Professional Documents
Culture Documents
3000 systems
TN/TS/TX
Version: 2.0.2
User Manual
TN-TS 3000
Rev. 2.0.2
Disclaimer
Save to the extent permitted by law, the Customer hereby undertakes not to alter or modify the whole
or any part of the software incorporated in the Products in any way whatever nor permit the whole or
any part of the software to be combined with or become incorporated in any other programs nor
decompile disassemble or reverse engineer the same nor attempt to do any other such things.
In no event shall [Thermo Fisher Scientific] have any obligation to repair or replace in accordance with
any warranties given with the Product in whole or in part, as the result of
The warranty shall not apply to any software which the Customers alters or modifies.
Thermo Fisher Scientific does not warrant that the software is error-free, will accomplish any particular
result or is fit for any particular purpose of or intended use by the Customer and it is for the Customer
to satisfy yourself that the software is so fit.
The photographs used in this manual can differ from the actual apparatus and set-ups. All
photographs, drawings and diagrams are for illustrative purposes only.
Page 2 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
Copyright
The content of this manual is protected by copyright.
All efforts have been made to ensure the accuracy of the contents of this manual. However should any
errors be detected Thermo Fisher Scientific would greatly appreciate being informed of them
The above notwithstanding Thermo Fisher Scientific can assume no responsibility for any errors in this
manual or their consequences.
For more information, check our website at www.thermo.com
Any use of this manual other than, intended by the producer, is prohibited without the prior written
permission of Thermo Fisher Scientific
2000-2007, Copyright reserved by Thermo Fisher Scientific Delft, The Netherlands
Page 3 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
Content
1.
2.
3.
4.
Page 4 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
4.2.7.
Outlet connection (TN)..................................................................................... 36
4.3.
PERMA PURE .............................................................................................................. 36
4.4.
GLASS-FIBER FILTER ................................................................................................. 37
4.5.
GAS CONNECTION TN-TS, SEPARATE AND SIMULTANEOUSLY .................................. 37
4.5.1.
Separate analyses............................................................................................. 37
4.5.2.
Simultaneous analyses ..................................................................................... 37
4.5.3.
Connection furnace outlet TS only ................................................................... 38
4.5.4.
Mode selection gas flow: separate or simultaneous ........................................ 40
4.6. UV-F DETECTOR MODULE ......................................................................................... 41
4.6.1.
Connections and settings on UV-F detector .................................................... 42
5.
Page 5 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
5.3.5.1.
Starting ThEuS...................................................................................... 55
5.3.5.2.
Creating a calibration ............................................................................... 58
5.4.
QUICK PERFORMANCE CHECK TN/TS MODE .............................................................. 59
5.4.1.
TN mode test (setting is low range).................................................................. 59
5.4.2.
TS-UV mode test (setting is mid-range) ........................................................... 59
5.5.
3000 SYSTEM STANDBY MODE .................................................................................. 60
5.6.
3000 SYSTEM SHUT DOWN ......................................................................................... 60
6.
TN WATER .................................................................................................................... 61
6.1.
INTRODUCTION .......................................................................................................... 61
6.2.
SPECIFICATIONS ........................................................................................................ 62
6.2.1.
Standardized methods ...................................................................................... 62
6.2.2.
Test results of the TN-3000 water .................................................................... 62
6.2.3.
Summary/conclusion ........................................................................................ 63
6.3.
MAINTENANCE OF THE GLASSWARE .......................................................................... 64
6.3.1.
Boat and introduction module.......................................................................... 64
6.3.2.
Outlining of the boat ........................................................................................ 65
6.3.3.
Replacement of the Nickel sample cylinder ..................................................... 65
6.3.4.
NeXYZ auto sampler......................................................................................... 66
6.3.5.
Furnace tube and outlet ................................................................................... 66
6.3.6.
Principle of the furnace outlet tube.................................................................. 68
6.3.7.
Cold trap, tubing and filter .............................................................................. 69
6.4.
SEVERAL REMARKS AND TIPS .................................................................................... 71
6.5.
FREQUENT MAINTENANCE ......................................................................................... 71
6.6.
TROUBLE SHOOTING .................................................................................................. 72
6.7.
FLOW DIAGRAM TN WATER ...................................................................................... 74
7.
Page 6 of 169
User Manual
TN-TS 3000
8.
Rev. 2.0.2
9.
10.
10.1.
3000 SYSTEM TX/TS MODE STARTING UP........................................................ 116
10.1.1. Preparation of reagents ................................................................................. 116
10.1.1.1.
Sulfuric acid solution ............................................................................. 116
10.1.1.2.
Halide electrolytic solution .................................................................... 116
10.1.1.3.
Sulfur electrolytic solution..................................................................... 116
10.1.2. AOX reagents ................................................................................................. 117
10.1.2.1.
Nitrate stock solution ............................................................................. 117
10.1.2.2.
Nitrate wash solution.............................................................................. 117
10.1.2.3.
p-Chlorophenol stock solution (200 mg Cl/L) ....................................... 117
10.1.2.4.
p-Chlorophenol standard solution (1 mg Cl/L) ...................................... 117
User Manual 3000 systems V2.0.doc
Page 7 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
10.1.2.5.
p-Chlorophenol test solution (100 g Cl/L)........................................... 117
10.1.3. POX reagents ................................................................................................. 117
10.1.3.1.
Dichloromethane stock solution (1000mg Cl/L).................................... 117
10.1.3.2.
Dichloromethane standard solution (100mg Cl/L) ................................ 117
10.1.3.3.
Dichloromethane test solution (100 g Cl/L) ........................................ 117
10.1.4. TX/EOX reagents............................................................................................ 118
10.1.4.1.
Aldrin stock solution (1000 mg Cl/L) .................................................... 118
10.1.4.2.
Aldrin standard solution (100 mg Cl/L)................................................. 118
10.1.4.3.
Aldrin test solution (10 mg Cl/L)........................................................... 118
10.1.5. TS/EOS reagents ............................................................................................ 118
10.1.5.1.
Diphenylsulfide stock solution (1000mg S/L) ....................................... 118
10.1.5.2.
Diphenylsulfide standard solution (100mg S/L) .................................... 118
10.1.5.3.
Diphenylsulfide test solution (10mg S/L) .............................................. 118
10.1.6. Preparation of samples .................................................................................. 119
10.1.6.1.
AOX sample preparation........................................................................ 119
10.1.6.2.
POX sample preparation ........................................................................ 121
10.1.6.3.
TOX sample preparation ........................................................................ 121
10.1.6.4.
EOX sample preparation ........................................................................ 122
10.1.7. Adjusting gas flows ........................................................................................ 124
10.1.8. Filling the scrubber........................................................................................ 124
10.1.8.1.
Sulfuric acid scrubber ............................................................................ 124
10.1.8.2. NOx-scrubber.......................................................................................... 125
10.1.9. Powering the system....................................................................................... 125
10.1.10.
Installing a selected Module ...................................................................... 125
10.1.11.
Titration cell (chloride).............................................................................. 126
10.1.12.
Titration cell (sulfur).................................................................................. 127
10.1.13.
Gas leakage test coulometric configuration .............................................. 128
10.2.
3000 SYSTEM NORMAL OPERATION.................................................................. 130
10.2.1. Visible inspection of glassware...................................................................... 130
10.2.2. Glassware maintenance ................................................................................. 130
10.2.2.1.
Scrubber ................................................................................................. 130
10.2.2.2.
Furnace tube ........................................................................................... 131
10.2.2.3.
Liquids module....................................................................................... 131
10.2.2.4.
AOX glassware ...................................................................................... 131
10.2.2.5.
POX glassware ....................................................................................... 132
10.2.2.6.
Solids glassware ..................................................................................... 132
10.2.3. Introduction module ....................................................................................... 132
10.2.3.1.
Solids Module ........................................................................................ 132
10.2.3.2.
Liquids Module ...................................................................................... 132
10.2.3.3. AOX Module.......................................................................................... 132
10.2.3.4.
POX Module .......................................................................................... 132
10.2.4. Standard setpoints .......................................................................................... 133
10.3.
3000 SYSTEM STANDBY MODE ......................................................................... 133
10.4.
3000 SYSTEM SHUT DOWN................................................................................ 134
11.
11.1.
11.2.
Page 8 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
11.2.1.1.
Manual introduction POX ...................................................................... 135
11.2.1.2.
Manual introduction AOX ..................................................................... 136
11.2.1.3.
Manual introduction Solids, water and heavy hydrocarbons ................. 137
11.2.1.4.
Manual injection EOX and light hydrocarbons.................................. 138
11.3.
AUTOMATIC ANALYSIS IN GENERAL .................................................................... 138
11.4.
AUTOMATIC ANALYSIS USING SPECIFIC MODULES/METHODS............................... 139
11.4.1.1.
Automatic analysis AOX ....................................................................... 139
11.4.2. Automatic introduction Solids, water and heavy hydrocarbons................ 139
11.4.2.1.
Automatic injection EOX and light hydrocarbons ............................. 139
12.
13.
14.
15.
16.
17.
18.
APPENDIX IV CONVERSION TABLE: MANUAL ROTAMETERS TO
DIGITAL MASSFLOW METERS .................................................................................... 167
19.
Page 9 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
1. GENERAL INFORMATION
1.1. Operating Manual
This operating manual has been written with the user of the 3000 system in
mind. For this reason the manual mainly gives instructions detailing
operation of the apparatus and does not give detailed directions for the
maintenance or repair of the apparatus.
The organization making use of the 3000 system must ensure itself that the
operator is qualified to use an instrument of this sort and is capable of
following the recommendations for its use.
The operator should closely follow the instructions contained in this operating
manual in order to ensure the proper operation of the instrument.
This manual makes use of special signs and pictograms in order to highlight
remarks and instructions, which require special attention.
These signs and pictograms are listed in section 1.2 of this chapter.
Chapter 2 General Safety Instructions" details the safety pictograms
appearing on the outside of / and inside the apparatus. All directions relating
to these pictograms must be complied with at all times.
Should you encounter problems or have questions, which are not discussed
in this manual, please do not hesitate to get in touch with your Thermo Fisher
Scientific supplier.
Voltaweg 22
2627 BC, Delft
The Netherlands
Tel.: +31 (0)15 2571314
Fax.:+31 (0)15 2572297
EMail: support.elemental.nl@thermofisher.com
(for technical questions and remarks)
support.sid.nl@thermofisher.com
(for questions and remarks about the users guide)
Web: http://www.thermo.com
Page 10 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
1.2. Pictograms
The following pictograms are used to highlight the information contained in
the text of this manual.
Special Attention
Text preceded by this sign should be read with special care.
Warning
Instructions preceded by this sign must be complied with
exactly.
Failure to do so may result in damage to the equipment or
physical injury. Furthermore, the measurement procedure may
be disturbed.
Electrical Hazard
Instructions preceded by this sign must be complied with
exactly. Failure to do so may result in physical injury.
Heat
Instructions preceded by this sign must be complied with
exactly. Failure to do so may result in physical injury.
Page 11 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
Page 12 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
Before using the 3000 system carefully read through this operating manual. It is
essential that the persons operating the apparatus or who come into direct
contact with it are fully informed of the nature and existence of all possible
hazardous areas in and around the apparatus.
2.1. Safety Marks on the equipment
Thermo Fisher Scientific uses the following safety colors and signs on the
analysis apparatus. These are based on the ISO 3864 international
standards for safety colors and signs. These signs indicate those locations
that require special attention and/or constitute a danger to personnel or the
apparatus.
The safety markings may be replaced or supplemented by explanatory texts.
All personnel coming into either direct or indirect contact with the 3000
system should be fully acquainted with these international safety-markings.
The signs and accompanying texts appearing on or inside the 3000 system
are shown below.
THE FURNACE CAN ATTAIN VERY HIGH
TEMPERATURES
HIGH VOLTAGE!
DO NOT REMOVE COVER!
Page 13 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
Page 14 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
Page 15 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
UV-Fluorescence
detector
Permapure
Chemiluminescense
detector
Gas outlet
Page 16 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
Gas entrance
Fig. 1:
Gas exit
Detection is based on the principle that SO2 molecules absorb ultraviolet (UV)
light and become exited, then decay to a lower energy state emitting UV light at
a specific wavelength.
The sample flows into the reaction chamber, where pulsating light (at a rate of
10 Hz) excites the SO2 molecules. The condensing lens focuses the pulsating
UV light into the mirror assembly. The mirror assembly contains eight selective
mirrors that reflect only the wavelengths, which excite SO2 molecules.
As the excited SO2 molecules decay to a lower energy state, an amount of UV
light is emitted that is proportional to the SO2 concentration. The band-pass filter
allows only the wavelengths emitted by the excited SO2 molecules to reach the
Photo Multiplier Tube (PMT). The PMT detects the UV light emission from the
decaying SO2 molecules. The photodetector located at the end of the
fluorescence chamber, continuously monitors the pulsating UV light source and
is connected to a circuit that compensates for fluctuations in the intensity of the
UV light. (AGC controlled)
Page 17 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
Vibrational
relaxation
Intersystem
crossing
Internal &
external
conversion
Absorption
Fluorescence
Vibrational
relaxation
Phosphorescence
SO2 + h1 SO*2
SO*2 SO2 + h 2
h1 = primary UV-Light
h2 = Emitted light of decaying SO2
Page 18 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
In seven steps:
1.
