PANIC NMR Validation Group – Website, Meetings and Organization

Validation of NMR: No Need to PANIC - Workshop held February 13, 2015, La Jolla, CA, U.S.A In conjunction with the 3rd PANIC conference in La Jolla, California, a 1-day NMR validation workshop was held that attracted approximately 80 interested participants. The agenda of the meeting is provided at this link (http://www.nmrvalidation.org/index.php/events/event-review) and registered participants can now download the presentations presented at the meeting. At the meeting it was decided to proceed with the idea of founding an organization dedicated to the development of validate NMR methods for use throughout all industry sectors. Organizational Scope: NMR spectroscopy provides a means to evaluate material with high compound and high material specificity. Information as to the chemical structure, stereochemistry, quantity, material composition, and material identity is encoded in the NMR spectrum. The high reproducibility of NMR spectroscopy from instrument to instrument and lab to lab makes NMR an excellent tool for material validation. Approaches to utilizing NMR as a material validation tool include using (1) targeted approaches, the identification and quantification of specific components, and (2) non-targeted approaches, the use of chemometric methods to evaluate the spectrum as a whole. Efforts to increase the number and the speed of validated NMR methods…

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Polyalphaolefin Hydrogenation – Residual Olefin Analysis – 1H NMR versus Bromine Number

1H NMR is an excellent tool for monitoring the residual olefin content of polymers after hydrogenation reactions. The fact that the olefin fall in a unique region of the spectrum means that it is a straightforward measurement to quantify the %H present as olefin or to correlate that olefin content with other analyses such as bromine number. Here is an example of a polyalphaolefin residual olefin analysis. The olefin proton content (%H) was plotted against bromine number values obtained on each of the samples. A linear correlation was obtain but two different correlations were observed that were dependent on the viscosity index of the polyalphaolefin being analyzed. Figure 1 shows the 1H NMR spectra obtained on neat samples on a Picospin-80 spectrometer operating at 82.3 MHz. The methyl and methlene protons of the polymer backbone are plainly seen and the olefin and alpha-olefin protons are observed.   Figure 2 shows the linear correlation between %H olefin and bromine number with the two correlations caused by different VI grade being indicated. The analysis shows that for the two viscosity grades the grade can be identified from the linear correlation that the data falls onto and the %H olefins content can directly…

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Residual Catalytic Cracker – Heavy Petroleum Feedstream Properties from 1H NMR at 43 MHz

Back in October we presented a talk at Gulf Coast Conference that concerned the prediction of the chemical and physical properties of heavy petroleum feeds being converted to higher value product in a residual catalytic cracker (RCC). Over the years we have analyzed these materials by 300 and 60 MHz NMR and obtained good PLS-regression models that can adequately predict properties for real-time process control and optimization in a petroleum refinery. With the advent of a large number of new benchtop NMR systems we have been convincing ourselves that these types of analyses can be performed by systems such as the Magritek Spinsolve 43 MHz. We ran a series of samples that had been sitting around our lab for 15 years by dissolving them at about 50 volume% in a 50/50 CDCl3/CS2 solvent system. For each sample we had laboratory test data for a number of chemical and physical properties of interest to process engineers. We regressed the lab data variability against the variability in the Magritek 43MHz 1H NMR spectra and obtained cross-validated PLS models. The presentation material is given here at this link - Gulf Conference Presentation - 43 MHz RCC Feedstream Regression Models

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From Atoms to Flavour: The Chemistry of Beer

Adam DiCaprio (ex PNA) gave an excellent Science Cafe Talk under the auspices of the ACS North Carolina Section at the Busy Bee Cafe in downtown Raleigh on December 2, 2014. CHanging gears from his previous talks he centered the discussion on malt and hop chemistry as well as an start-to-finish NMR analysis of production runs of a bottled commercial tavern ale. If you are interested in having Adam give a detailed chemistry seminar on beer at your section meetings please contact him directly at adam@process-nmr.com. A PDF version of his talk is available here .... ACS Science Cafe Talk - Dicaprio - Busy Bee Cafe - Raleigh NC - 12-2-14

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Comparison of 1H NMR Spectra Obtained at 42, 60, 82, and 300 MHz – Fish Oil Omega-3 Ethyl Ester Supplement Example

Process NMR Associates is currently developing NMR applications based on direct measurement of chemometric modeling on NMR data obtained on numerous NMR platforms. Our intention is to develop solutions that can be executed on any NMR platform. With this in mind we are currently developing a fish oil analysis application that can provide the EPA and DHA omega-3 fatty acid content of fish oil supplements manufactured by an ethyl ester esterification process. We have obtained data at 42 MHz, 60 MHz, 82 MHz and 300 MHz. The chemometric modelling yielded PLS models for all 4 field strengths that yield effectively the same result - DHA can be measured to +/- ~1.1 wt% and EPA can be measured to +/- ~2.2 wt% by a 40 second 1H NMR measurement. THe correlation is derived from a  regression of the 1H NMR variability with primary GC analysis values. This analysis has been shown for the 300 and 60 MHz data in a previous post on this blog. The same analysis was also obtained, with similar results, on 42 and 82 MHz platforms proving that individual applications can be automated and provided at all relevant frequencies of NMR analysis whether on superconducting lab systems or permanent…

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Presentations at SMASH 2014

"Beer Manufacturing and Analysis by NMR", John C. Edwards and Adam Dicaprio, Presented at the Mestrelab MNova Users, Meeting - SMASH, Atlanta, GA, September 7, 2014 Get PDF Here “Survey of Low Field NMR Spectrometer Platforms for Successful Screening of Sexual Enhancement and Weight Loss Supplements for Adulteration with Drugs and Drug Analogs", John C. Edwards, Kristie Adams, Anton Bzhelyansky , Presented at SMASH Conference, Atlanta, GA, September 7-10, 2014. Get PDF Here

