I have recently been forced into moving the blog site to a new server. The entire blog history has been placed in a single update. Sorry for any inconvenience this might cause.

Below are the entries from November 2005- September 2006

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-110

A 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 2006

HTS-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.

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 ChemistryThe 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) Analysis
The 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 Seeds
Sunflower, 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 Products
Time 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 Polysaccharides
Polysaccharides 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/Zeolites
The 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 applications
The 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 Distribution
Cellulose 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 Content
Pharmaceuticals (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 products
Simplicity of use in routine production measurements and in advanced laboratories for complicated analysis
Mobility of the hardware and low cost for the overall device
Non-invasive measurements of any sample
Hardware solutions for non-standard NMR applications
Permanent technical support and comprehensive scientific consulting
Fair price and absolute ease of operation!

Portable Low-Resolution NMR Analyzer

Spin Track Spectrometer

Analyzer is designed to perform:

All standard NMR applications
Development of new NMR-based techniques
Teaching 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 Connectivity
Fast sensors replacement
Compatible with all Microsoft® Windows® operating systems


Relax 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

Stationary Spin Track

Analyzer is designed to perform:

Standard routine NMR applications
Development of new NMR-based techniques
Teaching 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 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 Connectivity
Fast 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 Connectivity
Compatible 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

Filed under: Process NMR, Analytical NMR, Chemistry — Administrator @ 9:33 pm

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—Introduction
Ken Visscher—Open-Access Laboratories in Industry
Nick Burlinson—Design and Installation of a Departmental NMR Facility
Eugene 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.

The Anatomy of a Superconducting NMR Magnet

May 18th, 2006

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.

8th International Bologna Conference on Magnetic Resonance in Porous Media

May 16th, 2006

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.

Symbion Systems Inc

May 3rd, 2006

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.

May 3rd, 2006

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.

16th ISMAR 2007 – Website Posted

April 26th, 2006

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/

Energy Information

April 1st, 2006

Here are a few excellent links to the energy situation in the 21st Century:

Energy Technologies for the Twenty-First Century
WEC – Survey of Energy Resources 2001

DOE – This Week in Petroleum
Energy Information Administration
Main Site

Modern Drug Discovery – NMR Articles

March 15th, 2006

ACS Publication “Modern Drug Discovery” – Available NMR Articles
Screening with NMR
NMR Spectroscopy Software – Molecular biologists can now use proton NMR data to elucidate protein structure.
NMR on Target
Ultracool NMR Technology – Cryoprobes
Looking for Quality

NMR of Silicones in Pharmaceutical Developments

March 14th, 2006

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

March 14th, 2006

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

PNA Talk – Dr Giammatteo to Present Sigma Xi Seminar at Quinnipiac University

March 13th, 2006

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

NMR Applications in Food Quality

March 10th, 2006

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?

March 10th, 2006

A handy calculator from BP allows you to calculate your impact on global warming – Carbon Calculator.

Heavy Oil and Bitumen Upgrading

March 10th, 2006

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

Spatial Encoding Produces 2D-NMR in a Single Scan

March 9th, 2006

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

March 9th, 2006

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

Polymer Chemistry Resource

March 1st, 2006

Beautiful site that gives overviews of most polymer chemistry systems.

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 Swinss 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 excellent 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 excellent 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

February 18th, 2006

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.

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 p/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)         Silicon 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)

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 Edwards
Manager, Process and Analytical NMR Services
Process NMR Associates LLC,
87A Sand Pit Rd
Danbury, CT 06810, USA
Tel: (203) 744-5905


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 Dobmann
Fraunhofer-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 Spin Splittings and Chemical Shift Tutorials – NMR Chemical Shift Predictor

February 15th, 2006

The Chemistry Department at the University of Saint Thomas, St Paul, MN, has an excellent number of tutorials covering the prediction of NMR spectra as well as a 1H NMR predictor web page.


NMR Structural Elucidation of Mountain Dew Nailed

February 13th, 2006

Ken Skidmore at San Francisco State University has finally answered the question on our lips for about a decade now….can NMR do the dew? Seems that it can, in an incredible turn of events the syrup formula has finally been exposed for what it really is… a $%!* load of sugar – the NMR evidence is irrefutable.

BioNMR Forum

February 9th, 2006

BioNMR is a forum for NMR spectroscopists to discuss their projects and find help from the online NMR community.