2.
3.
4.
5.
6.
7.
NO + O3
NO2*
NO2* + O2
NO2 + h
The emitted light is detected by the PMT and the generated area is integrated and
converted into a value representing the amount of nitrogen in the sample.
In seven steps:
1.
2.
3.
4.
5.
6.
7.
Page 19 of 169
User Manual
TN-TS 3000
3.4.
Rev. 2.0.2
The following figure displays the flow path of the 3000 system.
(Optional extension with a Halogen detection cell requires an exchange of the
permapure dryer for a (heated) glass connection (part number: ECS300009).)
Dryer gas in
Ar
Liquid Module
Perma Pure
Vacuum pump
Ozone Killer
Ozone Generator
PMT detector
Temp. Contr.
Capillary
Page 20 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
Page 21 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
Page 22 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
Page 23 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
Page 24 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
3.6. Furnace
According to ASTM requirements, the furnace is divided into two temperature
zones.
The temperature in each zone can be adjusted individually, up to 1100C.
Maximum temperature difference between the zones is approximately 500C.
Two different furnace tubes are available:
A.
Standard furnace tube (for water applications and noncombustibles)
B.
Turbo tube (for petrochemical/hydrocarbon applications and
other highly flammables)
Both furnace tubes are supporting all available introduction modules.
3.6.1. Standard furnace tube
Actually, this is an empty tube mostly used for water samples where
chance of soot formation is practically excluded.
Page 25 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
Page 26 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
3.7. Conditioning
3.7.1. Drying
The gas flow coming from the furnace travels through a Perma pure
membrane dryer. The principle of the nafion perma pure membrane
dryer is the diffusion of water out of the gas stream, by co-polymers with
sulfuric acid ligands.
Page 27 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
Page 28 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
Page 29 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
6
5
3
1
2
1.
2.
3.
4.
5.
6.
7.
8.
9.
PMT housing
Gold plated, heated reaction chamber
Capillary location (heated)
Gas output
Ozone input
Analyses gas input
Heater connection
Photo Multiplier connections
Cooling block PMT (Peltier driven)
Page 30 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
4.2.
The power cable has to be connected to the 3000 system. The 3000
system has two additional power-outputs of 150 VA.
Page 31 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
Warning
Before turning the 3000 system on for the first
time, the voltage setting must be checked. The
small plate beneath the power lead should be
positioned in a way that the 230 V indication is in
the normal position (not upside down) and is read
from left to right when the operator is facing the
back of the apparatus.
The 115 V indication will then be upside down.
Should you need to switch from a 230 V to a 115
Volts supply, pull the plate away from the
instrument so that the prongs of the plug are fully
withdrawn from the apparatus and re-insert the
other way up.
Electrical Hazard
Do not open the cabinet when the power cable is
connected. Remove it from the wall outlet and
disconnect the cable from the analyzer
completely.
Special Attention
After supplying power to the analyzer and starting
the program, the furnaces and heating elements
will rise to the standard temperatures required by
the connected module. (initialization procedure)
When no module is connected, the apparatus will
go into standby mode (i.e. no furnace control).
Figure: com-connector
Warning
Wrong connections could lead to malfunction of
the analyzer or computer.
Page 32 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
Page 33 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
4.2.5.2.
Page 34 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
second flow meter from the right! The right flow meter
corresponds with the oxygen connector on the right!
4.2.5.3.
The furnace tube and outlet become very hot during the
operation of the 3000 system. Carelessness may result
in burns. Avoid contact with bare hands. Use special
protective gloves and/or tools for hot tube removal.
The safest way for removal is allowing the furnace to
cool down completely.
Page 35 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
Page 36 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
Page 37 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
UV fluorescence detector
Page 38 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
Coupling (PMECH0368)
Page 39 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
Simultaneous Mode
TN Mode Only
Loop in both connectors. (outlet from particle filter
goes into the molybdenum converter)
Page 40 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
Page 41 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
1
2
3
1.
2.
3.
4.
Page 42 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
For most applications the mid-range is considered the ideal working range
Warning
Before turning the UV detector module on for the
first time, the voltage setting must be checked.
The small plate beneath the power lead should be
positioned in a way that the 230 V indication is in
the normal position (not upside down) and is read
from left to right when the operator is facing the
back of the apparatus.
The 115 V indication will then be upside down.
Should you need to switch from a 230 V to a 115
V supply pull the plate away from the instrument
so that the prongs of the plug are fully withdrawn
from the apparatus and re-insert the other way
up.
Electrical Hazard
Do not open the cabinet before the power cable is
removed.
Special Attention
With power supplied to the UV detector, the
heating elements will rise to the standard
temperature required for optimum performance.
Page 43 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
5.2.
Preparation of standards
Furnace tube and permapure connection
Module connection
Powering the system
Adjust gas flow
Gas leakage test
Preparation of solutions
All necessary solutions, needed for good analysis are described below.
Page 44 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
Page 45 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
Formula
MM
101.1
132.13
75.06
Molfr N
0.138
0.212
0.187
Mix
Nitrate
Ammonia
Glycine
Conc. N mg KNO3 mg (NH4)2SO4 mg KNO3 and mg (NH4)2SO4 mg C2H5NO2
mg N/L
per L
per L
per L
per L
1
2
5
10
25
50
75
100
1000
7.22
14.44
36.11
72.21
180.54
361.07
541.61
722.14
7221.43
4.72
9.44
23.59
47.19
117.97
235.95
353.92
471.89
4718.93
3.61
7.22
18.05
36.11
90.27
180.54
270.80
361.07
3610.71
+
+
+
+
+
+
+
+
+
2.36
4.72
11.80
23.59
58.99
117.97
176.96
235.95
2359.46
5.36
10.72
26.81
53.61
134.04
268.07
402.11
536.14
5361.43
Page 46 of 169
User Manual
TN-TS 3000
5.2.3.1.1.
Rev. 2.0.2
Pipette 10 mL of the Nitrate stock solution into a measuring flask and fill to 100
mL with de-ionized or distilled water. Mix the solution thoroughly.
5.2.3.1.2.
Pipette 5 mL of the Nitrate stock solution into a measuring flask and fill to 100
mL with de-ionized or distilled water. Mix the solution thoroughly.
5.2.3.1.3.
Pipette 2.5 mL of the Nitrate stock solution into a measuring flask and fill to
100 mL with de-ionized or distilled water. Mix the solution thoroughly.
5.2.3.1.4.
Pipette 1 mL of the Nitrate stock solution into a measuring flask and fill to 100
mL with de-ionized or distilled water. Mix the solution thoroughly.
5.2.3.1.5.
Pipette 5 mL of the Nitrate stock solution into a measuring flask and fill to 1000
mL with de-ionized or distilled water. Mix the solution thoroughly.
5.2.3.1.6.
Pipette 1 mL of the Nitrate stock solution into a measuring flask and fill to 1000
mL with de-ionized or distilled water. Mix the solution thoroughly.
5.2.3.2. Preparation of the Ammonia stock
Exactly weigh 4718 mg of anhydrous Ammonia Sulfate. Quantitatively transfer
it to a measuring flask of 1000 mL using de-ionized or distilled water.
Exactly fill the flask to 1000 mL. Mix (shake) the solution thoroughly.
5.2.3.2.1.
Please follow the same procedure as described for the Nitrate standards using
the Ammonia stock solution. (Paragraph: 5.2.3.1.)
5.2.3.3. Preparation of the Ammonia-Nitrate mix stock
Exactly weigh 3610 mg anhydrous Potassium Nitrate and 2359 mg anhydrous
Ammonia Sulfate. Quantitatively transfer both salts to a measuring flask of
1000 mL using de-ionized or distilled water.
Exactly fill the flask to 1000 mL. Mix (shake) the solution thoroughly.
User Manual 3000 systems V2.0.doc
Page 47 of 169
User Manual
TN-TS 3000
5.2.3.3.1.
Rev. 2.0.2
Please follow the same procedure as described for the Nitrate standards using
the Ammonia-Nitrate mix stock solution. (Paragraph: 5.2.3.1.)
5.2.3.4. Preparation of the Glycine stock
Exactly weigh 5361 mg Glycine. Quantitatively transfer it to a measuring flask
of 1000 mL using de-ionized or distilled water.
Exactly fill the flask to 1000 mL. Mix (shake) the solution thoroughly.
5.2.3.4.1.
Please follow the same procedure as described for the Nitrate standards using
the Glycine stock solution. (Paragraph: 5.2.3.1.)
5.2.4. Furnace tube and permapure connection
Slide the furnace tube into the oven and connect the permapure to the outlet to the
furnace using the outlet glass-connector. Connect all tubing to the permapure as
described in paragraph 4.3
5.2.5. Module connection
Place the introduction module and connect all the tubing. Connect the module with
the clamp to the furnace tube. Install all gas connections (blue at blue and white at
white) and the ID-connector belonging to the module. (refer for detailed info for the
specific modules to 3.5 and 4.2.5
Page 48 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
Page 49 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
The introduction module has to be installed before the five flow meters
are adjusted.
From right to left:
A.
B.
C.
D.
E.
The different settings for water, organic -liquids and -solids are given at
Appendix I.
Note: The number of manual flow meters can differ per system
depending on the configuration.
Page 50 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
The furnace tube, outlet, modules, joints, etc may become very
hot during the operation of the 3000 SYSTEM. Carelessness may
result in burns.
Procedure 2
1. If there are no bubbles visible, a gas leakage has to be fixed. Adjust flows to the
normal levels. (setting according current method)
2. Disconnect the gas stream between furnace output and the permapure
connection.
3. Manually obstruct the gas stream on the outlet of the furnace tube (using a
septum) and observe the flow meters. They should drop approximately 5-10 mm
within 10-15 seconds. (do not block the flows longer than that) Removing the
septum from the output should clearly release pressure from the tube. This
indicates that no gas-flow leakage is present in the connectors, Module, Furnacetube and other joints. The leakage has to be further down the flow path. (leakage
could be found in the septum of the module, any gas connector, glass joints,
loose clamps, mineralized furnace tube, etc.)
4. Connect the permapure dryer again and obstruct the flow, coming from it. The
flow meters should drop approximately 5-10 mm within 10-15 seconds. Removing
the septum from the output should clearly release pressure from the permapure
dryer. This indicates that no gas-flow leakage is present in all connected parts in
User Manual 3000 systems V2.0.doc
Page 51 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
the flow path. The leakage has to be further down the flow path. (leakage could
be found in the gas connector going to the particle filter, the glass joints, due to
dirt on the grind surface, the furnace tube ball-joint, etc.
5. Resolve any other leakage problem found in the flow path and test it.
6. Finally connect a separate piece of tubing to the outlet connection of the particle
filter (see picture chapter 4.5.4 )and run the test from procedure 1 again.
7. The final check will be the number 3-5 step from procedure 1.
Following these steps should clearly lead to the problem and solution in the flow
path.
The next steps will guide you trough a gas leak test:
1. Check all connections and glassware for proper installation.
2. Close the oxygen-supply and adjust the Argon/Helium flow to 5 mm.
3. Connect a piece of tubing to the gas outlet of the 3000 system, or
the outlet of the UV module.
4. Put the outlet of the tubing in a glass beaker with water and observe
if small bubbles appear. (if not than a leakage or blockage is most
likely)
5. Reconnect the UV module (if applicable) and set gas flows to
proper levels again.
6. Cleaning glass connections, replacing septa and maintaining all
connectors in proper condition should prevent most of the leakage
problems.
Page 52 of 169
User Manual
TN-TS 3000
5.3.
Rev. 2.0.2
Furnace tube
In the furnace tube soothing is one of the causes of the memory
effect. Mineralization can also cause the same effect (the tube
sometimes becomes slightly porous).
Soot deposited at the end of the furnace tube is relatively easy to
remove.
1.
Remove the clamp between the tube and the Perma pure.
(end of the tube)
2.
Remove the clamp of the turbo oxygen. (end of the tube)
3.
Remove the clamp which connects the module to the tube
(front of tube) and remove the module.
4.
Remove the latch (stainless steel fork) between the tube
and the module. (front of tube)
5.
Set the furnace temperature to 1000 oC and pull back the
tube halfway (it should be clean in 10 minutes).
The tube could become opaque on the inside and sometimes on
the outside. This is recognized as mineralization of the furnace
tube. In some cases, Thermo Fisher Scientific can remedy this.
Please contact the Thermo Fisher Scientific Service Department
or your local representative for more information.
Page 53 of 169
User Manual
TN-TS 3000
5.3.2.2.
Rev. 2.0.2
SOLIDS glassware
During solids analysis, the boat and/or frit after many analyses
may cause a memory effect. By introducing samples into the
furnace tube too fast, condensation could appear into the sample
introduction section of the solids glassware. If this happens, a
second peak can occur when the hot boat returns from the
furnace. If this is visible, the glassware must be cleaned in an
oven at approximately 500 oC. Please contact the Thermo Fisher
Scientific Service Department for more information.