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John Edwards to be Guest Editor of 2 Special Issues of Magnetic Resonance in Chemistry Dedicated to Benchtop NMR

I have been invited to be a guest editor for Wiley publishing to pull together 2 special issues of Magnetic Resonance in Chemistry. I am putting out a general “call for papers” but I will harass people personally. We are looking for 10-20 papers for each issue. The deadline for submission of the papers is June 30 so no-one has an excuse that there isn't enough time. I do ask that you email me at the contact below to let me know that you are thinking of submitting and a title would be nice also (though I won't hold you to it). We hope to have the review and revide papers (if necessary) by late October and then publish by December 2014. The first will be on high resolution benchtop NMR in which I would like to include all permanent magnet systems capable of obtaining a spectrum. This is an open invitation to all the vendors and their customers of (in no particular order) Anasazi, Nanalysis, One Resonance Sensors, Magritek/ACT, Aspect, Qualion, Picospin, Resonance Systems, Oxford Instruments, Bruker, home built devices, I would also make the exception that HTS systems be included as they are also cryogen free. Any papers…

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Special Issue on Benchtop NMR systems in Wiley Journal “Magnetic Resonance in Chemistry” – please consider submitting a technical or review paper

I was just asked by Roberto Gil (Carnegie Mellon) to pull together a special issue if Magnetic Resonance in Chemistry" on the topic of Benchtop NMR. I will personally be hitting up everyone I know who is working in this area to provide technical papers on their work in this area. I also wanted to extend an invitation to the members of this group to submit a paper for this special issue. All topics will be considered but I would like to stay away from "traditional" 1H TD-NMR and restrict 1H TD-NMR applications to new approaches. On the high resolution side (45, 60, 80 MHz) I am hoping that applications with some real meat might be submitted rather than brochure type papers with just spectra of solvents and small molecules. Please feel free to contact me directly if you have ideas on submissions. My contact information is listed below. Sincerely, -- John C. Edwards, Ph.D. Manager, Process and Analytical NMR Services Process NMR Associates, LLC 87A Sand Pit Rd, Danbury, CT 06810, USA Tel: +1 (203) 744-5905 Cell: +1 (203) 241-0143 Skype: jcepna e-mail: john@process-nmr.com

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Register to Attend PANIC 2014 ! Deadline for Poster Submissions is December 20

The 2nd Annual Practical Applications of NMR in Industry Conference (PANIC) will be held February 3-5 in Charlotte, NC. An excellent scientific agenda has been put together (see here). The Brochure is available here. Take note of the early registration (January 10, 2014) and poster submission (December 20, 2013) deadlines. John Edwards of Process NMR Associates is on the organizing committee of PANIC and has been appointed as Treasurer of the Conference company. John will be presenting an oral presentation in the one of the Nutraceutical Session:                NMR-Based Authentication of Nutraceuticals, Herbal Supplements, and Food Additives: Economic- and Efficacy-Driven Adulteration of Aloe Vera, Herbal Erectile Dysfunction Supplements, and Acacia Gum                                                                                                 John Edwards, Ph.D., Process NMR Associates, LLC - Biography Multinuclear NMR spectroscopy offers an outstanding ability to perform targeted and non-targeted analysis of nutraceuticals, herbal supplements, and food additives. Economic adulteration of these materials with lower…

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MestreLab MNova Users Meeting – SMASH 2013 – PNA NMR Presentation

"Utilization of MNova in a Commercial NMR Testing Laboratory for: 1) Development of Automated Quantitative Analysis Methods by Direct Internal Standard NMR Measurements, and 2) Pre-Processing of Large NMR Datasets for Chemometric Regression Analyses to Derive Chemical and Physical Properties" - presented by John Edwards at the MNova Users Meeting - SMASH 2013 - Santiago de Compostela, Spain, September 22, 2013 PDF of Presentation Automated 1H qNMR analysis of complex mixtures - example of aloe vera powder 200x Final automated analysis output for aloe vera analysis - assignments and quantitative output. Chemometric analysis - spectrum processing and X-matrix preparation performed in MNova - ascii output imported into Eigenvector Research Solo for PLS regression or PCA analysis. Correlation of 1H NMR at 300 or 60 MHz with GC analysis of EPA and DHA content (wt%).  

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NMR Studies of Spontaneously Fermented Sour Beers

At the recent ACS NERM 2013 meeting Adam Dicaprio of Process NMR Associates presented two topics on sour beer analysis by NMR. "Small Molecule Chemistry of Spontaneously Fermented Coolship Ales" ... PDF Technical Poster "When Beer Goes Sour: An NMR Investigation" ... PDF - Oral Presentation NMR Assignments of interest. 1H qNMR obtained from relative molar ratios established from compaison of maleic acid internal standard with small molecule signals.

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Comparison of 60 and 300 MHz 1H NMR Data – Prediction Models for EPA and DHA Omega-3 Fatty Acid Content

At the recent ACS NERM 2013 meeting in New Haven CT, John Edwards gave a talk on the comparison of 60 and 300 MHz 1H NMR based predictive models for EPA and DHA omega-3 fatty acid content in a fish oil manufacturing process. The presentation can be found here..... PDF Presentation Note - spectra are read into the chemometrics software backwards ...

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2nd Annual Practical Applications of NMR in Industry Conference (PANIC) Announced

Conference Details: 2nd Annual Practical Applications of NMR in Industry Conference Organized by Cambridge Healthtech Institute Hilton Charlotte University Place, Charlotte, NC, February 3-5, 2014 Building on the success of last years 1st Annual PANIC NMR Conference it has been decided that the 2nd Annual PANIC NMR Conference would be organized cooperatively between the original organizing committee and CHI. Details on the conference can be found at: PANIC Conference Website A promotional flyer for the conference can be found here: PANIC NMR Flyer Anyone interested in industrial applications of all forms of NMR spectroscopy is encouraged to attend this practical NMR conference where the emphasis is placed on everyday utilization of the technology rather than cutting edge NMR research which is often far beyond the capabilities of the everyday user. John Edwards of Process NMR Associates is serving on the organizing committee and chairing two technical sessions - one on On-Line/At-Line/Benchtop NMR and another on NMR of Materials. If you are interested in presenting or sponsoring the conference please contact CHI through the website.