An excellent NMR users group exists (AMMRL-Association of Managers in Magnetic Resonance Laboratories) which consists of NMR facility managers and industrial NMR users. The group has an archive of questions posed and answers given to many issues that arise from the operation of Varian, Bruker and JEOL spectrometers predominantly in a college setting. Issues with NMR operation such as safety and peripheral infrastructure, as well as scheduling of users, manipulation of data and servicing of equipment are all covered in the discussions. Both groups can be joined at the sites above.

There is a Bruker users group archive directory located at http://calmarc3.cchem.berkeley.edu/archives/bum/. Membership of the Bruker users group can be obtaied by contacting he following e-mail (‘bruker-users-mail-request@purcell.cchem.berkeley.edu’). Membership to the Bruker brotherhood is carefully guarded and you will only be admitted if you operate Bruker equipment.

Free NMR Postprocessing Software – SpinWorks

February 9th, 2006

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.”


Olive Oil Regional Authenticity from NMR Spectroscopy

February 8th, 2006

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.

More on NMR of Wine from Physics in Action

February 8th, 2006

Magnetic resonance sniffs out bad wine
Physics 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 author
Claude Guillou and Fabiano Reniero are at the Joint Research Centre of the European Commission, Ispra, Italy.

NMR Method Patented to Determine Presence of Organic Sub-Structures in Molecules

February 8th, 2006

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

February 8th, 2006

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

February 8th, 2006

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.

Patented NMR Method for Quality Control of Medicinal Natural Products

February 8th, 2006

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

February 8th, 2006

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.

See Process NMR Associates for your NMR analysis needs.

