Micro-GC channel with µ-TCD Hardware CP-4900 DMD µ-DMD µ-DMD fully integrated into CP-4900 Micro-GC hardware µ-DMD serial connected, via heated transfer line,(inert) with µ-TCD (modified) Micro-GC operates under standard conditions Micro-GC channel with µ-TCD

Radio active cell is regarded as a closed source DMD Channel The radiation source used in the SVAC is 63Ni. This material is in the form of a 63Ni foil sheet that is placed within the manifold of the SVAC Sensor Cell Assembly. Radio active cell is regarded as a closed source

DMD Channel Sensor board Ni63 source Flow controller Check valve Main board and UI board Driftgas Zero Air or N2

Hardware CP-4900 DMD Housing modification Differences on standard CP-4900: main board revision/ IOC MPU firmware V1.30 build 01 Housing modification CP-4900 module TCD connections Heated transfer line DMD 4Watt NO UPGRADE POSSIBLE

Highlights of CP-4900 DMD CP-4900 DMD Analyzers Solutions Turnkey Solution for a specific application field Fully integrated into the CP-4900 Micro-GC Using µ-DMD (Micro Differential Mobility Detector) High sensitivity < 100 ppb detection limit Unique selectivity No interference with sample matrix Detect components even when they are co-eluting

Sensitivity CP-4900 DMD < 100ppb Sensitivity of CP-4900 DMD Sensitivity CP-4900 DMD < 100ppb 1 2 3 4 5 6 7 Hexane vapor as sample matrix. µ-DMD signal 1. Iso-propyl mercaptan 2. Tert-butyl mercaptan 3. Sec-butyl mercaptan 4. N-propyl mercaptan 5. Iso-butyl mercaptan 6. N-butyl mercaptan 7. Tert-amyl mercaptan +/- 100ppb each! µ-TCD signal

Selectivity of CP-4900 DMD Selectivity CP-4900 DMD No interference with sample matrix Methyl- and Ethyl Acrylate in a natural gas 1. Methylacrylate, 1.8 ppm 2. Ehtylacrylate, 2.5 ppm 1 2 C6-hydrocarbons µ-DMD signal µ-TCD signal

Principle of operation µ-DMD Micro-Differential Mobility Detector (µ-DMD) CP-4900 DMD, a joint developed by Varian, Inc. and Sionex Corporation, using Sionex's patented microDMXTM technology.

Principle of operation µ-DMD µ-DMD coupling µ-DMD serial connected, via heated transfer line,with µ-TCD

Principle of operation µ-DMD Ionization Component from µ-TCD are ionized Tunable ion filter Selective transmission of Components of interest, others are neutralized and hence not detected, they will pass through filter Detection Both positive and negative species are detected

Principle of operation µ-DMD The micro-Differential Mobility Detector (µ-DMD) is a tunable ion filter Detector Selectivity is gained by: Degree of ionization Filter per component Mobility of the ion Vc or compensation voltage, RF- voltage Detection Positive and negative ions Detector selectivity is additional to chromatographic selectivity

Principle of operation µ-DMD 1. Ionization step Ionization Source: Ni63 The effluent from the capillary column is ionized by supported by the beta-radiation emission of Ni63. Alternative ionization sources are under development: UV, Corona discharge (plasma ionization). One could consider discharge as a promising technique

Principle of operation µ-DMD 2. Entry ion filter by using Zero air or Nitrogen as drift gas Ionisation Source: Ni63 The Differential Mobility Detector (DMD) is a tunable ion filter, which selects the ion species allowed to pass through the filter by adjusting the voltage, applied between the ion filter electrodes (the drift-tube). The filtering mechanism is governed by the interaction between the ion and the net applied field that alternates between high and low electric field strength. The differential mobility detector is capable to isolate specific components or functionality’s out of a complex matrix. Apart from selective, the DMD is very sensitive.

Principle of operation µ-DMD 3. Various transmissions in the tunable ion filter Degree of ionization Mobility of the ion Voltage on electrode The drift tube is composed of two parallel plates, 500 micron apart fron each other; length is about 2 cm. As the ions move through the ion filter, a R(adio) F(requency) modulated voltage is applied over the plates the result is that the ions make a zig-zag movement between the plates. The ions that hit one of the plates, nett movement upwards or downwards, are neutralized and are swept out of the system. Those ions that have a nett axial movement equal 0 will pass through the plates towards a detector.

Principle of operation µ-DMD 4. Detection of positive and negative ions At the end of the drift tube, or ion filter the ions move towards the faraday detectors. There is one for positive ions and one for negative ions. Simultaneously two signals are processed. The information content is high compared to the standard gas chromatography detectors like tcd, fid etc.

Principle of operation µ-DMD Differential Mobility Spectroscopy Tunable ion filter, which selects the the ion species allowed to pass through the filter The filtering mechanism is governed by the interaction between the ion and the net applied field that alternates between the high and low electric field strength Ions which do not pass through the filter are neutralised Both positive and negative ions are detected

Summary CP-4900 DMD Markets

Trouble shooting on DMD Driftgas flow incorrect Noise problems on DMD Noise problems on CP-4900 Sensitivity problems Communication problems Flow controller check valve check for leakage DMD channel Interconnection board check driftgas pressure Check quality driftgas Adsorption of the component RS232 cable Expert Lite

DMD Channel transfer line Noise testing Cap the DMD off or remove the complete channel

DMD channel Each components 11 ppm 10m Porabound Q H2S:2015 COS:2683 CH3SH:2212 Each components 11 ppm DMD Channel: H2S:222486 COS:206760 CH3SH:366515

Loss of sensitivity What to check??? 1) Type and quality driftgas 2) Quality of the calibration mix 3) Tuning DMD

Heated transfer line

CP-4900 heated transfer line Take care when installing the heated transfer line over the TCD capillary

Expert Lite V2.0 Adjust Vc default after tuning Only adjust step size

IAR Generated Binar (*.a43) Upgrade for Sensor board Boot loader software IAR Generated Binar (*.a43) Upgrade for Sensor board Motorola S record(*.s) Upgrade for UI board

Boot loader software

Info on Sionex software Boot loader software 1) Upgrade software on User Interface board (UI board) 2) Upgrade software on Sensor board 1) Expert Lite info on UI and Sensor firmware