Process NMR Associates

NMR Blog Posts 2008-2009

2009-07-20T11:48:00.001-04:00

NMR Analysis of Vinegar for Authentification and Detection of Adulteration

Posted by: processn in NMR on January 28th, 2009

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 vinegars as well as a few comparative spectra of apple cider vinegar and malt vinegar.

3 Comments

NMR Analysis of Commercial Pear Cider

Posted by: processn in NMR on January 28th, 2009

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

Posted by: processn in NMR on October 31st, 2008

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.

3 Comments

Micro-ESR Spectrometry of Crude Oils

Posted by: processn in NMR on October 31st, 2008

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, vanadium is a contaminant that poisons the refinery catalyst. ESR has been used by refiners since 1962 to rapidly measure vanadium content in crude oil feedstocks both on-line and in laboratories. Active Spectrum Inc.’s Micro-ESR is shown below. It is 2.25″ in diameter by 2.5″ high. Power input is 12-30VDC, and the data interface is USB. The device is available as either an on-line sensor or as a benchtop unit.

Figure 2: Micro-ESR Sensor

Figure 3: Higher Homogeneity Spectrum of Merey Crude

Micro-ESR is complimentary to NMR in that it observes paramagnetic metals and organic radicals which are unobservable by NMR. The stable free radical signal is indicative and quantitative to the amount of asphaltenes in the crude oil sample and vanadium metal content is an important processing parameter for cracking processes as it is active in the passivation of catalysts. NMR on the other hand observed the detailed hydrocarbon chemistry of the sample and yields chemico-physical parameters such as aromaticity, paraffinicity, naphthenicity, distillation, density, PAH distribution. In combination these two technologies yield a detailed picture of the petroleum materials before and during the refining process.

Samples provided by John Edwards of Process NMR Associates, LLC. Micro-ESR analysis provided by James White of Active Spectrum, Inc,

Active Spectrum, Inc. 110 Glenn Way #15, San Carlos, CA 94070 650-610-0720 | 626-628-1970 f |activespectrum.com

Process NMR Associates, LLC. 87A Sand Pit Rd, Danbury, CT 06810 203-744-5905 | 203-743-9297 f |process-nmr.com

PDF Version of Application Note

For more information contact John Edwards (203) 744-5905

7 Comments

Residual Catalytic Cracking (RCC) – Feedstream Analysis by NMR

Posted by: processn in NMR on October 31st, 2008

Current Technique for Feedstream Analysis:
Analysis Performed – Refractive Index, Distillation, Specific Gravity
Calculation Obtained – Watson K-Factor
Outcome: aromatic carbon number, aromatic hydrogen number, total hydrogen content
Proposition: Detailed hydrocarbon analysis for kinetic model development.

Our experience is that an improved and useful analysis can be obtained from NMR
analysis. There are several ways to approach the NMR analysis and the
chemometric approach to correlating NMR data to physico-chemical parameters of
use to process control.

RCC Feedstream Analysis by 1H and 13C NMR: Multivariate Prediction of Chemical and Physical Properties

Presented at the 236th ACS National Meeting, Philadelphia PA, August 17-21, 2008

John C. Edwards Ph.D.
Process NMR Associates LLC
87A Sand Pit Rd, Danbury, CT 06810

Jincheol Kim,
SK Energy Co., Ltd, SK Energy Technology Center,
140-1, Wonchon-dong, Yuseong-gu, Daejeon 305-712, Korea

Summary of Slides

1) 60 MHz process NMR data available from online NMR unit.

2) 300 MHz 1H NMR data available from standard NMR experiments on laboratory NMR system at Process NMR Associates

3) Expansions of 1H NMR data on RCC Feeds

4) Calculated 1H NMR Parameters Represented as an alternative “spectrum” for use in chemometric modeling and linear regression.

5) 13C NMR Data obtained on RCC Feeds

6) Expansions of 13C NMR Data

7) 13C NMR and Average Molecule Parameters Calculated from 13C Spectrum

Calculated 13C NMR Parameters Represented as an alternative “spectrum” for use in chemometric modeling and linear regression.

9) Correlations of Spectra and Calculated Parameters to Physico-Chemical properties of RCC Feeds

10) Correlation of Spectra and Calculated Parameters to Density

11) Variable Selection for Linear Correlation of Calculated NMR Parameters to Physico-Chemical Properties of RCC Feeds.

12) Correlation of Calculated 13C NMR Parameters (C-Type and Average Molecule) with both high resolution 1H and 13C NMR spectra. Models created can be utilized by personnel with no NMR experience to calculate NMR parameters directly from the spectrum without any prior knowledge of integrations or calculations to be performed.

Summary
Chemical and Physical Properties of RCC Feedstreams can be determined
by 1H NMR (at 60 and 300 MHz) and by 13C NMR
H-Type and C-Type Parameters do not provide as good a correlation as is observed
by full spectrum regression. This is due to loss of resolved chemical shift information
when the spectrum is reduced to larger integral areas.
1H NMR can be combined with PLS regression modeling to provide detailed carbon
type analysis for RCC Feeds
Regression analysis of 13C NMR data can be utilized to fully automate the prediction
of 13C NMR type analysis : reducing the necessity for considerable knowledge and
analysis time on the part of the analyst.

For further Detail Contact John Edwards

1 Comment

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

Posted by: processn in NMR, PAT, Process NMR on September 23rd, 2008

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

2 Comments

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

Posted by: processn in NMR, PAT, Process NMR on September 23rd, 2008

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 Giammatteoor phone him at +1 (203) 744-5905 – see the Process NMR Associates website for further information

2 Comments

Quantitative NMR Analysis of Wine – qNMR

Posted by: processn in NMR on September 15th, 2008

Here is an example of a 1H NMR analysis of a 2007 Red Wine submitted for chemical analysis by John W.

If you are interested in wine analysis please contact us.

1 Comment

Solid-State 13C NMR Analysis of Carbonaceous Materials

Posted by: processn in Energy, NMR on September 15th, 2008

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.

1 Comment

60 MHz TD-NMR System

Posted by: processn in NMR, TD-NMR on September 13th, 2008

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).

1 Comment

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

Posted by: processn in Energy, NMR, Process NMR on February 28th, 2008

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 chemically closer to the hydrotreater constraint limit. The strength of NMR is that it quantitatively and accurately observesthe chemistry of each refinery stream and readily relates that chemistry to chemically dependent parameters such as distillation, cetane, freeze points, etc. The NPS strategy is to cut and control CDU diesel production as closely to the dibenzothiophene distillation limit as possible. Figure 1 illustrates this strategy in terms of both current and proposed NMR based measurements.

Figure 1: Overall NMR measurement and control outline highlighting measurement/control strategies.

Let NMR Process Systems deliver Spectro-Molecular Control to your refinery so that you can achieve real economic and production benefits.

3 Comments

Process NMR Associates – Archives – Gasoline Analysis by NMR and Chemometrics – ENC 1996

Posted by: processn in Chemistry, NIR, NMR, Process NMR on January 28th, 2008

Just came across an old presentation on gasoline analysis by NMR and chemometrics with direct comparisons to Mid-IR and NIR. Presented at the Experimental NMR Conference in March 1996….PDF (3 MB)

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Conjugated Diolefins Analysis by COSY NMR

Posted by: processn in Chemistry, NMR on January 28th, 2008

Conjugated diolefins are responsible for fouling of many processes in a refinery. COSY NMR analysis can determine the concentration of these species in many processed petroleum product streams….see PNA webs site.

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Schering-Plough Corporation Seeks Process Analytical Technology Manager

Posted by: processn in IR-ATR, NIR, NMR, PAT, Process NMR on October 29th, 2007

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.comÂ

3 Comments

NPS – IS : A New Approach to Process Analytical

Posted by: processn in Chemistry, Energy, IR-ATR, NIR, NMR, Process NMR, TD-NMR on October 29th, 2007

Press Release – NMR Process Systems – Swagelok Technology Conference, Teaneck NJ -October 23, 2007

NMR Process Systems, LLC Announces : NPS-IS^© – NPS Integrated Solutions

NMR Process Systems (NPS) announces a new era in advanced analyzer and process control solutions for on-line and at-line process applications. NPS’s Integrated Solutions (NPS-IS^©) approach is designed to take advanced on-line analysis to the next level in delivering real engineering and economic benefit to the user.

NPS-IS^©: the first and original source for any and all on-line NMR applications regardless of NMR vendor.

NPS-IS^©: the first to offer integrated advanced analytical solutions using multiple technologies in one box.

NPS-IS^©: the first to offer a fully integrated Swagelok sampling solution for improved sample switching and reliable measurement.

Too many spectroscopic based on-line analyzer projects (FTIR, NIR, NMR) have failed to meet expectations and/or objectives due to:

·Overselling the measurement

·Underestimating the sampling requirements

·Trying to replace all traditional analyzers with one technique.

NMR Process Systems is positioned to deliver the real benefits of advanced analytical systems in petroleum, petrochemical, chemical, food and beverage and pharmaceutical applications. Moving beyond the traditional replacement analyzer philosophy, NPS-IS^© integrating analyzers and advanced controls to deliver real process improvement and economic benefit. Such integration leverages the strength of any individual spectroscopy, shortens per stream analysis time, and builds in internal cross-checking to ensure accuracy.

For more information contact Paul Giammatteo Principal, NMR Process Systems

87A Sand Pit Rd, Danbury, CT 06810 U.S.A. Tel: (203) 744-5905

4 Comments

2008-03-24T13:33:00.000-04:00

May 14, 2007

Wine Analysis by NMR

Filed under: NMR, Process NMR, Chemistry — processn @ 6:38 pm

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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May 15, 2007

Omega-3 Dietary Supplements - NMR Analysis

Filed under: NMR, Chemistry — processn @ 7:39 am

Fish Oils - Flaxseed Oils

NMR is extensively utilized to analyze fish oils and edible oils high in omega-3 fatty acids.

Examples of ¹H and ¹³C data and analysis are provided below:

¹³C NMR Analysis of Fish Oil Supplement

¹³C NMR of Flaxseed Oil Supplement

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June 12, 2007

NMR Analysis of Jasmine Absolute - jasmine officinale - Egypt

Filed under: NMR — processn @ 12:51 pm

NMR analysis of Jasmine Absolute.

For more information on NMR of Essential Oils visit the PNA website.

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October 5, 2007

The Wood-Based Biorefinery in a Petroleum Depleted World

Filed under: NMR, Process NMR, Energy, Chemistry — processn @ 1:08 pm

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 21^st 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 all components of its raw material source for the production of chemicals, fuels, and power.

Woody “lignocellulosic” biomass is a complex, composite material consisting of three polymers in close association: hemicellulose, cellulose, and lignin plus small amounts of low molecular weight extractives and inorganics. In this presentation, a group of synergistic biomass feedstock and “biorefining” technologies under development at SUNY-ESF, in collaboration with many industrial and academic partners, will be discussed including: short-rotation fast growing willow production, biodelignification, hemicellulose extraction, polymer conversion to fermentable sugars, biodegradable thermoplastics and hemicellulose-based composites.

See the Stipanovic Website at SUNY_ESF for further details…..http://www.esf.edu/chemistry/faculty/stipanov.htm

Bio: Dr. Arthur J. Stipanovic is currently Professor and Chair of the Department of Chemistry at the SUNY College of Environmental Science and Forestry (SUNY-ESF) in Syracuse , NY , and also serves as Director, Analytical and Technical Services. His research interests include biodegradable polymers from renewable resources, high-throughput analytical techniques for determining the composition of woody biomass and new processes for the wood-based biorefinery. Dr. Stipanovic received both his B.S. and Ph.D. degrees from SUNY-ESF in polymer chemistry and much of his career was spent at the Texaco R&D labs in Beacon, NY, in new technology and lubricants research. He is a past Councilor and Executive Board member of the Mid-Hudson ACS section and, more recently, has served as Chair of the Syracuse section.

Directions: Vassar College is located off Raymond Avenue in Poughkeepsie , NY. Refer to the following link for driving directions and campus map: http://www.vassar.edu/directions/. Enter the Main Entrance of the campus on Raymond Avenue and go right towards the Mudd Chemistry Building. The Security Guard at the Main Entrance will direct you to parking.

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Process NMR Sessions at Eastern Analytical Symposium - November 14

Filed under: NMR — processn @ 1:26 pm

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 Break

3:35 “Applications of Time-domain NMR to Laboratory and On-line Polymer Analysis”
Maziar Sardashti,ConocoPhillips

4:00 “Challenges in On-line Water Cut Monitoring of Heavy Oil Thermal Operations Using Low Field NMR”
Sergey Kryuchkov, University of Calgary

4:25 “Benchtop Fluoride NMR: A Rapid QC/QA Method”
Chris Borgia, Colgate-Palmolive

Comments (0)

October 7, 2007

PNA Presentation at 9th Upstate NY NMR Symposium

Filed under: NMR, Process NMR — processn @ 8:35 am

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

Tentative Program

Time	Place	Speaker	Title
8:00-9:10 AM	Alumni Lounge Marshall Hall	Check-In Coffee + Bagels Poster Setup	Posters on Display
9:15	Alumni Lounge	Phil Borer Syracuse University	Welcome
9:30	“	Thomas Szyperski SUNY-Buffalo	Where do we stand on GFT projection NMR spectroscopy?
9:55	“	Yibing Wu SUNY-Buffalo	GFT-NMR based high throughput structure determination exemplified for NESG targets NeT4 and SR500A
10:10	“	Arindam Ghosh SUNY-Buffalo	NMR structure of NESG target MR32, a member of the family of Trm112p-like proteins
10:25	“	Bio-Break
10:35	“	David LeMaster Wadsworth Center - NYS Dept. of Health	Electrostatic stabilization and general base catalysis in the active site of the human protein disulfide isomerasea domain monitored by hydrogen exchange
11:00	“	Joseph Hornack RIT	The relaxivity of Gd-(DTPA-BMA) / Cu+2 mixtures and evidence for a Gd-(DTPA-BMA)-Cu complex.
11:25	“	Nelly Aranibar Bristol-Myers Squibb	Metabolomics in Drug Discovery and development
11:50	“	Lunch Poster Session
1:30 PM	140 Baker Lab	Nikolaos Sgourakis Rensselaer Polytechnic Institute	Pressure Effects on the Ensemble Dynamics of ubiquitin at the Picosecond-to-Nanosecond timescale investigated with isotropic reorientational eigenmode dynamics
1:55	“	Paul Giammatteo or John Edwards Process NMR Associates, LLC	New Developments in Non-traditional NMR Applications
2:25	“	George Crull Bristol-Myers Squibb	Extending Solid State NMR to Address Process Development Issues
2:50	“	Gwen Lubey P+G Pharmaceuticals	Solid State NMR Characterization of Risedronate Hydrate Forms and Dehydrated Risedronate
3:15	“	-	Break
3:30	Keynote Lecture	Prof. Ruth Stark CUNY	NMR Structural Studies of Protective Plant Biopolymers

Comments (0)

October 29, 2007

Process NMR Associates Develops Oxford QP-20 Spectrometer Replacement

Filed under: NMR, Process NMR — processn @ 5:29 pm

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, CT 06810 U.S.A. Tel: (203) 744-5905

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The RefinIR - FTIR-ATR Petroleum Product Analyzer

Filed under: Process NMR, Chemistry, IR-ATR — processn @ 5:32 pm

Press Release - NMR Process Systems - Gulf Coast Conference, Galveston Island, Texas - October 17, 2007

NMR Process Systems, LLC and Smith’s Detection Launch RefinIR^TM - 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

Comments (0)

NPS - IS : A New Approach to Process Analytical

Filed under: NMR, Process NMR, TD-NMR, Energy, IR-ATR, Chemistry, NIR — processn @ 5:34 pm

Press Release - NMR Process Systems - Swagelok Technology Conference, Teaneck NJ - October 23, 2007

NMR Process Systems, LLC Announces : NPS-IS^© - NPS – Integrated Solutions

NPS-IS^©: the first and original source for any and all on-line NMR applications regardless of NMR vendor.

NPS-IS^©: the first to offer integrated advanced analytical solutions using multiple technologies “in one box”.

NPS-IS^©: the first to offer a fully integrated Swagelok sampling solution for improved sample switching and reliable measurement.

Too many spectroscopic based on-line analyzer projects (FTIR, NIR, NMR) have failed to meet expectations and/or objectives due to:

· Overselling the measurement

· Underestimating the sampling requirements

· Trying to replace all traditional analyzers with one technique.

NMR Process Systems is positioned to deliver the real benefits of advanced analytical systems in petroleum, petrochemical, chemical, food and beverage and pharmaceutical applications. Moving beyond the traditional replacement analyzer philosophy, “NPS-IS^©” integrating analyzers and advanced controls to deliver real process improvement and economic benefit. Such integration leverages the strength of any individual spectroscopy, shortens per stream analysis time, and builds in internal cross-checking to ensure accuracy.

For more information contact Paul Giammatteo Principal, NMR Process Systems

87A Sand Pit Rd, Danbury, CT 06810 U.S.A. Tel: (203) 744-5905

Comments (0)

Schering-Plough Corporation Seeks Process Analytical Technology Manager

Filed under: NMR, Process NMR, IR-ATR, NIR, PAT — processn @ 8:58 pm

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.

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January 28, 2008

Conjugated Diolefins Analysis by COSY NMR

Filed under: NMR, Chemistry — processn @ 8:51 pm

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Process NMR Associates - Archives - Gasoline Analysis by NMR and Chemometrics - ENC 1996

Filed under: NMR, Process NMR, Chemistry, NIR — processn @ 8:55 pm

Just came across an old presentation on gasoline analysis by NMR and chemometrics with direct comparisons to Mid-IR and NIR. Presented at the Experimental NMR Conference in March 1996….PDF (3 MB)

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February 28, 2008

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

Filed under: NMR, Process NMR, Energy — processn @ 1:18 pm

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 refiner’s 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 hydrotreaters. 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 “chemically” closer to the hydrotreater constraint limit. The strength of NMR is that it quantitatively and accurately “observes” the chemistry of each refinery stream and readily relates that chemistry to chemically dependent parameters such as distillation, cetane, freeze points, etc. The NPS strategy is to cut and control CDU diesel production as closely to the dibenzothiophene distillation limit as possible. Figure 1 illustrates this strategy in terms of both current and proposed NMR based measurements.