13C NMR Analysis for Authentification of Gum Arabic

February 8th, 2006

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

February 7th, 2006

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 for
including 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 Oils
Ajowan EO Trachyspermum copticum – India (seed)
Allspice Berry EO Pimenta officinalis
Amyris EO Amyris Balsamifera – Jamaica
Angelica Root EO Angelica archangelica
Angelica Seed EO Angelica archangelica
Anise Seed EO Pimpinella anisum
Armoise EO Artemesia herba alba – Morocco
Balsam Peru EO Myroxylon balsamum
Balsam Tolu EO Myroxylon balsamum – El Salvador
Basil EO Ocimum basilicum
Bay Leaf EO Pimenta racemosa
Bay Laurel EO Laurus nobilus – Jamaica
Benzoin Liquid Resin Benzion Styrax – China
Bergamot EO Citrus bergamia
Birch Sweet EO Betula lenta
Black Pepper EO Piper nigrum – India
Blood Orange EO Citrus sinensis var.
Bog Myrtle EO Myrica gale – Europe
Cabrueva EO Myocarpus fastigiatus – South America
Cade EO Juniperus oxycedrus – Spain
Cajeput EO Melaleuca cajeputi
Calamus EO Acorus calamus
Camphor EO Cinnamomum camphora
Cananga EO Cananga odorata
Caraway Seed EO Carum carvi
Cardamom Seed EO Elattaria cardamomum
Cassia EO Cinnamomum Cassia – China
Catnip EO Nepeta cataria
Carrot Seed EO Daucus carota
Cedarwood EO Cedrus atlantica
Cedarwood Atlas EO Cedrus atlantica – Morocco
Cedarwood Chinese EO – Cupressus funebris – China
Cedarwood Himalayan EO Cedrus deodara – Himalaya
Cedarwood Mexicana EO Juniperus mexicana – Mexico (also Texas Cedarwood)
Cedarwood Virginian EO Juniperus Virginiana – USA
Cedar Leaf EO Thuja occidentalis – USA
Celery Seed EO Apium graveolens
Chamomile German EO Matricaria chamomilla
Chamomile Egypt EO Matricaria chamomilla
Chamomile Spain EO Matricaria chamomilla
Chamomile Roman EO Anthemis nobilis
Cinnamon Bark EO Cinnamomum
Cinnamon Leaf EO Cinnamomum zeylanicum
Citronella EO Cymbopogon nardus
Citronella Sri Lanka EO Cymbopogon nardus
Citronella Java EO Cymbopogon winterianus
Clary Sage EO Salvia sclarea
Clove Bud EO Eugenia caryophyllata
Clove Leaf EO Eugenia caryophyllata – Madagascar
Copaiba Balsam EO Copaifera officinalis
Coriander Seed EO Coriandrum
Cumin EO Cumimum cymimum
Cypress EO Cypressus sempervirens
Cypriol EO Cyperus scariosus – Brazil (Flowers)
Davana EO Aretemesia pallens
Dill Seed EO Anethum sowa – India
Dill Weed EO Anethum graveolens
Dragons Blood EO Croton lechleri – South America (Resin)
Dwarf Pine EO Pinus mugo
Elemi EO Canarium luzonicum
Eucalyptus Citriodora EO Eucalyptus citriodora
Eucalyptus Globulus EO Eucalyptus globulus
Eucalyptus Radiata EO Eucalyptus radiata
Eucalyptus Spain EO Eucalyptus globulus
Eucalyptus China EO Eucalyptus globulus
Eucalyptus Smithii EO Eucalyptus smithii – China (leaf)
Fennel Sweet EO Foeniculum vulgare
Fennel Hungary EO Foeniculum vulgare
Fennel Spain EO Foeniculum vulgare
Fennel Rectified EO Foeniculum vulgare
Fennel Sweet EO Foeniculum vulgare
Fir Needle EO Abies alba
Fir Siberian EO Abies sibirica – Austria (Needle)
Fir Canadian EO Abies balsamea – USA (Needle)
Frankincense EO Boswellia carteri
Galbanum EO Ferula galbaniflua – Turkey (Gum)
Garlic EO Allium sativum – Mexico (Bulb)
Geranium EO Pelargonium graveolens
Geranium Rose EO Pelargonium roseum – France
Ginger EO Zingiber officinale
Ginger Grass EO Cymbopogon martini – China
Grapefruit Pink EO Citrus paradise
Guaiacwood EO Bulnesia sarmienti – Paraguay
Helichrysum EO Helichrysum angustifolium
Helichrysum Italicum EO Helichrysum italicum
Hop EO Humulus lupulus
Hyssop EO Hyssopus officinalis
Juniper Berry EO Juniperus communis
Labdanum EO Cistus labdanum
Lantane EO Lantara camara – Madagascar
Lavandin EO Lavendula latifolia
Lavender EO Lavendula angustifolia
Lemon EO Citrus limon
Lemongrass EO Cymbopogon citratus
Lemon Myrtle EO Backhousia citriodora – Australia
Lime EO Citrus aurantium
Lime (Distilled) EO Citrus aurantifolia
Lime (Cold Pressed) EO Citrus aurantifolia
Litsea Cubeba EO Litsea cubeba – China
Mace EO Myristica fragrans – Spain (Husk)
Mandarin EO Citrus reticulata
Marjoram EO Origanum majorana
Melissa EO (Lemon Balm) Melissa officinalis
Mint Brazil EO Mentha arvensis
Mint China EO Mentha arvensis
Mint Japan EO Mentha arvensis
Mugwort EO Artemisia vulgaris
Mullein EO Verbascum thapsus – India (Leaf)
Myrrh EO Commiphora myrrha
Myrtle EO Myrtus communis
Neroli EO Citrus Aurantium – Egypt
Niaouli (Cineole) EO Melaleuca viridiflora
Niaouli (Nerolidol) EO Melaleuca quinquinervia
Nutmeg EO Myristica fragrans
Oat EO Avena sativa
Opoponax EO Commiphora guidotti – Ethiopia
Orange Bitter EO Citrus aurantium
Orange Sweet EO Citrus sinensis
Oregano EO Thymus capitatus
Palmarosa EO Cymbopogon martini
Parsley Seed EO Petroselinum sativum
Patchouli EO Pogostemon cablin
Pennyroyal EO Mentha pulegium
Pepper Black EO Piper nigrum
Peppermint EO Mentha piperita
Petitgrain EO Citrus aurantium
Pine Needle EO Abies sibirica
Pine Dwarf EO Pinus mugo – Austria (Needle)
Pine Scots EO Pinus sylvestris – Hungary (Needle Twig)
Pine EO Pinus pinaster – USA (Needle)
Ravensara EO Ravensara aromatica
Rosalina EO Melaleuca ericifolia – Australia
Rose EO Rosa centifolia
Rosemary EO Rosmarinus officinalis
Rosewood EO Aniba roseaodora
Sage EO Salvia officinalis
Sandalwood EO ( Mysore ) Santalum album
Spearmint EO Mentha spicata
Spike Lavender EO Lavandula latifolia
Spikenard EO Nardostachys jatamansi
Spruce EO Tsuga canadensis
Spruce Black EO Picea mariana – Norway (Needle)
Star Anise EO Illicium verum
Tagetes EO Tagetes minuta
Tangerine EO Citrus reticulata
Tarragon EO Dracunculus spp.
Tea Tree EO Melaleuca alternifolia
Thuja EO Thuja occidentalis
Thyme Red EO Thymus vulgaris
Thyme Sweet EO Thymus vulgaris – France
Thyme White EO Thymus vulgaris – Spain
Turmeric EO Curcuma longa – India
Valerian Root EO Val ariana officinalis
Verbena EO Lippia citriodora
Vetiver EO Vetiveria zizanoides
Wintergreen EO Gaultheria procumben
Wormwood EO Artemisia absinthium
Yarrow EO Achillea Millefolium – Bulgaria
Ylang-Ylang Extra EO Canaga odorata
Ylang-Ylang I EO Canaga odorata
Ylang-Ylang III EO Canaga odorata

