KORE PTR TOF-MS User Manual

Unipolar vertical

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Z-9524-M

Kore Technology Ltd, Cambridgeshire Business Park, Ely, Cambridgeshire CB7 4EA, UK

Tel. 44 (0) 1353 653030 Fax. 44 (0) 1353 653031

Unipolar Vertical

PTR TOF-MS

User Guide

Ver.

Date

20/09/13

Comment

Updated with GD maintenance

information

Initial

DFR/

MSN

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Summary of Contents for KORE PTR TOF-MS

Page 1 Z-9524-M Unipolar Vertical PTR TOF-MS User Guide Ver. Date Comment Initial 20/09/13 Updated with GD maintenance DFR/ information Kore Technology Ltd, Cambridgeshire Business Park, Ely, Cambridgeshire CB7 4EA, UK Tel. 44 (0) 1353 653030 Fax. 44 (0) 1353 653031...
Page 2: Table Of Contents
7.3 A note concerning the analyte pipe positioning................28 7.4 A note concerning the analyte pipe sealing.................29 8 APPENDIX A: OUR CURRENT THINKING ON OPERATING A KORE PTR-TOF-MS....31 8.1 Introduction..........................8.2 From source to detector......................8.3 What happens as I twiddle this knob (see also the manual)?............34...
Page 3: Introduction
“Main Instrument On/Off”. 2.2 Vacuum system All control and monitoring of the vacuum system is carried out through the Kore Pumping Control Unit. This unit is fully described in the accompanying Hardware Reference manual.
Page 4: Cabling
2.0x10 mbar. If the Kore power supplies are switched on before this point, the ‘Interlock Fail’ lights will illuminate and no high voltages will be enabled.
Page 5 ● Use only de-ionised water (or deposits will form on the bottle as the water evaporates). ● Fill the bottle to approximately half full. ● Replace the lid firmly. Commercial in Confidence © Kore Technology Ltd 2013...
Page 6: Analyte Gas Sampling
Otherwise the 'analyte out' line may be capped off. A full schematic of the gas pipework of the PTR is shown in Figure 4. Commercial in Confidence © Kore Technology Ltd 2013...
Page 7 I S S C H A N G E I N I T T H I R D A N G L E P R O J E C T I O N D O N O T S C A L E A l l V e s p e l ( o r V e s p e l - G r a p h i t e ) F e r u l e s 6 / 1 3 F e r r u l e w a s 1 / 1 6 0 .
Page 8: Setting Up The Gas Supply Into The Glow Discharge Region
(depending on the gas), the glow discharge can be started. The power supplies for driving the glow discharge are all within the Kore PTR Supply Unit. The glow discharge is started using the glow discharge switch on the front panel. An indicator lamp above the switch shows the status of the glow discharge.
Page 9 The voltage required for a discharge depends upon the gas species and also the parameter mbar.mm. For further information see general reference material on the subject of “Paschen curves” Figure 5 - Paschen curves for various gases Commercial in Confidence © Kore Technology Ltd 2013...
Page 10: Calculating E/N- The Townsend Number
120°C, with the PTR source flange itself at 120°C. The heating is under proprietary proportional control using the Kore Heating Controller. Each heated zone has temperature feedback with LED indication to show when the zone temperature has reached the setpoint (...
Page 11: Collecting Your First Mass Spectrum
Figure 8: Setting Acquisition options 4. When the Acquisition options have been set click ‘OK’ to return to the main screen. 5. Select the ‘Acquire Spectrum’ button to launch an acquisition. Commercial in Confidence © Kore Technology Ltd 2013...
Page 12 This status window is not part of GRAMS/AI, it is part of the underlying data collection program, runtdc.exe. For a full description of the software structure for operating the Kore 4G TDC, please consult the TDC manual.
Page 14: Removal And Refitting Of The Source
Figure 14 shows the instrument with the rear panel removed, showing the PTR oven and connections.    Figure 14 : PTR Oven and connections (1) PTR oven (2) Junction Box (3) Gas connections (hidden from view on far side) Commercial in Confidence © Kore Technology Ltd 2013...
Page 15 Any other means of venting may cause rapid pressure changes that could destroy one of the thin apertures within the instrument. It is recommended that the PTR TOF-MS is vented to dry nitrogen, connected to the Vent Gas connection provided on the Utilities Panel, near the instrument power inlet.
Page 16 The screw fixings that must be undone are coloured black. Do not unscrew any other fixings. Figure 18 - Oven top removal Commercial in Confidence © Kore Technology Ltd 2013...
Page 17 Unscrew the nut holding the metal pipe in the ceramic component using the 5/16” spanner provided (5/16” = 7.94mm, so an 8mm spanner could be used). Gently pull the pipe out of the ceramic. Commercial in Confidence © Kore Technology Ltd 2013...
Page 18 Analyte In GD Gas In GD Cathode connection GD Pressure Sense Via series resistors Blue GD Anode Black Reactor First Plate PTR Pressure Sense Reactor Entry Figure 25 - Source Flange Connections Commercial in Confidence © Kore Technology Ltd 2013...
Page 19 – unwrap it from the pipe so that it is free to move. (3) Disconnect the flange heater wires from the oven terminal block. Commercial in Confidence © Kore Technology Ltd 2013...
