The picospin-45 NMR Spectrometer A Breakthrough in Chemical Spectroscopy Center for Process Analysis and Control NeSSI Meeting Seattle, WA

Transcription

1 The picospin-45 NMR Spectrometer A Breakthrough in Chemical Spectroscopy Center for Process Analysis and Control NeSSI Meeting Seattle, WA picospin, LLC Jeffrey W. Sherman, Ph.D. November 6 th, 2012 picospin LLC, 5445 Conestoga Ct., Boulder CO USA

2 Outline Introduction/Review to FT-NMR picospin-45 Features Key Applications for Miniature NMR Spectrometers Demonstration

3 YES Frequency Resolution? NO Scope of NMR from 1946 to the Present NO Spatial Resolution? YES 1946: Bloch, Hansen, Packard, water at 10 MHz 1973: Lauterbur, 1mm dia. water tubes at 60 MHz Purcell, Torrey, Pound paraffin at 30 MHz Nothing early 1951: Arnold, Dharmatti, Packard ethanol at 32 MHz

4 YES Frequency Resolution? NO Scope of NMR from 1946 to the Present NO Spatial Resolution? YES Now: TD NMR, oil content in seed crops Now: Functional MRI of the human brain Now: Structure of bio-molecules by multidimension multi-nuclear NMR spectroscopy Now: MRI spectroscopy of the human brain

5 NMR Spectrometers from 1951 to the Present 1954: J.S. Waugh, Caltech 1951: H. Pfeifer, Leipzig

6 NMR Spectrometers from 1951 to the Present Magnet No Credit Cards 1952: Varian HR-30, J. Schoolery and V. Royden First commercial applications lab

7 NMR Spectrometers Available Today Varian 900 MHz ¼ Scale Bruker 400 MHz AVANCE III Qualion 60 MHz Refinery Analyzer Anasazi Aii 60 MHz picospin 45 MHz (to scale)

8 Why NMR Spectroscopy? picospin-45 ethyl acetate spectrum Most powerful analytical method in organic chemistry Identifies chemical groups Yields quantitative concentration ratios Reveals structure

9 Why NMR Spectroscopy? picospin-45 ethyl acetate spectrum Most powerful analytical method in organic chemistry Identifies chemical groups Yields quantitative concentration ratios Reveals structure

10 Introduction to NMR Coil Transmit

11 Introduction to NMR Coil ethanol frequency NMR Receive Spectrum

12 Typical 1H NMR Spectra 12

13 Why now? 1984: Nd 2 Fe 14 B magnets 1990s: Microcoil NMR experiments by A.G. Webb et al., U. of Ill. 2000s: Advances in Rf (Tx and Rx) Electronics (Mobile Phones) Radiofrequency Electronics Micro Coil Technology Magnetic Materials

14 Inside the Cartridge Channel A microcoil 0.3 mm ID quartz capillary PTFE transition

15 Capillary cartridge, magnet, preamplfier

16 Inside the Box Embedded web server Data converters, DSP Pulse sequencer Rx and Tx amplifiers Shim coil controller RF preamplifiers Permanent magnet Magnet temperature controller Fluid cartridge and sub-panel

17 picospin-45 Features 45 MHz Pulsed FT NMR spectrometer Proton NMR of liquids; 19 F version 40 ppb typical resolution Single-shot SNR for water lbs total weight; 7 x 5.75 x 11.5 Replaceable 300 µm ID capillary cartridge 20 µl sample volume Controlled by any web browser No cryogens, no compressed gas, etc. No special environment All solid-state, no moving parts Minimal maintenance

18 Key Markets and Applications

19 Mobile Applications - Having fun yet? NASA Zero-G Experiments

20 Mobile Applications - Having fun yet?

21 picospin-45 Applications: Chemical Education Prof. Steve Bertman, Western Michigan University

22 picospin-45 Applications: Chemical Education

23 picospin-45 Applications: Chemical Education

24 Educational Materials Outreach Development Sarah Dimick Gray Metropolitan State University, St. Paul, MN Goals: Our goal will be to provide picospin with written lab procedures, tested by undergraduates and ready to post online, of experiments utilizing the picospin NMR, accompanied by sample spectra. We will expect to publish our results in J. Chem. Ed. and present the results in the ACS Undergraduate Poster Session in the Spring National Meeting possibly accompanied by a 20 minute talk. Labs Isolation Essential Oil of Cloves, Eugenol or Cinnamon Separation of Two Solvents by Distillation Dehydration of Cyclohexanol to Cyclohexene Green(er) Oxidation of Menthol to Menthone Outcome Synthesis by Amidation of DEET 3-4 Written lab procedures Bromination of a Cycloalkene Student tested (Cyclopentene/Cyclohexene) Posted in the public domain Oxidation of a Primary/Secondary/Tertiary alcohol Publish in J. Chem. Ed. Present at ACS Undergraduate poster session Spring National meeting 2013 Professor presentation - 20 minute Anticipated late Summer 2012

25 High-Field NMR Spectroscopy Centers Teaching, Supplement to High-Field Capabilities, etc.

26 picospin-45 Applications: Reaction Monitoring Specialty Chemicals, Polymers, Biofuels, Cosmetics

27 picospin-45 Applications: QA/QC Specialty Chemicals, Polymers, Biofuels, Cosmetics

28 Mobile Applications Forensics, Military, First Responders, Regulatory, etc.

29 picospin-45 Applications: Mobile Laboratory Example

30 Sample Spectra Fuels Pharmaceuticals Essential Oils Regioisomers Reaction Monitoring Heteronuclear Coupling Horticulture Extracts 19 F NMR Temperature Measurement

31 picospin-45 Demonstration

32 picospin-45 Sample Spectra

33 Essential Oils

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42 19 F NMR & 13 C Satellites

43 picospin-45 Fluorine ( 19 F) NMR Back

44 picospin-45 Fluorine ( 19 F) NMR Back

45 Fuels, (Conventional and Bio) Gasoline Fatty Acids Methyl Esters (FAME)

46 Conventional 85 Octane Gasoline Enriched with up to 10% Ethanol Back

47 Gasoline Sample (red) 1:1 Ethanol:Gasoline (blue) Back

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52 Pharmaceuticals

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56 Horticulture/Extracts/Perfumes

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65 Reaction Monitoring: Transesterification Ethyl Acetate Methanol Methyl Acetate Ethanol

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69 In situ monitoring Back

70 Solutions: Acetone in MeOH [ ] Hemiacetal Acetal

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73 picospin-45 Demonstration