Professional Documents
Culture Documents
DL50/DL53/DL55/DL58
Titrators
1. Introduction
2. Setup
3. Methods
4. Sample data memory
5. Analysis
6. Auxiliary functions
7. DL58
8. Symbols and explanations
9. Error messages and malfunctions
10. Installation and maintenance
11. Accessories
12. Technical data
13. Index
14. Data sheet
15. ISO certificate, System validation
Introduction
1.
Introduction
In contrast to the Quick Guide, this Reference Handbook provides a complete description of
the operating principles of the DL50, DL53, DL55 and DL58 Titrators. Its layout has been kept
modular to ensure future supplementation or replacement of individual sections or pages; new
texts carry the date of issue in the footer on every page.
Safety notes
Measures for your personal protection and for operational safety are described in Section 2
of the Quick Guide. We strongly advise you to read these. The symbols listed there also appear
for texts in this Reference Handbook which require safety measures.
Keywords used
appears before all texts which refer to an error in the measured value acquiNOTICE
sition, data storage etc.
Note
Index
The index in Section 13 comprises key words from the Quick Guide and the Reference
Handbook.
Software version
The Reference Handbook applies to software version 2.x for all four titrators.
Note:
The following pages provide an overview of the menus and commands which are available
under the menu and auxiliary function keys.
FCC rules
This equipment has been tested and found to comply with the limits for a Class A digital device, pursuant to both
Part 15 of the FCC Rules and the radio interference regulations of the Canadian Department of Communications.
These limits are designed to provide reasonable protection against harmful interference when the equipment is
operated in a commercial environment. This equipment generates, uses and can radiate radio frequency energy
and, if not installed and used in accordance with the instruction manual, may cause harmful interference to radio
communications. Operation of this equipment in a residential area is like to cause harmful interference in which
case the user will be required to correct the interference at his own expense.
08/2004
1-1
Menus: Overview
Method
Setup
Resources
SETUP
Titrants
Sensors
Temperature sensors
Print
0.1 mol/L
0.1 mol/L
0.1 mol/L
Delete
SETUP
Modify
Titrant parameters
Name
NaOH
Concentration [mol/L] 0.1
Titer
1
Esc
Modify
OK
SETUP
Method:
OK
OK
Standard methods
Equivalence point titr'n
End point titration (EP)
Titer by EQP titration
Esc
Print
Add
METHOD
Modify
Titrants
NaOH
HCl
HClO4
Esc
Methods
Method ID
Standard methods
User methods
METTLER methods
Title
Sample
Stir
Esc
METHOD
Modify
METHOD
Modify
Titrant names
HCl
HClO4
AgNO3
EDTA
Esc
SETUP
OK
Method ID
00001
Title Equivalence point titr'n
Date/time 00-00-0000 00:00
Esc
Titrant parameters
SETUP
Method: 00001
Title
METHOD
Name
HClO4
Concentration [mol/L] 0.1
Titer
1
Esc
Modify
OK
Title
Sample
Stir
Esc
Method ID
00001
Standard methods
User methods
Delete
Print
OK
METHOD
Modify
Methods
1-2
OK
OK
METHOD
Modify
08/2004
Menus: Overview
Sample
No.
Status
Wt/vol.
Run
Meth.
Samples to be analyzed
ID
Number of samples
Method ID
User
RUN
1
00001
Start
Add
Add
SAMPLE
Esc
OK
Sample entry
SAMPLE
Number of samples
Method ID
2
00001
User
Esc
Defined are
Stirrer 1: Stand 1
Sensor 1: DM141
Drive 2: 0.1 mol/L AgNO3
Esc
Print
Current sample
Sample No. 2
SAMPLE
Sample ID
Weight [g]
1.36712
Limits [g]
0.02 2.0
Correction factor f
Esc
Balance1) OK
Stir function
Wt/Vol.
1.19831
1.36712
Meth.
00001
00001
OK
RUN
No. 1 of 1
Sample ID
Method ID
00001
OK
RUN
30
80
Hold2)
mV
ID
RUN
Balance1)
OK
Status
ready
ready
OK
Sample No. 1
Sample ID
Weight [g]
1.23452
Limits [g]
0.02 - 2.0
Correction factor f 1.0
Sample No. 1
SAMPLE
Sample ID
Weight [g]
1.19831
Limits [g]
0.02 2.0
Correction factor f
Esc
Balance1) OK
No.
1
2
RUN
E V curve
mL
Delete
Modify
1)
2)
Add
Table
Result list
Method: 00001
Sample 1
R1
= 29.26 %
Values
Curve2)
Hold2)
RUN
OK
08/2004
1-3
Stirrer
Sensor
Sensor
SENSOR
Measure potential
Measure temperature
Calibrate temperature sensors
Stirrer
Titration stand
Speed [%]
STIRRER
Stand 1
50
Modify
OK
Measure potential
Sensor
Unit of meas.
Titration stand
Esc
SENSOR
DG111
mV
Stand 1
Stirrer
Titration stand
Speed [%]
Start
STIRRER
Stand 1
50
Modify
Measured values
Stop
Start
SENSOR
43.7 mV
Stop
Burette
Changer
Sample changer
CHANGER
Burette
BURETTE
Rinse burette
Rinse tip
Dispense
OK
OK
Change lift position
Lift position
Esc
CHANGER
Burette drive
bottom
Modify
Rinse burette
Start
CHANGER
Esc
Drive 2
Modify1)
Rinse burette
Burette drive
bottom
BURETTE
BURETTE
Drive 2
Stop
Stop
1)
1-4
Start
08/2004
Results
Report
Results2)
RESULTS
Report3)
REPORT
Output
Printer
Results
All results
No
Yes
Modify
OK
Result list
Method: 00001
Sample 1
R1 = 29.26 %
Sample 2
RESULTS
Report
Start
REPORT
OK
2)
Misc.
3)
Data
Transfer
...
Miscellaneous
MISC.
Data transfer
DATA TRANSFER
Memory card
Computer4)
Remote control4)
OK
OK
Titrator settings
Date/time format
Date/time
Language
Esc
MISC.
Formats
Date format
Time format
Esc
OK
MISC.
Directory
OK
User methods
Resources
Memory copies
Esc
17-OCT-1995
17:04 (24 h)
Modify
4)
5)
08/2004
DATA TRANSFER
Display directory
Copy from titrator to card
Copy from card to titrator
Esc
Modify
Memory card5)
OK
DATA TRANSFER
OK
1-5
Setup
Setup
Contents
Page
2.
Setup ..........................................................................................................
2-3
2.1
2.1.1
2.1.2
2.1.3
Titrants .......................................................................................................
Delete .......................................................................................................
Modify .......................................................................................................
Add ...........................................................................................................
2-4
2-4
2-4
2-6
2.2
2.2.1
2.2.2
2.2.3
2.3
2.4
2.4.1
2.4.2
2.5
2.6
2.7
2.7.1
2.7.1.1
2.7.1.2
2.7.2
2.7.3
2.7.4
2.7.5
Peripherals .................................................................................................
Printer .......................................................................................................
Centronics interface: Settings for an EPSON printer ...............................
RS232 interface: Settings for an EPSON printer .....................................
Balance ....................................................................................................
System .....................................................................................................
Sample changer .......................................................................................
External keyboard ....................................................................................
2-18
2-18
2-19
2-20
2-21
2-23
2-25
2-26
2.8
2.8.1
2.8.2
2.8.3
2-27
2-27
2-27
2-28
08/2004
2-1
Setup
2-2
08/2004
Setup
2.
Setup
Setup
In order to perform titrations, the titrator must be acquainted with the titrants and their
concentrations and the sensors with a feasible unit of measurement. It must know the burette
drive on which the burette is located and the input to which the sensor is connected. It must
also be familiar with the settings of the attached devices such as a balance or printer in order
to transfer data. In this menu you define all these chemical and mechanical resources and store
them: you set up your titrator.
When you press the Setup key, the list of resources appears:
Titrants
Sensors
Temperature sensors
Polarized sensors
Auxiliary values
Titration stands
Peripherals
Solvents (only with ST20A)
The titrants and METTLER TOLEDO sensors in most frequent use are already stored in the
titrator. You can not only delete these resources and modify their parameters, but also define
new ones.
Note: All information concerning automation in this titrator's Reference Handbook relates to
the earlier METTLER TOLEDO Sample changer ST20A. Its name continues to appear
in some places. Operation of other METTLER TOLEDO sample changers via your
titrator is described in the corresonding Operating Instructions.
NOTICE
All resources needed for the METTLER methods are stored! If you delete one
of these, the titrator will wait until the start of a titration of the method before
displaying the error message that the resource is not installed.
Print
Depending on your choice of resource, its list with the corresponding parameters will be printed
out.
Modify
The list of the selected resources appears.
08/2004
2-3
Titrants
2.1
Setup
Titrants
When you select this menu and press <F4>, the stored titrants appear with their concentration
data:
Titrants
NaOH
HCl
HCl04
Esc
2.1.1
0.1 mol/L
0.1 mol/L
0.1 mol/L
Delete
SETUP
Add
Modify
OK
Delete
If you press <F2>, "Delete", the titrant NaOH will be deleted from the list.
2.1.2
Modify
If you press <F4>, "Modify", the parameters of the titrants appear and you can change their
names and values.
Name
Concentration [mol/L]
Titer
Burette volume
Burette drive
Titer
Date/time
NaOH
0.1
1.0
10 mL
Drive 2
do not check
00-00-0000 00:00
Name
You can change the name by pressing <F4> and selecting a different
name from the list of "Titrant names" which appears:
Scroll the menu with the key so that the selector bar is positioned on,
e.g. "HClO4" and confirm with OK: the name of the titrant is now HClO4.
Concentration
Titer
Change the titer only if you know its value. If you determine the titer of the
titrant with the titrator, its value will be entered here automatically together
with the date (see Titer function, Section 3.3.14).
2-4
08/2004
Titrants
Setup
Burette volume
Select the volume of the burettes you wish to use with <F4>: 1, 5, 10 or
20 mL.
Burette drive
Titer
You can choose whether to enter a date when you should check the titer
of the titrant:
Press <F4>, select "check on" in the mask which appears and then
press <F4> again:
Check on
Day
Month
Year
Esc
SETUP
1
1
1997
OK
If you select "check after" and then press <F4>, the following mask
appears:
Check after
No. of days
SETUP
10
Esc
OK
When the date has lapsed, you will receive an appropriate message
during an ongoing titration method which uses this titer.
Date/time
08/2004
You can neither enter nor delete the date. It refers to the titer determination of the titrant using the method function Titer and is thus entered here
automatically together with the time (see Titer function, Section 3.3.14)
As soon as you modify a parameter of the titrant, the date/time entry will
be deleted. The expiry date of the titer is an exception: If you modify this,
date and time will not be deleted.
2-5
Titrants
Setup
Storage procedure
The titrant with its modified parameters is stored when you confirm both the parameter mask
and the list of titrants with OK. If you quit the list with Esc, the following message appears:
Save changes?
SETUP
No
Yes
OK
Any change to a parameter is always stored without a message if you press a Menu or Auxiliary
function key.
2.1.3
Add
With this command you add a titrant to the titrants list, e.g. NaOH of concentration 1.0 mol/L
or with a different burette volume or a titrant not yet on the list. The following parameters always
appear:
Name
Concentration [mol/L]
Titer
Burette volume
Burette drive
Titer
Date/time
NaOH
0.1
1.0
10 mL
Drive 2
do not check
00-00-0000 00:00
You can modify the parameters by the procedure described in Section 2.1.2. If you define, e.g.
several NaOH solutions with the same concentration, you must also flag the names so that the
titrator can distinguish these, e.g. NaOH/1. If you do not, the following message appears:
Resource exists
SETUP
Modify name
Overwrite parameters
OK
Modify: The parameter mask for modification of the name appears.
Overwrite: The modified parameters are adopted.
2-6
08/2004
Sensors
Setup
2.2
Sensors
When you select this menu and press <F4>, the stored METTLER TOLEDO sensors with their
measurement unit appear:
Sensors
DG111
DG101
DG113
Esc
SETUP
pH
pH
mV
Delete
Add
Modify
OK
You can attach the listed sensors only to a pH option (see Sections 2.4 and 10.4).
2.2.1
Delete
If you press <F2>, "Delete", the sensor DG111 will be deleted from the list.
2.2.2
Modify
If you press <F4>, "Modify", the parameters of the sensors whose names and values you can
change appear.
Name
Unit of meas.
Sensor input
Zero point [unit]
Slope [mV/unit]
Temperature [C]
Date/time
Name
DG111
pH
Sensor 1
7.0
59.16
25.0
00000000
00:00
You can change the name by pressing <F4> and selecting a different
name from the list of "Sensor names" that appears.
Note: You do not need to define a reference electrode as it is part of the
sensing electrode at the corresponding sensor option (see Section
10.4).
Unit of measurement
08/2004
You select possible measurement units for the sensor from the selection
menu.
2-7
Sensors
Unit of measurement
Setup
mV:
Either there is no other suitable measurement unit with calibration parameters for the sensor or you need only mV. If you select
the unit mV for a sensor, the calibration parameters zero point,
slope and temperature are ignored by the titrator.
pH:
pM:
M represents any cation. If you select pM, next enter the calibration parameters for a pM electrode or have them entered by
the titrator (see page 2-9: Notes 1 and 2).
pX:
X represents any anion. If you select pX, next enter the calibration parameters for a pX electrode or have them entered by the
titrator (see page 2-9; Notes 1 and 2).
%T:
A:
S/cm: If you select S/cm, next enter the calibration parameters of the
conductivity cell.
mS/cm: If you select mS/cm, next enter the calibration parameters for
the conductivity cell.
You can perform conductivity measurements and conductivity
titrations with a conductometer fitted with an analog output.
Sensor input
2-8
08/2004
Sensors
Setup
Zero point
The zero point is the measured value at which the sensor indicates 0 mV
voltage (measuring chain zero point).
For the zero point of a pH electrode this is pH0 with the unit pH.
For the zero point of an ion selective electrode this is pM0 with the unit
pM, or pX0 with the unit pX.
The zero point of the phototrode is normally 0%T (100% T =
1000 mV).
The zero point of a conductivity cell is normally 0 S/cm or 0 mS/cm.
Slope
Temperature
Date/time
You can neither enter the date nor delete it. It refers to the calibration of
the sensor using the method function Calibration and is entered here
automatically together with the time (see Calibration function, Section
3.3.13).
Notes
1. When the titrator is delivered, the defined calibration data are theoretical values of a new
sensor. You must perform a calibration of your sensor if you wish to determine accurate
values (see Calibration function, Section 3.3.13).
2. With a calibration of pH, pM or pX sensors, the calibration data (zero point, slope,
temperature) are entered here automatically together with the date.
3. As soon as you change a sensor parameter, the date/time entry is deleted.
08/2004
2-9
Sensors
NOTICE
Setup
You should never transfer the calibration data of glass electrodes which you
obtain at sensor input 1 if you attach the electrode to, e.g. sensor input 2. To
obtain correct values, recalibrate the electrode!
Storage procedure
The sensor with the modified parameters is stored when you confirm both the parameter list
and the list of the sensors with OK. The modification of a parameter is always stored when you
press a Menu or Auxiliary function key (see corresponding section at the end of Section 2.1.2).
2.2.3
Add
With this command you add a sensor to the sensor list, e.g. a DG111 sensor with different
calibration parameters or a completely new sensor. The following parameters always appear:
Name
Unit of meas.
Sensor input
Zero point [unit]
Slope [mV/unit]
Temperature [C]
Date/time
DG
mV
Sensor 1
7.0
59.16
25.0
00000000
00:00
You change the parameters by the procedure described in Section 2.2.2. If you define, e.g.
several DG111 sensors, you must also flag the name to ensure the titrator can distinguish
these, e.g. DG111/2. If you do not, a message appears (see Section 2.1.3).
2-10
08/2004
Temperature sensors
Setup
2.3
Temperature sensors
When you select this menu and press <F4>, the stored temperature sensors appear with the
sensor type:
Temperature sensors
SETUP
TEMP A Pt100
TEMP B Pt100
TEMP C Pt1000
Esc
Modify
OK
You can attach temperature sensors only to a pH option (see Section 10.4).
You can neither delete a temperature sensor from the list nor add a new one to it. However,
you can define, e.g. several Pt100s or Pt1000s at the same sensor input.
Select, e.g. TEMP A, press <F4> and the following parameters appear:
Name
Sensor type
Sensor input
Zero point [C]
Date/time
TEMP A
Pt100
Temp 1
0.0
00000000
00:00
Name
Sensor type
Sensor input
Zero point
Date/time
You can neither enter nor delete the date. It refers to the calibration of the
Pt sensor and is entered here automatically together with the time (see
Section 6.1.3).
08/2004
2-11
Temperature sensors
Setup
Notes
1. The defined zero point is the theoretical value of a new Pt sensor. You must perform a
calibration of your sensor if you wish to determine the exact value. With a calibration the
zero point is entered here automatically with the date (see Section 6.1.3: Calibrate
temperature sensors).
2. As soon as you modify a parameter of the temperature sensor, the date/time entry is
deleted.
NOTICE
You should not transfer the zero point of temperature sensors which you obtain
at input Temp 1 if you attach the sensors to, e.g. input Temp 2! To obtain correct
values, recalibrate the sensor!
Storage procedure
The Pt sensor with the modified parameters is stored when you confirm both the parameter
mask and the list of the Pt sensors with OK. The modification of a parameter is always stored
when you press a Menu or Auxiliary function key (see corresponding paragraph at the end of
Section 2.1.2).
2-12
08/2004
Polarized sensors
Setup
2.4
Polarized sensors
When you select this menu and press <F4>, "DM142" appears as the only polarized METTLER
TOLEDO electrode stored in the titrator:
Polarized sensors
SETUP
DM142
Esc
Add
Modify
OK
You can attach this sensor only to a KF option (see Section 10.4).
Note: If you have added polarized sensors to the list, the Delete command appears (<F2>).
2.4.1
Modify
If you press <F4>, "Modify", the name and sensor input of the DM142 appear:
Sensor parameters
Name
Sensor input
Esc
SETUP
DM142
Sensor 2
Modify
OK
Name
You can change the name by pressing <F4> and selecting a different
name from the list of "Sensor names" that appears.
Sensor input
Storage procedure
The sensor with the modified parameters is stored when you confirm both the parameter list
and the list of the sensors with OK. The modification of a parameter is always stored when you
press a Menu or Auxiliary function key (see corresponding paragraph at the end of Section
2.1.2).
08/2004
2-13
Polarized sensors
2.4.2
Setup
Add
With this command you add a polarized sensor to the sensor list. The following parameters
always appear:
Sensor parameters
Name
Sensor input
Esc
SETUP
DM
Sensor 2
Modify
OK
You change the parameters by the procedure described in Section 2.4.1. If you define, e.g.
several DM142 sensors, you must also flag the name to ensure the titrator can distinguish
these, e.g. DM142/2. If you do not, a message appears (see Section 2.1.3).
2-14
08/2004
Auxiliary values
Setup
2.5
Auxiliary values
When you select this menu and press <F4>, the 20 memory locations for auxiliary values
appear: H1 - H20. You can use the Auxiliary value function to assign the results of a method,
such as blank values, potentials or volume or amount of substance consumption to this
memory. These values are then entered here automatically together with the date (see Section
3.3.15).
You yourself can also enter numeric values as an auxiliary value here and call them up under
the Calculation function.
Auxiliary values
H1
H2
H3
Esc
SETUP
1.0
1.0
1.0
Modify
OK
SETUP
OK
Auxiliary value
ID
Value
Date/time
You can neither enter nor delete the date. It refers to the determination
of the auxiliary value using the method function Auxiliary value and is
entered here automatically together with the time (see Section 3.3.15).
08/2004
2-15
Auxiliary values
Setup
Notes
1. You can delete the data of an auxiliary value only by overwriting them yourself or have the
titrator overwrite them using the Auxiliary value function.
2. The titrator does not tell you if you overwrite an auxiliary value. If you make frequent use
of the auxiliary value memory, you should thus print out a list of its values from time to time
(see page 2-3).
3. If you modify a parameter of the auxiliary value, the date/time entry is deleted.
Storage procedure
The auxiliary value with the modified parameters is stored when you confirm both the
parameter mask and the list of auxiliary values with OK. The modification of a parameter is
always stored when you press a Menu or Auxiliary function key (see appropriate paragraph
at the end of Section 2.1.2).
2-16
08/2004
Titration stands
Setup
2.6
Titration stands
When you select this menu and press <F4>, the names of the five possible titration stands
appear:
Titration stands
Stand 1
Stand 2
ST20A
Esc
SETUP
Modify
OK
Stand 1
is the titration stand you receive with the basic version of the titrator.
Stand 2
ST20A
Auto stand
is the name of the titration stand on which you can run a sample series
without being prompted to insert the next sample (see Section 5.1). With
this stand you can use, e.g. a robot to change the samples.
External stand is a titration stand you have set up in addition to the above-mentioned
titration stands if you, e.g. attach a stirrer to a rod stand.
You can neither delete a titration stand from the the list nor add a new one. If you select, e.g.
Stand 1 and press <F4>, the following appears:
Titration stand parameters
Name
Stand 1
Stirrer output
Stirrer 1
Esc
Modify
SETUP
OK
Name
Stirrer output
Press <F4> to select the output for the stirrer: Stirrer 1, 2, 3, 4 or "Not at
DL".
1, 2, 3, 4 refer to the position of the sensor option (see Section 10.4).
Select "Not at DL" if you use a stirrer which is not attached to the titrator:
The wait time specified under the Stir function is allowed to elapse within
the method, but you yourself are responsible for arranging stirring (see
Stir function, Section 3.3.3).
08/2004
2-17
Peripherals
2.7
Setup
Peripherals
When you select this menu and press <F4>, the names of the devices which you can attach
to the titrator via the RS232C interfaces, the Centronics interface or the DIN socket appear.
These devices are not defined by software in the factory.
Printer
Balance
System
Sample changer
External keyboard
2.7.1
Not
Not
Not
Not
Not
defined
defined
defined
defined
defined
Printer
To define and set your printer, select Printer and press <F4>:
Printer
Status
Printer type
SETUP
Not defined
EPSON ESC/P
Esc
Status
Printer type
Modify
OK
EPSON ESC/P
HP PCL Level 3
IBM Proprinter
ASCII
GA42
You can change the settings for the selected printer in the parameter mask, which appears
when you press <F4>.
Note: On delivery of the titrator, the Centronics option is installed in slot 4 which has a parallel
interface for the printer connection (see Section 10.4). An RS option with a serial printer
interface has to be installed in slot 4 in order to use the METTLER TOLEDO Printer GA42.
2-18
08/2004
Peripherals
Setup
2.7.1.1
LX/SX
Fanfold
81/2 * 11"
No
Straight
Type
Paper
NOTICE
You must not trigger a line or form feed at the printer if you
have selected "Automatic form feed" for "Single sheet"!
You can do this on the titrator with the following key combinations:
<Shift + F1> triggers a line feed,
<Shift + F2> triggers a form feed.
Paper format
Form feed
Frame lines
08/2004
2-19
Peripherals
2.7.1.2
Setup
You can also attach printers to a serial interface if you have installed an RS option in slot 4 (see
Section 10.4). You can use this interface to attach a GA42 Printer. While no software settings
are necessary for the GA42 Printer, you must set its DIP switch 2 to the ON position (see GA42
Operating Instructions).
Example of the default settings for an EPSON printer:
Type
Paper
Paper format
Automatic form feed
Frame lines
Baudrate
Parity
Number of data bits
Number of stop bits
LX/SX
Fanfold
81/2 * 11"
No
Straight
2400
Even
8 Bits
1 Bit
The settings for the first 5 parameters are the same as those for the
Centronics interface (see Section 2.7.1.1).
Baud rate
Parity
Data bits
Stop bits
2-20
08/2004
Peripherals
Setup
2.7.2
Balance
To define and set your balance, select Balance and press <F4>:
Balance
SETUP
Status
Transmn mode
Not defined
Unidirectional
Esc
Modify
OK
Status
Transmission
mode
Unidirectional
On inquiry of the weight, the balance continuously transfers the current weight value (without
a stability check), which is displayed by the titrator. You must confirm this display with <F5>
for the value to be accepted.
Data to titrator
Balance
Titrator
Bidirectional
On inquiry of the weight, the balance transfers the current weight value when requested by the
titrator, which then displays it (with stability check).
Many METTLER TOLEDO balances show the weight limits in the balance display (see Section
4.2). The titrator accepts the stable weight value when you press either <F5> on the titrator or
the transfer key of the balance.
Command from titrator
Balance
Titrator
Data to titrator
08/2004
2-21
Peripherals
Setup
Notes
1. On delivery of the titrator, the Centronics option is installed which has a 9-pin RS232
interface for the attachment of a balance (see Section 10.4). If you install an RS option in
slot 4, its balance interface is 8-pin. Depending on the installation, you must then have the
right connection cable (see Section 11.2: Peripherals).
RS232
9-pin:
RS232
8-pin:
2. The data output of the METTLER TOLEDO balance you wish to attach must be set as
follows:
Baud rate:
2400
Parity:
even
Mode:
"Send Cont." for transmission mode Unidirectional
"Send Stable" ("Send on Transfer") for transmission mode Bidirectional.
3. The following settings are important with AT balances:
Unit:
Prt
on
Print/Transfer command on
g
Weighing unit in g
Int-FACE:
SENd
S.Stb
Data transmission mode: Standby
bd
2400
Baud rate: 2400
PAr
-EParity: even
HS
OFF
Handshake (XON/XOFF) off
4. With AG, PG, AB, PB and PR balances, the LC-RS8 cable must be set as follows:
For bidirectional transfer
For unidirectional transfer
Left switch:
Position 0
Left switch:
Position 7
Middle switch: Position 3
Middle switch:
Position 3
Right switch:
Position 4
Right switch:
Position 4
5. In case of SARTORIUS balances you must select Bidirectional as the transmission mode.
The data output of the balance you wish to attach must be set as follows:
Data output:
Ext. print command/without stability
Baud rate:
2400
Parity:
even
Stop bit:
1
Weight unit:
g
2-22
08/2004
Peripherals
Setup
2.7.3
System
To define and set your computer or terminal, select System and press <F4>:
System
Status
Instrument type
SETUP
Not defined
Computer
Esc
Modify
Status
Instrument type
Instrument type
Computer
Color terminal
Monochrome term.
Esc
OK
SETUP
Modify
You can modify the settings for the Computer in the parameter mask, which appears when
you press <F4>:
Baud rate
Parity
Number data bits
Number stop bits
Bar code to computer
Character set
Send mode
Communication protocol
Start/end character
4800
Even
8 bits
1 bit
No
ASCII
Spontaneous
Normal
'{'/ CR
Baud rate
Parity
08/2004
2-23
Peripherals
Setup
Data bits
Stop bits
Bar code
Character set
Send mode
Communication
protocol
Start/end
character
Press <F4> to select: " '{' / CR " or " STX / ETX ".
These start and end characters for the messages to be sent depend on
the input possibility of your computer.
The computer needs an RS232C interface (DTE). The parameters baud rate, parity, number
of data bits and number of stop bits are freely selectable. Connection cables are listed in
Section 11.2.
You will find additional information on the communication between titrator and computer in
Section 6.8.2 and in the Operating Instructions for the computer interface (see Section 11.2).
2-24
08/2004
Peripherals
Setup
You can change the settings for the selected Terminal in the parameter mask which appears
when you press <F4>:
Baud rate
Parity
Number data bits
Number stop bits
9600
Even
8 bits
1 bit
Baud rate
Parity
Data bits
Stop bits
You can use a terminal of the type DEC VT340 or DEC VT241 as a color terminal and either
a DEC VT330 or DEC VT240 type as a monochrome terminal. The connection cable is listed
in Section 11.2.
You will find additional information on the configuration of the terminals and their operation in
Section 10.9.
2.7.4
Sample changer
Note: All information concerning automation in this titrator's Reference Handbook relates to
the earlier METTLER TOLEDO Sample changer ST20A. Its name continues to appear
in some places.
To define the sample changer, select Sample changer and press <F4>:
Sample changer
Status
Not defined
Esc
Status
08/2004
SETUP
Modify
OK
2-25
Peripherals
2.7.5
Setup
External keyboard
You can attach a PC keyboard which has a DIN socket using a DIN cable (see Section 10.8:
Attaching a keyboard). To define the keyboard, select External keyboard and press <F4>:
External keyboard
Status
Layout
SETUP
Not defined
US International
Esc
Modify
OK
Status
Layout
2-26
08/2004
Solvents
Setup
2.8
The parameters of this resource are needed only if you have defined and attached a sample
changer. You can connect time-controlled pumps, electromagnetic valves or dispensers to the
sample changer to dispense solvents.
When you select this menu and press <F4>, the stored solvents appear:
Solvents (only with ST20A)
H2O
CH3OH
CHCl3
Esc
2.8.1
SETUP
Delete
Add
Modify
OK
Delete
If you press <F2>, "Delete", H2O will be deleted from the list.
2.8.2
Modify
SETUP
Modify
OK
Name
You can modify the name by pressing <F4> and choosing a different
name from the list of "Solvent names" that appears.
Pump rate
The titrator uses the pump rate to calculate the volume to be dispensed
for time-controlled pumps or electromagnetic valves.
You must determine the pump rate of each metering device beforehand
for every solvent:
Add the solvent using the metering device to a measuring cylinder for
1 minute (stopwatch) and note the volume.
Repeat this procedure for, e.g. 20, 30 and 40 seconds.
Calculate the mean value per minute for the different volumes and
enter this value.
08/2004
2-27
Solvents
Setup
Output
Press <F4> to select the ST20A output to which you will attach the
metering device: "DOSE", "RINSE" or "DISPENSER".
Storage procedure
The solvent with the modified parameters is stored when you confirm both the parameter mask
and the list of solvents with OK. The modification of a parameter is always stored when you
press a Menu or Auxiliary function key (see appropriate paragraph at the end of Section 2.1.2).
2.8.3
Add
You can use this command to add a solvent to the list of solvents. The following mask always
appears:
Solvent parameters
Name
H2O
Pump rate [mL/min] 200.0
ST20A output
RINSE
Esc
SETUP
Modify
OK
2-28
08/2004
Method
Method
Contents
Page
3.
Methods .....................................................................................................
3-3
3.1
3.1.1
3.1.2
3.1.3
3.1.4
3-4
3-4
3-5
3-6
3-6
3.2
3.2.1
3-7
3-7
3.3
3.3.1
3.3.2
3.3.3
3.3.4
3.3.5
3.3.6
3.3.6.1
3.3.6.2
3.3.6.3
3.3.6.4
3.3.6.5
3.3.6.6
3.3.6.7
3-20
3-20
3-21
3-22
3-25
3-28
3-33
3-34
3.3.7
3.3.7.1
3.3.7.2
3.3.7.3
3.3.7.4
3.3.7.5
3.3.7.6
3-37
3-37
3-38
3-39
3-41
3-42
3-42
3.3.8
08/2004
3-1
Method
Method
Page
3.3.9
3.3.9.1
3.3.9.2
3.3.9.3
3.3.9.4
3.3.9.5
3.3.9.6
3.3.9.7
3.3.9.8
3-45
3-45
3-46
3-48
3-48
3-49
3-50
3-52
3-53
3.3.10
3.3.10.1
3.3.10.2
3.3.10.3
3.3.10.4
3.3.10.5
3.3.10.6
3.3.10.7
3-56
3-56
3-57
3-59
3-60
3-60
3-61
3-61
3.3.11
3.3.12
3.3.13
3.3.14
3.3.15
3.3.16
3-2
08/2004
Method
3.
Method
Methods
The titrator performs analyses automatically with the aid of predefined methods. When the
titrator is delivered, the Method menu already holds standard methods and methods developed by METTLER. You can modify these methods to suit your requirements and save them
as User methods.
A complete titration method comprises sample preparation, dispensing of auxiliary solutions,
stirring and wait times, the actual titration, result calculation and a report. These sub-steps are
defined as Functions in the titrator and they are executed in succession in an analysis. The
individual functions comprise Parameters, whose values or names you can modify.
You modify a method by changing the parameters of the preset functions.