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Process NMR Associates and Pfizer Present Joint Poster on Reaction Monitoring at PittCon

Pfizer has included the Aspect-60 MHz NMR system in their reaction monitoring investigations. The analysis was performed on reactions that were monitored in parallel by a Bruker 400 MHz NMR system. The poster of the initial results will be presented by Dr David Foley of Pfizer at this weeks PittCon in Philadelphia. The presentation is available here.

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SMASH Posters Cover Aloe Vera NMR Test Method, Heavy Petroleum Average Molecule Characterization, and 60 MHz Permanent Magnet NMR Applications

Quantitative 1H qNMR Method for Complex Mixture Analysis: Determination of Acetylated Polysaccharides, Glucose, Maltodextrin, Isocitrate, Preservatives, Additives and Degradation Products in Aloe Vera Leaf Juice - Raw Material and Consumer Products Practical Applications of Compact, Cryogen-Free High-Resolution 60 MHz Permanent Magnet NMR Systems for Reaction Monitoring and Online/At-Line Process Control Calculation of Average Molecular Descriptions of Heavy Petroleum Hydrocarbons by Combined Analysis by Quantitative 13C and DEPT-45 NMR Experiments

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Process NMR Associates to Contribute Invited Talk and 3 Posters at the 1st Practical Applications of NMR in Industry Conference (PANIC), October 15-17, Schaumburg IL

News - Dr. John Edwards of Process NMR Associates will be presenting the following 3 posters and invited talk at the 1st Practical Applications of NMR in Industry Conference (PANIC), Schaumburg, IL, October 15-17, 2012 Invited Talk On-line Applications of 60 MHz High-Resolution NMR Systems in Industry: Direct Measurements, Chemometric Correlations, and Multiple Spectroscopy Data Fusion John C. Edwards Process NMR Associates, LLC, Danbury, CT For the past two decades high resolution 1H NMR systems combined with chemometric analyses have been utilized in refineries and chemical plants to predict the chemical and physical properties of process streams and finished products. The ability to perform these analyses with on-line NMR instrumentation has allowed tighter control and optimization of the plant to obtain margin improvement, reduced reworking of off-specification materials, and higher yields of finished products. Examples of refinery and petrochemical applications will be given along with some examples of multinuclear NMR applications utilizing 31P and 19F NMR. The permanent magnet based 1.5 Tesla NMR instruments will be described along with a description of how these compact, cryogen-free NMR systems can be utilized on the bench-top or in the fume-hood as continuous or stop-flow chemistry sensors for reaction monitoring, mixing/dilution monitoring, or…

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Process NMR Associates to Present 3 Posters at SMASH NMR Conference, September 9-12, 2012

News - John Edwards of Process NMR Associates will be presenting the following 3 posters at SMASH NMR Conference, Providence RI, September 9-12, 2012. Process NMR Associates will also have a vendor table where John will be available to discuss the exciting range of high and low resolution permanent magnet NMR products available through the company and it's partners Aspect AI and Cosa-Xentaur. Poster 1 Quantitative Proton Nuclear Magnetic Resonance Spectrometry (1H-NMR) for Determination of Acetylated Polysaccharides, Glucose, Maltodextrin, and Isocitrate in Aloe Vera Leaf Juice John C. Edwards, Process NMR Associates, Danbury, Connecticut Aloe Vera is a botanical component that is used widely in the cosmetic, natural product, herbal supplement, and pharmaceutical industries. The widespread use of Aloe Vera has lead to the need to adequately analyze the authenticity, quality, and quantity of the various components present in this material. The qNMR method described here was developed and validated by Process NMR Associates (Danbury, CT) and is similar to an independently validated method developed by Jiao et al [1]. The method described is to be included in an upcoming Monograph on Aloe Vera published by the American Herbal Pharmacopoeia. The method can be used for the detection and quantitation…

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Process NMR (High, Mid and Low Resolution) Session at Practical Applications of NMR in Industry Conference

John Edwards (PNA) and Mark Zell (Pfizer) are co-chairs of a session of practical NMR applications in process control, reaction monitoring, miniaturized instrumentation, TD-NMR. John Edwards is also co-chairing a session (with Kathleen Farley of Pfizer) on quantitative NMR that contains an excellent talk on quantitative online NMR spectroscopy. Speakers in our sessions include: Session: On-Line/In-Line NMR and Time-Domain NMR Session Chairs: John Edwards, Process NMR Associates and Mark Zell, Pfizer, Inc. On-Line Applications of High-Resolution NMR in the Petroleum Industry - Direct Measurement, Chemometric Correlation, and Multiple Spectroscopy Data Fusion - John Edwards, Process NMR Associates, Danbury, CT USA Online NMR Reaction Monitoring in Pharmaceutical Process Development - David Foley, Pfizer Global Research and Development, Groton, CT USA Beyond Hammers in Search of Nails: An instrument technologist's perspective on developing miniaturized NMR spectrometers for new applications - Andrew McDowell, ABQMR, Inc., Albuquerque, NM USA LF-NMR Studies of Mechanically Induced Gel Syneresis in Cheese - Soren Engelsen, University of Copenhagen, Frederiksberg, Denmark NMR Quantification of Structural Features in Food Science and Technology - John van Duynhoven, Unilever – Vlaardingen, The Netherlands Rheological Measurements on Non-Newtonian Fluids Using a Process Compatible MRI - Michael McCarthy, University of California at Davis, Davis,…

