER DOWN, READY and STOP. PREPARE and START REQUEST are not tested.
Table 163
Control Function: REMOTE Test Key Operation Display 38:REMOTE TEST ENTER START Description Select function.
Disconnect REMOTE Cable and Press START REMOTE LINE TEST REMOTE LINE OK REMOTE FAILURE The REMOTE LINE TEST starts. When test is passed. Theres a trouble. Leaves function.
CLEAR
38:REMOTE TEST
639
Filter Check
39:FILTER CHECK This control function is used to check the motion of second order cutoff filter. The cutoff filter returns to original position at the end of this control function.
Table 164
Control Function: Filter Test Key Operation Display 39:FILTER CHECK ENTER DOWN or UP CLEAR CUT FILTER OFF CUT FILTER ON 39:FILTER CHECK Description Select function. Displays present filter status. Cutoff Filter moves in or out. Leaves function.
640
Table 165
Control Function: Zero Order Test Key Operation Display 40:0TH TEST OFF Description Select function. The test is still off and the grating is on set parameter wavelength. ENTER 0th STEP NOnnn Take the number of steps from 31:SET WL PARM. , (default) or use 200 steps. The stepper motor is moved to zero order position. Leaves function and grating is turned to set wavelength.
ENTER CLEAR
641
DAC Test
41:DAC TEST This control function is used to check the D/A converter by setting different bits. An AC voltage is added to the DC output and should be < 0.8 x 10-5 AU.
Table 166
Control Function: DAC Test Key Operation Display 41:DAC TEST ENTER UP UP UP UP UP UP UP CLEAR TESTING BIT 0 TESTING BIT 1 TESTING BIT 2 TESTING BIT 3 TESTING BIT 4 TESTING BIT 5 TESTING BIT 6 TESTING BIT 7 41:DAC TEST Description Select function. Bit 0 is tested. Bit 1 is tested. Bit 2 is tested. Bit 3 is tested. Bit 4 is tested. Bit 5 is tested. Bit 6 is tested. Bit 7 is tested. Leaves function.
Table 167
DAC DC Values
Bit 0 1 2 3 4 5 6 7 mV 27 32 42 62 104 22 185 511 jump of 5 mV jump of 10 mV jump of 20 mV jump of 40 mV GND plus offset voltage jump of 80 mV about half of maximum output voltage Decription
If you do not see a linear response, replace the DCB board. 642 Service Handbook for 1050 Series of HPLC Modules - 11/2001
VWD: Diagnostic & Troubleshooting Information Service Control Functions An AC voltage is added to the DC output and should be < 0.8 x 10-5 AU. Figure 235 DAC Test Bit 0 (AC)
Figure 236
If one or more tested bits are out of limit, then perform 44:DAC CALIB.
643
Pre-amplifier Gain
42:PREAMP GAIN This control function allows the check of gain switching on the DCB. The gain can be switched to 1, 2, 4 and 8.
Table 168
Control Function: Pre-Amplifier Gain Key Operation Display Description Change wavelength to 500 nm to reduce intensity of light. 42:PREAMP GAIN ENTER G1 R0.115 S0.045 Select function. Shows the photocurrent of reference and sample side with gain 1. Shows the photocurrent of reference and sample side with gain 2. Shows the photocurrent of reference and sample side with gain 4. Shows the photocurrent of reference and sample side with gain 8. The displayed values should double each time. If not, change wavelength to 500 nm or change DCB.
DOWN
G2 R0.227 S0.089
DOWN
G4 R0.455 S0.179
DOWN
G8 R0.914 S0.358
CLEAR
42:PREAMP GAIN
Leaves function.
644
EEROM Test
43:EEROM TEST This control function checks the EEROM and is used as factory test.
Table 169
Control Function: EEROM Test Key Operation Display 43:EEROM TEST ENTER EEROM TEST****** EEROM TEST OK CLEAR 43:EEROM TEST Description Select function. The blinking * indicates the checked section. Test was successful. If test failes, replace DCB. Leaves function.
645
DAC Calibration
44:DAC CALIB. This control function does a scaling between lower 12 bits and upper 8 bits of DAC and an automatic recalibration of the DAC internal voltages. It should be performed when the noise is higher than expected and a DAC non-linearity is found. The test runs automatically. The initial calibration is done at the factory. The lamp can be off, but the instrument should be on for some time for stabilizing the instrument to reduce drift.
Table 170
Control Function: DAC Calibration Key Operation Display 44:DAC CALIB. ENTER START Disconnect SIGNAL Cable and Press START DAC SCALING SCALING 0 f0 yyyy Scaling starts. Step 0 of 7 is displayed. pre-scaling done for step 0. Now you steps 1 to 7 are done. DAC CALIB. OK ENTER 44:DAC CALIB. DAC CALIB.FAILED CLEAR 44:DAC CALIB. Calibration was successful. Takes new factors and leaves function. Calibration was not successful. Keeps previous factors when calibratio failed and leaves function. Description Select function.
