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 The faithful Varian Unity-300 spectrometer has been replaced by a Mercury-300 VX spectrometer and a second 300 MHz Mercury Plus system has been installed.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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The Role of NMR in FDA Mandated Identity Testing of Nutritional Supplements

Process NMR Associates Offers Testing, Consultation, and Support in Meeting Your Identity Testing, Laboratory Methodology, and Process Analytical Requirements for FDA DS CGMP Rule Compliance. In conjunction with 21 CFR 111, the FDA’s Office of Nutrition, Labeling and Dietary Supplements has instituted the Dietary Supplement Current Good Manufacturing Practice Rule (DS GCMP Rule) and the Interim Final Rule effective December 2010. Laboratory compliance, including identity testing and analytical method protocols are now required for any manufacturer, packager, labeler or holder of dietary supplements without the previous exemption based on number of full time employees within the company. Smaller companies, typically without in-house laboratory and testing facilities, now need to obtain such services to meet the new compliance rules. Process NMR Associates (PNA), the process analytical consulting company and analytical testing company with over 45 years of experience in the field of nuclear magnetic resonance spectroscopy ("NMR") and organic spectroscopy (FTIR, NIR, ESR) is now offering expanded services for DS GCMP Rule compliance. As an example, The International Aloe Science Council (IASC), a trade association representing the global aloe vera industry, has selected Process NMR Associates, LLC (PNA) as its primary provider for Nuclear Magnetic Resonance (NMR) spectroscopic measurement of aloe…

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60 MHz NMR of Essential Oils from Benchtop System – Comparison to 300 MHz NMR Data

A comparison of the non-spinning 60 MHz NMR data compared with that obtained on a superconducting 300 MHz system are shown below for 10 Essential Oils - those essential oils are: Copaibo Balsam, Dill Weed, Citronella, Parsely Seed, Cinnamon Leaf, Balsam (Peru), Ginger, Eucalyptus Globulus, Petitgrain, Vetiver. We currently have a database of 1H (60 and 300 MHz) and 13C NMR data of around 110 essential oils. For further details on NMR analysis of essential oils please contact John Edwards

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Solid-State 13C NMR Analysis of Herbal Supplements

Solid-state 13C NMR is an excellent way to investigate what chemical functionality is present in herbal supplements. The large resonances at 60-105 ppm are due to cellulose/polysaccharides and some sugars. The peaks in the 0-60 ppm region are aliphatic carbons in fatty acid chains. Peaks in the 110-140 ppm region are alkene and aromatic carbons, while peaks in the 140 ppm and 150 ppm region are due to substituted aromatics and phenolic carbons. Peaks in the 160-200 ppm region are due to carboxylic acids, esters and amides. Solid-state NMR is a relatively simple technique that involves no sample preparation and observes the sample carbon chemistry in it's entirety. The analysis reveals relative amounts of chemical functionality that can be utilized for product-to-product comparison or batch-to-batch manufacturing comparison. The chemical specificity of the technique also means that adulterants can readily be detected and identified. A few examples of "off the shelf" herbal supplements are shown below. Figure 1: 13C CP-MAS NMR of Cranberry Extract, Green Tea Extract, and Milk Thistle Extract Figure 2: 13C CP-MAS NMR of Black Cohosh Root Extract, Echinecea Powder, and Bilberry Extract Figure 3: 13C CP-MAS NMR of Valerian Root Extract, Ginseng Extract, Saw Palmetto Extract, Grape…

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Benchtop Permanent Magnet High Resolution NMR Systems

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

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

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

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Press Release: IASC Chooses Process NMR Associates to Provide Analytical Services for Certification Program

The International Aloe Science Council (IASC), a trade association representing the global aloe vera industry, has selected Process NMR Associates, LLC (PNA) as its primary provider for Nuclear Magnetic Resonance (NMR) spectroscopic measurement of aloe vera in regards to the organizations seal-based certification program. PNA’s services include measurement of aloe vera concentration, sacharride distributions, formulation ingredients, and, contaminant/degradation products, in aloe vera powders, whole leaf extracts, whole leaf and inner leaf gel concentrates, drink concentrates, and, ready to drink formulations. The IASC certification program, which offers manufacturers the ability to place a seal on products demonstrating that it meets the established standards for quality and purity of aloe vera products available in the marketplace, has elected to use quantitative 1H NMR analysis as a means to determine compliance. “We are pleased to partner with Process-NMR Associates for providing analytical services related to the certification program,” said Devon Powell, Executive Director of the IASC. “PNA has demonstrated its capability to provide excellent analytical services in a timely manner to the organization and aloe vera industry at-large.” PNA performs the NMR methodology prescribed by IASC, quantifying constituents such as acemannan, and glucose, identifying breakdown products such as acetic acid, lactic acid, pyruvic…