Carrier oils
Apricot Kernel Oil Prunus armeniaca
Aloe Vera Oil Aloe barbadensis -USA
Avocado Oil Persea americana
Borage Oil Borago officinalis
Camelina Oil Camelina sativa
Camellia Oil Camellia sinesis – Japan (Seed)
Canola Oil Brassica napus – Canada
Castor Oil Ricinus communis – India (Seed)
Coconut Oil (Fractionated) Cocos nucifera
Coconut Oil (Virgin) Cocos nucifera
Corn Oil
Cottonseed Oil Gossypium seminis – USA (Seed)
Emu Oil
Evening Primrose Oil Oenothers biennis
Flax Seed (Linseed) Oil Linum usitatissimum – USA
Foraha (Tamanu) Calophyllum Inophyllum
Grapeseed Oil Vitis vinifera
Hazelnut Oil Corylus avellana
Hemp Seed Oil Cannabis Sativa
Jojoba Golden Simmondsia chinensis
Kukui Oil Aleurites moluccans
Macadamia Nut Oil Macadamia integrifolia – Australia
Olive Oil Olea eurpaea – Italy
Palm Oil Passiflora elacsis – USA
Palm Kernel Oil Passiflora aincarnata – Malaysia
Peanut Oil Arachis hypogeae – USA
Pecan Oil Algooquian paccan – USA
Pistachio Nut Oil Pistacia vera – USA
Rose Hip Seed Oil Rosa mosqueta
Safflower Oil Carthamus tinctorius – Guatamala
Sesame Oil Sesamum indicum
Soya Bean Oil Soja hispida – USA
Sunflower Oil (High Oleic) Helianthus annuus
Sweet Almond Oil Prunus dulcis
Walnut Oil Juglans ragia – USA
Wheatgerm Oil Triticum vulgare
Almond Fragrance Oil
Bitter Almond Fragrance Oil
Coconut Fragrance Oil
Rosemary 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

February 7th, 2006

Excellent NMR Acronym Summary Pages –     Oxford University,  

                                                                    University of Wisconsin

NMR on a Chip

January 25th, 2006

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

January 25th, 2006

MOUSE NMR application on Salmon

Mobile NMR of Polyethylene Pipes

January 25th, 2006

MOUSE NMR application to polyethylene pipes.

Upcoming NMR Meetings for 2006

January 25th, 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

January 25th, 2006

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.

Fast NMR Field Cycling

January 25th, 2006

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.

Anatomy of a Process NMR Spectrometer

January 2nd, 2006

Online NMR with Open Enclosure

Open RF Components of NMR Spectrometer

Open RF Components_2

Shim Unit DACS

Open Magnet Enclosure – Fully Shielded NdFe Permanent Magnet at 1.4 Tesla

NCUT – Workshop Proceedings

December 28th, 2005

Final Report of the Oil Sands Chemistry and Engine Emissions Roadmap Workshop

Fuel Technical Reviews from ChevronTexaco

December 28th, 2005

Motor Gasoline Technical Review
Aviation Fuel Technical Review
Diesel Fuel technical Review

Challenges in the Development of New Processes for Refining and Petrochemistry

December 28th, 2005

Overview of challenges to be faced in developing new refining and petrochemical processes.