The effect may be caused by mineralization of either the boat or
the frit, or both. Replacing them may be the only solution. The
service life of the sample crucible and the boat often depends on
the number of runs, the nature and components in the sample.
5.3.3.1.
Solids Module
Replace the septum when necessary but at least every week. If a
new sample boat is used or the boat is dirty, clean this by
introduction into the furnace tube during 4 minutes at 1000 oC.
5.3.3.2.
Liquids Module
Replace the septum when necessary, but at least once every
week. (service lifetime when auto sampler is used is usually
longer)
5.3.3.3.
TN water module
This is a special module and is supplied with additional hardware.
Please refer to the separate TN-water user manual for details.
Page 54 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
In the following window, click the New Queue button and enter a name for
the Queue that has to be created.
Page 55 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
Next, click the Add button. The following window will appear:
Page 56 of 169
User Manual
TN-TS 3000
Number of samples
Rev. 2.0.2
After all parameters have been entered, click the OK button. Above shown
example will generate the following queue:
By clicking the Add button again, the next (set of) sample(s) can be added.
Repeat this action until all desired samples have be added to this queue.
When finished adding samples click the analyze button. A similar window will
appear:
Make sure Analyze Queue is selected
(tagged) in order to analyze the whole queue.
Then click the OK button. The analyses will
start. Note: If no auto sampler is present, a
question will pop up asking the user to
inject/insert the sample.
Page 57 of 169
User Manual
TN-TS 3000
5.3.5.2.
Rev. 2.0.2
Creating a calibration
If in the box calibration line the option new is selected, a new calibration set
will be created. In that case a new name is requested:
In this menu, the new name the calibration order, signal and through zero
has to be selected/entered. The order is in case of a coulometer (TX and TS)
Is used, the order should be Absolute, otherwise in most cases a first order
(linear) is applied. Note: Afterwards the order can always be changed. If the
system has more then one (parallel) detector the desired signal has to be
selected. Through zero is used to force the calibration line through the zero
point (0,0).
Similar to analyzing samples, by clicking the analyze button, the calibration
standards are measured and calculated into a calibration curve.
For more details please refer to the manual provided with the software.
Page 58 of 169
User Manual
TN-TS 3000
5.4.
Rev. 2.0.2
Before actual samples are introduced an overall performance of the 3000 system
must be performed. If these test results are within the specification, samples- and
calibration procedures may be carried out, without further system proofing.
Before actual shipment to the final destination of the system a factory calibration is
carried out. This information is found in the test report, sent along with the system.
In the report test results and calibration data is found.
The data clearly shows the generated area for a specific standard.
This value may be used as an absolute reference for system performance.
By injecting standards with an injection speed of 1L/s, using the appropriate liquids
module manually or with the auto sampler a comparable result should be found.
5.4.1. TN mode test (setting is low range)
A 100 mg N/L standard is injected at 1 L/s. With flow- and temperature settings
according the liquids application for hydrocarbons the integrated area generated for
a 50 l injection volume should be approximately 100.000 mV.
For 100 L it should be 200.000 mV.
Maximum signal level is approximately 2100 mV. Above this level the signal may
appear flat-lined, indicating that the maximum level is reached and the result of the
total integration should be ignored.
Double-checking it with a 50 mg N/L standard should give half the area.
If the above mentioned areas are obtained, the system functions correctly and
calibration and analysis may be carried out. Incorrect areas (reduced with10% or
more) are an indicator of malfunction. In this case gas test 5.2.8 and overall system
check will have to be carried out.
5.4.2. TS-UV mode test (setting is mid-range)
A 50 mg S/L standard is injected at 1 L/s. With flow- and temperature settings
according the liquids application for hydrocarbons the integrated area generated for
a 50 L injection volume should be approximately 100.000 mV.
For 100 L it should be 200.000 mV.
Maximum signal level is approximately 2100 mV. Above this level the signal may
appear flat-lined, indicating that the maximum level is reached and the result of the
total integration should be ignored.
Double-checking it with a 25 mg S/L standard should give half the area.
If the above mentioned areas are obtained, the system functions correctly and
calibration and analysis may be carried out. Incorrect areas (reduced with10% or
more) are an indicator of malfunction. In this case gas test 5.2.9 and overall system
check will have to be carried out.
Page 59 of 169
User Manual
TN-TS 3000
5.5.
Rev. 2.0.2
Setpoint
25C
700C
700C
25C
Page 60 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
6. TN Water
6.1.
Introduction
This manual is an addition to the TN3000 manual and replaces the paragraphs
in this manual concerning the water configurations.
In contradiction to Total Nitrogen analysis in non-aqueous applications,
additional care of the glassware is essential in order to insure a typical life span.
In addition to this special care, some of the parts will have a relatively short life
span. The main problem with aqueous samples is that often salts are present
(i.e. sea water).
O 2/Ar mixture
Injection into boat
Introduction in furnace
Combustion
Cold trap (drying)
Filter
Water + Salts
Detection
Page 61 of 169
User Manual
TN-TS 3000
6.2.
Rev. 2.0.2
Specifications
0.5 .. 200
> 0.5
'Suitable'
Not specified
< 0.45 m
Not specified
0, 10, 20, 40, 60, 80, 100
Not specified
< 0.1%
slope <10%*
5%
min. 95%
Not specified
min. 95%
Not specified
97 ~ 105%
Not specified
Remark
mg/L
ppm
* between 20 ~ 80%
of the working range
175L
100L
50L/min
300mL/min
300mL/min
110mL/min
1000C
1000C
320C
Pos
Boat program
Speed
Delay
(mm) (mm/min)
90
100
170
0
10
1
2
2
(s)
50
100
65
5
Page 62 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
140000
120000
area (mV/s
100000
NH4
80000
NO3
Glycin
60000
y = -16.064x2 + 3083.6x - 538.37
R2 = 0.9996
40000
y = -1.46x2 + 3050x + 228.86
R2 = 0.9999
20000
0
0
10
20
30
40
50
60
conc. (mg/l)
70000
60000
area (mV/s
50000
NH4
40000
NO3
Glycin
30000
20000
y = -4.8538x2 + 3136.6x - 4.5776
R2 = 0.9999
10000
y = -25.542x2 + 2981.6x + 131.84
R2 = 0.9998
0
0
10
15
20
25
30
conc. (mg/l)
6.2.3. Summary/conclusion
The TN-3000 water system with Nickel boat introduction and cold trap works
good within the in NVN-EVN 12260 and DIN 38409 normalization providing
the total Nitrogen concentration is below 25 ppm and the Ammonia-Nitrate
relation is relevant. If this relation is not relevant, concentrations up to 2000
ppm can be measured.
Page 63 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
Range
Injection volume
Typ. Inj. Vol.
Within NVN/DIN
Ammonia
Nitrate
Extended
Ammonia
Nitrate
Glycin
Particles
6.3.
Low
1 ~ 800
200
High
1 ~ 800
200
0.5 ~ 25
0.5 ~ 30
ppm
ppm
0.2 ~ 75
0.2 ~ 40
0.2 ~ 80
< 250
1 ~ 1000
1 ~ 750
1 ~ 1000
< 250
ppm
ppm
ppm
m
L
L
Page 64 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
Injection opening
Quartz holder
Quartz boat
Quartz wool
Magnet
Magnet
Turning the screw clockwise will move the boat more towards the furnace.
Note: Make sure that the boat drive (magnet) is in its home position.
6.3.3. Replacement of the Nickel sample cylinder
The with quartz wool filled Nickel cylinders are a consumable and can be
ordered at you local distributor. Depending on the type of samples, injection
volume and frequency of analyses, the life span will vary significantly. Please
frequently check the integrity of the cylinder and replace it if necessary.
Warning
Salts of Nickel can be toxic. Handle with care.
Page 65 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
Looking closely to the boat, a little fixation point can be seen. Make sure that
the Nickel sample cylinder is locked properly at this point while the injection
opening is pointed up. As shown in the figure above, a little ball of quartz
wool is put into the quartz boot first before inserting the Nickel sample
cylinder. This extra wool is to better fixate the cylinder.
Fixation point
When to replace the Nickel cylinder: During normal use, the cylinder will
remain more or less the same shape. It will, however, become brittle or
porous. Also the color can change to gray and/or green. If the cylinder is
visually damaged (dents or cracks) this might be the result of a bad
alignment of the quartz boat and/or the auto sampler.
6.3.4. NeXYZ auto sampler
Normally, the calibration of the auto sampler is done by a service engineer
from Thermo Fisher Scientific. However, it is advisable to check is the side
outlet of the needle is pointing towards the furnace. In this way, it is ensured
that the sample is distributed evenly through the quartz wool and is
concentrated at the front of the boat. Checking the outlet position of the
needle can best be done when the sampler is running a washing cycle
(waste position).
Depending on the applied method (and syringe size), sample volumes up to
2 mL can be used. However, a typical value is 175 L.
6.3.5. Furnace tube and outlet
The quartz furnace tube is provided with a ceramic inlay. This inlay protects
the furnace tube from salts. An additional advantage is that the inlay has a
much higher heat capacity resulting in less cooling of the furnace when large
quantities of sample are introduced. A disadvantage is that if the furnace tube
has to be removed from the furnace, this has to be done very slowly (approx.
1 cm/min). If the tube has to be cleaned from e.g. parts of a broken quartz
boat, try to use the scraper tool supplied with the system. The best way to
collect the debris and other deposits is to make a little U-shaped boat from a
few layers of Aluminum foil and place this under the inlet of the furnace tube.
With the scraper tool, the fragments can be shoved into the Aluminum foil. If
User Manual 3000 systems V2.0.doc
Page 66 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
some material is stuck between the ceramic inlay and the quartz tube, just
leave it there. This can do no harm to the system. When some quartz
splinters can not be removed with the scraper tool they can also pushed
further into the furnace. Normally this material will not influence the
Scraper tool
measurements.
Is an analyzer is not used for a longer period of time it is common practice to
lower the furnace temperature and reduce the gas flows. In this case, it is
strongly advised not to set the furnace temperature below 750C. The gas
flows can be reduced to approx. 15 mL/min. If the furnace outlet is
disconnected from the cold trap, the flows can even be set to zero.
The outlet (quartz tube) from the furnace can easily be removed by releasing
the clamp and the wedge nut.
Warning
Please be very careful, the part that is normally inside the
furnace is around 1000C.
Let it cool to room temperature in a save place (for example on a metal
plate). If cooled sufficiently it can be washed using tap water.
TN filter
None return tube
Furnace outlettube
The none return tube (or recoil tube) is to prevent water from the cold trap
going back to the furnace in case the gas flows totally stop.
Page 67 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
Warning
This recoil tube is an additional safety device to prevent water
going back to the furnace. However, the used must always
disconnect the cold trap prior to setting the gas flows to zero.
The non return tube must be clean, upright and in the correct direction (gas
must flow from the furnace to the cold trap). If the outlet- or recoil tube is dirty
it can be easily cleaned with tap water. Before rebuilding the system, please
dry these parts for example with compressed air.
Ceramic inlay
Outlet Tube
Dead zone
Page 68 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
Air inlet/
Fill input
Siphon tube
Cooled water
(with Salts an d
soot particles)
Excess water outlet
When the system is running fine and the applied method is sufficiently
optimized, the liquid level in the cold trap should be more or less stable and
small amounts of water will be pushed out. This level can be adjusted by
shifting the siphon tube higher or lower (first loosen the red wedge nut). It
can be necessary to adjust the height after some time, depending on the
pollution of the filter (more pollution, higher pressure, higher siphon tube).
Another point that can be adjusted is the gas inlet
However, normally this inlet has to be installed just above the bottom of the
lower chamber. Make sure, no gas bubbles can escape directly to the
overflow siphon. Place a beaker under the overflow tube.
Page 69 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
resulting in constantly pushing out all the water. In this case an alternative for
the siphon tube is used. This tube has a little valve. During normal operation,
this valve has to be closed. Depending on the number of samples and the
injected volume, the cold trap will slowl fill up. Please frequently check the
level and when necessary shortly open the valve so, the excess of water is
pushed out. Note: The height of this tube does not have to be adjusted like
the siphon tube.
If the tubing (from the furnace outlet to the cold trap and from the cold trap to
the green filter housing) is polluted or wet, disconnect it and wash it with
ample water. Dry it with compressed air.
Depending on the type of samples, the special paper filter in the green filter
housing can be polluted with salts or other deposits. If so, replace the filter
according to the instructions in de TN3000 manual supplied with the system.
Warning
The deposits on the filter may be toxic.
Page 70 of 169
User Manual
TN-TS 3000
6.4.
6.5.
Rev. 2.0.2
Frequent maintenance
Daily:
Check if the boat and Nickel cylinder is still intact and properly outlined. If not,
or in case of any doubt replace it with a new one and clean the furnace tube.
Check the liquid level and temperature (is it cold) of the cold trap. When
necessary add or drain water. If the cold trap should be totally empty, also
add a few drops of a strong acid and check during the first few
measurements if the cold trap is not emptied too fast. If this is the case,
adjust the height of the siphon/overflow tube.