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Process NMR Associates to Present at 3 Meetings

I will be presenting a poster and two invited talks at three meetings this Summer and Fall. The first meeting is Petrophase XI 2010 (11th International Conference on Petroleum Phase Behaviour and Fouling) in Jersey City, NJ, June 13-17 - my poster is entitled: "Improved Approach to the Calculation of Average Molecular Descriptions of Heavy Petroleum Hydrocarbons by Combined Analysis by Quantitative 13C and DEPT-45 NMR Experiments". The poster describes a new methodology for 13C NMR analysis of heavy petroleum materials based on quantitative 13C and DEPT experiments which can be used in combination to calculate an average aromatic cluster size that is consistent with other analysis techniques. Published approaches being used currently underestimate the size of the aromatic groups in heavy petroleum materials. In July I will be presenting an invited talk: "A Self-Employed Application Chemists Odyssey in the World of Analytical Instrument Development The Viability of a $50K High Resolution NMR and $15K ESR Spectrometers", at the University of South Dakota, Vermillion, SD. The date has yet to be set. I will be presenting an invited talk in a session on reaction monitoring with NMR at SMASH 2010 in Portland Oregon, September 26-29 - my talk is entitled:…

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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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Permanent Magnet Based NMR for Omega-3 Fatty Acid Analysis

We are currently developing a spinner system for the process NMR system in order to improve spectral resolution sufficiently to quantify omega-3 fatty acids in fish oils. The omega-3 fatty acid methyl group can be discerned in the 1H spectra currently produced by the spectrometer but improvement can be made with sample spinning which will improve the quantitation.

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NMR Post-Processing Freeware

It was announced this week that the ACD NMR Processor Academic Edition is freely available for non-commercial use and can be downloaded from the ACD Website. Other Windows based NMR processing software packages are available and here is a listing of where they can be downloaded: 1) SpinWorks - written by Kirk Marat at the University of Manitoba - Download Here 2) GSim - written by Vadim Zorin Download Here 3) RNMR (Requires R Statistical Freeware Package) - Download Here - R Software can be obtained here 4) MatNMR (Requires MATLAB) - Download Here 5) Hires - Download Here

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Digital Spectrometers Will Change the Marketplace for NMR Technology

Digital Spectrometers based on field programmable gate arrays will soon change the face of NMR spectroscopy as a routine use analytical instrument. Stan Sykora in his excellent blog (http://www.ebyte.it/stan/blog07.html#07jun14) describes how the transition of NMR spectrometers to digital electronics has drastically reduced the footprint and price of NMR spectrometers and increased the potential complexity of the RF synthesis as well as the NMR post processing on the same chip. In fact single chips can hold multiple spectrometers enabling the building of single spectrometers that can perform experiments on multiple magnet systems. One of the best journal articles on the topic is by Kazuyuki Takeda "OPENCORE NMR: Open-source core modules for implementing an integrated FPGA-based NMR spectrometer", Journal of Magnetic Resonance, 192(2), 218-229, 2008. This gentleman also included all the core modules, console software, pulse programs and board designs required to build your own spectrometer (see Opencore Website). The availability of superconducting NMR magnets are still the barrier to entry for cheaper high field NMR systems but in the lower field NMR area these spectrometers will enable a drastic reduction in instrumentation cost and perhaps lead to a larger NMR market. In the near future I feel that NMR systems in…

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Reaction Monitoring by Process NMR

