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

Mar 30, 2015

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Joelle Gandy
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Page 1: Hardware CP-4900 DMD µ-DMD fully integrated into CP-4900 Micro-GC hardware µ-DMD serial connected, via heated transfer line,(inert) with µ-TCD (modified)

Hardware CP-4900 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

µ-DMD

Micro-GC channel with µ-TCD

Page 2: Hardware CP-4900 DMD µ-DMD fully integrated into CP-4900 Micro-GC hardware µ-DMD serial connected, via heated transfer line,(inert) with µ-TCD (modified)

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

Page 3: Hardware CP-4900 DMD µ-DMD fully integrated into CP-4900 Micro-GC hardware µ-DMD serial connected, via heated transfer line,(inert) with µ-TCD (modified)

DMD Channel

Flow controller

Check valve

Driftgas

Zero Air or N2

Main board and

UI board

Sensor board

Ni63 source

Page 4: Hardware CP-4900 DMD µ-DMD fully integrated into CP-4900 Micro-GC hardware µ-DMD serial connected, via heated transfer line,(inert) with µ-TCD (modified)

Hardware CP-4900 DMD

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

Page 5: Hardware CP-4900 DMD µ-DMD fully integrated into CP-4900 Micro-GC hardware µ-DMD serial connected, via heated transfer line,(inert) with µ-TCD (modified)

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

Page 6: Hardware CP-4900 DMD µ-DMD fully integrated into CP-4900 Micro-GC hardware µ-DMD serial connected, via heated transfer line,(inert) with µ-TCD (modified)

Sensitivity of CP-4900 DMD

1. Iso-propyl mercaptan2. Tert-butyl mercaptan3. Sec-butyl mercaptan4. N-propyl mercaptan5. Iso-butyl mercaptan6. N-butyl mercaptan7. Tert-amyl mercaptan

+/- 100ppb each!

1

2

3

45 6 7

Hexane vapor as sample matrix.

µ-TCD signal

µ-DMD signal

Sensitivity CP-4900 DMD < 100ppb

Page 7: Hardware CP-4900 DMD µ-DMD fully integrated into CP-4900 Micro-GC hardware µ-DMD serial connected, via heated transfer line,(inert) with µ-TCD (modified)

Selectivity of CP-4900 DMD

Selectivity CP-4900 DMD

No interference with sample matrix

1

2

C6-hydrocarbons

µ-DMD signal

µ-TCD signal

Methyl- and Ethyl Acrylate in a natural gas 1. Methylacrylate, 1.8 ppm2. Ehtylacrylate, 2.5 ppm

Page 8: Hardware CP-4900 DMD µ-DMD fully integrated into CP-4900 Micro-GC hardware µ-DMD serial connected, via heated transfer line,(inert) with µ-TCD (modified)

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.

Page 9: Hardware CP-4900 DMD µ-DMD fully integrated into CP-4900 Micro-GC hardware µ-DMD serial connected, via heated transfer line,(inert) with µ-TCD (modified)

Principle of operation µ-DMD

µ-DMD coupling

µ-DMD serial connected, via heated transfer line,with µ-TCD

Page 10: Hardware CP-4900 DMD µ-DMD fully integrated into CP-4900 Micro-GC hardware µ-DMD serial connected, via heated transfer line,(inert) with µ-TCD (modified)

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

Page 11: Hardware CP-4900 DMD µ-DMD fully integrated into CP-4900 Micro-GC hardware µ-DMD serial connected, via heated transfer line,(inert) with µ-TCD (modified)

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

Page 12: Hardware CP-4900 DMD µ-DMD fully integrated into CP-4900 Micro-GC hardware µ-DMD serial connected, via heated transfer line,(inert) with µ-TCD (modified)

Principle of operation µ-DMD

Ionization Source: Ni63

1. Ionization step

Page 13: Hardware CP-4900 DMD µ-DMD fully integrated into CP-4900 Micro-GC hardware µ-DMD serial connected, via heated transfer line,(inert) with µ-TCD (modified)

Principle of operation µ-DMD

Ionisation Source: Ni63

2. Entry ion filter by using Zero air or Nitrogen as drift gas

Page 14: Hardware CP-4900 DMD µ-DMD fully integrated into CP-4900 Micro-GC hardware µ-DMD serial connected, via heated transfer line,(inert) with µ-TCD (modified)

Principle of operation µ-DMD

3. Various transmissions in the tunable ion filter Degree of ionization Mobility of the ion Voltage on electrode

Page 15: Hardware CP-4900 DMD µ-DMD fully integrated into CP-4900 Micro-GC hardware µ-DMD serial connected, via heated transfer line,(inert) with µ-TCD (modified)