If present, empty the beaker under the overflow tube.
Add extra water if the level is too low (less then half the lower chamber).
Note: Acidification will not be necessary.
Weekly:
Clean the cold trap by rinsing it with ample water. Next, fill it to approx. 1 cm
below the upper chamber with water and a few drops of concentrated acid
like sulfuric or phosphoric acid.
Page 71 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
Check and if necessary replace the filter in the green filter holder next to the
furnace outlet.
Clean the outlet tube and the tubing connected of the furnace.
Check, and if necessary replace the blue septum in the injection port
(Aluminum funnel on top of a red screw).
6.6.
Trouble shooting
Problem: The cold-trap empties when a sample is introduced
Solutions: Increase the static height of the exit tube on the cold trap
Decrease the speed of the boat for entering and/or exiting the
furnace
Decrease the injection speed of the sample in the boat
Decrease the sample volume
Another possible reason for this problem can be that the sample is not
injected into the boat but into the introduction module. This can be caused by
wrong calibration of the boat and/or needle or when the boat is damaged.
Problem: The boat is not moving anymore, but the boat drive is.
Solutions: Check if the boat is still undamaged. If not, replace it.
If the boat is not damaged, clean the outside of the boat and the
inside of the introduction module with water. Beware that the
quartz wool does not get too wet. Make sure to dry the parts
carefully.
Check for blockage inside the furnace tube. Clean if necessary.
Note: Do not remove the tube from the furnace unless absolutely
necessary. Follow the instructions written above if the tube has to
be removed.
Page 72 of 169
User Manual
TN-TS 3000
Problem:
Solution:
Rev. 2.0.2
Page 73 of 169
Coldtrap
NO Convertor
Ozone Killer
Vacuum pump
Ozone Generator
Argon
Wash solution
Oxygen
6.7.
Temp. Contr.
Capillary
User Manual
TN-TS 3000
Rev. 2.0.2
Page 74 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
7. External samplers
Warning:
Always stop the software (ThEuS or ECS) running before
switching off the sampler. In not doing so, it can happen that
commands are still waiting to be executed while the sampler is
switch on again. This can cause malfunctions like a needle crash.
Page 75 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
ECA1700 autosampler
Page 76 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
Page 77 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
Check if the mounting brackets are already in place. If not position them as explained
in the picture.
Brackets
Brackets
Page 78 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
Replace the normal boat pusher with the extended one. (mounted on the carriage in
the boatdriver, which could be pre-installed)
Extended items
Standard Boat items
Note that the threads of the ECA bracket are pointing outwards!
(viewed from the furnace tube)
Install the ECA-AOX module, connect the clamp, which joints the furnace tube and
the module and insert the oxygen connector.
Check if the glass parts are aligned in the correct manner. (see picture next page)
Page 79 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
ECA fasteners
Rubber sealing
ECA AOX module
Fastener ECA
ECA Carousel
Position the ECA1700 sampler over the 3000 system, align it with the module and
lock the sampler, using the supplied fasteners.
Page 80 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
Warning
Do not temper with- or bypass the safety switch.
Operate the ECA1700 with closed access door only.
Not complying could result in injury.
The column pusher uses excessive force to empty the columns.
Stay away from the pusher during operation and keep the access door
closed!
Page 81 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
Page 82 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
Name
Standby
Evaporation
Combustion
Home
Position Speed
Pause
50 mm 15 mm/s
100 s
90 mm
5 mm/s
60 s
175 mm
5 mm/s
180 s
0 mm 10 mm/s
240 s
Note: The cooling time must be programmed in step 4. This is the Home
position of the boat-program. This step controls the cooling time before the
next sample is introduced.
Not doing so will affect the next result because of too high temperature in the
entrance zone.
Page 83 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
Page 84 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
Figure: ESA2000
7.3.2. ESA-AOX batch method, step by step
Water samples are put in a conical flask and approximately 50 mg of activated
carbon is added. The substance shakes for one hour and is filtrated over the Thermo
Fisher Scientific Frit. The Frit is a sample cup, which has a quartz-sintered filter layer,
capable of the separation between the water phase and the activated carbon. The
prepared Quartz Frits are placed on the carousel and protected by a cover, which
may be purged with Ar or He. The white unused fast connector, found on the 3000
system may be used for this purpose. The purge flow is adjusted with the regular flow
meter.
After a queue is listed and the start button is pressed the arm-hand lifts a Frit or
sample-cup from the carousel and puts it into the ESA module on top of the boat.
The grabber-hand has a neoprene sealing ring, which closes the entry of the module,
creating a gas-tight environment.
The boat, which carries the Frit plus carbon, moves into the high temperature
combustion zone. The content is oxidized completely and a signal appears on the
screen.
After combustion, the boat returns to the injection area and the Frit or sample-cup is
taken out and placed onto the carousel again. A laser beam is used to check if the
sample cups placed in the module are taken out as well. An error message will
appear and prompts the operator to take corrective action. (frit detected yes/no)
The laser control will prevent pile-up and malfunction. In the mean while, the boat is
being cooled as soon as the boat starts to retract. The cooling action is necessary to
lower the temperature of the boat and module, prior to the next sample introduction.
As soon as the curve on the screen reaches the baseline again and maximum
analysis time is reached, the analysis may be terminated and the curve is
automatically integrated and stored. The result appears on the screen and a printout
can be made. In the automatic mode, the next sample is being introduced.
Page 85 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
Page 86 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
Mounting brackets
Docking-station
Fastener
Page 87 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
Check if the mounting bracket for the Docking-station is already in place. If not
position it as showed in the picture.
Verify if the base plate including gas connections and ID connector is repositioned in
a way as the picture below.
Positioning ESA
Page 88 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
Spring
Rear- end support
Boat positioner
ESA Module
ESA position lock
Boat Magnet
Teflon Boat
positioning
Adjustment screws
ESA position lock
Page 89 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
Page 90 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
Center hand/arm
Positioned above the inlet (point 8)
This takes care of the hardware alignment for the 3000 system ESA2000
configuration. Besides this procedure a software calibration must be carried out.
This procedure is explained in the software part of this chapter.
Page 91 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
ESA2000 rear-view
Page 92 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
Warning
Do not temper with- or modify the laser settings or adjustment.
Laser light can be a threat to your eyesight.
Even though the intensity is not of a high level, do not look directly into
the beam.
Operate the ESA2000 with supplied cover only.
Not complying could result in injury.
Readjustments should be carried out by trained Thermo Fisher Scientific
technicians only!
7.3.8. ESA2000: System and software settings
Using the ESA2000 in combination with the 3000 system enables the operator to run
unattended analysis. This chapter briefly describes settings and system features for
automated sample throughput.
With the hardware alignment carried out correctly, the next step, software alignment
must be carried out. This is very important with first time installation or re-calibration,
in case of erratic functioning. The following steps will guide you through the
procedure.
Basic settings for the 3000 system in the ESA2000 mode are similar for the normal
AOX methods.
System flows, temperatures and coulometric settings are the same as for AOX,
according the batch and other manual methods.
However, for solid methods refer to application notes or reports, for correct settings.
Features and Differences for the ESA configuration are:
Page 93 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
Page 94 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
Warning
Prevent the hand from crashing onto the carousel. The alignment or
mechanical features of the stainless steel hand may be lost, because of
mechanical damage.
Page 95 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
7.3.10.
ESA Boat program and related settings
A special boat program is needed for the execution of the AOX batch method.
The following settings will have to be checked and if not present, they have to be
programmed. The Standard method is: ESA AOX or ESA solids.
Depending on the specific application the fan will start cooling at maximum capacity
(100%) as soon as the boat returns. The duration of cooling is approximately 4
minutes. Before the next sample gets introduced, the cooling will have to be shut
down or reduced to 10%. Check if this setting is correct in the Analysis method
window.
Normal cooling is 10% Forced cooling is 100%
For some applications a continuous maximum cooling is standardized.
Typical temperatures are 1000C for both furnace zones, similar to regular TOX/AOX
analysis. Outlet temperature for scrubber heating is 300C
Typical flows for the applications are:
O2 50mm (combustion/manual flow meter) = 330 mL/min
O2 15mm (bypass/manual flow meter) = 45 mL/min
Beside standard methods, customized method can be created and stored.
Name
Standby
Evaporation
Combustion
Home
Position Speed
Pause
0 mm 10 mm/s
0s
70 mm
5 mm/s
60 s
180 mm
5 mm/s
180-240 s
0 mm 10 mm/s
0s
Page 96 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
Name
Standby
Position1
Position2
Position3
Position4
Home
Position Speed
Pause
0 mm 10 mm/s
0s
60 mm
5 mm/s
60 s
75 mm
2 mm/s
60 s
100 mm
2 mm/s
30 s
150 mm
5 mm/s
120 s
0 mm 10 mm/s
0s
For more details, refer to the Software manual or the Thermo Fisher Scientific website: www.thermo.com
Page 97 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
Page 98 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
Page 99 of 169
User Manual
TN-TS 3000
Rev. 2.0.2
Warning
Do not use this introduction module for samples containing significant
quantities of (combustible) organic components, like oil, waxes etc.. The
sample is introduced in a flow of pure oxygen. Any combustible
component will ignite prematurely.
8.3.1.3.
Solids Module
The solids module is used for analysis of Total halogen (TX) or Total sulfur (TS)
content in solid samples. The module is meant for the analysis of halogen and sulfur
compounds in solid samples and liquids containing large molecular compounds with
boiling temperatures above 450C. These are carried into the furnace by a flow of
argon and burned in oxygen.
User Manual
TN-TS 3000
Rev. 2.0.2
User Manual
TN-TS 3000
Rev. 2.0.2
User Manual
TN-TS 3000
Rev. 2.0.2
User Manual
TN-TS 3000
Rev. 2.0.2
n. f 0
n. f
where: Q = the quantity of charge in Coulomb passing through the electrode surface in time t.
m=
mass of converted substance [mol]
F=
Faraday's constant (96487 C/mol)
n=
number of electrons involved in the electrode reaction (here n = 1)
t=
titration time
I=
current (as a function of time)
Integrating the current over time provides the quantity of charge used for titrating the
halide. The quantity of charge, which has been titrated is shown in C in the right
hand column in the measurement display. The quantity of halide present in the cell
can then be calculated from this figure. The calculations are carried out automatically
by the Thermo Fisher Scientific 3000 SYSTEM software.
User Manual
TN-TS 3000
Rev. 2.0.2
Where:
I =
R=
A=
C=
The cathode is contained in a glass tube, and is separated from the measurement solution by
means of a frit. The purpose of this frit is to exclude the effect of disruptive reactions around
this electrode.
0=
Outlet
G=
Gas inlet tube
Acid
The titration cell contains a solution of 75% acetic acid in
water. The concentration of silver ions in solution is
maintained at a constant level of about 10-7 M.
User Manual
TN-TS 3000
Rev. 2.0.2
Where: V
Amp
R
R
I
A
C
= Voltmeter
= Ammeter
= Variable resistance
= Reference electrode
= Indicator electrode
= Anode
= Cathode
User Manual
TN-TS 3000
Rev. 2.0.2
-------- > I2 + 2e
I2 + I- --------- > I3This process will continue until Ei-r no longer changes, i.e. until the concentration of I3has returned to the value it had before the addition of S02. The generator current will
then be equal to zero and all the S02 will have been converted into sulfate.
Here too the difference in potential between anode and cathode of:
Ei-r + Ebias = about 0.5 V
Ebias is in this case equal to + 0.145 V
The quantity of I- converted can be calculated from the charge needed for the
conversion. Then the quantity of S02 present in the cell can be determined according
to Faraday's Law.
The same remarks apply here to the titration curve as were made with respect to
halide analysis.
User Manual
TN-TS 3000
Rev. 2.0.2
Where: I =
R=
A=
C=
G=
Acid
The titration cell contains a solution of 0.1% KI, 0.1% NaN3 and
0.5 % acetic acid in deionized water.
The NaN3 (sodium azide) is added to prevent possible disturbances to the
measurement caused by nitrous oxides forming in the cell.
Warning
Sodium Azide is extremely toxic. Read the instructions of the
chemical safety sheet carefully and handle accordingly!
User Manual
TN-TS 3000
Rev. 2.0.2
Where: V
Amp
R
R
I
A
C
= Voltmeter
= Ammeter
= Variable resistance
= Reference electrode
= Indicator electrode
= Anode
= Cathode
User Manual
TN-TS 3000
Rev. 2.0.2
Acid
The titration cell contains a solution of 0.1% KI, 0.1% NaN3 and
0.5 % acetic acid in deionized water.
The NaN3 (sodium azide) is added to prevent possible disturbances to the
measurement caused by nitrous oxides forming in the cell.
User Manual
TN-TS 3000
Rev. 2.0.2
User Manual
TN-TS 3000
Rev. 2.0.2
9.1.2.2.
POX module
The POX module has to be placed up the boat driver part of the 3000 SYSTEM. The
glass outlet of the module can be connected directly to the furnace tube. Place the
clamps in the right position. If an AOX module is already installed, a special glass
outlet can be used to place on the inlet of the AOX-module.
