NMR Testing Laboratory

Industrial NMR Spectroscopy Applications

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MestreLab MNova Users Meeting – SMASH 2013 – PNA NMR Presentation

by Chemistry, Chemometrics, Herbal Supplement, NMR, Process NMR, qNMR, Reaction Monitoring

“Utilization of MNova in a Commercial NMR Testing Laboratory for: 1) Development of Automated Quantitative Analysis Methods by Direct Internal Standard NMR Measurements, and 2) Pre-Processing of Large NMR Datasets for Chemometric Regression Analyses to Derive Chemical and Physical Properties” – presented by John Edwards at the MNova Users Meeting – SMASH 2013 – Santiago de Compostela, Spain, September 22, 2013
PDF of Presentation

Automated 1H qNMR analysis of complex mixtures – example of aloe vera powder 200x

Final automated analysis output for aloe vera analysis – assignments and quantitative output.

Chemometric analysis – spectrum processing and X-matrix preparation performed in MNova – ascii output imported into Eigenvector Research Solo for PLS regression or PCA analysis. Correlation of 1H NMR at 300 or 60 MHz with GC analysis of EPA and DHA content (wt%).

 

Cryogen-Free NMR – High Resolution Permanent Magnet Systems – The Market Hots Up

by Chemistry, NMR, Process NMR

It is interesting times in the world of NMR – there are a number of new permanent magnet NMR systems hitting the market. I have seen a number of announcements appearing on LinkedIn and other sites in recent days and then there was a question asked about Cryogen-free NMR systems on the AMMRL server. There is a little confusion out there about who is doing what and what these newer NMR systems are capable of. We (Process NMR Associates and Aspect Italia) have been in the market with a high resolution 60 MHz system (3, 5, or 10mm sample tube) since 1997. Anasazi Instruments have been quitely selling hundreds of 60 and 90 MHz FT-NMR systems based on refurbished or newly manufactured Varian EM-360 and EM-390. New to the scene and making a splash with their marketing campaigns are Picospin (300 micron sample tube, 45 Mhz), Nanalysis (3, 5mm sample tube, 60 MHz). Finally, there is a system from Magritek/ACT (5mm sample tube, 42.5 MHz) that has been re-packaged and is now out there in the world. These systems all produce spectra and can be used in the traditional manner that current supercon systems are utilized. Time-Domain (TD) NMR systems should not be confused with these platforms – TD-NMR spectrometer manufacturers include Cosa-Xentaur, Bruker, Oxford Instruments, SpinLock, MR-Resources – which are used typically for hydrogen content, rheology, simple phase measurements (solid fat, water in oil, oil in water, porosity measurements utilizing relaxation analysis.

For the past 17 years we have been actively developing applications for permanent magnet systems shimmed to approximately 3 Hz at peak half height. The new magnet designs are robust and readily shims to 1-2 Hz at half height using 5 or 3 mm NMR tubes. 3 Hz at half height is possible for 10 mm NMR tubes. In the past the focus was in on-line applications in refining and petrochemical and lab systems were not actively marketed. With the third generation of NMR instrument it is time for these robust, non-cryogen, permanent magnet systems to be applied in laboratory and general quality testing applications.

In our laboratory we have an application development advantage in that we have high field 300 MHz NMR systems that are active in commercial NMR analysis and in high field method development. We also have ESR, FTIR-ATR, GC, moisture measurements, and other instruments that we can bring to bear on applications. We can readily develop 60 MHz applications using the 300 MHz NMR data as the basis set to provide primary parameters for analysis or to answer questions about the spectral overlaps that inevitably occur in 60 MHz data sets where 1 ppm on the spectrum axis represents only 60 Hz rather than 300 Hz. When a high field NMR spectroscopist observes a data comparison of spectra obtained at 60 MHz to the same spectrum obtained at 300 MHz (a resolution that most are familiar with) the penny suddenly drops concerning the possibilities that exist for NMR analysis at this field and an appreciation for the work that was performed for the first 30 years of NMR technology on 40 and 60 MHz CW NMR’s. We have become accustomed to our big supercon magnets and have forgotten what can be accomplished at 60 MHz. In these days of powerful computers for multivariate analysis and the ability ot perform global spectral deconvolution (GSD) the ability to develop killer-apps for bench-top, at-line, or in-line applications of 1H/31P/19F/23Na/11B NMR for 110V powered systems is here. The application of chemometrics and GSD at 60 MHz can allow the lower resolution issue of peak overlap to be overcome.

Comparing spectra obtained on our 300 MHz systems to the same samples on the 60 Mhz systems. Direct comparisons of the data make you realize that though the resolution isn’t anywhere near the same – the information is present in the 60 MHz spectrum. In the links below I have included a number of PDFs showing comparisons of complex essential oil spectra, fish oil and vegetable oils (looking at omega-3 fatty acid content), polyurethane adhesive polymers, shale oil, gasoline and a spectrum of Poloxamer which is a oxyethylene-oxypropylene copolymer utilized in the pharmaceutical industry that has an NMR based USP/NF method associated with it to determine the oxyethylene content.

