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Operating Instructions MS 403C Aolos Mass Spectrometer

NETZSCH-Gertebau GmbH Wittelsbacherstrae 42 D - 95100 SELB Telephone: +49 (0) 9287 881- 0 Telefax: +49 (0) 9287 881- 505 E-Mail: at@netzsch.com Internet: http://www.netzsch-thermal-analysis.com

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MS 403 C Aolos Operating Instructions

CONTENTS
SAFETY INSTRUCTIONS ..................................................................................1 INTRODUCTION ............................................................................................2 MAIN COMPONENTS .....................................................................................3 OPERATIONAL CONTROL AND STATUS DISPLAY ......................................................... 3 TEMPERATURE CONTROLLER .................................................................................. 4 HEATED GAS INLET SYSTEM ................................................................................... 5 STRUCTURE AND TECHNICAL SUPPORT ..................................................................... 7 PUMPING SYSTEM ............................................................................................ 8 PRESSURE GAUGE ............................................................................................. 8 ANALYSIS UNIT WITH ELECTRONICS ..................................................................... 8 ELECTRONIC BOARD ......................................................................................... 9 COMMISSIONING .......................................................................................10 INSTALLING AND CHANGING THE CAPILLARY ....................................................... 10 CHANGING THE CAPILLARY .......................................................................... 14 CLEANING THE ADAPTER ................................................................................. 23 INSTALLING THE ELECTRONIC UNIT OF THE QMA ................................................. 25 DISMOUNTING OR INSTALLING THE HOUSING ...................................................... 25 INSTALLING THE DATA LINE .............................................................................. 26 INSTALLING THE EVALUATION SOFTWARE ........................................................... 26 SWITCHING ON THE MEASURING UNIT ................................................................ 26 BAKING OUT THE VACUUM RECIPIENT ................................................................ 27 SWITCHING OFF THE MEASURING UNIT ............................................................... 28

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MS 403 C Aolos Operating Instructions

ELECTRICAL CONNECTIONS ...........................................................................29 TROUBLESHOOTING .....................................................................................31 APPENDIX ................................................................................................33 TECHNICAL SPECIFICATIONS ................................................................................. 33 SPARE PARTS .................................................................................................... 34

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MS 403 C Aolos Operating Instructions

Safety instructions
Before opening the measurement unit, you have to switch off the device and turn off the power supply. Even if the device is switched off, it is possible that the temperature of the gas inlet unit's furnace is very high (the word HOT is visible on sticker). Therefore it is necessary to check the surface temperature of the gas inlet unit if you have to do some work with the furnace (the word HOT is invisible on sticker). You can read the furnace temperature by switching on the device. It is then possible to decrease the programmed temperature value. To prevent contaminations of the vacuum system, you should use particle-free gloves when working with the ion-source or capillary.

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MS 403 C Aolos Operating Instructions

Introduction
The MS403C Aolos gas analysis system is used for the qualitative determination of gas components, which are emitted during the thermogravimetric analysis. The system consists of the following components: oil-free vacuum system Quadrupole-Mass Spectrometer(QMA200), range: 0 300 amu controlled heating transfer line with changeable capillary and gas inlet unit measuring and evaluation software

The Quadrupole-Mass Spectrometer is equipped with a crossbeamion source for a high linearity of signals with a low fragmentation of molecules and a channeltron (SEM) detector for fast and sensitive data evaluation. Vacuum is generated by a turbo molecular pump and a membrane pump connected in series. For the determination of working pressure in the vacuum recipient, a PKR 261 pressure gauge with a range of 1000 mbar - 109 mbar is used. The measured pressure is evaluated, saved and displayed by the software. The evaluation software is controlled by an analog trigger signal. There are also digital contacts for input and output at your disposal.

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MS 403 C Aolos Operating Instructions

Main components
Operational control and status display

QMS 403 C

transfer line

300
inlet system

online

300

heating

Figure 1: operational control

status display tansfer line inlet system pump state online heating

meaning green LED: temperature of the transfer line at the programmed value green LED: temperature of the furnace at the programmed value green LED: rated speed of the turbo pump is reached red LED: error turbo pump measurement is active the heating key switches on the furnace for the vacuum recipient automatically to heat the recipient (see bake out in manual).

transfer line inlet system

temperature controller for transfer line temperature controller for furnace

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MS 403 C Aolos Operating Instructions

Temperature controller

300
K1 K2
Figure 2: temperature controller

OMRON 702040 temperature controllers are available for the transfer line and the furnace. As a standard, both controllers are adjusted to a programmed temperature value of maximum 300C. This value can be adjusted to the different applications anytime by the operator. The controllers are switched on and off by the Quadrupole-Mass Spectrometer.