Figure 1: Overall NMR measurement and control outline highlighting measurement/control strategies.

Let NMR Process Systems deliver “Spectro-Molecular” Control to your refinery so that you can achieve real economic and production benefits.

2007-04-12T23:06:00.000-04:00

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 Xie, Bruker Optics, “Recent Developments in Time-domain NMR and its Applications in Polymer Industry”

Vaughn Davis, Progression Inc, “Time Domain NMR: Uses and Contributions to Process Control”

YiQiao Song, Schlumberger-Doll, “Recent Progress of NMR and MRI in Petroleum Exploration”

Maziar Sardashti, ConocoPhillips, “Applications of TD NMR to Laboratory and On-line Polymer Analysis”

Sergey Kryuchkov, University of Calgary, “Challenges in Online Water Cut Monitoring of Heavy Oil Thermal Operations Using Low Field NMR”

Chris Borgia, Colgate Palmolive, “Benchtop Fluoride NMR: A Rapid QC/QA Method”

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.

NMR Analysis of Essential Oils - Example of Sri Lankan Citronella

The data below shows the ability of ¹³C NMR to assign the natural product distribution found in essential oils. Once assignment of the oil hgas been obtained by ¹³C NMR the ¹H NMR can also be assigned. For QA/QC a benchtop 60 MHz system has enough resolution that authenticity of essential oils can be performed either visually of by PCA type analysis.

Ger - Geraniol GerAc - Geranyl Acetate iEugMe - Methylisoeugenol Bor - Borneol

aPin - alpha-pinene Lim - Limonene tOci - trans-beta-Ocimene Cen - Camphene

Cllo - Citronellol Clla - Citronellal GenD - Germacrene D aCal - Citral A (Geranial)

aTol - alpha-Terpiniol cOci - cis-beta-Ocimene Myr - Myrcene

Process NMR for Esterification Monitoring and Certification of Biodiesel

¹H NMR has been used extensively to analyze biodiesel the vegetable oil feeds, reaction intermediates, and final products of the biodiesel esterification process.

See Oliviera et al, Talanta 69 (2006) 1278-1284 and Gnothe, J. Am. Oil Chem. Soc 78, 1025-1028 (2001)

The final biodiesel product is a B5 (5% Biodiesel) or B20 (20% Biodiesel) blend of biodiesel in refinery produced diesel fuel. Researchers have performed method developments to analyze the biodiesel content in diesel fuels by NIR using 1H NMR as the primary method to quantify the biodiesel content. (See Jin et al, Fuel 86(7-8), 1201-1207 (2007) and Knothe J. Am. Oil Chem. Soc. 77 489-493 (2001). Process NMR at 60 MHz can be used to quantify the biodiesel directly. Below is an example slide of a biodiesel 1H NMR spectrum compared to two different diesel fuel spectra.

The chemistry that is directly observed in the NMR spectrum as well as the distinct chemical regions that are present in the diesel and biodiesel make this analysis relatively straightforward. Chemometrics can be used or quantitation can be obtained directly from a simple spectral calibration.

Biodiesel Production Monitoring

NMR can be used to follow the reaction of biodiesel directly, the following slides show the steps in the esterification process.

Glycerol content in the biodiesel or unconverted vegetable oil content can be determined easily directly from the spectrum.

Expansion of Incomplete Reaction Series

Work is currently underway to develop NMR calibration models that can predict the various quality parameters specified in ASTM D6751 for biodiesel.

These calibrations, based on either ¹H or ¹³C NMR, when validated would allow rapid testing of biodiesel production batches and would make complete analysis of small production batches economically feasible (there is no point making 300 gallons of biodiesel if you have to perform $2000 of testing on the batch).

Flying J Selects On-Line NMR Technology from NMR Process Systems LLC for Clean Fuels Production and Expansion Program at Bakersfield Refinery

2007-03-20T10:05:00.000-04:00

Press Release - NMR Process Systems - Danbury CT - January 19, 2007

As part of its announced multi-million dollar refinery improvement prog ram , Big West of California, LLC has selected NMR Process Systems LLC (NPS) to provide on-line NMR technology. The NPS integrated sampling and NMR analyzer system will enable the refinery to both increase its diesel production, as well as achieve quality targets needed for the new Clean Fuels Flying J will produce at it’s Bakersfield, CA, refinery. NPS’s NMR technology solutions, coupled with a Swagelok® sampling system, will perform simultaneous, multi-property diesel measurements required for process monitoring and control in the manufacturing of these new fuels. Installation is scheduled for the first quarter of 2007.

NMR Process Systems LLC, of Danbury, Connecticut (www.nmr-automation.com) is a process analytical technology and engineering services company, providing process analytical solutions to maximize plant and manufacturing operations in the refining, petrochemical, pharmaceutical and food industries. Solon, Ohio based Swagelok Company (www.swagelok.com) designs, manufactures, and delivers an expanding range of high-quality fluid system products and solutions.

Contact:
Paul J. Giammatteo
Product and Marketing Manager
NMR Process Systems, LLC
87A Sand Pit Road
Danbury, Connecticut 06810
Tel: +1-203-744-5905
paul@nmr-automation.com
www.nmr-automation.com

2007-03-20T10:04:00.000-04:00

International Humic Substances Society

International Humic Substances Society – details on standard humic and fulvic acid isolation methods – standard materials – NMR reference data on standard materials.

NMR Meetings and Society Links

A few society websites to keep an eye out for meetings as well as a few meeting links that I have come across recently.

International Society for Magnetic Resonance in Medicine

Clinical Magnetic Resonance Society

European Society for Magnetic Resonance in Medicine and Biology

Japanese Society for Magnetic Resonance in Medicine

Society for Cardiovascular Magnetic Resonance

Magnetic Resonance Managers Society

RSC NMR Discussion Group

Finnish NMR Discussion Group

Spanish Magnetic Resonance Society

Austrian NMR Discussion Group

Australian and New Zealand Society for Magnetic Resonance

German Magnetic Resonance Discussion Group

Italian Magnetic Resonance Discussion Group

49th Rocky Mountain Conference on Analytical Chemistry – July 22-26, 2007 – Beaver Run Resort, Breckenridge, Colorado

Society for Applied Spectroscopy
5th Alpine Conference on Solid-State NMR11th Brazilian NMR User Meeting / Workshop: NMR in South America – May 7-11, Rio de Janeiro State, BrazilFor information please contact Sonia Cabral de Menezes

45th Annual Meeting of The NMR Society of Japan Nov. 22-24, Kyoto, Japan

MRS Symposium “Magnetic Resonance in Material Science” Nov. 27 – Dec. 1, Boston, Massachusetts, USA

For further NMR meeting info visit http://www.process-nmr.com/meetings_and_events%202006.htm

September 27, 2006

Interactive NMR Frequency Map With IUPAC NMR Data

A very useful NMR frequency/receptivity map from Alexej Jerschow at New York University – Interactive Map and Table

Excellent Article on “Mobilizing Magnetic Resonance” from Physics World

An excellent view on the latest new technologies appearing on the scene of mobile magnetic resonance. Though the review is fairly thorough in the “new technologies”, it does not mention the mobile permanent magnet based spectrometers currently availbale from Process NMR Associates. I don’t know why traditional mobile NMR instrumentation is repeatedly ignored in this arena. The perception is out there that NMR will always be expensive to buy, maintain and operate. The truth of the matter is that high-resolution NMR instrumentation should cost less than $100K and low field relaxometers should cost below $30K. Automation is possible for all aspects of NMR operation from locking, shimming, pulse sequence calibration, gain settings, and post processing procedures. I’d love to hear comment from people on this as I’ve been scratching my head for years as to why people aren’t interested in low field spectrometers anymore for undergraduate and industrial applications.

September 25, 2006

NMR of Earwax

Yet another masterpiece from tenderbutton – NMR of earwax.

September 19, 2006

EUROMAR 2007 - Magnetic Resonance Conference

The EUROMAR 2007 magnetic resonance conference will be held in Tarragona, Spain, July 1-6 at the Tarragona Trade-Fair and Congress Centre. Satellite meetings will be held on July 6.

September 15, 2006

SMASH Conference 2006: Multi-Sample MAS Probe

I was at the SMASH conference in Burlington Vermont earlier this week and the presentation of the week in my opinion was the multi-sample MAS probe poster by Nelson et al. This is a probe based on a patent (6,937,020) filed by Professor Eric Munson’s NMR group at the University of Kansas, and built by David Lewis of Revolution NMR. The concept involves stacking multiple MAS rotor housings in the probe head and then shuttling them into the central sweet spot of the magnet for acquisition via a pneumatic device attached at the base of the probe. The RF is switched between independent RF inputs and each housing has an independent tune/match capability. The idea is to increase throughput by allowing extra acquisitions to be obtained on other samples during the relaxation delays of the independent experiments.An excellent video demonstration is available on the webpage dedicated to the probe, as well as references to the patent and the journal article covering the development (“Multiple-sample probe for solid-state NMR studies of pharmaceuticals”, Solid State Nuclear Magnetic Resonance 29 (2006), 204 – 213). Commercial release is expected in 2007.

July 28, 2006

New CAPP NMR Method - Olefin Content of Crude Oils, Condensates, and Diluents by 1H NMR

The Canadian Association of Petroleum Producers has produced a test method to quantify olefins in crude oils, condenates and diluents. The method is particularly aimed at heavy oils and bitumens and their products that are not amenable to traditional olefin analysis. The method is published at the following link. We have developed many methods similar to this and have the ability to quantify and speciate the olefins present in the sample. The current CAPP method developed by the Canadian Crude Quality Technical Association (CCQTP) can be used to obtain total olefin content. Further NMR analysis and a few other experiments would allow some more detailed olefin chemistry distributions to be determined as well as observe the presence of conjugated diolefins that would be particularly troublesome in the processing of these materials. 1H NMR spectroscopy can be used very effectively to obtain many chemical and physical properties of crudes, heavy crudes, bitumen, and the distillate products that are produced by these materials. 1H NMR spectral correlation with these properties by PLS or non-linear PLS regression can yield extremely robust models, and for the chemical properties much more detailed chemical structure information can be obtained fro combining 13C NMR data with 1H NMR results.

CCQTP is an association with members that span multiple segments of the Canadian oil industry -it’s history, mission, and membership can be found at the site.

On a related note an excellent technical site dealing with crude oil quality issues cane be found at the Crude Oil Quality Group website, which is a consortium with the following membership, dedicated to developing test methods and quality standards for crude oil trading that go well beyond the traditional gravity and sulfur measurements currently used. There are many additives, processing fluids, corrosive materials that can be found in crude oils that can cause processing issues for the buyer who purchases simply based on density and sulfur. The group has made public much of it’s meeting agenda archives and the presentations given at those meetings. It is an interesting read for those interested in petroleum chemistry issues.

At PNA we have been developing some high field and low field NMR techniques, looking at chemistry and relaxation in crude oils with naphthenic acid and corrosion issues. We would be interested in hearing from anyone interested in woprking with us to develop a relatively straight forward method for NAN and TAN analysis by NMR methods.

Quantitative NMR

Found and interesting site touting quantitative NMR as a new concept….seems strange as 99% of the NMR work I have done is considered quantitative. There is a perception out there that 13C NMR is always qualitative. This has been confirmed to me in conversations with organic chemistry professors who will perform quantitative 1H NMR all day long and even justify higher magnetic field instruments based on lack of resolution in 1H data as they have the perception that 13C is purely qualitative and don’t think of the superior resolution and chemical shift information present in 13C spectra. The website is at qnmr.com, and contains an excellent petroleum chemistry example of the development of quantitative 13C NMR for aromaticity determination by Joe Ray, ex Amoco NMR researcher. There is also an excellent link to a paper on the quantitative NMR of natural products.

Excellent Solid-State NMR Overview at Durham University

There is an excellent overview of solid-state NMR at my alma mater Durham Univeristy in the UK. The page can be found at the following link.

July 21, 2006

What a day! Took my NMR home with me at the end of the day !

Yesterday started typically, ran a few 1H NMR for some customers, developed a low-field NMR method for diesel and kerosene hydrogen content correlated to aromaticity, try to run some fibers for moisture and spin-finish. Suddenly 5:30 loomed, the Mrs called to ask when I’d home for dinner ….. so rather than incur the wrath of the spouse by continuing late with the work, I simply picked up my NMR and went home with it. The new SpinTrack 20 MHz system is essentially a desktop computer sized console with a 6×6×6 inch magnet weighing 14 lbs. The whole shabang runs off a USB connection to my laptop. Thus …. I spent today completing the work from the comfort of my home office … Beautiful ! Tomorrow I might just carry the system upstairs, put it on the coffe table and acquire some more data while watching the Tour de France on TV. Not many people can say they take their NMR machines home with them at night. This could become a regular thing for me.

July 19, 2006

Interesting News on High Temperature Superconductor Systems

Surfing the web I came across a surprising announcement … it appears that Progression Systems is interested in developing a 80 MHz high temperature superconductor electromagent system to utilize in their process NMR business. Does this mean that Progression will be entering the high resolution NMR domain or raising the resonance frequency and sensitivity of nuclei other than proton (27Al, 23Na, 31P, etc.)? Below is the news bulletin from Industrial Research Ltd (News Bulletin found at: http://www.irl.cri.nz/newsandevents/Mediareleases/joint-venture-for-hts110.aspx).

Joint venture for HTS-110A new joint venture between HTS-110 and US company Progression Inc will provide customers with a unique high temperature superconducting (HTS) magnet capability.1 May 2006HTS-110 Limited, an affiliated company of Industrial Research, focuses on HTS solutions for medical, scientific, energy, defence, transport and industrial markets. Progression is a world leader in the development and implementation of process Nuclear Magnetic Resonance (NMR) technologies, Laser Induced Breakdown Spectroscopy (LIBS) techniques, and Laser Induced Fluorescence (LIF) analysers for the mining, petrochemical, and polymer/polyolefin industries.

The new venture, Progression-HTS-110, will provide customers with unique high temperature superconducting (HTS) magnet capability. The new series of analyser will operate at 80MHz with the field strength of 2 Tesla generated by a HTS magnet.

Target markets for the analyser will include refining applications in the oil and gas industry, educational research and development, pharmaceutical and biochemistry applications.

Chief executive of Progression, Vaughn E. Davis, says the company is looking forward to working with HTS-110 Ltd and describes the deal as the perfect complementary vehicle to extend and build on the unique strengths of Progression’s leading market position in process NMR.

Chief executive of HTS-110, Dr Sohail Choudhry, says it is a strategic move to partner with Progression and extend HTS-110’s leading-edge technology into new markets.

“HTS is an advanced and rapidly developing new technology and we look forward to using that as a key driver for expanding the marketplace with Progression.

“Progression is an innovative company and we share a similar culture – that will work to our advantage and allow us to benefit from both our unique and complementary skills.”

It is anticipated the new company will be headquartered in Houston, Texas, under the leadership of Mr. Scott Simmons.

HTS-110 is a subsidiary company of Industrial Research Ltd – it’s HTS magnet technologies are described here.

Process NMR Technology Session Planned for Eastern Analytical Conference 2007

2007-03-20T10:03:00.000-04:00

Press Release - NMR Process Systems - Danbury CT - February 14, 2007

Dr Edwards of Process NMR Associates has been asked to organize a session on Process NMR Technology at the Eastern Analytical Conference to be held at the Garden State Exhibit Center, November 12-15, 2007. Below is a copy of the Call for Papers sent out on February 14, 2007.

Hello to all,

I have been asked by Cecil Dybowski to chair a session on Process NMR Technology at the 2007 Eastern Analytical Symposium to be held November 12-15 at the New Jersey Garden State Exhibit Center in Somerset New Jersey. At this point I am putting out some feelers to gauge the level of interest that is out there amongst NMR practitioners in this field. I would like the session(s) to encompass both high resolution and time-domain applications of NMR in process control applications and at-line in manufacturing facilities in all industry sectors. The work can be actual on-line examples or laboratory based analysis being used to justify or prove applications before they are spun out to the plant. Developments in hardware, software and chemometrics would also be of general interest and to this end hardware talks on magnet and NMR-sensor development and their potential application would be encouraged. Fully automated NMR analysis in the laboratory that simply requires a technician to load the samples would also be considered as a valid topic.

The abstract deadline for EAS is April 15th. If you are interested in presenting a paper I would appreciate hearing from you by e-mail. Once I know how much interest is out there I will begin pulling the details together and have the speakers submit abstracts through the EAS website. For your information the EAS is the premier analytical meeting for the U.S. East coast and it has a website at http://www.eas.org. Also, as an introduction to the symposium itself, I am providing a link to the program chairs letter - http://www.eas.org/symposium/symposium.html

The distribution I have included in this e-mail are of persons and organizations that I know are working in this field. If you have any colleagues, customers, or acquaintances who you feel could provide a good presentation on their research or applications please feel free to forward this e-mail on to them, or inform me of their e-mail address and I will contact them.

I look forward to hearing from you and hope that you will join us in New Jersey,

Best Regards,

John

Contact : John Edwards, (203) 744-5905 E-Mail: john@process-nmr.com

2006-07-17T16:30:00.000-04:00

July 17, 2006
Abstracts Available for Magnetic Resonance in Food Science Meeting
The Abstracts for the Posters and Speaker Sessions of the 8th International Conference on The Application of Magnetic Resonance in Food Science (July 16-19, 2006) can be found at the following locations – Poster Abstracts and Speaker Abstracts .

July 13, 2006
Stelar Develops New Benchtop FFC Spectrometer and Forms JV Company Invento
Stelar s.r.l. has announced that it will be producing a new benchtop design for it’s Fast Field Cycling NMR product becoming available in September 2006, and also the availability of a new single board NMR console - available June 2006. the company has also formed a JV company called Invento s.r.l. which is a combination of Stelar and a business incubator at the Univerity of Torino. The mission of Invento is to further the development of FFC NMR techniques as standard methodolgies in testing laboratories and to perhaps replace other TD-NMR spectrometers.

