The period of one year following installation (Japan only)
2 .Terms of Warranty
If a fault attributable to Shimadzu Corporation occurs within the warranty
period, we will perform the necessary repairs or part replacement free of
charge.
3 . Items Not Covered
The following faults are not covered by this warranty, even if they occur during
the warranty period.
Afterservice
1)
Faults resulting from incorrect handling
2) Faults resulting from repairs or modifications implemented by parties other
than Shimadzu Corporation or companies designated by Shimadzu Corporation
3) Faults not originating in the equipment itself
4)Faults occurring after use in severe environmental conditions, such as high
temperatures, high humidity levels, corrosive gases, or vibrations
5)Faults resulting from fires or natural disasters, such as earthquakes
6)Faults occurring after the product is moved or transported following initial
installation
7)Faults occurring in consumable parts or parts dependent on them
If any problem occurs with this instrument, inspect it and take appropriate
corrective action as described in the Section "7 Troubleshooting". If the
problem persists, or symptoms not covered in the Troubleshooting section
occur, contact your Shimadzu representative.
iii
Page 5
Safety Instructions
Safety Instructions
・To ensure safe operation of the instrument, read these Safety Instructions carefully before use.
・Observe all of the WARNINGS and CAUTIONS described in this section. They are extremely
important for safety.
・In this manual, warnings and cautions are indicated using the following conventions;
WARNING WARNING Indicates a potentially hazardous situation
which, if not avoided, could result in death or serious injury.
CAUTION Indicates a potentially hazardous situation which, if not
avoided, could result in minor or moderate injury, or property
damage.
NOTES Indicates information that may help increase the operating efficiency or
foster a greater understanding of the product.
■Application Precautions
WARN ING
The TD-20 Thermal Desorption Tube Autosampler system is used to concentrate samples for
GCMS-based qualitative and quantitative analysis. Do not use it for any purpose other than
the one described above.
Supply Periods for Service Parts
We have established a framework for supplying service parts from our Parts Center. The supply
period for a product is specified in the following way.
In principle, the period of 7 years following product discontinuation
Depending on the actions taken by the manufacturer at the time of discontinuation and on
fluctuations in the amount required, it may not be possible to maintain the supply of service
parts until the end of this 7-year period.
iv
Page 6
Installation Site Precautions
■Installation Site Precautions
The TD-20 Thermal Desorption Tube Autosampler system is used to concentrate samples for
GCMS-based qualitative and quantitative analysis.
In order to ensure the safe use of this product, observe the following points.
Safety Precautions
1.Do not use it for any purpose other than the one described above.
2.Follow the procedures described in this instruction manual.
3.Observe precautionary information.
4.Do not disassemble or modify this product.
5.If internal repairs are required, consult your Shimadzu representative.
6.If installation and Transfer are required, consult your Shimadzu representative.
In this instruction manual, precautionary information is labeled as follows.
WARNINGIndicates a potentially hazardous situation which, if not avoided,
could result in death or serious injury.
CAUTION Indicates a potentially hazardous situation which, if not avoided,
could result in minor or moderate injury, or property damage.
NOTE Indicates information that may help increase the operating efficiency
or foster a greater understanding of the product.
v
Page 7
Installation Site Precautions
■Installation Site Precautions
WARNING
・The power supply voltages and power consumptions of this instrument are listed below.
The power supply voltage of the instrument is indicated on the label on the back of the
instrument. Connect the instrument only to a power supply of the voltage indicated;
otherwise, fire or electric shock could result. Check that the power supply voltage is stable and that its
current capacity is sufficient to operate all the components of the system. If not, the instrument will not
operate at its rated performance.
Grounding is necessary to prevent electric shock in the event of an accident or electrical discharge, and
important for ensuring stable operation.
・
Do not place heavy objects on the power cord, and keep any hot items away.
The cord could be damaged, resulting in fire, electrical shock or malfunction. If the cord becomes damaged,
contact your Shimadzu representative immediately.
・
Do not modify the cord in any way. Do not bend it excessively or pull on it.
Frequency
Consumption
The cord could be damaged, resulting in fire, electrical shock or malfunction. If the cord becomes damaged,
contact your Shimadzu representative immediately.
・Do not Installation which the power switch is difficult to operate.
In emergency such as breakdown power source there is a possibility where it cannot operate
when it is necessary TO TURN OFF.
・Solvent which is used with the GCMS being to have the danger of ignition and poisonous,
ventilate the interior..
vi
Page 8
p
Installation Site Precautions
CAUTION
・The weight of this instrument is 43kg.
During installation, consider the entire weight combined with other GC components.
The lab table on which this instrument is installed should be strong enough to support the
total weight of the GC system. It should be level, stable and have depth of at least 600mm.
Otherwise, the instrument could tip over or fall off the table.
・Avoid installation sites that are exposed to corrosive gases or excessive dust.
These adverse conditions may be detrimental to maintaining the instrument performance
and may shorten its service life.
・Open the space above the 200mm, left side of the System.
There is an air intake for trap cooling on the left side of the system. When the space is little,
there is a
ossibility where you cannot show specification cooling ability.
vii
Page 9
A
Installation Site Precautions
■Precautions for Instrument Inspection, Maintenance, Adjustment and Care
WARNING
・Unplug the instrument before inspection, maintenance, or parts replacement.
Otherwise, electrical shock or short-circuit accidents could occur.
・Never remove the main cover.
This may cause injury or malfunction of the instrument. The main cover does not need to be
removed for routine maintenance, inspection and adjustment. Have your Shimadzu
representative perform any repairs requiring removal of the main cover.
・If the power cord plug gets dusty, remove the plug from
the power outlet and wipe away the dust with a dry cloth. If dust is allowed to accumulate, fire
could result.
・Replacement parts must be of the specifications given in "1.4 Component Parts" or "6.6
Maintenance Parts".
Use of any other parts may result in instrument damage and malfunction.
fter wiping off with the soft cloth where cleaning the device outside could soak the little
・
water or the neutral detergent, please wipe off the moisture with the cloth which dries.
・If any water gets onto the instrument, wipe it away immediately to prevent rust. Never use
alcohol or thinner solvents for cleaning the instrument.
They could cause discoloration.
viii
Page 10
Warning Lavels on the Equipment
Warning Lavels on the Equipment
②
①③
①
②
③
Front-Panel Interior Top
WARNING High Voltage
Do not open the case. Doing so may result in electric shock.
CAUTION High Temperture
Do not touch the valve unit, interface, or dryer during, or
immediately after, operation. Doing so may result in burn injury.
CAUTION There is a possibility
Before removing the cover, please turn off power. There is a
possibility of being put to the moving element.
Back
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Page 11
Emargency-Stop Procedure
Emargency-Stop Procedure
Stop operation of the TD-20 in the event of an emergency (e.g., resulting from an error), by
performing the following procedure. Before resuming operation, perform an inspection and, if
necessary, consult Shimadzu service personnel.
Emergency-Stop Procedure
(1) Turn OFF the power switch.
(2) Disconnect the power supply (i.e., remove the power cable).
(3) Turn OFF the carrier-gas supply.
Back
1: ON
0: OFF
(1)
〜: AC
Power Switch (1) and Power Cable (2)
x
(2)
Page 12
Operation Precautions
Operation Precautions
DO NOT select the Direct control menu during analysis. If the Direct control menu is selected, the
sample tube may be broken or damaged. Wait until after the status changes to "Ready" before
using the Direct control menu.
WARNING
Tube Set
Ready
xi
Page 13
f
d
p
Operation Precautions
Operation Precautions
WARNING
DO NOT remove the protection cover during analysis. Removing this cover may
cause an injury and/or equipment failure. Be sure to stop analysis before removing the
rotection cover.
Protection Cover
WARNING
Always wear safety glasses or goggles when handling solvents and the Glass Sample
tube. If solvent or a broken piece of glass gets into the eyes, it may cause blindness. I
solvent gets into the eyes, immediately flush them with large amounts of water an
seek medical attention.
