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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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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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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