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Newsflash: For Immediate Release – Process NMR Associates and Quantum Tessera Enter into Strategic Partnership

Process NMR Associates, LLC, Danbury, CT and Quantum Tessera Consulting, LLC, Collegeville, PA, USA Process NMR Associates, LLC (LLC) and Quantum Tessera Consulting, LLC are pleased to announce they have entered into a Strategic Partnership. This partnership will leverage PNA’s experience applying magnetic resonance techniques to such processes as reaction monitoring, active ingredient quality control, and the petroleum industry. PNA’s MR expertise extends into time-domain NMR, low field high resolution NMR (60MHz and 300MHz) applications, and chemometrics. Quantum Tessera brings its knowledge and experience about large molecule process development. Together, Process NMR Associates and Quantum Tessera can deliver higher value to clients process and manufacturing problems. Process NMR Associates and Quantum Tessera’s first project will be focused initially on NMR-based solutions for bioprocess monitoring and biofuel manufacture. Dr. John Edwards, Principal and Manager of Analytical Services at PNA comments, "The combination of Quantum Tessera Consulting and PNA will allow both companies to expand their customer base and allow them to offer a wider range of robust and innovative solutions to our clients.” Dr. Edward Zartler, CSO of Quantum Tessera, adds, “Process NMR associates has always led the field in NMR-based process analytics. This Strategic Partnership will result in synergies between…

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The Power of MestReNova Data Processing and Analysis Applied to 60 MHz 1H NMR Real Time Reaction Monitoring

The data analysis capabilities of the MestReNova NMR software makes processing and analyzing complex reaction mixture data a snap! Stacked plots are quick and easy and the integration routines rapidly process the peak areas into reaction profiles. Further steps allow the exponential fitting of the reaction profiles to yield kinetic information. Here are a few examples of the data visualization and rapid reaction profiling on a 60 MHz 1H NMR series obtained every 10 seconds (1 pulse) over the course of 25 minutes - the reaction is the esterification of tert-butanol with acetic anhydride in the presence of acid. Figure 1: Stacked Plot of the Aliphatic Region of the Spectrum with Reaction Chemistry Protons Identified Figure 2: Stacked Plot - Full Spectrum - Reaction Monitoring - 146 Spectra - 10 Seconds Apart Figure 3: Angled Stack Plot - Acetic Anhydride and tert-Butanol - Real Time Reaction Monitoring by 1H NMR at 60 MHz Figure 4: Stacked and Whitewashed Plot of 1H NMR data at 60 MHz - Real Time Reaction Monitoring of Acetic Anhydride with tert-Butanol Figure 5: Data Analysis Tool and production of reaction profiles. The MNova data analysis tools allow the user to integrate NMR reaction peaks and…

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Cryogen-Free NMR – High Resolution Permanent Magnet Systems – The Market Hots Up

It is interesting times in the world of NMR - there are a number of new permanent magnet NMR systems hitting the market. I have seen a number of announcements appearing on LinkedIn and other sites in recent days and then there was a question asked about Cryogen-free NMR systems on the AMMRL server. There is a little confusion out there about who is doing what and what these newer NMR systems are capable of. We (Process NMR Associates and Aspect Italia) have been in the market with a high resolution 60 MHz system (3, 5, or 10mm sample tube) since 1997. Anasazi Instruments have been quitely selling hundreds of 60 and 90 MHz FT-NMR systems based on refurbished or newly manufactured Varian EM-360 and EM-390. New to the scene and making a splash with their marketing campaigns are Picospin (300 micron sample tube, 45 Mhz), Nanalysis (3, 5mm sample tube, 60 MHz). Finally, there is a system from Magritek/ACT (5mm sample tube, 42.5 MHz) that has been re-packaged and is now out there in the world. These systems all produce spectra and can be used in the traditional manner that current supercon systems are utilized. Time-Domain (TD) NMR systems…

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1H NMR – 60 MHz Permanent Magnet System – Reaction Monitoring

Below are a few further examples of acetylation reactions of acetic anhydride with an excess of alcohol. The alcohols include tert-butanol and isopropanol. Reaction 1: Acetylation of t-butyl alcohol with acetic anhydride in the presence of acid. Reaction 2: Acetylation of Isopropanol with acetic anhydride in the presence of acid. Reaction 3: Methoxyacetone and hydroxylamine reaction in methanol to form an Oxime Resolution of the methylenes in the methoxyacetone and the reaction product is readily observed. All the above experiments were performed in an NMR tube. We are currently looking at the same reactions under flow conditions utilizing a HPLC pump and PEEK tubing to transport sample to the NMR probe at 5 ml/min.

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Chevron Installs Low Field NMR Application: 31P NMR Analysis of Phosphoric Acid Strength in Alkylation Process

New Flash: Chevron purchases high resolution 31P NMR system for at-line analysis of a phosphoric acid catalyzed alkylation process. The Chevron Richmond Refinery needed a simple and quick measurement of phosphoric acid strength and quality. Prior analysis procedures included transporting samples several miles from the refinery process to the technical center in order to perform the 31P NMR analysis on a high field superconducting NMR system. This process was also complicated by the fact that the process operators were not able to perform the analyses on the conventional high field NMR systems (400 MHz for 1H, 161 MHz for 31P) themselves, but had to wait for NMR technician and instrument availability. If sample analyses was required after research facility working hours the NMR lab technicians were required to come in and run the NMR for the process operators. A simple permanent magnet bench-top NMR system has now been placed in the existing process lab adjacent to the process unit control room. The NMR samples are placed in specially designed 9 mm (diameter) x 50 mm (length) sample tubes in order to accommodate sample handling issues (high viscosity sample with no solvents being added) and are place easily into the NMR…

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A Review of Applications of NMR Spectroscopy in the Petroleum Industry

John Edwards, principal of Process NMR Associates has authored a chapter entitled "A Review of Applications of NMR Spectroscopy in the Petroleum Industry" which appears in a new ASTM publication: Monograph 9 - Spectroscopic Analysis of Petroleum Products and Lubricants, Edited by Kishore Nadkarni. The chapter describes the application of high resolution 1H and 13C NMR, 1H TD-NMR, and solid-state NMR to petroleum chemistry and refining. The book can be ordered at the ASTM Bookstore.