646
Wavelength Compensation
45:WL COMPENSATE This control function is used to compensate non-lineratity of the grating drive. If the grating motor or the grating has been replaced or moved, this function MUST be executed. During this test, the flow cell should be empty (no windows) or clean filled with water or methanol (no air bubbles). Absorption in the flow cell causes an error. First step is to search for the 656 nm line emission of the deuterium lamp within a window of 50 steps. Then the processor sets the ideal (linear) steps for four interpolative points, 360.8 nm, 418.5 nm, 486 nm and 536.4 nm. 360.8 nm and 418.5 nm are absorption points of the holmium oxide spectra. 536.4 nm is a line emission from the deuterium lamp. Next, it scans each ideal interpolative point (25 steps) as reference. Then the holmium oxide filter is inserted and it scans again for the three absorption points of holmium oxide spectra (25 steps). If all found values are in limit, then the parameters are written into EEROM (visable with 31:SET WL PARAM.).
N OT E
Table 171
Control Function: WL Compenstation Key Operation Display 45:WL COMPENSATE ENTER ENTER CLEAR XXXstep y.yyyV CALIB. FINISHED PARAM. CHANGE ? to continue calibration to abort calibration displays steps and voltage during calibration new parameter, written into EEROM. Description Select function.
647
Table 171
Control Function: WL Compenstation Key Operation ENTER Display 45:WL COMPENSATE WL CALIB. FAILURE Description Takes new factors and leaves function. one or more peaks could not be found with 25 steps. Parameters are set to previous values. Keeps previous factors when calibration failed and leaves function.
CLEAR
45:WL COMPENSATE
648
29
29
N OT E
The information in this chapter is based on the original optical unit (version C). In June 1995 this optical was replaced by the enhanced version D to overcome baseline stability problems in unstable environments. For details on this D version refer to section Enhanced Optical Unit Information VWD: Enhanced Optical Unit Information on page 705.
Warnings
WA R N I N G Dangerous voltage is present in the cabinet, though it is covered and insulated. DO NOT TOUCH PARTS unless they are specified in the procedure. Be careful when you have to work in the optical unit. The lamp housing is hot. Be sure to wear a pair of safety or sun glasses. Since the deuterium lamp emits intensive ultraviolet light, it is dangerous to perform optical alignment without eye protection. Be careful not to expose your eyes directly to the light coming from the lamp.
650
651
Step 1: Replacement
Turn the lamp off. Loosen the two screws at the rear of the instrument which fix the cover and remove them. Remove top cover. Unplug the lamp and remove it. Exchange the lamp (no adjustment is required). Reconnect the lamp. Replace top cover. Turn the lamp on.
652
If CALIB. FAILURE occurs, press [CLEAR] to keep the old value and to leave function.
653
Step 3: WL CALIBRATION
The instrument scans for maximum light intensity of 656 nm line spectrum of deuterium lamp. Enter control function 21:WL CALIBRATION. [ENTER] 656nm 1900step [ENTER] or [CLEAR] 1875step 0.000V 1902step X.XXXV 656 1902stepOK? enters function displays the current parameter. to continue or to abort the instrument scans now for for maximum for 100 steps maximum when calibration successfully finished, press [ENTER] press [ENTER] to keep the new value and to leave function.
If CALIB. FAILURE occurs, press [CLEAR] to keep the old value and to leave function.
654
655
Figure 238
Flushing Procedure
Cleaning the cell (by using a glass syringe!) Flush with iso-Propanol. Flush with bidistilled water. Flush with nitric acid : water (5 : 95). Flush with bidistilled water. Flush with iso-Propanol C A UT I O N This concentration of nitric acide is dangerous and proper attention to safety should be given. Also, the nitric acid flushing procedure is not a certain cure for a dirty cell. It is to be used as a last attempt to salvage the cell before certain cell parts have to be replaced.
656
Leak Test
Remove the flow cell and connect the outlet tubing of the flow cell directly to the pump. Then flow an appropriate solvent (for example Isopropanol) at 10 ml/min. After several minutes check the cell visually. If it is necessary to check it for higher pressure, put an appropriate stainless steel tubing which can build up a back-pressure. C A UT I O N DO NOT apply higher back pressure to the flow cell than maximum pressure of the flow cell.
Table 172
Pressure Rating on Flow Cells Type Standard Flow Cell Ultra High-Pressure Cell Preparative Flow Cell Semi-Micro Flow Cell Pressure 40 bar 400 bar 40 bar 40 bar
657
658
Preparation for this procedure are: Remove the normal flow cell. Install the cuvette holder in the instrument and perform a wavelength calibration. Have cuvette with standard available.
Light path
Clear side
659
660
DCB Board
Note the parameters from 31:SET WL PARAM. Disconnect the power from the instrument. Remove main cover and disconnect all connectors from DCB. Replace DCB after loosening the 3 fixing screws. Fix all screws and reconnect all connectors to the DCB. Carefully remove the firmware ROM from removed DCB and insert it on new DCB. Replace main cover and turn the instrument ON. Turn lamp on and wait some minutes to stabilize the lamp. Perform functions 20:0th CALIB., 21:WL CALIBRATION, 44:DAC CALIB. and 45:COMPENSATE to input the detector specific parameters into the EEROM.