July 11, 2006
NMR Monitoring of Magnetic Field Strength of CERN Large Hadron Collider
A group of physicists at the University of Manchester are developing NMR probe technologies to monitor the magnetic field strength inside the solenoids of the Atlas LHC at CERN. The probe technology and accompanying NMR spectrometers are described on the Manchester website.

July 3, 2006
Process NMR Paper at San Francisco ACS Meeting - September 2006
ENITechnologie will be presenting a paper on the on-line application of NMR in lube plant operation at the upcoming ACS Meeting in San Francisco.

Experiencing Process MRA Industrial Lube Plant Application – Roberto Giardino1, Silvia Guanziroli1, Cinzia Passerini1, and Antonio Farina2. (1) EniTecnologie S.p.A, via Maritano, 26, San Donato M.se (MI), 20097, Italy, (2) Divisione Refining & Marketing – Raffineria di Livorno, Eni S.p.A, via Aurelia, 7, 57017 Stagno (LI), Italy.
In a conventional base oil production plant the operating conditions needed to produce products at a desired specification are very sensitive to feed quality. At Livorno refinery an on-line Process Magnetic Resonance Analyzer (MRA) has been installed to identify the feedstock and product composition and properly set an advanced process control system. By using MRA it is possible to reduce the product quality give-away due to feed quality variation. In this work the industrial experience acquired is reported.
Characterization, On-Line Monitoring, and Sensing of Petroleums and Petrochemicals 8:30 AM-11:30 AM, Thursday, 14 September 2006 Sheraton Palace—Telegraph Hill
Division of Petroleum Chemistry The 232nd ACS National Meeting, San Francisco, CA, September 10-14, 2006

June 19, 2006
Application Overview for Spin Track TD-NMR Spectrometers
Due to it’s broad versatility the Spin Track NMR Hardware supports all standard NMR routines such as AOCS Cd 16b-93, AOCS Cd 16-81, ISO 8292, IUPAC2.150 and creative scientific research. Spin Track has been successfully approved in the food and polymer industries for routine analysis. If your application is not described below please contact John Edwards for discussion.
Solid Fat Content (SFC) AnalysisThe quality of food products containing fats and oils depends on solid fat content (SFC). SFC determination is an essential measurement in the baking, confectionery, and fat industries. NMR has been established as the method for SFC determination by ISO 8292. Measurements of SFC by the Spin Track NMR analyzer can be performed quickly and accurately with great benefit for the manufacturer.
Simultaneous Rapid-Determination of Oil and Water in SeedsSunflower, soybean, groundnut, rape and mustard are appreciated for their oil content, but excess of water content reduces their price. Thus, an accurate and fast determination of oil and water content is important to both manufacturers and customers. The Spin Track NMR analyzer meets ISO 10565 requirements and gives the possibility to simultaneously determine of oil and water content.
Oil/Fat and Moisture analysis in Chocolate, Powdered Milk, Cheese and other Food ProductsTime of storage of food products depends strongly on moisture content. Excess moisture leads to microbiological activity and can make food consumption dangerous. Fat and moisture content also heavily influence taste. Manufacturers are also regulated to disclose the exact information on the fat content of their products. NMR is the most rapid and exact method to determine these essential parameters. The Spin Track NMR analyzer is especially suitable for regular analysis of food quality.
Curing Degree and Elasticity Analysis in Rubber-Type Materials
Over the past years Rheology has become widely accepted as a tool in the investigation of rubber properties. However, rheological testing equipment can be extremely expensive and complicated. NMR is very sensitive to the structure and properties of investigated rubber materials. The Spin Track NMR-analyzer allows investigators to obtain data complementary to rheology and can also prove to be more informative.
Moisture and Crystallinity Analysis in PolysaccharidesPolysaccharides like chitin, chitosan etc. are widely used because of inherent unique properties. Adsorbents and food bio-additions based on them require a regular check of quality. Spin Track NMR-analyzer allows investigators to obtain information about moisture, crystallinity, purity and structure of polysaccharides.
Porosity of Rock Cores/Heterogeneous Catalysts/ZeolitesThe possibility of oil development can be defined more exactly in the initial stages of exploration by using NMR. Rock cores saturated by bitumen or water provide information on degree of saturation, structure of saturating compounds, porosity, and diffusion characteristics. This information allows the prediction of oil production yields. The Spin Track NMR-analyzer with a 35mm probe gives the possibility to obtain such information.
Scientific applicationsThe spectrometer’s Relax software allows construction of many types of NMR pulse sequences, user-defined interfaces, data processing (digital experiments filtering, fitting, Fourier and Laplace transforms) and data manipulations. Thus, customers can directly run automated standard type NMR experiments just by “pressing one button” in the program shell, or create new applications using the powerful pascal-like script language. Widely used experiments like measurements of T1 and T2 (90-tau-90, 180-tau-90, CPMG, FID, Spin Echo, Solid-Echo) are included into the Relax software as default examples. The NMR measurements can be accompanied with the high precision calibration samples and built-in software calibration procedures. Easy automatic tuning of the NMR frequency, pulse-durations, TX power and RX gain is included into the software package.

Process NMR Associates Begins Marketing of Cutting Edge TD-NMR Spectrometer
Resonance Systems Ltd. has granted Process NMR Associates the rights to promote, market, and sell it’s NMR products and custom NMR hardware in the Americas, and Worldwide. The basic product of the company is a portable NMR-analyzer called Spin Track that can be used for many different low and high resolution NMR applications.
Spin Track meets the requirements of many relaxation and diffusion based NMR analyses:
Food industry (Solid Fat Content Analysis, Dairy Products, Oil and Moisture in Chocolate, Powdered Milk, Cheese and other food products; Oil and Moisture in seeds, Emulsion Characteristics)Lipid Analysis – Fatty Acid DistributionCellulose and paper manufacturing (Moisture/Crystallinity Analysis, investigations of ageing effects)Oil industry (rock cores analysis, oil-water, oil-water-gas, viscosity, physical property correlation, )Polymer and rubber industry (Curing degree and elasticity analysis, polymer ageing, glass transition, amorphous/crystalline content)Chemical industry (Density, Melting Points, Copolymer Ratios, Compatibility, Cure, Cross Linking, H or F content,Medicine (NMR Surface Analysis of Patients, Plasma Analysis)Environmental (Water Pollution, Forest Degradation, Soils, Fertilizers)Fibers – Moisture and Finish ContentPharmaceuticals (Tablet Analysis, Coatings/Components/Moisture, Hydrogen/Fluorine/Sodium Content)Relaxation, Diffusion, Particle Size, Pore Size Distribution
Utilization of mobile NMR measurement equipment from Process NMR Associates provides the following advantages:
Reduction of expenses associated with meeting quality requirements of productsSimplicity of use in routine production measurements and in advanced laboratories for complicated analysisMobility of the hardware and low cost for the overall deviceNon-invasive measurements of any sampleHardware solutions for non-standard NMR applicationsPermanent technical support and comprehensive scientific consultingFair price and absolute ease of operation!
Portable Low-Resolution NMR Analyzer
Analyzer is designed to perform:
All standard NMR applicationsDevelopment of new NMR-based techniquesTeaching quantum physics, NMR, analytical chemistry in Universities and Colleges
NMR analyzer Spin Track comprises functional parts (probes, preamplifier and duplexer, TX Power Amplifier, Sequence Generator and PC Interface, Data Acquisition System, NMR Transceiver) which can be purchased separately and used for the specific needs of an advanced customer (see example of connection assembly). Depending on the required magnet system the Spin Track can be used as NMR relaxometer or high resolution NMR spectrometer.
Basic characteristics of Spin Track analyzer:
Frequency range of the NMR spectrometer module: 5..60 MHz
Ringing time for 10 mm NMR probe is 8 ms
Probe tube diameter: up to 35 mm
Changeable preamplifiers and 50 Ohm matched duplexers with self bandwidth of 5 MHz
Customer-defined set of sensors (5, 10 and 30mm test-tube magnet systems, NMR surface sensors)
Adjustable TX output power up to 400 Watts
Adjustable RX channel gain up to 107
RX Sensitivity better than 1 mV (conditions: signal to noise ratio 3)
Adjustable digital filter bandwidth from 100 Hz up to 1 MHz
Pulse sequence length up to 64K events with resolution 100 ns
Quadrature 64Kx10-bit data acquisition system
Complete control of functions via personal computer – USB 2.0 ConnectivityFast sensors replacement
Compatible with all Microsoft® Windows® operating systems
Software
The product software, Relax, is a powerful tool containing many standard NMR relaxation routines and applications, and can also be used to create new pulse-sequences, pulsed field gradients, gains and attenuations, post-processing methodolgies of considerable complexity. The built-in script language is based on a widespread Pascal syntax and is enriched with commands for fitting, Fourier and Laplace transforms, Low-pass filtering, etc. The script supports dialogue windows, static messages, user-defined diagrams, data manipulation procedures. Relax also allows direct processing of data obtained when utilizing Spin Track as a high-resolution NMR spectrometer.
Stationary Low-Resolution TD-NMR Analyzer
Analyzer is designed to perform:
Standard routine NMR applicationsDevelopment of new NMR-based techniquesTeaching quantum physics, NMR, and analytical chemistry in Universities and Colleges
The Spin Track Stationary fulfills all requirements to conduct NMR measurements like portable version of NMR analyzer.In addition it is supplied with the possibility for increased probe volume to facilitate excellent statistical averaging of experimental results or to accomodate large samples.
Basic characteristics of Stationary Spin Track Analyzer:
Frequency range of the NMR spectrometer module: 5..60 MHz
Ringing time for 10 mm NMR probe is 8 ms
Probe tube diameter: up to 35 mm
Changeable preamplifiers and 50 Ohm matched duplexers with self bandwidth of 5 MHz
Customer-defined set of sensors (5, 10 and 30mm test-tube magnet systems, NMR surface sensors)
Adjustable TX output power up to 400 Watts
Adjustable RX channel gain up to 107RX Sensitivity better than 1 mV (conditions: signal to noise ratio 3)
Adjustable digital filter bandwidth from 100 Hz up to 1 MHz
Pulse sequence length up to 64K events with resolution 100 ns
Quadrature 64Kx10-bit data acquisition system
Complete control of functions via personal computer – USB 2.0 ConnectivityFast sensors replacement
Compatible with all Microsoft® Windows® operating systems
Relax Software
Educational Low-Resolution TD-NMR Spectrometer
Analyzer is designed to demonstrate NMR spin dynamics as well as provide a basic platform for undergraduate level chemistry and physics labs.Standard routine NMR applications (FID, Spin Echo, CPMG, Carr-Purcell, T1-Determination (90-90 or inversion recovery))Development of new NMR-based techniques – software allows development of pulse sequences by students without risk of instrument damage.Teaching quantum physics, NMR, and analytical chemistry in Universities and Colleges
Basic characteristics of Stationary Spin Track Analyzer:
Frequency range of the NMR spectrometer module: 10..20 MHz
NMR Probe tube diameter: 5 mm
10-20 MHz Magnets,
Surface NMR Sensors
Changeable preamplifiers and 50 Ohm matched duplexers with self bandwidth of 5 MHz
Adjustable TX output power up to 100 Watts
Adjustable RX channel gain up to 107
RX Sensitivity better than 1 mV (conditions: signal to noise ratio 3)
Adjustable digital filter bandwidth from 100 Hz up to 1 MHz
Pulse sequence length up to 64K events with resolution 100 ns
Quadrature 64Kx10-bit data acquisition system
Complete control of functions via personal computer – USB 2.0 ConnectivityCompatible with all Microsoft® Windows® operating systems
Relax Software
Custom NMR Components
For NMR engineers and advanced specialists Process NMR Associates offers accessories to upgrade, modernize, or build new NMR related devices (see connection example). All modules can be purchased separately and modules can be developed with unique characteristics to fulfill special requirements of the customer.
Surface NMR Sensors NMR Sequence Generator
Data Acquisition Unit Wide-Band NMR Transceiver
NMR Power Amplifier NMR Pre-Amplifiers and Duplexers
For more information and pricing please contact John Edwards
Back to Process NMR Associates Home Page

June 1, 2006
United States Department of the Interior - Oil Shale and Tar Sands Leasing Programmatic EIS
The public forum site of the department of the interior related to the environmental impact statement is found at the following location. The site contains excellent overviews of the tar sands and oil shales found in Wyoming-Colorado-Utah. Excellent Oil Shale site from the DOE with strategic significance reports and government policy statements.

Bruker BioSciences Corporation Announces Agreement to Acquire Bruker Optics Inc.
An interesting news article from Bruker world – “Bruker BioSciences Corporation Announces Agreement to Acquire Bruker Optics Inc. for $135 Million in Cash and Stock” dated April 17, 2006. Fascinating…. of particular interest from the process analytical and molecular spectroscopy side was Bruker Optics VP Dan Klevisha’s comment – ” For Bruker Optics, becoming part of a larger and public company will also allow us to explore complementary acquisitions.”

Materials Research Society - Symposium on Magnetic Resonance in Material Science
The Materials Research Society announces a call for papers for it’s Symposium (MM) on Magentic Resonance in Material Science to be held at the Fall Meeting in Boston on November 27 – December 1, 2006. Abstracts are due by June 20th.

Alternative Sources of NMR Equipment - Beyond the Big 3
There are a number of alternatives to buying new systems from Bruker-Varian-JEOL. A number of third party suppliers are present in the market selling and supporting refurbished used NMR systems. These companies can install and warranty the systems as well as maintain the cryogens for you if you wish. The companies that specialize in supercon NMR systems are Triangle Analytical, RS2D, NMR Associates, and MR Resources. A great place for used probes and repair is J S Research. Consoles can be obtained from Tecmag and from Anasazi (Anasazi also provides refurbished 60 and 90 MHz electro/permanent magnet systems). Spincore provides NMR spectrometer components for those who want to build their own instruments. Magritek, Minispec, Oxford Instruments, Resonance Systems, Progression, PCT, all sell TD-NMR instruments.
Process NMR Associates can guide you through this maze of choices.

May 31, 2006
Stan’s NMR Blog - Two Articles on Magnetic Field Noise Effects
Stan Sykora continues to expand his excellent NMR blog with two new articles on NMR signal reproducibility. His articles cover how field noise effects the repeatability of NMR signals such as FIDs and spectra and Hahn echoes and CPMG trains. In our experience of online NMR we have worked extensively on this topic with respect to the repeatability of the processed NMR spectrum and it’s effect on the repeatability/reproducibility of the chemometric predictions employed for process control. As Stan notes, if people have done a lot of work in this area it is certainly not being reported … mea culpa.

FAPRI World Agricultural Outlook 2006
The Food and Agricultural Policy Research Institute has published it’s annual U.S and World Agricultural Outlook for 2006.

May 30, 2006
Online TD-NMR Analyzers for 19F and 31P Analysis of Minerals and Phosphates
I guess you learn something everyday… The Harrison R. Cooper Systems Company of Bountiful Utah has been marketing low field Phosphorus-31 and Fluorine-19 NMR analyzers for a phospate mineral benefication process and for fluorine monitoring in mineral slurries. It appears from the site that only a few installations were made and no indication of successful outcomes or benefits are provided in the analyzer and process descriptions. I can’t decipher where the NMR technology originated….perhaps Auburn?

May 26, 2006
21.1 Tesla Quench Video
The University of Colorado Health Science Center installed a pumped 900 MHz system in 2005. They have an awesome video of a deliberate quench of the magnet as part of the ramping protocol. Here is the link to the video and here is a link to the NIH funded facility.

1H and 13C Shifts of Common NMR Solvents - Excel Table
Edward Vawter of QD Information Services has made available two useful excel spreadsheets containing the 1H chemical shifts and 13C chemical shifts of most common deuterated NMR solvents. He also has a few other useful articles available from his download page.

Hilarious NMR Adventures at Stanford
Dylan Stiles at Stanford has an often hilarious blog category dedicated to the NMR aspects of his natural product synthesis projects. He gets a lot of commentary which is great as I think he has the only NMR blog that anyone cares to read. His blog is at http://blog.tenderbutton.com/?cat=9.

NMR Post-Processing Software for Mac Users
Phillip Grandinetti of Ohio State University (Research Group Site) offers an NMR post processing program for mac users called RMN at his website. He has an alpha version that runs under OS X and he is looking for alpha-testers to kick the tires. A more mature version is available that runs under Mac Classic OS.
Mestrec laboratories also offer a cheap (50/100 Euro) software package that is available at iNMR.

May 22, 2006
AMMRL Meeting at 47th ENC - Asilomar, CA, April 2006 - Presentations
The AMMRL (Association of Managers in Magnetic Resonance Laboratories) held an annual meeting at which a number of presentations were given that give an idea of the economics and issues that arise for University NMR Facility Managers and Administrators, the links are below:Charlie Fry—IntroductionKen Visscher—Open-Access Laboratories in Industry Nick Burlinson—Design and Installation of a Departmental NMR FacilityEugene DeRose—Problems and Protections for Pumped Magnets Josh Kurutz—A Survey of Business Models for Academic Facilities David Vander Velde—Cryoprobes and Money (a.k.a. Losing Money) Klaas Hallenga—Practical Tips and Tricks with Cryogenic Probes
The AMMRL has a website with some basic information at http://chemnmr.colorado.edu/ammrl/ and has an invaluable archive of “user group” e-mails that discuss all aspects of running and maintaining an NMR facility (Email – Archives 1993-Present). If you have a question about instrument problems, instrument and cryogen maintenance, user training, user competency, safety issues, etc …. chances are the answers are already included in this database. The database can also be searched by key word to arrive at “on-topic” material.