Presented here are several simple reactions monitored by 60 MHz process NMR performed in a 5 mm NMR tube. Reaction #1: Acetic Anhydride in Water - Reacts to form Acetic Acid NMR Monitored Reaction Profile Reaction #2: Acetic Anhydride + Excess of Methanol + Acid - Yields Acetic Acid and Acetic Methyl Ester First Reaction was Performed without Shaking the Sample before Observation NMR Monitored Reaction Profile Second Reaction was Performed with a vigorous shake of the NMR tube before observation. NMR Monitored Reaction Profile For More Information Contact John Edwards

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Examples of 60 MHz Process NMR Spectral Resolution

These are non-spinning spectra obtained on a Qualion process NMR spectrometer operating at 58 MHz. The spec on water at this shim level is 1.5/5/20 Hz at 50%/10%/0.5% peak height. The first spectrum is of 91% isopropyl alcohol in water - store bought pharmacy product. The second spectrum shows the comparison of a 300 MHz 1H NMR spectrum of Advil compared to a non-spinning 58 MHz spectrum.

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A Self-Employed Application Chemists Odyssey in the World of Analytical Instrument Development: The Viability of a $50K High Resolution NMR and $15K ESR Spectrometers

Presented at Marist College, Poughkeepsie September 23, 2009 A Self-Employed Application Chemists Odyssey in the World of Analytical Instrument Development The Viability of a $50K High Resolution NMR and $15K ESR Spectrometers By John C. Edwards, Ph.D. Process NMR Associates, LLC, Danbury CT The availability of cheap commodity electronics developed for the cellular phone industry is revolutionizing the design of NMR and ESR spectrometers. Rather than instruments that fill half a room, cost $200-3,000K+, and intimidate users, it is possible to produce spectrometers that are an order of magnitude cheaper to produce. Examples of NMR and ESR spectrometer development projects will be described as well as the wide-ranging applications that these spectrometers can deliver to the areas or process control, food authentification and automated laboratory analysis. Bio: John Edwards was born and raised in Bolton, UK. He graduated from the University of Durham, UK with a B.Sc. in Chemistry in 1986. He obtained his Ph.D. in Physical Chemistry from the University of South Carolina in 1990, working on solid-state NMR applied to heterogeneous catalysts under the guidance of Professor Paul Ellis. From 1990-1997 he worked as a research chemist at the Texaco R&D facilityin Beacon, NY where he was responsible…

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News: Process NMR Associates and TopNIR Sign Partnership Agreement

Topnir Systems is proud to announce the signature in October 2009 of a Partnership Agreement with Process NMR Associates, LLC. This partnership enables Process NMR to utilize our field proven software in complementary fields NMR and MIR combining forces to deliver total solutions with increased added value to customers. Topnir Systems is a French company leader in the field of online Near InfraRed (NIR) analyzers. Topnir enables measuring and monitoring multiple hydrocarbon streams in less than one minute using a single online system. The company has a long history in the refining and petrochemicals business, being the first world wide to implement an online application designed to measure and control octane number for gasoline production, first NIR on-line application worldwide on Ethylene Plant Naphtha feed (1986), Gasoline (1989) and Crude (1991). The business started in the late 80s within BP Oil, with applications development around gasoline and diesel blending, as well as FCC, CDU, Reformer and Ethylene plant feed andproducts characterization. Major oil companies such as Shell, BP, Repsol, Aramco... have adopted Topnir solutions. Topnir has recently expanded its activities to provide platform independent software for NIR systems already installed in the field. Topnirs modeling technology offers a full set…

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PNA Presentations at 104th Gulf Coast Conference

Paul Giammatteo recently presented two papers at the Gulf Coast conference that was held in Galveston, Texas on January 20-21. His first paper was entitled "Counting Carbons for Tighter Control: Combining GC and NMR to Improve Distillate Manufacturing" and centers on the topics of Simulated distillation correlated to 1H NMR. The second paper was entitled "Analytical Data For Engineering Support: Improving the Lab/Process Interface". This paper details the development of a series of heavy petroleum applications on a Smiths Detection FTIR-ATR spectrometer. PDFs of the presentations can be obtained from the following links: 1) NMR Talk 2) FTIR-ATR Talk

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NMR Analysis of Vinegar for Authentification and Detection of Adulteration