DCB Firmware
Disconnect the power from the instrument. Remove main cover. Carefully replace the firmware ROM. Replace main cover and turn the instrument ON. Turn lamp on and wait some minutes to stabilize the lamp.
661
662
663
Leak Interface
Carefully remove the leak interface. Replace the defective item. All three parts (top, bottom and tubing are coming together as kit). Install the leak interface. Figure 242 Leak Interface
664
WA R N I N G
Be sure to wear a pair of safety or sun glasses. Since the deuterium lamp emits intensive ultraviolet light, it is dangerous to perform optical alignment without eye protection. Be careful not to expose your eyes directly to the light coming from the lamp.
665
Figure 243
Optical Unit
667
Figure 244
Location of Photodiodes
Sample
Reference
668
Grating Motor For [ ] items refer to Figure 245 on page 669. Refer to Removing the Optical Unit on page 666. Refer to Replacing Grating Assembly Parts on page 668 and take grating out. Remove the bottom plate of the optical unit. Remove the two springs. Unscrew the three screws [6] that fix the motor assembly [5] and take it out. Keep spring [3] and gasket [4]. Replace the spring [3], gasket [4] and complete motor assembly [5]. Reinstall the grating [1]. Refer to Optical Alignment Procedures on page 671. Figure 245 Grating Assembly
669
670
WA R N I N G
Be sure to wear a pair of safety or sun glasses. Since the deuterium lamp emits intensive ultraviolet light, it is dangerous to perform optical alignment without eye protection. Be careful not to expose your eyes directly to the light coming from the lamp.
671
672
VWD: Maintenance Information Optical Alignment Procedures Excute control function 40:0TH TEST OFF to set the grating motor position to 200 steps (center step number). Adjust the direction of the grating mirror [7] so that the light beam covers over the mirror M4 [6]. Remove the beam splitter [8] now so that you can see the center of the flow cell. Adjust the angle and direction of the mirror M4 [6] so that the light beam illuminates the center of the flow cell. Leave control function 40:0TH TEST OFF and return to normal display. Excute the 20:0th CALIB. and 21:WL CALIBRATION. Refer to Replacement of Deuterium Lamp on page 652, Step 2 and 3. If grating has been moved, use 45:COMPENSATE to compensate non-linearity of the grating motor. Set wavelength to 254nm. Place cover on optical unit (do not fix the screws at this time). M4 fine tuning Excute control function 16:PHOTOCURRENT. Remove the blank screw for mirror M4 adjustment (Figure 243 on page 666) on the top cover (leave the blank screw for beam splitter adjustment in). Adjust the angle of the mirror M4 with inserting a hexagon wrench (1.5 mm) through the top cover screw hole to get maximum photocurrent for the sample. Turn right to move image down and left for up. Replace the blank screw in the top cover. Excute the 20:0th CALIB. and 21:WL CALIBRATION. Refer to Replacement of Deuterium Lamp on page 652, Step 2 and 3. Install the beam splitter [8].
673
674
Table 173
Cleanable Optical Parts NOT CLEANABLE grating and all mirrors Touching or cleaning will result in decrease of reflaction/intensity CLEANABLE filters (holmium, cutoff and 0 order calibration), beam splitter, photo diodes You can wipe the surface with ethanol. In case you cannot remove stains, the part has to be replaced.
675
Upgrade to GPIB
Note the values for WL, 0 and 656 nm using 31:SET WL PARAM., just in case the EEROM looses the values. Turn off the instrument. Remove top cover of the instrument. Remove plate at the rear panel above the fan. Install the GPIB board in that location using the screws that hold the plate. Connect the GPIB cable to J12 of the DCB board. GPIB Address Setting The GPIB address setting is done with a switch (1) at the rear of the GPIB board. The factory setting is 10 (position A). Figure 248 Location of GPIB board
676
Performance Verification
Table 174
Noise and Drift Specifications Noise Drift 1.5 x 10-5 AU 5.0 x 10-4 AU/h
Preparations
Prime the pump and ensure there are no air bubbles in the system. Thoroughly degas about 300 ml of bidistilled water. Set pump to deliver bidstilled water at a flow rate of 1 ml/min. Set the attenuation to about 35 cm/mV. Set run time on recorder to 6.0 min. Turn-ON line power and deuterium lamp. Set wavelength to 254 nm, response time to 1 second and output voltage to 1 V.
677
Starting a run
Give the optical unit time to warm-up and stabilize. Start a run. The baseline noise should not exceed 7.5 V (1.5 x 10-5 AU|) equivalent to 4.5 mm at attenuation - 3 on a 3390/2/3 integrator and equivalent to 9 mm at attenuation - 3 on a 3394/6 integrator. Figure 249 Example of Noise Plot
This plot was taken with a 79853C VWD an 35900C A/D converter a LC DOS workstation flow cell windows removed, but gasket #2 installed. It shows, that the drift on this example is < 1 x 10-4 AU/hr and the noise at about < 1 x 10-5 AU.