Method
Functions
Parameters
08/2004
modify
3-3
Selecting methods
3.1
Method
Selecting methods
When you press the Method key, the following appears in the display:
Method ID
Standard methods
User methods
METTLER methods
_____
Under Method ID you can call up a method stored with an identification number; these are the
user and METTLER methods.
Standard methods are methods we have entered in the factory without a method identification.
User methods are the methods you have defined and saved (they are stored in the user data
memory).
METTLER methods are applications we have developed and stored for you.
Print
Method ID:
The recalled method is printed out with its functions and parameters.
Method groups: The list of methods of the selected group is printed out.
3.1.1
Method ID
The method identification is the 5-place, numeric identifier of a method (see Title function,
Section 3.3.1).
If you are familiar with the identification, enter it and press <F4>: The list of the functions of
this method appears (see Section 3.2).
Methods
Method ID
Standard methods
User methods
Delete
METHOD
00001
Modify
Note: With user methods, you can enter an asterisk (*) after the first, second or third digit of
the method ID: This replaces the remaining digits, e.g. 1*: All methods whose ID starts
with 1 appear in the display. When you confirm the desired ID with OK, the function list
of the selected method appears immediately.
3-4
08/2004
Selecting methods
Method
Delete
When you press <F2>, the selection menu "Delete method?" appears in which you can confirm
or cancel the command:
Yes: The method will be deleted.
No: The method remains stored.
If you wish to delete a METTLER method or a user method that is stored in the sample data
memory, an error message appears. You can not delete these methods (see Section 3.1.4 and
4.1).
3.1.2
Standard methods
If you select this group, the list of 21 methods entered in the factory appears with titles (see
Section 5.2 of the Quick Guide). The standard methods are used as basic methods for the
development of your own methods and can not be called up to perform an analysis as they
have no method identification.
As soon as you allocate an identification to a standard method, it is automatically stored as a
user method with a method ID when saved and can be called up by you for the analysis.
The parameters of the other functions are defined with default values or names for all methods;
you can accept or modify these (see Sections 3.2 and 3.3).
Print
The selected method with its functions and parameters is printed.
08/2004
3-5
Selecting methods
3.1.3
Method
User methods
If you select this group, a list of methods with the identification (and the name) first appears
if you have stored modified standard or METTLER methods, e.g.:
User methods
61
11152
00001
Esc
METHOD
Delete
Modify
Delete
When you press <F2>, the selection menu "Delete method?" appears in which you can confirm
or cancel the command:
Yes: The method will be deleted.
No: The method remains stored.
Note: The "Delete" command is not available when the method is stored in the sample data
memory (see Section 4.1).
Print
The selected method with its functions and parameters is printed.
3.1.4
METTLER methods
If you select this group, a list of applications developed by us with the identification and the
name of the method appears:
METTLER methods
90001
90002
90003
Esc
Acid content
Calibration pH electrode
Calibration F- electrode
Print
Modify
METHOD
You can modify METTLER methods to suit your requirements, but you must then give them a
new method identification under the Title function in order to save them (see Section 3.3.1).
Print
The selected method with its functions and parameters is printed.
3-6
08/2004
Modifying a method
Method
3.2
Modifying a method
You have selected, e.g. the "Equivalence point titration" under standard methods and then
press <F4>: The list of the functions of this method appears.
Title
Sample
Stir
EQP titration
Calculation
Calculation
Calculation
Report
You can modify the parameters of all functions:
Select the function and press <F4>: The mask with the Parameters defined for the function
appears and you can then change their values and names (see Section 3.3).
3.2.1
Storage procedure
METHOD
Modify
OK
You modify the Title function by entering, e.g. the method identification
00001 and confirming it with OK (see also Section 3.3.1):
08/2004
3-7
Modifying a method
Method
Method: 00001
METHOD
Title
Sample
Stir
Esc
Modify
OK
If you now press <F5>, the mask of the method groups reappears: the
method is stored.
Methods
METHOD
Method ID
Standard methods
User methods
Delete
00001
Modify
2. If you quit the list of the functions with Esc after you have modified parameters of functions, the following appears:
Save method?
METHOD
No
Yes
OK
No: Changes are not stored.
Yes: The titrator stores all modified parameter values.
The same message appears if you press a Menu or Auxiliary function key.
3-8
08/2004
Modifying a method
Method
3. Several functions such as "EQP titration" have a list of parameters which have subparameters. If you quit their mask with Esc after modifications, the following appears:
Save changes?
METHOD
No
Yes
OK
No: Changes are not stored.
Yes: The titrator stores the modified parameter values.
4. On storage, the titrator checks the method and, if it has found several errors, draws your
attention to the first of them.
a. When you have confirmed the error message, the list of method functions appears with
the selection bar on the first faulty function. After you have corrected its parameters and
saved the method again, the next faulty function appears etc.
b. If you have entered an existing method identification under the Title function, the following appears:
Method ID exists
METHOD
Modify ID
Overwrite method
OK
Modify ID
The list of method functions appears; under the Title function you can
modify the method ID and then save the method.
Overwrite method
The new or modified method is stored, that with the same identification
deleted.
08/2004
3-9
Functions
3.3
Method
Functions
You select all functions whose parameters you wish to modify by the procedure described in
Sections 3.1 and 3.2. The following explanations of all functions of the standard and METTLER
methods as well as their parameters thus pertain to the Modify command. The order of the
following sections corresponds to the below list of functions.
Title
Sample
Stir
Measure
Dispense
EQP titration
EP titration
Learn titration
EQP titration (Ipol/Upol)
EP titration (Ipol/Upol)
pH/mV-stat
Calculation
Calibration
Titer
Auxiliary value
Report
3-10
08/2004
Title
Method
3.3.1
Title
This function is used for recognition of the titration method. You must enter its method ID
parameter. You use this identification to call up the stored methods. The function has no
meaning in the sequence of the method. The following example shows the title mask of the
standard method "Equivalence point titration" (see Sections 3.2. and 3.2.1).
Title
_ _ _ _ _
Method ID
Title Equivalence point titr'n
Date/time 00-00-0000 00:00
Esc
METHOD
OK
Method ID
Title
Date/time
Date and time are entered here automatically when you save a modified
method. You can neither delete not overwrite this information.
08/2004
3-11
Sample
3.3.2
Method
Sample
Here you define the parameters needed for the entry of the sample data such as weight or
volume, the titration stand on which the sample should be titrated and whether the temperature
of the sample solution should be measured.
Sample ID
Entry type
Molar mass M
Equivalent number z
Titration stand
Temperature sensor
Weight
100
1
Stand 1
Manual
Note: If samples which are determined with this method are stored in the sample data memory
as "ready", you can not modify the sample ID and the entry type (see Section 4.1).
During a sample series, you can modify only the numeric parameter values for the
ST20A titration stand (see following page and Section 5.2.3).
Sample ID
Enter the identification of the sample if required. This is adopted for all
samples of a sample series. You can also enter and modify the ID in the
Sample menu (see Section 4.1).
Entry type
3-12
08/2004
Sample
Method
Molar mass M
Equivalent
number z
You can enter only one molar mass and one equivalent number for the
calculation. If your sample contains several substances which have to be
determined by equivalence points in the titration, you must enter their
molar mass and equivalent number in constant C under the Calculation
function (see Section 3.3.12).
Titration stand
Select the titration stand at which you wish to determine the sample from
the selection menu: "Stand 1", "Stand 2", "ST20A", "Auto stand" or
"External stand" (see Section 2.6).
Temperature
sensor
Press <F4> to select the sensor if you have attached one; if not, select
"Manual": the temperature entered before starting the method will then be
adopted in the processing of the method (see Section 5.1).
This parameter is used for the automatic measurement or adoption of the
temperature of the sample solution before the start of the Measure,
EQP/EP/Learn titration and pH/mV-stat functions. Thus the slope of the
pH electrode is temperature-corrected and incorporated in the calculation of the pH value (see Section 2.3: Temperature sensors).
Pump (1)
No
No
No
No
You have attached a pump to the sample changer that should pump
solvent into the titration vessel before every titration.
Press <F4> to activate the parameter, in the mask that appears select
"Yes" and then press <F4> again:
Pump
METHOD
Solvent
Volume [mL]
Stir
Esc
08/2004
H2O
10
No
Modify
OK
3-13
Sample
Method
Pump (1)
Select the solvent from the list (press <F4>) which contains the
solvents you have defined in the Setup menu. This solvent also defines
the ST20A output to which you must attach the pump (see Section 2.8).
Enter the volume that should be dispensed. You have defined the
pump rate of the device in the Setup menu.
Select whether the dispensing operation should be stirred (Yes) or not
(No).
Pump (2)
If you have attached a second pump to the sample changer, this will be
activated as soon as the first dispensing operation is at an end.
To activate the parameters, press <F4>, select Yes in the mask that
appears and then press <F4> again: The same mask as described
under Pump (1) appears.
Selecting the solvent also defines the ST20A output to which you must
attach the second pump (see Section 2.8).
Rinse
You have installed a rinsing unit in the titration head and attached a pump
to the sample changer to rinse the sensor and burette tip after every
titration.
Press <F4> to activate the parameter, select "Yes" in the mask that
appears and press <F4> again:
Rinse
Solvent
Volume [mL]
Esc
METHOD
H2O
10
Modify
OK
Select the solvent from the list (press <F4>) which contains the
solvents you have defined in the Setup menu. Selecting this solvent
also defines the ST20A output to which you must attach the pump (see
Section 2.8).
Enter the volume which should be dispensed.
Note: If you run sample series in succession on the sample changer
(possible only with DL55/DL58) and the titrator has titrated the last
sample of the last method, the sensor and burette tip are rinsed in
the middle beaker position. The sample beaker is then raised to
ensure the sensor does not dry out, in other words it remains in the
sample solution.
To prevent this, you must insert a conditioning beaker after the last
sample beaker.
3-14
08/2004
Sample
Method
Conditioning
You must activate this parameter if you wish to condition the sensor:
Press <F4>, select "Yes" in the mask that appears then press <F4>
again:
Conditioning
METHOD
Time [s]
Interval
Rinse
Esc
10
1
No
OK
S2
S3
S4
S5
S6
S7
S8
S9
S2
S3
S4
S5
S6
S7
S8
S9
3. If the ST20A does not detect a conditioning beaker after the 3rd
sample beaker, it searches for one by rotating backward. It then
conditions for 10 s, but does not perform rinsing to avoid overflow of
the beaker contents.
C
S1
S2
S3
S4
S5
S6
S7
S8
S9
4. After the last sample of a series, the time and rinse parameters are not
executed anymore.
08/2004
3-15
Stir
3.3.3
Method
Stir
You can modify the stirring speed and stirring and wait times.
Stir
METHOD
Speed [%]
Time [s]
50
10
Esc
OK
Speed
Time
3-16
08/2004
Measure
Method
3.3.4
Measure
You measure the potential of a solution under defined conditions. The titrator determines the
measured value as raw result E (see note 2 at the end of this section).
Sensor
Unit of meas.
E [mV]
t [s]
t(min) mode
t(max) [s]
Sensor
Unit of measurement
E [mV]
t [s]
t(min) mode
DG111
mV
0.5
1.0
Fix
30
Press <F4> to open the list containing the sensors you have defined in
the Setup menu (see Section 2.2). Confirm the one you want with OK.
The defined measurement unit is entered automatically.
If you select the unit from the selection menu, you should select mV or the
unit defined in the Setup menu, otherwise you will receive an error
message when the method is started.
The drift of the electrode potential must be less than E/t (0.5 mV/s)
during the period t (1 s) for the measured value to be acquired. This
happens within a defined time span t(min) and t(max). (See diagram in
Section 3.3.6.4: Equilibrium controlled measure mode).
t(min) is the earliest time for measured value acquisition. Select t(min)
from the selection menu:
t(min) mode
Fix
E > set value
E < set value
Esc
METHOD
Modify
Fix: Press <F4> to show the mask in which you can modify t(min).
E greater than set value: Instead of a fixed time, you can enter a condition: The measured value must be greater or
less than a certain set value: Press <F4> to
E less than set value:
show the mask in which you enter the set value
[mV, pH, ...].
08/2004
3-17
Measure
t(max) [s]
Method
Notes
1. If you have selected a temperature sensor under the Sample function, the temperature of
the sample solution is measured automatically before the titrator executes this function. If
you have not attached a sensor (parameter "Manual"), the titrator adopts the temperature
entered at the start of the method. The slope of the pH electrode is temperature-corrected
by this measured or entered value and incorporated in the calculation of the pH value.
2. The Measure, Dispense, EQP/EP/EQP (Ipol/Upol)/EP (Ipol/Upol)/EP/Learn titration and
pH/mV-stat functions generate Raw results (see Section 8.1: List of symbols). These you
can
print out as such on the attached printer (see Sections 3.3.16 and 8.1.1 for exceptions).
incorporate in the calculation (see Examples of formulas: Section 8.4).
obtain as a result if you assign them to the result R: e.g. R = E (see Section 3.3.12).
At the end of a titration, you obtain only the final results in the display of the titrator, the raw
results you can only print out.
The titrator stores raw results up to the determination of the next sample within a sample
series (see Section 8.5.6).
3-18
08/2004
Dispense
Method
3.3.5
Dispense
You dispense a certain volume of a titrant with a METTLER TOLEDO burette. The titrator
determines the dispensed volume as the raw result VDISP [mL] or QDISP [mmol] (see Section
8.1: List of symbols and Section 3.3.4: Measure function).
Dispense
Titrant
Concentration [mol/L]
Volume [mL]
1.0
Esc
Titrant
Concentration
Volume
METHOD
NaOH
0.1
Modify
OK
Press <F4> to open the list containing the titrants you have defined in the
Setup menu (see Section 2.1). Confirm the one you want with OK.
The defined concentration of the titrant is entered automatically.
Enter the volume to be dispensed. Instead of a number, you can enter a
formula.
Note: If you do not need the Dispense function in the method, enter 0 for the volume: The
function will then be skipped during the analysis.
08/2004
3-19
EQP titration
3.3.6
Method
Here you define the control and evaluation of an equivalence point titration. The equivalence
point is that point at which exactly the same number of equivalents of titrant and analyte have
reacted. In most cases, it is virtually identical to the inflection point of the titration curve. This
inflection point is recognized and the equivalence point calculated.
Titrant/Sensor
Predispensing
Titrant addition
Measure mode
Recognition
Termination
Evaluation
The titrator determines several measured values and volumes as raw results including the half
neutralization value EHNV (see Section 8.1: List of symbols and Section 3.3.4: Measure
function).
Note: If you have selected a temperature sensor under the Sample function, the temperature
of the sample solution is measured automatically before the titrator executes this
function. If you have not attached a sensor (parameter "Manual"), the titrator adopts the
temperature entered at the start of the method. The slope of the pH electrode is
temperature-corrected by this measured or entered value and incorporated in the
calculation of the pH value.
3.3.6.1
Titrant/Sensor
3-20
NaOH
0.1
DG111
mV
Press <F4> to open the list containing the titrants you have defined in the
Setup menu (see Section 2.1). Confirm the one you want with OK.
The defined concentration of the titrant is entered automatically.
08/2004
Method
Sensor
Unit of measurement
3.3.6.2
Press <F4> to open the list containing the sensors you have defined in
the Setup menu (see Section 2.2.). Confirm the one you want with OK.
The defined measurement unit is entered automatically.
If you select the unit from the selection menu, you should select mV or the
unit defined in the Setup menu, otherwise you will receive an error
message when the method is started.
Predispensing
Predispensing shortens the titration time. You can select one of four predispensing modes
when you press <F4>.
to
to
to
to
No
volume
potential
slope
(factor x sample size)
Volume
You dispense a specified volume [mL] which you can enter when you
press <F4>. Instead of a number, you can enter a formula.
You can also enter a wait time: After the predispensing, the titrator waits
for this time to elapse before it adds the titrant in a controlled manner.
Potential
You dispense to a specified potential [mV, pH, ....] that you can enter
when you press <F4>.
Slope
You dispense to a specified slope [mV, pH, ..../mL] of the titration curve;
this you can enter when you press <F4>.
Factor x
sample size
No
In predispensing to volumes or (sample size x factor), the titrator adds the titrant in three steps
(4/7, 2/7, 1/7 of the defined volume), which allows optimum calculation of the addition
increment in the subsequent dynamic titration. In the predispensing to potential or slope, the
titrant addition follows the selected parameters of the main titration, but the increments are
larger.
08/2004
3-21
Method
The titrator acquires the potential values ET1 and ET2 in the predispensing.
3.3.6.3
Titrant addition
METHOD
Dynamic
Incremental
Esc
Info
Modify
You can not decide what addition mode is optimum for your method until you know the titration
curve. You can obtain general information by pressing <F3>:
You generally select the dynamic addition mode for acid/base titrations in aqueous media
or for argentometric and redox titrations,
the incremental for acid/base titrations in nonaqueous media or for complexometric, redox
and surfactant titrations.
Dynamic
The volume increment added by the titrator changes within the defined
smallest and largest increment: V(min) and V(max). This should lead
to a constant potential difference E per increment.
Dynamic
E(set) [mV]
V(min) [mL]
V(max) [mL]
Esc
3-22
METHOD
8.0
0.02
0.15
Help
OK
08/2004
Method
Dynamic
E [mV]
E~~E(soll)
E(set)
E
E5
E4
E3
V4
V3
V [mL]
If no predispensing takes place, the titrator dispenses the first two volume
increments with V(min).
Help
If you press <F3>, you can adopt the values for all three parameters from
the mask that appears. With the proposed value groups, sufficient
measured points in the vicinity of the equivalence point should be
generated to optimize its evaluation:
For steep titration curves, a value for E must be selected which is
smaller than for flat titration curves, e.g. 8 mV.
For titration curves which show a sudden potential change, small
values for E and V(max) should be selected, e.g. 4 mV.
E [mV]
steep curve
flat curve
08/2004
3-23
Method
Dynamic
Note: The smallest increment that the titrator can dispense is 1/5000 of
the burette volume:
1 mL burette 0.0002 mL
5 mL burette 0.001 mL
10 mL burette 0.002 mL
20 mL burette 0.004 mL
Incremental
Esc
METHOD
0.3
Help
OK
E [mV]
E14
E13
E12
V [mL]
V12
V14
Help
If you press <F3>, you can adopt a value for V from the mask that
appears. The proposed values are intended to achieve the same goal as
in the dynamic titrant addition: sufficient measured points in the vicinity of
the equivalence point to optimize its evaluation:
For steep titration curves, a smaller V must be selected than for flat
curves to ensure there are sufficient measured points at the equivalence point.
For titration curves which exhibit a sudden potential change, a small V
should be selected.
3-24
08/2004
Method
3.3.6.4
Measure mode
You select the equilibrium controlled or timed increment measured value acquisition:
Measure mode
METHOD
Equilibrium controlled
Timed increment
Esc
Info
Modify
These parameters are used to define the wait time up to measured value acquisition following
an incremental addition. In the equilibrium controlled measure mode, the wait time is variable,
in the timed increment it is constant. You can not decide the optimum measure mode for your
method until you know the reaction time of the components and the response time of the sensor
used. General information is available under <F3>:
Select the equilibrium controlled measure mode for, e.g. acid/base titrations in aqueous
media, argentometric, complexometric, surfactant and redox titrations.
the timed increment mode for acid/base titrations in nonaqueous media.
Equilibrium
controlled
E [mV]
t [s]
t(min) [s]
t(max) [s]
0.5
1.0
3.0
30.0
3-25
Equilibrium
controlled
Method
E [mV]
164
163
162
t = 2 s
161
E = 1 mV
160
159
t = 2 s
158
E = 1 mV
t(min)
157
156
155
154
t(min)
153
b
152
Increment addtion
151
Increment addition
t [s]
0
t(min)
5 0
t(min)
a:
The defined equilibrium condition is not yet met.
t(min): The equilibrium condition is not met after 3 s.
b:
The equilibrium condition is met for the first time after 5.4 or 6.9 s.
This measure mode results in fast increment addition in the flat part of the
titration curve and slow addition in the steep part.
In addition to the potential, the titrator acquires the time and the titrant
volume. You can print out these measured values after the titration of a
sample (see Section 3.3.16: Report).
Help
When you press <F3>, you can adopt suggested values for all four
parameters from the mask that appears:
Fast titrations are, e.g. acid/base titrations in aqueous media,
slow titrations, e.g. precipitation titrations in nonaqueous media.
3-26
08/2004
Method
Timed increment
After every increment addition, the titrator allows the time you have
defined to elapse before it acquires the measured value.
Timed increment
t [s]
METHOD
3.0
Esc
Help
OK
Help
When you press <F3>, you can adopt suggested values for the time
interval from the mask that appears:
Enter small time intervals for, e.g. acid/base titrations in aqueous
media,
large intervals for, e.g. precipitation titrations in nonaqueous media,
90 seconds for, e.g. TAN/TBN titrations of oils.
E [mV]
Measured
value
Measured
values
Increment addition
Increment addtion
Increment addition
t [s]
t1 = 3 s
08/2004
t2 = 3 s
t3 = 3 s
3-27
3.3.6.5
Method
Recognition
Recognition of the equivalence point of a titration curve depends on the type of reaction of the
components and hence on the evaluation procedure (see Section 3.3.6.7):
1. With the evaluation procedures Maximum and Minimum, an equivalence point is recognized when the greatest (smallest) potential value of the titration curve is greater (less) than
two preceding and two subsequent values.
2. With the evaluation procedures Standard and Asymmetric, an equivalence point is recognized when the maximum of the absolute values of the 1st derivative of the titration curve
is greater than two preceding and two subsequent values.
3. With the evaluation procedure Segmented, an equivalence point is recognized when the
maximum of the absolute values of the 2nd derivative of the titration curve is greater than
two preceding and two subsequent values.
Note: For the first recognition of a possible equivalence point, the titrator needs a certain
number of measured points.
The number depends on the evaluation procedure.
Measured points of a predispensing are not taken into account!
Evaluation procedure
Required number
of measured points
Minimum/Maximum
Standard
Asymmetric
10
Segmented
Example illustrating the evaluation procedure Minimum: If the lowest potential value is
found at the third measured point, it is not recognized as an equivalence point.
You must or can support the equivalence point recognition using four parameters:
Threshold
Steepest jump only
Range
Tendency
3-28
10.0
No
No
None
08/2004
Method
Threshold
To ensure that minor disturbances in the curve profile are not recognized
as equivalence points, you must determine a threshold value:
+/-E, E/V or 2E/V2. This must be exceeded.
Notes
1. The threshold value should be maximum half as large as the expected
maximum value of the first or second derivative at the equivalence
point.
2. The threshold value depends on so many factors (solvent, concentration, sensor, type of reaction, etc.) that you can not define the "correct"
threshold value until you have performed the first titration.
Info
You can obtain general information on threshold values in the standard evaluation if you press <F3>:
For steep, normal and flat titration curves, ranges of threshold
values are given for the first derivative in "pH/mL" and "mV/mL".
With the other evaluation procedures, you can enter one of the following values for the first titration:
Evaluation procedure
mV
pH/pM/pX
%T
Asymmetric
10
0.2
Segmented
10
0.2
Minimum/Maximum
08/2004
3-29
Threshold
Method
Example of threshold value of a titration curve for the evaluation procedure Minimum
E [mV]
+100
0
-30
Threshold value
-100
Minimum
V [mL]
Example of threshold value of a titration curve for the evaluation procedures Standard
and Asymmetric
E [mV]
Titration curve
V [mL]
E/
V [mV/mL]
1st derivative
Maximum (absolute)
Measured value
Threshold
value
V [mL]
3-30
08/2004
EQ titration: Recognition
Method
Threshold
Example of threshold value of a titration curve for the evaluation procedure Segmented
Titration curve
E [mV]
V [mL]
1st derivative
E/
V [mV/mL]
V [mL]
2nd derivative
2E/
V2 [mV/mL2]
Maximum (absolute)
Measured value
Threshold value
V [mL]
Steepest jump
only
08/2004
You can also select this parameter for recognition of the equivalence
point (press <F4>): The titrator then recognizes only the steepest jump of
the titration curve.
3-31
Range
Method
You can also define a potential range for recognition of the equivalence
point. Equivalence points which lie outside this range are not recognized.
Press <F4>, select "Yes" in the mask that appears and then press <F4>
again:
Range
METHOD
Limit A [mV,pH,..]
Limit B [mV,pH,..]
100
-100
Esc
OK
As a further aid in recognition of the equivalence point, you can define the
tendency, namely in what part of the titration curve descending or
ascending the equivalence point should be located (see diagram).
Use <F4> to select the tendency: "None", "Positive" or "Negative".
E [mV]
Limit A = +200
Tendenz:
Tendency:positiv
positive
EQP
Limit B = +100
0
V [mL]
3-32
08/2004
Method
3.3.6.6
Termination
You can define how a titration should be terminated by selection of five different parameters.
The titrator can terminate the titration either
when the first of the selected conditions is met, or
when all the selected conditions are met.
An exception is the maximum volume: when this is reached, the titration is immediately
terminated!
at maximum volume [mL]
at potential
at slope
after number EQPs
comb. termination conditions
10.0
No
No
No
No
Maximum volume You must enter the maximum volume. It is intended as a safety precaution: if the titration is faulty, an excessive amount of titrant is not dispensed unnecessarily as the titration is always terminated.
Potential
METHOD
0.0
Esc
OK
08/2004
The titrator terminates the titration when the slope of the titration curve is
less than a certain value. The measured slope must exceed this absolute
value once and drop below it twice to terminate the titration.
Press <F4>, select "Yes" and press <F4> again: Enter the slope [mV,
pH,.../mL] in the mask that appears.
3-33
Number EQPs
Method
Comb. terminate- The titrator does not terminate the titration until all defined termination
conditions are met (exception: maximum volume, see above).
tion criteria
Select "Yes" with <F4>.
3.3.6.7
Evaluation
You determine which evaluation procedure is used to calculate the equivalence points found
and select potential values you wish to have evaluated.
Procedure
Potential 1
Potential 2
Stop for reevaluation
Procedure
Standard
No
No
No
3-34
08/2004
Method
Potential 1
In the selection of potentials, the titrator evaluates not only the equivalence points, but also the titrant consumption in mmol or mL required for
attainment of these potential values (see Section 8.1: List of symbols).
Press <F4>, select "Yes" and press <F4> again: Enter the first potential
[mV, pH,...] in the mask that appears.
Instead of a number, you can also enter a potential stored as an
auxiliary value or a formula (see Section 2.5: Auxiliary values).
Potential 2
Stop for
reevaluation
The EQP titration function is interrupted immediately before its completion if the termination conditions and the condition defined here are met.
This allows you to modify parameters of the equivalence point recognition
(all) and the evaluation (potential 1 and 2). All evaluations are performed
again using the modified parameters (see Section 5.2.2).
Press <F4>, select "Yes" in the mask that appears then press <F4>
again:
Reevaluation
Condition
Esc
METHOD
neq=0
Symbol
Modify
OK
The condition "neq = 0" means that the EQP titration function is interrupted immediately before its completion if no equivalence point has been
found.
08/2004
3-35
Method
Stop for
reevaluation
Modify
Use <F4> to select a different condition in the list that appears:
neq > 1:
If more than one,
neq < 2:
less than two, or
3 > neq > 0: one or two equivalence points are found,
the titration will always be interrupted.
Symbol
Press <F3> to show the list of symbols (see Section 8.1). You can select
symbols from this list to define your own condition, e.g. VEQ > 0.6:
- Select "neq > 1" (under "Modify" command)
- delete "neq"
- select "VEQ" from the symbol list
- then position cursor on "1" and replace by "0.6".
3-36
08/2004
EP titration
Method
3.3.7
Here you define the control and evaluation of an end point titration and thus titrate to a particular
value of the selected measurement unit.
NOTICE
Before an end point titration to a particular pH value, you should calibrate the pH
electrode used!
Titrant/Sensor
Predispensing
Titrant addition
End point
Tendency
Termination
The titrator determines several measured values and volumes as raw results (see Section 8.1:
List of symbols and Section 3.3.4: Measure function).
Note: If you have selected a temperature sensor under the Sample function, the temperature
of the sample solution is measured automatically before the titrator executes this
function. If you have not attached a sensor (parameter "Manual"), the titrator adopts the
temperature entered at the start of the method. The slope of the pH electrode is
temperature-corrected by this measured or entered value and incorporated in the
calculation of the pH value.
3.3.7.1
Titrant/Sensor
08/2004
NaOH
0.1
DG111
mV
Press <F4> to open the list containing the titrants you have defined in the
Setup menu (see Section 2.1). Confirm the one you want with OK.
The defined concentration of the titrant is entered automatically.
Press <F4> to open the list containing the sensors you have defined in
the Setup menu (see Section 2.2). Confirm the one you want with OK.
3-37
EP titration: Predispensing
Unit of measurement
3.3.7.2
Method
Predispensing
Predispensing shortens the titration time. You can select one or two predispensing modes
when you press <F4>.
Predispensing
to volume
to (factor x sample size)
No
Esc
METHOD
Modify
Volume
You dispense to a specified volume [mL] that you can enter when you
press <F4>. Instead of a number, you can enter a formula.
You can also enter a wait time: After the predispensing, the titrator waits
for this time to elapse before it adds the titrant in a controlled manner.
Factor x
sample size
No
In the subsequent continuous titrant addition, the titrator dispenses the volume in one step. It
acquires the potential values ET1 and ET2 (see Section 3.3.6.2).
In the subsequent dynamic titrant addition, it dispenses the volume in three steps (4/ 7, 2/ 7,
1/ 7 of the defined volume), which allows optimum calculation of the addition increment. It
acquires the potential values ET1 and ET2.
3-38
08/2004
Method
3.3.7.3
Titrant addition
METHOD
Dynamic
Continuous
Esc
Info
Modify
Press <F3> for general information on what addition mode you should select:
In general, select the dynamic addition mode for acid/base titrations in aqueous media,
argentometric and redox titrations,
the continuous mode for acid/base titrations in nonaqueous media.
Dynamic
For dynamic titrant addition in the EP titration, the same conditions apply
as in dynamic addition in the EQP titration (see Section 3.3.6.3). The
measured values are acquired with equilibrium control as in the EQP
titration (see Section 3.3.6.4).
E(set) [mV]
V(min) [mL]
V(max) [mL]
E [mV]
t [s]
t(min) [s]
t(max) [s]
8.0
0.02
0.15
1.0
1.0
2.0
10.0
dynamic
titrant addition
equilibrium
controlled
measured value
acquisition
08/2004
3-39
Dynamic
Method
Continuous
Continuous
METHOD
100.0
Help
OK
The titrator dispenses the titrant slowly at the start then at the maximum
rate until the defined control band. Within the control range, the dispensing rate decreases exponentially. In the vicinity of the end point, the
titrator adds the increment V(min) (the smallest increment that the
titrator can dispense is 1/5 000 of the burette volume).
E [mV, pH]
Start of the control range
+200
4
+100
5
6
8
End point
-100
V [mL]
3-40
08/2004
Method
Continuous
Help
When you press <F3> you can adopt suggested values for the continuous
addition from the mask that appears (confirm with OK).
For titration curves with a steep control range, the control band must be
larger than that for the flat control range.
For V(min) you can enter a formula instead of a number.
The titrator measures the initial potential ET1 after 1 - 3 seconds and for
the table of measured values it acquires a measured value every 5
seconds.
3.3.7.4
End point
METHOD
EP absolute
EP relative
Esc
Modify
EP absolute
The absolute end point is the value on the electrode signal scale referred
to zero.
Press <F4> and enter the potential [mV, pH, ...] in the mask that
appears.
Instead of a number, you can enter a formula or call up a potential stored
as an auxiliary value.
Example: You have stored the value of "EPOT" of H3PO4 for the 1st
equivalence point as H4. If you wish to titrate to this potential,
enter H4.
EP relative
The relative end point is the difference between the electrode signal at the
start of the titration and that at the end.
Press <F4> and enter the potential [mV, pH, ...] in the mask that
appears.
08/2004
3-41
EP titration: Tendency/Termination
3.3.7.5
Method
Tendency
A titration exhibits a positive or negative mV or pH change (see diagram). You have to define
this.
Press <F4> and select "Positive" or "Negative" in the mask that appears (press <F4>).
NOTICE
Start potential
+ 300
3
+ 200
4
EP relative = 310 mV (pH 5.2)
+ 100
6
0
End potential
3.3.7.6
V [mL]
Termination
METHOD
10.0
10
Esc
OK
Maximum volume You must define the volume. It is intended as a safety precaution: if the
titration is faulty, an excess amount of titrant is not added unnecessarily.