Polyurethane Polymers – 60 MHz vs 300 MHz – PDF

Essential Oils – 60 MHz vs 300 MHz – PDF

Fish Oils and Seed Oils – Omega-3 Content – 60 MHz vs 300 MHz – PDF

Poloxamer Analysis – Shale Oil and Gasoline Analysis – 60 MHz vs 300 MHz – PD

Process NMR is actively involved in development of NMR applications utilizing 60 MHz or 300 MHz NMR data. We can develop applications for you and also provide the robust, proven instrumentation that can make affordable, cryogen-free NMR analysis a common automated laboratory tool. We are also looking to prove the utility of this excellent technology in all industrial sectors – if you have an application and would like to see a feasibility study we would be happy to provide such an opportunity. We have NMR systems looking for things to do! Please contact us if you feel you have an application where NMR may provide an answer through direct measurement or chemometric calibration. We are also interested in developing multi-spectroscopy technique data fusion applications where NMR and IR are combined to provide “better answers”.

Anita Brandolini – NMR Spectroscopist and Professor – RIP

by Chemistry, NMR

We saddened to hear today that our good friend and NMR compatriot Anita Brandolini passed away a few weeks ago. We were informed by Mike Frey of JEOL that the North Jersey Section of ACS will be setting up a memorial as part of Project SEED. If you knew Anita or share her passion for teaching science to the young then please consider donating to this cause.

Anita J.Brandolini, 56, Assistant Professor of Chemistry at Ramapo College of New Jersey, died suddenly at her home in Hillsboro, NJ on March 10, 2012.
Originally from Morton, PA, Brandolini earned her B.S. in Chemistry in 1979 at Drexel University and her M.A. and PhD in Physical Chemistry in 1981 and 1983 at the University of Delaware. She was also a course Instructor for JEOL, USA, Inc.

Brandolini worked for 17 years at Mobil Chemical where she was a Team Leader and Senior Research Chemist in polymer analytical chemistry. She was an expert in the nuclear magnetic resonance of polymer systems publishing a book, NMR Spectra of Polymers and Polymer Additives (Anita J. Brandolini and Deborah D. Hills, New York; Marcel Decker, 2000) and contributing chapters on spectroscopy to numerous publications.

In 2000 Brandolini began a full time academic career accepting a two-year appointment at the College of New Jersey and then teaching at William Paterson University and Fairleigh Dickinson University before joining the Ramapo University faculty in 2007. She was an enthusiastic educator dedicated to undergraduate teaching and research and incorporating her industrial experience into her teaching, design of experiments, and writing. She believed strongly in undergraduate research and mentored many students. Her work primarily involved studies of the adsorption of polymers to surfaces and, more recently, the binding of dyes to nucleic acids.

Brandolini disseminated her love of chemistry broadly. She published a book for children Fizz, Bubble, and Flash: Element Explorations and Atom Adventures (Anita J.Brandolini, Charlotte, VT. Williamson Books, 2003) for which she was awarded the Parents’ Choice Foundation Silver Honor in 2003. She developed a website Keys to Chemistry, an interactive forum for students to practice chemistry, and she hosted a blog Dr. B’s Science Lab where she posted monthly themed experiments involving science for the whole family. She also gave many lectures at schools and at the New Jersey Liberty Science Center.

Brandolini was an active member of the ACS and its North Jersey Section. She was an ACS Councilor and served as Secretary and Chair of the Section. Nationally she was a member of the Committee on Project SEED and the Committee on Public Relations and Communications. In 2011 she was named a Fellow of the American Chemical Society.

The NJACS is establishing an Annual Project SEED Award to be given to an outstanding high school student at the SEED Poster Session held in September each year.

Donations to the Anita J. Brandolini SEED Fund should be sent to the following address:
Val Kuck
NJACS Project SEED Treasurer
45 Warfield St
Upper Montclair, NJ 07043

Please make checks payable to NJ Project SEED and in memo include The Anita J. Brandolini Fund.

ASTM F2259-03 (2008) – Determining the Chemical Composition of Alginates by 1H NMR Spectroscopy

by Chemistry, Herbal Supplement, NMR

Alginate is a linear polysaccharide composed of mannuronate (M) and a-L-guluronate (G). The polysaccharide is characterized by the relative ratio of M/G, G-Content, and average length of blocks of G in the polymer. M and G are:

ASTM F2259 recounts the standard sample preparation and 1H NMR analysis that allows the following parameters to be calculated:

The 1H Spectra obtained on a typical alginate sample are show below:


Finally the peaks representing the individual M and G components and sequences are deconvoluted from the spectrum.
The intensities obtained from the deconvolution are input into the excel spreadsheet shown above and the various ratios, M and G content and a series of diads and triads are calculated along with some G block lkength information. It is the block length information that often reveals telling differences between samples.

Process NMR Associates performs this analysis at a cost of $225 per sample. The samples, however, must be prepared by the customer using the methodology set forth in the test method.