678
Scaling Factors
The table below shows the scaling factors for the 339XA family of integrators. The 3390A, 3392A and 3393A have a full scale deflection of 75 mm. The 3394A and the 3396A have a full scale deflection of 150 mm, they also have an attenuation range between -8 and 36.
Table 175
Scaling Factors on 339X integrators ATTN -3 -2 -1 0 1 2 3 4 5 6 7 8 9 10 mV full scale 0.125 0.25 0.5 1 2 4 8 16 32 64 128 256 512 1024 mAU full scale 0.25 0.5 1 2 4 8 16 32 64 128 256 512 1024 2048
679
680
30
30
This chapter gives diagrams for parts identification and the complete parts listings respectively. Overall Diagram Optical Unit Flowcell Flow Cell Kits Accessory Kit N OT E The information in this chapter is based on the original optical unit (version C). In June 1995 this optical was replaced by the enhanced version D to overcome baseline stability problems in unstable environments. For details on this D version refer to section Enhanced Optical Unit Information VWD: Enhanced Optical Unit Information on page 705.
682
Overall Diagram
Table 176
Item Description
Overall Diagram
Part Nmber Item Description Part Nmber
1 Power Supply (5061-3375) 2 DCB Board Assembly, see * 2 ROM DCB Firmware C only 2 ROM DCB Firmware D only
15 Cover Assembly 16 GPIB Board Assembly 16 ROM GPIB Firmware Cable DCB-GPIB 17 Fan Assembly (LOW) 18 Cover Fan 19 Sheet Fan 20 Fan Assembly (HIGH) 21 Switch Bearing 22 Switch Bracket 23 Switch Shaft 24 Switch Top 25 Cable DCB-KDI 26 Optical Unit
79853-64101 79853-68711 79853-13004 79853-61610 79853-68503 79853-04102 N.A. 79853-68502 79853-61903 N.A. 79853-61901 79853-61902 79853-61609 see page 688
3 PSC Board for DCB 79853-66511 79853-66512 4 Cable PSC-DCB 5 Cover PSC 6 Leak Sensor Board 7 Leak Sensor Assembly 8 Sheet Front Panel 9 Front Panel Assembly 10 Display Interface (KDI) 11 Display Module (VFD) 12 Cable KDI-VFD 13 STD Flow Cell Assembly 13 Semi-micro Flow Cell Assembly 13 Ultra High Pressure Flow Cell Assembly 13 Prep Flow Cell Assembly TI 14 Bracket DPS
*
79853-61605 N.A. see page 687 see page 687 see page 687 see page 687 79853-66502 79853-66503 79853-61602 see page 693 see page 695 see page 697 see page 698 N.A.
Transport Screw Kit, contains 3 screws with washer and spacer PEEK Inlet Tubing Kit PEEK Waste Tubing Kit
If installed in instruments with PSC -66509, then PSC must be updated to 79853-66512.
683
Figure 250
684
Figure 251
685
Top
Tubing
Bottom
686
Font Panel
Table 178 Front Panel # Description Front Panel Complete Front Panel 1 Leak Sensor Board 2 Leak Sensor Assembly 3 Display Module Board (VFD) 4 Cable KDI-VFD 5 Display Interface (KDI) 6 Cable DCB-KDI O-ring, Leak Assembly Figure 253 Front Panel Part number 79853-60203 79853-60202 79853-66510 79853-66111 79853-66503 79853-61602 79853-66502 79853-61609 79853-82501
687
Optical Unit C
The parts identification of the optical unit is splitted into four sections: Optical Unit Inner Parts (Top) Optical Unit Inner Parts (Bottom) Grating Assembly Filter Assembly Flow Cell Assemblies N OT E The information in this chapter is based on the original optical unit (version C). In June 1995 this optical was replaced by the enhanced version D to overcome baseline stability problems in unstable environments. For details on this D version refer to section Enhanced Optical Unit Information VWD: Enhanced Optical Unit Information on page 705. For complete optical unit C replacements use part number 79853-60015. This upgrades to D version, see Part Numbers for Enhanced D Optical Unit on page 709
688