Delay
3-42
08/2004
Learn titration
Method
3.3.8
Learn titration
If you are not sure what parameters you should enter for the titration function, select the
standard method Learn titration and define the parameters for the titrant and sensor under the
Learn titration function.
Note: The titrator always titrates the entire volume of the burette used. You thus have to select
weight/volume of your sample in accordance with the burette volume.
Learn titration
METHOD
Titrant/Sensor
Esc
Modify
OK
NaOH
0.1
DG111
mV
Press <F4> to open the list containing the titrants you have defined in the
Setup menu (see Section 2.1). Confirm the one you want with OK.
The defined concentration of the titrant is entered automatically.
Press <F4> to open the list containing the sensors you have defined in
the Setup menu (see Section 2.2). Confirm the one you want with OK.
The defined measurement unit is entered automatically.
If you select the unit from the selection menu, you should select mV or the
unit defined in the Setup menu. Otherwise you will receive an error
message when the method is started.
When you start the method, the titrator executes one function after another. As soon as it has
completed the Learn titration function, it calculates the parameters from the response
behavior of the sensor, the shape of the titration curve and with consideration of the burette
volume.
It stores these as an EQP titration function and sends the data to the printer. While the data
are being printed, the titrator executes the remaining functions: The "Learn titration" has given
rise to an equivalence point titration!
08/2004
3-43
Learn titration
Method
12
Version
Learn titration
28-Oct-1996
14:36
EQP titration
Titrant/Sensor
Titrant ...............................
Concentration [mol/L] .................
Sensor ................................
Unit of meas. .........................
Predispensing .............................
Volume [mL] ...........................
Wait time [s] .........................
Titrant addition ..........................
E(set) [mV] ..........................
V(min) [mL] ..........................
V(max [mL] ...........................
Measure mode ..............................
E [mV] ...............................
t [s] ...............................
t(min) [s] ............................
t(max) [s] ............................
Recognition
Threshold .............................
Steepest jump only ....................
Range
...............................
Tendency ..............................
Termination
at maximum volume [mL] ................
at potential ..........................
at slope ..............................
after number EQPs .....................
n = ................................
comb. termination conditions ..........
Evaluation
Procedure .............................
Potential 1 ...........................
Potential 2 ...........................
Stop for reevaluation .................
NaOH
0.1
DG111
pH
to volume
1.0
0
Dynamic
12.0
0.08
0.4
Equilibrium controlled
1.0
1.0
2.0
20.0
2.0
No
No
None
10.0
No
No
Yes
1
No
Standard
No
No
No
If the titrator finds more than one equivalence point, it calculates the parameters for the one
with the steepest jump.
If the titrator does not find any equivalence points, it interrupts the method and an error
message appears (see Section 5.2.2).
The titrator first recognizes a possible equivalence point when this lies at the sixth measured
point (see Section 3.3.6.5).
As an EQP titration emerges immediately from the Learn titration function, you can titrate a
series of samples with the same content. If you have selected "Statistics" under the Calculation function, the result of the first sample will then be discarded!
3-44
08/2004
Method
3.3.9
Here you define the control and evaluation of a voltametric or amperometric equivalence point
titration. The equivalence point is that point at which exactly the same number of equivalents
of titrant and analyte have reacted. In most cases, it is virtually identical to the inflection point
of the titration curve. This inflection point is recognized and the equivalence point calculated.
Titrant/Sensor
Indication
Predispensing
Titrant addition
Measure mode
Recognition
Termination
Evaluation
The titrator determines several measured values and volumes as raw results (see Section 8.1:
List of symbols and Section 3.3.4: Measure function).
3.3.9.1
Titrant/Sensor
Titrant
Concentration
Sensor
08/2004
METHOD
Modify
OK
Press <F4> to open the list containing the titrants you have defined in the
Setup menu (see Section 2.1). Confirm the one you want with OK.
The defined concentration of the titrant is entered automatically.
Press <F4> to open the list containing the sensors you have defined in
the Setup menu (see Section 2.4.). Confirm the one you want with OK.
3-45
3.3.9.2
Method
Indication
METHOD
Voltametric
Amperometric
Esc
Voltametric
Modify
E [mV]
V [mL]
3-46
08/2004
Method
Amperometric
V [mL]
Note: Higher current or voltage values result in higher jumps (a steeper curve) in the equivalence point region, however the platinum pins of the electrode become contaminated
quicker.
08/2004
3-47
3.3.9.3
Method
Predispensing
Predispensing shortens the titration time. You can select one of two predispensing modes
when you press <F4>.
Predispensing
METHOD
toE volume
~ E(set)
to (factor x sample size)
No
Esc
Change
Volume
You dispense a specified volume [mL] which you can enter when you
press <F4>. Instead of a number, you can enter a formula.
You can also enter a wait time: After the predispensing, the titrator waits
for this time to elapse before it adds the titrant in a controlled manner.
Factor x
sample size
No
In predispensing to volumes or (sample size x factor), the titrator adds the titrant in three steps
(4/7, 2/7, 1/7 of the defined volume).
3.3.9.4
Titrant addition
You can enter only a constant increment for the volume (see Section 3.3.6.3: Incremental
titrant addition):
Titrant addition
V [mL]
METHOD
0.05
Esc
3-48
OK
08/2004
Method
3.3.9.5
Measure mode
You select the equilibrium controlled or timed increment measured value acquisition:
Measure mode
METHOD
Equilibrium controlled
Timed increment
Esc
Modify
These parameters are used to define the wait time up to measured value acquisition following
an incremental addition. In the equilibrium controlled measure mode, the wait time is variable,
in the timed increment it is constant. You can not decide the optimum measure mode for your
method until you know the reaction time of the components and the response time of the sensor
used.
Equilibrium
controlled
E [mV, A]
t [s]
t(min) [s]
t(max) [s]
0.5
1.0
3.0
30.0
08/2004
3-49
Timed increment
Method
After every increment addition, the titrator allows the time you have
defined to elapse before it acquires the measured value (see diagram in
Section 3.3.6.4).
Timed increment
t [s]
METHOD
3.0
Esc
OK
For both measure modes, the titrator acquires the potential, the time and the titrant volume.
You can print out these measured values after the titration of a sample (see Section 3.3.16:
Report).
3.3.9.6
Recognition
Recognition of the equivalence point of a titration curve depends on the type of reaction of the
components and hence on the evaluation procedure (see Section 3.3.9.8):
1. With the evaluation procedures Maximum and Minimum, an equivalence point is recognized when the greatest (smallest) potential value of the titration curve is greater (less) than
two preceding and two subsequent values.
2. With the evaluation procedures Standard and Asymmetric an equivalence point is recognized when the maximum of the absolute values of the 1st derivative of the titration curve
is greater than two preceding and two subsequent values.
3. With the evaluation procedure Segmented, an equivalence point is recognized when the
maximum of the absolute values of the 2nd derivative of the titration curve is greater than
two preceding and two subsequent values.
Note: For the first recognition of a possible equivalence point, the titrator needs a certain number of measured points (see Section 3.3.6.5).
You must or can support the equivalence point recognition using four parameters:
Threshold
Steepest jump only
Range
Tendency
3-50
10.0
No
No
None
08/2004
Method
Threshold
To ensure that minor disturbances in the curve profile are not recognized
as equivalence points, you must determine a threshold value:
+/-E, E/V oder 2E/V2. This must be exceeded.
Notes
1. The threshold value should be maximum half as large as the expected
maximum value of the first or second derivative at the equivalence
point.
2. The threshold value depends on so many factors (solvent, concentration, sensor, type of reaction, etc.) that you can not define the "correct"
threshold value until you have performed the first titration.
3. You will find examples of the threshold value for the different evaluation procedures in Section 3.3.6.5.
Steepest jump
only
You can also select this parameter for recognition of the equivalence
point (press <F4>): The titrator then recognizes only the steepest jump of
the titration curve.
Range
You can also define a potential range for recognition of the equivalence
point. Equivalence points which lie outside this range are not recognized.
Press <F4>, select "Yes" in the mask that appears and then press <F4>
again:
Range
Limit A [mV, A]
Limit B [mV, A]
METHOD
100
200
Esc
OK
08/2004
As a further aid in recognition of the equivalence point, you can define the
tendency, namely in what part of the titration curve descending or
ascending the equivalence point should be located (see diagram on
page 3-32).
Use <F4> to select the tendency: "None", "Positive" or "Negative".
3-51
Method
3.3.9.7
Termination
You can define how a titration should be terminated by selection of five different parameters.
The titrator can terminate the titration either
when the first of the selected conditions is met, or
when all the selected conditions are met.
An exception is the maximum volume: when this is reached, the titration is immediately
terminated!
at maximum volume [mL]
at potential
at slope
after number EQPs
comb. termination conditions
10.0
No
No
No
No
Maximum volume You must enter the maximum volume. It is intended as a safety precaution: if the titration is faulty, an excessive amount of titrant is not dispensed unnecessarily as the titration is always terminated.
Potential
METHOD
0.0
Esc
OK
3-52
The titrator terminates the titration when the slope of the titration curve is
less than a certain value. The measured slope must exceed this absolute
value once and drop below it twice to terminate the titration.
Press <F4>, select "Yes" and press <F4> again: Enter the slope
[mV/mL] or [A/mL] in the mask that appears.
08/2004
Method
Number EQPs
The titrator does not terminate the titration until all defined termination
conditions are met (exception: maximum volume, see above).
Select "Yes" with <F4>.
3.3.9.8
Evaluation
You determine which evaluation procedure is used to calculate the equivalence points found
and select potential values you wish to have evaluated.
Procedure
Potential 1
Potential 2
Stop for reevaluation
Procedure
08/2004
Standard
No
No
No
3-53
Procedure
Method
Notes
1. In an evaluation with the standard procedure is not possible, the
equivalence point is calculated by interpolation (see Section 8.3.1).
If an evaluation is not possible with the asymmetric procedure, the
equivalence point is calculated by the standard procedure or by
interpolation (see Section 8.3.4).
In both cases, the evaluation procedure will be documented for each
sample in the "raw results" report if it differs from the defined procedure. If you have to work according to GLP guidelines, you should
therefore always record the raw results (see Section 3.3.16).
2. If you determine the same sample with a voltametric and amperometric EQP titration, in many cases you must change not only the
parameters of the indication, measured value acquisition and recognition, but also the evaluation procedure. An example is the vitamin C
determination in a multivitamin drink with DPI [0.01mol/L]:
Voltametric titration: Standard
E [mV]
E [A]
E-V curve
E-V curve
E/V-V curve
E/V-V curve
2E/V2-V curve
2E/V2-V curve
V [mL]
3-54
V [mL]
08/2004
Method
Procedure
V [mL]
Potential 1
In the selection of potentials, the titrator evaluates not only the equivalence points, but also the titrant consumption in mmol or mL required for
attainment of these potential values (see Section 8.1: List of symbols).
Press <F4>, select "Yes" and press <F4> again: Enter the first potential
[mV, A] in the mask that appears.
Instead of a number, you can also enter a potential stored as an
auxiliary value or a formula (see Section 2.5: Auxiliary values).
Potential 2
Stop for
reevaluation
08/2004
3-55
EP titration (Ipol/Upol)
3.3.10
Method
EP titration (Ipol/Upol)
Here you define the control and evaluation of an end point titration with voltametric or amperometric indication.
Titrant/Sensor
Indication
Predispensing
Titrant addition
End point
Tendency
Termination
The titrator determines several measured values and volumes as raw results (see Section 8.1:
List of symbols and Section 3.3.4: Measure function).
3.3.10.1
Titrant/Sensor
Titrant
Concentration
Sensor
3-56
METHOD
Modify
OK
Press <F4> to open the list containing the titrants you have defined in the
Setup menu (see Section 2.1). Confirm the one you want with OK.
The defined concentration of the titrant is entered automatically.
Press <F4> to open the list containing the sensors you have defined in
the Setup menu (see Section 2.4). Confirm the one you want with OK.
08/2004
Method
3.3.10.2
Indication
METHOD
Voltametric
Amperometric
Esc
Voltametric
Modify
V [mL]
08/2004
3-57
Amperometric
Method
V [mL]
3-58
08/2004
Method
3.3.10.3
Predispensing
Predispensing shortens the titration time. You can select one or two predispensing modes
when you press <F4>.
Predispensing
to volume
to (factor x sample size)
No
Esc
METHOD
Modify
Volume
You dispense to a specified volume [mL] that you can enter when you
press <F4>. Instead of a number, you can enter a formula.
You can also enter a wait time: After the predispensing, the titrator waits
for this time to elapse before it adds the titrant in a controlled manner.
Factor x
sample size
No
With the predispensing, the titrator dispenses the volume in one step.
08/2004
3-59
3.3.10.4
Method
Titrant addition
The addition can only be continuous (see Section 3.3.7.3: Continuous titrant addition):
Titrant addition
Control band [mV, A]
V(min) [mL] 0.01
METHOD
500.0
Esc
OK
The titrator dispenses the titrant slowly at the start then at the maximum
rate until the defined control band. Within the control range, the dispensing rate decreases exponentially. In the vicinity of the end point, the
titrator adds the increment V(min) (see diagram in Section 3.3.7.3); the
smallest increment that the titrator can dispense is 1/5 000 of the burette
volume.
For V(min) you can enter a formula instead of a number.
The titrator measures the initial potential ET1 after 1 - 3 seconds and for
the table of measured values it acquires a measured value every 5
seconds. The titrator can store maximum 300 measured values. If this
limit is exceeded, it reduces the number of measured values by half by
leaving only every second measured value in the memory. The new
measured values continue to be acquired every 5 seconds.
Note: The control band determines the control and the speed of the end point titration. To enter
a "reasonable" value, you should perform an equivalence point titration with timedincrement measured value acquisition. Using the table of measured values of this
titration, you can determine both the end point potential and the control band exactly.
3.3.10.5
End point
METHOD
100.0
Esc
OK
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08/2004
Method
3.3.10.6
Tendency
Esc
METHOD
Negative
Modify
OK
Note: The tendency of a voltametric titration with a positive current intensity is negative, with
a negative current intensity it is positive. The tendency of an amperometric titration with
a positive voltage is positive, with a negative voltage it is negative.
3.3.10.7
Termination
You define the termination of a titration by selecting two resp. three parameters.
Termination
Maximum volume [mL]
Delay [s]
Maximum time [s]
Esc
METHOD
10.0
Yes
No
OK
Maximum volume You must define the volume. It is intended as a safety precaution: if the
titration is faulty, an excess amount of titrant is not added unnecessarily.
Delay
Maximum time
Instead of or in addition to the delay time, you can also enter a time when
the titration should be stopped.
Enter a maximum time when, e.g. you perform a stating (see METTLER
method 90016: Drift determination for KF titrations).
If you define a value for both termination parameters, the titration will be
terminated when one of the two values is reached.
Note: If the titration is terminated because the maximum time has been
reached, no end point will be calculated. VEND (VEX) is recorded
as the raw result.
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3-61
pH/mV-stat
3.3.11
Method
pH/mV-stat
With the aid of this function you can perform a pH-stating. You determine the parameters which
assure the constancy of a potential value, which lead to termination of the pH-stating and which
are used for the evaluation.
Titrant/Sensor
Pretitration
End point
Tendency
Termination
Storage interval
Evaluation
The titrator determines the following raw results (see also 8.1: List of symbols):
the titrant consumption in mL or mmol up to termination of the pH-stating.
the titrant consumption in mL or mmol up to attainment of defined time limits.
the mean titrant consumption in mL/min or mmol/min within the defined time limits.
the correlation coefficient CSTAT, which results from calculation of the mean titrant
consumption through linear regression.
Notes
1. If you have selected a temperature sensor under the Sample function, the temperature of
the sample solution is measured automatically before the titrator executes this function. If
you have not attached a sensor (parameter "Manual"), the titrator adopts the temperature
entered at the start of the method. The slope of the pH electrode is temperature-corrected
by this measured or entered value and incorporated in the calculation of the pH value.
2. In the recording of a titration curve, you obtain only the actual pH-stating. You can follow
the graphical plot of the pretitration only on the display.
Titrant/Sensor
To modify the titrant or the sensor, press <F4>:
Titrant
Concentration [mol/L]
Sensor
Unit of meas.
3-62
NaOH
0.1
DG111
mV
08/2004
pH/mV-stat
Method
Titrant
Concentration
Sensor
Unit of measurement
Press <F4> to open the list containing the titrants you have defined in the
Setup menu (see Section 2.1). Confirm the one you want with OK.
The defined concentration of the titrant is entered automatically.
Press <F4> to open the list containing the sensors you have defined in
the Setup menu (see Section 2.2). Confirm the one you want with OK.
The defined measurement unit is entered automatically.
If you select the unit from the selection menu, you should select mV or the
unit defined in the Setup menu, otherwise you will receive an error message when the method is started.
Pretitration
Select the pretitration if the potential value of your solution differs from the value you need for
the pH-stating:
Press <F4> and select "Yes" in the mask that appears.
Press <F4> and enter the control band [mV, pH, ...] in the mask that appears (see Section
3.3.7.3: EP titration, Titrant addition).
End point
End point
Potential [mV, pH,...]
Control band [mV, pH,...]
METHOD
8
0.7
Esc
OK
Potential
The value you enter here is kept constant during the pH-stating. Instead
of a number, you can enter a formula or call up a potential stored as an
auxiliary value (see example in Section 3.3.7.4).
Control band
The defined value controls the end point range: The lower the value, the
faster the titrator reacts to a deviation from the potential of the defined end
point.
Help
You can accept suggested values for the value of the control band: Press
<F3> and confirm a value in the mask that appears with OK.
For pH-statings whose end point lies in a steep control range, the
control band must be larger than for statings whose end point lies in a
flat control range.
08/2004
3-63
pH/mV-stat
Method
Tendency
The tendency you have to define refers to the titrant which is added. The kinetics of the reaction
determined by pH-stating are always in the opposite direction!
Press <F4> and select "Positive" or "Negative" in the mask that appears.
Termination
You define the termination of the pH-stating by the following parameters:
Maximum volume [mL]
t(min) [s]
t(max) [s]
Minimum consumption [mL]
Time span [s]
10
60
600
0.1
10
Maximum volume The entry is intended as a safety precaution: if the titration is faulty, an
excess amount of titrant is not added unnecessarily.
t(min)
t(max)
Min. consumption The stating is terminated when not more than 0.1 mL titrant are consumed
within 10 seconds (example of default parameters).
Time span
This condition can be effective at the earliest after 60 seconds [t(min)].
After 600 seconds [t(max)], the stating is terminated even if the condition
is not met.
Storage interval
You define a time interval for storage of the measurement data.
Press <F4> and enter the interval in the mask that appears.
With the default value, the current measured value and the associated volume are stored after
10 s.
The titrator can store and print out maximum 300 measured values. If the defined interval is
too small, after 300 measured values the titrator first eliminates the values of the pretitration.
If the limit of 300 measured values is then again exceeded, it reduces their number by half by
leaving only every second measured value in the memory. The measured values continue to
be stored at the defined interval.
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08/2004
pH/mV-stat
Method
Evaluation
The following parameters define the evaluation of the pH-stating:
Evaluation
METHOD
100.0
200.0
Esc
Time limit t1
Time limit t2
OK
1: Pretitration
2: When the end point is reached, the titrator
waits 5 s before sending an audio signal and
the message "Pretitration complete: Please
add sample!". The titrator continues to exert
control and stir.
3: You enter your sample and confirm the
message with OK: The titration starts. If you
have to remove the titration vessel for addition, you can stop the stirrer during this time
(see Section 6.2)
4: The termination condition of V/t is met,
the pH-stating is terminated.
V/t [mL/s]
3
2
4
t [s]
1
t(min)
t(max)
08/2004
3-65
Calculation
3.3.12
Method
Calculation
You can use this function to calculate one result R for every sample.
Formula
Constant
Decimal places
Result unit
Result name
Statistics
R=Q*C/m
C=M/(10*z)
3
%
No
Formula
Press <F4> to open the "List of formulas" and select a different formula
or enter the one you need for your calculation (see also Section 8.4:
Examples of formulas).
Constant
Press <F4> to open the "List of constants" and select a different constant
or enter the one you need for your calculation.
Symbol
You can select the symbols you need for your calculation from the list that
appears by pressing <F3>. It contains all symbols possible for the
individual functions (see also Section 8.1: List of symbols).
You can link together all available parameters and numeric values.
Example illustrating the entry of the formula "R=QSTAT(120,180)":
- Press <F4> and accept "R=VSTAT(100,200)",
- position the cursor on "V", delete it and select "Q" from the list,
- replace "100" by "120",
- skip the comma with the cursor and
- replace "200" by "180".
The following operations are available for calculations:
on the keypad
Addition:
Subtraction:
3-66
in "List of formulas"
+
lg(x)
ln(x)
Multiplication: *
Division:
/
pw(x)
ex(x)
sq(x)
sr(x)
08/2004
Calculation
Method
Decimal places
Result unit
Result name
Statistics
Notes
1. Some standard methods include three Calculation functions. If you need only one result,
delete the formula "Rn = ..." with CE. This skips the function when the method is processed.
2. For the calculation of a titration
curve with 3 equivalence points
(acidic mixture of 3 substances),
you must define the parameters
of the three Calculation functions.
R3
R2
R1
Q1
Q2
Q3
Formula
Constant
Unit
R1 = Q1 C1 / m
C1 = M / (10 z)
[%]
R2 = Q2 C2 / m
C2 = (60.01 1000) / 1
[ppm]
R3 = Q3 C3 / m
C3 = 53.5 / 1
[mg/g]
Another example is the METTLER method 90001: In addition to the NaOH consumption in
mL as a result, the acid content of HCl in mol/L and in g/L are calculated.
3. R and C are indexed according to the preset sequence. If you delete, e.g. the formula
"R2 =...", 3 remains as the index for the third calculation if you do not change it yourself (see
Section 8.2: Use of indices).
08/2004
3-67
Calculation
Method
4. You must enter the molar mass M and the equivalent number z of the 2nd and 3rd
Calculation function as numeric values or insert as Hj if you have stored them as auxiliary
values (see Section 2.5): M and z are defined in the Sample function for the calculation
of the first equivalence point (see Section 3.3.2).
5. If you do not know the number of equivalence points, you can have Q recognized by a
condition instead of defining indices for Q (see "List of formulas").
Example: R = Q (200 < EPOT < 300) means that the Q used for the calculation is that whose
equivalence point potential lies between 200 and 300 mV. If the titrator detects more than
one equivalence point in this range, it calculates the first (see also Section 8.4.3).
6. The titrator checks your entries when you quit the parameter mask with OK. If you have
entered wrong formulas or constants, you immediately receive an appropriate error
message, e.g.
Error No. 3
Wrong formula
Modify
Terminate
METHOD
OK
Modify:
You can change the entry.
Terminate: The entry last stored reappears.
If you have used raw results (e.g. R = QDISP) which the titrator can not determine as the
method does not include the Dispense function, you do not receive an error message until
the method is stored.
7. The titrator stores results until you start a new sample series or switch off the titrator (see
also Section 8.5.6).
8. If you abort the method with Reset, an evaluation of the data obtained to date follows. If
you were to abort the titration sequence (see point 2), e.g. shortly before the second
equivalence point, you would receive result R1 but not R2 and R3 (see Section 5.2.4).
9. Under the auxiliary function Results, you can
perform additional calculations after the titration of a sample (see Section 6.5.3)
eliminate results (outliers) on completion of a sample series and thus modify the statistical evaluation (see Section 6.5.5).
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08/2004
Calibration
Method
3.3.13
Calibration
You can use this function to calibrate an electrode: its zero point and its slope are calculated.
You determine the buffers which you use for calibration of the sensor. The potential of the
buffer solutions is acquired using the Measure function (see example in the Quick Guide).
Notes
1. As the slope of an electrode depends on the temperature, it is important to incorporate the
temperature in the calibration.
Before the Measure function, the temperature of the buffer solution is measured
automatically if you have attached a temperature sensor; otherwise, the temperature you
entered before the start of the calibration is used (see Sample function, Sections 3.3.2
and 5.1).
If you later measure the pH value of a solution at a different temperature, the slope of the
sensor is temperature-corrected by the titrator.
2. The calibration data (zero point, slope and calibration temperature) are entered automatically with the date in the parameter mask of the sensor (see Section 2.2.2).
3. Depending on the number of buffer solutions measured, the titrator performs the following
calibration:
With one buffer solution, it calculates the zero point of the sensor. The slope remains
unchanged.
With several buffer samples, it calculates the zero point and the slope of the sensor by
means of a linear regression through the measured points.
You can modify the following parameters:
Sensor
DG111
Buffer type
pH (DIN/NIST)
Result R
1
Minimum slope [mV/unit]
-55.0
Maximum slope [mV/unit]
-65.0
Sensor
Press <F4> to open the list containing the sensors you have defined in
the Setup menu (see Section 2.2). Confirm the one you want with OK.
Buffer type
Press <F4> and select the type in the mask that appears:
pH (DIN/NIST),
pH (MERCK),
pH (METTLER TOLEDO) or
pH, pM, pX.
08/2004
3-69
Calibration
Buffer type
Method
The titrator has 8 values each for DIN/NIST, MERCK Titrisol and METTLER
TOLEDO buffer solutions stored which you can select to calibrate pH
electrodes. Under "pH, pM, pX (free selection)" enter values of userselected buffer solutions to calibrate pH or ion-selective electrodes (see
Note 2).
Example illustrating selection of pH values of a MERCK buffer. Press
<F4> to display the selection menu:
pH (MERCK Titrisol)
First buffer
Second buffer
Third buffer
Esc
METHOD
pH 4
pH 4
pH 4
Modify
OK
If your first buffer solution does not have a pH value of 4, press <F4>
(otherwise, select 2nd buffer):
MERCK buffers
pH 3
pH 4
pH 5
pH 6
Esc
METHOD
OK
Select a different buffer value from this list, e.g. pH 3 and confirm with
OK.
In the "pH (MERCK Titrisol)" mask select the 2nd buffer and again
press <F4> to select its pH value, e.g. pH 7 etc.
Notes
1. The buffer values apply to a temperature of
25 C for DIN/NIST buffers
20 C for MERCK Titrisol buffers
25 C for METTLER TOLEDO buffers.
If you calibrate at a different temperature, these buffer values are
automatically temperature-corrected and recorded on the printout.
If you calibrate at a temperature that lies outside the defined range for
the corresponding buffer, "Temperature outside limits" appears in the
report; however, the calibration data will be recorded.
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08/2004
Calibration
Method
Buffer type
2. For the pH, pM, pX buffer values you can also enter formulas.
3. Positive ions result in a negative slope, negative ions in a positive
slope.
Result R
"1" (result index): The measured values E of the buffer solutions used are
stored under the first Calculation function: R1 = E (see Section 8.2: Use
of indices). The titrator calculates the zero point and the slope of the
electrode by linear regression by assigning the measured values to the
standard concentrations of the buffer solutions. The index must thus be
the same as under the Calculation function.
Minimum slope
Maximum slope
08/2004
3-71
Titer
3.3.14
Method
Titer
Titer is an assignment function: The result R or its calculated mean value x of the titration of
a titrant is assigned to the titer by t = R or t = x and automatically entered in the parameter
mask of the titrant with the date (see Section 2.1.2 and the example in the Quick Guide).
Titer
Titrant
NaOH
Concentration [mol/L]
Formula t = x
Esc
Titrant
Concentration
Formula t =
METHOD
0.1
Modify
OK
Press <F4> to open the list containing the titrants you have defined in the
Setup menu (see Section 2.1). Confirm the one you want with OK.
The defined concentration of the titrant is entered automatically.
Press <F4> to select from the selection menu:
"x", if you determine the titer with more than one sample so that the
calculated mean value is assigned to the titer. The statistical calculation
must be selected in the Calculation function for this.
"R" only if you determine the titer with a single sample.
Note: If you delete, e.g. one result of these titer determinations under the auxiliary function
Results, the new calculated mean value will not be entered in the parameter mask of
the titrant!
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08/2004
Auxiliary value
Method
3.3.15
Auxiliary value
Auxiliary value is an assignment function. The result (R or Ri) or its calculated mean value
(x or x [k]) or a raw result of the titration function is assigned to the auxiliary value Hj and
entered automatically with the date in the parameter mask of the auxiliary value (see Section
2.5 and Section 8.2: Use of indices).
20 auxiliary value memories are available: H1 - H20.
You can store, e.g. the following as auxiliary values:
the blank value of a titration (example of the standard method: "Blank by EQP titration")
a raw result that you obtain under the EQP or EP titration function, e.g. "H6 = VEQ".
You can call up these auxiliary values in the Calculation function.
Auxiliary value
ID
Formula
METHOD
H20=R1
Esc
OK
ID
Formula
Enter "H = R" or "Hj = Ri" if you determine the auxiliary value with a single
sample.
Enter "H = x " or "Hj = x [k]" only if you determine the auxiliary value with
more than one sample so that the calculated mean value is assigned to
the auxiliary value. The Statistics calculation must be selected in the
Calculation function for this.
You can also enter, e.g. "H (Hj) = VEND * 1.5" as a formula.
Symbol
If "Formula" is selected, you can open the list of symbols with <F3> (see
also Section 8.1). Select the symbol from this list which should be
assigned to the auxiliary value, e.g. for the formula "H6 = VEQ":
- Position the cursor on "2",
- replace "20" by "6",
- position the cursor on "R" and delete "R1",
- select "VEQ" from the symbol list.
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3-73
Report
3.3.16
Method
Report
METHOD
Yes
No
Modify
OK
Use <F4> to select the unit(s) or card to which the data should be sent:
Printer,
Memory card (not with DL50),
Computer,
Printer + memory card (not with DL50) or
Printer + computer.
Printer is stored as the default parameter (for the printer you have
defined, see Section 2.7.1).
If you have not defined a printer and/or computer, the function can not be
executed. This case neither initiates an error message nor does it
influence the titration.
If you have defined and switched on a printer, but this is set to "offline",
the titrator waits until you switch the printer to "online" and then starts to
transfer its data.
If you have defined and attached a computer, but have not switched it on,
an appropriate error message appears.
If you have selected memory card but have not inserted one, an appropriate error message appears.
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08/2004
Method
Report
Results
All results defined in the Calculation function are recorded for the current
sample after every titration. Use <F4> to select "No" if you do not want a
report.
All results
After the last titration of a sample series, the results of all samples are
recorded if you select "Yes" with <F4>. These include the statistics,
calibration, titer and auxiliary value data if the parameter or the functions
have been defined in the method.
Raw results
After every titration the raw results such as VEQ or VDISP of the current
sample are recorded if you select "Yes" with <F4>.
After every titration the table of measured values of the current sample
is recorded if you select "Yes" with <F4>.
Sample data
After the last titration of a sample series the sample data of all samples
are recorded if you select "Yes" with <F4> (ID, molar mass, equivalent
number, weight/volume, correction factor).
E V curve
After every titration the titration curve Potential vs Volume of the current
sample is printed out if you select "Yes" with <F4>.
E/V V curve
After every titration the 1st derivative of the titration curve Potential vs
Volume of the current sample is recorded if you select "Yes" with <F4>.
The ordinate representation is linear.
log E/V V
curve
After every titration the 1st derivative of the titration curve Potential vs
Volume of the current sample is recorded if you select "Yes" with <F4>.
The ordinate representation is logarithmic.
2E/V2 V
curve
After every titration the 2nd derivative of the titration curve Potential vs
Volume of the current sample is recorded if you select "Yes" with <F4>.
The ordinate representation is linear.
E t curve
After every titration the titration curve Potential vs Time of the current
sample is recorded if you select "Yes" with <F4>.
V t curve
After every titration the titration curve Volume vs Time of the current
sample is recorded if you select "Yes" with <F4>.
V/t t curve
After every titration the 1st derivative of the titration curve Volume vs
Time of the current sample is recorded if you select "Yes" with <F4>.
08/2004
3-75
Sample
Contents
Page
4.
4-3
4.1
4.1.1
4.1.2
4.1.3
4.1.4
4.1.4.1
4.1.4.2
4-4
4-6
4-7
4-7
4-8
4-8
4-8
4.2
4.3
08/2004
4-1
Sample
4.