Page 20 Figure 33 - Torlon fixing disassembly Figure 32 - Disassemble Swagelok Bulkheads Using these tools, disconnect the pipes from all the Torlon adaptors and the Swagelok bulkheads, as indicated in Figure 32 and Figure 33. Commercial in Confidence © Kore Technology Ltd 2013...
Page 21 It is necessary to rotate the oven so that the circular opening in the end plate can clear the cartridge heaters of the source flange. Carefully guide the oven end plate over the reactor and flange, as shown in Figure 35. Commercial in Confidence © Kore Technology Ltd 2013...
Page 22: Disassembling The Ptr Source
WARNING! All parts inside the PTR have been cleaned to UHV standards and UHV best practice should be observed when handling them. Use suitable gloves to prevent contamination. Commercial in Confidence © Kore Technology Ltd 2013 Figure 37 - Reactor stack and cell removal...
Page 23: Removing The Ptr Source Intact
Disconnect the backing line from the side of the boundary flange. Figure 38 - PTR backing line removal Remove the M8 cap-head bolts from the perimeter of the flange to remove the entire PTR source. Commercial in Confidence © Kore Technology Ltd 2013...
Page 24: Fitting The Ptr Source
The instrument has only fully vented when both the vacuum gauges read atmospheric pressure. It is only at this point that the dry nitrogen supply should be removed and the dis- assembly of the GD source commenced. Commercial in Confidence © Kore Technology Ltd 2013...
Page 25 You do not need high pressure, only enough to gently compress the O-ring seals. Remove the polymer ring. Take care to keep the O-ring seals clean The cathode is viewed showing the cathode space Figure 42 Commercial in Confidence © Kore Technology Ltd 2013...
Page 26: Inspecting And Cleaning The Anode Aperture
7.2 Inspecting and cleaning the anode aperture When the cathode is removed from the anode, on a new instrument you would see a shiny metallic anode aperture facing the cathode. Figure 44 Commercial in Confidence © Kore Technology Ltd 2013...
Page 27 400 micrometer aperture. Any material on or near this aperture could cause a blockage, and if it is non-conductive it can charge up and greatly affect the transmission of the instrument. Commercial in Confidence © Kore Technology Ltd 2013...
Page 28: A Note Concerning The Analyte Pipe Positioning
A simple way to set the positioning of the analyte pipe is as follows: Position the analyte pipe level with the ceramic piece (view from the underside of the anode plate. Figure 49 Commercial in Confidence © Kore Technology Ltd 2013...
Page 29: A Note Concerning The Analyte Pipe Sealing
Silcosteel pipe. If you need to change the ferrule you should not attempt to compress it with the ceramic voltage break in the anode. If you do this there is a good chance you will shear the ceramic. Commercial in Confidence © Kore Technology Ltd 2013...
Page 30 However, when you come to tighten the analyte pipe in situ, the ferrule is already 'pre-crushed' and only a light force will be required to make a seal between the ceramic and the pipe. Commercial in Confidence © Kore Technology Ltd 2013...
Page 31: Appendix A: Our Current Thinking On Operating A Kore
Z-9524-M 8 Appendix A: Our current thinking on operating a Kore PTR-TOF-MS GD Cathode Reagent gas i n GD Anode Analyte in Reactor Entry Reactor First Plate Reactor plate 26 (P26) Reactor Last Plate Reactor Exit Transfer optics Shield Transfer back...
Page 32: From Source To Detector
(or more precisely, with a similar probability distribution of possible paths). The Commercial in Confidence © Kore Technology Ltd 2013...
Page 33 The TOFMS geometry is orthogonal and the TOF source is pulsed. For best duty cycle the ions should travel through the TOF Commercial in Confidence © Kore Technology Ltd 2013...
Page 34: What Happens As I Twiddle This Knob (See Also The Manual)
In the later systems this adjustment is a pre-set, which is adjusted to give as even a field as possible i.e. no lensing action. Experience suggests that any minor Commercial in Confidence © Kore Technology Ltd 2013...
Page 35 T.lens. The adjustment is usually via 4 internal pre-set potentiometers, one for each deflector, which should be adjusted in pairs so as to be equally spaced around the T.lens potential on each of the axes x & y. Commercial in Confidence © Kore Technology Ltd 2013...
Page 36: Things To Catch You Out
These steer the beam in the TOFMS to try and maximise the proportion that hits the detector. By Kore convention the 'X' adjustment direction is towards/away from the detector. Bear in mind that the incoming ion beam already has momentum in the 'X' direction. The incoming beam may have significant energy spread in the 'X' direction, depending on the detail of scattering in the expending gas plume at the start of the transfer section.
Page 37 We suspect that the glow discharge is shifting mode to a 'bad' place, from where it won't recover unless completely extinguished. Commercial in Confidence © Kore Technology Ltd 2013...