Chemical Fingerprints of Cider – Cidercon 2018 Technical Presentation – Recorded and Presented on the Cider Chat Podcast

John Edwards presented a talk on the chemical analysis of ciders at Cidercon 2018. The talk was recorded by Ria Windcaller who produces the Cider Chat Podcast which specializes in interviews and news from the world of commercial and amateur cider making. Here is the information to listen or watch the presentation. I have set up your presentation as a full podcast episode and as a video recording, without the podcast. It totally works! Yay. :) Via the podcast your presentation begins around 13:02 minutes into this week’s episode. I learned so much about a area of study I didn’t even knew existed. I’m excited to think that your work will boost cider’s study as it does for the wine industry. There are lots of listening options to share as you please via Cider Chat- http://ciderchat.com/chemical-fingerprints/ This link above provides the description and a photo. It is set up to work with social media. I have posted it at the Cider Chat Facebook page if you want to see what it looks like, before sharing. Listen via: iTunes: https://apple.co/2yBsrz5 For Android the following Apps need to be downloaded to listen to podcasts. Stitcher: http://bit.ly/1OvdrDq Google Play: https://play.google.com/music/m/Ine7dtqx57ephmbncwrtubpkyt4?t=Cider_Chat and the Spotify…

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The Chemical Fingerprint of Beer from a Single Experiment with Minimum Sample Preparation – A Rapid Quantitive Analysis by 1H NMR Spectroscopy

NMR Spectroscopy is the premier tool utilized by chemists to obtain detailed chemical information on molecular structure and is used extensively in molecular structure verification, chemical purity analysis, and complex mixture analysis. We have developed a quantitative NMR analysis that yields a chemical fingerprint that brewers can utilize to follow detailed variations in the chemistry observed in the various stages of the brewing process (malting, mashing, boiling, fermentation, ageing, and blending). The analysis observes all molecules in the beer at the same time and each molecular component (acids, alcohols, amino acids, malt-oligosaccharides) yields a unique spectral fingerprint pattern that is related to the structure of the molecule. Though the spectrum consists of a large number of overlapped individual fingerprints it is possible to identify and quantify individual components because many components have signals that appear at unique and specific points in the spectrum. The quantitative analysis is performed by comparing the area under the individual molecule signals to that of an internal standard (Maleic Acid 99%). Molecular components are quantified on a weight/volume basis in mg/L (parts-per million). Ethanol is also quantified on a %volume/volume basis. The technique is not only applicable to the brewing process but is also being…

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References to 1H qNMR Applied to Fruit Juices and Alcoholic Beverages

qNMR “Validation of quantitative NMR”, F Malz, H Jancke, J Pharm Biomed Anal,  38, 813–823, (2005) “Quantitative 1H NMR spectroscopy”, S K Bharti, R Roy, Trends in Anal Chem, 35, 5-26 (2012) “NMR-based plant metabolomics: where do we stand, where do we go?”  H-K Kim, Y-H Choi, R Verpoorte Trends Biotech, 29(6), 267 (2011). “Universal quantitative NMR analysis of complex natural samples”, C Simmler, J G Napolitano, J B McAlpine, S-N Chen and G F Pauli, Current Opinion Biotech, 25, 51–59 (2014) “Quantitative 1H NMR: Development and Potential of a Method for Natural Products Analysis” G F Pauli, B U Jaki, D C Lankin, J. Nat. Prod., 68, 133-149 (2005) Juices “High-Field Proton NMR Studies of Apple Juices”, P S Belton, I Delgadillo, A M Gil, P Roma, F Casuscelli, I J Colquhoun, M J Dennis M Spraul, Mag Res Chem, 35, S52-S60 (1997) “Quantitative determination of (-)-epicatechin in cider apple juices by 1H NMR”, I Berregi , J I Santos , G del Campo , J I Miranda, Talanta 61 (2003) 139-145 “Use of the 1H Nuclear Magnetic Resonance Spectra Signals from Polyphenols and Acids for Chemometric Characterization of Cider Apple Juices”, G del Campo, J. I Santos, N…

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Quantitative 1H NMR Analysis of “Off-the-Shelf” Commercial Kombucha Beverages for Ethanol, Organic Acids and Residual Sugars Analysis