This menu is used for the entry and storage of sample data. You can enter weight or volume,
identification, correction factor and temperature for maximum 60 samples. The data remain
stored even if you switch off the titrator; data of analyzed samples, on the other hand, are
deleted.
The menu is always accessible during the analysis to allow the user
to see which samples have already been titrated
to modify or delete data of samples not yet analyzed
to enter data for additional samples.
The performance of the four titrators differs in this menu as follows:
DL50/DL53: You can enter data for only one sample series.
DL55/DL58: You can enter data for three sample series; these series can be run with
the same method or with three different methods.
You can enter the data of a so-called urgent sample.
With the Run key, method(s) and sample data are called up automatically and analyzed in
succession by the titrator (see Section 5).
08/2004
4-3
Sample
4.1
When you press the Sample key, the (blank) sample data list appears:
No.
Status
Wt/vol.
Meth.
ID
Add
Add
SAMPLE
OK
Sample entry
Number of samples
Method ID
User
Esc
SAMPLE
1
00001
OK
Enter, e.g. 00001 (example for the standard method "Equivalence point
titration", see Section 5.1): This calls up the method to be used for
analysis of the samples.
If you do not know the identification of the method, press <F4> "Modify":
The method groups appear.
Confirm either user or METTLER methods: The list of these methods
appears.
Confirm the method you need for the analysis.
User
4-4
08/2004
Sample
Note: The titrator also accepts methods stored on an inserted memory card or in an attached
computer: When you enter an identification whose method is not stored in the titrator,
the method is first searched for on the memory card and entered (not possible with the
DL50). If the method is not stored on the card, it is requested from the computer and
entered (see Operating Instructions: Computer Interface Description).
Press <F5> to show the sample data mask (weight entry as example):
Sample No. 1
Sample ID
Weight [g]
0.0
Limits [g]
0.02 - 2.0
Correction factor f
1.0
Esc
SAMPLE
Balance*
OK
Sample ID
Weight
(Volume)
SAMPLE
Modify entry
Save entry
OK
Modify: The sample data mask reappears.
Save: The weight is transferred. The sample data mask for the next
sample or the sample data list appears.
08/2004
4-5
Sample
Limits
You can not change the limits. These data do not appear if you have
defined a fixed volume in the Sample function.
Correction factor
You can enter a value for every sample that is reconciled in the
calculations if you enter f in the formula of the Calculation function.
Example: Each substance has a different, known moisture content
whose value you can insert for f:
1st sample: Moisture content = 4% f = 0.96 R = Q * C/(m * f)
2nd sample: Moisture content = 3% f = 0.97 R = Q * C/(m * f)
Temperature
Enter the temperature of the solution to be titrated. You can not change
the value if you have defined a temperature sensor in the Sample function.
When you confirm the entries, the sample data mask for the second and the third sample
appears, followed by the sample data list:
No.
2
3
Status
ready
ready
Wt/vol.
1.23454
1.67115
Delete
4.1.1
Meth.
00001
00001
ID
45321
45322
Modify
Add
SAMPLE
Selected sample
Sample series
Esc
OK
Selected sample
The sample highlighted by the selection bar when you confirmed "Delete"
is deleted.
Sample series
4-6
08/2004
Sample
Notes
1. You can not delete sample data of a series which are done until all defined samples have
been analyzed. When you then press <F2>, you can delete only the series.
2. If the titrator is controlled by a computer, you can not delete the sample data (see Section
6.8.3).
4.1.2
A list of all sample data contained in the sample data memory is printed out.
4.1.3
08/2004
4-7
Sample
4.1.4
4.1.4.1
DL50/DL53
You add data of a new sample to the existing data of a sample series:
Add
SAMPLE
Sample to series1)
Esc
1)
Sample to series
OK
If you have transferred the existing data from a computer, "Sample to series (data:
computer)" appears, see Section 4..
If the series has been processed, "New sample series" also appears.
The sample data mask for sample No. 4 of method 00001 appears
(example in Section 4.1.1).
As long as you do not delete the data of a series classed as done, you
can add data for a new sample to the series.
The data of a processed series are deleted when you
switch off the titrator
select "New sample series" in place of "Sample to series"
modify the method used to run the series.
4.1.4.2
DL55/DL58
You either add the data of an additional sample or that of a new series to the existing data of
a series. The series are processed by the titrator in the defined sequence.
Add
SAMPLE
4-8
1)
OK
appears when you have defined and attached a computer (see Section 4.3). If you
have transferred existing data from the computer. "Sample to series (data: computer)" also appears scroll display
08/2004
Sample
New sample
series
Status
Wt/vol.
Meth.
ID
1
2
ready
ready
1.36182
1.23454
00001
00001
45320
45321
Add
Select the blank line above the first sample and press <F5>: The "Add"
mask appears (see above and the sequence in Section 4.1).
Between two sample series
No.
2
3
1
2
Status
ready
ready
ready
ready
Wt/vol.
1.23454
1.67115
5
5
Meth.
00001
00001
2
2
ID
45321
45322
Add
Select a sample data line of the first series and press <F5> : The "Add"
mask appears (see above and sequence in Section 4.1).
After the last sample series
Select a sample data line of the last series and press <F5>: The "Add"
mask appears.
Sample to series
The sample data mask for sample No. 4 of method 00001 appears (example in Section 4.1.1).
You can add samples to a completed series before the titrator starts to
process the next series, in other words before you confirm the result list
of the last sample with OK.
As soon as you have confirmed the result list of the last sample of a series,
all its data are deleted when the next series is defined. You can then enter
the data for a new sample series.
08/2004
4-9
Sample
Urgent sample
If you have to analyze one sample immediately while a sample series is being processed by
the DL55/DL58, you can insert this after the active series sample. The sample series is
interrupted and then continued after the determination.
Example: The titrator is processing sample 2 of method 00001.
Press the Sample key and select the active sample:
No.
1
2
3
1
Status
done
active
ready
ready
Wt/vol.
1.36181
1.23454
1.67115
5
Meth.
00001
00001
00001
2
ID
45320
45321
45322
Add
Add
SAMPLE
OK
SAMPLE
1
00001
OK
Number samples You can not modify these: You can determine only one urgent sample at
a time!
Method ID
User
4-10
08/2004
Sample
After entry and confirmation of the sample data, the following appears:
No.
1
2
EX
3
Status Wt/vol.
Meth. ID
done
1.36181
00001 45320
active 1.23452
00001 45321
ready
0.41894
8
ready
1.67115
00001 45322
Delete
Print
Modify
Add
08/2004
4-11
Sample
4.2
If you have attached a balance to the titrator, you must have defined this in the Setup menu.
If not, "Balance" does not appear in the sample data mask.
Sample No. 1
Sample ID
Weight [g]
0.0
Limits [g]
0.02 - 2.0
Correction factor f
1.0
Esc
SAMPLE
Balance
OK
When you press <F4>, the value displayed on the balance appears, e.g.
Weight:
>
SAMPLE
1.36181
Esc
OK
4-12
08/2004
Sample
4.3
If you have loaded the DLWin or the LabX titration software or an appropriate program on the
attached computer, you can request the sample data stored on it. With the "Add" command,
the following appears automatically:
Add
New sample series
New sample series (data: computer)
Esc
Series entry
SAMPLE
OK
SAMPLE
ID
User
Esc
OK
ID
You enter the identification of the sample series stored in the computer.
This is transferred to the sample data memory with OK. These sample
data can only be printed out or displayed ("Modify" command).
User
If you wish to add the data of a new sample to a series transferred from the computer, confirm
"Sample to series (data: computer)" in the "Add" mask with OK. The sample data are added
to the sample data list.
You will find further information in the Operating Instructions for the computer interface or the
DLWin or LabX titration software.
08/2004
4-13
Run
Run
Contents
Page
5.
Analysis .....................................................................................................
5-3
5.1
5-4
5.2
5.2.1
5.2.2
5.2.3
5.2.4
5-7
5-11
5-11
5-12
5-12
5.3
5.4
08/2004
5-1
Run
Run
5.
Analysis
You perform titrations with a selected method. The data required for this are stored in the
Method and Setup menus. You prepare your sample, titrate it and receive the result.
You enter the sample data such as weight or volume directly before the start of each sample
determination. These data are also entered in the sample data memory. To modify them during
the titration or to add samples to a defined sample series, you can open the Sample menu.
While a method is running, you can call up the auxiliary functions "Stirrer" and "Results"; all
other auxiliary functions and the Setup and Method menus are blocked.
In this menu, the functions of the Run and command key <F5> are identical, in other words you
can press one or other key.
The performance of the four titrators differs in this menu as follows:
DL50/DL53:
DL55/DL58:
08/2004
5-3
Menu sequence
5.1
Run
When you press the Run key, there are two possibilities for the display (as an example of the
representation, the standard method "Equivalence point titration" is used. This has been
changed for the determination of CaCl2 and stored with the identification 00001):
No data in sample data memory:
Samples to be analyzed
Number of samples
Method ID
User
3
00001
Samples to be analyzed
3 samples,
Start
Defined are
RUN
Stirrer 1: Stand 1
Sensor 1: DM141
Drive 2: 0.1 mol/L AgNO3
Esc
Print
Method 00001
Delete
Start
Defined are
RUN
Stirrer 1: Stand 1
Sensor 1: DM141
Drive 2: 0.1 mol/L AgNO3
Esc
Print
OK
Sample No. 1
Sample ID
45320
Weight [g]
1.23452
Limits [g]
0.02 - 2.0
Correction factor f 1.0
RUN
RUN
OK
Current sample
RUN
No. 1 of 3
Balance*
Sample ID
Method ID
45320
00001
OK
OK
RUN
No. 1 of 3
Sample ID
Method ID
45320
00001
OK
Notes
1. If you have defined an expiry date for the titrant and this has lapsed, an appropriate
message follows the "Defined are" mask. In order to determine a titer before the sample
analysis, you can confirm the message with Esc.
2. When the sample data mask or that of the "Current sample" appears, the sample is active
in the sample data memory. The titrator executes the Sample function of the method and
starts to acquire the time for every determination as the raw result TIME (see Section 5.2:
Example of an analysis sequence and Section 8.1: List of symbols).
5-4
08/2004
Menu sequence
Run
3. The titrator also accepts methods which are stored on an inserted memory card or in an
attached computer: When you enter an identification whose method is not stored in the
titrator, the method is first sought on the memory card and entered (not possible with the
DL50). If the method is not stored there, it is requested from the computer and entered
(see Operating Instructions: Computer Interface Description).
Mask: Samples to be analyzed
Number samples Enter, e.g. 3; this enters a sample series.
Method ID
Enter, e.g. 00001: This calls up the method which should be used for
analysis of the samples.
If you do not know the identification of the method, press <F4> (Modify):
The method groups appear.
Confirm either user or METTLER methods: The list of these methods
appears.
Confirm the method you need for the analysis.
User
Delete
If, e.g. you have called up a method which you do not wish to use for the
analysis, you can delete it. You have this possibility available with direct
start if you confirm the "Defined are" mask with Esc (see page 5-4).
Mask: Defined are
This mask appears so that you can check whether you have attached the resources required
by the method.
You can exclude the mask from the sequence (see Section 6.7.3).
If you have not defined a resource or there is no RS or sensor option available for the defined
resource, an appropriate error message appears.
Mask: Sample No. 1 (sample data mask)
This mask does not appear if you
have defined "Fixed volume" as entry type in the Sample function
have not defined a predispensing to "factor x sample size" in the EQP/EP titration function
have defined results such as "R = Q" in the Calculation function(s) which do not require the
sample size m.
08/2004
5-5
Menu sequence
Run
If you still have to enter sample data such as the temperature for buffer solutions to be
measured in a sensor calibration, you can do this for every sample in the Sample menu (see
Section 4.1).
Sample ID
Weight
(Volume)
Limits
You can not change the limits. This information does not appear if you
have defined a fixed volume in the Sample function.
Correction factor
You can enter a value for each sample which is reconciled in the
calculations if you insert f in the formula of the Calculation function (see
Section 4.1).
Temperature
Enter that of the solution to be titrated. You can not change the value if
you have defined a temperature sensor in the Sample function.
5-6
08/2004
Analysis sequence
Run
5.2
RUN
Balance
OK
Current sample
RUN
Before you confirm this mask, fix the sample beaker to the titration stand.
No. 1 of 3
Sample ID
Method ID
45320
00001
OK
Stir function
Wait time [s]
Speed [%]
mV
RUN
Hold1)
30
80
E V curve
mL
Table
Values
Curve1)
Result list
Method: 00001
Sample 1
R1
= 29.26 %
Hold2)
RUN
1)
2)
OK
Sample No. 2
Sample ID
45321
Weight [g]
1.08723
Limits [g]
0.02 - 2.0
Correction factor f 1.0
RUN
Balance
Current sample
OK
RUN
No. 2 of 3
Sample ID
Method ID
45321
00001
OK
08/2004
5-7
Analysis sequence
Run
At the end of the series, the results of all samples appear in the display.
If you confirm this result list, the mask "Samples to be analyzed" again appears. The method
used to perform the last titration is entered as method.
In the sample data memory, all samples of this series are present as done. You can now add
samples to this series here (see Section 4.1.4).
As soon as you start a new series or an individual sample, all data of the executed series
will be deleted.
Notes
1. Changing stirrer speed
During a titration you can always activate the Stirrer key to change the stirrer speed (see
Section 6.2).
2. Method with two different titrants/sensors
If, e.g. you have to use two titrants for a back titration and have only one burette drive, the
following message (example) appears:
Change resources
RUN
OK
If you have to use two sensors to, e.g. set the pH before the actual determination with a
phototrode and have only one sensor option, "Sensor 1: DP660" appears.
The message always appears before the function in which the second resource is needed.
3. DL55/DL58: Curve display
During the EQP/EP titration or EQP/EP titration (Ipol/Upol) or pH/mV-stat function, the
command <F4> (Curve) remains active if the curve representation has been selected. You
can select the following curves for the display:
E V curve
Potential vs. Volume
E/V V curve
1st derivative (Potential vs. Volume)
log E/V V curve
1st derivative (Potential vs. Volume, logarithmic)
2E/V2 V curve
2nd derivative (Potential vs. Volume)
E t curve
Potential vs. Time
V t curve
Volume vs. Time
V/t t curve
1st derivative (Volume vs. Time)
5-8
08/2004
Analysis sequence
Run
4. Result list
a. During a titration, you can always activate the Results key to view the results generated
to date (see Section 6.5.1).
b. All results of a learn titration are marked in the display by an exclamation mark(!).
c. With a sample series, the titrator skips the list for each sample you have excluded from
the analysis sequence (see Section 6.7.3).
d. With a sample series, all menus and auxiliary functions between the individual
determinations are again accessible if you do not confirm the result list of the sample.
You can then, e.g. also modify the method used to analyze the samples of this series
(see Section 5.2.3).
This is no longer possible if you exclude the "Result list for each sample" from the
sequence (see point c.).
08/2004
5-9
Analysis sequence
Run
RUN
Balance
OK
Current sample
RUN
No. 1 of 5
Sample ID
Method ID
592
33
OK
mV
E t curve
Table
Press
Values
Curve1)
Sample
No.
Status
Wt/Vol.
1
2
3
active
ready
ready
0.0
0.0
0.0
Meth.
ID
33
592
33
593
33
594
Print
Modify
Sample No. 1
Sample ID
592
Weight [g]
0.1456
Limits [g]
0.02 - 2.0
Correction factor f
1.0
Add
SAMPLE
Balance
Press
Hold2)
OK
Run
mV
E t curve
Table
5-10
Values
Curve
Hold
08/2004
Analysis sequence
Run
5.2.1
5.2.2
Analysis is interrupted
RUN
Measured values
6.789
265.9
RUN
mL
mV
Table
Curve
Proceed
You can now confirm "Proceed" (the analysis is continued) or press the Results key to
perform the reevaluation, see Section 6.5.2.
08/2004
5-11
Analysis sequence
Run
Note: If a method is interrupted which is not stored in the titrator but has been requested from
the computer or a memory card, a reevaluation is not possible (see Section 5.1: Note
3 and Section 6.5.2).
5.2.3
After every sample determination, you can modify the method used to perform the series. A
requirement is that you do not exlude the "Result list for each sample" from the analysis
sequence (see Section 6.7.3).
If you wish to modify the functions of the method,
all parameters of the Sample function are blocked with the exception of the numeric
parameters you have defined for the ST20A titration stand.
with all other functions you can change only the numeric parameter values.
When you save the method, the printer automatically records the complete method with the
modified values: these remain stored for the method.
To continue the sample series, press the Run key twice: The prompt to insert the next sample
appears.
Note: You can not change a method which is not stored in the titrator but is requested from
the computer or the memory card.
5.2.4
Aborting analysis
If you wish to abort the sample which is currently being titrated, press the Reset key. The mask
"METTLER TOLEDO/DL5x/Version x.x" appears.
If you abort the sample at a time at which a result has already been calculated this is
displayed in the result list (auxiliary function "Results"). If no result has been calculated, only
the sample number will be listed.
Individual sample
The sample is present in the sample data memory as done and is deleted as soon as you start
the analysis of a new sample.
Sample series
A series is not aborted with Reset: The sample is present in the sample data memory as done.
With Run the display for the remaining samples of the series appears (example):
Samples to be analyzed
2 samples,
Method 00001
Delete
5-12
RUN
Start
08/2004
Run
5.3
If you confirm "Hold" during a sample determination, the titrator stops the function it is currently
executing. You can then modify the method used to analyze the sample:
- Press the Method key (example):
Methods
Method ID
METHOD
00001
Modify
Notice
METHOD
08/2004
5-13
Run
5-14
08/2004
Run
5.4
You can store three sample series in the sample data memory of the DL55/DL58. These are
processed in this menu by the titrator in sequence with your help. An attached sample changer
automates this procedure.
You can check the ongoing method in the Sample menu (see Section 4).
As soon as the next sample series is started, all data of the executed series are deleted. At
the end of the processed sample series, only the data of the last series remain stored. They
are deleted as soon as you start the determination of a new sample or series.
With all titration stands, the sample data mask appears only if you have not entered the weight
(volume) for the samples before the start of the method.
If you work with titration stand 1, 2 or an external stand, you must confirm the mask "Current
sample" for every sample.
If you have attached a sample changer, the titrator titrates the samples of all measurement
methods without the need for your intervention. A requirement is that
you have entered all sample data
you have excluded the mask "Defined are" from the analysis sequence (see Section 6.7.3)
the methods use the same resources or their setup data are defined at the other drive
(titrants), at a different sensor option (sensors) or at the other ST20A output (solvents) (see
comparison of the titration sequences on the following page).
If you work with the auto stand, the mask "Current sample" does not appear, in other words
each sample determination is started without confirmation. As a result, you can attach a robot
to handle sample changing. The same prerequisites hold for the automatic running of sample
series as for the use of the sample changer.
Note: All information concerning automation in this titrator's Reference Handbook relates to
the earlier METTLER TOLEDO Sample changer ST20A. Its name continues to appear
in some places. Operation of other METTLER TOLEDO sample changers via your
titrator is described in the corresonding Operating Instructions.
08/2004
5-15
Run
Comparison of the analysis sequences for three sample series at the ST20A titration stand or at stand 1, 2 or the
external stand. (The masks "Defined are" and "Result list for each sample" are excluded from the sequence for
stand 1/2/external.)
Samples to be analyzed
3 samples,
Method 00001
6 samples,
Method 2
10 samples,
Method 8
Delete
ST20A
Current sample
RUN
Start
Current sample
Stand 1/2/external
RUN
No. 1 of 3
No. 1 of 3
Sample ID
Method ID
RUN
Sample ID
Method ID
45320
00001
45320
00001
OK
The mask "Current sample" appears for every sample, but is confirmed automatically.
The titrator titrates all samples of method 00001.
It then starts to titrate the samples of method 2 (the
setup data are the same as for method 00001).
It then starts to titrate the samples of method 8 (the
setup data are the same as for method 00001). At the
end of all sample determinations of method 8, the
following appears:
Result list
Method: 8
Sample 1
R1 = 97.386 %
Sample 2
RUN
OK
Current sample
RUN
No. 1 of 6
Sample ID
Method ID
11
2
RUN
OK
OK
Result list
Method: 2
Sample 1
R1 = 4.234 mmol
R2 = 2.31 g/L
RUN
OK
Current sample
RUN
No. 1 of 10
Sample ID
Method ID
432148
8
OK
08/2004
Run
If the titrator has to process methods which have the same burette drives or sensor inputs in succession on the
sample changer, you have to intervene:
Samples to be analyzed
4 samples,
7 samples,
RUN
Method 00001
Method 111
Delete
Start
Current sample
RUN
No. 1 of 4
Sample ID
Method ID
45320
00001
RUN
Place the burette with the EDTA solution on burette drive 2 and attach the DP660/DP5 Phototrode to sensor input 1 (pH option in slot 1) and
plug into titration stand.
OK
08/2004
5-17
Auxiliary functions
Contents
Page
6.
6-3
6.1
6.1.1
6.1.2
6.1.3
6.1.4
Sensor ........................................................................................................
Measure potential........................................................................................
Measure temperature ..................................................................................
Calibrate temperature sensors ....................................................................
Measure voltage/current (Ipol/Upol) ............................................................
6-4
6-4
6-5
6-6
6-7
6.2
Stirrer .........................................................................................................
6-8
6.3
6.3.1
6.3.2
6.3.3
6.4
6.4.1
6.4.2
6.4.3
6.4.4
6.4.5
6.4.4
6.4.6
Burette ........................................................................................................
Rinse burette ...............................................................................................
Rinse tip ......................................................................................................
Dispense .....................................................................................................
Dispense continuously ................................................................................
Titrate manually ...........................................................................................
Dispense continuously (Ipol/Upol) ...............................................................
Titrate manually (Ipol/Upol) .........................................................................
6-11
6-11
6-12
6-12
6-13
6-14
6-15
6-16
6.5
6.5.1
6.5.2
6.5.3
6.5.4
6.5.5
Results .......................................................................................................
Display result list .........................................................................................
Perform reevaluation ...................................................................................
Perform calculations ....................................................................................
Display measured values ............................................................................
Modify statistics ...........................................................................................
6-18
6-18
6-18
6-20
6-21
6-22
6.6
08/2004
6-1
Auxiliary functions
Page
6.7
6.7.1
6.7.1.1
6.7.1.2
6.7.1.3
6.7.1.4
6.7.1.5
6.7.1.6
6.7.2
6.7.3
6.7.4
6.7.5
6.7.6
Miscellaneous ............................................................................................
Define titrator settings .................................................................................
Date/time format ..........................................................................................
Date/time .....................................................................................................
Language ....................................................................................................
Report header .............................................................................................
Titrator ID ....................................................................................................
Audio signal .................................................................................................
Adjust measuring inputs ..............................................................................
Shorten analysis sequence .........................................................................
Define user level .........................................................................................
Activate control input ...................................................................................
Activate control output .................................................................................
6-26
6-26
6-26
6-27
6-27
6-27
6-27
6-28
6-28
6-30
6-31
6-32
6-33
6.8
6.8.1
6.8.2
6.8.3
6.8.4
6-36
6-36
6-40
6-42
6-43
6-2
08/2004
Auxiliary functions
6.
Auxiliary functions
You can use these symbol keys to perform the activities mentioned below. These auxiliary
functions are independent of a titration method, but they can support or supplement a method.
While a titration is running, you can activate only the functions of the Stirrer and Results keys,
all other keys are blocked.
Measure potential or temperature of a solution
Calibrate temperature sensors
Measure voltage/current (Ipol/Upol)
Sensor
Burette
Results
Print out additional reports of the series last performed or sample last
titrated
Report
Misc.
...
Data
Transfer
08/2004
Copy data from titrator to the memory card and vice versa (not possible
with DL50)
Transfer data from the titrator to the computer
Select whether titrator should be controlled by the computer
Enter bar-code string (computer transfer)
METTLER TOLEDO DL50/DL53/DL55/DL58
6-3
Sensor
6.1
Sensor
When you press the Sensor key, the following auxiliary functions appear:
Measure potential
Measure temperature
Calibrate temperature sensors
Measure voltage/current (Ipol/Upol)
6.1.1
Measure potential
You can measure the potential of solutions (mV, pH, %T, etc.).
Sensor
Unit of meas.
Titration stand
Speed [%]
Temperature [C]
Temperature sensor
Report
t [s]
Sensor
Unit of measurement
DG111
mV
Stand 1
50
25.0
Manual
No
5
Press <F4> to open the list containing the sensors you have defined in
the Setup menu (see Section 2.2). Confirm the one you want with OK.
The defined measurement unit is entered automatically.
You can select a different measurement unit from the selection menu
(press <F4>).
Titration stand
Speed
Temperature
Temp. sensor
Report
t [s]
6-4
08/2004
Sensor
6.1.2
Measure temperature
TEMP A
C
Stand 1
50
No
5
Temp. sensor
Unit of meas.
Titration stand
Speed
Report
t [s]
08/2004
6-5
Sensor
6.1.3
You can calibrate your Pt100 or Pt1000 sensors. The zero point determined by this procedure
is entered together with the date in the parameter mask of the corresponding temperature
sensor (see Section 2.3).
Calibrate temperature sensors
Temperature sensor
Esc
Temp. sensor
SENSOR
TEMP A
Modify
Start
6-6
08/2004
Sensor
6.1.4
You can measure the voltage or the current of solutions with polarized sensors (mV, A).
Sensor
Indication
Titration stand
Speed [%]
Report
t [s]
DM142
Voltametric
Stand 1
50
No
5
Sensor
Press <F4> to open the list containing the polarized sensors you have
defined in the Setup menu (see Section 2.4). Confirm the one you want
with OK.
Indication
Titration stand
Speed
Report
t [s]
08/2004
6-7
Stirrer
6.2
Stirrer
You can start the stirrer and change its speed, e.g. to dissolve a substance.
Stirrer
Titration stand
Speed [%]
STIRRER
Stand 1
50
Modify
Start
Titration stand
Speed
STIRRER
50
OK
Change the speed and confirm with OK: the stirrer stirs at the new speed or is at a standstill
if you have entered zero.
To follow the analysis sequence in the display again, press the Run key.
6-8
08/2004
Changer
6.3
Sample changer
Note: All information concerning automation in this titrator's Reference Handbook relates to
the earlier METTLER TOLEDO Sample changer ST20A. Its name continues to appear
in some places. Operation of other METTLER TOLEDO sample changers via your
titrator is described in the corresonding Operating Instructions.
You can control the sample changer (titration stand: ST20A) and the attached pumps/
dispensers manually. For this you must define the sample changer in the Setup menu and have
attached it (see Section 2.7.4).
Sample changer
CHANGER
6.3.1
Esc
Position
CHANGER
bottom
Modify
Start
08/2004
6-9
Changer
6.3.2
Rotate turntable
Rotate turntable
Direction
Number of positions
CHANGER
forward
1
Esc
Modify
Start
Direction
Number of
positions
6.3.3
Dispense/rinse
If you have attached a pump or a dispenser to an ST20A output, you can dispense or rinse the
sensor in the titration vessel.
Dispense/rinse
ST20A output
Esc
ST20A output
CHANGER
RINSE
Modify
Start
6-10
08/2004
Burette
6.4
Burette
When you press the Burette key, the following auxiliary functions appear:
Rinse burette
Rinse tip
Dispense
Dispense continuously
Titrate manually
Dispense continuously (Ipol/Upol)
Titrate manually (Ipol/Upol)
6.4.1
Rinse burette
Rinse burette
Burette drive
Esc
Burette drive
BURETTE
Drive 2
Modify
Start
08/2004
6-11
Burette
6.4.2
Rinse tip
Rinse tip
Burette drive
BURETTE
Drive 2
Esc
Burette drive
Modify
Start
6.4.3
Dispense
BURETTE
Drive 2
10 mL
1.0
Modify
Burette drive
Burette volume
Volume
Start
6-12
08/2004
Burette
6.4.4
Dispense continuously
You can dispense stepwise and follow the potential change as a function of the dispensing in
the display. You must define the following parameters:
Burette drive
Burette volume
Rate [mL/min]
Sensor
Titration stand
Speed [%]
Temperature [C]
Temperature sensor
Drive 2
10 mL
1.0
DG111
Stand 1
50
25.0
Manual
Burette drive
Burette volume
Rate
Sensor
Press <F4> to open the list containing the sensors you have defined in
the Setup menu. Confirm the one you want with OK. The sensor acquires
the measured values in the measurement unit you have defined for this
sensor (see Section 2.2.2).
Titration stand
Speed
Temperature
Temp. sensor
08/2004
6-13
Burette
6.4.5
Titrate manually
You can titrate manually and follow the potential change as a function of the dispensed volume
in the display. You must define the following parameters:
Titrant
Concentration [mol/L]
Sensor
Unit of meas.
Titration stand
Speed [%]
Temperature [C]
Temperature sensor
Titrant
Concentration
Sensor
Unit of measurement
NaOH
0.1
DG111
mV
Stand 1
50
25.0
Manual
Press <F4> to open the list containing the titrants you have defined in the
Setup menu (see Section 2.1). Confirm the one you want with OK.
The defined concentration of the titrant is entered automatically.
Press <F4> to open the list containing the sensors you have defined in
the Setup menu (see Section 2.2). Confirm the one you want with OK.
The defined measurement unit is entered automatically.
You can select a different measurement unit from the selection menu
(press <F4>).
Titration stand
Speed
Temperature
Temp. sensor
6-14
08/2004
Burette
Use <F5> to start, interrupt and continue the titration, use <F1> to
terminate it.
Start:
Hold:
The results are displayed: the volume in "mL" and "mmol" and the potential in the selected measurement unit. You can print out these results.
6.4.6
You can dispense stepwise and follow the voltage and current change as a function of the
dispensing in the display. You must define the following parameters:
Burette drive
Burette volume
Rate [mL/min]
Sensor
Indication
Titration stand
Speed [%]
Drive 2
10 mL
1.0
DM142
Voltametric
Stand 1
50
Burette drive
Burette volume
Rate
Sensor
Press <F4> to open the list containing the polarized sensors you have
defined in the Setup menu (see Section 2.4). Confirm the one you want
with OK.
08/2004
6-15
Burette
Indication
Titration stand
Speed
6.4.5
You can titrate manually and follow the voltage or current change as a function of the dispensed volume in the display. You must define the following parameters:
Titrant
Concentration [mol/L]
Sensor
Indication
Titration stand
Speed [%]
Titrant
Concentration
Sensor
6-16
1/
I2
0.1
DM142
Voltametric
Stand 1
50
Press <F4> to open the list containing the titrants you have defined in the
Setup menu (see Section 2.1). Confirm the one you want with OK.
The defined concentration of the titrant is entered automatically.
Press <F4> to open the list containing the polarized sensors you have
defined in the Setup menu (see Section 2.4). Confirm the one you want
with OK.
08/2004
Burette
Indication
Titration stand
Speed
Hold:
The results are displayed: the volume in "mL" and "mmol" and the voltage
value in "mV" or the current value in "A". You can print out these results.
08/2004
6-17
6.5
Results
Results
You can also press the Results key during a titration. The following auxiliary functions can be
executed:
Display result list
Perform reevaluation1)
Perform calculations
Display measured values
Modify statistics
1) appears only when the titrator interrupts the analysis (see Section 6.5.2)
6.5.1
You can view the results generated in the titration of a sample or a sample series. The list is
displayed at the earliest (press <F5>) during the first titration (only "Method ID" and "Sample
1" appear if no result is available).
6.5.2
Perform reevaluation
The parameters for the reevaluation of an EQP titration are displayed when the titrator
interrupts the current EQP titration or EQP titration (Ipol/Upol) function immediately before
completion as the defined condition for the Stop for reevaluation parameter is met (see
Sections 3.3.6.7 and 3.3.9.8). In such a case, the message "Reevaluation required" appears
(see Section 5.2.2) and you can modify the following parameters under this auxiliary function
(example):
Threshold
Steepest jump only
Range
Tendency
Potential 1
Potential 2
Maximum volume
1000
No
Yes
Positive
No
No
5
6-18
08/2004
Results
08/2004
6-19
Results
6.5.3
Perform calculations
At the end of a titration, you can perform additional calculations for these samples. The function
appears when you press the Results key on completion of the titration. In the case of a sample
series, this is possible only if the "Result list for each sample" is not excluded from the sequence of a series (see Section 6.7.3).