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Reaction Monitoring Using NMR and Vibrational Spectroscopy – RSC Conference

Dr. John Edwards of Process NMR Associates will be attending an RSC sponsored one day symposium on "Reaction Monitoring Using NMR and Vibrational spectroscopy - An Industrial Perspective". The meeting will be held at the Pfizer Research Center in Sandwich, Kent, UK on March 22, 2011. Dr Edwards will be presenting a poster entitled "Practical Applications of Compact High-Resolution 60 MHz Permanent Magnet NMR Systems for Reaction Monitoring and Online Process Control". The abstract of the talk is presented below: For the past two decades high resolution 1H NMR at 60 MHz has been utilized to monitor the chemical physical properties of refinery and petrochemical feed-streams and products. These approaches involve the use of partial least squares regression modeling to correlate NMR spectral variability with ASTM and other official test methods, allowing the NMR to predict results of physical property tests or GC analysis. The analysis is performed in a stop flow environment where solenoid valves are closed at the beginning of the NMR experiment. This approach allows up to 5 or 6 different sample streams to be sent to the sample in order to maximize the impact of the instrument. The current work with these permanent magnet NMR systems…

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Benchtop Permanent Magnet High Resolution NMR Systems

The latest buzz in the NMR news release world has been the emergence of the 45 MHz picoSpin (www.picospin.com) miniature NMR system that boasts shoe box size dimensions, a resolution of 80 ppb (3.5 Hz at peak half height), and a tiny 300 micron probe dimension. The sample can be injected with a syringe or pump. A number of application examples and spectra are posted on the application pages of the company website. It is noted that the spectra require the signal averaging of 24-200 pulses requiring an estimated experimental time of 3-10 minutes The system claims to be the first miniature NMR system but I guess that depends on how you define "miniature". A number of "relatively small" high resolution permanent magnet NMR systems operating at 60 MHz have been around since the early '90s (Elbit-ATI, FoxboroNMR, Qualion, ASPeCT-MR, and ACT). The picoSpin NMR is definitely the first spectrometer to deliver high resolution NMR from such a small footprint permanent magnet combined with a capillary probe. The S/N of the picoSpin system is approximately 300:1 on a one pulse spectrum of water. On our 60 MHz systems we are routinely obtaining, non-spinning, one pulse spectra without signal apodization with…

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IFPAC Conference: Process NMR Associates and University of California, Davis to Present Process NMR and MRI Short Course Prior to Meeting

Short Course on Process NMR and MRI to be presented at the IFPAC Meeting (http://www.ifpac.com/) When: Monday, January17, 1:00pm to 5:00pm, and continues on Tuesday January 18, 8:00AM to 12 noon Location: Baltimore Marriott Waterfront Instructors: Michael J. McCarthy, Professor of Engineering, University of California, Davis, CA Paul J. Giammatteo, Ph.D., Process NMR Associates LLC, Danbury, CT The course is specifically designed and organized for industry professionals who want to add to their knowledge-base on magnetic resonance and process analytical technology. Topics include compositional analysis, rheological characterization, measurement of the state of mixing, visualizing transport and product stability as well as recent advances in process magnetic resonance sensors. This course will bring you up-to-date on the latest information concerning the applications and state-of-the art instrumentation for process magnetic resonance. Outline: * Introduction to Process NMR Magnetic resonance theory - Time-domain, High resolution, Diffusion, Imaging * Hardware - Spectrometers, magnets, probes * Coupling the sensor to the process * Applications will include: - Composition measurement - Property measurement - Rheology measurement - Product structure For Details contact Paul Giammatteo Tel: (203) 744-5905 or Michael McCarthy Tel: (530) 752 8921

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Diesel Production Control – Combination of NMR and Simulated Distillation to Yield On-Line Carbon Number Distributions

Process NMR Associates has developed a database of Simulated Distillation database on a large number of diesel fuels on our Shimadzu 2010-GC with SimDis Software. The analysis is being used to develop distillation prediction models for the process NMR systems as well as explore new avenues of control information that can be derived by combining carbon number distributions obtained from the GC data with the predictive capabilities of online NMR. For a PDF version of this application article download this: Combination of NMR and Simulated Distillation for Diesel Production Control Simulated distillation allows carbon number distributions to be calculated and in combination with chemistry observed in the NMR analysis the effect of aromatics and olefins on the paraffin distributios can be estimated. Online NMR predictions can be established that yield real-time carbon number distributions for production control and sulfur species monitoring. Contact: Paul Giammatteo Tel: +1 (203) 744-5905 Process NMR Associates Website

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Extensive NMR Diesel Database Enhances NMR Model Performance for Unit Control and Product Manufacturing

An extensive database (10 years) of diesel samples incorporating all refining processes (distillation through product blending) enables development of robust, wide ranging property predictions independent of crude sources and refinery processing. Consistent attention to data integrity enables expanding model ranges well beyond any typical single unit or process operation. The following slides elucidate the consistency in spectra whether obtained 10 years ago or last week, from within a refinery or on a laboratory spectrometer. If you are interested in finding out more about NMR and diesel production control contact Paul Giammatteo or phone him at +1 (203) 744-5905 - see the Process NMR Associates website for further information

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Process NMR Application: Spectro-Molecular Control for Enhanced Diesel Recovery