May 18, 2006
The Anatomy of a Superconducting NMR Magnet
Dr Joseph Vaughn of Florida State University has placed an autopsy of a Varian R2D2 7.05 Tesla NMR magnet on the department website. The innards of the magnet and probe are all exposed in the gory photographs. Check it out at the FSU chemistry site : http://www.chem.fsu.edu/facilities/cutaway_nmr_magnet.asp
This is one of the siblings of the magnets that we operate in our labortory at Process NMR Associates. The site is only for those with a strong stomach.

May 16, 2006
8th International Bologna Conference on Magnetic Resonance in Porous Media
Filed under: PNA, Process NMR, Analytical NMR — Administrator @ 11:58 am
This conference (MRPM8) will be held September 10-14 at the University of Bologna, Italy. It is being held a few days after the 6th Colloquium on Mobile magnetic Resonance in Aachen Germany, (September 6-8, CMMR6) to facilitate the attendance of conferees at both meetings.

May 3, 2006
Symbion Systems Inc
Symbion Systems Inc has developed a family of software products that provide a common interface for communicating with, networking, and controlling many analytical instruments, and sample systems, in a laboratory or process analysis setting. The software can control many individual analyzers from different vendors, process the data and visualize it, store the data in SQL databases, and perform complex chemometric analysis by calling various calibrations from many chemometric software platforms. The predictions obtained from process analytical instrumentation can be plotted, visualized, stored, and outputted under many standard formats for integration with process control and optimization software. A version can be obtained that is GLP/GMP/21 CFR, Part 11 compliant. The software will provide an excellent platform for development and execution of analytical laboratory methods, as well as process analytical applications.

One Moon Scientific Inc.
Bruce Johnson of One Moon Scientific (ex Merck) has produced a series of software tools for visualizing and analyzing spectroscopic data with particular emphasis on NMR data. His NMRViewJ can process and visualize NMR datasets in 1 or multiple dimensions and has built in molecular visualization and statistical data analysis tools. The software is “free” but Bruce asks that if you download and use it you should pay a “support contract fee” in order to support the ongoing development of the NMR software products.

April 26, 2006
16th ISMAR 2007 - Website Posted
Filed under: Analytical NMR — Administrator @ 11:09 am
The International Society of Magnetic Resonance announces the 16th Triennial Conference to be held at Kenting, Taiwan, October 14-19, 2007. Organized by the Taiwan Magnetic Resonance Society, Academia Sinica, Taiwan – Website is found at http://www.ismar2007.sinica.edu.tw/

April 1, 2006
Energy Information
Here are a few excellent links to the energy situation in the 21st Century:
Energy Technologies for the Twenty-First CenturyWEC - Survey of Energy Resources 2001 DOE - This Week in Petroleum Energy Information Administration – Main Site
Comments (0)
March 15, 2006
Modern Drug Discovery - NMR Articles
Filed under: Analytical NMR — Administrator @ 2:00 pm
ACS Publication “Modern Drug Discovery” – Available NMR ArticlesScreening with NMRNMR Spectroscopy Software – Molecular biologists can now use proton NMR data to elucidate protein structure.NMR on Target Ultracool NMR Technology – Cryoprobes Looking for Quality

March 14, 2006
NMR of Silicones in Pharmaceutical Developments
Dow Corning have published a small overview paper on manufacturing processes and development of silicones in pharmaceutical formulations. The paper includes characterization details by FT-IR and NMR.

The 6th Colloquium on Mobile Magnetic Resonance - Official Website now Posted
The 6th Colloquium on Mobile Magnetic Resonance has now posted an official website to cover the meeting at http://www.cmmr.de/index.htm

March 13, 2006
PNA Talk - Dr Giammatteo to Present Sigma Xi Seminar at Quinnipiac University
Hamden, Conn. – Dr. Paul J. Giammatteo, co-founder of Process NMR Associates, will present “Pulse, Acquire, Control: Ten Years of Online High-Resolution Nuclear Magnetic Resonance (NMR) in Refining, Petrochemical and Food Manufacturing” at 12 p.m. on Monday, March 27, in the Clarice L. Buckman Theater at Quinnipiac University.
The free lecture is open to the public and is part of Sigma XI Special Seminar Series.
From gasoline manufacturing to butter production, more than 140 online NMRs have been placed in manufacturing plants worldwide. Giammatteo will discuss installation and utilization of this technology, its application in the petroleum and petrochemical industries and the future in pharmaceuticals.
Giammatteo co-founded Process NMR Associates, based in Danbury, in 1997. He previously worked for Texaco for 17 years. Giammatteo received his doctorate in chemistry from Wesleyan University and has published and presented more than 30 papers.
For more information, contact James Kirby, associate professor of chemistry at Quinnipiac, at (203) 582-8275 or James.Kirby@quinnipiac.edu

March 10, 2006
NMR Applications in Food Quality
Overview document on Belgian Science Policy as it pertains to the use of low and high field NMR in the quality control of food.
Quantification by 1H NMR of Fatty Acids and Their Derivatives – by G. Knothe – USDA
An incredible repository of NMR information related to 1H and 13C NMR of Fatty Acids and their derivatives is found at the Lipid Library.

What is Your Carbon Footprint?
A handy calculator from BP allows you to calculate your impact on global warming – Carbon Calculator.

Heavy Oil and Bitumen Upgrading
“Bitumen from Canadian Oil Sands – The Worlds New Marginal Supply of Oil” – January 2006
“Oil Sands: Alberta’s Opportunity to Become a Significant Oil Exporter” – by Fluor, February 2004.
National Center for Upgrading Technology – Conference on “Upgrading and Refining of Heavy Oil, Bitumen and Synthetic Crude Oil” – September 2006 – Details
“Bitumen and Very Heavy Crude Upgrading Technology – A Review of Long Term R&D Opportunities” March 2004
Genoil demonstration of an upgraded bitumen – effects on TBP and other physical properties.
“Fueling an Integrated Energy Future” – Energy Innovation Network, December 2004
Kearl Lake Bitumen Extraction Project
“Historical Perspective of the Heavy Oil Resources of Utah”
USGS - “Heavy Oil and Natural Bitumen-Strategic Petroleum Resources”
“Non-Conventional Hydrocarbons – Where and How Much”
Energy Independence for North America Through Heavy Oil Upgrading – Presentation – same material but presented as a Paper
Alberta Energy Research Institute – Strategic Research Plan
Shell – Gasification in Heavy Oil Upgrading in Alberta
“The Impact of Emerging Research Techniques on Exploitation and Refining Technology Development” John Shaw – University of Alberta
“Alberta’s Oils Sands Opportunity”
Jacobs Engineering – Oils Sands Production Presentation
Total – Tar Sands Production Presentation
Effect of Tar Sands on World Oil Supply – Imperial Oil
Association for the Study of Peak Oil & Gas
Alternative Fuels – An Energy technology Perspective – March 2005
“Integration Opportunities for Coal/Oil Coprocessing With Existing Refineries”
Oil Sands Supply Outlook – March 2004

March 9, 2006
Spatial Encoding Produces 2D-NMR in a Single Scan
Ultrafast 2D NMR spectroscopy obtained in a single scan is described by Lucio Frydman of the Weizman Institutein his paper entitled “Single Scan 2D NMR”

Metabonomics Overview - High Field 1H NMR in Metabolite Profiling
Professor John Lindon (Metabometrix Ltd) provides an Overview of Metabonomics relating the role of high field 1H NMR in metabolite profiling in biofluids.

March 1, 2006
Polymer Chemistry Resource
Beautiful site that gives overviews of most polymer chemistry systems.

2006-03-01T10:43:00.000-05:00

DECRA-FID Processing to Obtain Quantitative NMR Data???? March 1st, 2006

A strange CPACT NMR project development – DECRA processing of FID data - this involves quantitative analysis of FID signals in order to avoid automated phasing routines – in our process NMR experience phasing is a critical issue in the reproducibility of online NMR data, however, it is not an unsurmountable problem that leads to the development of new processing techniques such as those described here. Robust, repeatable phasing algorithms can be developed and implemented.

The Oil Drum - Peak Oil Blog March 1st, 2006

The Oil Drum is a blog dealing with the impending global problem of Peak Oil Production also called “Hubbert’s Peak” – or should we say Peak “Easy” Oil Production.Other sites that cover this topic are: Peak Oil News, Peak Energy, Past Peak (A little bit anti-Bush), and Peak Oil.Org.

Fossil fuel developments in Oil Shale, Tar Sands, and Coal Liquifaction will have to replace the “Easy Oil”. At $70 per barrel these are all plausible but research and development dollars have to be allocated. Running the world on Corn production is not the way to go technologically even though it satisfies the farming lobby.

European Commision Report on Food Quality Sensors March 1st, 2006

A short European Commision Report on “Food Quality Sensors” – includes spectroscopy (NMR, UV/Vis, NIR-Vis, Vis-Fluorescence, thermoraphy, acoustic impulse, electronic noses).

Cheddar Cheese Flavour - Chemistry and Sensory Perceptions March 1st, 2006

An excellent review on the chemistry of cheddar cheese and the sensory perceptions that arise from that chemistry. Comprehensive Reviews in Food Science and Food Safety, Vol 2 (2003).

Time-Domain NMR of Lipid Mobility in Bread March 1st, 2006

Low resolution 1H TD-NMR was utilized to determine the mobility and translational diffusion coefficients of lipids in a low moisture (glassy) bread. The mobility of the lipids was found to be independent of moisture content. Journal of Cereal Science (28) 1998, 147-155.

Solid-State 13C NMR of Meteors March 1st, 2006

Solid-state 1H and 13C Nuclear Magnetic Resonance (NMR) Spectroscopic experiments on isolated meteoritic Insoluble Organic Matter (IOM) obtained from four different carbonaceous chondrite meteorites; a CR2 (EET92042), a CI1 (Orgueil), a CM2 (Murchison), and an undesignated rank 2 meteorite, Tagish Lake. Short overview web page of NMR investigations into the carbon chemistry of meteorites. Journal article on this subject in PDF can be found here.

If you are interested in having your meteor materials analyzed by solid-state 13C NMR contact John Edwards at Process NMR Associates.

NMR in Industry - Review Papers Available February 26th, 2006

Industrial Applications of Nuclear Magnetic Resonance
NMR in Process Control
Applications of NMR to Food and Model Systems in Process Engineering
Process NMR Spectrometry

Practical Applications of NMR in Civil Engineering February 26th, 2006

Practical Applications of NMR in Civil Engineering.

NMR of Hydrocarbons - Online Papers Available February 26th, 2006

Though we have been performing NMR analysis to accurately correlate 1H NMR spectra with physical and chemical properties of gasoline (distillation, octane numbers, benzene, aromatics, olefins, oxygenates, RVP, density) for over a decade, papers still appear in the literature to vindicate that NMR is a powerful tool in the gasoline testing arena.

In a Fuel paper (Vol 83, 2004, 187-193) the Swiss Federal Laboratories for Materials Testing and Research demonstrate a integral ratio method was demonstrated to yield excellent results for many gasoline parameters of interest to the engineer.
Another strong proponent of NMR utilization in the study of petroleum hydrocarbons is G.S. Kapur of the Indian Oil Corporation. Here are a few of his papers:
1) “Analysis of Hydrocarbon mixtures by Diffusion Ordered Spectroscopy”, Fuel 79, 1347-51 (2000).
2)”The qualitative probing of hydrogen bond strength by diffusion-ordered NMR spectroscopy”, Tetrahedron Letters 41, 7181-7185 (2000).
3)“Unambigous Resolution of a-Methyl and a- Methylene Protons in 1H-NMR Spectra of Heavy Petroleum Fractions”, Energy Fuels 2005, 19, 508-511
4)”Simplification an assignment of proton and 2-dimensional hetero-correlated NMR spectra of petroleum fractions using gradient selected editing pulse sequences” Fuel 81 (2002) 883-892

A practical guide to PFG spin echo NMR for mixture analysis has been written by Brian Antelek of Eastman Kodak.

Characterization of Coke - Analytical Approach February 25th, 2006

An RSC review paper (Catalysis Volume 17) on the Characterization of Coke (on catalyst surfaces) is presented at the RSC site. The review covers use of AES, IR, Raman, UV, NMR, XRD, SIMS, etc.

NMR and Porometry February 25th, 2006

An overview of NMR applied to porosity of technology materials is presented in the dissertation of Roland Valckenborg entitled “NMR of Porous Technology Materials” (Eindhoven University of Technology 2001).

Another site covering a peculiar NMR application to porosity is the site for NMR Cryoporometry. In this one measures pore size distribution by freezing liquids in the pores and then monitoring melting temperatures by NMR - as the melting point is depressed for crystals of small size the melting point depression gives a measurement of the pore simension that the frozen liquid was in. This is a speciality of Dr. J.B.W. Webber at the University of Kent, UK.

High Resolution Flow NMR for Reaction and Process Monitoring February 23rd, 2006

Where NMR will make an impact in the process monitroing arena is in reaction monitoring where it has huge advantages over optical spectrocopy due to the chemical resolution inherent in the spectrum. An excellent poster by Mailwald et al. presents flow NMR applied to reaction monitoring utilizing a superconducting NMR spectrometer.

Bayesian Analysis of NMR Data - Software Available February 23rd, 2006

Professor Larry Bretthorst (Washington University at St Louis) has made available a Varian VNMR based software package for Bayesian analysis of NMR data. He also maintains a site on Bayesian probability theory.

Overview of Solid-State 29Si NMR Studies of Silicone Gasket Materials

2006-02-20T14:02:00.000-05:00

Silicon-29 NMR has a unique ability to probe the detailed solid state chemistry of silicone rubber materials. The chemical shift range of the various silicone chemistry groups spans 120 ppm (at 4.9T this equates to 4800 Hz). This is a large dispersion which allows all chemistry types to be readily observed. In these, studies, however, we have not attempted to identify every chemical type present. We have identified general chemical types and followed their relative concentration from one sample to the next. Both cross polarization and single pulse experiments were performed on magic angle spinning samples (a full explanation of these two complimentary experiments is given below). Optimal experimental conditions were initially obtained and all subsequent samples have been analyzed under identical conditions to facilitate an understanding of the spectral changes from a chemistry as well as molecular mobility standpoint. Set NMR experiment conditions were used because of the time consuming nature of these experiments which typically take around 12 hours for each of the cross polarization and single pulse experiments.

Experimental
At the present time samples are being run on a Varian UnityPlus-200 spectrometer operating at a 29Si frequency of 39.74 MHz. The probe was a Doty Scientific 7 mm Supersonic CP/MAS probe using zirconia and Kel-F end caps. For the single pulse NMR experiments a pi/6 pulse of 2 microseconds was used with a relaxation delay of 4 seconds to facilitate quicker acquisition.The 4 second relaxation delay was obatined from full T1-inversion recovery experiments. Gated proton decoupling was used during FID acquisition. For the cross polarization experiments full contact time array experiments were obtained on the initial samples submitted. Due to the mobility of the polymer backbone the optimum cross polarization contact time for the polymer backbone was around 15 ms with signal lasting until 50+ ms. However, the more rigid structures in the polymer – such as the silicates, had optimum contact times around 3-5 ms. As a compromise we chose a 6.4 ms contact time which yielded good signal sensitivity for both the polymer and silicate components. Cross polarization inversion recovery experiments yielded a short relaxation delay of 2 seconds. A 1H pi/2 pulse of 4.6 ms was used along with gated proton decouplind during FID acquisition. For all samples the same experimental conditions have been maintained. MAS spinning speeds were around 7 kHz to avoid spinning side band coincidence on real signals. Also, to avoid MAS induced modulation of the contact-time, the variable amplitude cross-polarization contact pulse was used.

Silicone Chemistry Observed by NMR
The notation in use for silicone chemistry is M,D,T,Q (mono, di, tri and quaternary) denoting the oxygen substitution on the silicon atom. The polymer backbone itself is predominantly D i.e. [(SiO2(CH3)2]n which has a typical resonance frequency around –21 ppm. The termination of the polymer would be an M group (SiO(CH3)3) (found at +4 to +10 ppm) or MOH (SiO(CH3)2OH) (-10 to –15 ppm). Another area of interest in the spectrum is the –20 to –10 ppm region which is partially due to MOH but also due to D type silicon centers that are within 5 monomer units of a termination. Thus, if hydrolysis of the silicone backbone is occuring, this region will increase in intensity as one will now have more silicon centers close to termination points as well as more MOH terminations.

In some gaskets one observes small signals in the –60 to –70 ppm region which is due to T type silicone centers (SiO3(CH3))n, however this is usually not observed. The only other region where one observes signal is in the –80 to –120 ppm region of the spectrum. These silicon centers can only be Q1 (SiO(OH)3), Q2 (SiO2(OH)2), Q3 (Si(OSi)3(OH)) or Q4 (SiO4)types, as only silicons with 4 attached oxygens can appear in this region, any methyl substitution would cause these silicons to appear in the +10 to –70 ppm range of the spectrum. Of relevance to any discussions on silicone polymers it should be noted that Q1 is equivalent to M(OH)3 , Q2 is equivalent to D(OH)2 , Q3 is equivalent to TOH.

When one looks at the NMR experiments for the certain silicones one does not observe a resonance at +10 to +4 ppm. This indicates that the predominant polymer termination is MOH. Silicate is observed, however, it is not clear if this silicate is a filler for hydrogen bonding crosslinking or actual polymer Q4/Q3/Q2 sites of directly condensed silicates acting as bonded crosslinking agents.

SP-MAS NMR Experiments
In this experiment one quantitatively observes all silicon species in the system allowing a “bulk” silicon type distribution to be calculated. One observes a narrow resonance at –21 ppm which is due to the silicone polymer backbone (-O-Si(CH3)2-O-)n. Very little signal is observed in the –20 to –10 ppm region indicating that the polymer chains are quite long. In the –80 to –120 ppm region of the spectrum one observes silicon present in silicate that has been added as a cross-linking agent. The hydrogen bonding between the silicone polymer and the Si-OH groups of the silicate add structural integrity to the gasket. It is differences in the silicate silanol (Si-OH) chemistry that may account for changes in compressibility of the gasket during service. Thus, one will observe relative changes in the amount of 29Si signal observed in the –80 to –103 ppm and –10 to –23 ppm regions of the spectrum. This region is where Q3 (Si(OSi)3(OH)), Q2 (Si(OSi)2(OH)2), and Q1 (Si(OSi)(OH)3) groups are found.