DL55/DL58: The auxiliary function also appears if you interrupt the titration and then press
the Results key.
When you select the auxiliary function, the following parameters appear:
Formula Rx =
Constant Cx =
Decimal places
Result unit
Result name
Q*Cx/m
M/(10*z)
3
%
Formula
Press <F4> to open the "List of formulas" and accept a different formula
from the list or enter the one you need for your calculation (see also
Section 8.4: Examples of formulas).
Constant
Press <F4> to open the "List of constants" and accept a different constant
from the list or enter the one you need for your calculation.
Symbol
You can take the symbols you need for your calculation from the list you
obtain when you press <F3>. This includes all symbols possible for the
individual functions (see Section 3.3.12: Calculation function and Section
8.1: List of symbols).
Decimal places
Enter the number of decimal places you wish to have in your result.
Result unit
Result name
6-20
08/2004
6.5.4
Results
On completion of every titration, you can display the table of measured values or view the
titration curve of this sample again. The function appears when you press the Results key at
the end of the titration. With a sample series, this is possible only if the "Result list for each
sample" is not excluded from the sequence of the series (see Section 6.7.3).
When you select the auxiliary function, the following appears (example):
Measured values
RESULTS
5.621 mL
-267.3 mV
Table
Curve1)
OK
You can view either the table of measured values, the measured value
pair Potential/Volume or the titration curve.
1)
DL50:
DL53:
With the "(display) Curve" command, the E-V curve is shown in the case of an EQP/
EP titration and the E-t curve with a pH-stat titration.
1) DL55:
The "(display) Curve" command remains active when you have selected it. Press
<F4> to show the selection menu from which you can select one of the possible
curve representations:
DL58:
E V curve
E/V V curve
log E/V V curve
2E/V2 V curve
E t curve
V t curve
V/t t curve
Potential vs Volume
1st derivative (Potential vs Volume)
1st derivative (Potential vs Volume, logarithmic)
2nd derivative (Potential vs Volume)
Potential vs Time
Volume vs Time
1st derivative (Volume vs Time)
08/2004
6-21
6.5.5
Results
Modify statistics
If you have selected Statistics: Yes in the method under the Calculation function(s), the mean
value is calculated with a sample series of 2 samples, with more than 2 samples you also obtain
the standard deviation and the relative standard deviation. This auxiliary function is then
accessible under the Results menu to modify the statistical evaluation, i.e. to allow elimination
of outliers.
The function appears when you press the Results key on completion of every titration. This is
possible only if the "Result list for each sample" is not excluded from the sequence of the series
(see Section 6.7.3).
Modify statistics
RESULTS
Display evaluation
Delete result
Undo deletion
Esc
Display
evaluation
OK
n
x
s
RESULTS
= 6
= 1.234 %
= 0.01268 %
OK
Delete result
Using the result list you decide what sample result is an outlier and then
delete it.
Delete result
Sample No.
Result R
RESULTS
1
1
Esc
OK
Enter the number of the sample whose result should be deleted, e.g.
2.
Enter the number (index) of the result defined by the Calculation function.
6-22
08/2004
Delete result
Results
If you confirm OK, the result is deleted and the statistical data are
calculated with the new number of samples. You can delete several
sample results and always view the final result in the mask "Statistical
evaluation" (example):
Statistical evaluation
s
= 0.00346 %
srel = 0.112 %
Outlier
Sample No. 2 deleted
RESULTS
OK
You can use the parameter "All results" of the auxiliary function Report
to print out the new evaluation (see Section 6.6).
Undo deletion
As long as the result list of this sample series remains stored, you can
undo the deletion for all sample results:
Undo deletion
Sample No.
Result R
RESULTS
1
1
Esc
OK
Enter the number of the sample and that of the corresponding result R:
The result of this sample will be reincorporated in the statistical
calculation.
08/2004
6-23
Report
6.6
Report
On completion of each sample series, you can print out additional reports or transfer them to
a computer (see also Section 3.3.16: Report function). In the case of a sample series, this is
possible only if you have not excluded the "Result list for each sample" from the sequence of
the series (see Section 6.7.3).
DL55/DL58: You can activate the auxiliary function if you interrupt the titration and then press
the Report key.
Report
Output
Printer
Results
All results
REPORT
No
No
Modify
Start
Output
Press <F4> to select the output unit to which the data should be sent:
Printer,
Memory card (not with the DL50)
Computer,
Printer + memory card (not with the DL50) or
Printer + computer.
Results
All results
Results of all samples generated to date are recorded when you select
"Yes" with <F4> and press <F5>. They also include the statistical data if
these have been calculated (see Section 6.5.5).
Raw results
The raw results of the sample last determined are recorded when you
select "Yes" with <F4> and press <F5>.
Table of
The table of measured values of the sample last determined is recorded
measured values when you select "Yes" with <F4> and press <F5>.
Sample data
The sample data of all samples of the current series are recorded when
you select "Yes" with <F4> press <F5>.
E V curve
6-24
08/2004
Report
E/V V curve
The 1st derivative of the titration curve Potential vs Volume of the sample
last determined is recorded when you select "Yes" with <F4> and press
<F5>. The ordinate representation is linear.
log E/V V
curve
The 1st derivative of the titration curve Potential vs Volume of the sample
last determined is recorded when you select "Yes" with <F4> and press
<F5>. The ordinate representation is logarithmic.
2E/V2 V
curve
The 2nd derivative of the titration curve Potential vs Volume of the sample
last determined is recorded when you select "Yes" with <F4> and press
<F5>. The ordinate representation is linear.
E t curve
V t curve
V/t t curve
The 1st derivative of the titration curve Volume vs Time of the sample last
determined is recorded when you select "Yes" with <F4> and press <F5>.
08/2004
6-25
Misc.
...
6.7
Miscellaneous
6.7.1
You can or must select or define the following settings for the titrator:
Date/time format
Date/time
Language
Report header
Titrator ID
Audio signal
6.7.1.1
Date/time format
You have several possibilities for the date and time notation. If you wish to change the existing
formats, select this menu line and press <F4>:
Formats
Date format
Time format
MISC.
17-OCT-1995
17:04 (24 h)
Esc
Modify
Date format
Time format
OK
If you change the formats, e.g. after a month they are transferred to all
data stored at the time.
6-26
08/2004
Misc.
6.7.1.2
...
Date/time
To change the date or the time, select this menu line and press <F4>; the mask appears in
which you can overwrite the date.
6.7.1.3
Language
In the titrator all texts are stored in English, German, French, Italian and Spanish. To change
the active language, select this menu line and press <F4>:
Language
Active language
Esc
Active language
6.7.1.4
MISC.
English
Modify
OK
Report header
If you wish to enter an identifier or a text (with attached keyboard) which should appear in the
header of every report of a titration method, select this menu line and press <F4>:
Report header
MISC.
Text:
Text:
Esc
6.7.1.5
OK
Titrator ID
If you wish to enter an identification for your titrator this is always recorded select this menu
line and press <F4>; the mask appears in which you can enter an identification.
08/2004
6-27
Misc.
...
6.7.1.6
Audio signal
An audio signal confirms either every keystroke or draws your attention to instructions, notes
and error messages. When the titrator is delivered, all these parameters are assigned a signal.
To change this, press <F4>:
Audio signal
Keystroke
Results
Messages
Esc
MISC.
Yes
Yes
Yes
Modify
OK
Keystroke
Results
Yes: A brief signal sounds after every result that appears in the display.
If you do not wish to hear this, press <F4>: "No.
Messages
Yes: A signal draws your attention to error messages, notes and instructions.
If you do not wish to hear this, press <F4>: "No.
6.7.2
The measuring inputs for sensors and temperature sensors must be adjusted to ensure the
titrator measures potential and temperature values correctly.
The adjustment of the measuring inputs is performed by METTLER TOLEDO and the calibration
data of the characteristic line of each input recorded on a data sheet, which is enclosed with
every sensor option (see Section 10.5.1).
The measuring inputs of the pH option installed in slot 1 of the titrator in the factory are adjusted;
the calibration data are stored and can be printed out (see mask).
Measuring inputs
MISC.
Option in slot 1
Option in slot 21)
Esc
1)
6-28
Modify
OK
08/2004
Misc.
...
Notes
1. If you receive a data sheet with a pH option which contains instructions for the entry of the
calibration data, you must follow these: If, for example, you install this or an additional option
in slot 2, you must enter the data of the data sheet for slot 2 (overwrite default values!).
Calibration data
Sensor 1:
Temp 1 (Pt100):
Esc
MISC.
Offset
Slope
Offset
0
30950
-15463
OK
2. If you receive a data sheet with a pH option which contains only calibration data, these are
stored on the option itself. They are automatically adopted for every slot and can not be
deleted. In this case you can only view the data:
Calibration data
Sensor 1:
Temp 1 (Pt100):
Esc
MISC.
Offset
Slope
Offset
0
30950
-15463
OK
3. You always receive a data sheet with a KF option which contains only calibration data, in
other words the data are stored on the option and are automatically adopted for each slot;
they can not be deleted:
Calibration data
Sensor 2 (Ipol):
Sensor 2 (Upol):
Esc
08/2004
MISC.
Offset
Slope
Offset
0
26025
0
OK
6-29
Misc.
6.7.3
...
Shorten analysis sequence
During the sequence of an analysis, information is shown in the display which you must confirm
with OK to allow the titrator to continue working:
the mask "Defined are" appears at the start (see Section 5.1), and
on completion, the "Result list" for every titrated sample within a series (see Section 5.2).
You can exclude these two masks from the analysis sequence to accelerate it.
Shorten analysis sequence
MISC.
Defined resources
Result list for each sample
Esc
Yes
Yes
Modify
OK
Defined
resources
Result list
for each sample
Yes: Within a sample series the result list appears after the determination
of each sample if you are working with titration stand 1, 2 or external.
If this is not required, select "No" with <F4>.
With series which you perform at a sample changer (titration stand:
ST20A) or at an auto stand, the mask is skipped automatically (see
Sections 5.1 and 5.4).
6-30
08/2004
Misc.
6.7.4
...
You can decide if all people who work with the titrator should also have access to the Setup
or Method menu, i.e. have the possibility to delete resources or modify methods. If you have,
e.g. temporary staff who can perform only routine analyses, it is good practice to block their
access to these menus.
Define user level
User level
Esc
MISC.
Expert
Modify
OK
Expert
In the factory setting of the titrator, you have access to all menus. To
change this, select "Routine" with <F4>.
Routine
In the Setup menu you can only print out the defined resources.
In the Method menu you can only print out the methods.
In the Data transfer menu, you can not
- transfer data to the computer
- remote-control the titrator
- transfer data to and from the memory card
- delete data on the memory card
- format a memory card.
In the Analysis menu you can not modify an ongoing method (DL55/
DL58: see Section 5.3).
Expert
MISC.
Routine
Esc
OK
and while holding down the Shift key, press key 1 three times: "Expert"
and the "Modify" command reappear.
08/2004
6-31
Misc.
6.7.5
...
Activate control input
The RS option has a socket whose two TTL inputs you can activate (see Section 10.7). To do
this, you must have
installed the option in the third slot,
attached the devices whose signal should be scanned.
Activate control input
Input
In 3.1
Esc
Input
MISC.
Modify
Start
Level sensor
500 mL
If the container holds more than 500 mL, the sensor sends the input
signal Off.
If the container holds less than 500 mL, the sensor sends the input
signal On to indicate that the container should be filled.
6-32
08/2004
Misc.
6.7.6
...
The RS option has a socket whose four TTL outputs you can control (see Section 10.7). To
do this, you must have
installed the option in the third slot
attached the devices you intend to control.
Note: TTL are signals which do not transfer power. To operate devices such as a pump,
you must connect an amplifier in the circuit (see Section 10.7)
Activate control output
Output
Control mode
MISC.
Out 3.1
On/Off
Esc
Modify
Start
Output
Press <F4> to select: "Out 3.2", "Out 3.3", "Out 3.4" or Out 3.1".
Control mode
MISC.
In 3.1
Normal
Modify
OK
6-33
Misc.
...
Control mode
Example: A pump is attached via a TTL output, a level sensor via a TTL
input:
TTL socket
Container with
level sensor
Pump with
supply vessel
The titrator checks at the start whether the signal of the selected input is
in Section 6.7.5).
With this voltage of 0 V the titrator controls the pump (normal output
signal) so that it starts to pump liquid from the supply vessel into the
container with the level sensor.
As soon as this container holds more than 500 mL, the pump is switched
off automatically.
Inverted: The pump can be controlled only with the 5 V signal instead of
the normal output signal of 0 V. When the pump is switched off,
the voltage is 0 V.
Sequential
You can use this special mode to control, e.g. a dispenser.
Sequential
Number of pulses
Pulse duration [s]
Interval [s]
Esc
MISC.
10
1.0
1.0
OK
6-34
08/2004
Misc.
Control mode
1st pulse
Interval
Off
...
3rd pulse
Pulse duration
On
08/2004
6-35
Data
Transfer
6.8
Data transfer
With the DL53, DL55 and DL58 you can back up your data on a memory card. You can also
transfer the data to a computer or control the titrator from the computer; for this you can enter
a bar-code string.
Memory card
Computer 1)
Remote control1)
Bar-code string
1)
1) These
parameters do not appear until you have defined the computer in the Setup
menu (see Section 2.7.3)
6.8.1
Memory card
You can use a memory card with the DL53, DL55 and DL58 to
1.
store user methods and resources when the user data memory is full
back up all data of the user data memory, i.e. resources and user methods.
You can reload these data when needed on the same or on another titrator of the same
type. The cards you can use are listed in Section 12.8, insertion information in Section
10.6).
2.
store reports of analyses.
You can print these out from the card at any time.
DL50: You can use only a memory card supplied by METTLER TOLEDO to load a new software
version.
Formatting a new card
Remove the write protection of the card and insert card.
Confirm "Memory card" with OK: The message "Card not readable" appears. If you confirm
this with OK, the following appears:
Format card
DATA TRANSFER
Esc
6-36
Start
08/2004
Data
Transfer
Start: The card is formatted and the end of the operation displayed.
Note: Formatting of a 1 MB SRAM card takes approx. 30 seconds, that of a 2 MB Flash card
approx. 4 minutes.
The formatting generates a directory and commands.
Confirm "Memory card" in the Data Transfer mask again:
Display directory
Copy from titrator to card
Copy from card to titrator
Format card
Directory
Directory
User methods
Resources
Memory copies
Reports
Esc
DATA TRANSFER
OK
18-Oct-1996
22-Oct-1996
22-Oct-1996
Delete
DATA TRANSFER
11:48
14:34
10:03
OK
<F5> shows the list of the reports for each sample of the series (see
following page):
08/2004
6-37
Data
Transfer
Directory
Reports (samples)
1 [1] 18-Oct-1996
2 [1] 18-Oct-1996
3 [1] 18-Oct-1996
Esc
Delete
DATA TRANSFER
11:48
12:01
12:23
Print
1, 2 and 3 refer to the sample No., [1] to the number of the Report function
(index, relevant only with special methods). [*] appears if the report has
been sent by the auxiliary function Report (Report key).
<F4> prints out the results and/or curves defined in the function.
From titrator...
Copy to card
DATA TRANSFER
User methods
Resources
Memory copy
Esc
OK
DATA TRANSFER
Method ID
Esc
Modify
Start
Enter the identification of the method; if you do not know this, press <F4>:
The list of user methods appears from which you can select the one you
wish to copy.
If a method with the same ID is stored on the card, an appropriate
message appears.
Resources: <F5> is used to show the list of resources from which you
can select those you wish to copy. Resources stored on the card will be
overwritten.
6-38
08/2004
Data
Transfer
From titrator...
DATA TRANSFER
Start
You use this procedure to generate a backup copy of the user data
memory.
Start: All stored resources and user methods are copied and stored as
"memory copies" on the card with date and time (see following
page). During the copying operation, the message "Data are transferred" appears.
From card...
Copy to titrator
User methods
Resources
Memory copies
Esc
DATA TRANSFER
OK
User methods: Use <F5> to show the mask of the method ID. If you do
not know the identification, press <F4>: The list of user methods appears
from which you can select the one you wish to copy.
If a method with the same ID is stored in the user data memory, an
appropriate message appears.
If the sample data list contains data, you can not copy the method until
you have deleted these data (see Section 4).
Resources: Use <F5> to show the list of resources from which you can
select those you wish to copy.
Titrants stored in the titrator are overwritten if their names and concentrations are the same as the titrants being copied. All other titrants
remain stored.
Sensors and solvents stored in the titrator are overwritten if their names
are the same as those being copied.
All other resources are overwritten (temperature sensors, auxiliary
values, titration stands, peripherals).
08/2004
6-39
Data
Transfer
From card
DATA TRANSFER
16:45
10:12
14:34
Load
Start
DATA TRANSFER
Start
Start: All data of the user data memory are overwritten by those of the
memory copy of Oct. 10, 1996.
If the sample data list contains data, you can not load the copy
until you have deleted these data (see Section 4).
Format card
6.8.2
To delete all data on the card in one operation, you can reformat the card
(see start of this section).
Computer
You can transfer user methods and/or defined resources from the titrator to a computer. A
requirement for this is that you have
defined the computer in the Setup menu and attached it
loaded the DLWin or the LabX titration software or an appropriate program.
Switch on the computer and start required program.
Confirm "Computer" with OK:
Computer
DATA TRANSFER
Esc
6-40
OK
08/2004
Data
Transfer
From titrator...
Transfer to computer
DATA TRANSFER
User methods
Resources
Memory copy
Esc
OK
User methods: Use <F5> to show the mask with the method ID. If you
do not know the identification, press <F4>: the list of user methods
appears from which you can select the one you wish to transfer.
Resources: Use <F5> to show the list of resources from which you can
select those you wish to transfer.
Memory copy: With <F5> the following appears:
Transfer
DATA TRANSFER
Start
Start: All data except those in the sample data memory are transferred.
During the operation, the message "Data are transferred" appears.
Note: You can also transfer data stored in the computer back to the titrator. You will find further
information in the Operating Instructions of the computer interface or in the Operating
Instructions of the DLWin or the LabX titration software.
08/2004
6-41
Data
Transfer
6.8.3
Remote control
You determine whether the titrator is controlled exclusively by a computer. The requirement
for this is that you have loaded the DLWin or the LabX titration software or an appropriate
program.
Remote control
DATA TRANSFER
Status
Off
Esc
Status
Modify
OK
Press <F4> to select "On": The titrator can be controlled only by the
computer, i.e. you can neither enter data on the titrator, nor start an
analysis nor execute an auxiliary function.
When you have confirmed "On", all that appears is:
Data transfer
DATA TRANSFER
Remote control
Bar-code string
Esc
OK
To follow the entries and commands of the computer in the display of the titrator, you can use
the following keys:
Arrow keys
Scroll parameters of a mask
Run key
Display of the active function of an ongoing method
Sample key
Sample data list
Data transfer key
Switch off remote control
Enter a bar-code string (see next section).
You will find further information on remote control in the Operating Instructions of the computer
interface or in the Operating Instructions of the DLWin or the LabX titration software.
6-42
08/2004
Data
Transfer
6.8.4
Bar-code string
This parameter is intended for automatic systems. The string which is read in by a defined and
attached bar-code reader is immediately transferred to the computer (see Section 2.7.3).
If you do not have a bar-code reader, you can enter the string here with the titrator keyboard.
Enter bar-code string
DATA TRANSFER
>
Esc
OK
When you confirm the entry with OK, the string is transferred to the
computer.
08/2004
6-43
DL58
DL58
Contents
Page
7.
7-3
7.1
7.1.1
7.1.1.1
7.1.1.2
7.1.2
7.1.2.1
7.1.2.2
7.1.2.3
7-4
7-4
7-4
7-5
7-5
7-6
7-6
7-6
7.2
7.2.1
7-7
7-7
7.3
7.3.1
7.3.2
7.3.3
7.3.4
7.3.4.1
7.3.4.2
7.3.4.3
7.3.4.4
7.3.5
7.3.6
7.3.7
7-10
7-10
7-11
7-11
7-12
7-12
7-13
7-14
7-14
7-15
7-16
7-18
08/2004
7-1
DL58
7.
DL58
The DL58
This section explains the resources, commands and functions for the development of methods
which the other three titrators do not possess. With the preloaded METTLER and standard
methods, you can change only the parameters of the functions. The DL58 memory holds
additional, Special methods which allow the insertion of identical or new functions or the
deletion of existing functions thus enabling you to develop completely new methods.
Setup menu
Method menu
Special methods
Resources
Commands
Functions
Control inputs
Add
Temperature
Control outputs
Delete
Instruction
Pump
Two-phase titration
Control input
Control output
Sync
Note: You can also run the special methods with the DL53 and DL55 if you purchase a dongle
and the special methods available on memory cards (see Section 11.2).
08/2004
7-3
Control inputs
7.1
DL58
Additional resources
"Control inputs" and "Control outputs" are available in the Setup menu as additional resources
which you must define.
7.1.1
You can use the parameters of this resource only if you have installed an RS option in the third
slot. The two inputs In 3.1 and In 3.2 of the TTLIO socket are used for the attachment of devices
whose signal should be scanned (see Sections 6.7.5 and 10.7).
If you select this menu and press <F4>, the following appears:
Control inputs (only with TTLIO)
SETUP
Esc
Add
Modify
OK
Notes
1. When the titrator is delivered, the English name for the fill level sensor is defined. Should
you wish to store the Spanish name, use the Modify command (see Section 7.1.1.1).
2. If you have added device names to the list, the Delete command appears (<F2>).
7.1.1.1
Modify
Press <F4>, "Modify", to show the parameters of the control input whose name and input you
can change.
Control input parameters
Name
Input
SETUP
Esc
Modify
OK
Name
You can change the name by pressing <F4> and selecting a new name
from the list of input names which appears.
Input
7-4
08/2004
Control outputs
DL58
Storage procedure
The definition of the control input is stored when you confirm both the parameter mask and the
list of names of the control inputs with OK. The modification of a parameter is always stored
when you press a Menu or Auxiliary function key (see corresponding paragraph at the end of
Section 2.1.2).
7.1.1.2
Add
With this command you can add a new device to the list of the defined devices. The following
mask always appears:
Control input parameters
Name
Input
SETUP
_ _ _ _ _ _ _ _ _ _ _ _ _ _
In 3.1
Esc
Modify
OK
You can modify the parameters by the procedure described in Section 7.1.1.1.
If you define, e.g. several devices with the same name, you must provide these with an
additional identification so that the titrator can distinguish them, e.g. Fill level sensor/2. If you
do not, a message appears (see Section 2.1.3).
7.1.2
You can use the parameters of this resource only if you have installed an RS option in the third
slot. The four outputs Out 3.1...Out 3.4 of the TTLIO socket are used for the attachment of, e.g.
dosing equipment (see Sections 6.7.6 and 10.7).
If you select this menu and press <F4>, the following appears:
Control outputs (only with TTLIO)
SETUP
Pump
Dispenser
Valve
Esc
Delete
OK
Add
Modify
Note: When the titrator is delivered, the English name for the stored devices is defined. Should
you wish to store the Spanish name, use the Modify command (see Section 7.1.2.1).
08/2004
7-5
Control outputs
7.1.2.1
DL58
Delete
If you press <F2>, "Delete", the device for the defined output will be deleted from the list.
7.1.2.2
Modify
Press <F4>, "Modify", to show the parameters of the control output whose name and output
you can change.
Control output parameters
Name
Output
SETUP
Pump
Out 3.1
Esc
Modify
OK
Name
You can change the name by pressing <F4> and selecting a new name
from the list of output names which appears.
Output
Select with <F4>: "Out 3.1", "Out 3.2", "Out 3.3" or Out "3.4".
Storage procedure
The definition of the control output is stored when you confirm both the parameter mask and
the list of names with OK. The modification of a parameter is always stored when you press
a Menu or Auxiliary function key (see corresponding paragraph at the end of Section 2.1.2).
7.1.2.3
Add
With this command you can add a new device to the list of defined devices. The following mask
always appears:
Control output parameters
Name
Output
Esc
SETUP
_ _ _ _ _ _ _ _ _ _ _ _ _ _
Out 3.1
Modify
OK
You can change the parameters by the procedure described in Section 7.1.2.2.
If you define, e.g. several devices with the same name, you must provide these with an
additional identification so that titrator can distinguish them, e.g. Pump/2. If you do not, a
message appears.
7-6
08/2004
Special methods
DL58
7.2
Special methods
If you press the Method key and scroll the menu downward (Shift and -key), the following
appears:
Methods
METTLER methods
Special methods
METHOD
OK
Special methods
91001
91002
METHOD
Surfactant determination
Vitamin C determination
Esc
Delete
Modify
You can change these two special methods to meet your requirements and store them under
a different method ID. Each new method is stored in the "Special methods" group.
7.2.1
Additional commands
You can modify the special method by changing or deleting its functions or by adding new
functions. Virtually all functions can occur more than once in a method.
Special method
delete
Functions
add
Parameters
08/2004
modify
7-7
Special methods
DL58
Press <F4> when the surfactant determination is selected: The list of functions appears.
Method: 91001
Add
Method: 91001
Title
Sample
Stir
Two-phase titration
Esc
Add
Method: 91001
Sample
Stir
Two-phase titration
Calculation
Esc
Delete
Add
Modify
OK
METHOD
Modify
OK
METHOD
Title
Sample
Stir
Esc
METHOD
Modify
OK
Add
You can insert a new function after every selected function (see following
page). If you select a wrong order when inserting functions (e.g. you can
not place the EQP titration function before the Sample function), an error
message appears, but not until the method is stored.
Delete
You can not delete the Title function as it is used to identify the method
and must always be placed at the head of the functions.
You can not delete the Sample function as it provides the titrator with
information regarding the titration stand at which titration is performed.
7-8
08/2004
Special methods
DL58
If, e.g. Stir is selected and you press <F3>, the list of functions you can add appears:
Stir
..............................
(6)
Measure
..............................
(10)
Temperature
..............................
(10)
Instruction
..............................
(10)
Dispense
..............................
(6)
Pump
..............................
(6)
EQP titration
..............................
(*)
EP titration
..............................
(*)
Learn titration
..............................
(*)
..............................
(*)
EP titration (Ipol/Upol)
..............................
(*)
Two-phase titration
..............................
(*)
pH/mV-stat
..............................
(2)
Control input
..............................
(6)
Control output
..............................
(6)
Calculation
..............................
(12)
Auxiliary value
..............................
(20)
Titer
..............................
(1)
Calibration
..............................
(1)
Report
..............................
(8)
Sync
..............................
(20)
Select the function you wish to add and press <F5>. It will be inserted under the Stir function.
Note: The number in brackets is the maximum possible number of this function a special
method can contain.
(*): A special method can contain maximum 6 titration functions.
08/2004
7-9
Temperature
DL58
7.3
Additional functions
7.3.1
Temperature
You can use this function to measure the temperature of a solution under defined conditions.
The titrator acquires the measured value as raw result T (see Note a. in Section 3.3.4).
Sensor
Unit of meas.
T [C, F, K]
t [s]
t(min) mode
t(max) [s]
Temp A
C
0.02
2.0
Fix
30.0
Sensor
Unit of meas.
T
t
The temperature drift must be less than T/t (0.01 C/s) during the
period t (2 s) if the temperature is to be acquired as a measured value.
This occurs within a defined time interval t(min) and t(max).
t(min) mode
t(min) is earliest time for the acquisition of the measured value. Select
t(min) from the selection menu:
t(min) mode
Fix
T > set value
T < set value
Esc
METHOD
Modify
Fix: With <F4> the mask appears in which you can change t(min).
T greater than set value: Instead of a fixed time you can select a condition: The measured value must be greater or
T less than set value:
less than a specified set value: <F4> is used
to show the mask in which you can enter the
set value [C, F, K].
t(max)
7-10
08/2004
Instruction/Pump
DL58
7.3.2
Instruction
This function allows you to intervene manually in the sequence of the titration method, in other
words the method is interrupted. The entered text appears at the desired position during the
current method in the display. The method does not continue until you confirm the instruction
with Run.
Instruction
Text
Text
Text
Esc
Text
7.3.3
METHOD
_ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _
OK
Pump
With the aid of this function you can add solvent with a pump attached to the sample changer.
Pump
METHOD
Solvent
Volume [mL]
Stir
Esc
H2O
10
No
Modify
OK
Solvent
With <F4> select the solvent from the list which contains those you have
defined in the Setup menu (see Section 2.8).
Volume
Enter the volume that should be added. You have defined the pump rate
of the device in the Setup menu.
Stir
Select whether (Yes) or not (No) stirring should be effected during the
dosing operation.
08/2004
7-11
Two-phase titration
7.3.4
DL58
Two-phase titration
This section explains the first 4 parameter groups of this titration function. The explanations
for those of the group Recognition, Termination and Evaluation can be found in Sections
3.3.6.5 through 3.3.6.7.
Titrant/Sensor
Predispensing
Titrant addition
Measure mode
Recognition
Termination
Evaluation
The titrator records several measured values and volumes as raw results (see Section 8.1).
7.3.4.1
Titrant/Sensor
7-12
Hyamine
0.004
DP550
mV
Press <F4> to open the list containing the titrants you have defined in the
Setup menu (see Section 2.1). Confirm the one you want with OK.
The defined concentration of the titrant is entered automatically.
Press <F4> to open the list containing the sensors you have defined in
the Setup menu (see Section 2.2.). Confirm the one you want with OK.
The defined measurement unit is entered automatically.
If you select the unit from the selection menu, you should select mV or the
unit defined in the Setup menu, otherwise you will receive an error
message when the method is started.
08/2004
Two-phase titration
DL58
7.3.4.2
Predispensing
Predispensing shortens the titration time. You can select one of two predispensing modes
when you press <F4>.
Predispensing
to volume
to (factor x sample size)
No
Esc
METHOD
Modify
Volume
You dispense a specified volume [mL] which you can enter when you
press <F4>. Instead of a number, you can enter a formula.
You can also enter a wait time: After the predispensing, the titrator waits
for this time to elapse before it adds the titrant in a controlled manner.
Notice: The wait time includes the time of the dosing operation!
Factor x
sample size
No
The titrator adds the volume in one step. It adopts the potential values
ET1 and ET2.
E [mV]
ET2
ET1
V [mL]
08/2004
7-13
Two-phase titration
7.3.4.3
DL58
Titrant addition
For the two-phase titration, only the incremental addition mode is available.
Titrant addition
V [mL]
METHOD
0.05
Esc
The volume increment that the titrator adds is constant (see Section
3.3.6.3: Incremental titrant addition).
7.3.4.4
OK
Measure mode
You define the duration of the mixing and separation time as well as the stirrer speed during
the separation time.
Measure mode
Mixing time [s]
15.0
Separation time [s]
50.0
Stirrer speed (sepn time) [%] 10
Esc
METHOD
OK
Mixing time
After the addition of every increment, the two phases are stirred for this
time at the speed selected in the Stirrer function.
Separation
time
During this time, the two phases should separate so that a stable
measured value of the corresponding phase can then be acquired.
Stirrer speed
You can set your "own" speed for the separation time or set it to 0.
Note: If you use the auxiliary function Stirrer to
change the speed during the mixing time, this applies only to the
mixing time during the two-phase titration and for any functions
after the two-phase titration.
change the speed during the separation time, this applies only
to the separation time during the two-phase titration.
7-14
08/2004
Control input
DL58
7.3.5
Control input
With this function you can influence the progress of a method externally via the inputs of the
TTLIO socket. This is possible only with an RS option installed in the third slot (see Section
10.7). The titrator waits for the defined signal to be detected or the maximum time to elapse
before it processes the next function.
Control input
Name
Input signal
Max. time [s]
Esc
METHOD
_ _ _ _ _ _ _ _ _ _
Rising
10.0
Modify
OK
Name
With <F4> open the list containing the names of the inputs you have
defined in the Setup menu (see Section 7.1.1). Confirm the one you wish
to use with OK.
Input signal
With Rising or Falling you specify the direction of change of the input
signal when the signal you have defined is detected.
Max. time
This time defines the wait time for detection of the signal. On elapse of this
time, processing of the method continues even if no signal has been
detected.
08/2004
7-15
Control output
7.3.6
DL58
Control output
With this function you can generate TTL signals. This is possible only with an RS option
installed in the third slot (see Section 10.7). The nature of the signal depends on the control
mode you have selected. The standard status of the control outputs is "high".