6 Direct Thermal-Desorption Analysis with the TD-20 ..........................................................117
7 Form of Measurements Samples and Setting Method......................................................... 118
8 Consideration of Physiochemical Properties of Target Constituents ..................................119
9 Breakthrough Volumes for TD-20's Second Trap .................................................................120
10 Deciding the Concentration Range for the Target Constituent.........................................121
11 Deciding the Split Ratio.......................................................................................................122
12 Deciding the Temperature for Each Component ................................................................123
13 Service Life of Sample Tube and Secondary Trap ..............................................................123
14 Ghost Peaks .........................................................................................................................124
15 Inspection Methods for Ghost-Peak Sources.........................................................................125
xvi
Page 18
Chapter 1
Overview
This chapter provides information on the characteristics, configuration, and
specifications of the TD-20, points to note regarding unpacking, and descriptions
of accessories.
1.1 Introduction
1
Chapter Contents
This section provides an overview of the TDTS-2010.
1.2 Configuration
This section describes the component configuration for the TD-20.
1.3 Opening the Package
This section specifies points to note when opening the package
1.4 Accessories
This section describes the accessories.
1.5 Installation Conditions and Gas Specifications
This section specifies the main unit's installation environment and
the gases used. In order to ensure safety and proper performance, be
sure to observe the points mentioned in this section.
1.6 Measurement Samples
This section describes the measurement samples.
1.7 Specifications
This section provides specifications for the TDTS-2010.
Page 19
Chapter1 OverView
1.1 Introduction
The TD-20 is used to introduce VOCs (volatile organic compounds) sampled with a sample
tube into a GCMS (gas chromatograph mass spectrometer) using the cold trap/thermal
desorption (TD) method.
With the TD method, a gas is passed through a tube (i.e., the trap tube) that is filled with
an adsorbent material so that VOCs in the gas are adsorbed by the material. The trap tube
is then heated to desorb the VOCs from the material. The trap tube is sometimes cooled in
order to increase the amount of adsorption.
In addition to the analysis of VOCs, the TD method is also used for the analysis of SVOCs
(semi-volatile organic compounds).
The TD-20 uses a thermo-module to cool the trap tube and so a refrigerant, such as liquid
nitrogen, is not required. This means that, in terms of installation conditions and running
costs, the TD-20 is superior to products that use a refrigerant.
The TD-20 can be completely controlled from the PC used to control the GCMS.。
1.2 Configration
Fig. 1.2 shows the configuration of the TD-20, together with the GCMS-QP2010
Fig.1.2 System Overview
2
Page 20
Chapter1 OverView
1.3 Opening the Package
If the product's package has been severely damaged, consult your Shimadzu representative before
opening the package. After opening the package, check that the contents of the package concur with
the content list. (Refer to Table 1.4.) If any contents are missing or damaged, consult your Shimadzu
representative immediately.
1.4 Accessories
No.
品名
P/N
数量
1
SPANNER, ROUND, DOUBLE-ENDED, 6×8
2
SPANNER, ROUND, DOUBLE-ENDED,
3
4
5
6
7
CABLE SET, UC-943-J02
10×12
SPANNER, 6×7
CABLE ASSY, BJ-4511
COLUMN, PACKING, ALUMINUM
PIPE, MF-MF, L-500
071-60816-11 1
086-03003 1
086-03011 2
086-03051 1
225-19051 1
201-35183 1
201-48557-50 2
8
9
10
PIPE, MF-GF, L-500
PIPE, GF-GF, 2×100
FERRULE, GV, 1/8, 2 PCS
3
201-48560-50 1
201-48562-10 1
223-54423-91 1
Page 21
Chapter1 OverView
11
12
13
14
15
16
17
O-RING, REPLACEMENT TOOL
NUT, SSNE, 103408
ALLEN WRENCH, HKS
OPEN-END WRENCH, OEW
TD-20 INSTRUCTION MANUAL
Columun Oven Cover PLATE
START CABLE ASSY
223-54588 1
223-56363 1
223-56396-01 1
223-56396-11 1
223-57451 1
223-57362 1
351-18075-91 1
18
19
20 Sampling Tube TENAX TA 223-57102-91 1
21 SUS Empty Tube 223-57091 1
22
23 Cap 223-54226-91 4
24 3port Pipe MF-MM-MF 201-48386 1
Table 1.4 TD-20 Accessories (PN223-57008-91)
SYSTEM DISK, TDU2
FERRULE, GVF/005
Pipe、SPLIT-MF L-500
351-18090-91 1
670-15003-04 1
223-57421-91 1
4
Page 22
f
Chapter1 OverView
1.5 Installation Conditions and Gas Specifications
1.5.1 Installation Conditions
In order to ensure proper performance, observe the following conditions.
CAUTION
In environments where VOCs are used, in addition to leakage that occurs when the cap for
the sample tube is attached or removed, VOCs are gradually adsorbed by parts making
contact with the gas, such as O-rings, and are detected* in measurement. Ensure that the
installation environment contains no potential sources of constituents that may influence
the target constituent.
*In environments where a 0.1-ppm concentration of toluene is present, approx. 5 ng o
toluene is detected in analysis.
1.5.2 Gas Specifications
In order to ensure proper performance, use gases satisfying the following specifications.
1. Carrier Gas
Gas Helium
Supply pressure 0.5 to 0.9 MPa
Purity 99.9999% min.
2. Purge Gas
Gas Dry air or helium
Supply pressure 0.3 to 0.9 MPa
Purity No dust or moisture
CAUTION
For the carrier gas, use helium gas of at least the purity specified above, including
gas discharged from the plumbing and pressure regulators, and air mixed together
due to leakage. Performance may be adversely affected if the purity is less than the
specified level.
5
Page 23
Chapter1 OverView
1.6 Measurement Samples
The TD-20's measurement sample is a sample tube of length 90 mm and outer diameter 1/4". The
following types of sample tube are available. No sample tube is provided with the TDTS-2010. Obtain
Cooling temperature From 50ºC below room temperature to 0ºC (set in 1ºC units)
From 45ºC below room temp. when Valve Temp.ºover260C
Heating temperature 80ºC to 350ºC (set in 1ºC units)
Heating time 0 to 30 min (set in 0.01-min units)
5. Interface Unit
Maintained temperature 80ºC to 350ºC (set in 1ºC units)
6. Gases
Carrier gas Helium (99.9999% purity) or a similar product, 0.5 to 0.9 MPa
Consumption: 4 L/cycle max.*
Purge gas Air (dehumidified)**, 0.2 to 0.3 MPa
Consumption: 3 L/cycle max.
7
Page 25
* When using a capillary column with a total flow rate not exceeding 100 mL/s.
** When using air for purge gas, trap cooling minimum temperature became higher
than Herium.
7. Entire System
Specified environment Temperature: 18ºC to 28ºC; Humidity: 50% to 70%
Operating environment Temperature: 13ºC to 28ºC; Humidity: 80% max.
Storage environment Temperature: 0ºC to 40ºC
Power supply 100 VAC, 10 A (max.)
Dimensions: 323 (W) × 500 (H) × 500 (D) mm (Not including projections.)
Weight 43 kg
Chapter1 OverView
8
Page 26
Chapter 2
Names and Functions of Parts
This chapter provides the names and explains the functions of the different parts
of the system.
Chapter Contents
2.1 Front
This section describes the parts on the front of the TD-20.。
2
2.2 Right Side
This section describes the parts on the right side of the TD-20.
2.3 Back
This section describes the parts on the back of the TD-20.
2.4 Front-Panel Interior
This section describes the parts inside the front panel of the TD-20
2.5 Top
This section describes the parts on the top of the TD-20
2.6 Floe-Line Configration
This section describes the parts on the top of the TD-20.
2.7 Flow-Line During Pretreatment
This section describes the state of the TD-20's flow line during
pretreatment.
9
Page 27
Chapter2 Names and Functions of Parts
2.1 Front
2
3
5
4
1
1. Front Panel
The front panel can be removed by removing
the front-panel screw and lifting it up to
reveal the transfer line, the valve oven unit,
the cold-trap unit, and the gas-control unit.
