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COMPOSITION ? (QUALITATIVE ANALYSIS) HOW MUCH ? (QUANTITATIVE ANALYSIS) WHAT FORM ? (SPECIATION)

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Presentation on theme: "COMPOSITION ? (QUALITATIVE ANALYSIS) HOW MUCH ? (QUANTITATIVE ANALYSIS) WHAT FORM ? (SPECIATION)"— Presentation transcript:

1 COMPOSITION ? (QUALITATIVE ANALYSIS) HOW MUCH ? (QUANTITATIVE ANALYSIS) WHAT FORM ? (SPECIATION)

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3 Mass Spectrometry Topic I

4 Present Detector Technology – Faraday Cups Gain is stable and precisely known (gain=1)Gain is stable and precisely known (gain=1) Bandwidth is consistent with use in sector-based mass spectrometryBandwidth is consistent with use in sector-based mass spectrometry Useful for I ion  10 -15 amp (1 ion/sec  1.6  10 -19 amps)Useful for I ion  10 -15 amp (1 ion/sec  1.6  10 -19 amps) Implies that one needs about 6250 ions/sec for detection by Faraday cupImplies that one needs about 6250 ions/sec for detection by Faraday cup Faraday Cage Collector Electrode Load Resistor Out to amplifier

5 “FARADAY ELECTRODE” output High Z

6 Electron Multiplier Detector Secondary Electrons Incident Ion

7 Electron Multiplier Detector Detection Efficiency Mass (m/z) 0 Electron multiplier has a gain that is dependent upon the mass or kinetic energy of the incoming ion.

8 Electron Multiplier Detector Detection Efficiency (%) Energy (eV) 0 100 80 60 40 20 10 10 4 10 3 10 2

9 - h e PtSi Photoactive Layer Silicon Multiplexer Focal Plane Array Individual preamps for each pixel In bump bonds

10 “FARADAY CUP” RESET 36 f F MUX 4.4  V / e --  20 e -- read noise @ 77 K

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12 Ion Source Electrostatic Sector Magnetic Sector Array Detector on Focal Plane - + Mattauch-Herzog Mass Spectrometer Geometry

13 Design Specifications Noise - 5 electrons read noise (highest gain) 39.6 microvolts / electron (highest gain) Well size - 80,000 e to 16,000,000 e 50 micron pitch Read rate - 1 mega sample per second into 30pfd &10kohm Nondestructive / Destructive Readout

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15 “FARADAY ELECTRODE” RESET 10 f MUX 990 f Gain F F

16 Detection Limit 8 IONS ! & we are still optimizing it !! Keep tuned 2.5 electrons of read noise with NDRO

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18 CMS 35 lbs. 75 watts GC, Pumps Mass spec. etc.

19 Ion Mobility Spectrometry Ion Mobility Spectrometer IMS is a technique that is being employed to solve problems where portable instrumentation and ruggedness is necessary 1 New Instruments Demand Lower Detection Limits 2 Must Operate through a Wide Range of Temperatures 3 Must Operate at Atmospheric Pressure 4 High S/N Ratio 1 New Instruments Demand Lower Detection Limits 2 Must Operate through a Wide Range of Temperatures 3 Must Operate at Atmospheric Pressure 4 High S/N Ratio Applications Using Ion Mobility Spectrometers Field-Portable detection of chemical warfare agents Detection of explosives, nerve agents, toxins, and other hazardous chemicals at safety inspection stations and in the environment Structural conformation studies of proteins, polymers, and various other molecules

20 Ion Mobility Spectrometer Ionization Chamber Drift Region Drift Rings Gas Inlet Gas Outlet -- Electric Field Ion Shutter Faraday Plate Drift Gas Inlet

21 Chemical Identification Based Upon Ion Mobility

22 Relationship of Ion Mobility to Molecular Terms 3 16 e N 1 m 1 M + 2 k  T 1 +   r 2    K =K = Drift Velocity: v d = K E Mobility: K = d t d E EElectric Field Strength t d Drift Time mIon Mass (analyte) NNumber Density TTemperature  Collision Integral dDrift Path Length eUnit Charge MMolecular Mass (drift gas) kBoltzmann-Constant rMinimum in Potential Curve  Correction Term

23 “FARADAY ELECTRODE” output High Z

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25 “FARADAY ELECTRODE” RESET 8 f F MUX

26 New interlocking 8 ring microIMS

27 25pg TNT -1825VDC Emco PS, 90C 100/50 ml/min Cl-/Air Filament, inj 125C. Filters OFF Resolution 84. Run a baseline noise 0.005 S/N=30 Detection Limit = 2.5 pg 1-31-05

28 5pg TNT 95 o C 25V Injector Block 0.85A Filament, 1200 us Pulse B.C. FIRW on ( 0.9 pg Det. Lmt.)

29 8in. 18 in. 12 in. Proposed Vehicle Based IMS

30 Time (ms) Intensity (ADU) e - peak 47 attograms in single sweep RDX Detection Limit = 5 attograms RDX

31 Conclusions CTIA is ideal for IMS –Fast (1 MHz or higher per pixel) –Low read noise –1000 x sensitivity improvement over current micro-IMS device. –Expect further improvement with differential devices and cooling. –Don’t need low secondary electron yield coatings or exotic geometries for IMS.

32 Conclusions CTIA is ideal for IMS –Fast (1 MHz or higher per pixel) –Low read noise –1000 x 10,000 x sensitivity improvement over current micro-IMS device. –Expect further improvement with differential devices and cooling. –Don’t need low secondary electron yield coatings or exotic geometries for IMS.

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35 Miniature Optical Bench 14mm How do you make an optical bench that is just 14mm long?

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41 Axsun’s Handheld Substance ID Solutions Raman Handheld Substance Identifier Concept Raman Probe TEC High Power Laser Diode TEC Spectrometer Battery Fiber Optics

42 Raman Spectral Range Dependence on Excitation Excitation 246nm Raman Shift (cm -1 ) 200040000 270.4nm256.5nm244.0nm 488.0nm 785.0nm 540.8nm 931.2nm 606.4nm 1144.3nm 224.3nm 980nm1225nm1450nm

43 900-1700 nm is critical “molecular fingerprint” region for scientific research and analysis of food, pharmaceutical, chemical, and plastic products. Ideal NIR sensor will have high QE between 900-1700 nm, high sensitivity, high dynamic range. NIR Spectroscopy/Imaging With Focal Plane Arrays

44 Photon-Processor™ Extreme Low Light Level Digital Video Imager Low Cost Patented Technology Camera Electronics On-chip Day/Night Operation SXGA (1024 X 1280) Resolution Low Power <600 Mw @ 3 VDC Photon-Processor™ Light Photoelectrons CMOS Imager Video Output Photocathode

45 Light Photoelectrons CMOS Imager Video Output Photocathode

46 Complete NIR Spectrometer Wavelength Reference Power Reference Amp DSP processor 24-bit A/D converters SLED source MEMS tunable filter PC and software Single element InGaAs detector Wired or wireless Spectrometer Sample Butterfly packages Probe or optics Blue lines are light, red are electrical

47 Reference Block Diagram WARM (Wavelength & Amplitude Reference Module) –Ultra stable beamsplitters tap off known quantities of light –Absolute wavelength reference provided by an integrated quartz etalon and a miniature acetylene gas cell that are temperature controlled to 0.1 o C –Amplitude reference provided by matched single element photodetectors that divide out responses from every point of a scan

48 WARM ( wave, amplitude- reference ) Module

49 Tunable laser spectrometer, in portable package With embedded PC and sample interface LCD Display Sample interface Tunable laser spectrometer


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