Control output
Name
Control mode
Instruction
Esc
METHOD
_ _ _ _ _ _ _ _ _ _
Fixed time
Modify
OK
Name
With <F4> open the list containing the names of the outputs you have
defined in the Setup menu (see Section 7.1.2). Confirm the one you wish
to use with OK.
Control mode
The mode determines the number and nature of the generated TTL
signals. The following modes are possible (press <F4> ): "Fixed time",
"On/Off", "Input controlled" or "Sequential".
Fixed time
Select this mode when you wish to operate a device that is attached to the
control output over a fixed time period.
Enter the time during which the control output should be switched on.
On/Off
With this mode you can, e.g. switch on a device attached to the control
output at the start of the method and switch it off at the end of the method.
Select whether the control output should be switched on or off. The
status of the control output will be automatically set to off on completion
of the method.
Input controlled
This mode allows a device attached to the control output to be switched
on or off by a device attached to the control input (e.g. pushbutton). The
function is ended when the signal at the defined control input changes or
after elapse of a maximum time.
7-16
08/2004
Control output
DL58
Control mode
Input controlled
Name
Output signal
Max. time [s]
Esc
METHOD
_ _ _ _ _ _ _ _ _ _
Normal
10.0
Modify
OK
Name: With <F4> open the list containing the names of the inputs you
have defined in the Setup menu (see Section 7.1.1). Use OK to confirm
the one which should control the control output function.
Output signal "Normal": The signal is routed directly from the control
input to the control output.
Output signal "Inverted": The signal of the control input is first inverted
and then routed to the control output.
Max. time: The maximum time defines the wait time for the signal change.
On elapse of this time, the method is processed further even if no signal
has been sent.
Sequential
Use this mode to select devices which you can use to either trigger
various actions through different sequences or repeat particular actions
through single pulses of the sequence (see Section 6.7.6).
Sequential
Number of pulses
Pulse duration [s]
Interval [s]
Esc
METHOD
10
1.0
1.0
OK
08/2004
You can enter a text which is shown while the function is active.
7-17
Sync
7.3.7
DL58
Sync
Under this function you specify the parameters for the synchronization of the titrator with an
external control unit. The synchronization takes place via the system interface (RS option in
the slot 3!).
Sync
METHOD
Sync mode
Code
Comment
Esc
Send
1
Modify
OK
Sync mode
Code
Enter a number between 1 and 32, which is sent to the external control
unit.
Comment
Notes
1. You will find additional information regarding the communication between the titrator and
the external control unit in the Operating Instructions "DL50/DL53/DL55/DL58: RS232C
Interface Description".
2. Two titrators can also be synchronized by means of the system interface using the Sync
function. You must then connect the two titrators using a null modem.
7-18
08/2004
Contents
Page
8.
8-3
8.1
8.1.1
8-3
8-8
8.2
8.2.1
8.3
8.3.1
8.3.2
8.3.3
8.3.4
8-14
8-14
8-14
8-15
8-16
8.4
8.4.1
8.4.2
8.4.3
8-17
8-17
8-18
8-19
8.5
8.5.1
8.5.2
8.5.3
8.5.4
8.5.5
8.5.6
08/2004
8-1
8-2
08/2004
List of symbols
8.
In this section you will find additional information which supplements Sections 3 to 7.
8.1
List of symbols
This list shows you the abbreviations of all symbols of the parameters and the raw results
determined by the titrator together with their definition. If you enter the symbols using an
external keyboard, you must comply with the uppercase or lowercase notation.
Function/Resource
Symbol
Titrant
ZERO
SLOPE
Auxiliary value
Sample
(Sample data)
Correction factor
TIME
Sensor
Current sample
08/2004
Definition
8-3
List of symbols
Function
EQP titration
Learn titration
Symbol
Definition
ET1
ET2
VEQ
VEX
QEX
VEND
QEND
EPOT
Calculated equivalence point potential of the equivalence or end point VEQ in the defined unit of the
sensor used
EHNV
neq
P1
P2
VP1
VP2
or potential P2
QP1
QP2
or potential P2
EP titration(Ipol/Upol)
EQP titration (Ipol/Upol)
Two-phase titration*
EQP titration
EQP titration (Ipol/Upol)
Two-phase titration*
8-4
08/2004
List of symbols
Predispensing to
a: Volume or
(factor x sample size)
b: Potential
c: Slope
E [mV]
neq = 3
3
EPOT3
EHNV3
EPOT2
EHNV2
EPOT1
EHNV1
VEQ1
Q1
VEQ2
Q2
VEQ3
Q3
VEX
QEX
V [mL]
VEND
QEND
E [mV]
+200
P1
+100
-100
P2
-200
VP1/QP1
08/2004
V [mL]
VP2/QP2
8-5
List of symbols
Function
Symbol
pH/mV-stat
Definition
VTOT
QTOT
VT1
VT2
VT
QT1
QT2
QT
CSTAT
VSTAT
QSTAT
V/
V/tt[mL/s]
[mL/s]
V [mL]
VTOT
QTOT
VT2
QT2
VSTAT
QSTAT
VT1
QT1
t [s]
t1
t2
t [s]
t1
t2
8-6
08/2004
List of symbols
Function
Symbol
Definition
Measure
Dispense
VDISP
QDISP
R
C
Calculated result
Calculation constant
Cx
Standard deviation
srel
Calculation
Temperature*
08/2004
8-7
List of symbols
8.1.1
Analysis/Function
Raw results
Current sample
TIME
no
Measure
yes
Dispense
VDISP, QDISP
yes
EQP/EP titration
Learn titration
EQP/EP titration (Ipol/Upol)
Two-phase titration*
ET1, ET2
VEQ, Q
VEX, QEX
VEND, QEND
EPOT
no
yes
yes
no
yes
EQP titration
EQP titration (Ipol/Upol)
Two-phase titration*
EHNV
neq
P1, P2
VP1, QP1
VP2, QP2
no
no
yes
yes
yes
pH/mV-stat
VTOT, QTOT
VT1, QT1
VT2, QT2
VT, QT
VSTAT, QSTAT
CSTAT
yes
no
no
no
yes
no
Temperature*
yes
Notes:
1. * Two-phase titration, Temperature: Special methods
2. To obtain the raw results which are not printed out as standard, assign these to the result
R, e.g. R = QP1, R = VT1.
8-8
08/2004
Use of indices
8.2
Use of indices
As some functions can occur a number of times within a method and parameters can also
appear a number of times within a function, indices are needed in addition to the parameter
symbol (see Section 8.2.1: Compilation of the symbols by indexing forms).
The titrator recognizes 4 different indexing forms:
1. Parameters without index
These parameters include, e.g. c, t, M, ZERO, SLOPE, TIME. The parameters always refer
to the current titrant, the current sensor or the current sample determination.
The parameters of the functions which occur only once within the standard methods also
do not need an index, e.g. E of the Measure function or VSTAT of the pH/mV-stat function.
2. Parameters of the form Xi
Parameters which use an index without brackets are all those whose link with the method
function is meaningless. This indexing form includes R, C and H.
Example: R3: third result (see fourth indexing form)
Note: R = R1 holds, in other words if the index = 1 it may be omitted. This also applies to
the indexing forms under points 3 and 4.
3. Parameters of the form X [j]
Index j is the function counter. This indexing form includes, e.g. VDISP, QEX and x.
Example: QDISP[2]: Measured value of the second Dispense function (extract from
standard method "2 Step titration (EQP)")
Dispense
Stir
EQP titration
Calculation
Calculation
08/2004
8-9
Use of indices
Report
Dispense
Stir
EQP titration
Calculation
EQP titration
E [mV]
Q1[1] Q
QEX[1] QEX.
EQP1
V [mL]
Q1[1]
8-10
QEX[1]
08/2004
Use of indices
Calculation
Formula ..................................
Constant.................................
Decimal places ......................
Result unit ..............................
Result name ...........................
Statistics.................................
R1 = Q1[1]
4
mmol
HCl
Yes
EQP titration
E [mV]
EQP1
EQP2
V [mV]
Q1[2]
Q2[2]
Calculation
Formula ..................................
Constant.................................
Decimal places ......................
Result unit ..............................
Result name ...........................
Statistics.................................
Calculation
Formula ..................................
Constant.................................
Decimal places ......................
Result unit ..............................
Result name ...........................
Statistics.................................
R2 = Q1[2]+QEX[1]
4
mmol
CH3COOH
Yes
R3 = Q2[2]
4
mmol
NH4Cl
Yes
In the second (third) Calculation function, you define the mmol consumption for acetic acid.
Here, you take into account the titrated excess of the first EQP titration function.
In the third (fourth) Calculation function you define the mmol consumption for NH4Cl.
Note: The two Dispense functions of the standard method are skipped (0 mL has been defined
as volume in the method); the second Calculation function is skipped (no formula has
been defined in the method for the result).
08/2004
8-11
Use of indices
8.2.1
Analysis/Resource /
Function
Symbol
Unit
Current sample
TIME
[s]
Titrant
[mol/L]
Index
Examples
t
Sensor
Sample
ZERO
[mV, pH ...]
SLOPE
[g] or [mL]
[g/mol]
z
f
Auxiliary value
Calculation
R
C
Measure**
[mV, pH ...]
Temperature*
[C, F, K]
Dispense
VDISP
QDISP
[mL]
[mmol]
ET1
ET2
VEX
[mL]
QEX
[mmol]
VEND
[mL]
QEND
[mmol]
EQP/EP titration
EQP/EP titration
(Ipol/Upol)**
Two-phase titration*
8-12
H1H20
Xi
R3
C2
X[j]
QDISP[2]
QEX[2]
08/2004
Use of indices
Function
Symbol
EQP titration
EQP titration(Ipol/Upol)**
Two-phase titration*
neq
EP titration
EP titration (Ipol/Upol)**
pH/mV-stat**
Unit
Index
Examples
neq[3]
P1
VP1
[mL]
QP1
[mmol]
P2
VP2
[mL]
QP2
[mmol]
VEQ
[mL]
[mmol]
EPOT
VTOT
[mL]
QTOT
[mmol]
VT1
[mL]
QT1
[mmol]
VT2
[mL]
QT2
[mmol]
VSTAT
[mL/min]
QSTAT
[mmol/min]
Q[2]
X[j]
VT1[2]
CSTAT
Calculation
(Statistics)
x[3]
srel
EQP titration
EQP titration(Ipol/Upol)**
Two-phase titration*
VEQ
[mL]
[mmol]
EPOT
EHNV
Q2[1]
Xi[j]
EPOT1[2]
Note: The parameters of the functions which occur only once in a method do not need an
index in "[ ]".
* Temperature, Two-phase titration: Special methods;
** Measure, pH/mV-stat, EQP titration (Ipol/Upol), EP titration (Ipol/Upol): two or more
of these functions are possible only with special methods.
08/2004
8-13
Evaluation procedures
8.3
Evaluation procedures
The titrator has various evaluation procedures for precise determination of the equivalence
points of a titration curve:
Standard
Minimum/maximum
Segmented
Asymmetric
8.3.1
Standard
You use this procedure for all S-shaped titration curves. The evaluation uses an iterative
procedure (nonlinear regression) [1]. The titration of a strong acid with a strong base is used
as a mathematical model. With this model, the determined equivalence point always lies in the
vicinity of the inflection point.
E
Inflection point
8.3.2
Minimum/maximum
The result of this evaluation is the calculated minimum (maximum) from the measured points
of the titration. The classical example of a titration curve with a minimum is the determination
of surfactants with photometric indication.
The minimum (maximum) is calculated by a polynomial approximation of the titration curve in
the region of the minimum (maximum). The equivalence point is recognized directly using the
data of the titration curve.
8-14
08/2004
Evaluation procedures
8.3.3
Segmented
V
E/V
1st derivative
1. Ableitung
2E/V2
2. Ableitung
2nd derivative
08/2004
8-15
Evaluation procedures
8.3.4
Asymmetric
With pronounced asymmetric curves, the standard procedure can lead to a systematic error.
The difference between the true equivalence point and the inflection point can then be greater
than the precision normally attained. For these cases, the titrator is equipped with the evaluation based on the Tubbs method [2].
This empirical approximation method is a tried and tested procedure for the evaluation of
asymmetric, analog recorded titration curves. It can also be applied to titration curves
measured digitally. The result of the Tubbs evaluation provides a better approximation of the
true equivalence point than the inflection point.
The evaluation procedure is based on the following considerations:
E
M2
Intersection
point EQP
M1
A circle of curvature with minimum radius can be drawn on both branches of the
titration curve. The ratio of the two radii
is determined by the asymmetry of the
curve. The mean intersection point of
the line connecting the centers of the
circles M1 and M2 with the titration curve
represents the sought-after equivalence
point. Theoretical calculations show that
the true equivalence point with asymmetric titration curves always lies between the inflection point and that branch
of the titration curve which has the greater curvature (the smaller radius of curvature).
In the titrator the calculation is implemented according to Ebel [3]. This involves approximating
those parts of the titration curve which lie in the region of the greatest curvature by a hyperbola.
The vertex is determined for each approximated hyperbola. This point on the hyperbola lies
at the site of greatest curvature. The mid-points of the assigned smallest radii of curvature are
the focal points of the two hyperbolae. As in the graphical variant, the intersection point of the
line connecting the two focal points with the titration curve results in the required equivalence
point.
For the evaluation at least six measured points both before and after the inflection point of the
titration curve are required in the region of the greatest curvature. If the titration curve has a
profile which does not allow calculation of the radii of curvature, the titrator calculates the
equivalence point by the standard procedure. This will be indicated in the report of the "raw
results".
[1]
[2]
[3]
S. Ebel, E. Glaser, R. Kantelberg and B. Reyer, Fres. Z. Anal. Chem., 312, 604 (1982)
8-16
08/2004
Examples of formulas
8.4
Examples of formulas
8.4.1
Results
R = Q C / m (standard formula)
C = f (M, z, unit)
R = m / (VEQ c C)
R = QC
R=Q
R = VEQ
mL consumption as result
R = VEQ / m
R = (QDISP Q) C / m
Back titration:
QDISP: dispensed amount of substance in mmol of
the Dispense function
Q: mmol consumption up to the equivalence point
or end point of an EQP or EP titration function.
R = (Q Hj) C / m
R = (Q / m Hj) C
R = ET1 [2]
R = pw(E) 1000
R = lg(E)
08/2004
8-17
Examples of formulas
8.4.2
Constants
Unit
C = M/z
mg / g or g/L
C = M / (10 z)
% (g/100 mL)
C = M 1000 / z
ppm (mg/kg)
ppm (mg / L)
C = 1/z
mol / kg (mmol / g)
C = 56.1
C = M / (1000 z)
Titer
C = 1000
mmol / L
C=1
mol / L
8-18
C = M/z
mg
C = 1/z
mmol
08/2004
Examples of formulas
8.4.3
To calculate the titrant consumption in mmol of a particular equivalence point when a titration
curve has several equivalence points, you can have Q identified by a condition, e.g.
R1 = Q(EPOT > -50)
R1 = Q(EPOT ~ 100)[2]
R1 = Q(EPOT ~ P1)
R1 = Q(EPOT ~ H11)
Note: You can also define these conditions with VEQ or EPOT, e.g. R 1= EPOT(VEQ ~ 5).
08/2004
8-19
Restrictions
8.5
8.5.1
8.5.2
8.5.3
Per sample determination, the titrator can determine maximum 16 equivalence points (EQP
titration), divided between one or two EQP titration functions. If there are more than 16
equivalence points, these will not be determined, but the determination will be continued.
8.5.4
The titrator can store 300 measured values per titration function (EQP, EP, Learn, EQP (Ipol/
Upol), Two-phase); it then aborts the function. With the titration functions EP (Ipol/Upol) and
pH/mV-stat, the number of measured points will be reduced automatically (see Sections
3.3.10 and 3.3.11).
8.5.5
The titrator can store 180 results per sample series; it then aborts the series.
Example: If you titrate 40 samples with a method, the titrator can store 4 results for each
individual sample.
8.5.6
8-20
08/2004
Contents
Page
9.
9-3
9.1
9-3
9.2
9-6
08/2004
9-1
9-2
08/2004
9.
9.1
You yourself can rectify all errors which the titrator displays as messages. Some of these
messages refer to this section (errors 1...6).
However, if the EPROM or RAM test following startup of the titrator failed ("test failed"), the only
measure available is: "Press any key to continue". The program memory or the program data
memory is faulty.
After any key has been pressed, the titrator attempts to continue the startup process: This may
be successful, but does not necessarily guarantee 100% perfect operation.
Measure: Please contact METTLER TOLEDO service!
1. Internal ERROR: ... (error which should be noted down, e.g. PB, M1)
Parts of the hardware may be faulty.
Measure: Before you contact METTLER TOLEDO service,
note the fault and the operation which initiated it,
note the instrument number of the titrator (rear panel)
print out the system information, which provides details of the titrator
equipment:
Press the shift and <F4> keys to print out the information.
Finally, inform the service of these points and the attached peripherals with
the defined configuration.
2. Memory faulty
Parts of the user data memory are faulty.
Measure: Call METTLER TOLEDO service to have the memory changed. Meanwhile,
you can still continue working with the titrator.
3. Faulty data deleted
a. The titrator has stored only parts of a method, e.g. as the power failed during storage
of this method. It deletes the entire method (it is also possible that it has deleted several
methods). As a result, the sample data of this method which are stored in the sample
data memory will also be deleted.
Measure: Confirm the message.
Check which of your methods have been deleted and reenter.
08/2004
9-3
b. The titrator has stored only parts of parameters of a resource, e.g. as the power failed
during storage of these parameters. It deletes the entire list of this resource (e.g. all
titrants or all sensors).
Measure: Confirm the message.
The titrator now loads the default list of the deleted resource, e.g. all
titrants stored in the titrator in the factory.
Check which list has been changed:
If the user data memory has insufficient storage space, only the titrants
which can be accommodated in the available space will be stored.
If the memory is full, the titrator will not store any titrants. In such a case,
you must delete data of other resources or one of your methods to create
memory space.
Switch the titrator off then on again.
Check that all resources are again available.
If the error messages appears repeatedly, inform METTLER TOLEDO service!
9-4
08/2004
c. The titrator performs a learn titration. If the method for this is stored on the memory
card or in the computer, the parameters of the function are not stored.
Measure: Confirm the message.
Always perform a learn titration with a method stored in the titrator and
do not remote-control the titrator!
If the error message appears repeatedly, contact METTLER TOLEDO service!
08/2004
9-5
9.2
The following compilation of errors and malfunctions are not reported by the titrator and may
frequently help you rectify the faults yourself without the need to contact METTLER TOLEDO
service.
If you have to contact the service, please print out the system information to obtain details of
the titrator equipment and pass these data on to the service:
Press the Shift and <F4> keys to print out the information.
Fault
Possible cause
Rectification
No display on titrator
Switch on device
Wrong settings
Configuration (switch settings)
wrong
Settings and
configuration must match
(see Section 2.7)
Wrong potential or
pH values
Electrode faulty
9-6
08/2004
Contents
Page
10.
10.1
10.2
10.2.1
10.2.2
10.2.3
10.2.4
10.2.5
10.3
10.4
10.5
10.5.1
10.6
10.7
10.8
10.8.1
10.9
08/2004
10-1
10.
Burette drive
You can clean the housing of the titrator with a cloth moistened with ethanol.
10.1
Position 2
Coupling
Ribbon cable
DL55/DL58
If you wish to use a second burette drive, follow the
above procedure:
Unscrew the burette guide at position 1 etc.
08/2004
10-3
Interchangeable burette
10.2
10.2.1
The 5, 10 and 20 mL burettes differ only in the size of their cylinder, centering ring and piston,
whereas the 1 mL burette has a different construction: its piston is longer, piston guide and
cylinder holder ''replace'' the centering ring of the other burettes. Instead of the locking screw,
its glass cylinder is fastened with an O-ring and a knurled nut.
1 mL burette
5 / 10 / 20 mL burette
Connection tubing
Knurled nut
Stopcock
O-ring
Stopcock
Locking screw
Cylinder holder
Glass cylinder
Piston
Piston rod
Piston guide
Protection tube
Piston
Lip seals
Piston rod
Burette housing
10-4
Centering
ring
08/2004
10.2.2
Interchangeable burette
Suction tube
Dispensing tube
Tip
holder
Burette
assembled
Stopper
Burette holder
Gasket
1 L bottle
08/2004
Fitting
10-5
Interchangeable burette
10.2.3
3
1
Note
Before sliding the burette onto the titrator,
check the exact position of the stopcock and
the piston rod.
If the piston has been pushed too far into the
cylinder, carefully take it out a short way. Then
press the burette onto the burette holder thus
positioning the piston exactly. Piston must
project 7 mm!
10-6
Position of the
valve
Position of the
piston
08/2004
10.2.4
Interchangeable burette
Depending on the titrant, you should clean the burette cylinder, piston, stopcock and tubing
relatively often.
Slide the burette off the titrator, invert it so that the stopcock points towards you and carefully
take out the piston; this causes the burette contents to flow out through the suction tubing
(waste or titrant bottle!).
In the same position, turn the stopcock through 90 clockwise and any liquid in the stopcock
will flow out through the dispensing tubing (waste bottle!).
Unscrew the suction, dispensing and connection tubing.
1 mL burette
Unscrew the knurled screw of the burette
and remove the O-ring from the glass cylinder using tweezers.
Unscrew the holder of the glass cylinder
and take out the cylinder.
Caution: Do not misplace O-ring!
5, 10, or 20 mL burette
Unscrew the locking screw of the burette
and take out the glass cylinder.
Caution: Do not misplace the centering
ring of the burette housing!
Depending on the contamination caused by the titrant, rinse cylinder and tubing with acids
or deionized H2O then with ethanol and finally dry the parts with oil-free compressed air or
vacuum.
Rinse the stopcock with solvents or deionized H2O only! Then dry it with oil-free compressed air.
Never place O-rings in organic solvents!
Never attempt to remove any crystals in the cylinder by scratching with a hard object! Pipe
cleaners or Q tips are more suitable.
Never put the parts in a drying oven whose temperature is above 40 C!
Replace the piston if it leaks or is badly scored at the edge. Pay special attention to crystal
formation between the lip seals of the piston if you work with NaOH/KOH and KF solutions!
08/2004
10-7
Interchangeable burette
10.2.5
General information
You can remove air bubbles at the piston surface by taking the burette out of the guide and
lightly tapping its base. This causes air bubbles to rise to the top. Then rinse the burette.
You can remove air bubbles in the tubes by tapping the tubes with your fingers while titrant is
being siphoned off or dispensed. If this does not help, undo the suction tube so that titrant flows
back into the bottle, screw it on again and rinse the burette (air purging). In obstinate cases
undo both tubes, rinse with deionized H2O and ethanol and dry using oil-free compressed air
or vacuum.
Titrants such as KMnO4 or KOH in MeOH can easily crystallize in the tip of the burette and block
it. If you have no immediate use for a titrant, it is best to empty and clean the dispensing tube:
Unscrew connection to let the titrant flow out. Check the threaded connection and wipe off any
drops.
KF titrants are subject to outgassing, above all at elevated room temperatures (SO2), which
leads to the formation of air bubbles in the tubes and in the burette (stopcock). You should thus
rinse these burettes before titrations!
10-8
08/2004
10.3
Titration stand
3
9a
9
13
8
10
12
11
5
6
4
7
Always test the titration vessel for firm seating in the titration head! If it falls
off, you could injure yourself if working with toxic titrants and solvents or
strong acids or bases.
08/2004
10-9
Rear view
10.4
No. 1
No. 2
No. 3
Input:
Reference electrode
No. 4
TTLIO socket
Sensor inputs:
Sensor 1
Sensor 2
Temperature sensor
input: Temp 1
Stirrer outputs:
Stirrer 1
Stirrer 2
Analog outputs
pH
KF
RS
Centronics option
Connector for
power cable
On/off
switch
The diagram shows a possible occupancy of all slots. The basic version of the titrator has the
following installed
a pH option at slot No. 1
an Centronics option at slot No. 4.
pH and KF options
You can install a sensor option in any slot. Each option has a number which is also affixed to
the data sheet enclosed with each sensor option (see Section 10.5.1).
DL53/55/58: You can use the inputs and outputs of maximum four sensor options, e.g. two pH
options at slot No. 1 and 2, two KF options at slot No. 3 and 4.
DL50:
You can use the inputs and outputs of maximum one sensor option.
Centronics option
You can use the Centronics option only if it is installed in slot No. 4. The TTL inputs and outputs
of the socket can be used only for the commands preallocated by the titration software (see
Section 10.7).
10-10
08/2004
Installing options
RS options
You can install an RS option either in slot No. 3 or slot No. 4. Although the options are identical,
the functions of the connections are not!
Slot No. 3: You can freely control the TTL inputs and outputs of the socket.
To the upper RS interface you can attach only a sample changer,
to the lower only a computer or a terminal.
Slot No. 4: You can use the TTL inputs and outputs of the socket only for the commands
stipulated by the titration software (see Section 10.7).
To the upper RS interface you can attach only a balance,
to the lower only a printer.
10.5
Soldering scheme
2
3
1
4
Shield
Pt100/Pt1000 sensor
08/2004
10-11
Memory card
10.5.1
When the titrator is delivered, the measuring inputs are calibrated for a sensor and temperature
sensor (Pt100 and Pt1000) of the pH option. The data sheet filed in Section 14 documents the
data for the characteristic line of the measuring inputs of this pH option.
If the data are not stored on the actual option, you must reenter them (see Section 6.7.2)
if system data are lost (see Section 9.1)
if you install this option in a different slot.
If you order an additional pH option, you receive a data sheet with the number of the option
and the calibration data for its measuring inputs. You must enter these data for correct potential
and temperature measurements if they are not stored on the actual option (see Section 6.7.2).
The data for the characteristic line of the measuring inputs are always stored on KF options!
Note: As the characteristic line of the measuring inputs can exhibit long-term drift, we advise
you to have the inputs recalibrated every 2 years by METTLER TOLEDO Service.
10.6
Note: Ensure that you are not electrostatically charged when you perform this operation! We
recommend you touch the metallic part of the titrator housing before you insert the
memory card to ensure the charge is not transferred to the titrator interior.
10-12
08/2004
10.7
TTLIO
The TTLIO socket of the Centronics option has two inputs and four outputs (In 1/In 2 and
Out 1...Out 4). These are assigned by the titrator to commands which are triggered during an
analysis. You can wire these inputs and outputs mechanically or electronically to trigger the
defined commands by auxiliary units or systems (see following examples).
The RS option has the same TTLIO socket as the Centronics option. When it is installed in slot
3, the inputs and outputs are always available and freely configurable (see Sections 6.7.5 and
6.7.6). At slot 4, they are assigned by the titrator to commands which you trigger during an
analysis:
Socket
1
signal ground
In 1 (Pin 2) ........
In 2 (Pin 3) ........
supply voltage
2
3
4
8
5
7
Wiring mechanically
If you wire, e.g. pin 1 (ground) with pin 2 (input 1) by
attaching a manual event sensor, you can initiate the
start of the analysis with this switch. The mask
"Defined are" must be blocked from the analysis
sequence for this as it can not be confirmed (see
Section 6.7.3).
08/2004
In
Event sensor
GND
10-13
TTLIO
Wiring electronically
Input In 1 or In 2
Titrator
external
Titrator
Out
In
GND
GND
GND
external
Titrator
external
Relay
Relay
VCC
Out
Out
GND
Note: TTL are signals which do not transfer power. To operate, e.g. a pump it is necessary
to connect an amplifier in the circuit.
10-14
08/2004
10.8
External keyboard
Attaching a keyboard
A DIN socket is located on the left side of the titrator and can be used for the attachment of an
external keyboard for alphanumeric entries.
Attach the keyboard using the appropriate DIN cable (see Section 12.10: Technical data).
The following table shows the keys and key combinations which correspond to the command,
menu, auxiliary function and entry keys of the titrator:
Titrator
External keyboard
key
key
F1
F2
F3
F4
F5
F1
F2
F3
F4
F5
Setup
Method
Sample
Run
F12
F10
F11
F9
<Alt> + key
Sensor
Stirrer
Changer
Burette
Results
Report
Misc...
Data Transfer
<Ctrl>+ key
e
s
c
b
r
p
m
d
Reset
Arrow key / Shift +
Arrow key / Shift +
Break (Pause)
/ Page up
/ Page down
Shift
1...9, .
Del
CE (Shift + Del)
Shift
1...9, .
Del
Shift + Del
(b)1...9
(a)1...9
The characters /, -, +, =, etc., which are written with the Shift key, depend on the assignment
of the keyboard. Additional characters not on the titrator keypad are:
x <Alt Gr> + x
08/2004
<Alt Gr> + u
<Alt Gr> + d
10-15
Bar-code reader/terminal
10.8.1
You can attach a bar-code reader to the external keyboard. To ensure this is recognized by
the titrator, you must program a "header" and "terminator" with the external keyboard (see
Operating Instructions of the keyboard in question). The titrator requires the key sequence
"Shift"/"Enter" for both parameters.
You can then read in, e.g. the bar code for the sample identification without having to define
the bar-code reader in the Setup menu.
You must define the bar-code reader if you wish to use it for direct data transfer to a computer
(see Section 2.7.3).
10.9
You have attached the terminal to the titrator and defined it (see Section 2.7.3). To configure
it, proceed as follows:
Switch off the titrator.
Switch on the terminal and wait until the message VT340 OK appears.
Press the Set-Up key: The SET-UP DIRECTORY appears.
a. If you have already configured the terminal for other connections, first select Recall
Factory Default Settings to reactivate the default settings.
b. If you have not yet used the terminal, you can change some of the default parameters
directly.
Select General Set-UP and change the following parameters:
Terminal mode
VT300-8bit
Select Display Set-Up and change the following parameters:
Scrolling
jump
Status Display
host writable
Select Communications Set-Up and change the following parameters:
Transmit Speed
9600 *
Receive XOFF Point
512
Character Format
8 bits, even parity *
* These parameters must match the defined terminal settings! (See Section 2.7.3)
Select Keyboard Set-Up and change the following parameters:
Keypad mode
numeric, so that the numeric keys of the numeric key field (on
extreme right of keyboard) are active.
10-16
08/2004
Terminal
Terminal
key
key
F1
F2
F3
F4
F5
F6
F7
F8
F9
F10
Setup
Method
Sample
Run
F14
F12
F13
F11
Sensor
Stirrer
Changer
Burette
Results
Report
Misc...
Data Transfer
8
5
4
7
3
2
1
6
F20
/ Prev. screen
/ Next screen
Shift
1...9, .
Del
Shift +
Shift +
Shift
1...9, .
Remove
08/2004
Reset
Arrow key / Shift +
Arrow key / Shift +
10-17
Accessories
Contents
Page
11.
11.1
11.2
11.3
08/2004
11-1
Accessories
11.
Accessories
All instrument components of and working aids for the titrator that form part of
the standard equipment and
the optional accessories
are listed below.
Each part that is listed with an order number can be ordered from METTLER TOLEDO.
08/2004
11-3
Accessories
11.1
Standard equipment
Interchangeable burette
(DL50 Graphix/
DL50 Rondolino only)
Propeller stirrer
Burette drive
Rondolino
(DL50 Rondolino only)
Titration stand
(DL50 Graphix only)
Electrode holder
(DL53/DL55/DL58 only)
11-4
08/2004
Accessories
DL50
Graphix
Titration stand
Rondolino
Electrode holder
Burette drive DV90
Interchangeable burette
(10 mL) DV1010*
Propeller stirrer
incl. 2 stirring rods
pH option
Centronics option
RS option
Titration Software LabX light
Power cable
Electrode cable
Printer cable
RS connection cable
Reference Handbook
Quick Guide
Memo card
Application broschure No. 12
Small accessories
DL50
Rondolino
DL53
DL55
DL58
x
x
x
x*
x*
x
x
x
x
x
x
x
x
x
x
x
x
x
x
x
x
x
x
x
x
x
x
x
x
x
x
(see next page)
x
x
x
x
x
x
x
x
x
x
x
x
x
x
x
08/2004
11-5
Accessories
DL50
Graphix
DL50
Rondolino
DL53
DL55
DL58
11-6
08/2004
Accessories
11.2
Optional accessories
The numbers enclosed in parentheses refer to the purchase order, e.g. of an interchangeable
burette. In case of additional orders some parts are available only in multipack form or as a
minimum quantity.