2. Desorber Unit
This unit attaches/removes the sample
tube's caps and performs heating. The unit
is covered with a cover, which can be
removed to allow replacement of the seal
block's O-ring.
3. Handling Arm
This arm has a grip function that allows it
to move the sample tube between the tray
and desorber unit. It can perform 360º
rotations, move vertically, or trace the
circumference of a circle.
4. Interface (IF)
This part passes through the capillary
column. It connects the valve oven and the
GC column oven and the tip is attached to
the GC column oven's interior. Its
temperature is maintained by the heater.
5. Power Indicator
This indicator lights green when the power
is turned ON.
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Page 28
Chapter2 Names and Functions of Parts
2.2 Right Side
7
6. Screw
This M4 screw secures the front panel.
7. Intake Inlet and Exhaust Outlet
These holes are for taking in and
discharging the air used to cool the cooler
unit's radiator. (The inlet is at the top and
the outlet is at the bottom.) Placing objects
within 20 cm of the inlet or outlet may
adversely affect the cooling efficiency.
8. Carrier-Gas Pressure-Adjustment Hole
The carrier-gas pressure can be adjusted by
turning the pressure-adjustment knob using
a flat-bladed screwdriver. The pressure is
indicated by the carrier-gas pressure gauge
(28). (Initial value: 100 kPa.)
9. Purge-Gas Pressure-Adjustment Hole
The purge-gas pressure can be adjusted by
turning the pressure-adjustment knob using
a flat-bladed screwdriver. The pressure is
indicated by the carrier-gas pressure gauge
(29). (Initial value: 100 kPa.)
8
6
11
12
9
CAUTION
Except in cases of special
necessity, the initial values for
the flow rate and gas pressure
at locations (8) to (12) can be
used.
13
10. Dryer and Purge-Gas Flow-Rate
Adjustment Hole:Note used.
11. Backflush-Gas Flow-Rate Adjustment
Hole
This needle valve is used to adjust the flow
rate of the backflush gas. "Backflush" refers
to the purging of the carrier gas from the
6-port valve to the transfer line. (Initial
value: 50 mL/min.) The flow rate can be
adjusted by turning the knob with a
flat-bladed screwdriver.
12. Sample-Tube Purge-Flow-Rate
Adjustment Hole
This needle valve is used to adjust the flow
rate of the gas that purges the sample tube.
The flow rate can be adjusted by turning the
knob with a flat-bladed screwdriver. It is
initially set to approx. 60 mL/min.
13. Power Switch
0 = OFF, 1 = ON.
11
Page 29
Chapter2 Names and Functions of Parts
2.3 Back
15
23
19
16
14. Carrier-Gas Inlet (Carrier)
This inlet connects to the carrier-gas
plumbing. The joint is MM type.
15. Sample Purge Outlet (S. Purge)
This is the outlet for the sample-tube purge
gas and is connected via plumbing to the
joint above of the same name. The joint is
MMtype.
16. Leak Check Outlet (L. Check)
This is the connection port for the leak check
line and is connected via plumbing to the
joint above of the same name. The joint is
MMtype.
17. Purge Gas Inlet (Purge)
This inlet connects to the purge-gas
plumbing.
18. Pump Vent (Vent)
This is the exhaust outlet for the
sample-tube purge gas. The joint
13
14
18
19. Autosampler-Unit Connection Terminal
This terminal is used to connect the
autosampler unit above. It connects to 9-pin
mini-DIN connectors.
20. AC Inlet and Power Cable
21. PC Connector
This connector is used to connect to the PC
used to perform control. It is connected with
the 9-pin RS-232C cross cable that is
provided as an accessory.
22. Start-Signal Connection Terminal
This terminal is used to send the start
signal to the GC. It is connected to the GC
start input using the start cable that is
provided as an accessory.
23. AFC Inlet (Carrier)
This inlet connects to the AFC carrier-gas
plumbing.
24. AFC Inlet (Split)
22
24
21
20
17
This inlet connects to the AFC split-gas
12
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Chapter2 Names and Functions of Parts
2.4 Front Interior
25
33
32
31
28
25. Transfer Line (Line)
This line connects the sample tube and the
valve oven and can be maintained at
temperatures of up to 350ºC.
26. Valve Oven
The 6-port selection valve and the
connective plumbing can be maintained at
temperatures of up to 300ºC. If the cover is
removed, the main unit is shunted
backwards, making access to the plumbing
and valve easier.
27. Cooler Unit
This unit is used to cool the trap tube. The
temperature can be reduced to 50ºC below
room temperature with the thermo-module
and increased to 350ºC with the heater.
*From 45ºC below room temperature when
Valve temp. over 260ºC
30
26
27
29
28. Carrier-Gas Pressure Gauge
This gauge indicates the primary pressure of
the gas supplied from the carrier-gas inlet.
It can indicate pressures of up to 600 kPa.
The carrier gas is used for backflush and
purging the sample tube.
29. Purge-Gas Pressure Gauge
This gauge indicates the primary pressure of
the gas supplied from the purge-gas inlet. It
can indicate pressures of up to 600 kPa. The
purge gas is used for purging the
thermo-module and the dryer. Usually, dry
air or carrier gas is used.
30. 6-Port Selection Valve
This 2-position valve is used to switch the
flow line when introducing/desorbing the
sample to/from the trap tube. It is
motor-driven.
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Page 31
Chapter2 Names and Functions of Parts
31. Fan
This sirocco fan is used to cool the cooler
unit. It turns continuously while the power
is ON.
32. Trap Tube
This Silcosteel® tube has an outer diameter
of 3.2 mm, an inner diameter of 2.0 mm, and
is filled with adsorbent. During sampling it
is cooled and during thermal desorption it is
heated rapidly. A graphite-vespel ferrule is
used at the point of connection and so there
is no air leakage. The adsorbent is Tenax
TA.
33. Split Block
This joint is used to connect the capillary
column. It uses a nut and a graphite-vespel
ferrule.
34. Reset Switch
This switch is used to reset the TD-20
and HandringArm circuit. When you
reset, other than please do not push.
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Page 32
Chapter2 Names and Functions of Parts
2.5 Top
Upper Level 2
Lower Level 1
37
36
35
Upper Level 48
Lower Level 47
35. Sample Tray
Up to 48 sample tubes can be set in the
sample tray. Even numbers are used for the
upper levels and odd numbers are used for
the lower levels. Sample tubes must be set
in both the upper and lower levels. When a
sample tube is desorbed, the gas is purged
in the direction of the perimeter and so the
tube must be set with the end from which
the sample is injected and aspired facing the
perimeter. At the front on the right, there is
a notch only in the upper level. This position
is used to shunt the upper-level sample tube
when the lower-level sample tube is set in
the desorber unit. Do not set a sample tube
in this position.
Shunt Position
36. Sample-Tube Heating Block
Thermal desorption is performed on a
sample tube (with its caps removed) by
bringing it into contact with the sample-tube
heating block. After thermal desorption, the
block is cooled with a fan and the tube is
returned to the sample tray.
37. Seal Block
This block performs sealing with an O-ring
in order to facilitate the passing of gas
through a sample tube (with its caps
removed). The seal block has a front side
and a rear side. The rear side (purge-gas
supply side) is not heated.
15
Page 33
Chapter2 Names and Functions of Parts
2.6 Flow-Line Configuration
The diagram below shows the TD-20's flow-line configuration and the name of each part.
Fig 2-6-1 TD-20Flow-Line Configuration
16
Page 34
Chapter2 Names and Functions of Parts
Symbol Explanation Symbol Explanation
P1
P2
G1
G2
SV1 Purge solenoid valve (24 V) MFC Mass flow controller
The carrier gas is flowing through the trap tube into the columun.The trap tube is at the
standbay temperature
2.Tube Set ,leaktest progresses
sample tube has been set and a pressure leakege test is being perfomed.The sample tube is
18
Page 36
Chapter2 Names and Functions of Parts
3.Trap tube beeing cooled
The carrier gas is flowing through the trap tube into the columun.The trap tube is cooled.The
sample tube is at the standbay temperature.