Government natioanl Renewable Energy Laboratory – Publications

December 28th, 2005


Excellent Paper on Reaction Modeling Trends

December 28th, 2005

Reaction Modeling Trends – a paper by KBC

Low Sulfur Diesel

December 28th, 2005

Excellent review of the effect of the new low sulfur diesel EPA legislation on fuel supply and costs – DOE Report The entire low sulfur diesel report from DOE can be downloaded from here.
Also an excellent paper from Topsoe on revamping HDS units to meet the new specification.
Finally a Chevron technical review of diesel fuels.

IASC – NMR Methodology for Aloe Vera Certification

December 28th, 2005

The International Aloe Science Council has mandated that quantitative 1H NMR analysis be used to certify the quality of Aloe Vera products being sold or placed on the market. Attached here is an article on the subject as well as the certification details from IASC. An excerpt from the article states: “By means of NMR spectrum, it is possible to record all the essential components of Aloe vera and thus make a clear statement regarding the quality of the product. Impurities, be they natural or artificial, can be detected. Decomposition products give information about the period of time elapsing between the leaves being harvested and processed, or about the age of the raw material.”

Process NMR Associates has developed the NMR methodologies prescribed by IASC and can quantify Acemannan, glucose and Malic Acid in the presence of a Nicotinic Acid Amide Standard. Breakdown products such as acetic acid, lactic acid, pyruvic acid, succinic acid can be readily quantified as can the presence of additives such as citric and benzoic acids. Adulterants such as maltodextrin can be readily quantified and the presence of n0n-aloe vera products can also be determined.

Contact John Edwards for details.

Academics View of the NMR Marketplace

December 28th, 2005

Here is an article from Spectroscopy Magazine that typifies the view of NMR. NMR as a sensor for industrial control is still not a concept that readily springs to mind even with people intimately involved in NMR research.

New Russian TD-NMR Company

December 28th, 2005

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.

Fantastic Gift Ideas for The Person Who Has Everything

December 25th, 2005

My sister and brother-in-law opened my eyes to the socially conscious way to give gifts to people who already have more than they need. Who wouldn’t appreciate a gift that leads to the construction of a toilet in a Congo refugee camp? These cool, “make a difference” gifts can be bought online at Oxfamunwrapped.com. Here is my gift for Christmas…
Toilet constructed in Phillip, Democratic Republic of Congo

Mid-Hudson ACS – Planned March 2006 Meeting Schedule

December 22nd, 2005

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.

John Edwards becomes Mid-Hudson ACS Chair-Elect

December 22nd, 2005

John Edwards has been voted in as Chair-Elect of the Mid-Hudson ACS Section.

Solid-State NMR and Polymorphism

December 1st, 2005

At PNA we have recently been working on some interesting polymorph projects utilizing solid-state 13C NMR. Excellent reviews of this subject are given at: Robin Harris of University of Durham (my alma mater) and Cardiff School of Chemistry
A good example of polymorphism determined by NMR in 4-azasteroid systems is given here….Morzycki et al…Steroids 67, 621 (2002).
The FDA have summarized the effects of polymorphism in pharmaceutical solids (PDF Version)

We perform these studies on a dedicated Varian UnityPlus-200 spectrometer to yield spectral and relaxation data to allow the determination of drug-excipient interactions, as well as simple polymorph differentiation and amorphous material content. Both 13C SP-MAS and CP-MAS experiments are utilized in these studies along with T1 and cross-relaxation time determinations.

See Process NMR Associates for your Polymorphism Analysis

NMR Capabilities Expanded at Process NMR Associates

November 16th, 2005

We have recently added TD-NMR capabilities to out suite of NMR services by acquiring Oxford Instruments spectrometers that perform TD-NMR at 2.5 and 20 MHz. The 20 MHz system is an 18 mm Oxford QP20 system, while the 2.5 MHz system is a custom spectrometer operating with a 50 mm bore magnet for large sample analysis. This will allow us to expand into commodities testing such as total hydrogen analysis, oil and water content analysis, and will also allow us to develop low field process NMR applications.

Process NMR Technology at CPACT

November 14th, 2005

A summary of process NMR projects undertaken by CPACT from 1998-2001 is shown on the CPACT website. It’s difficult to decipher why the projects did not come to fruition. Work on the projects appears to have ceased.