Principle of operation µ-DMD

4. Detection of positive and negative ions

Page 16: Hardware CP-4900 DMD µ-DMD fully integrated into CP-4900 Micro-GC hardware µ-DMD serial connected, via heated transfer line,(inert) with µ-TCD (modified)

Principle of operation µ-DMD

Both positive and negative ions are detected

Differential Mobility Spectroscopy

Page 17: Hardware CP-4900 DMD µ-DMD fully integrated into CP-4900 Micro-GC hardware µ-DMD serial connected, via heated transfer line,(inert) with µ-TCD (modified)

Summary CP-4900 DMD Markets

no Analyzer Application Detection Limit DMD Why Markets1 Sulfur odorants in

Natural GasTHTTBMMES

0.5 mg/m3 (100 ppb)

2 Sulfur-free odorants inNatural Gas

Methyl Acrylate

Ethyl Acrylate

0.35 mg/m3 (100 ppb)0.45 mg/m3 (100 ppb)

SafetyEnvironmental

Gas transportationGas DistributionCity gatesFuel cellsCatalysts

3 Anesthetic gases in air HalotaneEnfluraneIsofluraneDesfluraneSevoflurane

<100 ppb Safety Operating TheatersAnesthetic gascompaniesRecovery rooms

4 Sulfur hydrocarbons inHC matrices

Hydrogen SulfideCarbonyl sulfideMethyl Mercaptan

200 ppb

5 Mercaptanes C1-C4 ingas

Methyl MercaptanEthyl MercaptanI-Propyl Mercaptann-Propyl MercaptanTBM, tert-Butyl Mercaptan

<100 ppb

SafetyEnvironmentalCorrosion

Petro-chemicalprocessesCatalystsFuel cellsDe-sulfurisationcompanies

6 CFC’s & HCFC’s in air For exampleCFC-11CFC-12CFC-113CFC-114CFC-115

100 ppb SafetyEnvironmental

Personal monitoringEnvironmentalcompaniesEmission controlcompaniesCFC & HCFCProducers

Page 18: Hardware CP-4900 DMD µ-DMD fully integrated into CP-4900 Micro-GC hardware µ-DMD serial connected, via heated transfer line,(inert) with µ-TCD (modified)

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

Flow controller

DMD channel

Interconnection board

check driftgas pressure

Check quality driftgas

Adsorption of the component

RS232 cable

Interconnection board

Expert Lite

Page 19: Hardware CP-4900 DMD µ-DMD fully integrated into CP-4900 Micro-GC hardware µ-DMD serial connected, via heated transfer line,(inert) with µ-TCD (modified)

DMD Channel transfer line

Noise testing

Cap the DMD off or remove the complete

channel

Page 20: Hardware CP-4900 DMD µ-DMD fully integrated into CP-4900 Micro-GC hardware µ-DMD serial connected, via heated transfer line,(inert) with µ-TCD (modified)

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

Page 21: Hardware CP-4900 DMD µ-DMD fully integrated into CP-4900 Micro-GC hardware µ-DMD serial connected, via heated transfer line,(inert) with µ-TCD (modified)

Loss of sensitivity

What to check???

1) Type and quality driftgas

2) Quality of the calibration mix

3) Tuning DMD

Page 22: Hardware CP-4900 DMD µ-DMD fully integrated into CP-4900 Micro-GC hardware µ-DMD serial connected, via heated transfer line,(inert) with µ-TCD (modified)

Heated transfer line

Page 23: Hardware CP-4900 DMD µ-DMD fully integrated into CP-4900 Micro-GC hardware µ-DMD serial connected, via heated transfer line,(inert) with µ-TCD (modified)

CP-4900 heated transfer line

Take care when installing the heated transfer line over the

TCD capillary

Page 24: Hardware CP-4900 DMD µ-DMD fully integrated into CP-4900 Micro-GC hardware µ-DMD serial connected, via heated transfer line,(inert) with µ-TCD (modified)

Expert Lite V2.0

Only adjust

step size

Adjust Vc default

after tuning

Page 25: Hardware CP-4900 DMD µ-DMD fully integrated into CP-4900 Micro-GC hardware µ-DMD serial connected, via heated transfer line,(inert) with µ-TCD (modified)

Boot loader software

Motorola S record(*.s)

Upgrade for UI board

IAR Generated Binar (*.a43)

Upgrade for Sensor board

Page 26: Hardware CP-4900 DMD µ-DMD fully integrated into CP-4900 Micro-GC hardware µ-DMD serial connected, via heated transfer line,(inert) with µ-TCD (modified)

Boot loader software

Page 27: Hardware CP-4900 DMD µ-DMD fully integrated into CP-4900 Micro-GC hardware µ-DMD serial connected, via heated transfer line,(inert) with µ-TCD (modified)

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