Optical Unit (complete assembly) 79853-69015 Plate Optical Top 1 Deuterium Lamp Assembly Lamp housing 2 Filter Assembly 3 Entrance Slit Assembly 4 Mirror #1 5 Mirror #2 6 Mirror #3 or #4 Figure 254 79853-04108 79883-60002 79853-22006 see page 692 79853-23103 79853-68107 79853-68108 79853-68109 Optical Unit C Inner Parts TOP
7 Grating Assembly 8 Beam Splitter 9 Pre-Amplifier Board, SAMPLE 10 Sensor, Sample 11 Pre-Amplifier Board, REF 12 Sensor, Reference Reference Slit Spacer Reference Sensor PTFE Ring 53C
see page 691 79853-20402 79853-66507 79853-61109 79853-66508 79853-61110 79853-23104 79853-24702 79853-24500
689
Optical Unit (comple assembly) Plate Optical Base 1 Optical Body 2 Plate Sample Sensor 3 Position Sensor Assembly, Grating 4 Plate Reference Sensor 5 Spring #1, Grating 6 Grating Assembly Figure 255
79853-60015 79853-04109 N/A 79853-04110 79853-61106 79853-04111 79853-29102 see page 691
7 Filter Assembly
7 Position Sensor Assembly, Filter 79853-61107 8 Cable Assembly, Sample 9 Cable Assembly, Reference Spacer, Optical (metal foot) Insulator, Optical (rubber foot) Foot Kit Optical 79853-61607 79853-61608 79853-24701 79853-85401 79853-22005
690
Grating Assembly
Table 181
Grating Assembly # 1 Description Grating Hex Screw M3 14 mm lg 2 3 4 5 Spring #2, Grating Gasket Grating Motor Assembly Screws M3 6 mm long Photo Sensor 79853-61106 79853-64606 79853-29103 Part number 79853-64605
Figure 256
Grating Assembly
691
Filter Assembly
Table 182
Filter Assembly # Description 1 Filter Assembly 2 Lever Position Sensor 3 Position Sensor Filter 4 Screws M3 6 mm long 79853-61107 Part number 79853-67903
Figure 257
Filter Assembly
692
Table 183
Standard Flow Cell C (SST/Ti) Item 1 2 3 4 5 6 7 Description Cell Screw Conical Spring 10/pk Ring 2/pk Gasket #1 PTFE Window Quartz Gasket #2 PTFE Gasket #3 PTFE STD Flow Cell 8 mm SST STD Flow Cell 8 mm Ti PEEK Inlet Tubing Kit Cell Kit STD, includes items 4 (2x), 5 (2x), 6 (1x) and 7 (1x) 5 4 6 7 Window Quartz Kit Gasket #1 PTFE Kit STD 10/pk Gasket #2 PTFE Kit STD 5/pk Gasket #3 PTFE Kit STD 5/pk see Note below 79853-60011 5062-8522 79853-68718 79853-68719 79853-68720 79853-68721 79853-68722 2 10 5 5 Part Nmber 79853-27201 79853-27203 79853-27202 10 2 Qty
N OT E
The original STD flow cell 79853-60008 was replaced in June 1995 by the D version 79853-60000. For parts ID refer to Standard Flow Cell D Repair Parts on page 710.
693
Figure 258
694
Table 184
Semi-Micro Flow Cell (SST/Ti) Item Description 1 Cell Screw (same as STD) 2 Conical Spring (same as STD) 3 Ring (same as STD) 4 Gasket #1 PTFE (same as STD) 10/pk 5 Window Quartz (same as STD) 6 Gasket #2 PTFE Micro Semi-Micro Flow Cell (complete) PEEK Capillary 400 mm lg ID 0.12 mm Fitting for PEEK capillary Part Nmber 79853-27201 79853-27203 79853-27202 79853-68720 79853-68719 79853-68724 79853-60010 5021-1823 0100-1516 2/pk 10/pk 2/pk 10/pk 2/pk 10/pk Qty
Cell Kit Micro, includes items 4 (2x), 5 (2x) and 79853-68723 6 (2x) Figure 259 Semi-Micro Flow Cell (SST)
695
Table 185
High Pressure Flow Cell (SST) Item Description 1 Cell Screw (same as STD) 2 Ring POLYIMIDE 3 Window Quartz 4 Gasket #1 POLYIMIDE 5 Gasket #2 POLYIMIDE High Pressure Flow Cell SST 79853-68740 79853-68729 79853-68730 replaced by UHP Cell, see Ultra High Pressure Flow Cell (SST) on page 697 5062-8522 2/pk 10/pk 5/pk Part Nmber 79853-27201 Qty
Cell Kit HP, includes items 2 (2x), 3 (2x), 4 (2x) 79853-68728 and 5 (1x)
N OT E
The gaskets, windows and rings are not compatible with the Ultra High Pressure Cell (79853-600013) that replaced the high pressure flow cell (79853-60009). For parts identification refer to Ultra High Pressure Flow Cell (SST) on page 697.