NMR and Spectroscopy Events in the Tri-State Area – November 2005

November 9th, 2005

Eastern Analytical Symposium will have a lot of NMR, PAT and spectroscopy sessions according to their technical session schedule. Paul Giammatteo of Process NMR Associates will present on Thursday November 17 – here are the details of his session –
Process Spectroscopy in Industry – Chemicals, Food and PAT, Arranged in Conjunction with the Delaware Valley Section of SAS
Chair, Lois Weyer, ATK Elkton
9:00 Pulse, Acquire, Control: Ten Years of On-Line High Resolution NMR in Refining, Petrochemical, and Food Manufacturing, P. J. Giammatteo and J. C. Edwards, Process NMR Associates
9:40 Process NIR at DuPont: A 20 Year Retrospective, C. H. Sohl, DuPont Engineering Research and Technology
10:20 Break
10:40 Rapid Composition Monitoring for Bio-Sustainable Processes: Useful Tools and Unmet Needs, A. M. Brearley, Consultant
11:20 PAT Applications for Pharmaceutical Processing, B. Diehl, Pfizer, Inc.

The NMR group of the Northern Jersey ACS section will be hosting a talk on Cryoprobe Technology combined with Principal Component Analysis.
The details of the talk are:

Wednesday, November 16, 2005 – The NJACS Proudly Presents:
“New Directions of CryoProbe Technology”
by Kimberly L. Colson, Ph.D. Bruker BioSpin Corp.

The utilization of new NMR technologies, such as CryoProbe technology, has revolutionized the applicability of NMR to many areas of study through a significant gain in sensitivity. In addition, advances in automation and the implementation of statistical approaches to examining variations amongst large datasets have enabled NMR to be used as a tool for classification of samples, and hence for examination of quality control, adulteration, quantification, biomarker discovery, etc.

CryoProbe technology enhances 1H, 13C, 15N, 19F, and 31P NMR sensitivity by a factor of four. This allows components in small quantities to be detected and allows NMR spectra to be acquired 16 times faster than previous methods. Although widely accepted for protein and small molecule structure analysis CryoProbe technology is not yet fully utilized in more challenging applications such as quality control, sample quantification, metabonomics and biomarker discovery. One reason is that the NMR data obtained on large datasets and on complex mixtures produces data that are often difficult to evaluate.

Simple comparison or quantification between large data sets is tedious and often impractical. However, combining the use of new CryoProbe Technology with the pattern recognition and multivariate statistical methods, like principle component analysis (PCA), allows rapid comparison of these large complex data sets. Principle component analysis algorithms can classify an object based on identification of inherent patterns in a set of experimental measurements or descriptors and facilitates the visualization of inherent patterns. Data set comparisons is therefore easier.

This powerful combination of CryoProbe technology, Statistical Analysis methods and new NMR experiments can be employed in many areas including the analysis of pharmaceuticals, natural products, metabolites, synthetic materials, foods, flavors, fragrances, and metabolites, to rapidly assess the composition of substances for quality control, mixing levels, product verification, and product identification. In this lecture we will explain the components that make up this new approach and demonstrate its utility with some examples.

Location: Woodbridge Hilton. Dinner at 6:30 p.m. Seminar at 7:00 p.m.

Buffet dinner: $10 for students and post-docs, $30 for all others, No charge for the seminary only. Beverages provided In the Bar at 5:45 p.m.

ASPeCT Magnet Technologies Ltd.

November 9th, 2005

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.

PNA – Who We Are

November 4th, 2005

Process NMR Associates LLC (PNA) was founded in 1997 by John Edwards and Paul Giammatteo in Danbury CT. Both were Ph.D. chemists working at the Texaco Fuels and Lubricants Research Center in Beacon, New York. Paul was group leader of process analytical and organic spectroscopy and John Edwards was the NMR spectroscopist for the Texaco corporation. Between them they have over 40 years of experience in NMR, organic spectroscopy, process analytical, and petroleum/petrochemical chemistry. Their laboratory includes a 300 MHz Varian NMR spectrometer for liquids analysis, a 200 MHz spectrometer for solids analysis, 2 benchtop TD-NMR spectrometers (2 MHz and 20 MHz), and three 60 MHz process NMR units.