Over the past few years our analytical NMR service has been developing a detailed chemical fingerprint analysis of alcoholic beverages by quantitative 1H NMR (qHNMR). Beyond the typical analyses of beer, wine, port, hard cider, sake and spirits, we have been looking at other fermented beverages such as kombucha, kefir, kvass, mead, ginger beer and perry. As well as the final fermented beverages we have been actively investigating the various starting materials such as malt wort, apple juice, honey, grape juice, fruit juices, and tea. The NMR analysis can provide a rapid quantitative analysis without any sample preparation based on the molar ratio of integration value of unique molecular fingerprint peaks with the integrated signal of an internal standard. In our case we typically use maleic acid as an internal standard as it’s singlet signal peak appears in a non-overlapping are of the spectrum to the chemistry we are interested in following. The information that can be derived from the NMR experiment covers a wide dynamic range of component molecule concentrations from 10-100,000 ppm. The analysis observes all fully dissolved chemical constituents and the spectral response is linear with regard to all chemical types. As a primary analytical method the…

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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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1H qNMR of Alcoholic Cider – Analysis of Small Molecule and Residual Sugar Chemistry

1H quantitative NMR (qNMR) has been utilized to assess the the small molecule and carbohydrate chemistry of a number of home-brewed and commercial alcoholic ciders. A quantitative chemistry distribution of the products of the various fermentations that occur in cider making. Malolactic fermentation as well as fermentation by saccharomyces and wild yeasts occur in the cider making process which traditionally occurred without the intentional addition of yeast by the manufacturer. The distribution of small molecules produced by the yeast and bacterial metabolomes at work in the process can yield information of the sensory perception of ciders produced in different ways. An investigation of the residual sugar chemistry of commercial ciders gives some indication of the process of sweetening commercial cider products with sugar additions after fermentation is complete. These typical commercial ciders are very different in chemistry distribution compared to very dry cider styles such as those found in the Basque region of Spain where fermentation is taken to the extreme resulting in complete conversion of sugars to alcohol but also glycerols to 1,3 propandiol. Finally it was decided to determine how much quantitative chemistry information could be obtained from benchtop NMR systems operating in the 60 MHz range. These…

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PNA to Present 4 Topics at the 2015 ACS North East Regional Meeting

John Edwards of Process NMR Associates will be presenting 4 papers at the 2015 ACS Northeast Regional Meeting that will be held in Ithaca, NY, June 10-13, 2015. ABSTRACT ID: 2283171 ABSTRACT TITLE: 1H qNMR of Alcoholic Cider - Analysis of Small Molecule and Residual Sugar Chemistry (final paper number: 43) SESSION: Food Chemistry SESSION TIME: 5:00 PM - 9:00 PM PRESENTATION FORMAT: Poster DAY & TIME OF PRESENTATION: Wednesday, June, 10, 2015, 5:00 PM - 9:00 PM ROOM & LOCATION: Emerson Suites - Campus Center ABSTRACT ID: 2283063 ABSTRACT TITLE: Nutritional Supplement and Diesel Fuel Application Development for Benchtop NMR Systems Operating at 42, 60, and 80 MHz – Equivalency with Supercon NMR (final paper number: 336) SESSION: Analytical Chemistry SESSION TIME: 9:00 AM - 11:30 AM PRESENTATION FORMAT: Oral DAY & TIME OF PRESENTATION: Friday, June, 12, 2015 from 9:45 AM - 10:05 AM ROOM & LOCATION: 222 - Williams Hall ABSTRACT ID: 2283105 ABSTRACT TITLE: Survey of Low Field NMR Spectrometer Platforms for Successful Screening of Sexual Enhancement and Weight Loss Supplements for Adulteration with Drugs and Drug Analogs (final paper number: 386) SESSION: Medicinal Chemistry SESSION TIME: 1:00 PM - 3:20 PM PRESENTATION FORMAT: Oral DAY…

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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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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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Benchtop NMR Systems – Sensitivity with Complex Pharmaceutical Molecules

