Purity Analysis of Synthetic Organic Compounds
EMSL Project ID
26591
Abstract
NMR spectrometer time is requested for Dr. Garry W. Buchko (EMSL) to analyze occasional organic samples for Drs. Scott Harvey and Bob Wright. These latter NSD staff (PNNL) are both analytical chemists that specialize in chromatography. NMR studies will help solve various research problems encountered with synthesis and separation tasks on a variety of DOE projects that serve our nation. One of the primary objectives of these studies will be to verify the structure of synthetic intermediates and to verify the purity of the final products. In addition, the purity of commercially available products will be verified. All the organic compounds will have prior PNNL-IOPS approval and established IOPS protocols will be used for preparing samples within EMSL, in PNNL facilities, or at off-site locations. The NMR experiments to be performed are high-resolution one-dimensional proton and two-dimensional TOCSY experiments. Because the samples will usually be very concentrated, between 1-10 mM, the amount of EMSL-NMR instrument time required will be small, on the order of 1-3 hours per sample (including setup). Indeed, these experiments are an ideal opportunity to push the use of EMSL NMR spectrometers to the maximum and collect data in the short periods of "idle-time" that often exist for various reasons (e.g.: after a long 3D experiment and between a "fill", while waiting for/preparing a sample, when samples turn "bad" early). Time may not even officially need to be scheduled as the majority may be "squeezed in" by discussions with EMSL staff and outside users whenever an organic sample is ready to be analyzed.
Project Details
Project type
Exploratory Research
Start Date
2007-06-29
End Date
2008-06-29
Status
Closed
Released Data Link
Team
Principal Investigator
Related Publications
Scott D. Harvey, Garry W. Buchko, Richard B. Lucke, Cherylyn W. Wright, Angela M. Melville, Anthony J. Scott, and Bob W. Wright, The structure and purity of a reference dye standard used for quantification of C.I. Solvent Red 164 in fuels, Dyes and Pigments, 82:307-315 (2009).