NMR Process Systems - Integrated Solution Application for Crude Unit and Downstream Processes: Spectro-Molecular Control for Enhanced Diesel Recovery NMR Process Systems (NPS) on-line NMR based analytical and process control strategy for enhanced diesel recovery at the crude distillation unit maximizes clean diesel recovery by enabling closer cut point control in the mid-section of the CDU. Clean Fuels regulations in both the European and American markets have had a substantial impact on a refiners ability to maximize product draws at the refinery front end. Extremely low sulfur requirements for gasoline and diesel have resulted in refiners now being more constrained at the hydro-treaters. Lack of reliable, focused, measurement and control of critical CDU product draws has forced many refiners to significantly undercut these draws in order to ensure minimum error in the final product blends, especially with respect to total sulfur. Depending on a refinery's crude supply and CDU capacity, a conservative estimate of 300-500+ barrels per day of loss diesel production is typical. With an average of $25-$35 per barrel margin loss, the economic impact of these Clean Fuels Regulations are substantial. Integrating proven NMR technology with a focused measurement and control strategy enables crude unit operations to cut…

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Schering-Plough Corporation Seeks Process Analytical Technology Manager

Title: Process Analytical Technology (PAT) Manager Description: Implement Process Analytical Technology (PAT) throughout all the Global Quality Sites to identification of incoming materials and monitor manufacturing processes. Work directly with the sites and Schering Plough Research Institute to help support / initiate the development, validation, and deployment of PAT at the sites. Review, evaluate, implement, and manage PAT activities. Provide guidance / technical help to the sites to conduct evaluation and purchase commercial PAT related analytical equipment (e.g. NIR / FT-NIR, Raman / FT-Raman, IR / FT - IR etc.). Maintain analytical instruments in the lab to comply with cGMP standards and requirements. Train and mentor laboratory staff on PAT to generate analytical data for routine experiments. Generate network and infrastructures with various sites of the corporation. Take full ownership / responsibility and provide effective, meaningful, result driven and pro-active leadership on all PAT projects. Responsible to transfer knowledge / technology of PAT related projects and activities to sites. Job is located in New Jersey. Respectfully, Vincent L. Graziano Recruiting Manager / Global Staffing Schering-Plough Corporation 556 Morris Avenue, S1-1 Summit, N.J. 07901 Ph: 908-473-2745 Fx: 908-473-2793 Ph: 908-298-5232 (Kenilworth) Careers: Employment Opportunities email: vincent.graziano@spcorp.com 

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The RefinIR – FTIR-ATR Petroleum Product Analyzer

Press Release - NMR Process Systems - Gulf Coast Conference, Galveston Island, Texas - October 17, 2007 NMR Process Systems, LLC and Smith's Detection Launch RefinIRTM - The New Refinery Products Analyzer In a joint development effort NMR Process Systems and Smith's Detection have developed a range of petroleum analyzer products based on a mid-infrared spectrometer which utilizes an attenuated total reflection (ATR) sample interface. The ATR allows wipe and swipe sample introduction that is ideal for heavy petroleum analysis. Chemometric approaches to chemical and physical property prediction have been developed as well as analysis by spectral database matching. The FTIR-ATR spectrometer is called the RefinIR which can be utilized in the laboratory for rountine, multi-parameter prediction of  petroleum product properties or to aid in process troubleshooting on unusual samples or solid foulants. For more information contact Paul Giammatteo Principal, NMR Process Systems 87A Sand Pit Rd, Danbury, CT 06810 U.S.A.  Tel: (203) 744-5905

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Process NMR Associates Develops Oxford QP-20 Spectrometer Replacement

In a joint development effort Process NMR Associates and Resonance Systems Ltd have developed a replacement NMR spectrometer for the Oxford QP-20 TD-NMR analyzer. In many cases the excellent magnet and probe of the QP-20 continue to work effectively long after the NMR spectrometer has died. The Spin Track-20 spectrometer enables the user to completely replace the QP-20 NMR system while retaining the use of the original magnet and probe configuration. The product represents state-of-the-art digital NMR technology allowing newly developed TD-NMR methodologies to be applied to complex systems with all the advantages of a windows computer system (replacing the paper cartridge of the original system). Customers who have malfunctioning QP-20 NMR systems can obtain a modern digital NMR system within 8 weeks of order and for less than $16,000. The modular design of the Spin Track TD-NMR systems allows our engineers to develop replacement systems for all benchtop NMR systems such as those marketed by Oxford Instruments, Bruker Minispec, and Resonance Systems. Contact us if you have a non-functioning system that might be a candidate for the Spin Track upgrade. For more information contact John Edwards Principal, Process NMR Associates - Spin Track Division 87A Sand Pit Rd, Danbury,…

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PNA Presentation at 9th Upstate NY NMR Symposium

State University of New York College of Environmental Science and Forestry (SUNY-ESF) Syracuse, NY, 13210 Alumni Lounge– Marshall Hall October 12, 2007 Co-Organizers SUNY-ESF Syracuse University SUNY Upstate Medical University Bristol-Myers Squibb Art Stipanovic Phil Borer Stewart Loh Doug Weaver Dave Kiemle Stephan Wilkens   Sponsors SUNY-ESF Syracuse University Bruker Biospin Bristol-Myers Squibb Process NMR Associates LLC Isotec Cambridge Isotope Laboratories Varian Inc. The 9th annual Upstate NY NMR Symposium will be held at SUNY-ESF on Friday, October 12th featuring keynote speaker Professor Ruth E. Stark, Director Institute for Macromolecular Assemblies, CUNY. Others from around the region will also highlight their work in short presentations and posters. Tentative oral presentation program Poster session program (posted by 9/12) There is no cost to attend this symposium due to the generosity of the sponsors listed above but pre-registration is required Registration form Lodging arrangements have not been made for this symposium but a variety of options are available: Lodging Options The conference will be held in the Alumni Lounge (a.k.a. Nifkin Lounge), Marshall Hall on the SUNY-ESF campus located adjacent to Syracuse University. Maps and Directions Parking has been arranged in the Irving Garage just a short walk from Marshall Hall (campus…