Connect the gas connectors (O2: Blue on blue, Ar: White on White). Place the clamps
in the right position. Place POX ID-connector.
9.1.2.3. Solids Module
The solids module has to be slide into the furnace tube. Be sure the white Teflon
magnet in the boat module is installed just above the white Teflon boat driver. This is
a magnetic connection. Connect the gas connectors (O2: Blue on blue, Ar: White on
White). Place the clamps in the right position. Place SOL ID-connector.
9.1.2.4. Liquid Module
The liquid module has to be placed in the boat driver part of the 3000 SYSTEM and
slide into the furnace tube. Connect the gas connector (O2: Blue on blue). Place the
clamps in the right position. Place LIQ ID-connector.
9.1.3. Furnace tube
The quartz furnace tube has to be sliced into the furnace compartment with the
narrow end towards the outlet side.
Special Attention
Avoid touching the surface of the furnace tube with your bare fingers. The
traces of grease left by your fingertips will create hotspots and reduce the
service life of the furnace tube.
9.1.4. Connection tube furnace scrubber
The heated connection tube is the connection between the furnace tube outlet and
the sulfuric acid scrubber. Follow the next steps for installing the tube.
The furnace tube and outlet become very hot during the operation
of the 3000 SYSTEM. Carelessness may result in burns.
User Manual
TN-TS 3000
Rev. 2.0.2
4. Connect the inlet of the scrubber to the outlet of the heated connecting tube (balljoint), using clamp no. 12. (D)
5. Insert the connector (electrical) into the socket. (E)
6. Adjust the temperature of the outlet. (typical 300C)
7. Adjust the gasses and fill the scrubber with sulfuric acid.
9.1.6. Sulfuric acid scrubber connected
A
B
C
D
E
9.1.7. NOx-scrubber
Sometimes it is necessary to use a NOx-scrubber. Make sure that a clean and dry
drip tray is placed in the Cell compartment. The NOx-scrubber is connected directly
onto the gas inlet of the titration cell. Follow the next steps for installing the scrubber:
1.
2.
3.
4.
User Manual
TN-TS 3000
Rev. 2.0.2
GAS
INLET
GAS OUTLET
/ INJECTION
SULFUR CELL
GAS
INLET
OUTLET
User Manual
TN-TS 3000
Rev. 2.0.2
G
A
B
F
D
C
Figure: Titration Cell and cooling
1. Insert the connector through the hole of the Titration compartment (5-pole DINconnector (A)
2. Place the Titration Cell on the stirring motor (B)
3. Connect the inlet coming from the scrubber onto the gasinlet (without NOx
scrubber) (E)
User Manual
TN-TS 3000
10.
Rev. 2.0.2
After installation the 3000 SYSTEM is ready for operation. The following paragraphs
should be read carefully, otherwise the measurement is worthless. Please note that
the software manual should be read before switching on the 3000 SYSTEM.
Special Attention
Read the Thermo Fisher Scientific software manual for TOC systems
before operating the 3000 SYSTEM.
10.1. 3000 SYSTEM TX/TS mode Starting up
Before starting up the 3000 SYSTEM several solutions should be prepared. In the
next paragraphs the following subjects will be described:
1. Preparation of reagents
2. Preparation of samples
3. Adjust gas flow
4. Filling the scrubbers
5. Powering the system
6. Gas leakage test
10.1.1.
Preparation of reagents
All necessary solutions needed for a good analysis are described below. For some
specific applications refer to the application notes.
10.1.1.1. Sulfuric acid solution
The Sulfuric acid scrubber needs a solution of 95-98% sulfuric acid (H2SO4). No
further solution or dilutions should be made.
Acids
Read the chemical safety sheet before working with sulfuric acid and
follow the safety instructions.
User Manual
TN-TS 3000
10.1.2.
Rev. 2.0.2
AOX reagents
POX reagents
User Manual
TN-TS 3000
10.1.4.
Rev. 2.0.2
TX/EOX reagents
TS/EOS reagents
User Manual
TN-TS 3000
Rev. 2.0.2
10.1.6.
Preparation of samples
The sample preparation of the most common measurements (AOX, POX, TOX and
EOX) is described in the next paragraphs. All descriptions are following the known
standards.
10.1.6.1. AOX sample preparation
Preparation of AOX samples follows the known standards:
AOX
DIN
ISO
SCAN
EPA
Warning
Do not use this introduction module for samples containing significant
quantities of (combustible) organic components, like oil, waxes etc.. The
sample is introduced in a flow of pure oxygen. Any combustible
component will ignite prematurely.
User Manual
TN-TS 3000
Rev. 2.0.2
AOX sampling
Sampling
Removal of active chlorine
Storage at 4C.
DOC analysis
< 10mg/L
> 10mg/L
Dilute sample
> 1000mg/L
Dilute sample
Choose method
Batch method
Column method
100 ml sample
100 ml sample
pH 2-3
pH 2-3
Washing by 25 ml nitrate
Quartzfrit filtration
Washing by 25 ml water
Press out columns into two crucibles
AOX analysis
AOX analysis
User Manual
TN-TS 3000
Rev. 2.0.2
Storage at 4 degr. C
pH 2-3
POX analysis
POX method
AOX batchmethod
User Manual
TN-TS 3000
Rev. 2.0.2
Soil
Water
Oil
User Manual
TN-TS 3000
Rev. 2.0.2
Store at 4 degr. C
pH = 2
Water layer pH = 9
Extract with 100 ml petroleum ether
Separation of organic phase
Collect extracts
Concentrate to 5 ml by evaporation
Concentrate to 1 ml
EOX analysis
EOX analysis
User Manual
TN-TS 3000
Rev. 2.0.2
10.1.7.
Adjusting gas flows
Before operation gases have to be supplied with a maximum pressure of 3 bar. Open
the gas headers on the gas supply line in the following order.
Close all flow meters by turning the black knob in the clockwise direction. (do not
over- tighten them)
1. Open the gas headers on the gas supply line.
2. Set the oxygen bypass flow meter to 10 mm (35 mL/min) by turning the black
knob counter clockwise. (left flow meter)
The introduction module has to be installed before the next two steps can be
executed.
3. Set the oxygen flow meter to 50 mm (330 mL/min), minimum 40 mm (200
mL/min) (middle flow meter)
4. Set the argon flow meter to 40 mm (200 mL/min), minimum 25 mm (90 mL/min)
(right flow meter)
(Only operating together with the liquids and solids module.)
Note: Instead of manual flow (Rota) meters, digital mass flow controllers can be
installed. In this case, all flow settings will be automatically done by the ThEuS
software.
10.1.8.
Filling the scrubber
Before operation the scrubber has to be filled with sulfuric acid.
10.1.8.1.
Special Attention
Make sure that the drip tray is clean and dry and has been placed in
the scrubber compartment.
Place the small beaker under the scrubber.
Fill the scrubber in the following order:
1. Install the selected sample introduction module connect it and open the gas
flow.
2. Open the scrubber compartment and position the drip-tray.
3. Shut both stopcocks of the scrubber, the red handles in horizontal position
4. Remove upper glass stopper from the scrubber
5. Fill the scrubber buffer with 95-98 % sulfuric acid
6. Remove any spilled sulfuric acid.
7. Replace upper glass stopper.
8. Check that the lower stopcock of the scrubber is shut. Fill the absorber of the
scrubber to the red line by opening the upper stopcock (red handle in vertical
position) and lift up glass stopper until scrubber is filled.
User Manual 3000 systems V2.0.doc
User Manual
TN-TS 3000
Rev. 2.0.2
9. If the gas is connected take care that a flow is running through the scrubber
immediately after filling.
10. Close upper stopcock (red handle in horizontal position)
11. Close the scrubber compartment.
10.1.8.2. NOx-scrubber
Fill the scrubber in the following order:
1. Open the titration cell compartment and place the drip-tray.
2. Disconnect the outlet of the splash trap with the NOx-scrubber
3. Fill the NOx scrubber with 95-98 % sulfuric acid till the mark on the glass.
4. Remove any spilled sulfuric acid.
5. Reconnect the outlet of the splash bulb to the NOx-scrubber, using clamp no. 12.
6. If the gas is connected take care that a flow is running through the scrubber
immediately after filling.
7. Close the compartment.
10.1.9.
Powering the system
If all steps above are carried out carefully and the instrument is connected to a computer
the 3000 SYSTEM can be switched on with the ON/OFF switch on the backside of the
instrument.
1. Switch on the computer
2. Switch on the 3000 SYSTEM.
Now the instrument needs some time to stabilize.
From room temperature up to 1000C for the furnaces, take approximately 30-45
minutes.
A fresh titration cell will take up to 10-15 minutes to generate a proper baseline.
10.1.10.
Installing a selected Module
Place the module on/in the boat driver, located at the right-hand side of the analyzer.
Connect all Argon/Helium and Oxygen inlet tubing, coming from the module (quick
connector) onto the connector socket found on 3000 SYSTEM. Connect the module
with the clamp to the furnace tube and secure it with the screw.
User Manual
TN-TS 3000
Rev. 2.0.2
10.1.11.
Titration cell (chloride)
Make sure the cell (the glass) is clean. Any gray deposit should be removed by filling
the cell with ammonia and leaving it for 15 minutes in a ventilated cabinet, then rinse
thoroughly with water. Pre-rinse the cell with a small quantity of electrolyte in order to
remove any excess water. Fill the cell with electrolyte up to a level between the
marks/level lines. (Never use organic solvents to clean the cell.)
Fill the electrode with the halide electrolyte solution and add the four electrodes like
described in paragraph 8.6.1.1. Fill the cell with the correct electrolyte solution, up to
the level mark. Before and during cell replenishing, the gain must be set to zero in
order to prevent heavy pollution of the cell and/or damage to the coulometer
electronics. Once the cell is filled and the electrodes have been inserted, the cell can
be placed onto the stirrer motor.
If the cell replenishment was carried out correctly, with the bias for the halideanalysis at -315 mV and for the sulfur-analysis at 135-145 mV, a positive signal
should be shown. The current has to have a value between approximately 200 and
600 A.
Depending on the speed of the cell (condition of the electrodes) and gain level, the
signal should return within 3 to 5 minutes. If upon return, the signal at first drops to
negative and then returns to a positive signal to arrive at a base line between
approximately -0.5 to +1 A, you may have a case of overshoot due to the excess
gain.
For the halide-cell approximately 5 L of 0.1 to 0.2 M NaCl has to be injected directly
into the cell before decreasing the gain. While doing this, make sure the needle tip is
fully immersed in the electrolyte in order to obtain a regular signal. This procedure
must be carried out twice. If any overshoot occurs, the gain must be decreased.
After carrying out the procedure of above, the recovery must be tested.
Halide-analysis:
A 2 mM solution of NaCl can be used. Inject 10 L of the solution. In theory, this
should result in a yield of 1.92 mC, but in practice this value could be exceeded with
approximately 10% due to the contribution of light that enters the cell when the cover
is opened, a statically charge coming from the syringe and operator etc.
If the test results are correct, the cell, coulometer and PC have been tested and are
working properly.
If the subsequent connection of the gases results in insufficient yield or
reproducibility, the cell need not be included in any further trouble-shooting
procedures.
User Manual
TN-TS 3000
Rev. 2.0.2
10.1.12.
Titration cell (sulfur)
Make sure the cell (the glass) is clean. Any deposit should be removed by cleaning it
with water and/or a tissue paper. Pre-rinse the cell with a small quantity of the sulfurelectrolyte in order to remove any excess water. Fill the cell with electrolyte up to a
level between the marks/level lines. (Never use organic solvents to clean the cell.)
Add the four electrodes like described in paragraph 8.6.2.1. Fill the cell with the correct
electrolyte solution, up to the level mark. Before and during cell replenishing, the gain
must be set to zero in order to prevent heavy pollution (incorrect titration) of the cell
and/or damage to the coulometer electronics. Once the cell is filled and the
electrodes have been inserted, the cell is placed onto the stirrer motor. Connect the
sulfur cell to the output of the splash bulb with the gasses turned on. Turn the gain
back on. (level set at 10%) If the cell replenishment was carried out correctly, with the
bias for the sulfur-analysis at 135-145 mV, a positive signal should show. If the signal
goes negative, put the gain to zero again and inject a sample/standard first. This
procedure is carried out, using the liquids module and an organic sulfur standard. If
the sample introduction is finished the gain may be turned to the previous level again.
Check if the cell runs positive now. Depending on the speed of the cell (condition of
the electrodes) and gain level, the signal should return within 3 to 5 minutes. If upon
return, the signal at first drops to negative and then returns to a positive signal to
arrive at a base line between approximately -0.5 to +1 A, you may have a case of
overshoot due to the excess gain.
After carrying out the above procedure, the recovery must be tested.
Reproducibility is important at this stage (within 5 %). The yield must be 80 % or
higher.
If the test results are correct, the cell, coulometer and PC have been tested and are
working properly.
If the subsequent connection of the gases results in insufficient yield or
reproducibility, the cell need not be included in any further trouble-shooting
procedures.
User Manual
TN-TS 3000
10.1.13.
Rev. 2.0.2
Procedure 1
For reliable and accurate analysis the 3000 SYSTEM needs to be free of leakage.