Initially Process NMR Associates (PNA) concentrated on supporting the Invensys MRA product which had been formed by a JV between Invensys and the Elbit ATI NMR company. From 1997-2003 PNA was the application development and technical marketing consultants to that product. In 2003 PNA made a strategic decision to leave the relationship with Invensys and has concentrated on developing it’s analytical NMR service for industry. Currently PNA serves over 100 small and large companies for their liquid and solid-state NMR needs.

In October 2005 PNA entered into a JV arrangement with TTC Labs Inc (Fond du Lac WI). This JV is NMR Process Systems Inc and it will be involved in marketing, installing, servicing and enabling process NMR controlled APC and optimization projects.

Tailor-Made Hydrocarbons

November 4th, 2005

With the US public suddenly awakening to the fact that they have been squandering a finite natural resource with the current SUV craze, there is a huge amount of interest being generated in increase refining capacity, renewable sources of energy and the developoment of a crude oil substitute. With energy prices going to remain the same or increase, I think that Gasification Technology in combination with Fischer Tropsch synthesis will bail us out from the Mad Max scenario of 50 years hence.

Gasification can take many input feeds such as municipal waste, sewage, coal, plastics, bitumen, heavy oil, waste oils, biomass, etc. These are gasified to SynGas (H2/CO) which initially contains many impurities (metals, sulfur, oxides, chlorine etc) some impurities for a refractory (glass) that is removed from the gasifier and this refractory can be readily disposed as it encapsulates a lot of the “nasties”. The gaseous component of the product can be treated to yield pure syngas which can then be passed over Fischer Tropsch (FT) catalyst. The FT process is a gas-to-liquids process that recombines the elements present in the gas into hydrocarbons. The produced hydrocarbons can then be tailor made for the application (fuels, lubes, monomers) by cracking and/or hydroisomerization. FT is also a valuable technology as the large oil companies see it as a technology to develop their stranded gas deposits into a more readily transportable material so that these assets can be monetized.

From waste we will derive the energy required for the future. Shell, Exxon, British Petroleum, Syntroleum, and Sasol-Chevron are just a few of the companies working on GTL technology. Rentech Inc are another company working in collaboration with Texaco and Sasol (now Sasol-Chevron). Here is their statement regarding FT….GTLSite.pdf

13C NMR is the perfect way to monitor the detailed molecular chemistry of the products made by GTL processes. On-line 1H NMR or at line 13C would allow chemistry to be controlled on a timescale of minutes.

The information out there is vast from organizations such as Alaska Natural Gas Transportation and their ideas for the BP project at Nikiski. Modular designs of various process components will lead to small plants and improved product quality.

An excellent summary of the technology is found at Chemlink, Exxon, Sasol, DOE, Eltron Research, Foster Wheeler, SRI Consulting, Statoil, G-T-L, and Thailand.

GTL technology development will have fall out effects in the natural gas market – an excellent economics artive of LNG and GTL is found at EnergyPulse. A Congressional Report also investigates the GTL and natural gas markets. A great source of centralized energy news is EnergyBulletin.net which harvests many articles from around the world dealing with “peak oil” reporting. The Energy Blog is another excellent source of Energy Related Material.

The next big push will be to develop the oils shale, heavy oil and tar sand deposits that are found in Alberta, Utah, and the Orinoco Basin to name a few. These are the only deposits that can yield enough hydrocarbon for the GTL Technologies and meet energy needs for the foreseeable future. Strategically the development of these heavy resources to marketable fuels would remove the US dependence on imported oil.

Mid-Hudson ACS – New Website and Blog

November 4th, 2005

The Mid-Hudson Section of the American Chemical Society has a new website at http://www.midhudsonacs.org and a new blog at http://www.midhudsonacs.org/Blog

Mid Hudson ACS – November Meeting

November 4th, 2005

The Mid-Hudson Section of the American Chemical Society and the Chemistry Department of Vassar College Announce:
“Morphology Of Effect Materials” by Dr. Geoff Johnson, Engelhard Corporation, Wednesday, November 9, 2005 Time: 7:00 PM
Location: Vassar College , Mudd Chemistry Building, 3rd Floor – Science Visualization (Sci Vis) Lab
Contact Joseph Tanski (Vassar) at 845-437-7503 or by e-mail at jotanski@vassar.edu.