696
Table 186
Ultra High Pressure Flow Cell (SST) Item Description 1 Cell Screw 2 Ring PEEK UHP 3 Window Quartz Kit, UHP 4 Gasket #1 POLYIMIDE Kit UHP 5 Gasket #2 POLYIMIDE Kit UHP Ultra High Pressure Flow Cell SST PEEK Tubing Assembly Cell Kit UHP, includes items 2 (1x), 3 (2x), 4 (2x) and 5 (2x) 79853-68734 79853-68737 79853-68738 79853-60013 5062-8522 79853-68733 2/pk 2/pk 2/pk Part Nmber 79853-27200 Qty
Figure 260
697
Table 187
Preparative Flow Cell (Titanium) Item Description 1 2 3 4 5 6 6 6 6 7 8 Cell Screw (same as STD) Conical Spring (same as STD) Ring (same as STD) Gasket #1 PTFE (same as STD) Window #1 Quartz (same as STD) Gasket #2 PTFE (0.1) for 0.9 l Gasket #2 PTFE (0.2) for 1.8 l Gasket #2 PTFE (0.5) for 4.4 l Gasket #2 PTFE (1.0) for 8.8 l Window #2 Quartz Gasket #3 PTFE Preparative Flow Cell (complete) PEEK Tubing Assembly Cell Kit PREP, includes items 4 (1x), 5 (1x), 6 (1 of each size), 7 (1x) and 8 (1x) 79853-60012 5062-8522 79853-68725 Part Nmber 79853-27201 79853-27203 79853-27202 79853-68720 79853-68719 10/pk 2/pk 10/pk 2/pk Qty
Window Quartz Kit PREP includes items 5 (1x), 79853-68726 7 (1x) Gasket Kit PREP includes one of each size of gasket #2 79853-68727
698
Figure 261
699
Cuvette Holder
Table 188
Control Module Parts Item Description Cuvette Holder Part Number 79853-60016
For informationon the use of the cuvette holder, refer to Using the Cuvette Holder on page 658. Figure 262 Cuvette Holder
700
Accessories
These parts are shipped with the 79853C VWD
Table 189
Accessories Description Manual Getting Ready Cable Remote PEEK Waste Accessory Kit Standard Accessory Kit includes Fitting Fuse 250 V 2A Fuse 250 V 3A Wrench 1/4-5/16 inch Screwdriver POZI 1 PT 3 Leak Interface Kit Manual SOP 0100-1516 2110-0002 2110-0003 8710-0510 8710-0899 79853-68731 79853-90009 1 3 3 1 1 1 1 Part number 01050-90211 5061-3378 5062-8535 79853-68701 QTY 1 1 1 1
701
Screws
Below table lists all screws within the instrument. They can be bought locally, if needed.
Table 190
Screws Location filter motor grating motor mirror adjustment grating adjustment grating motor Size Length Type hexagon socket set screw with cup point hexagon socket set screw with cup point hexagon socket set screw with dog point
M 2.3 4 mm lg M3 M3 M3 M3 3 mm lg 8 mm lg
to fix assemblies on the optical body; cover on M 3 the DCB board; plate of lamp house; KDI and VFD board; mirrors, filter and grating; position sensor REF sensor plate SAMP and REF amplifier boards cover assembly; optical unit top cover; DCB and GPIB boards from rear panel; M3 M3 M3 M4
6 mm lg
to fix assemblies on the base; DCB abd GPIB M 4 board; leak detector assembly; front panel bracket; SAMP and REF covers; optical unit bottom cover; blank screws of optical unit top cover; plate for cell on the optical body; blank plate of cell; lock screws M4
12 mm lg screw
702
Table 190
Screws Location lamp house fan assemblies cell All screws are plus-shaped type. Size M4 M4 M5 Length Type
703
704
31
31
Since June 1995, the design of the optical unit for the 79853C Variable Wavelength Detector (VWD) was changed to improve its performance under unstable temperature conditions. Together with the enhanced optical unit (D), the standard flow cell was changed (79853-60000). N OT E In this document the term D is used for the new enhanced optical design and C for the original optical design.
Compatibility
This new enhanced optical unit (D) is fully backward compatible with all 79853C VWDs shipped since January 1992. The new standard flow cell (79853-60000) is backward compatible with the C optical unit. Some of the parts for the enhanced optical unit (D) are not usable in the C version. In case of replacing a C optical unit with an enhanced D optical unit, the new standard flow cell is required.
706
Introduction
To overcome wander problems due to temperature variations of the lab environment, the optical unit of the 79853C Variable Wavelength Detector (VWD) has been modified. Following hardware modifications were implemented in June 1995: different coupling of the lamp housing (lens between lamp housing and optical casting). area around mirror M1 and M2 has been redesigned to eliminate one mirror - result is a mirror #1 assembly with a plane mirror. redesigned entrance slit holder. Slits are changeable (standard/test). beam splitter assembly no longer vertically adjustable. reference slit assembly redesigned for better optimization. new standard flow cell with different aperture material and different inlet capillary. Figure 263 Optical Path of Enhanced Optical Unit
new lens assembly new entrance slit assembly new mirror #1 assembly
707
Support Considerations
Prefix Change
The enhanced Optical Unit (D version) was introduced in production units in June 1995. Since the detector appears to look the same as before, a prefix change was made. All units with prefix 3522 J 04305 and above have the new optical installed. N OT E Some units with a prefix lower than 3522 J 04305 have been installed on customer sites prior to the official shipments.
Identification
Following identifications for the enhanced D version are available: Prefix and serial number 3522 J 04305 and above (rear of instrument) firmware revision 4.31 (press CTRL 12 ENTER ENTER DOWN) label on the optical unit ENHANCED ILLUMINATION SYSTEM handle of new reference slit looking out of the opticals cover plate (see Figure 266 on page 715).