4.Desorption
The carrier gas is flowing through the trap tube,which has been heated, into the columun.The
sample tube is being air-cooled to standby temperature.
19
Page 37
Chapter2 Names and Functions of Parts
5.Sample tube conditioning
When sample tube conditioning method uses, not letting flow the gas to the trap possible at "3.
Sampling" process.
6.Trap Conditioning
The carrier gas is flowing through the trap tube,which has been heated.And Line is back
-flushed
20
Page 38
Chapter3 Basic Operations
Chapter 3
Basic Operations
This chapter provides explanations on starting and stopping the system.
3.1 Starting the System
This section explains how to start the system.
3
Chapter Contents
3.2 Stopping the System
This section explains how to stop the system.
3.3 Starting and Stopping in Daily Analysis
This section explains how to start and stop the system in daily
analysis
Page 39
Chapter3 Basic Operations
3.1 Starting the System
This section explains how to start the system. Be sure to use the following procedure to
start the system after installation or after the system has been stopped, for example, to
perform maintenance.
3.1.1 Supplying Power and Gas
(1) Turn ON the power to the GC.
(2) Turn ON the power to the MS.
(3) Turn ON the power to the PC and the display.
(4) Turn ON the power to the TD-20.
(5) Mount a pressure regulator to the cylinder and check that there is no leakage.
(6) Adjust the cylinder's pressure regulator so that the secondary pressure is in the range
0.5 to 0.9 MPa.
(7) Open the main valve for the carrier gas.
22
Page 40
Chapter3 Basic Operations
3.2.2 Starting the GCMS
(1) Click the Windows Start button and select Program − GCMSsolution − GCMS analysis.
(2) The Login window shown below is displayed. Type the user name and the corresponding
password and click OK.
Fig 3.2.1 Login Window
(3) The GCMS analysis application starts and the GCMS Real Time Analysis window
opens.
Fig 3.2.2 GCMS Realtime Analysis Window
(4) Click the Vacuum Control icon in the assistant bar.
23
Page 41
Chapter3 Basic Operations
(5) The Vacuum Control window shown below is displayed. Click the Auto Startup
button. The Auto Startup indicator flashes and the vacuum system starts up. When all
the components have started (in order) and the vacuum system is ready, Ready is
displayed.
(6) Click Close to close the Vacuum Control window.
(7) This completes the GCMS startup procedure.
Fig 3.2.3 Vacuum Control Window
3.2.3 GC Settings
(1) Click the GC tab to display the following information and settings.
(2) Left
(2) Right
(3)
(4)
(5)
(2)Make settings for the injection port and carrier gas as shown below. (These are examples
of the settings made for a 0.32-mm × 60-m capillary column.)
Fig 3.2.4 GC Settings
Fig 3.2.5 Flow-Rate Settings
24
Page 42
Chapter3 Basic Operations
(3) Set the column oven temperature as shown below.
(4) Make the settings for the column used. Click Set for the column.
Fig 3.2.6 Column Oven Temperature
Fig. 3.2.7 Column Setting
(5) The Column Setting window shown below is displayed. Enter the parameters for the
column used. To do this, first click Add to add a line, then type the column name, the
(film) thickness, the length, the (inner) diameter, and the maximum temperature, and
then click Select. With the column selected, click OK.
(6) Click Ready Check.
Fig. 3.2.8 Column Registration
Fig. 3.2.9 Ready Check Button
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(7) The Ready Check window shown below is displayed. Select the Column check box under
Heat Unit and click OK.
Fig. 3.2.10 Ready Check
(8) This completes the GC settings. Refer to the GC-2010's instruction manual for more
details on GC settings.
The next step is to make the MS settings. To temporarily stop the setting procedure,
select Save Method File As from the File menu, type an appropriate name, and
save the file.
3.2.4 MS Settings
(1) Click the MS tab to display the following window.
Fig. 3.2.11 MS Settings
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(2) As an example, make the settings shown below.
Fig. 3.2.12 Example of Settings Used to Analyze VOCs in Scan Mode
(3) When all the settings have been made, select Save Method File As from the File menu,
type an appropriate name, and save the file.
(4) This completes the MS settings. Refer to the GCMS-QP2010's instruction manual for
more details on MS settings.
3.2.5 Tuning
After making the GC and MS settings, perform tuning using the following procedure.
(1) Click in the GCMS Real Time Analysis window.
Fig. 3.2.13 Autotuning Button
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(2) The Tuning window shown below is displayed. Click to start tuning.
Fig. 3.2.14 Execution of Autotuning
h(3) When tuning is completed, select Save Tuning File As from the File menu, type an
appropriate name, and save the file.
(4) This completes the tuning procedure. Refer to the GCMS-QP2010's instruction manual
for more details on tuning.
NOTE
If the detector voltage set in Fig 3.2.3 is higher than the result obtained as a result of
tuning (see below), reset the detector voltage so that it is lower than the tuning result.
Save the file after making this setting. (It is recommended that the detector voltage is set
to a value between 0.1 and 0.2 kV less than the tuning result.)
Fig. 3.2.15 Detector Volta
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3.2.6 Checking the GCMS Vacuum
Use the following procedure to check that there are no leaks in the plumbing and that the
MS vacuum level is sufficient. Check the vacuum at least 2 to 5 hours after it is drawn.
(1) Click
in the GCMS Real Time Analysis window.
Fig. 3.2.16 Tuning Button
(2) The Tuning window shown below is displayed.
Fig. 3.2.17 Tuning Window
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(3) Set the m/z values to 28 and 69, and set the detector voltage to 0.7 kV.
Fig. 3.2.18 Tuning Settings
(4) Click the BFTB Open/Close and Filament ON/OFF buttons (in this order) in the toolbar.
Fig. 3.2.19 BFTB Open/Close and Filament ON/OFF Buttons
(5) The kind of waveforms shown below are displayed. Check that the intensity for m/z 28
is at half that for m/z 69. If it is not, this indicates that there is a leak and so, after
tightening the joints and making other adjustments, check the vacuum level again. (If
the peaks are small, increase the factors accordingly.)
Fig. 3.2.20 Peak Monitor
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3.2.7 Starting the TD-20
(1)While GCMSsolution is running、Select TD Method Editor in Tool.
(2) The first time the TD-20 is started, the PID set window shown below is displayed. Click
the Copy button and then click the Set button. The temperature-control PID constants set for
the TDTS-2010 are saved at the PC.
CAUTION
If inappropriate values are set as the PID constants, the system may not operate
normally and so be sure to save the PID constants at the PC using the above
procedure.
Fig3.2.21 Starting TDU
Fig3.2.22
PID Settings
CAUTION
If a message indicating a communications error is displayed, it is possible that
communications between the TD-20 and the PC are not being exchanged normally.
Check the following points.
1. Check that the RS-232C connectors joining the TD-20 and the PC are connected
properly.
2. Check that power to the TD-20 is ON.
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(3) If communications are being exchanged normally, The TDU main window shown below is
displayed.
Fig3.2.23
TDU Main Window
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3.2.8 Configuration Settings for TD-20
Use the following procedure to check the TD-20's configuration settings and to set and change
parameters as necessary. The settings are saved as configuration-setting files.
(1) Click the Configuration tab to display the Configuration window shown below.
Fig3.2.24 TDU Configuration Setting Window
(2) As an example, make the settings shown below. (Refer to Chapter 4 for details on the settings.)
Fig3.2.25 TDU Configuration Settings
(3) When all the settings have been made, select Save As from the File menu, type an
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appropriate name, and save the file. The Analysis window is displayed.
Click the SET button to enable the settings in the TD-20.
Use the following procedure to set and save the analysis parameters. The settings are saved as
method files.
(1) Click the Analysis tab to display the Analysis window shown below.
Fig3.2.27
(2) As an example, make the settings shown below. (Refer to Chapter 4 for details on the
settings.)