About the lecture: Classic pearlescent pigments have evolved far beyond the biologically derived mother-of-pearl that originally inspired them. The class of synthetics that includes pearlescent pigments is now called “effect materials.” This renaming emphasizes that appearance is the sum of many sensory effects, not just color. The most robust effect materials are composed of thin layers of metal oxides coated onto inorganic substrates. The layer structure determines color effects, but the morphology of the substrate plays a significant role in the overall effect. There is also a class of effect materials composed of bismuth oxychloride, in which the morphology of the BiOCl crystal is solely responsible for the observed effects.

About the speaker: Dr. Johnson is originally from South West England, near Bath . He received a BS in Chemistry from the University of Birmingham, UK and his MS in Chemistry from the École Nationale Supérieure de Chimie de Montpellier , France . He earned a PhD in Inorganic Materials Chemistry with Professor Mark Weller at the University of Southampton, UK. Dr. Johnson’s postdoctoral experience includes work in zeolite chemistry with Professor John Parise at SUNY Stony Brook and chemical catalysis at Worcester Polytechnic Institute with Fabio Ribeiro. He joined Engelhard in 2001 as a Research Chemist at the Corporate R&D facility in Iselin , New Jersey . In June 2004, he joined Engelhard’s Appearance and Performance Technology facility in Ossining , New York as a Senior Scientist. Dr. Johnson is a member of the Royal Society of Chemistry, American Chemical Society, Materials Research Society, and International Zeolite Association.

Directions to Vassar College : Vassar College is located at 124 Raymond Avenue in Poughkeepsie , NY . Refer to the following link for driving directions and campus map: www.vassar.edu/directions/. Enter the main entrance of the campus on Raymond Avenue .

Invensys divests interest in FoxboroNMR Ltd

November 4th, 2005

In June 2005 Invensys divested its majority stockholder position in FoxboroNMR Ltd the manufacturer of the NMR spectrometer upon which the Invensys MRA product is based. This means that FoxboroNMR will be marketing a process NMR solution through various market channels rather than having NMR systems sales occur exclusively through Invensys. Here is the press release concerning this item.

Polyolefins – Process TD-NMR

November 4th, 2005

Progression Inc (formerly Auburn and then Oxford Instruments) have been placing low field time-domain (TD) NMR spectrometers in the field for 15+ years. The main arena for their on-line analysis is polyolefins though they are now trying to extend their application base into coal and mining. They have 120+ systems in the field which is a lot considering that most NMR spectroscopists aren’t even aware of their existence. They have recently publised two application notes on TD-NMR applied to polypropylene resins and polyethylene resins. The bottom line is that most TD-NMR spectrometers can perform the analysis, however, the sample grabbing, pre-conditioning and delivery to the NMR are key.

It would be interesting to take detailed liquid-state 1H and 13C analyses, with complimentary solid-state 13C CP- and SP-MAS relaxation data in order to map the correlation between TD-NMR FID and CPMG profiles and the detailed chemistry of the samples.

NMR Console Purchase

November 4th, 2005

Today I bought a Varian Unity-400 console with three channels, solids amps, gradients, magnet leg assembly, HAL box and monitor panel for $2200. In the mid 90’s that spectrometer would have cost $300,000 +. NMR equipment seems to depreciate quicker than a Pontiac. My pack rat mentality is in full swing.

We operate a Varian VXR300S for liquids analysis and a Varian UnityPlus-200 for solids and liquids analysis. Sitting in the adjacent space of our of our office I have 2 full VXR-300 consoles as board swap for my liquids system, a VXR-400, a Varian 300 MHz R2D2 magnet, two 60 MHz process NMR spectrometers, and two boxes full of acquisition control board, ADC boards, sum-to-memory boards, etc.

I question why any small company would buy a new spectrometer when you must pay through the nose and watch it depreciate at a terrific rate. Then you have to deal with the fact that you are held hostage by the spectrometer manufacturer as failed components are only available through them initially at high exchange rates, and they will not ship you a board unless you have taken their maintenance course.

If you buy 10 year old spectrometers, either third party, or from ebay and other auctions, you can support yourself for pennies on the dollar. People actually laugh when I say I support the spectrometer service aspects of my business by surfing ebay and the internet.

One great third party supplier is Triangle Analytical who install and service spectrometers and take the worry of Cryogen refills away with their Helium (and Nitrogen if you want it) fill contracts. The perception of NMR as an expensive instrument to buy or mainatain is simply not true any more.

If anyone has old NMR spectrometers, probes, magnets, or amplifiers laying around let me know…I can probably find a home for them.