Order No.
Burette drive
Burette drive
DV90
Interchangeable burettes
Interchangeable burette, complete
DV1001
DV1005
DV1010
DV1020
comprising:
1 L brown glass bottle (1)
71296
and
Burette holder (1)
23645
and
Piston (1)
08/2004
1 mL
5 mL
10 mL
20 mL
DV1001
DV1005
DV1010
DV1020
51107535
51107115
51107116
51107117
11-7
Accessories
Order No.
and
Stopcock (1) with valve disk1) made of:
PTFE (light-gray) (standard equipment of interchangeable burette)
ceramic (dark-brown) (optional accessories)
51107537
51107525
1) Both valve disks are chemically resistant. For 24-hour use with titrants that
and
Light protection tube (1)
23644
and
Dispensing tube (1) with siphon tip
0.70 m
25687
and
Suction tube (1)
0.83 m
25688
23981
and
Gasket (1)
for 1 L brown glass bottle
and
Tip holder (1) for burette tip
and
Stopper ST 14.5 (1)
23960
23646
and
HCl
c=
Date:
mol/L
HCl
c=
Date:
mol/L
NaOH
c=
Date:
mol/L
NaOH
c=
Date:
AgNO3
c=
Date:
mol/L
1/2 H2SO4
c=
Date:
mol/L
1/2 H2SO4
c=
Date:
mol/L
mol/L
AgNO3
c=
Date:
mol/L
KF
c=
mg H2O/mL
Date:
KF
c=
mg H2O/mL
Date:
c=
Date:
mol/L
c=
Date:
mol/L
c=
Date:
mol/L
c=
Date:
mol/L
c=
Date:
mol/L
c=
Date:
mol/L
c=
Date:
mol/L
c=
Date:
mol/L
c=
Date:
mol/L
c=
Date:
mol/L
c=
Date:
mol/L
c=
Date:
mol/L
c=
Date:
mol/L
c=
Date:
mol/L
c=
Date:
mol/L
c=
Date:
mol/L
c=
Date:
mol/L
c=
Date:
mol/L
c=
Date:
mol/L
c=
Date:
mol/L
c=
Date:
mol/L
c=
Date:
mol/L
c=
Date:
mol/L
c=
Date:
mol/L
c=
Date:
mol/L
c=
Date:
mol/L
c=
Date:
mol/L
c=
Date:
mol/L
c=
Date:
mol/L
c=
Date:
mol/L
c=
Date:
mol/L
c=
Date:
mol/L
c=
Date:
mol/L
c=
Date:
mol/L
c=
Date:
mol/L
c=
Date:
mol/L
c=
Date:
mol/L
c=
Date:
mol/L
c=
Date:
mol/L
c=
Date:
mol/L
c=
Date:
mol/L
c=
Date:
mol/L
c=
Date:
mol/L
c=
Date:
mol/L
c=
Date:
mol/L
c=
Date:
mol/L
c=
Date:
mol/L
c=
Date:
mol/L
c=
Date:
mol/L
c=
Date:
mol/L
11-8
51107506
08/2004
Accessories
Order No.
Additional parts for the burette
Dispensing tube with siphon tip
1.00 m
25961
23961
23915
71478
set of 5
23240
Merck, DE
Fisher, US
23774
23787
51107065
51108760
Titration stands
08/2004
DV92
11-9
Accessories
Order No.
Titration stands
comprising:
DV92
25655
Propeller stirrer
incl. 2 stirring rods
51109150
25651
23842
25653
25652
25650
25654
23451
23452
101974
11-10
51108760
08/2004
Accessories
Order No.
Additional parts for the titration stand
Titration vessel 100 mL
polypropylene, red colored
set of 1400
25777
set of 20
101446
set of 10
23515
23516
51107655
set of 16
101448
23834
Gas inlet
23721
23821
Electrode holder
08/2004
23517
101230
51108730
11-11
Accessories
Order No.
Propeller stirrer
incl. 2 stirring rods
Propeller stirring rod
101229
655073
Adapter cable
(mini DIN male / RCA female)
11-12
51109150
0.50 m
51107216
51108016
51190969
51108149
Diaphragm pump
incl. suction tube
51108012
51108779
51108780
51370200
51370210
08/2004
Accessories
Order No.
Sensors
08/2004
DG111-SC
DG101-SC
DG113-SC
DG114-SC
DG115-SC
DM140-SC
DM141-SC
11-13
Accessories
Order No.
Ion selective measuring electrodes
Fluoride ISE
Chloride ISE
Nitrate ISE
Sodium ISE
Potassium ISE
Lithium ISE
Ammonia GSE
Ammonium ISE
Magnesium ISE
Cyanide ISE
Sulfide ISE
Calcium ISE
Bromide ISE
Fluoroborate ISE
Silver ISE
Cadmium ISE
Iodide ISE
Barium ISE
Surfactant sensitive electrode
Reference electrode for
ion selective electrodes
surfactant sensitive electrodes
DX219
DX235
DX262
DX223
DX239
DX207
DX217
DX218
DX224
DX226
DX232
DX240
DX280
DX287
DX308
DX312
DX327
DX337
DS500
51089931
51089933
51089934
51089930
51089932
51107673
51107677
51107679
51107684
51107681
51107675
51107683
51107671
51107676
51107682
51107672
51107680
51107674
51107670
DX200
Inlab 301
51089935
52000128
89601
89602
51108034
DP5
89600
1) If sensors with DIN connectors are attached via the adapter cable to the titrator,
the advantages offered by the triaxial cable high level of protection against
electrostatic interference are in part lost. In the case of sensors with a very high
resistance, e.g. DG113 in nonaqueous solutions, we advise against use of the
adapter cable.
11-14
08/2004
Accessories
Order No.
Temperature sensors
Pt1000 sensor
DT1000
88321
51107269
08/2004
DM143-SC
1.00 m
51108061
DV705
Thermostatable beaker
(for KF titration vessel)
51107497
Stand rod
51107495
11-15
Accessories
Order No.
Peripherals
METTLER TOLEDO balances with data output
Printer
17.37
19.31 5 g
8.003 9 g
7.773 g
6.554
10.50 g g
8.097 6 g
5.876 g
3.205 g
1.098 g
g
RS-P42
METTLER
TOLEDO
GA4
2 Prin
ter
DR42
OU
T
OU 1
T
OU 2
T
OU 3
T
IN 4
1
IN
2
ON
OUT 2
24 VDC 1.2 A
OUT 3
100-240 V
50/60 Hz
unfused
max. 9 A
OUT 4
TBox DR42
Sample changer
Rondolino
Sample changer
Rondo 60
51107424
51108304
Titration software
- LabX pro titration (for Windows 2000/XP)
- Instrument licenses for Titrators
11-16
08/2004
Accessories
Order No.
Memory Card
for DL53 and DL55
USER DATA
ME-51107230
Miscellaneous
Keypad cover
set of 3
51107667
Adapter cable
(banana sockets-DIN connector)
0.23 m
25914
51107230
DL53 DL55
DL53 DL55+
DL53 DL53+
DL55 DL55+
DL53 DL58
DL55 DL58
51107210
51107211
51107212
51107213
51107275
51107276
11101051
59759
229065
08/2004
229029
51190363
11-17
Accessories
Order No.
Connection cable: RS option
Connection cable for AM, PM, AT balances
51107196
51107195
11-18
229185
200495
200495
201508
201508
201507
08/2004
Accessories
Order No.
Options
RS option: 2 RS232C interfaces (DCE)
plus 1 TTLIO socket
51107172
51107289
51107269
51107152
Documentation
Reference Handbook
German
English
French
51709613
51709614
51709615
Quick Guide
German
English
French
Spanish
Italian
51709616
51709617
51709618
51709619
51709620
Memo card
German
English
French
Spanish
Italian
51709621
51709622
51709623
51709624
51709625
German
English
51724764
51724765
Computer Interface
Description
German
English
51709495
51709496
08/2004
11-19
Accessories
11.3
Basics of Titration
Basiswissen in der Titration
51725008
51725007
Fundamentals of Titration
Grundlagen der Titration
Bases du Titrage
704153
704152
704154
Guide to pH Measurement
Anleitung zur pH-Bestimmung
51300047
51300058
51300075
51300201
51724716
51724715
51724717
51724765
51724764
51725015
51725014
51710082
51107233
51107234
51107235
51107236
51107237
51107238
11-20
08/2004
Accessories
We have developed applications for the METTLER TOLEDO DL770, DL67, DL70ES and DL77 Titrators, which
have a method concept similar to that of the DL50, DL53, DL55 and DL 58 series. You will find these useful when
defining the parameters of your method functions.
DL70 Application Brochure 1 (18 Customer Methods)
DL70 Applikationsbroschre 1 (18 Kundenapplikationen)
724492
724491
724557
724556
724559
724558
724561
724560
51724634
51724633
51724646
51724645
51724648
51724647
51724650
51724649
51724652
51724651
51724769
51724768
51724908
51724907
51724910
08/2004
51724909
51724912
51724911
11-21
Technical Data
Contents
Page
12.
12.1
12.2
12.3
12.4
12.5
12.6
12.7
12.8
12.9
12.10
12.10.1
12.10.2
12.10.3
12.10.4
12.10.5
12.11
08/2004
12-7
12-7
12-7
12-7
12-8
12-9
12-1
Technical Data
12.
Technical data
12.1
Measurement system
08/2004
Temperature input via keypad or automatically with the aid of a temperature sensor
12-3
Technical Data
Voltage source
Range
Resolution
-1270 to +1270 mV
10 mV in the range -1270 to +1270 mV
1 mV in the range -127 to +127 mV
Measurement range
Resolution
Maximum permissible error
Current source
Range
Resolution
-127 to +127 A
1 A in the range -127 to +127 A
0.1 A in the range -12.7 to +12.7 A
Measurement range
Resolution
Maximum permissible error
12.2
-150 to +150 A
0.01A (16-bit AD converter)
0.1%
-1500 to +1500 mV
0.1mV (16-bit AD converter))
0.1%
Outputs
Stirrer output
Voltage range
Speed stabilized
Analog output
Gain
Offset: max. permissible error
Range
Range: max. permissible error
Output resistance
12-4
08/2004
Technical Data
12.3
12.4
Interchangeable burettes
Volume
Materials which come into contact with
the titrant
12.5
3800 rpm
Pmax.:
Ptypical:
6W
1.2 W at 12 V
Display
Languages
12.7
1, 5, 10 and 20 mL
Propeller stirrer
Maximum speed
Power consumption
12.6
Memories
Database
08/2004
12-5
Technical Data
12.8
12.9
Balance
Attachment via RS232C interface of the Centronics or an RS option at slot No. 4 for all
METTLER TOLEDO and SARTORIUS balances
Printer
Attachment via Centronics interface of the Centronics option or via RS232C interface of an RS
option at slot No. 4 for various commercial
graphics printers (on use of the RS option with
XON/XOFF protocol)
Sample Changer
Terminal or computer
(LIMS: in-house laboratory
information management system)
12-6
08/2004
Technical Data
12.10
12.10.1
DIN socket
DATA
2
4
GND
4
+
VCC
VCC: 5 V
Titrator
12.10.2
TTLIO socket
3
4
8
5
7
GND
In 1
VCC: +5 V, max. 60 mA
In 2
Out 1
In:
Out 2
Out 3
+5 V
VCC
6
7
8
Out 4
Titrator
12.10.3
9-pin, D-Sub
Pin assignment
RxD (In)
Data to titrator
TxD (Out)
DSR
RSGND
4
3
2
BR
Shielding
08/2004
+12 V
330
5
Titrator
12-7
Technical Data
12.10.4
A: Data ready
D0
B:
D1
C:
D2
D:
D3
E:
F:
Data
D4
G:
I
H
K
T
H:
D5
I:
D7
P
N
D6
K: Data adopted
/ACK
L: Printer occupied
BUSY
M: End of paper
B
C
PE
N: Printer active
SLCT
/AUTO FDXT
P: Printer error
/ERROR
R: Initializing printer
/INIT
S: Printer selected
/SLCTIN
GND
T:
GND
U:
Signal ground
Titrator
12-8
08/2004
Technical Data
12.10.5
RS232C socket
Shielding
1
4
8
5
TxD (Out)
Data to titrator
RxD (In)
RSGND
330
+12 V
DSR
Titrator
12.11
Additional data
Housing
Polyester
Titration stand
Polypropylene
Keypad
Polyester, splashwater-proof
Dimensions
Weight
Power supply
Fuse
Frequency
50/60 Hz
400 mA
Ambient conditions
08/2004
12-9
Index
Index
Numbers incorporating dashes refer to sections in the Reference Handbook (example: 3-38),
Numbers without dashes refer to the Quick Guide (example: 9).
<F1>...<F5> 9, 10
E
EP titration function 3-39
EQP titration function 3-25
EQP titration function (Ipol/Upol) 3-49
measure function 3-17
E(set)
EP titration function 3-39
EQP titration function 3-22
t
EP titration function 3-39
EQP titration function 3-25
EQP titration function (Ipol/Upol) 3-49
measure function 3-17
Accessories
optional accessories 11-7
standard equipment 11-4
Activate
control input 6-32
control output 6-33
Adjust measuring inputs 6-28
Amperometric indication
EP titration function (Ipol/Upol) 3-58
EQP titration function (Ipol/Upol) 3-47
Analysis
aborting (Reset) 5-12
fading out 5-11
is interrupted 5-11
menu sequence 5-4
"Run" menu 5-3
start 5-4
Analysis sequences (examples)
CaCl2 determination 5-7
calibration of a pH electrode 27
comparison: titration stand 1/ST20A 5-16
determination of the HCl content 12
pH-stating 5-10
titer determination (NaOH) 32
with the sample changer 5-17
Arrow keys 7
Asterisk (*) 3-4, 3-11
Asymmetric (evaluation procedure)
equivalence point recognition 3-28, 3-50
evaluation parameter 3-34, 3-53
explanation 8-16
08/2004
13-1
Index
Burette drive
inserting 10-3
selecting 2-5
Burette volume
selecting 2-5
smallest increment 3-24
Burette tip 6-12
C (constant) 3-66, 8-7
c ( nominal concentration) 8-3
c * t (actual concentration) 8-3
Calculation(s)
formulas 8-17
function 3-66
indices 8-9
performing (auxiliary function) 6-20
Calibration
function 3-69
pH electrodes 27
sensors 3-69
temperature sensors 6-6
Calibration data
measuring inputs 6-29
sensors 2-9, 2-10, 3-69
temperature sensors 2-12
Centronics interface
GA42 printer 2-18
printer configuration 2-19
Centronics option
connection possibilities 10-9
installing 10-10
Changer 6-9
Character set (computer) 2-24
Clock (titrator) 6
Code (sync function) 7-18
Combined termination conditions 3-34, 3-53
Command keys 9
Communication protocol (computer) 2-24
Computer
bar-code reader 2-24
bar-code string 6-43
configuration 2-23
connection 10-10
data transfer 6-40
remote control 6-42
Concentration (titrant) 2-4, 8-3
Conditioning 3-15
Conductivity measurement 2-8
Conductometer 2-8
Constants
calculation function 3-66
calculations (auxiliary function) 6-20
examples 8-18
13-2
08/2004
Index
Date
entering 6-27
selecting format 6-26
Date specification
auxiliary values 2-15
methods 3-11
sensors 2-9
temperature sensors 2-11
titrants 2-5
Defined are (mask)
exclusion 6-30
meaning 5-5
Delay 3-42, 3-61
Directory (memory card) 6-37
Dispense
auxiliary function (burette) 6-12
auxiliary function (ST20A) 6-10
continuously 6-13
continuously (Ipol/Upol) 6-15
function 3-19
DL58
commands 7-3
functions 7-3
resources 7-3
DLWin software 4-13, 6-41
Documentation
information 4
Drift (potential measurement) 3-17
Dynamic (titrant addition)
EP titration function 3-39
EQP titration function 3-22
E (potential) 3-17, 8-7
EHNV (half neutralization value) 3-20, 8-4
Electrodes (METTLER TOLEDO) 2-7, 2-13
End point
EP titration function 3-41
EP titration function (Ipol/Upol) 3-60
pH/mV-stat function 3-63
range 3-40, 3-60
titration 3-37, 3-56
Entry keys 10
EP
absolute 3-41
relative 3-41
EP titration (function) 3-37
EP titration (Ipol/Upol) (function) 3-56
EPOT 8-4
EQP titration (function) 3-20
EQP titration (Ipol/Upol) (function) 3-45
Equilibrium controlled measured value acquisition
EP titration function 3-39
08/2004
13-3
Index
adding 7-8
deleting 7-8
DL58 7-3
explanation 20, 3-3
maximum number 7-9
modifying 3-10
overview 24
selecting 3-7
13-4
08/2004
Index
Memory card
directory 6-37
formatting 6-36, 6-40
inserting 10-11
interface 12-6
types 12-6
use 6-36
Memory copy(ies)
copying on memory card 6-39
loading to titrator 6-40
transferring to computer 6-41
Menus
explanation 8
keys 8
overview 1-2, 1-3
Method
concept 19
deleting 3-5
explanation 3-3
generating 24
modifying 3-7
modifying (current sample series) 5-12
modifying (ongoing method: DL55/DL58) 5-13
on computer 4-5
on memory card 4-5
printing 3-4
storage procedure 3-7
Methods
menu 3-3
printing 3-4
selecting 3-4
Method ID
defining 3-11
entering 4-4, 5-5
explanation 3-4
METTLER methods 3-6
modifying 3-9
standard methods 3-5
METTLER methods
90001: performance 14
90002: performance 27
explanation 19
modifying 25, 3-6
printing 3-6
Minimum (evaluation procedure)
equivalence point recognition 3-28, 3-50
evaluation parameter 3-34, 3-53
explanation 8-14
Misc. ... 6-26
Mixing time (two-phase titration function ) 7-14
Modify: command (<F4>) 10
Molar mass M
calculation function 3-68
entering 3-13
08/2004
13-5
Index
13-6
Resources
changing 5-8
copying on memory card 6-39
copying to titrator 6-39
deleting 2-3
DL58 7-3
explanation 2-3
list 2-3
modifying 2-3
printing 2-3
transferring to computer 6-41
Result(s)
auxiliary function 6-18
deleting 6-22
examples 3-67, 8-17
learn titration 5-9
maximum number/sample series 8-20
R 3-66, 3-71
recording 3-75, 6-24
Rx 6-20
storage specification 8-20
units 3-67, 8-17
Result list
displaying 6-18
exclusion 6-30
notes 5-9
Rinse
auxiliary function (ST20A) 6-10
tip (burette) 6-12
titration stand parameters 3-14
Routine (user level) 6-31
RS option
connection possibilities 10-11
installing 10-11
RS232 interface
GA42 printer 2-20
printer configuration 2-20
Run
analysis menu 5-3
key function 5-3
s (standard deviation) 8-7
Safety measures
for operational safety 5
for your protection 5, 10-3
Safety notes 1-1
Sample
function 3-12
ID (identification) 4-5, 5-6
08/2004
Index
Samples
maximum number 8-20
status 4-7
Sample changer
auxiliary function 6-9
connection 10-10
defining 2-25
sample series 5-6, 5-15
titration stand 2-17
titration stand parameters 3-13
Sample data
adding 4-8
deleting 4-6
entering 4-4, 5-5, 5-10
list 4-4, 4-6
memory (sample menu) 4-3
modifying 4-7
on computer 4-13
printing 4-7
recording 3-75, 6-24
storage specification 36, 4-3
Sample data mask
analysys menu 5-5
sample menu 4-5
Sample series
deleting 4-6
entering 4-4
with auto stand 5-6, 5-15
with ST20A 5-6, 5-15
Sample series (DL55/DL58)
entering 4-9
executing 5-15
Sample size 3-21, 3-38, 3-48, 3-59, 8-3
Save (storage procedure)
auxiliary values 2-16
devices for control intput 7-5
devices for control output 7-6
methods 3-7
polarized sensors 2-13
sensors 2-10
solvents 2-28
temperature sensors 2-12
titrants 2-6
Segmented (evaluation procedure)
equivalence point recognition 3-28, 3-50
evaluation parameter 3-34, 3-53
explanation 8-15
Send mode (computer) 2-24
08/2004
Sensor(s)
adding 2-10
auxiliary function 6-4
deleting 2-7
modifying 2-7
order No. 11-10
pH option 2-7
resource 2-7
storage procedure 2-10
Sensor inputs
polarized sensors 2-13
sensors 2-8
temperature sensors 2-11
Separation time (two-phase titration function) 7-14
Sequential
activating control output (auxiliary function) 6-34
control output function 7-17
Setup (menu) 2-3
Shorten analysis sequence 6-30
SLOPE 8-3
Slope
calculation 3-69
entry through determination 2-9
explanation 2-9
minimum/maximum value 3-71
pH electrode 26
theoretical value 2-9
Slots 10-10
Software LabX 4-13, 6-41
Software version 1-1
Solvents
adding 2-28
deleting 2-27
modifying 2-27
storage procedure 2-28
Special methods
DL58 7-7
explanation 7-3
Speed
defining 3-16
modifying 5-8, 6-8
srel (relative standard deviation) 8-7
ST20A
connection 10-10
outputs 2-28
Stand 1/2 (titration stands) 2-17
Standard (evaluation procedure)
equivalence point recognition 3-28, 3-50
evaluation parameter 3-34, 3-53
explanation 8-14
Standard deviation s 3-67
13-7
Index
Standard method(s)
application examples 22
explanation 19, 3-5
functions 20
modifying 25, 30
number 20
printing 3-5
Start/end character (computer) 2-24
Statistics
modifying 6-22
selecting for calculations 3-67
Status
remote control 6-42
peripherals 2-18
samples 4-7
Steepest jump only 3-31
Stir (function) 3-16
Stirrer
auxiliary function (stirrer) 6-8
output 2-17
speed 5-8, 6-8
Stirring time 3-16
Stop bits
computer 2-24
printer 2-20
terminal 2-25
Stop for reevaluation 3-35, 3-55, 5-11
Storage interval (pH/mV-stat function) 3-64
Storage procedure
measured values 3-64, 3-74, 8-20
raw results 8-20
results 8-20
sample data 4-3
Symbols
explanation 8-3
list 8-3
Sync (function) 7-18
Synchronization mode (Sync function) 7-18
System
computer/terminal 2-23
titrator (information) 9-3, 9-6
13-8
T (temperature) 7-10
t (titer) 3-72, 8-3
t(max)
EP titration function 3-39
EQP titration function 3-25
EQP titration function (Ipol/Upol) 3-49
measure function 3-18
temperature function 7-10
t(min)
EP titration function 3-39
EQP titration function 3-25
EQP titration function (Ipol/Upol) 3-49
measure function 3-17
temperature function 7-10
Table of measured values
displaying 5-7, 6-21
recording 3-75, 6-24
Technical data
burette 12-5
burette drive 12-5
Centronics socket 12-8
DIN socket 12-7
display 12-5
measurement system 12-3
memories 12-5
outputs 12-4
peripherals 12-6
RS232C connector (Centronics option) 12-7
RS232C socket (RS option) 12-9
stirrer 12-5
TTLIO sockets 12-7
Temperature
correction 3-13, 3-69
entering 2-9, 4-6, 5-6
function 7-10
measurement 2-9, 3-13, 3-18, 3-20, 3-37,
3-62, 3-69, 7-10
measuring (auxiliary function) 6-5
Temperature sensor(s)
calibrating 6-6
Lemo cable plug 10-10
Pt100/Pt1000 2-11
resource 2-11
selecting 3-13
storage procedure 2-12
Tendency
EP titration function 3-42
EP titration function (Ipol/Upol) 3-61
EQP titration function 3-32
EQP titration function (Ipol/Upol) 3-51
pH/mV-stat function 3-64
08/2004
Index
Terminal
configuration (keyboard) 10-16
configuration (titrator) 2-25
connection 10-11
key assignment 10-17
Termination (parameters)
EP titration function 3-42
EP titration function (Ipol/Upol) 3-61
EQP titration function 3-33
EQP titration function (Ipol/Upol) 3-52
pH/mV-stat function 3-64
Threshold 3-29, 3-51
Threshold value
evaluation procedure "Asymmetric" 3-30
evaluation procedure "Minimum/Maximum" 3-30
evaluation procedure "Segmented" 3-31
evaluation procedure "Standard" 3-30
TIME 5-4, 8-3
Time
entering 6-27
sample function (conditioning) 3-15
selecting format 6-26
stir function 3-16, 5-7
Time specification
auxiliary values 2-15
methods 3-11
sensors 2-9
temperature sensors 2-11
titrants 2-5
Timed increment measured value acquisition
EP titration function 3-41
EP titration function (Ipol/Upol) 3-60
EQP titration function 3-27
EQP titration function (Ipol/Upol) 3-49
Titer
checking 2-5
determination (NaOH solution) 32
entering 2-4
entry through determination 2-4
explanation 30
function 3-72
Title
function 3-11
METTLER methods 19
standard methods 19
Titrant
adding 2-6
concentration 2-4, 8-3
deleting 2-4
modifying 2-4
storage procedure 2-6
08/2004
Titrant addition
EP titration function 3-39
EP titration function (Ipol/Upol) 3-60
EQP titration function 3-22
EQP titration function (Ipol/Upol) 3-48
pH/mV-stat function 3-63
two-phase titration function 7-14
Titrate
manually 6-14
manually (Ipol/Upol) 6-16
Titration curves
1st derivative 3-30, 3-31, 3-54, 8-15
2nd derivative 3-31, 3-54, 8-15
displaying 5-8, 5-8, 6-21
recording 3-75, 6-24
Titration stand
equipping 10-9
meaning 7-8
order No. 11-7
resource 2-17
selecting 3-13
Titrator
battery 6
cleaning housing 10-3
connections 6, 10-10
documentation 4
front view 6
ID (identification) 6-27
internal clock 6
keypad 7
opening housing 10-3
rear view 6, 10-10
remote control 6-42
self test 7
settings 6-26
Transmission mode (balance)
bidirectional 2-21
unidirectional 2-21
TTL inputs
activating 6-32
wiring electronically 10-14
wiring mechanically 10-13
TTL outputs
activating 6-33
wiring electronically 10-14
TTLIO socket(s)
inputs and outputs 10-13
technical data 12-7
used by titrator 10-13
Turntable (sample changer) 6-10
Two-phase titration
function 7-12
special method 7-12
13-9
Index
13-10
Wait time
predispensing 3-21, 3-38, 3-48, 3-59, 7-13
stir function 3-16, 5-7
Weight
entering 4-5, 5-6
selecting 3-12
transferred by balance 4-12
Weight limits
at weight entry 4-5, 5-6
entering 3-12
x (mean value) 8-7
z (equivalent number) 3-13, 3-68, 8-3
ZERO 8-3
Zero point (sensor)
calculation 3-69
entry through determination 2-9
explanation 2-9
pH electrode 26
theoretical value 2-9
Zero point (temperature sensor)
entry through determination 2-12
explanation 2-11
theoretical value 2-12
08/2004
Indice
Indice
Los nmeros separados por un guin (ejemplo 3-38) se refieren al captulo correspondiente
en el Manual de Instrucciones, las cifras aisladas a la Gua de Manejo (ejemplo 9).
<F1>...<F5> 9, 10
E
func. medir 3-17
func. valoracin EP 3-39
func. valoracin EQP 3-25
func. valoracin EQP (Ipol/Upol) 3-49
E (nom.)