PNA has been conducting a number of studies into the adulteration of male enhancement herbal suplements with PDE5 inhibitors such as viagra, cialis and a wide number of analogs (Mw approximately 475 amu). Standard materials for the analogs are quite expensive so in th eprocess of developing ID and purity methods on our NMR systems we ran the 1H NMR on our 300, 60, and 43 MHz NMR systems at a concentration of 5mg/ml which equates to 0.01 Molar. This PDF of the NMR data demonstrates the sensitivity and resolution obtainable on these bench-top 5mm NMR systems. They can readily look at samples at these concentrations. They can readily be utilized as screening tools or as quantitation and identification analyzers. The PDF file containing the Varian 300, Aspect-60, and Magritek 43 MHz data can be found here: NMR Data-0.01 Molar_PDE5 Analogs 300_60_43_MHz

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Beer and Cider Analysis – Example of Spectral Repeatability of Benchtop 60 MHz NMR System

Here is an example of spectral reproducibility. We are doing a lot of beer NMR at the moment on our 300 MHz NMR and for "giggles" we are running many samples through the various bench-top systems in our lab. We have been quantifying small organic acids (lactic, acetic, succinic , malic, citric, etc.) as they can give some idea of yeast activities and health during fermentation. We are also quantifying  and studying the 1,4/1,6 linkage distribution of residual dextrins. The series of superimposed spectra below consists of 28 spectra of a freeze dried beer sample (a unique Belgian Dubbel. Each spectrum was 128 pulses and took approximately 30 minutes per spectrum. So the superimposed data represents a 14 hour continuous stability test.The data was automatically processed with 16K zero-fill and autophase.It looks pretty damn good.   We've been looking at a lot of sour beers - here is a home-brewed Flemish Red aged in an oak barrel - note the high lactic and acetic content. We've also been analyzing a lot of hard ciders - commercial and home-brewed varitieties of various styles - very different from one sample to another in the small molecule and sugar chemistry.     1H…

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Benchtop NMR – Screening Tool for Adulterated Herbal Supplements

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 Edwards1, Kristie M Adams2, and Anton Bzhelyansky2 1Process NMR Associates, Danbury, CT 2United States Pharmacopeial Convention, Rockville, MD The adulteration of dietary supplements (or natural health products) with synthetic pharmaceuticals is an area of increasing concern, which presents substantial risk to public health. Widely available in retail and via the Internet, these products are often marketed as sexual enhancement, weight loss and/or bodybuilding supplements. Unlike prescription drugs, supplements do not require premarket approval by FDA before they are made available for public consumption. In fact, the agency can only take investigational action after the adulterated product has caused harm and the adverse event has been reported via MedWatch (FDA’s online portal for voluntary reporting of adverse events associated with drugs, medical devices and dietary supplements). Development of analytical tools for screening and identification of adulterated products in the marketplace represents a significant step forward in the fight against adulterated dietary supplements. Several organizations, including AOAC and USP, have undertaken initiatives to evaluate and recommend analytical methodologies for screening supplements for adulteration. HPLC and mass…

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1H Benchtop NMR Analysis of Physical and Chemical Properties of Diesel Fuel

1H Benchtop NMR has great potential to increase the throughput of both routine and emergency fuel sample analysis in refinery laboratories. Currently fuel samples must be passed through multiple dedicated analyzers to obtain information such as density, H-Content, aromatics, olefins, saturates, benzene, Octane numbers, cetane index, cetane number, distillation curves, vapor pressure, flash point, pour point, freeze point, cloud point, etc. Correlation of the 1H NMR spectra of these refinery fuel samples to these primary test results will allow all parameters to be predicted in about 40 seconds from the 4 pulse spectrum of the pure fuel. Here we have a few examples obtained on some diesel fuels that were submitted to our lab for ASTM D7171 – Hydrogen Content by TD-NMR. We had density, H-content, and aromatics wt% by GC. Below are three example correlation obtained on the Picospin 80 system (that requires 32 pulses per sample due to the capillary sample size). The results were very similar for the 300, 60, and 42 MHz data obtained on the three other NMR system in our laboratory. The comparative results are shown in Table II. The results are very similar independent of the field strength of the NMR system. The…

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Nutritional Supplement and Diesel Fuel Application Development for Benchtop NMR Systems Operating at 42, 60, and 80 MHz – Equivalency with Supercon NMR