A detailed description of the controllers is included in the manual.

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MS 403 C Aolos Operating Instructions Heated gas inlet system


transfer line

protection grid

fixing screws

Figure 3: gas inlet unit with protection grid

The temperature-controlled (max. 300C) gas inlet system consists of the furnace and the transfer line with an inside capillary. The protection grid is fixed to the displacement unit by 4 fixing screws and has to be removed before opening the measurement unit (see Figure 3 and Figure 4).
displacement unit

furnace
Figure 4: gas inlet unit without protection grid

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MS 403 C Aolos Operating Instructions

The displacement unit can be fixed at the highest position on the back side by fixing a screw. The quick-release fastener (see Figure 5) between the vacuum recipient and the gas inlet system consists of the stretch fastener and the copper sealing (max. torque: 7-8 Nm).
quick-release fastener

Figure 5: quick-release fastener

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MS 403 C Aolos Operating Instructions Structure and technical support


2 1 3 4

8 6
Figure 6: QMA measurement unit without cap

1 2 3 4 5 6 7 8

turbo molecular pump controller for turbo molecular pump sealing cap of the resource reservoir membrane pump pressure gauge analysis unit of the QMA with ion-source, rod system, and detector unit electronic unit of QMA electronic board

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MS 403 C Aolos Operating Instructions

Pumping system
The pumping system is free of oil. Exhaust gases from the pumping system will be diverted from the device by the EXHAUST connection and should be connected to an extractor unit by using an exhaust tube (external diameter 6 mm).

Pressure gauge
The pressure gauge measures a voltage which is proportional to the pressure. Voltage is read in by the QMA analog input and evaluated by the software. The measurement, and therefore the output signal of the pressure gauge, depends on the type of gas. The pressure gauge is calibrated to N2. If other gases are used, the measured value has to be corrected with a gas calibration factor (dependent on the gas). Please consult the manual of the PKR 261.

Analysis unit with electronics

10

11

Figure 7: analysis unit of QMA

9 10 11

clip for electronic unit UHV flange with copper sealing for analysis unit ion-source window

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MS 403 C Aolos Operating Instructions

The analysis unit is connected to the vacuum recipient by a UHV-flange with copper sealing. With the help of the show glass, you can check the functioning of the cathode (shining if the cathode is on). The electronic unit can be separated from the analysis unit by disconnecting the clip and the supply cables (see Figure 8).

12

Figure 8: supply cables on electronic unit

12

supply cables on electronic unit

Electronic board
The electronic board is for controlling the pumps and takes over switching functions. All connecting lines are pluggable. Below the board, there are relays for the power switch of the heating circuit.

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MS 403 C Aolos Operating Instructions

Commissioning
Before the first installation, ensure that the power plug of the instrument is unplugged and that the power switch is off (position 0).

Installing and changing the capillary


In the delivery status, the transfer line is dismantled and the quartz capillary is coiled inside the furnace of the gas inlet unit.

For a first installation of the capillary, you have to do the following steps:
1. Removing the protection grid Loosen the screws. Remove the protection grid.

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MS 403 C Aolos Operating Instructions


2. Opening the furnace The word HOT on the sticker must be invisible (that means furnace is cold).

ATTENTION! If the sign HOT can be seen, there is a danger of burning! Loosen the screws. Remove the front side of the furnace.
sticker HOT front side of the furnace

3. Connecting the transfer line to the furnace Plug the end of the transfer line from which electrical cables
transfer line

emerge into the receptacle so that the transfer line extends 5 mm from the insulation material into the furnace (if necessary, the insulation

receptacle fixung screws

material must be pushed back into the original position).

5mm insulation material

Affix the transfer line with both


screws.

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MS 403 C Aolos Operating Instructions


4. Pushing the capillary into the transfer line For the first commissioning, the capillary is coiled inside the furnace. Uncoil the capillary inside the furnace and push it into the transfer line until the capillary protrudes (a few cm) from the adapter on the
transfer line furnace

STA side.

5. Affixing the capillary to the adapter (STA side)


adapter

Push a new graphite sealing (ferrule) and the nut over the protruding capillary. Cut the protruding capillary.

graphite sealing (ferrule) 90 mm nut

1. scarify

capillary

2. snap off

Affix the protruding capillary (Coil the remaining capillary into the furnace so that it can be pulled out on the STA side.) with the graphite sealing (ferrule) and the nut so that approx. 90 mm of the capillary extends from the adapter (see figure).