Fig3.2.28 Analysis Settings
When all the settings have been made, select Save As from the File menu, type an
(3)
appropriate name, and save the file.
Analysis Window
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3.2.6 Checking the Vacuum
After making the GC gas settings, drawing the MS vacuum, and making the TDTS configuration
settings, and before increasing the temperature of the system components, use the following
procedure to check that there is no vacuum leakage.
(1)
Click in the GCMS Real Time Analysis window.
Fig3.2.29 Tuning Selection
The Tuning window shown below is displayed. Click the Peak Monitor View icon . Set
(2)
"water/air" as the monitor group and turn ON the filament.
Fig3.2.30 Tuning
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(3) Check that the intensity for m/z 28 is no greater than half that for m/z 69. If it is greater,
this indicates that there is a leak and so, after tightening the joints and making other
adjustments, check the vacuum level again. (If the vacuum-drawing time is less than 12
hours, observe developments and if N2 (m/z 28) is decreasing, wait and see how far it
drops.)
3.2.7 TD-20 Conditioning
(1) Click the Heater ON button. The Waiting (TD) window is displayed and the temperature of
each unit starts to increase.
Fig3.2.31 Heater ON Button
(2) Click the Conditioning button.
Fig3.2.32 Conditioning Button
NOTE
Perform conditioning after the valve oven's temperature reaches the set value.
If the temperature is low, it may not be possible to expel residual matter sufficiently.
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(2)The window shown below is displayed. Set the Conditioning time to 20 minutes, select
the Back flush and Valve on check boxes, and click Start. Conditioning starts, and then
stops automatically when the set time has elapsed. "Back flush" refers to the operation
where the sample-tube seal joints are purged from the 6-port selection valve in the reverse
direction with carrier gas. The flow rate is adjusted to approx. 50 mL/min.
Fig 3.2.33 Conditioning Settings
This completes the TD-20 startup procedure.
NOTE
Click Cancel to stop conditioning before completion.
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3.3 Stopping the System
This section explains how to stop the system. Be sure to use the following procedure to stop the
system when, for example, performing maintenance.
3.3.1 Stopping the GCMS
(1) Click the Vacuum Control icon in the assistant bar.
(2) The Vacuum Control window shown below is displayed. Click the Auto Shutdown
button. The Auto Shutdown indicator flashes green and the vacuum system shuts
down. When all the components (in order) and the vacuum system have stopped,
Ready is displayed.
Fig 3.3.1 Vacuum Control Window
(3) Click Close to close the Vacuum Control window.
(4) Select Quit Analysis from the File menu.
(5) The GCMS analysis-completion window shown below is displayed. Click OK to close
GCMSsolution.
(6) This completes the GCMS shutdown procedure.
Fig3.3.2
GCMS Analysis-Completion Window
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3.3.2 Stopping the TD-20
(1) Click the Heater OFF button in the TDU toolbar.
(2)Select Quit from the File menu.
(3)The Program abort confirmation window shown below is displayed. Click Ye s to
stop the TDU.
Fig3.3.3 Tool Button
(4)This completes the TD-20 shutdown procedure.
The heater is not turned OFF when the TDU is stopped.
Fig3.3.4 Program Abort Confirmation Window
NOTE
3.3.3 Turning OFF Power and Stopping the Carrier
Gas Supply
(1) Turn OFF the power to the TD-20.
(2) Turn OFF the power to the GC.
(3) Turn OFF the power to the MS.
(4) Close the main valve on the carrier-gas cylinder.
(5) Shut down the PC and turn OFF the power to both the PC and the display.
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3.4 Starting and Stopping in Daily Analysis
3.4.1 Stopping in Daily Analysis
After the system is stopped, if it is to be used again within a few days, keeping the units
warm makes it possible to perform analysis under appropriate conditions sooner. Even if the
power to the TD-20 is turned OFF, leaving the MS vacuum system in the operating state
makes it easier to resume analysis work later. This section explains how to stop the system
in daily analysis, leaving the vacuum system in the operating state.
(1) Make any necessary settings, such as those required to lower the flow rate or
temperature. The carrier-gas consumption and power consumption can be
reduced.(*1) Refer to the GCMS instruction manual for details on handling
GCMSsolution.
(2) Click the Heater OFF button in the TDU toolbar.
(3) Select Quit from the File menu in the TD-20 menu bar.
(4) The Program abort confirmation window shown below is displayed. Click OK to
stop the TD-20.
(5) Select Quit Analysis from the File menu in the GCMS menu bar.
Fig. 3.4.1 Tool Buttons
Fig. 3.4.2 Program Abort Confirmation Window
(6) The GCMS analysis-completion window shown below is displayed. Click OK to
stop GCMSsolution.
(7) Shut down the PC and turn OFF the power to the PC, display, and printer.
CAUTION
Do not turn OFF the power to the GCMS or the TD-20. Do not execute SYSTEM OFF
for the GC. Do not set the TD-20's inlet pressure to 0.
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3.4.2 Starting in Daily Analysis
Use the following procedure to resume operation after the system has been stopped using
the procedure for daily analysis.
(1) Turn ON the power to the PC and the display.
(2) Start LABsolution and the TDU control software.
(3) Click the Heater ON button in the TDU toolbar. After the Waiting window is displayed,
the temperatures of the units start to increase.
Fig. 3.4.4 Tool Buttons and Waiting Window
(4) Click the Conditioning button in the TDU toolbar.
Fig. 3.4.5 Tool Buttons
NOTE
Perform conditioning after the valve oven's temperature reaches the set value.
If the temperature is low, it may not be possible to expel residual matter
sufficiently.
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(5) The window shown below is displayed. Set the Conditioning time to a time in a range
going from a few minutes to several tens of minutes
on check boxes and click Start. Conditioning starts, and then stops automatically when
the set time has elapsed. "Back flush" refers to the operation where the sample-tube
seal joints are purged from the 6-port selection valve in the reverse direction with
carrier gas. The flow rate is adjusted to approx. 50 mL/min.
(*1) A conditioning time of 20 minutes is sufficient for VOC measurement.
Fig. 3.4.6 Conditioning Window
Note: Click Cancel to stop conditioning before completion.
(*1)
. Select the Back flush and Valve
(6) This completes the procedure for starting the system in daily analysis.
CAUTION
If conditioning is not performed, the elution of substances that have adsorbed to or
remain in trap tube or the column may cause ghost peaks in the next analysis, and it
may not be possible to obtain accurate analysis results.
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Chapter4 Menu Operations
Chapter4
Menu Operations
2 4
This chapter provides information on the functions and other aspects of the
TD-20 control software (TDU).
Chapter Contents
4.1 Main Window
This section describes the configuration of the TD-20 control
software's main window.
4.2 Configuration Window
This section provides information on the Configuration window.
4.3 Analysis Window
This section provides information on the Analysis window.
4.4 Menus
This section describes the functions available with the pull-down
menus.
4.5 Tool Buttons
This section describes the functions of the tool buttons.
4.6 Time Monitor
This section describes the time monitor.
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(3)
(2)
(1)
(6)
(7)
Chapter4 Menu Operations
4.1 Main Window
This section provides information on the main window of the TDU (TD-20 control software).
4.1.1 4.1.1 Configuration of Main Window
When the TDU is started, the main window shown in Fig. 4.1.1 is displayed. The functions of
and icons in different parts of this window are explained below.
Title bar
Menu bar
Toolbar
Analysis tab
(5) Configuration tab
Time monitor
Log window
Fig. 4.1.1 TDU Main Window
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Number Name Explanation
(1) Title bar
(2) Menu bar
(3) Toolbar
(4) Analysis tab
(5) Configuration tab
(6) Time monitor
(7) Log window
The name of the application, process, or method file
currently running is displayed.
The command menus corresponding to the currently
displayed window are displayed.
-> Refer to 4.4.
The command-tool buttons corresponding to the
currently displayed window are displayed.
-> Refer to 4.5.
The TDTS analysis settings are made from this
sub-window.
-> Refer to 4.3.
The TDTS configuration settings are made from this
sub-window.