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The Wood-Based Biorefinery in a Petroleum Depleted World

The Mid-Hudson Section of the American Chemical Society and Vassar College Announce The Wood-Based Biorefinery in a Petroleum Depleted World Dr. Arthur J. Stipanovic, Professor and Chair, Department of Chemistry State University of New York, College of Environmental Science and Forestry (SUNY-ESF) Wednesday, November 7th, 2007 Time: 7:00 pm Location: Mudd Chemistry Building, Third Floor Refreshments will be served at 6:30 pm Vassar College, Poughkeepsie, New York Contact: Dr Joseph Tanski (jotanski@vassar.edu, 845-437-7503) Abstract: The 21st century is envisioned to become the age of biology as renewable biomass resources replace petroleum in energy and industrial product applications. Motivated by concerns over national energy security, global CO2 reduction, a need for biodegradable products, and enhanced rural economic development, the engineering and construction of biorefineries for the manufacture of fuels, chemicals, polymeric materials and power from renewable resources is now a critical national priority. The context and intent of a biorefinery must be much more than simply replacing crude oil with renewable raw materials. A successful biorefinery must: 1) efficiently separate its raw material source into individual components, and, 2) be able to convert these components into marketplace products. The biorefinery must mirror the efficiency of today's modern petrochemical refinery in using…

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Wine Analysis by NMR

Brief Overview of Wine Analysis by 1H and 13C NMR Wine analysis by 1H or 13C NMR can be used to follow acid content during maturation. Lactic, succininc and acetic acid can be followed readily by both techniques and presence of sugar, glycerol, and methanol can be observed. Chemometric approaches are starting bear fruit with respect to quantitative analysis:

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NMR Without Solvents – Biodiesel Production Process – FAME, Glycerol, FFA, and Methanol

1H and 13C NMR NMR is typically obtained using deuterated NMR solvents to lock the field during acquisition. In some cases the use of these solvents is problematic as it prevents observation of solublized phases present in the sample. As an example we show here the NMR data obtained on a biodiesel production process. One of the major issues with the FAME product is the presence of glycerol in the product. NMR analysis is usually performed by dissolving the FAME in CDCl3 in which glycerol is completely insoluble. Thus NMR analysis performed in this way does not allow analysis of residual glycerol content. However, if the FAME is run neat this issue does not arise. Another analysis of enormous interest from the process control standpoint is the analysis of the glycerol/methanol phase. This phase contains considerable free fatty acids as well as the glycerol by product and excess methanol from the transesterification process. The three components are readily observed by 1H and 13C NMR, and 23Na can be used to observe NaOH content in the phase. Finally the shift and shape of the observed OH resonance can yield information on the pH of the glycerol phase. Typically this analysis is…

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Monitoring of a Biodiesel Transesterification Process with a TD-NMR Spectrometer

The 19.5 MHz Spintrack NMR analyzer was utilized to study a FAME biodiesel production reaction. The samples analyzed were:  1) Used vegetable oil 2) Partially transesterified biodiesel product (bad biodiesel)  3) High yield FAME biodiesel product  4) Glycerin by-product from the process   CPMG T2 decays were generated and then that data was processed with a inverse laplace transformation to produce T2 distribution profiles. NMR Experiment explanation is given below:     The CPMG data obtained on the four samples is shown below: The T2 distribution profiles obtained by inverse Laplace transformation of the CPMG data are shown below:     Plainly TD-NMR can play a role in monitoring the biodiesel production process.  

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TD-NMR Analysis of Catalytic Cracker Feedstocks

The 19.5 MHz Spintrack NMR analyzer was utilized to study a large series of  vacuum gas oils and FCC feeds for which PNA also has laboratory test data. The analysis was performed on a SpinTrack 19.5 MHz TD-NMR spectrometer - CPMG T2 decays were generated and then that data was processed with a inverse laplace transformation to produce T2 distribution profiles. These T2 distribution profiles are currently being correlated to physical and chemical property data. NMR Experiment explanation is given below:     The CPMG data obtained on the four samples is shown below:   The T2 distribution profiles obtained by inverse Laplace transformation of the CPMG data are shown below:   The correlation between T2 distribution and the metal content, viscosity, distillation range, density, asphaltene content are all being investigated at the current time.

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13C NMR of FAME Biodiesel

pdf version Below are examples of 13C NMR data obtained on biodiesel (FAME) and the vegetable oil precursor that it was made from by transesterification process involving microwave activation of the reaction between triglycerides and methanol in the presence of a caustic catalyst. Process NMR Associates is developing correlations between 13C NMR data and biodiesel properties stipulated in ASTM 6751.

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Detailed 13C NMR Analysis of Hydrocarbons – Patent Applications

Today one often finds hydrocarbon mixtures described by the detailed carbon type analysis that is possible from 13C NMR. Many petroleum related products are being described in this way in patents leading to a novel way of describing a material and restricting others from using those same materials in products of their own. See Exxon, Mobil, and Chevron patents such as:  6,090,989 ;  6,210,559  ;  6,059,955  ;  6,846,778  ;  20050077208  ; and 20050077209 In this PDF file we have shown some of the details present in a 13C NMR spectrum on petroleum products such a base oils, gas oils, diesels, etc. Details of NMR Analysis There are some issues with the assignements of many of these patents ... for more details on how NMR might be of use in the patent process contact John Edwards

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Naphtha Chemistry Analysis by 1H NMR

PDF Version 1H NMR has been used extensively by Process NMR Associates to determine PIONA analysis of Naphthas and to determine detailed aromatics breakdown in aromatics unit feeds, products, and intermediate products. Below are a few examples of naphtha chemistries that are observed and quantified by 1H NMR. Conjugated Olefin analysis is performed by a combination of HH-COSY and 1D 1H NMR.   For more details contact John Edwards

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Process NMR Symposia to be held at EAS 2007