Benchtop high-resolution NMR systems are available at a number of field strengths and probe configurations. However beyond the obvious academic instruction market for these instruments very few applications have been demonstrated across all available platforms and thus proving the general applicability of benchtop NMR technology to industrial quality control. We will present two chemometric-based applications that have been developed at 4 different field strengths utilizing Varian Mercury 300 MHz, Magritek Spinsolve 42 MHz, Aspect AI 60 MHz, and Thermo Picospin 80 MHz NMR systems. Partial-least-squares (PLS) regression correlations were obtained on all 4 platforms relating to: 1) Omega-3 fatty acid composition of samples taken from various points in a nutritional supplement manufacturing process. Excellent correlations were obtained on all 4 NMR instruments proving that NMR technology is applicable to in-lab, at-line. or on-line analysis of fish oil derived omega-3 fatty acid supplements. The 40 second NMR analysis effectively replaces a 60+ minute GC analysis. 2) Physical and chemical property determination of diesel fuels where excellent correlations were obtained between 1H NMR variability and parameters such as density, aromatic content by GC, hydrogen content by 1H TD-NMR (ASTM D7171 method), and sulfur content. Many more physical and chemical properties can be…

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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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Agilent drops a bombshell – big changes are coming for the NMR community

Agilent Technologies to Close Nuclear Magnetic Resonance Business SANTA CLARA, Calif., Oct. 14, 2014 Agilent Technologies Inc. (NYSE: A) today announced it is exiting its Nuclear Magnetic Resonance business. Agilent entered the NMR business in 2010, with the acquisition of Varian. Since then, the business has not met growth and profitability objectives. "Today's announcement represents a difficult decision necessary to drive improved profitability," said Mike McMullen, president and chief operating officer, and CEO-elect. "The NMR team has been extremely dedicated and has made many excellent contributions. However, this action is a step in ensuring that our investments are placed on higher-value life sciences, applied markets and diagnostics solutions that will continue to drive growth across the company." Agilent will stop taking new NMR system orders immediately, but the company will continue to meet customer commitments for orders in progress and for ongoing support contracts. Agilent will continue to provide service on all installed NMR systems. The company expects that this decision will eliminate about 300 jobs, mostly within the next 12 months. The majority of the affected positions are located in Yarnton, U.K., and Santa Clara, California. Today's announcement is part of Agilent's strategy to address the business shortfalls of…

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Presentation and Posters – Magnetic Resonance in Food Conference 2014 – Cesena Italy

“Liquid and Solid-State 27Al qNMR of an Elemin Senonian Trace Minerals Supplement for Identification, Chemical Structure, Quantitation of Active Ingredient in the Product, and Product Stability”, Boris Nemzer, John C. Edwards, presented at XII International Conference on the Applications of Magnetic Resonance in Food Science: Defining Food by Magnetic Resonance, Cesena, Italy, May 20-23, 2014. Get PDF Here “Liquid and Solid-State Multinuclear 13C and 11B qNMR FruitexB Fructoborate Complex Nutritional Supplement. Identification, Chemical Structure, Quantitation of Active Ingredient in Product, and Product Stability”, Boris Nemzer, John C. Edwards, presented at XII International Conference on the Applications of Magnetic Resonance in Food Science: Defining Food by Magnetic Resonance, Cesena, Italy, May 20-23, 2014. Get PDF Here “1H qNMR of EPA and DHA Omega-3 Fatty Acid Esters - PLS Regression Models Obtained by 60 and 300 MHz NMR - At-Line and On-Line Monitoring of a Fish Oil Nutritional Supplement Manufacturing Process”, John C. Edwards, Paul J. Giammatteo, invited oral presentation at XII International Conference on the Applications of Magnetic Resonance in Food Science: Defining Food by Magnetic Resonance, Cesena, Italy, May 20-23, 2014. “Application of High Field and Cryogen-Free Bench-Top NMR Platforms to the Monitoring and Quantitation of PDE5 Inhibitor Adulteration of…

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Presentation and Posters at PANIC 2014

“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 C. Edwards, invited presentation at the 2nd PANIC, Charlotte, NC, February 3-5, 2014. Get PDF Here “Development of an Automated Complex Mixture Analysis qNMR Method within Mestrelab MNova - Application to Aloe Vera and the Beer Brewing Process", John C. Edwards, Adam J. Dicaprio, Michael A. Bernstein, presented at the 2nd PANIC, Charlotte, NC, February 3-5, 2014. Get PDF Here “Small Molecule Chemistry of Spontaneously Fermented Coolship Ales”, Adam J. Dicaprio, John C. Edwards, presented at the 2nd PANIC, Charlotte, NC, February 3-5, 2014. Get PDF Here “Liquid and Solid-State 1H, 13C, and 11B qNMR Analysis of Fruitex-B®– A Calcium Fructoborate Comple: Chemical Structure and identification, quantitative analysis and stability study”, Boris Nemzer, John C. Edwards, presented at the 2nd PANIC, Charlotte, NC, February 3-5, 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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Herbal Supplement for Erectile Dysfunction Found to Contain Thio Structural Analog of Sildenafil (Viagra)

