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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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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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ELECTRICAL CONNECTIONS ...........................................................................29 TROUBLESHOOTING .....................................................................................31 APPENDIX ................................................................................................33 TECHNICAL SPECIFICATIONS ................................................................................. 33 SPARE PARTS .................................................................................................... 34
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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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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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Main components
Operational control and status display
QMS 403 C
transfer line
300
inlet system
online
300
heating
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).
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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.
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protection grid
fixing screws
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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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
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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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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.
10
11
9 10 11
clip for electronic unit UHV flange with copper sealing for analysis unit ion-source window
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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
12
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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Commissioning
Before the first installation, ensure that the power plug of the instrument is unplugged and that the power switch is off (position 0).
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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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
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STA side.
Push a new graphite sealing (ferrule) and the nut over the protruding capillary. Cut the protruding capillary.
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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Attach the adapter from the top onto the STA. Turn the adapter counterclockwise until it stops. Affix the adapter with the 4 nuts.
Place the protection grid over the adapter. Affix the protection grid with the 3 screws.
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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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fixing screw
screw.
Loosen the screws (only loosen, do not remove!). Remove the protection grid (lift it upwards).
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Loosen the 4 nuts (only loosen, do not remove!). Turn the adapter clockwise. Remove the adapter (lift it upwards).
Pull the capillary out of the transfer line and dispose of it correctly.
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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.
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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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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).
capillary
Coil the remaining capillary into the furnace so that it can be pulled out on the STA side.)
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Attach the adapter from the top onto the STA. Turn the adapter counterclockwise until it stops. Affix the adapter with the 4 nuts.
Push the protection grid over the adapter. Fix the protection grid with the 3 screws.
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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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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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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.
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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.
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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).
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.
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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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Electrical connections
CONTROL
TMU
P1 POWER
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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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
TRANSFER LINE:
contact 1 2 3 4
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Troubleshooting
In the following table, there are notes to eliminate possible errors.
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.
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.
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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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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Appendix
Technical specifications
575
610
530
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
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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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