Parameters Calculated:
Silicate Content – %Si in silicate filler
Q4 - %Si atoms in Q4 silicate – Si(OSi)4
Qn – %Si atoms in Qn silicate (Q1, Q2, Q3)Q4/Qn Ratio – Silanol (Si-OH) distribution
% Polymer – %Si in D & MOH polymer units

Relative changes in these parameters can be utilized to interpret changes in silicon chemistry caused by coolant exposure and service.

CP-MAS NMR Experiments
This experiment warrants a detailed explanation as the results are not quantitative from a “bulk” silicon chemistry standpoint. The CPMAS experiment utilizes the strong NMR signal that can be generated from protons (H) in the sample. The experiment preferentially observes silicons that are in close proximity to H. However, mobility is also a “problem” in this experiment. The way the experiment works is that the protons in the sample are polarized initially and magnetization is transferred from the protons to the silicons via their dipole-dipole interaction (similar to the interaction between 2 bar magnets). This interaction weakens the further the H and Si are from each other, and also weakens if there is considerable molecular motion. In the case of these samples this means that in the silicate region of the spectrum one observes an enhancement of the signal due to Si-OH containing species. In the case of the silicone polymer, however, one observes an overall decrease in the signal at –21 ppm due to the –(O-Si(CH3)2-O-)n backbone due to its rapid segmental (rubbery) molecular motions. One observes a large signal (that is hardly observable in the SPMAS spectra) in the –5 to –20 ppm region. This is due to silicone silicons that are at or directly adjacent to crosslinking sites (where there could be a D-silicate bond, or polymer termination sites such as MOH. The fact that they are enhanced by the CP technique indicates that these termination proximate silicons are motionally restricted compared to the rest of the silicone backbone. They represent either strongly hydrogen-bonded regions or chemical crosslinks of the type (O2(CH3)2Si–O–Si-O–Silicate) where a defect in the silicone backbone has reacted with a silanol of the silicate filler to form a Si-O-Si bond. This experiment is very powerful when used to observe relative changes in Si-OH chemistry in the silicate region and relative mobility changes in the polymer backbone.

Parameters Calculated:
% polymer backbone – %Si in mobile silicone backbone
% restricted polymer backbone – %Si in motionally restricted regions of the silicone backbone (D units in close proximity to cross-linking sites, termination sites (MOH) or adjacent to termination sites).
Silicate Content – %Si in silicate filler.
Q4 - %Si in Q4 silicate – Si(OSi)4
Qn – %Si in Qn silicate (Q1, Q2, Q3)
Q4/Qn Ratio – relative change in silanol (Si-OH) distribution

As with the SP-MAS calculated parameters one can utilize these parameters to determine changes in silicon chemistry resulting from coolant exposure and service.

Table I Summary of 29Si NMR Chemical Shift Regions
Chemical Shift
Region (ppm) Species
+10 to +4 Polymer termination sites (SiO(CH3)3) M
-5 to –15 Polymer Termination Sites (SiO(CH3)2OH) MOH
-10 to -20 Motionally restricted silicone polymer. Cross-linked and H-bonded –(O-Si(CH3)2-O-)n D units within five monomer units of polymer termination(-21) D Units – motionally unrestricted silicone –(O-Si(CH3)2-O-)n
-75 to -85 Q1 Si(OSi)(OH)3 Silicate Center (M(OH)3)
-85 to -94 Q2 Si(OSi)2(OH)2 Silicate Center (D(OH)2)
-94 to -104 Q3 Si(OSi)3(OH) Silicate Center (TOH)
-104 to -120 Q4 Si(OSi)4 Silicate Center (Q)

Discussion
In use one observes that the gasket silicon chemistry changes dependent on additive chemistry and temperature/pressure conditions. When the polymers degrade one observes a general loss of D type signal intensity in the 29Si SP/MAS experiment as well as a corresponding increase in silicate content. One does not typically see changes in Q4 type but instead large changes in Q3 and Q2 content. These changes occur regardless of the presence of silicate in the coolant. This leads one to deduce that the Q3 and Q2 types are being generated by degradation of the polymer itself rather than a change in the chemistry of the silicate that was present in the sample initially. The author is not privy to additives and experimental conditions so he cannot speculate on the effect of silicate and other additives on the speed of the degradation that occurs. At the same time that Q3 and Q2 types are increasing in intensity the CP/MAS experiment clearly shows that there is a large increase in the relative amount MOH types and D types close to terminations (-5 to –20 ppm region). This proves that the exposure to coolants causes a hydrolysis of the Si-O-Si bond. However, it should also be notes that for the Q3 and Q2 types to appear one must also be hydrolyzing the Si-CH3 bonds.

The complimentary nature of the SP/MAS and CP/MAS experiments along with the use of only on set of experimental CP/MAS conditions means that relative changes in the various silicon chemistries can be analyzed to quantify the degree of degradation that a polymer has gone through.

Excellent Silicone Chemistry Link – Silicones in Pharmacutical Applications

For more information on this topic please contact:
John EdwardsManager, Process and Analytical NMR Services
Process NMR Associates LLC,
87A Sand Pit Rd
Danbury, CT 06810, USA
Tel: (203) 744-5905

2006-02-16T00:40:00.000-05:00

High Temperature Simulated Distillation in Petroleum Characterization February 16th, 2006
“High Temperature Simulated Distillation” by Dan Villalanti et al. in Encyclopedia of Analytical Chemistry, “Yield Correlations between Crude Assay Distillation and High Temperature Simulated Distillation” by Villalanti et al., and “Refinery Analytical Techniques Optimize Unit Performance” . All discuss the panacea of developing rapid HTSD as a suitable replacement for the very lengthy crude assay distillation.

Exxon Technology Reviews - February 15th, 2006
Residue Upgrading Technologies are discussed in severla papers including one presented in India, and another at ERTC 2004 in Prague In Moscow at the 1st Bottom of the Barrel Technology Conference a paper was presented on “Delivering Value for Resid and Heavy Feed“.

Trends in NMR Logging - Schlumberger Review Article - February 15th, 2006
Oil exploration companies are using NMR measurements in a number of downhole applications, such as characterizing formation fluids during reservoir evaluation and assessing formation producibility. In their article “Trends in NMR Logging” Schlumberger describe how NMR technology is changing the way reservoirs are designed, developed and managed. A similar paper, “Advances in NMR Logging” is presented by Robert freedman of Schlumberger.Another review was produced in 1995, and “How to Use Borehole Nuclear Magnetic Resonance” was produced in 1997.
NMR Petrophysics offers NMR logging courses and provide NMR log analysis services.
A paper on the effect of sorbed oil on 1H NMR response was published byStanford University researchers.
A book is available on the subject entitled, “NMR Logging – Principles and Applications”
“Oil-Viscosity Predictions From Low-Field NMR Measurements” by J. Bryan and A. Kantzas, U. of Calgary/Tomographic Imaging and Porous Media Laboratory, and C. Bellehumeur, U. of Calgary

Application of TD-NMR in Civil Engineering - February 15th, 2006
Practical Applications of NMR in Civil Engineering by Bernd Wolter, Frédéric Kohl, Nina Surkowa, Gerd DobmannFraunhofer-Institut fuer zerstoerungsfreie Pruefverfahren (IZFP), Saarbruecken, Germany

Book Chapter - Monitoring Thermal Processes by NMR Technology - February 15th, 2006
A neew book on Emerging Technologies for Food Processing has been published by Elsevier, edited by professor Da-Wen Sun ( National University of Ireland, Dublin) and has contribution from KVL Quality & Technology: Monitoring Thermal Processes by NMR Technology by Nanna Viereck, Marianne Dyrby and Søren B. Engelsen. (Oct 2005)

MathNMR - NYU Software for Spin and Spatial Tensor Manipulations - February 15th, 2006
Professor Alexej Jerschow has made available a Mathematica package that allows calculation of spin and spatial tensors – it is available at the following link : MathNMR.
Also available at this site are a very handy palm utility that lists frequencies, gyromagnetic ratios, natural abundances, receptivities, magnetic and quadrupolar moments, and reference compounds of most NMR active nuclei – download PalmNMR. He also provides a nicely designed interactive NMR frequency map.

Italian patent - New Pre-Saturation Methodology - PERFIDI - February 15th, 2006
Stanislav Sykora, in his NMR blog describes a recent patent applied for by himself and Paola Fantazzini, under the auspices of the University of Bologna. The patent surrounds a new pulse sequence that will allow selective excitation of components of a complex mixture based on the T1 relaxation differences between the NMR active nuclei in the components. The pulse sequence pre-amble is called PERFIDI. The Italian patent (#BO2005A000445 of July 01, 2005) is currently confidential but the invcentors have set up a website for potential licensors of the technology. The website includes a brief overview of the patent.

NMR Processing Freeware - SpinWorks

2006-02-09T16:25:00.000-05:00

Dr. Kirk Marat at University of Manitoba has developed (and continues to develop) and excellent NMR processing freeware package that works very intuitively and well.

The FTP link to download the software is ftp://davinci.chem.umanitoba.ca/pub/marat/SpinWorks/.
The current version is 2.5.3. There is also an excellent documentation PDF file to help users work through the program functionality.

This is how Dr Marat describes his software on his home page:
“What is SpinWorks:
SpinWorks has two functions: The first is to provide easy basic off-line processing of 1D NMR and 2D data on personal computers. SpinWorks other function is the simulation and iterative analysis of complex second order spectra including dynamic NMR problems and certain solid-state NMR problems, in a manner similar to our UNIX Xsim program. SpinWorks 2.4 is the forth release of SpinWorks version to contain 2D processing. Full support is included for Bruker (XwinNMR/UXNMR) and Varian (Unix VNMR) data formats. Included F1 detection modes include States, TPPI, States-TPPI, Single Detection (QF), and echo-antiecho. There have also been some improvements and bug fixes in the 1D and simulation routines, and these should be at least as stable as those in version 1.3. While the program is to the point where it should (I hope) be useful, there will, no doubt, be bugs and there are things that don’t yet work. The aim of the program is to make a program easy enough for undergrads to process magnitude COSY spectra (for example) with a single mouse click, and yet still be flexible enough for research use. SpinWorks currently handles only one data set at a time. However, most new computers have sufficient memory to run two or three copies of SpinWorks simultaneously. This can be very useful when examining the rows and columns of a 2D data set.

Computer Requirements:
SpinWorks requires a 486 or higher processor (Pentium recommended) running Windows 95, 98, NT 4.0, Windows 2000 Pro, or XP (NT 4.0, XP or Win 2000 recommended). Windows ME is probably O.K., but is untested. Installation currently requires about 5 Mbytes of disk space exclusive of NMR data. 32 Mbytes or more of RAM are recommended, depending on NMR data set and simulation sizes. SVGA 800 x 600 or better display required (1024×768 or better recommended). For 2D processing a Pentium class processor with 64 Mbytes of memory is the practical minimum. For 2D you should also have your display set to at least 16 bit colour, otherwise the image and contour level colours will be strange. I have received reports (but have not confirmed) that SpinWorks will run under Linux with the WINE package and on a Mac with SoftWindows. A three-button mouse is ideal, but SpinWorks will work just fine with a two-button mouse. Note that on “Wheel Mice” the mouse wheel also serves as the middle mouse button. The mouse wheel can also be used for vertical scaling of 1D spectra.”

Some NMR Technology Patents

2006-02-09T15:47:00.000-05:00

Process NMR Technology Patents

Qualion NMR Patents
4998976 5063934 5072732 5162734 5184078 5320103 5371464 5462054 5978694 6281775 6310480 6670877 200400114236 20050040827

Other In-Line NMR Patents

Mobility Detected NMR - 6479994 6549007 6744251 6828892
Blending Control by NMR - 5796251
Ex-Situ NMR - 20030052677
Oil-Water Emulsion Compositions by NMR - 6794864
Bitumen Content by NMR - 6630357
Mobile NMR Analyzer - 5994903
Detection of Spoilage - 5270650
Microcoil Benchtop NMR - 5654636 6097188
Control of Process by NMR Gas Analyzer - 5265635

To search and get adobe acrobat pdf versions of patents go to Freepatentsonline.com
http://www.freepatentsonline.com/#.pdf
where # is patent number without commas patent 5,265,635 is 5265635.pdf

Time-Domain NMR Spectrometers - Benchtop and Online Relaxometers

2006-02-09T15:42:00.000-05:00

Time Domain Process NMR Spectrometers - Bench Top and On-Line Relaxometers
There are several NMR analyzers on the market that use an entirely different approach to some of the more simplistic on-line NMR applications. These spectrometers are very different from the Invensys MRA system in that they do not produce an chemical information. The Invensys MRA is a fully shimmed 60 MHz high resolution FT-NMR spectrometer that yields high resolution 1H NMR spectra which contain detailed chemical information that can be correlated with changes in chemical and physical properties. The other type of process NMR equipment is a low resolution time domain spectrometer that consists of a 1-30 MHz NMR system tied to an un-shimmed magnet. Only time domain data is acquired and relaxation time constants are calculated or correlated to physical properties or mixed phase content of mixtures.

For an overall view of NMR applied to process control or quality testing we are providing several links to papers or sites which adequately describe this "flip-side" of process NMR spectrometry.

On-Line Process NMR Relaxometry - Based on Auburn International/Oxford Instruments/Progression Technology - Polymer Qualities
The Analyst - Review Paper on Process NMR Spectrometry Covering Mainly Relaxometry Applications
Magritek - Low Field Portable and Specialty NMR Equipment
Minispec Analyzer from Bruker - Application Note Web Page
Maran NMR Analyzer from Universal Systems Inc - Applications Page
On-Line TD-NMR - Progression Inc
Applications of NMR Relaxometry - Process Control Technologies Inc

Time Domain Process NMR Spectrometers - NMR MOUSE
A handheld NMR surface analyzer is now available from Bruker or the collaborative research group that developed the technology.
NMR Mouse - Aachen Group Bruker Minispec MOUSE
Applications of NMR Mouse More Applications

Time Domain Process NMR Spectrometers - NMR Logging Tool
NMR logging tools have been developed for down-hole profiling of oil well pore structure and fluid reservoir structure and composition. This is NMR 1 mile down a hole.
Schlumberger NMR Logging Tool Description
Overview Paper - Trends in NMR Logging
Overview Paper - How to Use Down-Hole NMR
Lecture on Down-Hole NMR Logging

Compendium of Alternative Fuels Links

2006-02-09T15:39:00.000-05:00

Alternative Fuels - General Links
Alternative Fuel Vehicle Directory
AlternativeFuels.Com
Alternate Energy Store
EPA - Alternative Fuels and Additives
Canadian Renewable Fuels Association
Scenarios for a Clean Energy Future
Center for Renewable Energy
Fuel Economy . GOV
How Does a Fuel cell Work?
Fuel Cell Information Center
Renewable Energy Magazine
A Clean Energy Future - Alberta Energy Research Institute
Federal Tax Treatment of Alternative Fuels
Alternative Fuels from Renewable Resources
Renewable biological systems for alternative sustainable energy production (FAO Agricultural Services Bulletin - 128)
Technologies for Clean Energy

Fuel Cells
US DOE Fuel Cells Program 2002 Review Meeting Reports
DOE Technical Publications
DOE General Information
DOE - Fuel Cell Related Links
Fuel Cell Today
The Business of Fuel Cells
SAE - Fuel Cell Technology Showcase
The Hydrogen and Fuel Cell Investor

Hydrogen
US DOE Hydrogen Program 2002 Review Meeting Reports
National Hydrogen Energy Roadmap
DOE Technical Publications
DOE General Information Fact Sheets
DOE Links to Organizations and Associations
DOE - Hydrogen Program Glossary
National Vision of America's Transition to a Hydrogen Economy
Hydrogen Now!
The Hydrogen Economy - Jeremy Rifkin
Hydrogen Economy Again
How Stuff Works - The Hydrogen Economy
The Coming Hydrogen Economy - Fortune
UK Parliament - Prospects for a Hydrogen Economy
Australia - State Sustainability Report - H Economy
The Hydrogen Economy in the 21st Century
Hydrogen and Fuel Cells
The Future of the Hydrogen Economy - Bright or Bleak?
European Perspectives on Facilitating the Hydrogen Economy
Shell Hydrogen Perspectives
Hydromax

Biodiesel
Biodiesel FAQ's
Biodiesel - AFDC
Biodiesel.Org
Canadian Renewable Fuels Association
Marine Biodiesel Handbook
Biodiesel Overview
Biodiesel Legislation - Final Rule
Resources on the Web

Biomass Conversion
BioFuels - DOE
Biofuels - Links
Regional Biomass Energy Program
Biomass Links from ORNL
Energy Crops
American Bioenergy Association
Biomass Conversion Technologies
Biomass Resources
Biomass Applications and Links
Biomass Sources for Industry
Advanced Processes for Biomass Conversion
Advanced Processes for Biomass Conversion to Energy
Biomass Fact Sheet
Biogas and Liquid Fuels from Biomass

Ethanol
Renewable Fuels Association - Ethanol Industry
Ethanol Marketplace
EPA Fact Sheet

Water-Diesel Mixtures
Lubrizol PuriNOx

Diesel Fuel and Gasoline Legislation
Diesel Fuel Regulations - EPA
Gasoline Regulations - EPA

Coal
Coal - Bridge to the Hydrogen Economy

Wood
Liquid Fuels from Wood
Biomass Feedstocks
Wood to Alcohol Fuels - Technology Status
Synthetic Liquid Fuels from Wood and Coal
Wood to Oil Process
Wood and Biomass to Fuel

Heavy Oil and Bitumen
Heavy Oil - Energy Source of the 21st Century
Canada's Heavy Oil and Tar Sands - Overview

Gas to Liquids
DOE - Natural Gas to Liquid Fuels
Rentech Inc - Gas to Liquids Technology

Steam Reforming
Steam Reforming Process - Synetix

Syn GasSynergy Technologies SynGas Process
SynGas Generation Technologies

Refining Overviews
Kittiwake : Fuel and Lube Oil Training Manual

Working Definitions of Use When Comparing Online Analyzer Results with Laboratory Test Data

2006-02-09T15:29:00.000-05:00

Working Definitions

Accuracy – the ability of any test method, lab analysis, or analyzer, to yield the true value of the sample as a result of the measurement. That is, the result of the measurement gives the true value within the error of the measurement. The accuracy of any method is best determined by round-robin testing of that method.