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MS 403 C Aolos Operating Instructions


6. Affixing the transfer line to the STA by gas connection adapter
adapter on the transfer line

Attach the adapter from the top onto the STA. Turn the adapter counterclockwise until it stops. Affix the adapter with the 4 nuts.

connection on the STA side

7. Attaching the protection grid on STA side


protection grid

Place the protection grid over the adapter. Affix the protection grid with the 3 screws.

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MS 403 C Aolos Operating Instructions


8. Closing the furnace Coil the remaining capillary circularly into the furnace so that it can be pulled out easily on the STA side. Attach the front side of the furnace. Affix the protection grid.

Changing the capillary


1. Removing the protection grid Loosen the screws. Remove the protection grid.

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MS 403 C Aolos Operating Instructions


2. Opening the furnace The word HOT on the sticker must be invisible (that means furnace is cold).

ATTENTION! If the sign HOT can be seen, there is a danger of burning! Loosen the screws. Remove the front side of the furnace.
sticker HOT front side of the furnace

3. Opening the quick-release fastener Loosen the screw connection of the quick-release fastener with a combination wrench. Remove the quick-release fastener.

screw connection

quick-release fastener

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MS 403 C Aolos Operating Instructions


4. Pushing the furnace upwards Loosen the fixing screw. Move the furnace into
displacement unit

the highest position. Tighten the fixing

fixing screw

screw.

5. Removing the protection grid on the STA side


protection grid

Loosen the screws (only loosen, do not remove!). Remove the protection grid (lift it upwards).

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MS 403 C Aolos Operating Instructions


6. Loosening the adapter on the STA side
adapter on the transfer line

Loosen the 4 nuts (only loosen, do not remove!). Turn the adapter clockwise. Remove the adapter (lift it upwards).

connection on the STA side

7. Removing the old capillary


To remove the old capillary, you have to remove the nut in the furnace as well as the nut on the adapter on the STA side (see next figure).

Pull the capillary out of the transfer line and dispose of it correctly.

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MS 403 C Aolos Operating Instructions

adapter

nut
graphite sealing (ferrule) nut capillary

capillary guide

furnace

adapter

8. Cutting the new capillary Cut a new capillary to a length of about 220 cm. Scarify the capillary.

Snap off the capillary at the scarified point.

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MS 403 C Aolos Operating Instructions


9. Installing the new capillary in the furnace Push the nut and the
capillary

graphite sealing (ferrule) over the capillary. Slightly shorten the end of the capillary over
nut graphite sealing (ferrule) hole in base plate

which the nut and graphite sealing have just been pushed. Push this end of the capillary through the hole in the base plate and capillary guide so that the excess length is 10 mm. Tighten the nut.

capillary guide

10mm

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MS 403 C Aolos Operating Instructions


10. Pushing the capillary into the transfer line Push the capillary into the transfer line until the capillary protrudes (a few cm) from the adapter on the STA side.
transfer line furnace

11. Affixing the capillary to the adapter (STA side)


adapter

Push a new graphite sealing (ferrule) and the nut over the protruding capillary. Cut the protruding capillary again. Affix the protruding capillary with the graphite sealing (ferrule) and the nut so that approx. 90 mm of the capillary extends from the adapter (see figure).

graphite sealing (ferrule) 90 mm nut

capillary

Coil the remaining capillary into the furnace so that it can be pulled out on the STA side.)

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MS 403 C Aolos Operating Instructions


12. Affixing the transfer line to the STA by gas connection adapter
adapter on the transfer line

Attach the adapter from the top onto the STA. Turn the adapter counterclockwise until it stops. Affix the adapter with the 4 nuts.

connection on the STA side

13. Attaching the protection grid on STA side


protection grid

Push the protection grid over the adapter. Fix the protection grid with the 3 screws.

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MS 403 C Aolos Operating Instructions


14. Pushing the furnace downwards Check whether there is a copper sealing between the flanges. Loosen the screw on
flange

the displacement unit (see 4). Move the furnace downwards.

copper sealing

15. Closing the quick-release fastener Put on the quickrelease fastener. Tie up the screw with a torque of 7-8 Nm.

torque 7-8 Nm

quick-release fastener

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MS 403 C Aolos Operating Instructions


16. Closing the furnace Coil the residual capillary circularly into the furnace so that it can easily be pulled out on the STA side. Attach the front side of the furnace. Affix the protection grid.

Switch on the furnace and perform a measurement.

