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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NMR Detection of Tomato Paste Spoilage in 1000 Liter Metal Lined Totes

Poster to be Presented at the 56th ENC, Asilomar CA, April 2015 NMR Detection of Tomato Paste Spoilage in 1,000 L, Metal Lined Totes Michele Martin1; Paul Giammatteo2; Michael McCarthy1; Matthew Augustine1 1University of California, Davis, Davis, California; 2Process NMR Associates, Danbury, CT Abstract Low field nuclear magnetic resonance (NMR) is used as a non-invasive method for detecting spoiled tomato paste. It is shown that the 1H T1 and T2 relaxation times change as tomato paste spoils due to changes in viscosity and/or changes in the concentration of paramagnetic compounds. With the goal of developing a spoilage detector that can be used in a tomato processing facility, a γBo = 19.5 MHz single-sided handheld NMR instrument is used. Due to the dominance of diffusion on relaxation measurements made with the single sided instrument, the slope of the amplitude of a spin echo for three different delay times is used to provide a viscosity dependent parameter that permits the differentiation between pristine and spoiled tomatoes. One-Sided NMR - Non-Invasive Analysis of Tomato Paste  

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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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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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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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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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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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Process NMR Associates Expands and Updates NMR Testing Facilities

Process NMR Associates has just finished completion of a complete update and expansion of the NMR facilities at it's Danbury CT location. The faithful Varian Unity-300 spectrometer has been replaced by a Mercury-300 VX spectrometer and a second 300 MHz Mercury Plus system has been installed. This second 300 MHz NMR includes PFG and an indirect detection probe. These instruments compliment a Varian UnityPlus-200 spectrometer equipped with a 7 mm Solid-State MAS probe for analysis of solid materials. The doubling of the liquid-state NMR capacity will allow rapid turnaround of all sample submissions and expand the experimental capabilities of the facility. Process NMR Associates is a private corporation providing analytical NMR services and consulting since 1997. The NMR facility in Danbury includes two 300 MHz, one 200 MHz, and two 60 MHz high resolution NMR spectrometers. The facility also houses a 10mm, 18mm, and 40mm TD-NMR facility for relaxation studies. The company also has gas chromatography, micro-ESR, and FTIR-ATR capabilities. For details of the analytical services provided please contact John Edwards.

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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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Process NMR Associates – Journal Article Published

An article by Dr. John Edwards of Process NMR Associates and researchers at the Southern Regional Research Center of the US Department of Agriculture (Dr. H.N. Cheng, Lynda H. Wartelle, K. Thomas Klasson) has been accepted for publication in the Elsevier Journal Carbon. The paper entitled "Solid state NMR and ESR studies of activated carbons produced from pecan shells" is available at the following link: Carbon Paper . Process NMR Associates provided the solid-state 13C NMR, TD-NMR, and ESR spectroscopy for the analysis of the activated carbons derived from pecan shells.

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60 MHz TD-NMR System

Process NMR Associates and Spin Resonance Ltd have recently completed the construction a small 60 MHz (1.4T) 5mm TD-NMR system that can be utilized to study T1 and T2 characteristics of novel contrast agents at typical MRI frequencies. Here are a few pictures of the magnet. It is based on N42 neodymium-iron discs (120mm diameter x 30 mm deep).

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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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