A herbal supplement marketed to alleviate erectile dysfunction was recently submitted for testing in our laboratory because it was surprisingly effective considering it should only contain the traditional herbals utilized for this problem such as Oyster, 2-Deoxy-D Glucose, Barberry, Snow Lotus, Bombyx Mori L., Ginger Root, Salfron Crocus. Above: 1H NMR of ED Herbal Supplement - this is an extract of the powder from  the capsules into 80:20 CD3CN:D2O - Observed suspicious specific small molecule peaks - herbals are usually broad featureless complex mixture spectra. This is something in different - a specific drug material appears to have been added.Comparison with the spectrum of Viagra (Sildenafil Citrate) below shows a strong similarity between the 2 active ingredients. We also obtained the COSY, 13C and DEPT NMR Spectra on the ED herbal supplement. These are shown below. The analysis of the NMR data led us to find that the extractable components of the sample contained predominantly Sulfoaildenafil (thioaildenafil) which is a strutural analog of Sildenafil (Viagra) and is not approved by any health regulation agency for use in erectile dysfunction medicines or supplements. Apparently these structural analogs to Viagra are found widely in herbal supplements sold for this malady. I guess…

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Solid-State 13C NMR of Drug API and Tablets

We have an excellent solid-state Doty Scientific Supersonic 7mm CP-MAS probe for our Varian UP-200 spectrometer. This is a nice field strength for solid-state 13C analyses as it allows for spectra at higher sensitivity than a 100 MHz but still has the advantage that 7 kHz is enough to push the aromatic MAS sidebands beyond 0 ppm so that more accurate aromaticity values can be calculated. The probe is still working after 20 years and we are using the original rotors and have never had to replace any of the capacitors. We have run approaching 20,000 experiments with this probe. Here are some of the nice spectra we have been getting recently on drug API and tablets. Above: Solid-State 13C NMR of Rapamycin API Above: Solid-State 13C NMR of Ranitidine HCl - Zantac Tablet Above: Solid-State 13C NMR of Simvastatin 20 mg Tablet Solid-State 13C NMR of Tylenol 3 - Acetamenaphin + Codeine Above: Solid-State 13C NMR of Amoxicillin Capsules Above: Solid-State 13C NMR of Diovan 50 mg Tablet Above: Solid-State 13C NMR of Divalproex Tablet Above: Solid-State 13C NMR of Herbal Supplement Capsule Found to Contain Thioaildenafil - A Structural Analog of Sildenafil (aka Viagra) Above: Solid_State 13C NMR…

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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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Trans Fats by 13C NMR

The same trans fat analysis can be performed by 13C NMR. The arrows on the stacked plot indicate the regions of the spectrum tat correlate to trans fat carbon chemistry.

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Trans Fat Analysis by 300 MHz 1H NMR

This topic has become pertinent again with the interest of FDA in trans-fat content in processed foods - more information here.Back in 2006 we performed a cursory analysis of trans fat reference materials that we purchased from AOCS. We performed a series of 1H NMR analysis and performed a chemometric PLS analysis correlating the 1H NMR spectral variability to trans fat content, PUFA (polyunsaturated fatty acid content), SAFA (saturated fatty acid content), and MONO (monounsaturated fatty acid content). Excellent correlations were obtained between wt% values obtained by GC analysis and the rapid 1H NMR analysis (2 minutes on a 300 MHz NMR). 1H NMR spectra on the standard samples are shown in the figures below as well as the GC data that was used in the regressions. A PCA analysis of  the NMR data nicely categorized the various types of samples as well as the trans fat contents of the samples with nice separation being shown in the PC1 vs PC2 score plot. The various correlations for trans fat, SAFA, PUFA, and MONO are shown below.    