Cleaning the adapter


protection grid

Loosen the screws (only loosen, do not remove!). Remove the protection grid (lift it upwards).

allen screws

Unscrew the allen screws so that the support ring is moveable (now you can reach all three hexagon head screws on the adapter, see next picture).

support ring

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MS 403 C Aolos Operating Instructions


Loosen (only loosen, do not remove!) the hexagon head screws on the adapter. Turn the adapter counterclockwise and lift it upwards.

hexagon head screws

Use a screw driver and unscrew the gas tube (the gas tube consists of a temperature guidance tube with a separate cover tube, see next figure below).

gas tube
gas tube

screw driver

Remove the cover tube for cleaning the slot of the temperature guidance tube.

temperature cover tube guidance tube (with slot for gases)

Install the adapter in reverse order.

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MS 403 C Aolos Operating Instructions Installing the electronic unit of the QMA
If the electronic unit was dismantled for transport, place it in horizontal position on the analysis unit. Unfix the clip on the electronic unit and set the device on the analysis unit so that the spring catches the nut on the flange of the analysis unit easily. If necessary, you may turn the electronic unit on its own axis. Fasten the clip sturdily by hand and plug in the connecting cables (see Figure 8) and affix them.

Dismounting or installing the housing


Before dismounting the housing remove the upper cover plate (lift it upwards) and then loosen the two front located allen screws below the plate. In order to pull out the front cover loosen the lower four hexagon head screws on the front cover. Disconnect the connecting cables for the operating elements and the temperature controllers on the respective board. For removing the right or left cover plate loosen also the lower hexagon head screws on the respective cover and the allen screws on the rear. The Installation of the cap must be done in reverse order. Details are shown in Figure 9.

upper cover plate

Figure 9: removing the cover plates

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MS 403 C Aolos Operating Instructions

Installing the data line


Connect the ends of the serial cable for data exchange to the serial interface of the PC (COM1/COM2) and to the RS-232 connector on the back side of the Aolos instrument. Connect the STA trigger cable to the ANALOG I/O connector on the Aolos instrument.

Installing the evaluation software


Install the evaluation software as directed in the manual. Check that the data exchange through the serial interface is active with the help of the Parset.exe program (see short manual QS). Check that the MSDiagnose diagnostic program is available. If necessary, install it as directed in the enclosed software documentation.

Switching on the measuring unit


Be sure that the cap is locked and that the line for exhaust gases is installed. Check the quick-release fastener for a tight fit. After connecting the line cord, turn on the instrument with the power switch. The pumping system is started and signals the achievement of the minimum necessary pressure (pump state display on the front of the instrument, max. 5 minutes). The temperature controller of the gas inlet system starts heating the transfer line and the furnace of the gas inlet system. The current temperature of the transfer line and the gas inlet system can be read from the temperature controllers. After 30 40 minutes, the furnace will have reached the programmed temperature value (300C). After the status display lights up, you can start the MSDiagnose diagnosis program and the pressure in the recipient will be displayed.

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MS 403 C Aolos Operating Instructions


5

For air or nitrogen (N2), the system pressure should be at about 2x10 If the system pressure is much less than 2x10
5

mbar when

5 the transfer line is heated to 300C (room temperature approximately 5x10 mbar).

mbar, the capillary is probably

congested. A pressure value of more than 4x10 indicates a leak in the vacuum system. If the necessary pressure is achieved, you can switch on the cathode (see software manual). When the displays of pump state on the front are active, then the system is ready for measurement.

Please consider that for measurements with the Aolos-MS the gas flow on the connected instrument (e.g. STA) must not be switched off.

Baking out the vacuum recipient


If the instrument has not been active for several days, it is suggested that the recipient be baked out to remove adsorbed gases. To do this, press the bake key on the front of the measuring unit. If the red light on the front is shining, the measurement will probably not be correct, since the recipient is still being heated and therefore the basic signal is still rising.

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MS 403 C Aolos Operating Instructions

Switching off the measuring unit


Before switching off the measuring unit, be sure that the cathode and the SEV are turned off. Exit the measuring program. The measuring unit should be switched off by the power switch on its back side at least 10 minutes after the cathode was switched off.

For different models, the vacuum system will be ventilated through the transfer capillary or by an air valve. After switching off the unit, the rotor of the turbo molecular pump will still be turning. About 5 minutes after that, you can open the recipient or move the system. Premature ventilation or transport can damage the turbo molecular pump.

The temperature of the furnace will remain at above 50C for at least 30 minutes (HOT sticker).

