Presented at Marist College, Poughkeepsie
September 23, 2009

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

By John C. Edwards, Ph.D.
Process NMR Associates, LLC, Danbury CT

The availability of cheap commodity electronics developed for the cellular phone industry is revolutionizing the design of NMR and ESR spectrometers. Rather than instruments that fill half a room, cost $200-3,000K+, and intimidate users, it is possible to produce spectrometers that are an order of magnitude cheaper to produce. Examples of NMR and ESR spectrometer development projects will be described as well as the wide-ranging applications that these spectrometers can deliver to the areas or process control, food authentification and automated laboratory analysis.

John Edwards was born and raised in Bolton, UK. He graduated from the University of Durham, UK with a B.Sc. in Chemistry in 1986. He obtained his Ph.D. in Physical Chemistry from the University of South Carolina in 1990, working on solid-state NMR applied to heterogeneous catalysts under the guidance of Professor Paul Ellis. From 1990-1997 he worked as a research chemist at the Texaco R&D facilityin Beacon, NY where he was responsible for global NMR support of upstream, downstream, and petrochemical Texaco ventures. In 1997 he formed Process NMR Associates which operates as a commercial analytical NMR spectroscopy service and consultancy. Process NMR Associates along with its engineering company partners, develops, markets, and supports on-line process NMR spectrometers utilized for control and optimization of refinery, petrochemical, pharmaceutical and food manufacturing operations. The company also acts as an application development company for several analytical instrument companies and supports the chemometric development of several process analytical products. He currently resides in Poughkeepsie, NY, with his wife and 3 sons. He is an affiliate professor of Chemistry at Marist College, a Research Associate at SUNY New Paltz, and an active member of the American Chemical Society.

A copy of the presentation can be provided on request… contact John Edwards if interested.

Topnir Systems is proud to announce the signature in October 2009 of a Partnership Agreement with Process NMR Associates, LLC.

This partnership enables Process NMR to utilize our field proven software in complementary fields NMR and MIR combining forces to deliver total solutions with increased added value to customers.

Topnir Systems is a French company leader in the field of online Near InfraRed (NIR) analyzers. Topnir enables measuring and monitoring multiple hydrocarbon streams in less than one minute using a single online system. The company has a long history in the refining and petrochemicals business, being the first world wide to implement an online application designed to measure and control octane number for gasoline production, first NIR on-line application worldwide on Ethylene Plant Naphtha feed (1986), Gasoline (1989) and Crude (1991). The business started in the late 80s within BP Oil, with applications development around gasoline and diesel blending, as well as FCC, CDU, Reformer and Ethylene plant feed andproducts characterization. Major oil companies such as Shell, BP, Repsol, Aramco… have adopted Topnir solutions.

Topnir has recently expanded its activities to provide platform independent software for NIR systems already installed in the field. Topnirs modeling technology offers a full set of properties from a single model which offers the advantage of a robust, reliable system requiring very light maintenance. In addition Topnir is field proven to have ASTM and better results.

Process NMR Associates, LLC is an American company and leader in the field of online Nuclear Magnetic Resonance (NMR) process applications. The company also has a long history in the refining and petrochemicals business, being the first world wide to implement online NMR applications for gasoline and diesel blending, FCC, CDU, Reformer and Ethylene plant feed and products characterization.

Topnir Systems
425, rue RenéDescartes
Espace Descartes, Bat C
Parc de la Duranne
13857 Aix-en-Provence, France
Tel +3350 73 47 / Fax+3350 73 50
Web: www.topnir..com
USA Contact: Julie Williams Tel: +1-508-736-2696

Process NMR Associates, LLC
87A Sand Pit Road
Danbury, Connecticut 06810 USA
Tel +203-744-5905
Fax +203-743-9297
Web: www.process-nmr.com
Contact: Dr. Paul Giammatteo

Paul Giammatteo recently presented two papers at the Gulf Coast conference that was held in Galveston, Texas on January 20-21.

His first paper was entitled “Counting Carbons for Tighter Control: Combining GC and NMR to Improve Distillate Manufacturing” and centers on the topics of Simulated distillation correlated to 1H NMR.

The second paper was entitled “Analytical Data For Engineering Support: Improving the Lab/Process Interface”. This paper details the development of a series of heavy petroleum applications on a Smiths Detection FTIR-ATR spectrometer.

PDFs of the presentations can be obtained from the following links: 1) NMR Talk 2) FTIR-ATR Talk

Over the past few years balsamic vinegars have been the subject of a number or NMR studies to determine authenticity, degree of aduleration, and age. 1H NMR has been used to quantify the relative concentrations of a series of organic components (ethanol, fructose, glucose, acetic acid, succinic acid, lactic acid, butandiol, etc (ref 1). 13C NMR has been used to determine the aunthenticity and degree of adulteration (ref 2) as well as the length of the ageing process that a given sample has undergone. Also the formation of glucose and fructose acetates during maturation and ageing has been studied by 1H and 13C NMR.

Refs.
1) Caligiani et al., Anal. Chim. Acta, 585 (2007) 110-119
2) Consonni et al., Talanta, 75 (2008) 765-769
3) Consonni et al., Anal. Chim. Acta, 611 (2008) 31-40
4) Consonni and Caligiani, Talanta, 73 (2007) 332-339
5) Cirlini et al, Food Chemistry, 112 (2009) 51-56

The concentration and distribution of the organic components has been found to correlate well with ageing process analysis, identification of adulteration, and determination of authenticity of traditional balsamic vinegars and balsamic vinegars of Modena.
Below are a series of spectra showing what can chemistry can be quantified in the balsamic vinegars as well as a few comparative spectra of apple cider vinegar and malt vinegar.

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