Therefore a gas leak test has to be performed.
The next steps explain the gas leak test:
1. Close the flow regulator for the oxygen-supply and lower the Argon-flow to
approximately 5 mm.
2. Observe the flow in the Sulfuric Acid of the scrubber. There still has to be a low
flow visible.
3. Shut down the stirrer of the Titration Cell and observe if a similar bubble appears.
This demonstrates that even at low flow-rates the gas arrives into the Cell and at
the same time proves that all other connected items are gas-tight.
The furnace tube, outlet, modules, joints, etc may become very
hot during the operation of the 3000 SYSTEM. Carelessness may
result in burns.
Procedure 2
1. If there are no bubbles visible, a gas leakage has to be fixed. Adjust flows to the
normal levels. (setting according current method)
2. Disconnect the gas stream between furnace output and the connection furnace
scrubber.
3. Manually obstruct the gas stream on the outlet (using a septum) and observe the
flow meters. They should drop approximately 5-10 mm within 10-15 seconds.
Removing the septum from the output should clearly release pressure from the
tube. This indicates that no gas-flow leakage is present in the connectors,
Module, Furnace-tube and other joints. The leakage has to be further down the
flow path. (leakage could be found in the septum of the module, any gas
connector, glass joints, loose clamps, mineralized furnace tube, etc.)
User Manual
TN-TS 3000
Rev. 2.0.2
4. Connect the connection furnace scrubber and scrubber again and obstruct the
flow, coming from the scrubber. The flow meters should drop approximately 5-10
mm within 10-15 seconds. Removing the septum from the output should clearly
release pressure from the scrubber. This indicates that no gas-flow leakage is
present in all connected parts in the flow path. The leakage has to be further
down the flow path. (leakage could be found in the gas connector going to the
scrubber, the glass joints, due to dirt on the grind surface, the furnace tube,
connection furnace scrubber, scrubber-inlet, -outlet etc.
5. Install the splash bulb again including the tubing and repeat the obstruct
procedure.
6. The final check will be the number 3 step from procedure 1.
Following these steps should clearly lead to the problem and solution in the flow
path.
User Manual
TN-TS 3000
Rev. 2.0.2
10.2.1.
Visible inspection of glassware
All glassware parts should be checked regularly, once a week, on scratches,
disposals and blocking of the gas path. After the inspection a gas leak test should be
performed. (refer to 10.1.13 for gas leakage test)
10.2.2.
Glassware maintenance
10.2.2.1. Scrubber
If the capillary in the scrubber (final gas inlet into the sulfuric acid) appears black, this
may cause blockage or serious restriction to the flow. In addition, the "soothing" may
cause memory effects to occur. Therefore, a clean scrubber is necessary.
Take the necessary precautions to avoid contact with sulfuric acid.
Ware protective gloves, goggles and clothing, according safety
procedures on the laboratory.
Failure to do so may result in physical injury.
Cleaning procedure:
1.
Remove all H2SO4 from the scrubber.
2.
Remove the drip tray from the system.
3.
Disconnect the connecting plug to the scrubber.
4.
Remove the bypass gas connection from the glassware.
5.
Remove the scrubber from the system and remove all stop cocks.
6.
Rinse off as much of the pollution as possible (taking care not to damage the
heater ribbon).
7.
Rinse out the scrubber with water.
8.
Heat the scrubber in an oven at 500 oC for approx. 30 minutes (leaving the
plastic connection plug to protrude through the oven door!).
9.
After re-installation, make sure the heater ribbon reaches the set temperature
again (300C) and carry out the gas test.
User Manual
TN-TS 3000
Rev. 2.0.2
User Manual
TN-TS 3000
Rev. 2.0.2
Introduction module
User Manual
TN-TS 3000
Rev. 2.0.2
10.2.4.
Standard setpoints
The software controls most of the setpoints. These parameters are related to a
method. These methods describe all parameters necessary for running some
applications.
Setpoint
700C
700C
25C
User Manual
TN-TS 3000
Rev. 2.0.2
User Manual
TN-TS 3000
11.
Rev. 2.0.2
This chapter gives a brief description of the actual procedure for analysis.
Basically there are two possibilities for running samples: Manually or automatically.
Once the unit is switched on and all setting like temperature, flows etc have reached
their desired levels, the actual analysis may be started.
11.1. Manual analysis in general
An analysis is considered a manual analysis when the sample is introduced in a
one at the time sequence. This means:
1.
2.
3.
4.
5.
6.
7.
8.
Some system configuration could come without a boat driver. This device is
responsible for the actual movement of the sample boat and automatic plunger
pushing for syringe injection (controlled by stepper motor and software).
In case of not having a boat driver, the sample boat and plunger from the syringe
are controlled by hand.
11.2. Manual analysis using specific modules/methods
User Manual
TN-TS 3000
Rev. 2.0.2
The following steps should take you quickly through the procedure and run an actual
sample.
1. Open a new queue list and key-in the necessary parameters (for more details,
refer to the software manual)
2. Open analysis in the controller window and select the box methods. Choose
the appropriate POX analysis method according the application.
3. Open evaluation and select the absolute calculation method (the calibration
field at this point is not used)
4. Place the sample in the POX module (for sample prep refer to: 10.1.6.2) and
allow the first sample to heat up to approximately 60C, which usually takes
about 8 minutes. In the mean while the second sample is placed to avoid waiting
time for the next analysis.
5. Lower the injection head of the POX module and observe if both needles have
penetrated the septum sufficiently.
6. Select or add in the queue list the sample to be analyzed and press analyze.
Depending on program settings the analysis terminates when sample is
completely purged and the baseline reaches its normal baseline level again.
Manual termination is possible by keying in a lower number of minutes/seconds
analysis time or putting the cursor at the finishing baseline and click on the right
mouse key. This will automatically key in the selected time.
7. The next sample should have reached operational temperature and is ready for
analysis. Select the sample to be analyzed and repeat the steps starting from 5.
11.2.1.2. Manual introduction AOX
The AOX module is positioned in the boat driver and connected onto the furnace
tube of the 3000 SYSTEM system.
The AOX module connector should be inserted into the ID-connector. Closing the
software program (controller window) and starting it again initiates the AOX module
settings. The AOX temperature settings should be visible on the screen. Check all
system parameters like gas flow (see chapter 10.1.13), temperatures, program
settings, method selection, detection cell performance (see chapter 10.1.11) etc.
Warning
Do not use this introduction module for samples containing significant
quantities of (combustible) organic components, like oil, waxes etc.. The
sample is introduced in a flow of pure oxygen. Any combustible
component will ignite prematurely.
The following steps should take you quickly through the procedure and run an actual
sample.
1. Open a new queue list and key-in the necessary parameters (for more details,
refer to the software manual)
2. Open analysis in the controller window and select the box methods. Choose
the appropriate AOX analysis method (batch or column) according the application.
(for more details see chapter 10.1.6.1)
User Manual 3000 systems V2.0.doc
User Manual
TN-TS 3000
Rev. 2.0.2
3. Open evaluation and select the absolute calculation method (the calibration
field at this point is not used)
4. Place the prepared carbon-sample in the AOX module.
5. Select or add in the queue list the sample to be analyzed and press analyze.
Depending on program settings the analysis terminates when sample is
completely oxidized and the baseline reaches its starting point again. Manual
termination is possible by keying in a lower number of minutes/seconds analysis
time or putting the cursor at the finishing baseline and click on the right mouse
key. This will automatically key in the selected time. Note that a certain cooling
time is needed for the sample boat to reach an acceptable temperature again. A
hot boat could oxidize the sample in an early stage, producing erratic numbers.
(typical cooling time is 4 minutes)
6. Now the 3000 SYSTEM is ready for the next analysis. Select the sample to be
analyzed and repeat the mentioned steps starting from 4.
11.2.1.3. Manual introduction Solids, water and heavy hydrocarbons
The Solids module is positioned in the boat driver and connected onto the furnace
tube of the 3000 SYSTEM.
The Solids module connector should be inserted into the ID-connector. Closing the
software program (controller window) and starting it again initiates the Solids module
settings. The Solids temperature settings should be visible on the screen. Check all
system parameters like gas flow (see chapter10.1.13), temperatures, program
settings, method selection, detection cell performance (see chapter10.1.11) etc.
The following steps should take you quickly through the procedure and run an actual
sample.
1. Open a new queue list and key-in the necessary parameters (for more details,
refer to the software manual)
2. Open analysis in the controller window and select the box methods. Choose
the appropriate Solids analysis method according the application. (for more
details check your application note or check the web: www.thermo.com )
3. Open evaluation and select the absolute calculation method (the calibration
field at this point is not used)
4. Place the sample in the Solids module. (by weight in a sample cup or via syringe
by volume injection in a sample cup)
5. Select or add in the queue list the sample to be analyzed and press analyze.
Depending on program settings the analysis terminates when sample is
completely oxidized and the baseline reaches its starting point again. Manual
termination is possible by keying in a lower number of minutes/seconds analysis
time or putting the cursor at the finishing baseline and click on the right mouse
key. This will automatically key in the selected time. Note that a certain cooling
time is needed for the sample boat to reach an acceptable temperature again. A
hot boat could oxidize the sample in an early stage, producing erratic numbers.
(typical cooling time is 4 minutes)
6. Now the 3000 SYSTEM is ready for the next analysis. Select the sample to be
analyzed and repeat the mentioned steps starting from 5.
User Manual
TN-TS 3000
Rev. 2.0.2
1. Open a new queue list and key-in the necessary parameters (for more details,
refer to the software manual)
2. Open analysis in the controller window and select the box methods. Choose
the appropriate EOX/TX analysis method according the application. (for more
details see chapter10.1.6.4)
3. Open evaluation and select the absolute calculation method (the calibration
field at this point is not used)
4. Take a 100L syringe and fill it with the prepared EOX or TX (light hydrocarbon)
sample.
5. Select or add in the queue list the sample to be analyzed and press analyze.
6. Insert the needle through the septum and let the syringe rest on the support. The
plunger pusher in the boat driver performs the injection itself. Injection speed
and volume are software controlled and application dependable.
7. The analysis terminates when sample is completely oxidized and the baseline
reaches its starting point again. Manual termination is possible by keying in a
lower number of minutes/seconds analysis time or putting the cursor at the
finishing baseline and click on the right mouse key. This will automatically key in
the selected time. Now the 3000 SYSTEM is ready for the next analysis. Select
the sample to be analyzed and repeat the mentioned steps starting from 4.
11.3. Automatic analysis in general
An analysis is considered automatic analysis once samples are unattended
introduced into a sample introduction module by means of an autosampler and the
sequence runs all samples according the queue list. In order to prepare the 3000
SYSTEM plus autosampler for actual analysis, a few parameters should be checked.
1.
2.
3.
4.
User Manual
TN-TS 3000
Rev. 2.0.2
7. the unit waits until the curve has returned to baseline and terminates the analysis
as soon as the maximum time has elapsed or the appropriate baseline level is
reached. (depending on software settings)
8. the calculated result appears on the screen and the sampler starts the next
sample injection/introduction.
11.4. Automatic analysis using specific modules/methods
User Manual
TN-TS 3000
12.
Rev. 2.0.2
Malfunction
The response is too slow or
Recovery is too low or too high
Possible cause
Perma pure is blocked
Perma pure is melted
Soothing in the perma pure
Vacuum pump is out of order
(drying of the gasses)
Gas leakage
Wrong calibration line
Incorrect baseline
Action
Replace the perma pure
Replace the perma pure
Clean it or replace it by a new
perma pure
Contact the Thermo Fisher
Scientific Service Department
Check the apparatus
Analyze a new calibration set
or choose the right one
Replace the needle
Replace for proper one
Replace or clean the Filter
Check the oven temperature
Check the solvent, if
necessary clean by distillation.
Replace or clean filter
Correct for needle content
Software Error
User Manual
TN-TS 3000
Malfunction
Generally too high baseline
no signal
Possible cause
Rev. 2.0.2
Action
Gas problems
User Manual
TN-TS 3000
13.
Rev. 2.0.2
No cell current.
Possible cause
Gain control on zero.
Cathode or anode disconnected.
Action
Dirty cell.
User Manual
TN-TS 3000
Malfunction
Possible cause
Rev. 2.0.2
Action
User Manual
TN-TS 3000
Malfunction
Possible cause
Rev. 2.0.2
Action
Gas leaks
User Manual
TN-TS 3000
Malfunction
Irregular or repeating spikes
Possible cause
Air bubbles in the injection
syringe (EOX, EOS)
Condense in the splash bulb
(HCl absorption)
Rev. 2.0.2
Action
Clean the syringe and check if
there still is enough wash
solution available
Dry the splash bulb and check
the O2 and Ar/He flows
Increase the temperature to
normal levels.
Contact the Thermo Fisher
Scientific Service Department
Check the possible causes
Cell problems
Gas problems
In correct baseline
User Manual
TN-TS 3000
14.