Compatibility Matrix
Due to a redesign, several components are usable in the enhanced D version only. Refer to Table 191 on page 709 for details. N OT E Both optical unit versions (C and D) can be operated with firmware revision 4.24 (79853-13005). Due to the modifications, the photocurrent readings are about 50% of those of the original C opticals. To make them comparable the firmware for the enhanced D version got a new revision and part number.
708
VWD: Enhanced Optical Unit Information Part Numbers for Enhanced D Optical Unit
Table 191
Part Number 79853-60000 79853-69014 79853-69015
for D only, includes test slit backward compatible**, includes test slit for D only, includes test slit for D only, includes test slit from C used for SAMPLE and REFERENCE on D from C used for SAMPLE and REFERENCE on D same part number as before, but test slit added for D only, added also to 79853-69014/15 and 79853-69511 (DCB) Test slit plus STD slit
with C version optical units with C version optical units; part number 79853-68109 should only be used for 79853C optical until stock has expired.
N OT E
The part numbers 79853-68110, -68111, -68112, -68113 and -64605 include beside the test slit in addition a seal to close the hole for Mirror 4 adjustment setscrew. Close the hole with this seal during replacements (see Figure 266 on page 715 for the location).
709
VWD: Enhanced Optical Unit Information Standard Flow Cell D Repair Parts
Table 192
Figure 264
6 7 5 4 3 2 1
710
Tools required:
Test Slit (supplied with mirror or grating assembly) Pozi Driv PT1 hexagonal wrench (1.5 mm) hexagonal wrench (2.5 mm) pair of tweezers (not too sharp points)
Pre-requisites:
Assure that the flow cell is clean, flushed with water and bubble free. Remove detector from system. Place the detector on a bench. Remove the main cover.
711
Additional Information
For additional information about replacements and the use of the Service control Functions refer to VWD: Maintenance Information on page 649 and Service Control Functions on page 622.
WA R N I N G
Do not remove the Entrance Slit Holder nor loosen it. Otherwise the optical unit has to be exchanged completely.
N OT E
The photocurrent readings with test slit installed are much lower than with the standard slit.
712
entrance slit
713
5 Carefully insert the test slit (with round hole) into the entrance slit holder. The slit must sit flat on the holder with the white side towards the incoming light.
714
715
reference image
716
8 Install new mirror #3 or #4 assembly. 9 Position the white image precisely onto the reference slit: - horizontally by rotating the mirror, - vertically using the setscrew of the mirror 10 Carefully replace the cover of the optical unit. Take care for the reference aperture handle. 11 De-activate CTRL 40: 0TH TEST OFF, press CLEAR, CLEAR and BALANCE. 12 Set =250 nm. 13 Activate CTRL 16: PHOTOCURRENT. 14 Optimize the sample readings using the setscrew of mirror #4 through the hole in the optical unit cover, see Figure 266 on page 715. 15 Optimize the reference readings with the reference aperture, see Optimizing the Reference Readings on page 725. 16 Install the standard slit and perform electronic calibrations, see Installing the Standard Slit on page 726.
717
VWD: Enhanced Optical Unit Information Replacing the Grating or Grating Motor
11 Activate service function CTRL 40: 0TH TEST ON. 12 Turn the grating so that the center of the image is on the reference slit (a small horizontal and vertical deviation can be accepted). 13 Fix the grating with the setscrew. 14 De-activate and re-activate CTRL 40: 0TH TEST and check the position of the image on the reference slit. If not correct, loosen the grating and repeat steps 12 to 14.
718
VWD: Enhanced Optical Unit Information Replacing the Grating or Grating Motor
15 Do a vertical adjustment with Mirror #4 for precise vertical fit of image on reference slit, using the setscrew of mirror #4 through the hole in the optical unit cover, see Figure 266 on page 715. 16 Carefully replace the cover of the optical unit. Take care for the reference aperture handle. 17 De-activate CTRL 40: 0TH TEST OFF, press [CLEAR], [CLEAR] and [BALANCE]. 18 Execute CTRL 20: 0th CALIB. 19 Activate CTRL 40: 0TH TEST ON and readjust the Beam Splitter for ideal horizontal fit. 20 De-activate CTRL 40: 0TH TEST OFF. 21 Set =250 nm. 22 Activate CTRL 16: PHOTOCURRENT. 23 Optimize the sample readings, using the setscrew of mirror #4 through the hole in the optical unit cover, see Figure 266 on page 715. 24 Unlock the reference aperture, see Unlocking the Reference Aperture on page 723. 25 Optimize the reference readings with the reference slit, see Optimizing the Reference Readings on page 725. 26 Install the standard slit and perform electronic calibrations, see Installing the Standard Slit on page 726.
719
720
N OT E
For easier repositioning the lens ring is marked with color paint, see Figure 269 on page 722. The position of the marker could differ from instrument to instrument and may be different to the position shown in the figure. 5 Remove, clean or replace the lens. If reusing old lens use markings for repositioning.
721
Figure 269
Lens Position
marker
lens assembly
N OT E
The more plane lens side with smaller aperture faces towards the lamp.