-> Refer to 4.2.
The time required for analysis and the state of
analysis progress are displayed.
-> Refer to 4.6.
A record of operations (e.g., starting analysis or saving
data) is displayed.
Table 4.1.1 Explanation of TDU Main Window
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4.1.2 Switching between Windows
The main window consists of three sub-windows, the Analysis, Configuration, windows.
Switch between these windows by clicking the tabs. (See Fig4.1.1) The windows are
shown in Fig4.1.2.
(1) Analysis Window
(2) Configuration Window
Fig. 4.1.2 TDU Main Window
Number Name Explanation
(1) Analysis window
(2) Configuration window
Displays menus related to TDTS operating sequences,
temperature settings, and execution.
Displays menus for making the settings required for
TDTS operation. It is used, for example, to set the
autosampler used and the maximum temperatures for
the temperature control units.
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4.2 Configuration Window
This window is used to check the TD-20 configuration settings and to set and save
parameters. The settings are saved as configuration-setting files (*.cfg). Click the
Configuration tab to display the Configuration window shown below.
Fig4.2.1 Configuration Window
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Setting Description Unit Setting range Initial value
Auto
sampler
type
System Sets the type of LabSolution used.
Max temp Sets the maximum temperature for
Ready
check
Focusing Sets whether or not the interface is
CRG Do not select this option unless the
Rate Hi Sets the rate at which the temperature
Timeout Sets the time limit. After the start of
BF while
DSB
Dry purge Not used. Do not select. Selected or not
Select Tube auto sampler. Tube
Canister
P&T unit
P&T sampler
GCMSsolution
Select GCMSsolution.
the corresponding temperature control
unit. If this temperature is exceeded,
an error message is displayed, a sound
is emitted from the main unit, and the
system stops.
Sets whether or not to check if the set
temperature has been reached.
If this is selected, until the
corresponding unit reaches the set
temperature, the next operation is not
performed.Select this option for Trap.
Do not select this option for Interface
unless the optional cryofocus is used,
and do not select it for Val ve .
cryofocused. Do not select this option
unless the optional cryofocus is used.
optional cryofocus is used.
rises during heating of the trap tube.
Normally, set to "low"
pretreatment, if the trap tube's cooling
temperature does not reach the set
temperature within this time limit, an
error message is displayed and
operation is stopped.
Sets whether or not back flush of the
transfer line is performed after the
sample is taken in. Normally, do not
select this option. If it is selected, back
flush of the transfer line is performed
during desorption at 50 mL/min.
ºC All except Valve:
Selected or not
Selected or not
Selected or not
High speed:
min 0.1 to 60 10
Selected or not
GCsolution
0 to 400
Valve: 0 to 350
selected
selected
selected
Approx. 30ºC/s
Low speed:
Approx. 20ºC/s
selected
selected
None
GCMSsolution
Valve: 300
Interface: 350
Trap: 350
Line: 350
Dryer: 100
Block: 350
Trap: Selected
Other units: Not
selected
Not selected
Not selected
Low speed
Not selected
Not selected
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4.3 Analysis Window
This window is used to set and save the TD-20's analysis parameters. The settings are saved
as method files (*.met).Click the Analysis tab to display the Analysis window shown below.
Fig. 4.3.1 Analysis Window
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Setting Description
set
time Sets the aspiration time. min0 to 240 1
Line purge time
Line flush time
Wait time time
Cooling
wait
Valv e
temp
Trap cool
temp
Trap heat
temp
time
set
set
set
wait
time
Sets the purge flow rate for the sample
tube. Normally, a volume of 300 mL
(60 mL/min × 5 min) is used.
Sets the duration for which sample is
delivered when replacing the contents
of the transfer line with sample before
analysis. Normally, this setting is not
used and so set to 0 min.
Back flush is turned ON for the set
duration immediately before sampling.
This setting is used if dry purging of
the sample tube is required but
normally it is not used and so set it to
0 min.
Sets the wait time that applies after
completion of trap heating. Used to
synchronize the analysis cycle in batch
analysis.
When this time is set, even if the trap
tube reaches the set temperature, the
next operation is not performed until
this time has elapsed. As with the wait
time, this time is used to synchronize
the analysis cycle with a constant
period.
Sets the temperature for the valve
oven. A setting in the range 150ºC to
170ºC is used for VOC measurement,
whereas a setting in the range 250ºC to
300ºC is used for SVOC measurement.
Sets the cooling temperature for the
trap tube.
Sets the temperature to which the trap
tube is heated. If it is too high, it may
cause ghost peaks, and if it is too low, it
may cause carryover.
Sets the trap tube's waiting
temperature (i.e., temperature in the
state where the trap tube is not heated
or cooled).
Sets the duration for which the trap
tube is heated.
Unit Setting
range
21 to 150 60 Sample
mL/
min
min 0 to 5 0
min 0 to 5 0
min 0.01 to 1,440 5
min 0 to 655 0
ºC 0 to 350 35
ºC −80 to 350 35
ºC 0 to 350 35
ºC 50 to 100 50
ºC 0 to 30 1
Initial
value
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IF heat
temp
Block
Line set
set
wait
set
wait
Sets the heating temperature for the
interface. A setting in the range 150ºC
to 170ºC is used for VOC measurement,
whereas a setting in the range 250ºC to
300ºC is used for SVOC measurement.
Sets the waiting temperature for the
interface. This setting is not used
unless cryofocusing is performed.
Sets the heating temperature for the
sample tube's heating block.
A setting in the range 250ºC to 300ºC is
used for TenaxTA tube. If the
temperature is too high, it may cause
ghost peaks, and if it is too low, it may
cause carryover.
Sets the block's waiting temperature.
This setting is not used unless
cryofocusing is performed.
Sets the line's heating temperature. A
setting in the range 150ºC to 170ºC is
used for VOC measurement, whereas a
setting in the range 250ºC to 300ºC is
used for SVOC measurement.
ºC −170 to 350 35
ºC 0 to 100 35
ºC 0 to 350 35
ºC 0 to 100 35
ºC 0 to 350 35
* The temperatures for the different components in the analysis settings cannot be set to values
exceeding the maximum temperatures set in the configuration settings.
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4.4 Menus
The pull-down menus are the same for the Analysis, Configuration, and Batch analysis windows.
However, unavailable items are dimmed.The menu hierarchy is shown in Fig. 4.5.1.
2.
menu
Edit
1.
menu
File
3.
View
menu
4.
Direct control
menu
5.
Run
menu
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4.4.1 File Menu
Item Explanation
New Used to create a new file. Has the same function as the New
button in the toolbar.
Load Used to open an existing file. Has the same function as the Load
button in the toolbar.
Save overwrite Used to replace the file of the same name. Has the same function
as the Save overwrite button in the toolbar.
Save Used to create a file with a different name.
Comment Used to enter comments in files.
Print Used to print a file or render it as a "txt" file. Has the same
function as the Print button in the toolbar.
Exit Use to quit the TDU program.
4.4.2 Edit Menu
Item Explanation
Cut Used to cut the selected characters.
Copy Used to copy the selected characters to the clipboard.
Paste Used to paste the contents of the clipboard.
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4.4.3 View Menu
Number Item Explanation
(1) Tool button Used to display/hide the tool buttons.
(2) Event monitor Used to display/hide the event monitor.
(3) Time monitor Used to display/hide the time monitor.
(4) Log window Used to display/hide the log window.
(5) Waiting value Used to allow setting of the waiting temperatures.
(6) Adjustment room temp Used to display/hide the reading of the TD-20
unit's built-in temperature sensor.
(1) Tool buttons
(5) Waiting temperatures
(3) Time monitor
(4) Log window
(2) Event monitor
(6) Adjustment room
temperature
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4.4.4 Direct Control Menu
The operations of the TD-20 can be executed individually from the Direct control menu.
