Whole Leaf Marker and Maltodextrin in Aloe Vera Raw Materials – Dry Weight Quantity – Extended 1H NMR Analysis Method

Process NMR Associates has developed an extension of its 1H NMR analysis of Aloe Vera raw materials and products analysis. Powder aloe vera raw materials (100x/200x) can be analyzed directly and juice samples (1x, 5x, 10x, commercial products) must be freeze dried for this analysis. The whole leaf markers utilized in this test to indicate the presence of whole leaf material are iso-citrate and iso-citrate lactone which are formed in the green leaf part of the aloe plant as part of the citric acid cycle. It is possible to assign and quantify the following components of an aloe vera juice or powder: * aloe vera components: acemannan, glucose, malic acid * whole leaf markers: isocitrate, iso-citrate lactone, citric acid * degradation products: lactic acid, acetic acid, fumaric acid, pyruvic acid, formic acid, succinic acid, and ethanol * adulterants: maltodextrin * preservatives: sorbate, benzoate * additives: sucrose, fructose, glycine, flavorants (contain ethanol and propylene glycol) For the components above it is possible to obtain a wt% of that component in a juice sample - the freeze drying process is then used to determine the wt% solids in the juice and the dry weight concentrations of the organic components in the solids.…

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Talks to be Presented at IFPAC 2012 – Baltimore, MD January 22-25

Talk 1 by John Edwards Mutivariate Analysis of 1H and 13C NMR Data of Residual Catalytic Cracker Feed-Streams: NMR Pre-Processing Strategies that Allow the Development of Predictive Models of Physical and Chemical Properties that are Independent of NMR Instrument Magnetic Field Strength John C. Edwards*# and Jincheol Kim† *Process NMR Associates, LLC, 87A Sand Pit Rd, Danbury, CT 06810 USA † SK Innovation Co., Ltd, SK Innovation Technology Center, 140-1, Wonchon-dong, Yuseong-gu, Daejeon 305-712, Korea # Speaker Historically refinery control engineers are familiar with GC derived chemical properties such as aromatics, benzene, PONA, olefins in wt% or vol%, as well as physical properties such as distillation, viscosity, conradson carbon, sulfur, density, etc. We have developed generally applicable multivariate regression methods that allow many of these familiar chemical and physical properties to be derived from quantitative 1H or 13C NMR data. We have also developed magnetic field independent data manipulation methods that allow 1H or 13C NMR derived parameters to be utilized as the X matrix “spectral” data rather than the spectra themselves. This allows field independent models to be developed as these parameters are calculated from the spectrum and are the same regardless of the magnetic field strength at which…

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New Conference Being Planned for Practical Applications of NMR in Industry

CASSS announces the first Practical Applications of NMR Conference 2012. Save the Date: October 15-17, 2012. The conference will be held at the Hyatt Regency Schaumberg, Schaumberg, IL USA. John Edwards has volunteered to serve on the organizing committee and will be developing a session of talks on on-line/at-line NMR and TD-NMR technologies. Other exciting sessions will revolve around other practical NMR applications in industry - more details will be posted when the program has been developed further.

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1H NMR – 60 MHz Permanent Magnet System – Reaction Monitoring

Below are a few further examples of acetylation reactions of acetic anhydride with an excess of alcohol. The alcohols include tert-butanol and isopropanol. Reaction 1: Acetylation of t-butyl alcohol with acetic anhydride in the presence of acid. Reaction 2: Acetylation of Isopropanol with acetic anhydride in the presence of acid. Reaction 3: Methoxyacetone and hydroxylamine reaction in methanol to form an Oxime Resolution of the methylenes in the methoxyacetone and the reaction product is readily observed. All the above experiments were performed in an NMR tube. We are currently looking at the same reactions under flow conditions utilizing a HPLC pump and PEEK tubing to transport sample to the NMR probe at 5 ml/min.

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Selective Observation of High Resolution 19F Spectrum by 1.4 Tesla Process NMR System

Below is an example of a 19F NMR Spectrum obtained at 54.6 MHz on a 1.4 Tesla permanent magnet-based NMR System. This is a 2 minute spectrum obtained by co-averaging 16 FIDs after zero-fill, autophase, referencing of each individual FID. The NMR system is not locked. No apodization of the NMR FID data was performed. For more details on potential applications of 19F NMR please contact John Edwards (Tel: +1 203-744-5905)

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Chevron Installs Low Field NMR Application: 31P NMR Analysis of Phosphoric Acid Strength in Alkylation Process

New Flash: Chevron purchases high resolution 31P NMR system for at-line analysis of a phosphoric acid catalyzed alkylation process. The Chevron Richmond Refinery needed a simple and quick measurement of phosphoric acid strength and quality. Prior analysis procedures included transporting samples several miles from the refinery process to the technical center in order to perform the 31P NMR analysis on a high field superconducting NMR system. This process was also complicated by the fact that the process operators were not able to perform the analyses on the conventional high field NMR systems (400 MHz for 1H, 161 MHz for 31P) themselves, but had to wait for NMR technician and instrument availability. If sample analyses was required after research facility working hours the NMR lab technicians were required to come in and run the NMR for the process operators. A simple permanent magnet bench-top NMR system has now been placed in the existing process lab adjacent to the process unit control room. The NMR samples are placed in specially designed 9 mm (diameter) x 50 mm (length) sample tubes in order to accommodate sample handling issues (high viscosity sample with no solvents being added) and are place easily into the NMR…

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