Reproducibility – the determination of the spread around the true value. Determined by multiple measurements of the same samples at multiple sites (round-robin testing). It is the true error of the method.

Repeatability – the measurement of the spread around a test result from a single analyst and/or single analyzer at the same site on the same sample. However, this does not mean that the result is accurate (produces the true value).

Precision - the level to which any measurement can be accurate. That is, 46 or 46.259.

Bias – a definite offset from the true value. Consecutive single point measurements can be biased.

Model Definitions

Global Model: Any chemometric based prediction that incorporates lab analyses and samples from multiple locations on multiple streams, multiple processes, and multiple stream sources (i.e. crudes). By definition then, the prediction is accurate (predicting the true value) to within reproducibility. In order to compare a global model prediction to any single point lab measurement, the lab must first validate that the lab can meet the reproducibility requirements of the method, or ascertain it’s actual reproducibility by as described in ASTM D3764. Once the lab measurements are validated, single point lab measurement comparisons to the chemometric prediction should be within reproducibility limits. Global models are less prone to bias errors and drift.

Model Training: The process of enabling a global model to statistically recognize (i.e. f-test, mahalanobis distance, etc) the spectral results of a specific analyzer at a specific location. Requires no extensive lab sampling and analyses or exorbitant input of local unit and process specific spectral files to the model.

Local Models and Localization: Local models are built on data from a specific process unit, in a specific location, usually incorporating only lab analyses from the on-site laboratory. This effectively makes the model an on-line duplicate of the on-site laboratory and therefore subject to bias. Further, if a model is localized too much, it can be prone to drift (moving away from the true value) and/or fail to predict outside of the model space when the process changes or experiences an upset.

NMR Reproducibility: The limits of the differences between a valid, single point lab measurement and an NMR predicted result. This value is determined by the primary method and range of samples that the model is built on.

NMR Repeatability: The limits of the differences between successive predictions on a blocked in sample in the NMR under defined conditions. This value is determined bythe primary method and range of samples that the model is built on.

NMR Model and Application Strategies

NMR models based predictions are based on two types of applications: Process Control or Product Certification.

Process Control: Feed Forward and/or Feedback

NMR models cover a wider sample range.
Very Robust: continue to accurately predict over wide process ranges.
Reproducibility differences between the NMR prediction and any single point lab measurement will be slightly higher.

Product Certification: i.e. Blending

NMR model ranges are narrowed and confined with respect to the product (i.e. gasoline and blend components only)
NMR validation set at product certification levels.
Models are not as robust. That is, a gasoline blending model will not predict a diesel fuel as accurately as a more broad based model.

For more information on this topic please contact:
John Edwards
Manager, Process and Analytical NMR Services
Process NMR Associates LLC,
87A Sand Pit Rd
Danbury, CT 06810, USA
Tel: (203) 744-5905

Online Process NMR Unit Description

2006-02-09T14:18:00.000-05:00

Example of a Process NMR Unit
This analyzer, manufactured by Qualion Ltd, is marketed by Donahue Process Systems Inc.

1. Rack Mounted Computer
The rack-mounted computer provides supervisory control for all other units in the analyzer cabinet. This unit is a PC supplied with standard peripherals and I/O functions, such as an analog-to-digital converter for Channels I and Q, a system control board, control for the sample switching system, and a direct digital synthesizer (DDS). It also provides a communication link to a remote computer or modem link.
2. Switching Control Unit (RF Box)
The Switching Control Unit contains the following major components:
36 MHz crystal oscillator RF Sources Module Lock Transmitter Module
Lock Receiver Module Main Transmitter Module Main Receiver Module 36 MHz RF Filter

3. Shim Control Unit
The Shim control unit converts the digital shim signals from the computer and generates the current for the 50-shim coil pairs. It contains a communication board for coms to the computer, 50 ADC’s and 50 current generators.

4. Power Supply I/O Unit
The Power Supply I/O unit contains digital output modules for sample stop and sample switching valve control, digital input modules for enclosure alarms. A RS-485 Field Point connection for analog outputs and a RS-485 Modbus connection for digital connection to a DCS. It also provides all dc operating voltages for the system.

5. Magnet
The magnet is permanent and built from multiple segments of neodymium- boron-iron. This material is used because its very high field strength-to-mass ratio achieves the desired flux density in a small, compact package. Because the flux must be extremely uniform over the entire air gap, construction of the magnet is complex. The magnet is fabricated from several segments bonded together to form the basic assembly. In addition to the bonded segments of magnetic material, each magnet also contains 50 coils of wire arranged about a Shimming Unit mounted in the center of the magnet between the pole pieces. These coils are used as small electromagnets; the strength and polarity of which can be controlled by varying the current through them so as to improve uniformity of the overall field of the magnet assembly.
Prior to assembly in the manufacturing plant, each magnet segment is “cured” at a high temperature to stabilize its field strength. In the fabrication process, the absolute field strength of each individual segment of the magnet is measured. A computer analysis of this data then determines the best placement of each segment in the final assembly to achieve a consistent, uniform field for the assembled magnet. The segments are then bonded together to form the final magnet assembly. The assembly is placed inside a soft iron cylinder, the ‘envelope’, which constrains the magnetic flux and prevents the magnetic field outside the magnet housing from exceeding a value of as little as 5 gauss. More importantly, the iron cylinder raises field strength in the center of the magnet by pushing the flux toward the center; a process called “condensing the field”. There are electric heater strips and thermistors on the magnet and envelope to heat the assembly to the desired temperature.

6.Probe
The sample probe is mounted inside the permanent magnet in the air gap between the magnet poles. The probe contains two coils; the first, the ‘Main Coil’ is wound around a ceramic or molybdenum tube that is inserted in a hole through the shimming unit in the center of the gap between pole pieces of the magnet. The second coil, the ‘Lock Coil’ is wound on a sealed capsule of lithium chloride beside the main coil in the sample probe inside the permanent magnet. This is provided as a reference standard for setting the frequency of the main transmitter.
The constant magnetic field of the permanent magnet is perpendicular to the axis of the transmitter coil in the sample probe. Since the pulsed ac field introduced by the coil around the sample tube coincides with the vertical axis of the probe, the pulsed magnetic field is therefore perpendicular to the constant magnet field of the permanent magnet.

7. Heater Control Unit
The Magnet Heater Control Unit controls the temperature of the magnet and the envelope. The temperature of the magnet is set at 41°C and the temperature of the envelope is maintained at 37°C. The Heater Control Unit is mounted on the interior wall of the Magnet Enclosure Cabinet and has two PID loops that accept measurement input signals from the thermistors mounted on the magnet itself and the envelope. The outputs of these two PID loops control the currents to electric heater strips.

8. Enclosure
The NMR analyzer is housed in a two-door NEMA Type 4 enclosure approximately 48 inches high, 44 inches wide and 30 inches deep. Floor stands are approximately 12 inches high and are welded to the body to make it a freestanding enclosure.

The enclosure with equipment installed weighs approximately 1500 pounds and is equipped with transportation eyebolts. It is fabricated from 304 stainless steel, with all seams continuously welded and ground smooth. A center partition divides the enclosure into Magnet (left) and Electronics (right) compartments.

The magnet side is home to the gas leak detector and the ambient temperature is maintained at 72°F ±1°F. This is accomplished by means of an air conditioner on the outside left wall of the enclosure working in conjunction with a bank of five 500-watt strip heaters and a PID Controller. The ambient temperature in the Electronics side is controlled by an air conditioner on the outside right wall with an internal thermostat set at approximately 70°F.

Principle of Operation
The Qualion Process NMR System

A sample is selected via the sample switching control and the S.C.S. (Sample Control System) and is flowed through the Main probe, through the Magnet. After a specified time the sample stop valve locks the sample in the magnet and holds it, we then have a specified time until the Main circuit then Pulses the sample, waits and receives the signal. This signal that is received is called a F.I.D. (Free Induction Decay).

The FID is read in the time domain, meaning the Y axis is time and in this time domain we can perform various processing functions, the FID is then Fast Fourier Transformed (F.F.T.) into the frequency domain.

The signal is then digitally processed passed though the prediction models to obtain a prediction, the prediction is then transmitted to a DCS or receiver via analog or modbus outputs. After this has happened the sample stop valve is opened and the cycle is repeated. The lock circuit is constantly performing a NMR experiment on the Lithium Chloride, this is done as a reference. The frequency of Lithium in the NMR magnet is around 22 MHz and therefore does not interfere with observing hydrogen at 60 MHz. Because the magnet is highly dependent on temperature it is impossible to maintain a constant temperature and there for, as we know where the Lithium Chloride peak should be we can reference the main circuit to the same as the Lithium Chloride peak is away from where is should be.

Main Circuit
The crystal oscillator outputs a 36 MHz signal, which is sent to the DDS card. The DDS unit multiplies, divides, and/or phase shifts the signal and outputs a 51 MHz signal that is used as the main transmitter and receiver local oscillators (MAIN_TX_LO and MAIN_RX_LO). A 9 MHz signal from the DDS unit is added to the MAIN_TX_LO signal to produce the main transmitter frequency of 60 MHz, which is transmitted to the diplexer and then switched to the main transmitter coil in the probe. After the main transmitter pulse is removed, the nuclei relax and generate a 60 MHz signal in the coil, which flows to the diplexer, where it is automatically switched to the receiver input. The received signal is amplified and then mixed with the MAIN _RX_LO signal (51 MHz) to produce an Intermediate Frequency (IF) of 9 MHz. This signal is then mixed with 9 MHz from the DDS card to produce an audio frequency of approximately 1 kHz. The audio signal is then split into two equal channels, I and Q, phase separated by 90°. The I and Q signals are then input to the ADC, where they are converted to digital form for input to the PC.

Lock Circuit
The purpose of the lock system is to provide control of the frequency of the main transmitter pulse, automatically compensating for any minor variations in magnet field strength and temperature. The lock system continuously detects the resonant frequency of the nuclei in a known sample fluid, lithium chloride, and then sets the frequency of the main transmitter to be a fixed ratio to this reference. Since the reference fluid capsule is located inside the main probe, it is subjected to the same magnetic field and temperature as the main transmitter/receiver. Therefore, a change in one affects the other. The lock system functions in the same general way as the main transmitter system, except that the basic transmitter frequency is approximately 22 MHz, the resonance frequency of lithium in a magnetic field of 1.5 tesla. The frequency of the lock transmitter is swept over a range of about 1 MHz (22-23 MHz) as it searches for the resonance frequency of lithium. When it first detects a resonant response (significant increase in signal level) as it increases frequency during the search, it stores this value and then jumps to a higher frequency and approaches resonance from the other direction. When it detects a resonance response as it approaches from the other direction, it stores this frequency and then jumps to a frequency at the mid point between the two stored values and then “locks” on this frequency as the resonance frequency of lithium. The output of the lock system is used as the set point of the main transmitter circuit, which maintains the main transmitter frequency in a fixed ratio to this “lock” frequency.

Shimming
To obtain a rough magnetic field, the field homogeneity of the permanent magnet is adjusted by mechanical alignment of the magnet pole faces. The more parallel the pole faces, the more homogeneous the magnetic field. The first step in the process of adjusting magnetic homogeneity is to adjust the position of the magnet's pole faces by turning adjustment bolts which hold the pole faces in position. Adjusting these bolts tilts the pole faces relative to each other with the aim of making the pole faces more parallel. In old electromagnetic magnets, if the bolts ran out of range, thin pieces of brass were placed between the magnet yoke and the pole pieces to move the pole pieces as parallel as possible. These thin pieces of brass were also placed in other strategic locations to make the pole faces parallel in a manner not addressed by the adjustment bolts. The metal pieces were called shim stock and the seemingly endless process of placing and removing pieces of shim stock acquired the name "shimming". This is, however, a simple mechanical adjustment that only gets the NMR to a symmetric half height of 700 Hz. To increase performance, reduce the difficulty of adjusting magnetic homogeneity, and reduce the manufacturing difficulty of the magnets, an electronic "shimming" process is used, which uses a series of small electromagnets (essentially shaped coils) having very specific magnetic field contours. These small coils are placed around the sample area in different orientations. Each small coil can be used to adjust the shape of the magnetic field gradients by simply passing different currents through the coil. A complete series of these coils can be used to adjust the magnetic field homogeneity to a given level of “purity”. The process of adjusting the magnetic field homogeneity by adjusting the current in each of the coils has retained the name “shimming” and the small coils assumed the name "shims".

Systems are marketed through Donahue Process Systems Inc

Contact John Edwards for details and visit the Process NMR Associates web page for application examples.

Process NMR Associates NMR Testing Services - Examples of Solid-State NMR Applications

2006-02-09T13:55:00.000-05:00

Solid-state NMR analyses cover a wide range of applications that cannot be addressed by liquid-state experiments. In solid-state NMR samples are place in 7mm diameter spinning rotors and spun at high speeds (3-14 kHz) in order to allow acquisition of NMR spectra with sufficient resolution to allow chemical determinations to be made.

An excellent overview of solid-state NMR is presented by Prof. Robert Schurko.

In the following pages we will give several examples of applications that have been undertaken by PNA. We have a large amount of experience in the solid-state NMR area. Some of the topics below cannot be exemplified due to restrictions placed on the analyses. Where this is the case I have included a link to a document that adequately demonstrates the use of NMR in that area.
Silicon-29 NMR of
i) Gasket Materials (Various Silicones)
ii) Heterogeneous Catalysts (clays, zeolites, aluminosilicates, various molecular sieves).

Carbon-13 NMR of
1) Combustion Chamber Deposits
2) Coals, Coke, Soils, Kerogens, Asphaltenes
3) Carbon Based Catalysts
4) D iesel Engine Soot
5) Gaskets and Seal Materials (Silicones, NBR, HNBR)
6) Polymers (EPDM, Terpolymers, Rubbers, Nylons, Polyethers, Polyurethanes, PVC,)
7) Sugars, Polysaccharides, and Polypeptides
8) Catalyst Coking Studies
9) Medicine Tablet Dosing Studies
10) Insoluble Materials from Various Sources (Compositional Studies)
11) Natural Organic Matter (Soil, Humus, Kerogen)
12) Polymorphism - Crystal Form Determination - Amorphous Content

Heteronuclear NMR Studies (31P, 27Al, 7Li, 19F, 23Na, 11B, 1H, 2H)
A) 31 P NMR Of Diesel Soot
B) 2 H NMR of Wax Crystallization Dynamics in Lubricant Base Oils
C) 27Al Studies of Aluminas, Surface-Modified Aluminas, Aluminosilicates and Clays
D) 11 B, 27Al, and 29Si Studies of Boron Substituted Zeolites and Aluminosilicates
E) Solid State NMR of Silicates and Oxides - A Review by Stebbins
F) Zeolite Synthesis

Chemical Shift Tables
i) Carbon-13
ii) Nitrogen-15
iii) Silicon-29
iv) Aluminium-27
v) Phosphorus-31
vi) Fluorine-19

NMR Periodic Table (University of Illinois)

For more information on this topic please contact:
John Edwards
Manager, Process and Analytical NMR Services
Process NMR Associates LLC,
87A Sand Pit Rd
Danbury, CT 06810, USA
Tel: (203) 744-5905

Process NMR Associates Services - Examples of Liquid-State NMR Analysis

2006-02-09T13:50:00.000-05:00

Analytical liquid-state NMR experiments are performed on our Varian VXR-300S superconducting NMR spectrometer operating at 7.2 Tesla. A 200 MHz Varian UnityPlus200 Spectrometer and a JEOL Eclipse 300 are also available for liquid-state experiments. We also have two Qualion process NMR units available for process NMR application development, and two low field NMR spectrometers (2.5 and 20 MHz Oxford Instruments spectrometers, for time-domain NMR experiments.

Here is a listing of past NMR projects that Process NMR Associates has been involved with.

Table 1 and Table 2 show the 1H and 13C functional group chemical shifts that can be utilized to derive detailed molecular information on samples of interest in the petroleum and petrochemical industries. Detailed molecular information can be obtained from petroleum related samples such as crude oils, base oils, diesels, bitumen, asphaltenes, naphthas. Based on these particular chemical types that can be identified it is possible to generate average molecular parameters that allow the effects of various processes to be observed when the NMR parameters are compared for samples taken before, during and after the desired processing.

The following describe several typical liquid state NMR applications that are routinely performed at PNA.

Crude oil (including heavy oil) analysis - detailed chemical breakdown obtained that allows effects of various thermal and hydrothermal upgrading processes as well as desulfurization to be followed by their effects on a series of detailed average molecule parameters. Table 3 and Table 4 shows the detailed analysis parameters that can be obtained on crude oil samples as well as all other petroleum products. Example data for crude oils can be found here.

Petroleum Product Analysis - this includes a large number of NMR interpretations on samples such as used motor oils, lubricant oils, gasolines, diesel fuels, greases, waxes, gas oils, recycled oils, fatty oils, vegetable oils, edible oils, etc. Detailed chemical information as well as the quantity and type of contaminants can be determined. For example, in used motor oils 31P NMR can be used to determine the degradation of the Zinc dithiophosphate anti-wear agents, as well as the presence of contaminants originating in the gasoline (polyether, and PIB based additives) and diesel fuel (heavy aromatics). Lubricant oil physical properties can be determined from the detailed chemistry observed in the 13C and 1H NMR spectra.