Item Explanation Notes
ON Aspirate
OFF
ON Valv e
OFF
ON Back flush
OFF
ON Aux Relay
OFF
Leak test If selected with a sample tube in the set
Reset arm Used to reset the tube-handling arm. If
Reset desorber Used to reset the desorber unit. This
Moving tube Used to move the tube from one position to
Set tube Used to perform the sequence of operations
Release tube Used to perform the sequence of operations
Rinse purge Not used.
Used to turn the flow controller ON/OFF.
ON: Aspiration starts
OFF: Aspiration stops
Used to turn the 6-port valve.
ON: Line passing through trap
OFF: Line directly connected to column
Used to execute back flush.
ON: Back flush starts
OFF: Back flush stops
Controls the Sample Tube Purge solenoid
relay.
position, a leak test is executed.
selected during measurement, the tube
may be dropped or it may not be possible
to grip it.
command can be used to take out the
sample tube if it is broken or if it remains
in the set position because of an error.
another by operating the tube-handling
arm.
required to remove the caps from the tube
and set it in the seal block.
required to remove the tube from the seal
block and reattach the caps.
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Fig. 4.4.1 Direct Control Menu
CAUTION
Because the possibility of executing instructions for directly controlling the components
is not directly related to the system status, the execution of an inappropriate instruction
could result in damage to the sample tube.
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4.4.5 Run Menu
Item Explanation
Start/Stop Used to start/stop pretreatment. Has the same function as the
Start button in the toolbar.
Heater on/off Used to turn ON/OFF TD-20 temperature control. Has the
same function as the Heater on/off button in the toolbar.
Conditioning Used to call the Conditioning window. Has the same function
as the Conditioning button in the toolbar.
Cooler purge Used to call the Cooler purge window. If there is condensation
inside the cold-trap unit, use before analysis. Has the same
function as the Cooler purge button in the toolbar.
Set Used to send the parameter settings (e.g., for temperature and
flow rate) to the TD-20 unit. Has the same function as the Set
button in the toolbar.
Reset error Used to clear errors. Has the same function as the Reset error
button in the toolbar.
Connect/Disconnect Used to connect/disconnect the communications port. Has the
same function as the Connect/Disconnect button in the toolbar.
QC/QA Test Not Used
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4.5 Tool Buttons
2
1
Numbe
r
1 New
2 Load
3 Save overwrite
4 Print
5 Event monitor
6 Time monitor
7 Log
8 Heater on/off
9 Set
10 Start
11 Conditioning
12 Cooler purge
13
14 Port setting (*1) Used to set the communications port. (*Do not change.)
15 PID setting (*1) Used to set the PID constants. (*Do not change.)
16 Tray setting (*1) Used to set the tray file. (*Do not change.)
17 Command input (*1) Used to call the command-input window.
18 Reset error (*2)
Connect/Disconnect
(*1)
3 4 5 6 7 891011 12 13 14 15 16 17
Button name Function
Table4.6
Functions of Tool Buttons
Used to create a new file. Has the same function as the New
item on the File menu.
Used to open an existing file. Has the same function as the
Load item on the File menu.
Used to overwrite and save files. Has the same function as
the Save overwrite item on the File menu.
Used to print a file or render it as a text file. Has the same
function as the Print item on the File menu.
Used to display/hide the event monitor. Has the same
function as the Event monitor item on the View menu.
Used to display/hide the time monitor. Has the same
function as the Time monitor item on the View menu.
Used to display/hide the log window. Has the same function
as the Log window item on the View menu.
Used to turn ON/OFF TDTS temperature control. Has the
same function as the Heater on/off item on the Run menu.
Used to send the parameter settings (e.g., for temperature
and flow rate) made with the menus for the TD section to
the TDTS unit. Has the same function as the Set item on the
Run menu.
Used to start pretreatment. Click it again to stop
pretreatment. Has the same function as the Start/Stop item
on the Run menu.
Used to call the Conditioning window. Has the same function
as the Conditioning item on the Run menu.
Used to call the Cooler purge window. If there is
condensation inside the cold-trap unit, use before analysis.
Has the same function as the Cooler purge item on the Run
menu.
Used to connect/disconnect the communications port. Has
the same function as the Connect/Disconnect item on the
Run menu.
Used to clear errors. Has the same function as the Reset
error item on the Run menu.
18
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Chapter4 Menu Operations
(*1) Displayed only when the Configuration window is selected.
(*2) Displayed only when the Analysis window is selected.
4.6 Time Monitor
Displays the progress of pretreatment.
The colors and times
correspond.
Wait time: 0.5 min
Desorption
Trap heating
Time for
one c
cle
Current state of
progress
Sampling
Sample: 5 min
•
•
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Chapter5
Analysis Procedures
This chapter uses representative examples to describe the flow of operations
involved in analysis, from the setting of analysis conditions to actual analysis. It
also explains how to perform continuous analysis.
5
Chapter Contents
5.1 Executing Single Analysis
This section explains how to perform a single analysis.
5.2 Settings for Batch Analysis
This section describes the settings required to perform continuous
analysis with batch-analysis functions.
5.3 Executing Batch Analysis
This section explains how to perform batch analysis.
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5.1 Executing Single Analysis
Use the following procedure to execute a single analysis.
5.1.1 TD-20 Analysis Settings
When the TDU software is installed, two commands are added to " the tool " menu of the
GCMSsolution.
TD Configuration :
Used to select communication port and the method file of the single analysis.
TD Method Editor :
Start TDU program.Used to edit TDU method file.
(1) In " the TD configuration " check "Use TD " and select the TD method.
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(2)This window is used to set and save the TD-20's analysis parameters. The settings are
saved as method files (*.met).Click the Analysis tab to display the Analysis window shown
below.
Fig. 5.1.1 Analysis Window
(3) Set the temperature, flow rate, and time for each part.
(4) When all the settings have been made, select Save As from the File menu, type an
appropriate name, and save the file.
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5.1.2 Preparing for Single Analysis
(1) Set the sample in the TD-20 sample tray.
<-The sample is added from the outside.
NOTE Be sure to set samples in both the upper and lower levels.
(2) Click in the GCMS Real Time Analysis window.
Fig. 5.1.2 GCMS Real Time Analysis Window
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(3) Click .
Chapter5Analysis Procedures
Fig. 5.1.3 GCMS Real Time Analysis Window
(4) The Sample Login window shown below is displayed. Type the sample name, sample ID,
data filename, and data description, and click OK.
Fig. 5.1.4 Sample Login Window
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(5) Click . The GC/GCMS parameters set in 5.1.1 are sent to the GC/GCMS unit and
preparation for analysis is completed.
Fig. 5.1.5 Preparing for Analysis
(7) After the tube is moved to the desorber unit, the Waiting (TD) window shown below is
displayed, and cooling of the trap tube starts.
Fig. 5.1.6 Waiting Window
NOTE It is necessary the TDU software starting. When the TDU
software has not started, being linked with the Standby button, it
starts automatically. Please do not end the TDU software
measurement midway..
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(8) Processing takes place in the order "Cooling" -> "Taking in Sample" -> "Desorption"
-> "Waiting". The current state of analysis can be monitored using the TDU Analysis
window.
Current status
Elapsed time
Colors correspond.
Sampling
Current state of progress
Processes carried ou
Waiting
Desorption
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(9) If analysis is performed normally, a chromatogram is displayed in the GCMS Real Time
Analysis window.
Fig. 5.1.8 Chromatogram Window
(10) The GC/GCMS status changes from Analysis to Preparing/Ready when analysis is
completed.
Fig. 5.1.9 Status Monitor Window
Note: To stop TD-20 pretreatment before completion, click the Stop button.
NOTE
When analysis is stopped before completion, it is possible that sample is left in the trap tube
or the column. Be sure to perform conditioning before resuming analysis.
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5.2 Settings for Batch Analysis
(1) Set the samples in the sample tray.
<-The sample is added from the outside.
NOTE Be sure to set samples in both the upper and lower levels.
(2) Click in the GCMS Real Time Analysis window.
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(3) The sample tube number of the TD-20 in the column " of vial number " of the batch table, the
method file for the TD is set to the column of the " sampler file ", respectively.
