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NMR Analysis of Essential Oils – Example of Sri Lankan Citronella

by Chemistry, NMR, Process NMR

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

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

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

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

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

Process NMR for Transesterification Monitoring and Certification of Biodiesel

by Chemistry, Energy, NMR, Process NMR

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

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

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

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

Biodiesel Production Monitoring

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

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

Expansion of Incomplete Reaction Series

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

These calibrations, based on either 1H or 13C NMR, when validated would allow rapid testing of biodiesel production batches and would make complete analysis of small production batches economically feasible (there is no point making 300 gallons of biodiesel if you have to perform $1300 of testing on the batch).

Process NMR Technology Session Planned for Eastern Analytical Conference 2007

by NMR, Process NMR

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

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

Hello to all,

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

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

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

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

Best Regards,

John

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

Process NMR Spectroscopy Seminar Series to be Held at 2007 Eastern Analytical Symposium

by Chemistry, NMR, Process NMR

John Edwards of Process NMR Associates has agreed to chair a session at the Eastern Analytical Symposium in Somerset, New Jersey in November, 2007. The session is entitled “Process NMR Spectroscopy”. If you are interested in presenting a technical paper at this session please contact John directly at john@process-nmr.com

Also listed here is the 2007 Call for Papers for the upcoming meeting.

New Site Dedicated to Magnetic Resonance in the Food Sciences

by Chemistry, NMR, Process NMR

A new website has been introduced that focusses on the applications of Magnetic Resonance (NMR, MRI, Relaxometry) to the chemistry and physics of foods. The website can be found at magres.foodsciences.org

This organization also arranges the biannual conference on Application of Magnetic Resonance in Food Science – they have an excellent poster session with PDF versions of the poster presentations published to the web – Poster PDFs