Rev. 2.0.2
PANAL0125
PANAL0174
CONSUMABLES TS 3000
Glass fiber filters, 10 pcs
Septum, diam. 12mm, 10 pieces
Quartz sample boat, solids
Set of Standards; 0, 1, 5, 10 mg S/L di-n-butyl sulfide in
toluene dibenzothiophene, 1 mg S/L
Combustion tube universal model 3000
Ceramic needle, 150 mm
PGENE0031
PGENE0032
TN3000022
PGENE0052
PANAL0025
PINJE0012
PANAL0211*
CONSUMABLES TN 3000
PANAL0161 Paper filters 5m, 10 pcs
PGENE0029 Catalyst Pt on ceramic base, 100 gr
PANAL0025 Septum, diam. 12mm, 10 pieces
PANAL0167* Ammoniumsulphate, 50 gr
PANAL0168* Potassiumnitrate, 50 gr
PANAL0126
MODUL0004
PGENE0039
PGENE0038
User Manual
TN-TS 3000
Rev. 2.0.2
PANAL0021
ECS300006
ECS200006
ECS300009
ECS300010
PANAL0046
PANAL0047
PANAL0049
PANAL0050
PANAL0051
PANAL0052
PANAL0072
PANAL0073
PANAL0074
PANAL0075
PANAL0076
PANAL0092
PANAL0038
PINJE0012
User Manual
TN-TS 3000
PANAL0094*
PPTRE0047
PPTRE0049
PPTRE0058
PANAL0094*
PGLAS0032
PPTRE0012
PPTRE0022
Rev. 2.0.2
CONSUMABLES EOX
PANAL0025 Septum, diam. 12mm, 10 pieces
PANAL0095* Standard Aldrin in water, 0 and 5 mg CI/L 10 x 2 mL
PANAL0097* Blank to standard aldrin, 5 x 2 mL
PGENE0002 Syringe 100 L, 71 mm needle, p.s. 5
PGENE0004 Injection needle Hamilton, 71mm, p.s. 5, 3 pcs
CONSUMABLES POX
PINJE0003
POX samplebottle 100 mL complete
PINJE0002
Septum, 24mm, 10 pieces
PANAL0102* Standard DiChloroMethane 10 mg Cl/L; 10 mL
ELS200003
ELS200016
ELS200042
ELS300005
ELS300006
ELS300003
ELS300004
ELS300007
ELS200015
ELS200032
User Manual
TN-TS 3000
Rev. 2.0.2
EGM170007
EGM170016
EGM170008
EGM170014
MODUL0011
PGLAS0602
PPTRE0047
TN3000-065
TN3000-068
TN3000-063
TN3000-066
TN3000-064
TN3000-075
PMECH-0007
TN3000-061
TN3000-067
TN3000-062
ELS2100-12
PANAL 0025
MODUL 0006
ELS215011
PMECH-0008
PMECH-0009
MODUL-0009
ESA200029
ESA200030
10
10
60/10
60/10
65
50/65
100
100
1)
2)
Tips:
850/700
900/700
1000/700
900/700
-----------------
60/10
60/10
50
50
40
30
30
mm
Oxygen
40
mm
Oxygen
40/50
40/50
10/15
05
120
120
65.0
55.0
15
15
20
20
30
30
20
20
The temperature for the solids method can be higher, but that depends of the sort of sample you want to measure.
When you use a 75 mm needle (100 l) the next value can be used for the injection speed
0.1 mm/sec = 0.167 l/sec
100
100
10
10
Sol-Petro
Sol-Water
sort
Method
Liq-Petro
Liq-Water
110
110
0.6
1.2
190
240
15.
sort
Method
User Manual
TN-TS 3000
Rev. 2.0.2
Appendix I : Settings
User Manual
TN-TS 3000
16.
Appendix II
Rev. 2.0.2
TOLUENE
CAS # 108-88-3
RTECS # XS5250000
ICSC # 0078
UN # 1294
EC # 601-021-00-3
TOLUENE
Methylbenzene
Toluol
C6H5CH3/C7H8
Molecular mass: 92.1
TYPES OF
ACUTE HAZARDS/
HAZARD/
SYMPTOMS
EXPOSURE
FIRE
Highly flammable.
Vapour/air mixtures are
explosive.
EXPLOSION
EXPOSURE
INHALATION
Dizziness. Drowsiness.
Headache. Nausea.
Unconsciousness.
Dry skin. Redness.
SKIN
Redness. Pain.
EYES
INGESTION
SPILLAGE DISPOSAL
PREVENTION
STORAGE
ICSC: 0078
FIRST AID/
FIRE FIGHTING
Prepared in the context of co-operation between the International Program on Chemical Safety &
the Commission of the European Communities IPCS CEC 1993
User Manual
TN-TS 3000
Rev. 2.0.2
D
A
T
A
PHYSICAL
PROPERTIES
ICSC: 0078
PHYSICAL STATE; APPEARANCE:ROUTES OF EXPOSURE:
COLOURLESS LIQUID , WITH
The substance can be absorbed into
CHARACTERISTIC ODOUR.
the body by inhalation, through the
skin and by ingestion.
PHYSICAL DANGERS:
The vapour is heavier than air and INHALATION RISK:
may travel along the ground; distant A harmful contamination of the air can
ignition possible. As a result of flow, be reached rather quickly on
agitation, etc., electrostatic charges evaporation of this substance at
aregenerated.
20C.
CHEMICAL DANGERS:
EFFECTS OF SHORT-TERM
Reacts violently with strong oxidants EXPOSURE:
causing fire and explosion hazard. The substance irritates the eyes and
the respiratory tract. Exposure could
cause central nervous system
OCCUPATIONAL EXPOSURE
depression. Exposure at high levels
LIMITS (OELs):
TLV: 50 ppm; 188 mg/m3 (as TWA) may result in cardiac dysrhythmia,
unconsciousness and death.
(skin) (ACGIH 1993-1994).
EFFECTS OF LONG-TERM OR
REPEATED EXPOSURE:
Repeated or prolonged contact with
skin may cause dermatitis. The
substance may have effects on the
central nervous system , resulting in
decreased learning ability and
psychological disorders. Animal tests
show that this substance possibly
causes toxic effects upon human
reproduction.
Boiling point: 111C
Relative density of the vapour/airMelting point: -95C
mixture at 20C (air = 1): 1.06
Relative density (water = 1): 0.87
Flash point: 4C c.c.C
Solubility in water: SO2ne
Auto-ignition temperature: 480C
Vapour pressure, kPa at 20C: 2.9 Explosive limits, vol% in air: 1.1-7.1
Relative vapour density (air = 1): 3.2 OctaSO2l/water partition coefficient
as log Pow: 2.69
ENVIRONMENTAL
DATA
NOTES
Depending on the degree of exposure, periodic medical examination is indicated.
Transport Emergency Card: TEC (R)-31
NFPA Code: H 2; F 3; R 0;
Neither the CEC or the IPCS nor any person acting on behalf of the CEC or the IPCS is
IMPORTAN responsible for the use which might be made of this information. This card contains the
T LEGAL collective views of the IPCS Peer Review Committee and may not reflect in all cases all the
NOTICE: detailed requirements included in national legislation on the subject. The user should verify
compliance of the cards with the relevant legislation in the country of use.
User Manual
TN-TS 3000
Rev. 2.0.2
ARGON
ARGON
(liquefied, cooled)
Ar
Atomic mass: 39.95
CAS # 7440-37-1
RTECS # CF2300000
ICSC # 0154
UN # 1951
TYPES OF
ACUTE HAZARDS/
HAZARD/
PREVENTION
SYMPTOMS
EXPOSURE
not combustible. Heating will
cause rise in pressure with
FIRE
risk of bursting.
FIRST AID/
FIRE FIGHTING
For cylinders, see notes. In
case of fire in the
surroundings: all
extinguishing agents allowed.
EXPLOSION
EXPOSURE
INHALATION
SKIN
Asphyxia. Dizziness.
Unconsciousness.
Ventilation.
ON CONTACT WITH
LIQUID: FROSTBITE.
Cold-insulating gloves.
Protective clothing.
INGESTION
SPILLAGE DISPOSAL
STORAGE
PACKAGING & LABELLING
Ventilation. NEVER direct water jet Store outside or in a separate wellon liquid (extra personal
ventilated building. Cool.
UN Hazard Class: 2.2
protection: self-contained
breathing apparatus).
SEE IMPORTANT INFORMATION ON BACK
Prepared in the context of co-operation between the International
Programme on Chemical Safety & the Commission of the European
ICSC: 0154
Communities IPCS CEC 1993
User Manual
TN-TS 3000
Rev. 2.0.2
ARGON
I
M
P
O
INHALATION RISK:
On loss of containment this gas can
cause suffocation by lowering the
oxygen content of the air in confined
areas.
CHEMICAL DANGERS:
T
A
N
OCCUPATIONAL EXPOSURE
LIMITS (OELs):
TLV not established.
EFFECTS OF SHORT-TERM
EXPOSURE:
The liquid may cause frostbite.
EFFECTS OF LONG-TERM OR
REPEATED EXPOSURE:
D
A
T
A
PHYSICAL
PROPERTIES
ENVIRONMENTAL DATA
NOTES
UN number 1006 for argon,
compressed. In case of fire:
keep cylinder cool by
spraying with water. High
concentrations in the air
cause a deficiency of oxygen
with the risk of
unconsciousness or death.
Transport Emergency Card:
TEC (R)-17
Neither the CEC or the IPCS nor any person acting on behalf of the CEC or the IPCS is
IMPORTANT responsible for the use which might be made of this information. This card contains the
collective views of the IPCS Peer Review Committee and may not reflect in all cases all the
LEGAL
detailed requirements included in national legislation on the subject. The user should verify
NOTICE:
compliance of the cards with the relevant legislation in the country of use.
User Manual
TN-TS 3000
Rev. 2.0.2
OXYGEN
OXYGEN
Oxygen, compressed
(cylinder)
O2
Molecular mass: 32.0
CAS # 7782-44-7
RTECS # RS2060000
ICSC # 0138
UN # 1072
EC # 008-001-00-8
TYPES OF
HAZARD/
EXPOSURE
FIRE
EXPLOSION
ACUTE HAZARDS/
SYMPTOMS
PREVENTION
FIRST AID/
FIRE FIGHTING
EXPOSURE
INHALATION
SKIN
Redness.
Safety goggles.
EYES
INGESTION
SPILLAGE DISPOSAL
STORAGE
Evacuate danger area! Consult an Fireproof. Separated from
expert! Ventilation.
combustible and reducing
substances. Cool.
User Manual
TN-TS 3000
Rev. 2.0.2
OXYGEN
I
M
P
O
R
T
A
N
T
D
A
T
A
OCCUPATIONAL EXPOSURE
LIMITS (OELs):
TLV not established.
EFFECTS OF LONG-TERM OR
REPEATED EXPOSURE:
Lungs may be affected by inhalation
of high concentrations. Symptoms
may be delayed.
PHYSICAL
PROPERTIES
ENVIRONMENTAL
DATA
NOTES
Do NOT use in the vicinity of
a fire or a hot surface, or
during welding. Also consult
ICSC # 0880.
Transport Emergency Card:
TEC (R)-842
Neither the CEC or the IPCS SO2r any person acting on behalf of the CEC or the IPCS is
IMPORTAN responsible for the use which might be made of this information. This card contains the
T LEGAL collective views of the IPCS Peer Review Committee and may not reflect in all cases all the
NOTICE: detailed requirements included in national legislation on the subject. The user should verify
compliance of the cards with the relevant legislation in the country of use.
User Manual
TN-TS 3000
Rev. 2.0.2
SODIUM AZIDE
CAS # 26628-22-8
RTECS # VY8050000
ICSC # 0950
UN # 1687
EC # 011-004-00-7
TYPES OF
ACUTE HAZARDS/
HAZARD/
SYMPTOMS
EXPOSURE
Decomposes on heating.
FIRE
EXPLOSION
PREVENTION
FIRST AID/
FIRE FIGHTING
EXPOSURE
INHALATION
SODIUM AZIDE
Azide
Azium
NaN3
Molecular mass: 65.02
Cough. Headache.
Shortness of breath.
Unconsciousness. Nasal
stuffiness. Blurred vision.
Slowing heart beat. Fall in
blood pressure.
MAY BE ABSORBED!
Redness. Blisters.
STRICT HYGIENE!
Local exhaust or breathing
protection.
Remove contaminated
clothes. Rinse skin with
plenty of water or shower.
Redness. Pain.
Safety goggles, or eye
First rinse with plenty of
protection in combination
water for several minutes
with breathing protection.
(remove contact lenses if
EYES
easily possible), then take to
a doctor.
Abdominal pain. Nausea.
Do not eat, drink, or smoke Rinse mouth. Do NOT induce
Sweating (further see
during work.
vomiting. Give plenty of
INGESTION
Inhalation).
water to drink. Rest. Refer for
medical attention.
SPILLAGE DISPOSAL
STORAGE
PACKAGING & LABELLING
Evacuate danger area! Consult an expert! Fireproof. Separated from Do not transport with food and
Sweep spilled substance into plastic
acids, food and feedstuffs, feedstuffs.
containers; if appropriate, moisten first to
metals, especially lead and T+ symbol
prevent dusting. Carefully collect remainder, its compounds.