N OT E
If a new lens is installed, mirror #1 assembly has to be realigned after this procedure, see Replacing Mirror #1 Assembly on page 715. 6 Reassemble the flat spring. 7 Replace the Lamp housing and tighten it. 8 Reassemble the detector.
722
723
4 Replace the reference pre-amplifier cover (to prevent stray light). 5 Fit the front panel with one screw at the right of the mainframe. 6 Turn on the detector and the lamp 7 Set wavelength to 250 nm. 8 Return to your replacement procedure.
724
725
test slit
3 Carefully insert the standard slit into the entrance slit holder. The slit must sit plane on the holder. 4 Carefully replace the cover of the optical unit. Take care for the reference aperture handle, see Figure 266 on page 715. 5 Execute CTRL 20: 0th CALIB. 6 Execute CTRL 21:
l CALIBRATION.
726
32
32
Since the introduction of the 79853C Variable Wavelength Detector in 1991, the following hardware and firmware changes have been implemented.
728
Product History
Since introduction of the 79853C Variable Wavelength Detector in January 1992 following changes have been implemented.
Prefix Changes
Table 193 Prefix Changes Serial Number 3145 J 00101 3152 J 00263 Changes Start of customer shipments Additional Information ∅
New amplification factor of reference See Modified side due to high output of new DAD Pre-Amplifier Gain on lamps. page 734. Introduction of DCB firmware revision See SN 01050-055 on 4.22 page 734. Introduction of DCB firmware revision See SN 01050-055 on 4.23 page 734. Introduction of DCB firmware revision See SN 01050-055 on 4.24 page 734. Introduction of PTFE ring in optical unit See SN 01050-068 on page 734.
Volume changes on Preparative Flow See Table 138 on page Cell in September 1992 574 and Table 187 on page 698. 3225 J 02011 3323 J 03117 3334 J 03255 Introduction of new DCB/PSC boards See SN 01050-072 on page 734. Introduction of new lamp housing Change of manufacturing process for to improve stability photo diodes mounting against humidity Ultra High Pressure cell replaced High Pressure Cell in 1993
729
Table 193
Prefix Changes Serial Number 3522 J 04305 Changes Enhanced optical unit D with STD flow cell D in June 1995 Additional Information to improve temperature stability, see VWD: Enhanced Optical Unit Information on page 705
730
Table 194
DCB ROM Firmware Revisions Revision Major Changes 4.08 Comments Used for first internal Waldbronn/Avondale units and some demo units. PHOENIX problem: wont stop when running with A/D Concerter (for example ABORT). CTRL 45 COMPENSATE bug fix, calibrated wavelength deviation might exceed the specification. CTRL 22 HOLMIUMCHECK for GLP reasons added. New algorithm for CTRL 45 COMPENSATE and CTRL 22 HOLMIUMCHECK. Not released.Used for internal Waldbronn/Avondale tests. Released for 79853C in January 1992. For replacements use part number 79853-13005 (4.24). NEEDS GPIB ROM version 0.20 or above (79853-13004) Released for 79853C in March 1992. Started with serial number 3152J00489. For replacements use part number 79853-13005 (4.24). NEEDS GPIB ROM version 0.20 or above (79853-13004) Released for 79853C in April 1992. Started with serial number 3217J00603. For replacements use part number 79853-13005 (4.24). NEEDS GPIB ROM version 0.20 or above (79853-13004)
4.09
4.21
4.22
4.23
Removed bug: Incorrect wavelength setting during stepper motor intialisation bewteen 536.4 nm and 600 nm.
731
Table 194
Removed bug : EEROM DATA LOST1 Released for 79853C in June 1992. Removed bug : Wavelength accuracy Started with serial number between 360 nm and 486 nm 3225J00773. For replacements use part number 79853-13005 (4.24). NEEDS GPIB ROM version 0.20 or above (79853-13004) For Enhanced Optical Unit D only Released for 79853C in June 1995. Started with serial number 3522J04305. For replacements use part number 79853-13000 (4.31). NEEDS GPIB ROM version 0.20 or above (79853-13004)
4.31
732
Table 195
GPIB ROM Revisions Revision Major Changes 0.04 0.05 LC APPACK problem: BUFFER OVERFLOW message preventing run buffer overflow. Comments First official realease for 79853A. Released for 79853A.
0.08
Also useable for 79853C. PHOENIX Released for 79853A and 79853C. problem: prevents hang-ups at power For replacements use part number on (if VWD is switched on after 79853-13004 (0.2X) PHOENIX has been switched on). PHOENIX problem: prevents VECTRA 486 hang-ups. additional changes for future PHOENIX enhancements. NOT officially released. Released for 79853A and 79853C in January 1992. Required for 79853C firmware revision 4.21 and above. For replacements use part number 79853-13004 (0.2X)
0.09 0.20
733
734
In This Book This manual contains technical information about the Agilent 1050 liquid chromatographs. This manual is available as electronic version (Adobe Acrobat Reader file) only.