Polymer Characterization - 1H and 13C NMR can be used effectively to determine the monomer ratio of various mixed copolymers, the number average molecular weight, effectiveness of hydrogenation, olefin analysis, molecular conformation, etc. Typical polymers analyzed are PIB, PE, PP, mixed butene-ethylene, PVC, polystyrene, styrene copolymers, EP copolymers, methacrylates, synthetic rubbers, polybutenes, PTFE, nylons, specialty acrylates and polyurethanes, etc.

Multinuclear experiments - various NMR active nuclei can be studied to determine the chemical make-up of catalysts, polymers, and modified materials. Nuclei commonly observed are 29Si, 31P, 19F, 27Al, 11B. Table 5 shows the typical 29Si chemical shifts observed for siloxanes and silicates. The structure and molecular weight of these materials can be readily obtained by NMR.

Multidimensional NMR Experiments - Various specialized NMR experiments can be used to determine the basic chemical functionality of a sample (DEPT), the structural detail and connectivity (COSY, HETCOR), as well as the conformation of a molecule (2D-3D NOE experiments). For example, COSY experiments can be used to determine the conjugated diolefin content of gasolines and naphthas.

Unknown Compound Structural Elucidation - Detailed NMR experiments can be used in conjunction with sample isolation techniques to allow identification of unknown compounds that are of interest in competitive analysis reverse engineering, product marketing and field issues, customer satisfaction issues, and environmental studies.

Product Quality and Natural Product Purity - Liquid-state NMR is routinely used to determine the quality and purity of dietary supplements. Typical examples may be purity of synthesized body building food supplements, or quality of aloe vera juices and freeze dried powder. An example of pass and fail Aloe Vera quality test is given here. This Aloe Vera test is now required by the International Aloe Science Council. See this short write-up of the official test method.

Database Development - Process NMR Associates is currently developing several databases - Examples: Heavy Hydrocarbon NMR Database and Essential Oils Database.

Here are some simple NMR experiments demonstrating the methodology that can lead to full chemical characterization.

Process NMR Associates is interested in developing NMR quality control databases in conjunction with various industries. We are also not limited to NMR database development. We currently have stable stored sample sets that can be utilized to develop IR, Raman or other spectroscopy databases.

For more information on this topic please contact:
John Edwards
Manager, Process and Analytical NMR Services
Process NMR Associates LLC,
87A Sand Pit Rd
Danbury, CT 06810, USA
Tel: (203) 744-5905

Online Applications of NMR Technology

2006-02-09T13:43:00.000-05:00

On-Line Applications of Nuclear Magnetic Resonance Technology

The applications shown here were developed by Process NMR Associates while contracted in an application development and technical marketing capacity for the Invensys MRA product. We maintain rights to these applications and market them through Donahue Process Systems Inc

Refinery Applications
Crude Blending
PDVSA CDU Optimization Presentation
Product Blending
Crude Switching
CDU Rundown
PDVSA CDU Application Presentation
FCC Feed
FCC Feed Application Note
FCC Products
Reformer/Platformer
BP Reformer Application Note
Acid Alkylation
Base Oil Manufacture

Internal Tank Farm Management
Bitumen Upgrading Process

Petroleum Exploration
Whole Crude Analysis
Custody Transfer

Petrochemical Applications
Steam Cracker
BASF Steam Cracker Application Note
Equistar ISA Presentation - Naphtha/Condensate Cracker Optimization
Aromatics Plant
Styrene-Butadiene Rubbers
Ethylene-Propylene Copolymers

Food Applications
Butter
Cream Cheese
Sour Cream, Milk, Cheeses, Yogurt
Beverages (Juices and Alcoholic)
Baby Food and Soups
Sodium Content of Food and Drink

Pulp and Paper Industry
Black Liquor Evaporation Process

LNG and Power Industry
BTU Analysis and Limited Speciation of Gas Components

The Other Aspect of Process NMR is Time Domain NMR Spectroscopy - Learn More

These Applications and Others Marketed through Donahue Process Systems Inc.
For Technical Information Contact john@process-nmr.com or see the Process NMR Associates Website

NMR Methods

2006-02-08T17:16:00.000-05:00

NMR Method Patented to Determine Presence of Organic Sub-Structures in Molecules
Bristol-Myers Squibb researchers have patented a methodology to determine the presence of particular molecular substructures in compounds by PCA analysis of NMR spectroscopy data. This analysis is performed on entire spectra or particular regions defined by the substructures of interest. US Patent 6,895,340

Ex-Situ NMR available for license from Berkley Lab
Ex-situ NMR (US Patent 6,652,833) is currently available for license from the Lawrence Berkely Lab. This NMR analysis is described in a paper presented in Physique and in the following Science article (“High-Resolution NMR Spectroscopy with a Portable Single-Sided Sensor” by J. Perlo, V. Demas, F. Casanova, C. A. Meriles, J. Reimer, A. Pines, and B. Blumich (2005). Science 308: 1279-1279

Spoilage of Wine observed by NMR of Intact Bottles
A large bore superconducting magnet and specialized probe is all that is required to check that your $4500 bottle of Mouton Rothschild 1865 is not a extraordinarily expensive bottle of vinegar US Patent 6,911,822. See also this magazine atricle and the website of the company that is using the first commercial system in Morristown New Jersey – Wine Scanner Inc

Patented NMR Method for Quality Control of Medicinal Natural Products
Pattern recognition technology in conjunction with 1H and 13C NMR spectroscopy is used to determine the standard specification expected for medicinal grade natural products – see US Patent 6,806,090

Food Authentification by SNIF-NMR
Gérard Martin of Eurofins Scientific, CNRS, Nantes University, Nantes – France, writes:” Methodology: No dramatic improvement in NMR instrumentation originated during the last decade where an 11.4 T spectrometer, fitted with dedicated 2H{1H} probe and a 19F locking canal represents a good compromise between cost and efficiency. Since the main challenge for 2H-SNIF-NMR is to overcome its low sensitivity, efforts were directed in this way. The cheapest solution is to avoid the use of an internal reference that spares room in the cell for more molecules of interest and this can be done in two ways. First, the isotope ratios may be computed from the molar ratios of the deuterium isotopomeres, and the overall (D/H) value measured by Mass Spectrometry (IRMS). An alternative is to replace the chemical reference by an electronic signal conveniently generated (ERETIC method).
Wines and juices: Since 1991, the European data bank on wines has been established years after years and contains now the isotopic data of several thousands of wines from the main producing countries in Europe. Illegal enrichment of wines can be checked out and, according to the pertinence of the data bank, geographic origins of QWPSR wines can be controlled. Private ventures took also an interest in building up specific databanks of wines from third countries. The market of fruit juices has been stabilized by SNIF-NMR and the quantity of sucrose added in pure juices has been severely reduced. A joint approach using SNIF-NMR and IRMS is very useful for fighting against other sophisticated frauds.
Aromas and perfumes: The replacement of vanillin from beans (Vanilla Planifolia) by synthetic vanillin is an old practice and during thirty years, isotopic methods (IRMS and SNIF-NMR) were a nightmare to the fraudsters. Biotechnology forms the subject of the last serial of the vanillin saga: vanillin obtained from ferrulic acid by fermentation has been declared “natural” providing that all the steps and ingredients taking part in its manufacture are “natural”. The potentiality of isotopic analysis for solving the problem of the natural status of biotechnological vanillin will be discussed. Progresses in the authentication of aromatic molecules obtained from the shikimate pathway and of monoterpenes bio synthesized according to the deoxyxylulose pathway are also pointed out.
Miscellaneous applications of SNIF-NMR: During the last decade, fats and oils, fishes, dairy products and coffees received a great attention form the official and private laboratories in charge of the consumer protection. Legal (tobacco) and illegal (heroin) drugs have also been authenticated by SNIF-NMR.”
See also – Eurofins Site, and the following papers in The Chemical Educator (Elsevier), and this US Customs Service Report, explain the technique and a simple application very well.
SNIF NMR methodology has actually been patented US Patent 6,815,213, US Patent 4,550,082.
An excellent overview of where NMR analysis fits in the isotopic methods utilized in the European Union to detect fraudin food products is given by the European Commission’s Joint Research Centre
See Process NMR Associates for your NMR analysis needs.

13C NMR Analysis for Authentification of Gum Arabic
35 samples of Gum Arabic (acacia senegal) were analyzed by 13C NMR spectroscopy and the “average 13C NMR peak relative intensities” were calculated. This average 13C NMR signature can be used to determine the authenticity of a gum arabis sample and allows for observation of adulterants which are typically gums from other tropical trees (eg. gum talha (Acacia Seyal), Combretum, etc.). 13C NMR has been suggested as a specification of Gum Arabic quality in the following paper:“Gum arabic (Acacia senegal): unambiguous identification by 13C-NMR spectroscopy as an adjunct to the Revised JECFA Specification, and the application of 13C-NMR spectra for regulatory/legislative purposes.” by Anderson DM, Millar JR, Weiping W., Chemistry Department, University, Edinburgh, UK. Published in Food Additives and Contaminants, 1991 Jul-Aug;8(4):405-21
See Process NMR Associates for your 13c analysis needs.

NMR Database - Essential Oils and Carrier Oils
PNA has created and extensive NMR database comprising 160+ Essential Oils and 40+ Fixed Oils.Process NMR Associates is interested in developing a comprehensive database of NMR data that can be correlated to GC/GCMS data.If you have essential oils that have GC or GCMS data associated with them, we would be happy to provide you with a free 1H/13C analysis in exchange forincluding your EO and analytical data into the current database. Contact John Edwards if you are interested.The database includes 1H and 13C NMR spectra of the following oils:
Essential OilsAjowan EO Trachyspermum copticum – India (seed)Allspice Berry EO Pimenta officinalisAmyris EO Amyris Balsamifera – JamaicaAngelica Root EO Angelica archangelicaAngelica Seed EO Angelica archangelicaAnise Seed EO Pimpinella anisumArmoise EO Artemesia herba alba – MoroccoBalsam Peru EO Myroxylon balsamumBalsam Tolu EO Myroxylon balsamum – El SalvadorBasil EO Ocimum basilicumBay Leaf EO Pimenta racemosaBay Laurel EO Laurus nobilus – JamaicaBenzoin Liquid Resin Benzion Styrax – ChinaBergamot EO Citrus bergamiaBirch Sweet EO Betula lentaBlack Pepper EO Piper nigrum – IndiaBlood Orange EO Citrus sinensis var.Bog Myrtle EO Myrica gale – EuropeCabrueva EO Myocarpus fastigiatus – South AmericaCade EO Juniperus oxycedrus – SpainCajeput EO Melaleuca cajeputiCalamus EO Acorus calamusCamphor EO Cinnamomum camphoraCananga EO Cananga odorataCaraway Seed EO Carum carviCardamom Seed EO Elattaria cardamomumCassia EO Cinnamomum Cassia – ChinaCatnip EO Nepeta catariaCarrot Seed EO Daucus carotaCedarwood EO Cedrus atlanticaCedarwood Atlas EO Cedrus atlantica – MoroccoCedarwood Chinese EO - Cupressus funebris – ChinaCedarwood Himalayan EO Cedrus deodara – HimalayaCedarwood Mexicana EO Juniperus mexicana – Mexico (also Texas Cedarwood)Cedarwood Virginian EO Juniperus Virginiana – USACedar Leaf EO Thuja occidentalis – USACelery Seed EO Apium graveolensChamomile German EO Matricaria chamomillaChamomile Egypt EO Matricaria chamomillaChamomile Spain EO Matricaria chamomillaChamomile Roman EO Anthemis nobilisCinnamon Bark EO CinnamomumCinnamon Leaf EO Cinnamomum zeylanicumCitronella EO Cymbopogon nardusCitronella Sri Lanka EO Cymbopogon nardusCitronella Java EO Cymbopogon winterianusClary Sage EO Salvia sclareaClove Bud EO Eugenia caryophyllataClove Leaf EO Eugenia caryophyllata – MadagascarCopaiba Balsam EO Copaifera officinalisCoriander Seed EO CoriandrumCumin EO Cumimum cymimumCypress EO Cypressus sempervirensCypriol EO Cyperus scariosus – Brazil (Flowers)Davana EO Aretemesia pallensDill Seed EO Anethum sowa – IndiaDill Weed EO Anethum graveolensDragons Blood EO Croton lechleri – South America (Resin)Dwarf Pine EO Pinus mugoElemi EO Canarium luzonicumEucalyptus Citriodora EO Eucalyptus citriodoraEucalyptus Globulus EO Eucalyptus globulusEucalyptus Radiata EO Eucalyptus radiataEucalyptus Spain EO Eucalyptus globulusEucalyptus China EO Eucalyptus globulusEucalyptus Smithii EO Eucalyptus smithii – China (leaf)Fennel Sweet EO Foeniculum vulgareFennel Hungary EO Foeniculum vulgareFennel Spain EO Foeniculum vulgareFennel Rectified EO Foeniculum vulgareFennel Sweet EO Foeniculum vulgareFir Needle EO Abies albaFir Siberian EO Abies sibirica – Austria (Needle)Fir Canadian EO Abies balsamea – USA (Needle)Frankincense EO Boswellia carteriGalbanum EO Ferula galbaniflua – Turkey (Gum)Garlic EO Allium sativum – Mexico (Bulb)Geranium EO Pelargonium graveolensGeranium Rose EO Pelargonium roseum – FranceGinger EO Zingiber officinaleGinger Grass EO Cymbopogon martini – ChinaGrapefruit Pink EO Citrus paradiseGuaiacwood EO Bulnesia sarmienti – ParaguayHelichrysum EO Helichrysum angustifoliumHelichrysum Italicum EO Helichrysum italicumHop EO Humulus lupulusHyssop EO Hyssopus officinalisJuniper Berry EO Juniperus communisLabdanum EO Cistus labdanumLantane EO Lantara camara – MadagascarLavandin EO Lavendula latifoliaLavender EO Lavendula angustifoliaLemon EO Citrus limonLemongrass EO Cymbopogon citratusLemon Myrtle EO Backhousia citriodora – AustraliaLime EO Citrus aurantiumLime (Distilled) EO Citrus aurantifoliaLime (Cold Pressed) EO Citrus aurantifoliaLitsea Cubeba EO Litsea cubeba – ChinaMace EO Myristica fragrans – Spain (Husk)Mandarin EO Citrus reticulataMarjoram EO Origanum majoranaMelissa EO (Lemon Balm) Melissa officinalisMint Brazil EO Mentha arvensisMint China EO Mentha arvensisMint Japan EO Mentha arvensisMugwort EO Artemisia vulgarisMullein EO Verbascum thapsus – India (Leaf)Myrrh EO Commiphora myrrhaMyrtle EO Myrtus communisNeroli EO Citrus Aurantium – EgyptNiaouli (Cineole) EO Melaleuca viridifloraNiaouli (Nerolidol) EO Melaleuca quinquinerviaNutmeg EO Myristica fragransOat EO Avena sativaOpoponax EO Commiphora guidotti – EthiopiaOrange Bitter EO Citrus aurantiumOrange Sweet EO Citrus sinensisOregano EO Thymus capitatusPalmarosa EO Cymbopogon martiniParsley Seed EO Petroselinum sativumPatchouli EO Pogostemon cablinPennyroyal EO Mentha pulegiumPepper Black EO Piper nigrumPeppermint EO Mentha piperitaPetitgrain EO Citrus aurantiumPine Needle EO Abies sibiricaPine Dwarf EO Pinus mugo – Austria (Needle)Pine Scots EO Pinus sylvestris – Hungary (Needle Twig)Pine EO Pinus pinaster – USA (Needle)Ravensara EO Ravensara aromaticaRosalina EO Melaleuca ericifolia – AustraliaRose EO Rosa centifoliaRosemary EO Rosmarinus officinalisRosewood EO Aniba roseaodoraSage EO Salvia officinalisSandalwood EO ( Mysore ) Santalum albumSpearmint EO Mentha spicataSpike Lavender EO Lavandula latifoliaSpikenard EO Nardostachys jatamansiSpruce EO Tsuga canadensisSpruce Black EO Picea mariana – Norway (Needle)Star Anise EO Illicium verumTagetes EO Tagetes minutaTangerine EO Citrus reticulataTarragon EO Dracunculus spp.Tea Tree EO Melaleuca alternifoliaThuja EO Thuja occidentalisThyme Red EO Thymus vulgarisThyme Sweet EO Thymus vulgaris – FranceThyme White EO Thymus vulgaris – SpainTurmeric EO Curcuma longa – IndiaValerian Root EO Val ariana officinalisVerbena EO Lippia citriodoraVetiver EO Vetiveria zizanoidesWintergreen EO Gaultheria procumbenWormwood EO Artemisia absinthiumYarrow EO Achillea Millefolium – BulgariaYlang-Ylang Extra EO Canaga odorataYlang-Ylang I EO Canaga odorataYlang-Ylang III EO Canaga odorata
Carrier oilsApricot Kernel Oil Prunus armeniacaAloe Vera Oil Aloe barbadensis -USAAvocado Oil Persea americanaBorage Oil Borago officinalisCamelina Oil Camelina sativaCamellia Oil Camellia sinesis – Japan (Seed)Canola Oil Brassica napus – CanadaCastor Oil Ricinus communis – India (Seed)Coconut Oil (Fractionated) Cocos nuciferaCoconut Oil (Virgin) Cocos nuciferaCorn OilCottonseed Oil Gossypium seminis – USA (Seed)Emu OilEvening Primrose Oil Oenothers biennisFlax Seed (Linseed) Oil Linum usitatissimum – USAForaha (Tamanu) Calophyllum InophyllumGrapeseed Oil Vitis viniferaHazelnut Oil Corylus avellanaHemp Seed Oil Cannabis SativaJojoba Golden Simmondsia chinensisKukui Oil Aleurites moluccansMacadamia Nut Oil Macadamia integrifolia – AustraliaOlive Oil Olea eurpaea – ItalyPalm Oil Passiflora elacsis – USAPalm Kernel Oil Passiflora aincarnata – MalaysiaPeanut Oil Arachis hypogeae – USAPecan Oil Algooquian paccan – USAPistachio Nut Oil Pistacia vera – USARose Hip Seed Oil Rosa mosquetaSafflower Oil Carthamus tinctorius – GuatamalaSesame Oil Sesamum indicumSoya Bean Oil Soja hispida – USASunflower Oil (High Oleic) Helianthus annuusSweet Almond Oil Prunus dulcisWalnut Oil Juglans ragia – USAWheatgerm Oil Triticum vulgareAlmond Fragrance OilBitter Almond Fragrance OilCoconut Fragrance OilRosemary Oil Extract
NMR Reference: Ref: “Essential Oils Analysis by Capillary Gas Chromatography and Carbon-13 NMR Spectroscopy ” by K.H. Kubeczka and V. Formacek, 2nd Ed, Wiley, NY (2002)
Essential Oil Chemistry Reference: Journal of Essential Oil Research
See Process NMR Associates Essential Oils Page

NMR Acronyms
Excellent NMR Acronym Summary Pages – Oxford University, University of Wisconsin

NMR on a Chip
All you need to purchase with this PCI Card NMR spectrometer is an amplifier, a magnet and probe. Details can be obtained at the Spincore RadioProcessor Page. Benchtop high resolution NMR is very close to being a reality. Combining new spectrometer design with micro-probe and sample automation such as that found at Protasis will make benchtop QA-QC spectrometers a reality and place NMR spectrometers in the hands of people who can utilize them for routine testing at an affordable price.