func. valoracin EP 3-39
func. valoracin EQP 3-22
t
func. medir 3-17
func. valoracin EP 3-39
func. valoracin EQP 3-25
func. valoracin EQP (Ipol/Upol) 3-49
Accesorios
accesorios facultativos 11-7
equipo bsico 11-4
Acondicionamiento (ST20A) 3-15
Activar
entrada mando a distancia 6-32
salida mando a distancia 6-33
Acumulador 6
Adicin de reactivo
func. pH/mV-Stato 3-63
func. valoracin EP 3-39
func. valoracin EP (Ipol/Upol) 3-60
func. valoracin EQP 3-22
func. valoracin EQP (Ipol/Upol) 3-48
func. valoracin en dos fases 7-14
Adquisicin datos medidos: incremental tiempo
func. valoracin EP 3-41
func. valoracin EP (Ipol/Upol) 3-60
func. valoracin EQP 3-27
func. valoracin EQP (Ipol/Upol) 3-49
Agitador
funcin auxiliar (Stirrer) 6-8
seleccionar salida 2-17
Agitar (funcin) 3-16
Ajustar entradas de medida 6-28
Anlisis
empezar 5-4
men "Run" 5-3
se interrumpe 5-11
secuencia men 5-4
terminar (Reset) 5-12
visualizar 5-11
08/2004
13-11
Indice
Bureta
burbujas de aire 10-8
funcin auxiliar 6-11
insertar 10-6
instalar 10-4
llenar 13
llenar (lavar) 6-11
mantenimiento 10-4, 10-7
montaje 10-5
C (constante) 3-66, 8-7
c (concentracin nominal) 8-3
c * t (concentracin real) 8-3
Cabeza de val. auto
definicin 2-17
serie(s) de muestras 5-6, 5-15
Cabeza de val. externa 2-17
Cabeza de valoracin
medios auxiliares 2-17
montaje 10-8
nmero de pedido 11-7
seleccionar 3-13
significado 7-8
Clculo posterior 6-20
Clculo(s)
frmulas 8-17
funcin 3-66
indicativos 8-9
realizacin (funcin auxiliar) 6-20
Calibracin
electrodo de pH 27
funcin 3-69
sensores 3-69
sondas de temperatura 6-6
Cambiador de muestras
cabeza de valoracin 2-17
conectar 10-10
definir 2-25
funcin auxiliar (Changer) 6-9
parmetros cabeza de valoracin 3-14
serie de muestras(s) 5-6, 5-15
Cambiar: mando (<F4>) 10
Cambio de buretas: ver buretas
Cambio de lengua 11, 6-27
Centronics: ver interface/tarjeta
Cdigo (func. sincronizacin) 7-18
Cdigo de barras 6-43
Coeficiente de correlacin 3-62, 3-65, 8-6
Combinacin de teclas 10
Concentracin (reactivo) 2-4, 8-3
Concepto
de manejo 7
de mtodos 19
Conductmetro 2-8
13-12
Constantes
ejemplo 8-18
funcin auxiliar clculo 6-20
funcin clculo 3-66
Continua (adicin de reactivo) 3-40, 3-60
Control de entrada
activar salida mando a distancia (funcin auxiliar) 6-33
func. salida mando a distancia 7-16
Control de equilibrio (adquisicin de los valores
medidos)
func. medir 3-17
func. valoracin EP 3-39
func. valoracin EQP 3-25
func. valoracin EQP (Ipol/Upol) 3-49
Copia de la memoria
carga al titulador 6-39
copia a la tarjeta memoria 6-39
transferir al ordenador 6-41
Criterios de terminacin combinados 3-34, 3-53
CSTAT (coeficiente de correlacin) 3-62, 8-6
Curso del anlisis (ejemplo )
calibracin electrodos de pH 27
comparacin: Cabeza de valoracin 1/ST20A
5-16
con cambiador de muestras 5-17
determinacin CaCl2 5-7
determinacin del contenido HCl 12
determinacin del ttulo (NaOH) 32
regulacin del pH 5-10
Cursor 10
Curvas de valoracin
1 derivada 3-30, 3-31, 3-54, 8-15
2 derivada 3-31, 3-54, 8-15
impresin 3-75, 6-24
visualizacin 5-7, 5-8, 6-21
Cx (constantes de clculo) 8-7
Data Transfer (transmisin de datos) 6-36
Datos de calibracin
entradas de medida 6-29
sensores 2-9, 2-10, 3-69
sondas de temperatura 2-12
Datos de muestra
aadir 4-8
borrar 4-6
cambiar 4-7
condiciones de memorizacin 36, 4-3
desde ordenador 4-13
entrar 4-4, 5-5, 5-10
imprimir 4-7
informe 3-75, 6-24
lista 4-4, 4-6
memoria (men Sample) 4-4, 5-5, 5-10
08/2004
Indice
Datos tcnicos
agitador 12-5
buretas 12-5
conector Centronics 12-8
conector DIN 12-7
conector RS232C (tarjeta RS) 12-9
conector TTLIO 12-7
enchufe RS232C (tarjeta Centronics) 12-7
memorias 12-5
motor de bureta 12-5
pantalla 12-5
perifricos 12-6
salidas 12-4
sistema de medida 12-3
Deriva (medida del potencial) 3-17
Desviacin estndar relativa (srel) 3-67
Desviacin estndar (s) 3-67
Dinmica (adicin de reactivo)
func. valoracin EP 3-39
func. valoracin EQP 3-22
Directorio (tarjeta memoria) 6-37
Diversos (Misc. ...) 6-26
DLWin Software 4-13, 6-41
DL58
funciones 7-3
mandos 7-3
medios auxiliares 7-3
Documentacin
informacin 4
Dosificacin
continua 6-13
continua (Ipol/Upol) 6-15
Dosificacin previa
func. valoracin en dos fases 7-13
func. valoracin EP 3-38
func. valoracin EP (Ipol/Upol) 3-59
func. valoracin EQP 3-21
func. valoracin EQP (Ipol/Upol) 3-48
Dosificar
funcin 3-19
funcin auxiliar (buretas) 6-12
funcin auxiliar (ST20A) 6-10
E (potencial) 3-17, 8-7
EHNV (valor de semineutralizacin) 3-20, 8-4
Electrodo de referencia 2-7
Electrodos (METTLER TOLEDO) 2-7, 2-13
Electrodos de pH
calibrar 26
pendiente 26
punto cero 26
08/2004
Electrodos polarizados
almacenar 2-13
aadir 2-14
cambiar 2-13
tarjeta KF 2-13
medios auxiliares 2-13
Embolo
colocacin 10-4
montaje 10-4
Encabezamiento de informe 6-27
Entrada mando a distancia
activar (funcin auxiliar) 6-32
funcin 7-15
Entradas de sensores
func. salida mando a distancia 7-17
sensores 2-8
sensores polarizados 2-13
Entradas mando a distancia
definir 7-4
medios auxiliares 7-4
Entrar tiempo
mtodos 3-11
reactivo 2-5
sensor de temperatura 2-11
sensores 2-9
valores auxiliares 2-15
EP
absoluto 3-41
relativo 3-41
EPOT 8-4
Esc (salir) mando (<F1>) 9
Estadsticas
cambiar 6-22
incluir en el clculo 3-67
Estado
mando a distancia 6-42
muestras 4-7
perifricos 2-18
Estn definidos (mscara)
bloquear 6-30
significado 5-5
Estndar (procedimiento de evaluacin)
explicacin 8-14
parmetro de evaluacin 3-34, 3-53
reconocimiento punto de equivalencia 3-28,
3-50
ET1 3-22, 3-38, 8-4
ET2 3-22, 3-38, 8-4
Evaluacin
func. pH/mV-Stato 3-65
func. valoracin EQP 3-34
func. valoracin EQP (Ipol/Upol) 3-53
13-13
Indice
Evaluacin posterior
condicin satisfecha 5-11
definir una condicin 3-35, 3-36, 3-55
ejecucin 6-18
Experto (nivel de usuario) 6-31
Extincin 2-8
f (factor de correccin) 4-6, 5-6, 8-3
Fallos 9-6
Fecha
entrar 6-27
seleccionar formato 6-26
Fecha caducidad (reactivo) 5-4
Forma de control (activar salida mando a distancia)
control por entrada 6-33
marcha/parada 6-33
secuencial 6-34
Forma de control (func. salida mando a distancia)
control por entrada 7-16
marcha/parada 7-16
secuencial 7-17
tiempo fijo 7-16
Frmula(s)
constantes 8-18
funcin auxiliar clculos 6-20
funcin clculo 3-66
funcin ttulo 3-72
funcin valores auxiliares 3-73
para limitar los puntos de equivalencia 8-19
resultados 8-17
Funcin(es)
aadir 7-8
borrar 7-8
cambiar 3-10
DL58 7-3
explicacin 20, 3-3
nmero mximo 7-9
seleccionar 3-7
visin de conjunto 24
Funciones auxiliares
explicacin 9, 6-3
teclas 6-3
visin de conjunto 1-4, 1-5
Funciones de clculo 3-66
H (valor auxiliar) 2-15, 8-3
Hoja de datos
tarjeta KF 10-12
tarjeta pH 10-12
13-14
ID mtodos
cambiar 3-9
definir 3-11
entrar 4-4, 5-5
explicacin 3-4
mtodos estndar 3-5
mtodos METTLER 3-6
ID muestras 4-5, 5-6
Impresora
ASCII 2-18
conectar 10-10
configuracin 2-19, 2-20
definir 2-18
In 3.1/3.2 (entradas TTL) 6-32
Incremental (adicin de reactivo) 3-24, 3-48, 7-14
Indicacin
func. valoracin EP (Ipol/Upol) 3-57
func. valoracin EQP (Ipol/Upol) 3-46
Indicacin amperomtrica
func. valoracin EP (Ipol/Upol) 3-58
func. valoracin EQP (Ipol/Upol) 3-47
Indicacin de fecha
mtodos 3-11
reactivo 2-5
sensores 2-9
sondas de temperatura 2-11
valores auxiliares 2-15
Indicacin voltamtrica
func. valoracin EP (Ipol/Upol) 3-57
func. valoracin EQP (Ipol/Upol) 3-46
Indicativos (forma)
ejemplos 8-9, 8-10
resumen 8-12
Informe
funcin 3-74
funcin auxiliar (Report) 6-24
Informe de comunicacin (ordenador) 2-24
Instalacin (men Setup) 2-3
Instalacin y mantenimiento 10-3
Instruccin
funcin 7-11
funcin salida mando a distancia 7-17
Interface Centronics
configuracin impresora 2-19
impresora GA42 2-18
Interface RS232
configuracin impresora 2-20
impresora GA42 2-20
Interpolacin (evaluacin) 8-14
Intervalo (acondicionamiento) 3-15
Intervalo de memorizacin (func. pH/mV-Stato)
3-64
08/2004
Indice
08/2004
13-15
Indice
Mtodo
almacenar 3-7
borrar 3-5
cambiar 3-7
cambiar ( mtodo en curso: DL55/DL58) 5-13
cambiar (actual serie de muestras) 5-12
desde ordenador 4-5
desde tarjeta memoria 4-5
elaboracin 24
explicacin 3-3
imprimir 3-4
Mtodos
imprimir lista 3-4
men 3-3
seleccionar 3-4
Mtodo(s) del usuario
borrar 3-6
copiar en la tarjeta memoria 6-38
copiar en titulador 6-39
explicacin 19, 3-6
imprimir 3-6
ttulo con valoracin EQP 34
transferir a ordenador 6-41
Mtodo(s) estndar
cambiar 25, 30
ejemplo de uso 22
explicacin 19, 3-5
funciones 20
imprimir 3-5
nmero 20
Mtodos especiales
DL58 7-7
explicacin 7-3
Mtodos METTLER
90001: Ejecucin 14
90002: Ejecucin 27
cambiar 25, 3-6
explicacin 19
imprimir 3-6
Mnimo (procedimiento de evaluacin)
explicacin 8-14
parmetro de evaluacin 3-34, 3-53
reconocimiento punto de equivalencia 3-28,
3-50
Misc. ... (Diversos) 6-26
Motor de bureta
instalar 10-3
seleccionar 2-5
13-16
Muestra
funcin 3-12
men memoria de datos de muestras 4-3
en curso (mscara): aviso 5-6
urgente (DL55) 4-10
Muestras
estado 4-7
nmero mximo 8-20
neq (nmero punto(s) de equivalencia) 8-4
Nivel de usuario 6-31
Nombre
funcin 3-11
mtodos estndar 19
mtodos METTLER- 19
Nmero de equivalencia
entrada 3-13
func. clculo 3-68
OK mando (<F5>) 9
Ordenador
cdigo de barras (string) 6-43
conectar 10-10
configuracin 2-23
lector de cdigo de barras 2-24
mando a distancia 6-42
transmisin de datos 6-40
Out 3.1...3.4 (salidas TTL) 6-33
P1/P2 8-6
Papel (impresora)
formato 2-19
hojas nicas 2-19
papel sin fin 2-19
Parada para evaluacin posterior 3-35, 3-55, 5-11
Parada pospuesta 3-42, 3-61
Parmetros (aclaracin) 20
Paridad
balanza 2-22
impresora 2-20
ordenador 2-23
terminal 2-25
Parte trasera del titulador 10-9
Pendiente
clculo 3-69
electrodo de pH 26
explicacin 2-9
registrar 2-9
valor mximo/mnimo 3-71
valor terico 2-9
08/2004
Indice
08/2004
13-17
Indice
13-18
Soluciones tampn
tampones DIN/NIST 3-70
tampones MERCK 3-69
tampones METTLER TOLEDO 3-69
Solventes
almacenar 2-28
aadir 2-28
borrar 2-27
cambiar 2-27
Sonda de temperatura
almacenar 2-12
calibrar 6-6
enchufe Lemo 10-10
medios auxiliares 2-11
Pt100/Pt1000 2-11
seleccionar 3-13
srel (desviacin estndar relativa) 8-7
ST20A
conectar 10-10
salidas 2-28
Stand 1/2 (cabezas de valoracin) 2-17
Stirrer (agitador) 6-8
Sustancia patrn 30, 31
T (temperatura) 7-10
t (ttulo) 3-72, 8-3
t(mx)
func. medir 3-18
func. temperatura 7-10
func. valoracin EP 3-39
func. valoracin EQP 3-25
func. valoracin EQP (Ipol/Upol) 3-49
t(mn)
func. medir 3-17
func. temperatura 7-10
func. valoracin EP 3-39
func. valoracin EQP 3-25
func. valoracin EQP (Ipol/Upol) 3-49
Tabla de valores medidos
hacer un informe 3-75, 6-24
visualizar 5-7, 6-21
Tamao de muestras 3-21, 3-38, 3-48, 3-59, 8-3
Tarjeta Centronics
installacin 10-10
posibilidades de conexin 10-9
08/2004
Indice
Tarjeta KF
electrodos polarizados 2-13
entradas de medida: datos de calibracin 6-29
entradas y salidas 10-10
instalar 10-11
Tarjeta memoria
directorio 6-37
formatizacin 6-36, 6-40
insercin 10-11
interface 12-6
tipos 12-6
uso 6-36
Tarjeta pH
entradas de medida: datos de calibracin 6-29
entradas y salidas 10-10
instalar 10-11
sensores 2-7
Tarjeta RS
instalacin 10-11
posibilidades de conexin 10-11
Tecla(s)
de entrada 10
flecha 7
Reset 7, 5-12
de mandos 9
Teclado (titulador) 7
Teclado externo
asignacin de las teclas 10-15
conectar 10-15
definir 2-26
Temperatura
correccin 3-13, 3-69
entrar 2-9, 4-6, 5-6
funcin 7-10
medir 2-9, 3-13, 3-18, 3-20, 3-37, 3-62, 3-69,
7-10
medir (funcin auxiliar) 6-5
Tendencia
func. pH/mV-Stato 3-64
func. valoracin EP 3-42
func. valoracin EP (Ipol/Upol) 3-61
func. valoracin EQP 3-32
func. valoracin EQP (Ipol/Upol) 3-51
Terminacin (parmetros)
func. pH/mV-Stato 3-64
func. valoracin EP 3-42
func. valoracin EP (Ipol/Upol) 3-61
func. valoracin EQP 3-33
func. valoracin EQP (Ipol/Upol) 3-52
08/2004
Terminal
asignacin de teclas 10-17
conectar 10-11
configuracin 10-16
sincronizacin 2-25
Tiempo
entrar 6-27
func. agitar 3-16, 5-7
func. muestra (acondicionar) 3-15
seleccionar formato 6-26
Tiempo
de agitacin 3-16
de espera 3-16
de mezcla (func. valoracin en dos fases) 7-14
de separacin (func. valoracin en dos fases)
7-14
fijo (func. salida mando a distancia) 7-16
mx. (func. entrada mando a distancia) 7-15
mximo (func. valoracin EP (Ipol/Upol)) 3-61
TIME 5-4, 8-3
Tipo de medicin
func. valoracin en dos fases 7-14
func. valoracin EQP 3-25
func. valoracin EQP (Ipol/Upol) 3-49
Tipo de sincronizacin (func. sincronizacin) 7-18
Tipo de transmisin (balanza)
bidireccional 2-21
unidireccional 2-21
Tipo de transmisin (ordenador) 2-24
Titulador
acumulador 6
apertura de la carcasa 10-3
autotest 7
conexiones 6, 10-10
configuracin 6-26
documentacin 4
ID (identificacin ) 6-27
limpieza de la carcasa 10-3
mando a distancia 6-42
reloj interno 6
teclado 7
vista frontal 6
vista trasera 6, 10-10
Ttulo
controlar 2-5
determinacin (disolucin NaOH) 32
entrar 2-4
explicacin 30
funcin 3-72
registrar 2-4
Transmisin de datos (Data Transfer) 6-36
13-19
Indice
TTL (entradas)
activar 6-32
cableado electrnico 10-14
cableado mecnico 10-13
TTL (salidas)
activar 6-33
cableado electrnico 10-14
TTLIO (conectores)
datos tcnicos 12-7
entradas y salidas 10-13
usado con titulador 10-13
Umbral 3-29, 3-51
Unidad de medida (sensores) 2-8
Unidades 3-67, 8-17, 8-18
Valoracin
a punto de equivalencia 3-20, 3-45
a punto final 3-37, 3-56
de aprendizaje funcin 3-43
en dos fases funcin 7-12
EP (funcin) 3-37
EP (Ipol/Upol) (funcin) 3-56
EQP (funcin) 3-20
EQP (Ipol/Upol) (funcin) 3-45
manual 6-14
manual (Ipol/Upol) 6-16
mtodo especial 7-12
previa (func. pH/mV-Stato) 3-63
resultados 5-9
Valoraciones Karl-Fischer
accesorios 11-12
Valor del umbral
procedimiento de evaluacin estndar 3-30
procedimiento de evaluacin: asimtrica 3-30
procedimiento de evaluacin: mnimo/mximo
3-30
procedimiento de evaluacin: segmentada 3-31
Valor de semineutralizacin 3-20
Valor medio x
func. clculo 3-67
func. ttulo 3-72
func. valor auxiliar 3-73
Valor(es) auxiliar(es)
almacenar 2-16
entrar 2-15
funcin 3-73
medios auxiliares 2-15
registrar 2-15
Valores medidos
instrucciones para memorizacin 3-64, 3-74,
8-20
nmero mximo/func. valoracin 8-20
visualizar 5-7, 6-21
13-20
08/2004
Indice analitico
Indice analitico
I numeri separati da un trattino (esempio: 3-38) si riferiscono alle sezioni e pagine del manuale
d'uso, mentre i numeri senza trattino si riferiscono alle istruzioni di base (esempio: 9).
<F1>...<F5> 9, 10
E
funzione Misurare 3-17
funzione Titolazione EP 3-39
funzione Titolazione EQP 3-25
funzione Titolazione EQP (Ipol/Upol) 3-49
E(nom.)
funzione Titolazione EP 3-39
funzione Titolazione EQP 3-22
t
funzione Misurare 3-17
funzione Titolazione EP 3-39
funzione Titolazione EQP 3-25
funzione Titolazione EQP (Ipol/Upol) 3-49
Abbreviare lanalisi 6-30
Accessori
accessori facoltativi 11-7
equipaggiamento di base 11-4
Accumulatore 6
Aggiunta di titolante
funzione pH/mV-Stat 3-63
funzione Titolazione a due fasi 7-14
funzione Titolazione EP 3-39
funzione Titolazione EP (Ipol/Upol) 3-60
funzione Titolazione EQP 3-22
funzione Titolazione EQP (Ipol/Upol) 3-48
Agitare (funzione) 3-16
Agitatore
funzione ausiliaria (Stirrer) 6-8
selezionare luscita 2-17
Allineamento degli ingressi di misura 6-28
Analisi
arresto 5-11
eclissare 5-11
inizio 5-4
interrompere (Reset) 5-12
menu Run 5-3
svolgimento del menu 5-4
Arresto (parametri di)
funzione pH/mV-Stat 3-64
funzione Titolazione EP 3-42
funzione Titolazione EP (Ipol/Upol) 3-61
funzione Titolazione EQP 3-33
funzione Titolazione EQP (Ipol/Upol) 3-52
08/2004
13-21
Indice analitico
13-22
Connettore(i) TTLIO
dati tecnici 12-7
ingressi ed uscite 10-13
utilizzati dal titolatore 10-13
Continua (aggiunta di titolante) 3-40, 3-60
Controllo dallingresso
attivare luscita comando a distanza (funzione
ausiliaria) 6-33
funzione Uscita comando a distanza 7-16
Copia(e) della memoria
caricare sul titolatore 6-39
copiare su scheda di memoria 6-39
trasferire al computer 6-41
Costanti
esempi 8-18
funzione ausiliaria Calcoli 6-20
funzione Calcolo 3-66
CSTAT (coefficiente di correlazione, pH-Stat)
3-62, 8-6
Cursore 10
Curve di titolazione
1a derivata 3-30, 3-31, 3-54, 8-15
2a derivata 3-31, 3-54, 8-15
documentare 3-75, 6-24
visualizzare 5-7, 5-8, 6-21
Cx (costante di calcolo) 8-7
Data
introdurre 6-27
selezionare il formato 6-26
Data (indicazione)
metodi 3-11
sonde 2-9
sonde della temperatura 2-11
titolanti 2-5
valori ausiliari 2-15
Data di scadenza (titolante) 5-4
Data Transfer (trasferimento dei dati, funz. ausil.)
6-36
Dati di calibrazione
ingressi di misura 6-29
sonde 2-9, 2-10, 3-69
sonde della temperatura 2-12
Dati dei campioni
aggiungere 4-8
cancellare 4-6
condizioni di memorizzazione 36, 4-3
definire dal computer 4-13
documentare 3-75, 6-24
introdurre 4-4, 5-5, 5-10
modificare 4-7
stampare 4-7
08/2004
Indice analitico
Dati tecnici
agitatore 12-5
buretta 12-5
connettore Centronics 12-8
connettore RS232C (Opzione RS) 12-9
connettori TTLIO 12-7
display 12-5
connettore DIN 12-7
memoria 12-5
motore della buretta 12-5
periferiche 12-6
sistema di misura 12-3
spina RS232C (Opzione Centronics) 12-7
uscite 12-4
Deriva (misura del potenziale) 3-17
Deviazione standard relativa srel 3-67
Deviazione standard s 3-67
Dinamica (aggiunta di titolante)
funzione Titolazione EP 3-39
funzione Titolazione EQP 3-22
Disturbi 9-6
DL58
comandi 7-3
funzioni 7-3
mezzi ausiliari 7-3
DLWin Software 4-13, 6-41
Documentazione
informazioni 4
Dosaggio
continuo 6-13
continuo (Ipol/Upol) 6-15
Dosare
funzione 3-19
funzione ausiliaria (buretta) 6-12
funzione ausiliaria (ST20A) 6-10
E (potenziale) 3-17, 8-7
ESC (<F1>) 9
EHNV (valore di semineutralizzazione) 3-20, 8-4
Elettrodi (METTLER TOLEDO) 2-7, 2-13
Elettrodo di riferimento 2-7
Elettrodo per pH
calibrare 26
pendenza 26
punto zero 26
Emissione (protocolli) 3-74, 6-24
EP
assoluto 3-41
relativo 3-41
EPOT 8-4
Esperto (livello utente) 6-31
Estinzione 2-8
ET1 3-22, 3-38, 8-4
ET2 3-22, 3-38, 8-4
08/2004
13-23
Indice analitico
Indicazione voltametrica
funzione Titolazione EP (Ipol/Upol) 3-57
funzione Titolazione EQP (Ipol/Upol) 3-46
Indicazioni di sicurezza 1-1
Indice (scheda di memoria) 6-37
Indici
esempi 8-9, 8-10
riassunto 8-12
Ingressi del comando a distanza
definire 7-4
mezzi ausiliari 7-4
Ingressi TTL
attivare 6-32
avvolg. elettronico (wiring) 10-14
avvolg. meccanico 10-13
Ingresso del comando a distanza
attivare (funzione ausiliaria) 6-32
funzione 7-15
Ingresso delle sonde
sonde 2-8
sonde della temperatura 2-11
sonde polarizzate 2-13
Installazione (menu "Setup") 2-3
Installazione e manutenzione 10-3
Interfaccia Centronics
configurazioni delle stampanti 2-19
stampante GA42 2-18
Interfaccia RS232
configurazioni delle stampanti 2-20
stampante GA42 2-20
Interpolazione (valutazione) 8-14
Intervallo (condizionare) 3-15
Intervallo di memorizzazione (funz. pH/mV-Stat)
3-64
Istruzione
ESC (<F1>) 9
funz. Uscita comando a distanza 7-17
funzione 7-11
OK (<F5>) 9
modificare (<F4>) 10
LabX Software 4-13, 6-41
Lavare
funzione ausiliaria (ST20A) 6-10
parametri dello stativo di titolazione 3-14
la punta 6-12
Lettore di codici a barre
collegare 10-16
definire 2-24
Limiti di peso
introdurre 3-12
introduzione dei dati dei campioni 4-5, 5-6
13-24
Limiti di volume
introdurre 3-12
introduzione dei dati dei campioni 4-5, 5-6
Linee di cornice (protocollo) 2-19
Lingua (cambiare) 11, 6-27
Lista dei dati dei campioni 4-4, 4-6
Lista dei risultati
bloccare 6-30
indicazioni 5-9
visualizzare 6-18
Liste (spiegazione) 8
Livello utente 6-31
M (massa molare) 3-68, 8-3
m (quantit del campione) 8-3
Manuale (introduzione della temperatura) 3-13
Manutenzione
buretta 10-7
titolatore 10-3
Maschera dei dati del campione
menu Analisi 5-5
menu "Sample" 4-5
Maschere (spiegazione) 8
Massa molare M
introdurre 3-13
funzione Calcolo 3-68
Massimo (procedura di valutazione)
parametri di valutazione 3-34, 3-53
riconoscimento del punto dequivalenza 3-28,
3-50
spiegazione 8-14
Memoria dei dati dei campioni (menu "Sample")
4-3
Memoria dei dati utente 12-5
Memoria dei valori ausiliari 3-73
Memorizzare
dati dei campioni 4-3
metodi 3-7
risultati 8-20
risultati grezzi 8-20
sensori polarizzati 2-13
solventi 2-28
sonde 2-10
sonde della temperatura 2-12
strumenti per ingresso comando a distanza 7-5
strumenti per uscita comando a distanza 7-6
titolanti 2-6
valori ausiliari 2-16
valori misurati 3-64, 3-74, 8-20
Menus
riassunto 1-2, 1-3
spiegazione 8
tasti 8
08/2004
Indice analitico
Messaggi di errore
con riferimento al cap. 9.1 9-3
"EPROM test failed" 9-3
"RAM test failed" 9-3
Titolazione in auto-studio 5-11
Metodi
menu 3-3
selezionare 3-4
stampare la lista 3-4
Metodi METTLER
90001: Esecuzione 14
90002: Esecuzione 27
modificare 25, 3-6
spiegazione 19
stampare 3-6
Metodi speciali
DL58 7-7
spiegazione 7-3
Metodi standard
esempi di applicazione 22
funzioni 20
modificare 25, 30
numero 20
spiegazione 19, 3-5
stampare 3-5
Metodi utente
cancellare 3-6
copiare su scheda di memoria 6-38
copiare sul titolatore 6-39
spiegazione 19, 3-6
stampare 3-6
titolo con titolazione EQP 34
trasferire al computer 6-41
Metodo
a partire dal computer 4-5
cancellare 3-5
memorizzare 3-7
modificare 3-7
modificare (metodo in corso: DL55/DL58) 5-13
modificare (serie di campioni in corso) 5-12
realizzare 24
spiegazione 3-3
stampare 3-4
sulla scheda di memoria 4-5
Mezzi ausiliari
cambiare 5-8
cancellare 2-3
copiare su scheda di memoria 6-39
copiare sul titolatore 6-39
DL58 7-3
lista 2-3
modificare 2-3
spiegazione 2-3
stampare 2-3
trasferire al computer 6-41
08/2004
13-25
Indice analitico
13-26
08/2004
Indice analitico
Punto(i) di equivalenza
campo 3-32, 3-51
formule per circoscrivere 8-19
numero massimo/determinazione di campioni
8-20
riconoscimento 3-28, 3-50
spiegazione 3-20, 3-45, 8-14
Q 8-4
QDISP 3-19, 8-7
QEND 8-4
QEX 8-4
QP1/QP2 8-4
QSTAT 8-6
QT1/QT2 8-6
QTOT 8-6
Quantit del campione 3-21, 3-38, 3-48, 3-59, 8-3
R (risultati) 3-66, 8-7
Report (protocollo) 6-24
Reset (tasto) 7, 5-12
Results (risultati) 6-18
Riconoscimento (punto di equivalenza) 3-28, 3-50
Risultati grezzi
condizioni di memorizzazione 8-20
documentare 3-75, 6-24
riassunto 8-8
spiegazione 3-18
Risultato(i)
cancellare 6-22
condizioni di memorizzazione 8-20
documentare 3-75, 6-24
esempi 3-67, 8-17
funzione ausiliaria (Results) 6-18
numero massimo/serie di campioni 8-20
R 3-66, 3-71
Rx 6-20
titolazione in auto-studio 5-9
unit 3-67, 8-17
Ritardo nellarresto 3-42, 3-61
Rivalutazione
condizione soddisfatta 5-11
definire la condizione 3-35, 3-36, 3-55
eseguire 6-18
Routine (livello utente) 6-31
Run
funzione dei tasti 5-3
menu Analisi 5-3
08/2004
13-27
Indice analitico
13-28
08/2004
Indice analitico
Tempo
di agitazione 3-16
di attesa 3-16
di mescolazione (funz. Titol. a due fasi) 7-14
di separazione (funz. Titol. a due fasi) 7-14
fisso (funz. Uscita comando a dist.) 7-16
funzione Agitare 3-16, 5-7
funzione Campione (condizionare) 3-15
introdurre 6-27
massimo (funz. Ingresso comando a dist.) 7-15
massimo (funzione Titolazione EP (Ipol/Upol))
3-61
selezionare il formato 6-26
TIME 5-4
Tendenza
funzione pH/mV-Stat 3-64
funzione Titolazione EP 3-42
funzione Titolazione EP (Ipol/Upol) 3-61
funzione Titolazione EQP 3-32
funzione Titolazione EQP (Ipol/Upol) 3-51
Terminale
assegnazione dei tasti 10-17
collegare 10-11
configurazione 10-16
configurazione (titolatore) 2-25
Testata del protocollo 6-27
TIME 5-4, 8-3
Titolante
aggiungere 2-6
cancellare 2-4
concentrazione 2-4, 8-3
memorizzare 2-6
modificare 2-4
Titolatore
accumulatore 6
aprire linvolucro 10-3
autodiagnosi 7
collegamenti 6, 10-10
comando a distanza 6-42
configurazione (titolatore) 6-26
documentazione 4
ID (identificazione) 6-27
orologio interno 6
pulire linvolucro 10-3
tastiera 7
vista anteriore 6
vista dorsale 6, 10-10
08/2004
Titolazione
a punto dequivalenza 3-20, 3-45
a punto finale 3-37, 3-56
EP (funzione) 3-37
EP (Ipol/Upol) (funzione) 3-56
EQP (funzione) 3-20
EQP (Ipol/Upol) (funzione) 3-45
manuale 6-14
manuale (Ipol/Upol) 6-16
Titolazione a due fasi
funzione 7-12
metodo speciale 7-12
Titolazione in auto-studio
funzione 3-43
resultati 5-9
Titolazione Karl Fischer
accessori 11-12
Titolo
funzione 3-11
metodi METTLER 19
metodi standard 19
Titolo (concentrazione)
controllare 2-5
determinazione (sol. di NaOH) 32
funzione 3-72
introdurre 2-4
spiegazione 30
trascrizione automatica 2-4
Trasferimento dei dati (Data Transfer) 6-36
Unidirezionale (modo di trasmissione) 2-21
Unit 3-67, 8-17, 8-18
Unit di misura (sonde) 2-8
Uscita del comando a distanza
attivare (funzione ausiliaria) 6-33
funzione 7-16
Uscite del comando a distanza
definire 7-5
mezzi ausiliari 7-5
Uscite TTL
attivare 6-33
avvolg. elettronico (wiring) 10-14
13-29
Indice analitico
Valore(i) ausiliare(i)
funzione 3-73
introdurre 2-15
memorizzare 2-16
mezzi ausiliari 2-15
trascrizione automatica 2-15
Valore di semineutralizzazione 3-20
Valore di soglia
procedura di valutazione: asimmetrico 3-30
procedura di valutazione: minimo/massimo 3-30
procedura di valutazione: segmentato 3-31
procedura di valutazione: standard 3-30
Valore medio x
funzione Calcolo 3-67
funzione Titolo 3-72
funzione Valore ausiliario 3-73
Valutazione
funzione pH/mV-Stat 3-65
funzione Titolazione EQP 3-34
funzione Titolazione EQP (Ipol/Upol) 3-53
Varia (Misc. ...) 6-26
VDISP 3-19, 8-7
Velocit (agitatore)
definire 3-16
modificare 5-8, 6-8
Velocit della pompa (solventi) 2-27
Velocit di trasmissione
bilance 2-22
computer 2-23
stampante 2-20
terminale 2-25
VEND 8-4
VEQ 8-4
Versione del software 1-1
VEX 8-4
Vista dorsale del titolatore 10-9
Volume
introdurre 4-5, 5-6
selezionare 3-12
Volume della buretta
lincremento pi piccolo 3-24
selezionare 2-5
Volume fisso
avviso 5-5
selezionare 3-12
Volume massimo
funzione pH/mV-Stat 3-64
funzione Titolazione EP 3-42
funzione Titolazione EP (Ipol/Upol) 3-61
funzione Titolazione EQP 3-33
funzione Titolazione EQP (Ipol/Upol) 3-52
13-30
VP1/VP2 8-4
VSTAT 8-6
VT 3-65, 8-6
VT1/VT2 8-6
VTOT 8-6
x (valore medio) 8-7
z (numero di equivalenza) 3-13, 3-68, 8-3
ZERO (punto zero degli elettrodi) 8-3
08/2004
Contents
Page
ISO 9001 certificate for METTLER TOLEDO ......................................................................
Certificado ISO 9001 para METTLER TOLEDO .................................................................
Certificato ISO 9001 per la METTLER TOLEDO ................................................................
15-3
15-3
15-3
15-4
15-6
15-8
08/2004
15-1
08/2004
15-3
Product Guidelines
Performance Specifications
Documentation Plan
Software Specifications
Quality Plan
Project Management System
Test Plan
Customer Requirements
Review Reports
Source Code
Mettler-Toledo GmbH, Analytical will maintain possession of all documents and their reproductions and
may require a non-disclosure agreement to be provided by those requiring access to these documents.
Schwerzenbach,
January 1999
15-4
08/2004
Project Study
Project Start
Project Release
Phase:
Basic Know how
Product Guidelines
Performance Specifications
Quality Plan
Documentation Plan
Project Plan
Review Report
Phase:
Feasibility
Software Specifications
Test Plan
Review Report
Phase:
Confirmation
Review Report
Project End
Phase:
Readiness
Review Report
Usage
Phase out
08/2004
15-5
Schwerzenbach,
Enero 1999
15-6
08/2004
Comienzo del
proyecto
Fase:
Conocimientos
bsicos
Fase:
Viabilidad
Fase:
Verificacin
Protocolo de revisin
Fase:
Preparacin
Protocolo de revisin
Utilizacin
Sustitucin
08/2004
15-7
La Mettler-Toledo GmbH, Analytical, rimarr in possesso di tutti i documenti e di tutte le loro copie e
contrarr un accordo di discrezione con coloro che desiderassero visionare tali documenti.
Schwerzenbach,
Gennaio 1999
15-8
08/2004
Inizio del
progetto
Fase:
Fattibilit
Fase:
Conferma
Rapporto di revisione
Fase:
Disponibilit
Rapporto di revisione
Utilizzazione
Sostituzione
08/2004
15-9
*P51709614*
ME-51709614F