John Edwards of Process NMR Associates has organized and sponsored two symposium sessions at the Eastern Analytical Symposium in Somerset New Jersey, November 12-15, 2007. One session will focus on high-resolution process NMR and the other on applications of TD-NMR in process control. The speakers and talk titles are listed below. Check the EAS site for exact details on the date and time of the sessions (EAS website). If you are interested in attending and would like to submit a paper for presentation visit the EAS Abstract submission site. Session Title: Process NMR Technology - High Resolution NMR John Edwards, Process NMR Associates, "Introduction to NMR in Process Control" Miko DeLevy, Qualion NMR Analyzers, "Standardizing and Stabilizing NMR Calibration Transfer" Paul Giammatteo, NMR Process Systems, "More from the Barrel - On-line NMR Increases Diesel Production and Quality" Marcus Trygstad, Invensys Process Systems, "Taking NMR into the Refining Process:  Best Practices and Benefits" Andreas Kaerner , Eli Lilly, "Get Your Head Out of the Sand: Use of Reaction-NMR to Better Understand Reactions in Process Development" Veena Bansal, Indian Oil Corporation, "Direct Prediction of Gasoline Properties for Monitoring Refinery Processes by 1H NMR Spectroscopy" Session Title: Process NMR Technology - TD-NMR Harry…

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Trans Fat Analysis by NMR

A series of Trans Fat standards was purchased from AOCS. The ability of 1H and 13C NMR to predict Trans Fat Content as well as  Saturated, Poly-unsaturated, and Mono-unsaturated Fat Content The data of the samples is presented in the table below:     PLS regression techniques were used to correlate 1H and 13C NMR spectral variation to the unsaturation level and type of unsaturation of the samples.   Processed 13C data is shown below:     1H NMR data is shown below:     The following correlations were obtained from the 13C NMR data.              

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NMR Analysis of Essential Oils – Example of Sri Lankan Citronella

The data below shows the ability of 13C NMR to assign the natural product distribution found in essential oils. Once assignment of the oil hgas been obtained by 13C NMR the 1H NMR can also be assigned. For QA/QC a benchtop 60 MHz system has enough resolution that authenticity of essential oils can be performed either visually of by PCA type analysis. Ger - Geraniol         GerAc - Geranyl Acetate        iEugMe - Methylisoeugenol       Bor - Borneol aPin - alpha-pinene        Lim -  Limonene        tOci - trans-beta-Ocimene      Cen - Camphene Cllo - Citronellol        Clla - Citronellal        GenD - Germacrene D         aCal - Citral A (Geranial) aTol - alpha-Terpiniol         cOci - cis-beta-Ocimene        Myr - Myrcene

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Process NMR for Transesterification Monitoring and Certification of Biodiesel

1H NMR has been used extensively to analyze biodiesel the vegetable oil feeds, reaction intermediates, and final products of the biodiesel transesterification process. See Oliviera et al, Talanta 69 (2006) 1278-1284 and Gnothe, J. Am. Oil Chem. Soc 78, 1025-1028 (2001) The final biodiesel product is a B5 (5% Biodiesel) or B20 (20% Biodiesel) blend of biodiesel in refinery produced diesel fuel. Researchers have performed method developments to analyze the biodiesel content in diesel fuels by NIR using 1H NMR as the primary method to quantify the biodiesel content. (See Jin et al, Fuel 86(7-8), 1201-1207 (2007) and Knothe J. Am. Oil Chem. Soc. 77 489-493 (2001). Process NMR at 60 MHz can be used to quantify the biodiesel directly. Below is an example slide of a biodiesel 1H NMR spectrum compared to two different diesel fuel spectra. The chemistry that is directly observed in the NMR spectrum as well as the distinct chemical regions that are present in the diesel and biodiesel make this analysis relatively straightforward. Chemometrics can be used or quantitation can be obtained directly from a simple spectral calibration. Biodiesel Production Monitoring NMR can be used to follow the reaction of biodiesel directly, the following slides…

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Process NMR Technology Session Planned for Eastern Analytical Conference 2007

Press Release - NMR Process Systems - Danbury CT - February 14, 2007   Dr Edwards of Process NMR Associates has been asked to organize a session on Process NMR Technology at the Eastern Analytical Conference to be held at the Garden State Exhibit Center, November 12-15, 2007. Below is a copy of the Call for Papers sent out on February 14, 2007.  Hello to all, I have been asked by Cecil Dybowski to chair a session on Process NMR Technology at the 2007 Eastern Analytical Symposium to be held November 12-15 at the New Jersey Garden State Exhibit Center in Somerset New Jersey. At this point I am putting out some feelers to gauge the level of interest that is out there amongst NMR practitioners in this field. I would like the session(s) to encompass both high resolution and time-domain applications of NMR in process control applications and at-line in manufacturing facilities in all industry sectors. The work can be actual on-line examples or laboratory based analysis being used to justify or prove applications before they are spun out to the plant. Developments in hardware, software and chemometrics would also be of general interest and to this end hardware…

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Process NMR Spectroscopy Seminar Series to be Held at 2007 Eastern Analytical Symposium

John Edwards of Process NMR Associates has agreed to chair a session at the Eastern Analytical Symposium in Somerset, New Jersey in November, 2007. The session is entitled "Process NMR Spectroscopy". If you are interested in presenting a technical paper at this session please contact John directly at john@process-nmr.com Also listed here is the 2007 Call for Papers for the upcoming meeting.

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New Site Dedicated to Magnetic Resonance in the Food Sciences

A new website has been introduced that focusses on the applications of Magnetic Resonance (NMR, MRI, Relaxometry) to the chemistry and physics of foods. The website can be found at magres.foodsciences.org This organization also arranges the biannual conference on Application of Magnetic Resonance in Food Science - they have an excellent poster session with PDF versions of the poster presentations published to the web - Poster PDFs

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