Fat Content of Live Salmon
MOUSE NMR application on Salmon

Mobile NMR of Polyethylene Pipes
MOUSE NMR application to polyethylene pipes.

Upcoming NMR Meetings for 2006
47th ENC Conference will be held April 23 – 28, 2006, at The Asilomar Conference Center, Pacific Grove, California – Program.
EUROMAR - York will be held July 16-21, 2006 at The University of York Main Campus, Programme
22nd International Conferences on Magnetic Resonance in Biological Systems will be held August 20-25, 2006 in Goettingen, Germany – programme
6th Colloquium on Mobile NMR will be held 6-8 September 2006 in Aachen, Germany – Program
SMASH 2006 will be held September 10-13 at the Sheraton Hotel in Burlington, Vermont – Program
The NMR Symposium of the 48th Rocky Mountain Conference on Analytical Chemistry will be held July 23 – 27, 2006. The conference site is the Beaver Run Resort & Conference Center in Breckenridge, Colorado.
21st Meeting of the Central European NMR Discussion Groups will be held April 23-26, 2006, Valtice, Czech Republic in the hotel HUBERTUS in Valtice Castle
14th ISMRM will be held 6-12 May 2006 in Seattle Washington – program
ANZMAG 2006 will be held February 12-16 at the Murramarang National Park, NSW, Australia – Programme

Fast NMR Field Cycling
Stelar s.r.l of Italy manufacture a fast field cycling NMR spectrometer that shuttles a sample in and out of a varying magnetic field to generate T1 longitudinal relaxation profiles obtained by measuring T1 at a series of different magnetic field strengths. Stelar has developed low-inductance, air-coil magnets and power supplies capable of switching the field electronically to any desired value in a matter of milliseconds while, at the same time, maintaining the high field stability and homogeneity required by NMR. This allows the link between NMR relaxation phenomena and molecular dynamics to explored initially in the following application fields: the hydration of paramagnetic metal ions and organometallic complexes, the dynamics of liquid crystals, and the dynamics of proteins.

More on NMR of Wine from Physics in Action

2006-02-08T17:14:00.000-05:00

Magnetic resonance sniffs out bad winePhysics in Action: November 1998, Claude Guillou and Fabiano Reniero
Nuclear magnetic resonance (NMR) has come a long way since it was discovered in the 1940s. This physical phenomenon, which arises from the intrinsic spin possessed by many nuclei, has provided a better understanding of the physics of nuclei and molecules. It has also been exploited to analyse the properties of many different materials in chemistry, physics, polymer science and biomedicine.
Recent developments in the use of high magnetic fields and pulsed NMR techniques have made it possible to probe the structure of organic compounds as complex as proteins. Imaging machines based on the NMR principle have also been developed, and now provide a powerful and non-invasive tool for diagnosing a variety of medical conditions. However, less well known are the applications of NMR for analysing food and drink. At the Joint Research Centre at Ispra, we are using a technique to detect whether a wine has been adulterated with foreign substances. This method is based on an NMR measurement of the deuterium content of wine.
Nuclear magnetic resonance is observed for nuclei with non-zero nuclear spin, which includes both the hydrogen nucleus (a proton) and the deuterium nucleus (a proton and a neutron). However, the physical properties of these two isotopes dictate that the NMR signal produced by deuterium nuclei is over 100 times weaker than that produced by the same number of hydrogen nuclei. The natural abundance of deuterium is also extremely low, with typical samples of hydrogen containing only about 0.015% of deuterium. This means that the NMR signal due to deuterium in a natural sample containing hydrogen is about a million times weaker than the signal due to hydrogen.
Despite this drawback, deuterium has very interesting properties for quantitative NMR. Deuterium has a quadrupole magnetic moment rather than a dipole moment, which means that it is unaffected by the nuclear Overhauser effect. This effect – in which radiofrequency radiation applied to the nucleus changes the strength of the resonance – is often exploited to enhance the NMR signal, but it also degrades the precision of quantitative techniques. Indeed, deuterium spectra generally show distinct peaks that are suitable for quantitative purposes.
An important advantage of NMR is that the deuterium content can be determined for each of the sites in a hydrogen-containing molecule that are not magnetically equivalent. For ethanol, for example, it is possible to determine separately the deuterium content of the methyl group (CH2D) and the methylene alcohol group (CHD) in the deuterium NMR spectrum. The low natural abundance of deuterium means that it is only necessary to consider molecules containing a single deuterium atom.
How does the deuterium content of wine indicate whether it has been adulterated? This is possible because the deuterium content of water in the hydrosphere and biosphere is not a constant. As an extreme example, ice at the South Pole has very low deuterium content, with a deuterium-to-hydrogen ratio of about 90 parts per million (ppm), while ocean water has a value of about 156 ppm. This natural variation is due to thermodynamic and kinetic effects that take place during the water cycle, when water evaporates from the ocean and precipitates over land. The transpiration of water from plants also favours lighter isotopes, leading to a greater abundance of deuterium in the water contained in plants.
The deuterium content of the water in any plant, including the vines used in wine production, therefore depends on several factors that can be related to the geoclimatic conditions during plant growth. Moreover, the water in the plant is used in the photosynthesis of different chemicals, in particular the production of glucose. This transfers the isotopic content of the water to the glucose and other sugars present in the plant, which means that both the metabolism and physiology of the plant influence the final deuterium content of the sugars. The deuterium content of the sugars therefore provides a good indication of their botanical origin.
Although sugars are particularly difficult to study with deuterium NMR, it is possible to detect the deuterium content of the methyl group in ethanol, which is produced during the yeast fermentation of wine. Ethanol is responsible for most of the alcoholic content of wine, and it retains a deuterium-to-hydrogen ratio representative of the sugars from which it is produced. Quantitative NMR can therefore be used to determine whether the ethanol present in wine originates from the sugars naturally present in the grapes or whether other sugars have been added to boost the alcoholic content. This practice – known in the trade as “chaptalization” – is allowed in the European Union, but only within specified limits.
A simple way of using NMR to detect sugar in wine is to compare the deuterium content of the wine being tested with a genuine wine from the same geographical origin. This requires an accurate determination of the NMR signal from the genuine wine, which is being done for all European wine-producing countries by our laboratory and other official laboratories of the European Union. The NMR data of more than 10 000 samples, together with an exhaustive description of the wines, have been collated since 1991 and now provide a powerful tool against fraudulent practice.
Other isotopic indicators, such as the content of oxygen-18 in wine or carbon-13 in ethanol, can be used to help detect other types of fraud, such as watering down the wine or false declarations of geographic origin. These parameters are usually measured by mass spectrometry, but this does not provide the site-specific information given by deuterium NMR.
Isotopic techniques, particularly the NMR analysis of deuterium, can also be used to control the authenticity of fruit juices by first converting the sugars into ethanol using controlled fermentation. Deuterium NMR can also be used to characterize the origin of natural flavours such as vanillin or raspberry. In future the combination of nuclear magnetic resonance and mass spectrometry will almost certainly lead to many other applications in detecting frauds in food.
About the authorClaude Guillou and Fabiano Reniero are at the Joint Research Centre of the European Commission, Ispra, Italy.

Olive Oil Regional Authenticity from NMR Spectroscopy

2006-02-08T17:11:00.000-05:00

High field 1H and 13C NMR has been used to identify the region where an olive oil was produced – See Segre et al. Other methodologies have involved reacting hydroxyl groups in the olive oil with phospochloridite which allows detailed 31P NMR signatures to be obtained that reveal detailed chemistry distributions within the olive oil allowing an even greater discernment of chemical differences based on origin.

Much of the work in this area has been performed by Apostolos Spyros in Crete. Here are a few of his papers:

“Application of 31P-NMR spectroscopy in food analysis. I. Quantitative determination of mono- and diglycerides in virgin olive oils”. A. Spyros, Photis Dais, J. Agric. Food Chem., 2000, 48, 802 . (pdf)

“Quantitative determination of the distribution of free hydroxylic and carboxylic groups in unsaturated polyester and alkyd resins by 31P NMR spectroscopy”.A. Spyros, J. Appl. Polym. Sci., 2002, 83, 1635. (pdf)

“Kinetics of diglyceride formation and isomerization in virgin olive oils by employing 31P NMR spectroscopy. Formulation of a quantitative measure to assess olive oil storage history”. A. Spyros, A. Fillipidis and P. Dais, J. Agric. Food Chem., 2004, 52, 157. (pdf)

This approach has also been applied to other edible oils so that their presence as adulterants can be observed and quantified:

“Classification of edible oils by employing 31P and 1H NMR Spectroscopy in combination with multivariate statistical analysis. A proposal for the detection of seed oil adulteration in virgin olive oils “. G. Vigli, A. Fillipidis, A. Spyros and P. Dais, J. Agric. Food Chem., 2003, 51, 5715. (pdf)

“Detection of extra virgin olive oil adulteration with lampante olive oil and refined olive oil using NMR spectroscopy and multivariate statistical analysis”. G. Fragaki, A. Spyros, G. Siragakis, E. Salivaras, P. Dais, J. Agric. Food. Chem., 2005, 53, 2810.(pdf)

Please contact Process NMR Associates with your potential 31P analysis.

Online NMR Spectrometer

2006-01-02T15:42:00.000-05:00

Process NMR unit in NEMA enclosure. Magnet is in the left hand side of the cabinet. Sample flows through magnet but is halted in probe by dual solenoids controlled by pulse sequence. From top to bottom of the electronics rack is a computer with pulse sequence generator, a spectrometer with amplifier, shim driver DAC units, and a power supply.

Online 58.3 MHz NMR Spectrometer Magnet

2006-01-02T15:37:00.000-05:00

Fully shielded permanent magnet system for high resolution NMR spectrometer.

New Russian TD-NMR Company

2005-12-28T14:32:00.000-05:00

Just found a new player in the TD-NMR spectrometer domain – Resonance Systems Ltd. They also have a blog. Appears to be a new system similar to Magritek technology as well as Minispec.

Mid-Hudson ACS - Planned Meetings for Spring 2006

2005-12-28T14:27:00.000-05:00

Meeting #1
“Science Policy: Chemistry and Nuclear Waste Disposal” Dr. Douglas J. Raber GreenPoint Science
Wednesday, March 15, 2006, Orange County Community College Middletown, Refreshments: 6:15 PM, Lecture: 7:00 PM (Room TBA)* Room to be announced on the Mid-Hudson ACS listserv and at www.midhudsonacs.org. Contact Tim MacMahon (OCCC) at 845-341-4575 or by e-mail at tmacmaho@sunyorange.edu.

About the lecture: Soon after the end of World War II, peaceful uses of atomic energy became a major thrust of scientific endeavor around the world. At present, the world derives 16 percent of its electricity from nuclear power, mainly in industrialized countries. The level is 20 percent in the United States and 75 percent in France. Concerns about safety in the nuclear power industry have been a source of continuing controversy for many years, and the single most important challenge in this area is what to do with nuclear waste. The spent nuclear fuel from a reactor is highly radioactive and will remain so for an extremely long time. The potential for release of radioactive material into the environment is strongly coupled to the chemical properties of the waste material, so many of the problems and many of the potential solutions are chemical in nature. This talk will present issues in current national policy and will discuss the interplay between science and policy, using several National Research Council studies to illustrate the complexity of the problem. How is scientific input obtained? How is it utilized? Does it receive the respect that it deserves? And what can you do to improve the situation?

About the speaker: Dr. Raber is a science policy consultant with GreenPoint Science, which he formed in 2004. Previously, he served for thirteen years as Director and then Senior Scholar of the Board on Chemical Sciences and Technology at the National Academy of Sciences and its operating arm, the National Research Council (NRC). Before joining the NRC in 1989, he was a member of the faculty of the University of South Florida from 1970 to 1990, publishing some 70 research articles. Dr. Raber is active in ACS governance, serving recently on the C&EN Advisory Board, the Committee on Chemistry and Public Affairs, and the Committee on Science (which he previously chaired). He recently completed several terms as the Secretary of the U.S. National Committee for IUPAC and currently serves as Chair of the Chemical Technology Operating Council of the AIChE. Dr. Raber’s responsibilities at the NRC centered on organizing and directing science and science policy studies, particularly in the areas of federal policy and its interrelationships with the chemical sciences. These efforts resulted in more than 50 reports and monographs that provide technical policy guidance on topics that encompass R&D opportunities, laboratory safety and management, nuclear waste disposal, and the threat of terrorism.

Directions: From Rte. 17M West in Middletown turn left onto Fulton Street. Turn left onto Wawayanda Ave. Turn left onto Grandview Ave. Enter parking lot on right. For complete directions and campus map, visit http://www.sunyorange.edu/aboutus/directions/index.shtml.

Meeting #2
“Nanoscale Building Blocks for Mesoscopic Materials” Dr. Tom Mallouk, Pennsylvania State University, Monday, March 20, 2006, at IBM* Refreshments: 6:15 PM, Lecture: 7:00 PM

*Registration for this talk is required. Contact Charles Davis (IBM) at 845-892-9570 or by e-mail at cdavis@us.ibm.com by March 13. Photo ID must be presented at the site. Room information and directions will be provided to all registered attendees.

About the speaker: Dr. Mallouk is the DuPont Professor of Materials Chemistry and Physics and the Director of the Center for Nanoscale Science at Penn State. His research focuses on the assembly of nanoscale materials and their applications to interesting problems in chemistry, including photocatalysis, molecular electronics, environmental remediation, fuel cell electrochemistry, chemical sensing, and catalytically driven movement.

Meeting #3
“Mechanism of Oxidation of DNA by Pt(IV) Complexes” Dr. Sunhee Choi, Department of Chemistry and Biochemistry, Middlebury College
Friday, March 31 2006, Vassar College, Refreshments:6:15 PM, Lecture:7:00 PM Mudd Chemistry Building (Room TBA)*

*Room to be announced on the Mid-Hudson ACS listserv and at www.midhudsonacs.org.
Contact Joe Tanski (Vassar) at 845-437-7503 or by e-mail at jotanski@vassar.edu.

About the lecture: Platinum complexes are biologically important for their anticancer activities. The interaction of DNA with PtII complexes has been extensively studied by many research groups. PtIV complexes are kinetically inert and their reaction with DNA was not generally expected. However, Dr. Choi’s research has shown that PtIV complexes with highly electron-withdrawing and bulky ligands have high reduction potentials and high reactivity toward 5’-GMP. Furthermore, a PtIV complex, trans-Pt(d,l)(1,2-(NH2)2C6H10)Cl4, [PtIVCl4(dach)], which has a high reduction potential, oxidizes 5’-dGMP, 3’-dGMP and 5’-d[GTTTT]-3’. Kinetic studies and the proposed mechanism will be discussed.

About the speaker: Dr. Sunhee Choi is Professor of Chemistry and Biochemistry at Middlebury College in Vermont. Dr. Choi received a B.A. degree from Seoul National University in 1973 and went on to receive a master’s degree in Physical Chemistry at the Korean Advanced Institute of Science in 1975. She earned her Ph.D. in Physical Chemistry at Princeton University in 1982 in the laboratory of Professor Thomas G. Spiro. After her Ph.D. she became an industrial chemist at Colgate-Palmolive where she was awarded the Colgate Presidential Award for Technical Excellence and obtained a U.S. Patent for cold water detergency. In the fall of 1987, she joined the faculty at Middlebury. Dr. Choi is active in research in metals in biological system with many of her undergraduate colleagues. Her research has been funded from a variety of sources such as the National Institutes of Health, National Science Foundation, Petroleum Research Fund, Research Corporation, and Vermont-EPSCOR.

Directions: Vassar College is located off Raymond Avenue in Poughkeepsie, NY. Refer to the following link for driving directions and campus map: http://www.vassar.edu/directions/. Enter the Main Entrance of the campus on Raymond Avenue and The Main Building and College Center are in front of the Main Entrance. The Security Guard at the Main Entrance will direct you to parking. The Villard Room is on the second floor of the Main Building/College Center. The Alumnae House is located across the street from the tennis courts on Raymond Ave at Vassar.

ASPeCT Magnet Technologies Ltd

2005-11-09T11:45:00.000-05:00

A company that has recently been developing cutting edge permanent magnet systems is ASPeCT Magnet Technologies who are developing MRI and NMR magnets for industrial applications. The magnets are fully shielded permanent magnets of varying bore size that enable fully shimmed 60 MHz process FT-NMR systems as well as industrial and medical MRI. Our interest is obviously in their NMR magnets but there also possibilities developing to use gradient shimming to allow spatially specific high resolution spectra to be obtained from objects being imaged….eg. water/sugar NMR spectra obtained from citrus fruits. The ASPeCT website contains 2 presentations of the various technologies under development.

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ASPeCT Magnet Technologies Ltd