Over the past few years balsamic vinegars have been the subject of a number or NMR studies to determine authenticity, degree of aduleration, and age. 1H NMR has been used to quantify the relative concentrations of a series of organic components (ethanol, fructose, glucose, acetic acid, succinic acid, lactic acid, butandiol, etc (ref 1). 13C NMR has been used to determine the aunthenticity and degree of adulteration (ref 2) as well as the length of the ageing process that a given sample has undergone. Also the formation of glucose and fructose acetates during maturation and ageing has been studied by 1H and 13C NMR. Refs. 1) Caligiani et al., Anal. Chim. Acta, 585 (2007) 110-119 2) Consonni et al., Talanta, 75 (2008) 765-769 3) Consonni et al., Anal. Chim. Acta, 611 (2008) 31-40 4) Consonni and Caligiani, Talanta, 73 (2007) 332-339 5) Cirlini et al, Food Chemistry, 112 (2009) 51-56 The concentration and distribution of the organic components has been found to correlate well with ageing process analysis, identification of adulteration, and determination of authenticity of traditional balsamic vinegars and balsamic vinegars of Modena. Below are a series of spectra showing what can chemistry can be quantified in the balsamic…

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NMR Analysis of Commercial Pear Cider

For comparison with the home made ciders analyzed in the previous posting I am including the NMR of analysis of a commercial pear cider. The previous ciders were very dry while the pear cider was decidedly sweet. The carbohydrate content is a notable difference. The 1H spectrum is shown with chemical components identified.

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1H NMR Analysis of Hard Apple Cider

There have been quite a lot of NMR studies centered around apple cider (non-alcoholic) and apple cider vinegar. However a search of the literature turns up no reference for NMR analysis of hard apple cider. This effort was undertaken to analyse the alcohol content of the ciders and to determine the malic and acetic acid content. Ciders were produced by Dr Tim McMahon of Orange Community College, NY....for his own consumption. Below are the NMR spectra obtained by regular 1H acquisition and with BINOM solvent suppression. Data was obtained on our Varian 300 MHz spectrometer. Samples were prepared by degassing followed by addition of 1 drop of D2O as lock solvent.

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Micro-ESR Spectrometry of Crude Oils

Process NMR Associates, LLC (Danbury CT) and Active Spectrum, Inc (San Carlos CA) are collaborating in the application of micro-ESR technology to petroleum applications. The initial work has focussed on crude oils but will soon be expanded to residues and cracker feedstocks. Five samples of crude oil were tested by Micro-ESR spectrometry. The samples were: 1. Vasconia, Magdalena Basin, Columbia (V=39 ppm) 2. Merey, Eastern Venezuela Basin, Venezuela (V=303 ppm) 3. Oriente, Oriente Basin, Ecuador (V=65 ppm) 4. Qua Iboe, Agbada Formation, Niger Delta (V=2 ppm) 5. Basrah Light, Zubair Zone, Iraq (V=29 ppm) The following spectra were observed: Figure 1: Micro-ESR Spectra of Crude Oil The central peak is a combination of a persistent carbon-centered organic radical (g = 2.003) found in asphaltenes, and a vanadyl (VO2+) peak. The additional smaller peaks are associated with vanadyl only. For producers, the technique could be used to rapidly measure asphaltene concentration on-line. The spin density of the organic radical is a function of the maturity of the oil and will of course vary between deposits. Notwithstanding, rapid electronic measurement of asphaltenes remains a topic of great interest. Similar techniques have also been used to assess the quality of coals. For refiners,…

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

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

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

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

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Solid-State 13C NMR Analysis of Carbonaceous Materials

Over the past 20 years we have obtained the solid-state NMR analysis of pretty much every carbonaceous material that exists - including coal/oil shales/bitumen, polymers/catalysts/fibers, cellulose/polysaccharides/foodstuffs/gels, deposits/dried sewage/meteorites/soils/clays, etc. With the increased attention to coal liquifaction and gasification technologies we have developed an interest in creating an NMR database for coals. Coals were obtained from the Penn State Coal Sample Bank at a very reasonable cost. We have performed CP-MAS, DD-MAS, Variable Contact Time, and T1 inversion recovery experiments on all the samples. We are currently developing regression relationships between the NMR data and the physical and chemical testing data that is provided with the samples. At some point we will write this up as a journal article. Here are some snippets of data from the coal analysis along with a few results obtained on the menagerie of samples we look at on any given day including some oil shales, engine deposits, refinery coke, asphaltenes, and pipe tobacco. Please inquire if you are interested in the details of the above analyses.