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MS 403 C Aolos Operating Instructions

Electrical connections

RS 232 TRANSFER LINE

CONTROL

TMU

P1 POWER

ANALOG I/O EXHAUST

Figure 10: Aolos back side

designation POWER RS-232 CONTROL ANALOG I/O TRANSFER LINE TMU EXHAUST P1/P2

function voltage serial interface to PC digital in/output analog in/output operating voltage transfer line service for turbo pump gas outlet pumping system analog pressure read out

version switches, filter, 2 backups Sub-D 9pin connector Sub-D 15pin connector Sub-D 15pin connector plug-in connector, 4 pin screw connection 5 pin screw connection connection tube: 6 mm

The analog trigger signal for the control of the QMA is fed by the ANALOG I/O connector (contact 14 and 15).

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MS 403 C Aolos Operating Instructions configuration of contacts


CONTROL: contact 1 2 3 4 8 15 12 13 14 5, 6, 7, 9,10, 11 meaning DI#0 (1) DI#0 (2) DI#1 (1) DI#1 (2) DO#0 (24VDC) DO#0 (0 VDC) 0 VDC 0 VDC 24 VDC free

ANALOG I/O:

contact 7 8 9 10 11 12 13 14 15 1 through 6

meaning AI_CH1+ AI_CH1AO_CH1+ AO_CH2+ AO_CH3+ AO_CH4+ AO_COM AI_CH0 + AI_CH0 free PKR PKR

Trigger STA Trigger STA

TRANSFER LINE:

contact 1 2 3 4

meaning 48 VAC 48 VAC NiCr/Ni NiCr/Ni (L) (N) (+) (-)

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MS 403 C Aolos Operating Instructions

Troubleshooting
In the following table, there are notes to eliminate possible errors.

problem pressure oversized (p > 2x10 mbar)


-5

possible causes

error correction

Quick-release fastener Retighten quick-release is loose. Capillary screw connection is loose; broken capillary. fastener; if necessary, change the copper sealing. Retighten the screw connection, replace the graphite sealing (ferrule), or change the capillary. Temperature of gas Check programmed temperature value.

(pump state signal is ok.)

inlet unit too low. very low pressure (much less than 2x10 5 mbar) no pump state Leak at the quickrelease fastener or capillary screw connection. Capillary congested.

Retighten quick-release fastener; if necessary, change copper sealing, retighten screw connection, replace the graphite sealing (ferrule), or change the capillary.

display after warm up

Counter

pressure

at Check whether the exhaust system is functioning. Replace air valve. Demount pump and do a maintenance check. Remove the pump and do a maintenance.

the exhaust line. Air valve defective. Membrane pump defective. Turbo pump defective.

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MS 403 C Aolos Operating Instructions


no transfer line or Error at heater loop of temperature display the transfer line or of the furnace. Check programmed temperature value at the Omron controller; check the fuse for the heater loops, missing supply voltage, relay defective, heating cartridges defective. no measurement signals Cathode switched off Switch on the emission, or defective. switch over to the second filament. SEM switched off or Switch on SEM and check working voltage too the voltage. low . incorrect measurement results Ion flow signals too low. Bad IQ-focus. Working voltage of SEM too low. Check settings for emission/SEM, check system pressure. Focus the IQ-source (TuneUp.exe). Check the SEM voltage.

The substitution of components of the pumping system, ion-source or the channeltron is prohibited unless the work is carried out by specialists.

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MS 403 C Aolos Operating Instructions

Appendix
Technical specifications

575

610

530

dimensions: weight: electrical connection: power consumption: gas inlet:

575x610x530 mm 60 kg 230 VAC 50/60 Hz (optional 115 VAC 60Hz) 600 VA single-stage, heating up to 300C quick-release fastener at the direction of the recipient Crossbeam 1 - 300 amu Faraday / SEM (Channeltron) MID (max. 64 channels) Scan Analog Scan Bargraph

ion-source: range: detector: type of measurement:

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MS 403 C Aolos Operating Instructions Spare parts article


transfer line, heatable up to 300C, with fused silica capillary, length 1.5 m transfer line, heatable up to 300C, with fused silica capillary, length 2.0 m gas tube: temperature guidance tube cover tube capillary 75 m graphite sealing for adapter (14.5x8x2 mm) graphite sealing for transfer line (14.5x10x3 mm) graphite sealing (ferrule) for capillary copper sealing quick-release fastener quick-release fastener filament copper sealing DN63CF copper sealing DNCF40 formation chamber operating fluid reservoir for turbo pump

order number
6.226.1-91.5 6.226.1-91.10

HTP4000A18.011-03 HTP4000A18.011-04 NGB 802922 NGB 802858 NGB 802859 NGB 802958 NGB 802957 NGB 802990 NGB 804366 GB 427061 GB 426408 NGB 809659 NGB 804367

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