* When the column of the " sampler file " is not indicated in the batch table, the right
clicking the mouse, as indicated the sampler file with " table style ", please select " table style
" command from the menu which is indicated, set.
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(4)Click
(5) As with single analysis, TD-20 pretreatment starts, and then GCMS analysis starts.
(6) After the first analysis is completed, the second analysis starts automatically. Batch analysis
is completed when analysis has been performed the number of times set for Cycle.
Note: To stop pretreatment before completion, click the GCMS Stop button.
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5.3 Sample Tube Conditioning Method with TD-20
It is neccesary to conditioning(Baking) when brand-new Sample tube useing.
It is general to use the product, sample tube conditioner, but also it is possible to do with
the TD-20.
NOTES
Sample tube conditioning with TD-20, when the Sample tube was highly polluted, there is
a possibility pollution remaining and effect on the next Analysis.Do not conditioning
hi
(1) The method of the TD-20 is included in the TDU installation CD, the TubeCond.met is
used. This method bake sanple tube 60 minutes, but outgas does not enter into the 2nd
olluted Sample Tube.
trap tube.
(2) When batch processing could conditioning Multi Sample Tube. Use the short dummy
method file of the GCMSsolution. This file's analysis time should short(0.2min). The data
file forms, but does not have meaning please eliminate afterwards.
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Chater6
Maintenance and Service Parts
This chapter explains how to replace service parts and how to install software. It
also provides service-part lists and information related to the maintenance of
equipment.
6
Chapter Contents
6.1 Precautions
This section provides precautions related to maintenance procedures.
6.2 Replacing the Capillary Column
This section explains how to replace the capillary column.
6.3 Replacing the Trap Tube
This section explains how to replace the trap tube.
6.4 Replacing the Seal Block's O-rings
This section explains how to replace the seal block's O-rings.
6.5 Replacing the MS Filter
This section explains how to replace the MS filter.
6.6 Replacement Criteria
This section provides criteria for replacing maintenance parts.
6.7 Service-Parts List
This section contains a list of maintenance parts.
6.8 Installing the Software
This section explains how to install the software when, for example, it stops
operating normally.
6.9 Uninstalling the Software
This section explains how to uninstall the software.
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Chapter6 Maintenance and Service Parts
6.1 Precautions
WARNI NG
1. Be sure to observe all the precautions specified for the procedures described in
this chapter.
2.
The valve oven, interface, and Transferline reach high temperatures. Wait for 1hr
after HeaterOff to decrease to a temperature close to room temperature before
performing the procedures described in this chapter.
6.2 Replacing the Capillary Column
CAUTION
Be sure to stop the GCMS vacuum system before replacing the column. If the column
is removed with the vacuum system operating, air may enter the MS and the
detector may be damaged. Refer to the GCMS-QP2010's instruction manual for
details on sto
(1) Open the GC-2010's front door.
(2) Loosen the nut of the splitter on the right side of the oven using a spanner and
the vacuum system.
remove it. (See Fig6.2.1.)
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Chapter6 Maintenance and Service Parts
Fig6.2.1 Replacing Capillary Column
(3) Connect a capillary column using a vespel ferrule(PN:670-15003-04 for 0.4mmID) and
Nut(PN:223-56363) . Column insertion length is the same as the Injector of GC 34mm.
It can use the column installation jig for the Injector. (See Fig6.2.1)
CAUTION
Cut the tip of the capillary column using a capillary cutter (optional).
(4) Close the column oven's door.
(5) Refer to the GCMS-QP2010's instruction manual for details on connecting the column
on the detector side.
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6.3 Replacing the Trap Tube
CAUTION
Be sure to turn OFF the TD-20 heater with the TDU control software before
removing the trap tube. If the trap tube is removed with the heater ON, the carrier
gas may leak, and this may cause air to enter the MS and the detector may be
(1) Remove the TD-20's front cover.
(2) Remove the valve oven's cover. To do this, lift the cover up slightly, and remove the
catch on the both side before finally removing the cover to front.
Fig 6.3.1 Removing Valve Block's Cover
(3)Remove the valve block's Fixing screws(3 pieces)and remove the block.
Fig 6.3.2 Removing Valve Block's Fixing Screws
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(4)Push the block gently, taking care not to touch the plumbing or the valve, so that it
moves back approx. 1 cm. Remove the trap tube in this state.
Fig 6.3.3
(5)
Remove the M12 nuts on the right and left of the trap tube using the spanners
provided as accessories in the way showing in Fig 6.3.4
Push the block
Fig 6.3.4 Removing the Nuts
(6)Remove the ferrules and the hexagon cap nuts.
(7)
Remove the trap tube from the right side of the cold-trap unit.
Fig 6.3.5 Removing Trap Tube
(8) Insert the new trap tube from the right side of the cold-trap unit.
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(9)Attach the previously removed hexagon cap nuts and the ferrules provided as
accessories (P/N: 223-54423-91) to the trap tube.
Cold Trap Unit
(10)After tightening the joints at both ends by hand, further tighten them by 1.5
The line indicates left side of Trap Tube
rotations using the spanners provided as accessories.
(11)Pull the oven forward until it reaches the edge of the guide. (Make sure that the
plumbing parts that protrude outside the oven stay within the notch.)
(12)Set the front block,and fix with screws. To do this, insert the protrusion on the left side
of the lid into the oven's slit, lower the lid slightly so that the catch engages with the slit,.
Return the front cover to its original state.
CAUTION
When the trap tube is difficult to enter, there is a possibility the point being caught
to the coil of the heater. In that case while turning the trap tube to clockwise, when
you insert, it becomes difficult to be caught. When you push in unreasonably, there is
a possibility of breaking the heater.
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6.4 Replacing the Seal Block's O-rings
6.4.1 Replacing the Front Seal Block's O-rings
(1) Remove the screws securing the desorber cover to the top of the TD-20 and then
remove the desorber cover. The seal block becomes visible as shown in Fig. 6.4.1.
Fig 6.4.1 FIxing Screws of Desorber Cover
(2) Push down top of the insurator of the transfer(Fig 6.4.2)。
Fig 6.4.2 Removing Insulator
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Chapter6 Maintenance and Service Parts
(3) After removing the fixed screw of seal block fixing block, the seal block appears(Fig6.4.3).
Fig 6.4.3 Removing Seal Block Fixing Screw
(4) Remove joint nut of seal block and piping, with 8mm and 1/4' spanner, make the seal
block single unit (fig 6.4.4).
Fig 6.4.4 Removing Seal Block
(5) Replace the KALREZ o- ring (PN036-15670-09)with the pincette.
Filter (PN: 223-54674-01) When using it
puts to O-ring and the seal block tube
O-ring
Fig 6.4.5 KALREZ o- ring replacement
Positioning pin
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(6) After locking seal block in piping, in order as before for the positioning pin of the transfer
line to be agreeable to the groove of seal block, while installing, from above holding down with
fixing block it tightens the fixed screw, (figure 6.4.6).
Fig 6.4.6 Seal Block Fixing Nut
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6.4.2 Replacing the Rear Seal Block's O-rings
(1) Loosen the screw securing the back end of the seal block by hand, remove it, and
then lift out the seal block.
(Fig 6.4.7)。
Fig 6.4.7 Removing Rear Seal-Block
Pull out the seal block and replace the two O-rings (P/N: 223-57013) inside using
(2)
tweezers. (See Fig 6.4.8.)
(3)
Return the seal block to its original position and tighten the screws.
1. Remove the knurled screw.
Back End of Seal Block
2. Pull out the seal block.
O-ring
Seal block
3. Remove the O-ring using tweezers.
Fig.6.4.3 Back End of Seal Block
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Chapter6 Maintenance and Service Parts
6.5 Replacing the MS Filter
(1) Remove the TD-20's front cover. The MS filter (P/N: 221-34121-94) to be replaced is attached
to the top-left section. Two or three layers of aluminum packing (P/N: 201-35183) must be
inserted when attaching the G-shaped joint.
MS Filter
Fig 6.5.1 Replacing the MS Filter
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