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Beware of Adulteration of “Herbal Supplements” for Erectile Dysfuntion

We recently performed an analysis of a competitive product for a company working on developing "herbal supplements" for erectile dysfunction. They ended up not paying for the analysis so we thought we would just publish it generically as a "point of interest". It was described to us that the product worked incredibly well which immediately made it suspicious ... NB: we didn't actually try it out ourselves. The bottom line is that the product was not "herbal" at all .. it was thiosildenafil an analog of Viagra. "Herbal Supplement" Viagra Stacked comparison plot. COSY Beware out there. If you are on alpha-blockers for heart condition and buy an innocent looking "herbal" for ED issues .. it may actually be pharmaceutical grade viagra with all the use warnings that go with it.

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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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Practical Applications of NMR in Industry Conference (PANIC) – Student Travel Grants Available

CASSS is pleased to provide a limited number of student travel grants for PhD students and post-docs who present posters at the Practical Applications of Nuclear Magnetic Resonance Conference (PANIC). PhD students or post-doctoral fellows conducting research with professors in universities throughout the world are eligible. CASSS would like to gratefully acknowledge the Suraj Manrao Student Travel Science Fund for their contribution to subsidize one additional science student to attend the PANIC Conference. To apply for a student travel grant, students should submit: Your abstract online (Please click here to submit your abstract) A letter requesting consideration for the grant A letter of recommendation from your professor or advisor A PDF of your abstract A CV for the candidate All documents can be emailed to the NMR Symposium Manager, Linda Mansouria at lmansouria@casss.org. The deadline to apply for a student travel grant is Friday, July 13, 2012.

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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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Anita Brandolini – NMR Spectroscopist and Professor – RIP

We saddened to hear today that our good friend and NMR compatriot Anita Brandolini passed away a few weeks ago. We were informed by Mike Frey of JEOL that the North Jersey Section of ACS will be setting up a memorial as part of Project SEED. If you knew Anita or share her passion for teaching science to the young then please consider donating to this cause. Anita J.Brandolini, 56, Assistant Professor of Chemistry at Ramapo College of New Jersey, died suddenly at her home in Hillsboro, NJ on March 10, 2012. Originally from Morton, PA, Brandolini earned her B.S. in Chemistry in 1979 at Drexel University and her M.A. and PhD in Physical Chemistry in 1981 and 1983 at the University of Delaware. She was also a course Instructor for JEOL, USA, Inc. Brandolini worked for 17 years at Mobil Chemical where she was a Team Leader and Senior Research Chemist in polymer analytical chemistry. She was an expert in the nuclear magnetic resonance of polymer systems publishing a book, NMR Spectra of Polymers and Polymer Additives (Anita J. Brandolini and Deborah D. Hills, New York; Marcel Decker, 2000) and contributing chapters on spectroscopy to numerous publications. In 2000…

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Whole Leaf Marker and Maltodextrin in Aloe Vera Raw Materials – Dry Weight Quantity – Extended 1H NMR Analysis Method

Process NMR Associates has developed an extension of its 1H NMR analysis of Aloe Vera raw materials and products analysis. Powder aloe vera raw materials (100x/200x) can be analyzed directly and juice samples (1x, 5x, 10x, commercial products) must be freeze dried for this analysis. The whole leaf markers utilized in this test to indicate the presence of whole leaf material are iso-citrate and iso-citrate lactone which are formed in the green leaf part of the aloe plant as part of the citric acid cycle. It is possible to assign and quantify the following components of an aloe vera juice or powder: * aloe vera components: acemannan, glucose, malic acid * whole leaf markers: isocitrate, iso-citrate lactone, citric acid * degradation products: lactic acid, acetic acid, fumaric acid, pyruvic acid, formic acid, succinic acid, and ethanol * adulterants: maltodextrin * preservatives: sorbate, benzoate * additives: sucrose, fructose, glycine, flavorants (contain ethanol and propylene glycol) For the components above it is possible to obtain a wt% of that component in a juice sample - the freeze drying process is then used to determine the wt% solids in the juice and the dry weight concentrations of the organic components in the solids.…

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Talks to be Presented at IFPAC 2012 – Baltimore, MD January 22-25