R: 28-32
then remove to safe place (extra personal
S: (1/2-)28-45
protection: complete protective clothing
UN Hazard Class: 6.1
including self-contained breathing
UN Packing Group: II
apparatus).
SEE IMPORTANT INFORMATION ON BACK
Prepared in the context of cooperation between the International
Programme on Chemical Safety & the Commission of the European
ICSC: 0950
Communities IPCS CEC 1993
SKIN
Protective gloves.
User Manual
TN-TS 3000
Rev. 2.0.2
SODIUM AZIDE
I
M
P
O
R
T
A
N
T
D
A
T
A
PHYSICAL
PROPERTIES
ENVIRONMENTAL
DATA
NOTES
The occupational exposure
limit value should not be
exceeded during any part of
the working exposure. Smite
is a trade name.
Transport Emergency Card:
TEC (R)-61G12b
Neither the CEC or the IPCS nor any person acting on behalf of the CEC or the IPCS is
IMPORTANT responsible for the use which might be made of this information. This card contains the
collective views of the IPCS Peer Review Committee and may not reflect in all cases all the
LEGAL
detailed requirements included in national legislation on the subject. The user should verify
NOTICE:
compliance of the cards with the relevant legislation in the country of use.
User Manual
TN-TS 3000
Rev. 2.0.2
ICSC: 0362
CAS # 7664-93-9
SULFURIC ACID
RTECS # WS5600000
Sulfuric acid 100%
ICSC # 0362
Oil of vitriol
UN # 1830
H2SO4
EC # 016-020-00-8
Molecular mass: 98.1
TYPES OF
ACUTE HAZARDS/
FIRST AID/
HAZARD/
PREVENTION
SYMPTOMS
FIRE FIGHTING
EXPOSURE
Not combustible. Many
NO contact with flammable NO water. In case of fire in
reactions may cause fire or substances. NO contact with the surroundings: powder,
explosion. Gives off irritating combustibles.
AFFF, foam, carbon dioxide.
FIRE
or toxic fumes (or gases) in a
fire.
Risk of fire and explosion on
In case of fire: keep drums,
contact with base(s),
etc., cool by spraying with
combustible substances,
water but NO direct contact
EXPLOSION
oxidants, reducing agents or
with water.
water.
PREVENT GENERATION IN ALL CASES CONSULT A
OF MISTS! AVOID ALL
DOCTOR!
EXPOSURE
CONTACT!
Corrosive. Burning
Ventilation, local exhaust, or Fresh air, rest. Half-upright
sensation. Cough. Laboured breathing protection.
position. Artificial respiration
INHALATION
breathing.
if indicated. Refer for medical
attention.
Corrosive. Redness. Serious Protective gloves. Protective Remove contaminated
skin burns. Pain.
clothing.
clothes. Rinse skin with
SKIN
plenty of water or shower.
Refer for medical attention.
Corrosive. Redness. Pain. Face shield or eye protection First rinse with plenty of
Severe deep burns.
in combination with breathing water for several minutes
protection.
(remove contact lenses if
EYES
easily possible), then take to
a doctor.
Corrosive. Abdominal pain. Do not eat, drink, or smoke Rinse mouth. Do NOT induce
Burning sensation. Collapse. during work.
vomiting. Refer for medical
INGESTION
attention.
SPILLAGE DISPOSAL
STORAGE
PACKAGING & LABELLING
Collect leaking liquid in sealable Separated from combustible and Unbreakable packaging; put
containers. Do NOT absorb in
reducing substances, strong
breakable packaging into closed
saw-dust or other combustible
oxidants, strong bases, other
unbreakable container. Do not
absorbents (extra personal
materials, food and feedstuffs (see transport with food and feedstuffs.
protection: complete protective
Notes). May be stored in stainless C symbol
clothing including self-contained steel containers (see Notes).
R: 35
breathing apparatus).
S: 2-26-30
UN Hazard Class: 8
UN Packing Group: II
Prepared in the context of cooperation between the International Program on Chemical
ICSC: 0362
Safety & the Commission of the European Communities IPCS CEC 1993
User Manual
TN-TS 3000
Rev. 2.0.2
ICSC: 0362
PHYSICAL
PROPERTIES
INHALATION RISK:
Evaporation at 20C is negligible; a
harmful concentration of airborne
particles can, however, be reached
quickly on spraying.
CHEMICAL DANGERS:
The substance is a strong oxidant
and reacts violently with combustible
and reducing materials. The
EFFECTS OF SHORT-TERM
substance is a strong acid, it reacts EXPOSURE:
violently with bases and is corrosive Corrosive. The substance is very
to most common metals forming a
corrosive to the eyes the skin and the
flammable/explosive gas (hydrogen respiratory tract. Corrosive on
see ICSC # 0001). Reacts violently ingestion. Inhalation of an aerosol of
with water and organic materials with this substance may cause lung
evolution of heat (see Notes). Upon oedema (see Notes).
heating, irritating or toxic fumes (or
gases) (sulfur oxides) are formed.
EFFECTS OF LONG-TERM OR
OCCUPATIONAL EXPOSURE
REPEATED EXPOSURE:
LIMITS (OELs):
Lungs may be affected by repeated or
TLV: ppm; 1 mg/m3 (as TWA); 3
prolonged exposure to an aerosol of
mg/m3 (as STEL) (ACGIH 1993this substance. Risk of tooth erosion
1994).
upon repeated or prolonged exposure
PDK: 1 mg/m3 (USSR 1988).
to an aerosol of this substance.
MAK: ppm; 1 mg/m3; respirable
fraction of aerosol (1991).
Boiling point (decomposes): 340C Solubility in water: miscible
Melting point: 10C
Vapour pressure, kPa at 146C: 0.13
Relative density (water = 1): 1.8
Relative vapour density (air = 1): 3.4
This substance may be hazardous to the environment; special attention
should be given to water organisms.
ENVIRONMENTAL
DATA
NOTES
The symptoms of lung oedema often do not become manifest until a few hours have passed and they are
aggravated by physical effort. Rest and medical observation are therefore essential. NEVER pour water
into this substance; when dissolving or diluting always add it slowly to the water. Store in an area having
corrosion resistant concrete floor.
Transport Emergency Card:
TEC (R)-10B
NFPA Code: H 3; F 0; R 2; W
Neither the CEC or the IPCS nor any person acting on behalf of the CEC or the IPCS is
IMPORTANT responsible for the use which might be made of this information. This card contains the
collective views of the IPCS Peer Review Committee and may not reflect in all cases all
LEGAL
the detailed requirements included in national legislation on the subject. The user should
NOTICE:
verify compliance of the cards with the relevant legislation in the country of use.
User Manual
TN-TS 3000
Rev. 2.0.2
ALDRIN
CAS # 309-00-2
RTECS # IO2100000
ICSC # 0774
UN # 2761
EC # 602-048-00-3
TYPES OF
HAZARD/
EXPOSURE
FIRE
EXPLOSION
ALDRIN
HHDN
1,2,3,4,10,10-Hexachloro-1,4,4a,5,8,8a-hexahydro,endo,exo-1,4:5.8dimethanonaphthalene
C12H8Cl6
Molecular mass: 364.9
ACUTE HAZARDS/
SYMPTOMS
Not combustible. Liquid
formulations containing
organic solvents may be
flammable.
Explosion hazard will depend
on the solvent used or on the
characteristics of the dust.
PREVENTION
FIRST AID/
FIRE FIGHTING
In case of fire in the
surroundings: all
extinguishing agents allowed.
PREVENT DISPERSION OF
DUST! STRICT HYGIENE!
EXPOSURE
AVOID EXPOSURE OF
(PREGNANT) WOMEN!
(see Ingestion).
Ventilation (not if powder). Fresh air, rest. Artificial
respiration if indicated. Refer
INHALATION
for medical attention.
MAY BE ABSORBED! See Protective gloves. Protective Remove contaminated
Ingestion.
clothing.
clothes. Rinse and then wash
SKIN
skin with water and soap.
Safety goggles or face
First rinse with plenty of
shield.
water for several minutes
(remove contact lenses if
EYES
easily possible), then take to
a doctor.
Dizziness. Headache.
Do not eat, drink, or smoke Do NOT induce vomiting.
Nausea. Vomiting.
during work.
Rest. Refer for medical
INGESTION
Weakness. Muscle twitching.
attention.
SPILLAGE DISPOSAL
STORAGE
PACKAGING & LABELLING
Sweep spilled substance into
Separated from food and
Do not transport with food and
containers. Carefully collect
feedstuffs. Cool. Dry.
feedstuffs.
remainder, then remove to safe
T symbol
place. Do not let this chemical
R: 24/25-40-48
enter water courses or sewers
S: 22-36/37-44
(extra personal protection:
UN Hazard Class: 6.1
complete protective clothing
Severe marine pollutant.
including self-contained breathing
apparatus).
Prepared in the context of cooperation between the International
Programme on Chemical Safety & the Commission of the European
Communities IPCS CEC 1993
ICSC: 0774
User Manual
TN-TS 3000
Rev. 2.0.2
ALDRIN
PHYSICAL
PROPERTIES
ENVIRONMENTAL
DATA
INHALATION RISK:
Evaporation at 20C is negligible; a
CHEMICAL DANGERS:
harmful concentration of airborne
The substance decomposes on
heating producing toxic and corrosiveparticles can, however, be reached
quickly on spraying.
fumes (chlorine fumes, hydrogen
chloride.) Reacts with acids,
oxidants, active metals, phenols, acidEFFECTS OF SHORT-TERM
catalysts. Can be corrosive due to
EXPOSURE:
the slow evolution of hydrogen
The substance may cause effects on
chloride in storage.
the central nervous system , resulting
in convulsions.
OCCUPATIONAL EXPOSURE
EFFECTS OF LONG-TERM OR
LIMITS (OELs):
TLV : ppm; 0.25 mg/m3 (as TWA)
REPEATED EXPOSURE:
(skin) (ACGIH 1991-1992).
The substance accumulates in the
human body. Aldrin may be present in
human placental tissues and blood.
Boiling point at 0.267 kPa: 145C
Melting point: 104C
Relative density (water = 1): 1.54
NOTES
Other melting points: 40-60C (technical grade). Technical aldrin is a tan to dark brown waxy solid.
Carrier solvents used in commercial formulations may change physical and toxicological properties. Do
NOT take working clothes home. The recommendations on this Card also apply to ICSC # 0787
(dieldrin). Aldrine, Aldrex, Aldrite, Aldrosol, Drinox, Seedrin, Octalene are trade names.
Transport Emergency Card:
TEC (R)-61G53b
NFPA Code: H2; F0; R0;
Neither the CEC or the IPCS nor any person acting on behalf of the CEC or the IPCS is
IMPORTANT responsible for the use which might be made of this information. This card contains the
collective views of the IPCS Peer Review Committee and may not reflect in all cases all
LEGAL
the detailed requirements included in national legislation on the subject. The user should
NOTICE:
verify compliance of the cards with the relevant legislation in the country of use.
User Manual
TN-TS 3000
Rev. 2.0.2
User Manual
TN-TS 3000
Rev. 2.0.2
User Manual
TN-TS 3000
Rev. 2.0.2
User Manual
TN-TS 3000
17.
Rev. 2.0.2
Operating procedure
Starting procedure:
1. Start the PC and run the Thermo Fisher Scientific software.
2. If not correct, set the system parameters (temp. etc)
3. Check if glass parts are clean and properly positioned.
4. Connect Argon (white) and Oxygen (blue) connectors of the introduction module.
5. Open Gas supplies with a pre-pressure of approximately 3 bar for Argon and
Oxygen.
6. Adjust all flows on the analyzer by using the flow-regulators.
7. Check all settings in the Software. E.g. smoothing and delay
8. Wait for the signal to stabilize.
9. System is ready for analyses.
Standby procedure:
1. Remove all liquids (e.g. Sulfuric Acid) if applicable.
2. When using an ELS 3000 take furnace needle out of the introduction module
3. Close Argon and Oxygen supplies.
4. Set furnaces at 700 oC.
5. Shut down the software.
6. System is in standby position.
User Manual
TN-TS 3000
Rev. 2.0.2
0.03
11.8
20.8
37.2
58.2
86.3
119
164
197
258
287
359
374
408
0.69
13.4
34.1
53.0
72.6
100
140
192
238
301
364
427
494
579
For example:
10 mm Oxygen is equal to a (mass) flow of 37.4 mL/min
200 mL/min Argon (massflow) is equal to 40-41 mm on the Rotameter scale
45 mm Helium is equal to 301 mL/min
User Manual
TN-TS 3000
19.
Rev. 2.0.2
Dimensions (W x H x D)
Weight
Input Voltage
Frequency
Fuses
Power
Power/Installation class
230/115 V AC
50/60 Hz
2 x 6.3 A slow at 230 volt nominal
2 x 12 A slow at 115 volt nominal
max. 1250 VA
Class II
Storage temperature
Operating temperature
Humidity
Safety class
Furnace
0 50 C
10 30 C
20 85% (noncondensing)
Class I**
42V; 800W
Connections
User Manual
TN-TS 3000
Rev. 2.0.2
Please visit us at
www.thermo.com