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

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

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Schering-Plough Corporation Seeks Process Analytical Technology Manager

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

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The RefinIR – FTIR-ATR Petroleum Product Analyzer

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

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Process NMR Associates Develops Oxford QP-20 Spectrometer Replacement

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

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PNA Presentation at 9th Upstate NY NMR Symposium

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

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Process NMR Sessions at Eastern Analytical Symposium – November 14

Eastern Analytical Symposium - November 12-15, 2007 Garden State Convention Center, Somerset, New Jersey Process NMR Technology Sessions Wednesday, November 14, 2007 Chair: John Edwards, Process NMR Associates Sponsored by Process NMR Associates Process NMR Technology I: High-Resolution Studies 9:00 Introduction to NMR in Process Control John Edwards, Process NMR Associates 9:25 Standardizing and Stabilizing NMR Calibration Transfer Miko DeLevy, Qualion NMR Analyzers 9:50 More from the Barrel - On-line NMR Increases Diesel Production and Quality Paul Giammatteo, Process NMR Associates 10:15 Break 10:35 Taking NMR into the Refining Process: Best Practices and Benefits Marcus Trygstad, Invensys Process Systems 11:00 "Get Your Head Out of the Sand: Use of Reaction NMR to Better Understand Reactions in Process Development" Andreas Kaerner, Eli Lilly 11:25 Direct Prediction of Gasoline Properties for Monitoring Refinery Processes by H-1 NMR Spectroscopy Veena Bansal, Indian Oil Company Process NMR Technology II: Time-Domain Studies Chair: John Edwards, Process NMR Associates Sponsored by Process NMR Associates 2:00 "Recent Developments in Time-domain NMR and Its Applications in Polymer Industry" Harry Xie, Bruker Optics 2:25 "Time-domain NMR: Uses and Contributions to Process Control" Vaughn Davis, Progression 2:50 "Recent Progress of NMR and MRI in Petroleum Exploration" YiQiao Song, Schlumberger-Doll 3:15…

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The Wood-Based Biorefinery in a Petroleum Depleted World

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

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Wine Analysis by NMR

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

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

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

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

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

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TD-NMR Analysis of Catalytic Cracker Feedstocks

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

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13C NMR of FAME Biodiesel

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

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Detailed 13C NMR Analysis of Hydrocarbons – Patent Applications

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

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Naphtha Chemistry Analysis by 1H NMR

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

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NMR Job Opportunity – Saudi Aramco

Saudi Aramco Research and Development are searching for an experienced NMR spectroscopist - see details Anyone who has NMR employment opportunities should contact Process NMR Associates. We would be happy to post you job listing to our blog and website. If interested please e-mail a job description, requirements, and contact information to John Edwards

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Quantifying Adulteration of Licorice With Maltodextrin by Liquid and Solid-State NMR

Three samples were analyzed to determine if liquid or solid-state NMR techniques could be utilized to quantify adulteration of licorice powders by maltodextrin. Samples analyzed were: Maltodextrin, Licorice #1, Licorice #2 Licorice #1 and Licorice #2 were analyzed by a combination of liquid-state 1H and 13C NMR on a Varian Unity-300 spectrometer, and solid-state 13C NMR on a Varian UnityPlus 200 spectrometer. The resulting spectra are shown in the attached plots. One of the Licorice samples is adulterated by maltodextrin to an unknown concentration, the other licorice sample is pure licorice. Which sample was which was not known during the analysis. Initially it was hoped that the addition of maltodextrin to the licorice would be readily observed as new peaks appearing in the spectrum of the licorice sample. However, it can be seen that in both the 1H and 13C NMR there is considerable overlap of the peaks in the spectra of pure licorice and maltodextrin. When no observable maltodextrin peaks could be assigned it was decided to simply use the quantitative integral data from the regions of the spectrum where the maltodextrin overlaps with the licorice spectrum compared to the integrals obtained from regions solely assignable to licorice. In…

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Process NMR Symposia to be held at EAS 2007

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

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Trans Fat Analysis by NMR

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

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