Talk 1 by John Edwards Mutivariate Analysis of 1H and 13C NMR Data of Residual Catalytic Cracker Feed-Streams: NMR Pre-Processing Strategies that Allow the Development of Predictive Models of Physical and Chemical Properties that are Independent of NMR Instrument Magnetic Field Strength John C. Edwards*# and Jincheol Kim† *Process NMR Associates, LLC, 87A Sand Pit Rd, Danbury, CT 06810 USA † SK Innovation Co., Ltd, SK Innovation Technology Center, 140-1, Wonchon-dong, Yuseong-gu, Daejeon 305-712, Korea # Speaker Historically refinery control engineers are familiar with GC derived chemical properties such as aromatics, benzene, PONA, olefins in wt% or vol%, as well as physical properties such as distillation, viscosity, conradson carbon, sulfur, density, etc. We have developed generally applicable multivariate regression methods that allow many of these familiar chemical and physical properties to be derived from quantitative 1H or 13C NMR data. We have also developed magnetic field independent data manipulation methods that allow 1H or 13C NMR derived parameters to be utilized as the X matrix “spectral” data rather than the spectra themselves. This allows field independent models to be developed as these parameters are calculated from the spectrum and are the same regardless of the magnetic field strength at which…

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New Conference Being Planned for Practical Applications of NMR in Industry

CASSS announces the first Practical Applications of NMR Conference 2012. Save the Date: October 15-17, 2012. The conference will be held at the Hyatt Regency Schaumberg, Schaumberg, IL USA. John Edwards has volunteered to serve on the organizing committee and will be developing a session of talks on on-line/at-line NMR and TD-NMR technologies. Other exciting sessions will revolve around other practical NMR applications in industry - more details will be posted when the program has been developed further.

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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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Selective Observation of High Resolution 19F Spectrum by 1.4 Tesla Process NMR System

Below is an example of a 19F NMR Spectrum obtained at 54.6 MHz on a 1.4 Tesla permanent magnet-based NMR System. This is a 2 minute spectrum obtained by co-averaging 16 FIDs after zero-fill, autophase, referencing of each individual FID. The NMR system is not locked. No apodization of the NMR FID data was performed. For more details on potential applications of 19F NMR please contact John Edwards (Tel: +1 203-744-5905)

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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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COSA Xentaur Instrument Corporation and Process NMR Associates, LLC sign Application Development Agreement

COSA Xentaur Corporation, the company that specializes in high technology analyzers for a wide range of applications in petrochemical, energy, environmental, pharmaceutical, semiconductor and plastics industries, has joined with Process NMR Associates, LLC (PNA) as its application development partner for Cosa Xentaur’s new spectroscopy based products lines. Initial development will be a Time Domain Nuclear Magnetic Resonance (TD -NMR) to be introduced at PittCon 2011 in March. COSA Xentaur is focused on providing innovative measurement solutions to a wide range of analytical and process applications. It is COSA Xentaur’s philosophy to supply industrial and laboratory users with cutting edge technology in a reliable and affordable instrument with full application engineering and service support. PNA provides solution based applications for a wide range of spectroscopy platforms. These include on-line, at-line, and laboratory automated analyses that are utilized worldwide in petroleum refineries, petrochemical, chemical, and food manufacturing. “Process NMR Associates is pleased to form this partnership with COSA Xentaur,” said Paul Giammatteo, Operations Manager. “This commitment enables both companies to deliver incomparable, solution driven applications on quality instrument platforms to meet the changing needs of analytical laboratories in a number of industries.”

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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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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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ASTM F2259-03 (2008) – Determining the Chemical Composition of Alginates by 1H NMR Spectroscopy

Alginate is a linear polysaccharide composed of mannuronate (M) and a-L-guluronate (G). The polysaccharide is characterized by the relative ratio of M/G, G-Content, and average length of blocks of G in the polymer. M and G are: ASTM F2259 recounts the standard sample preparation and 1H NMR analysis that allows the following parameters to be calculated: The 1H Spectra obtained on a typical alginate sample are show below: Finally the peaks representing the individual M and G components and sequences are deconvoluted from the spectrum. The intensities obtained from the deconvolution are input into the excel spreadsheet shown above and the various ratios, M and G content and a series of diads and triads are calculated along with some G block lkength information. It is the block length information that often reveals telling differences between samples. Process NMR Associates performs this analysis at a cost of $225 per sample. The samples, however, must be prepared by the customer using the methodology set forth in the test method.

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