Routine analysis by high precision gas chromatography/mass selective detector/isotope ratio mass spectrometry to 0.1 parts per mil

Stable isotope methods are potentially quite useful for validating natural or enhanced mineral degradation of contaminants. For this reason, a continuous flow gas chromatograph (GC), isotope ratio mass spectrometer (IRMS) has been coupled with a quadrupole mass selective detector (MSD) to allow simultaneous mass spectral and stable carbon isotope ratio data to be obtained from a single chromatographic analysis. This allows the target contaminant and any extra-cellular degradation intermediates to be both qualified and quantified. Previously acceptable limits of precision (0.3 parts per mil) are undesirable given the small fractionation observed during aerobic degradation. To further understand the fate of organic contaminants and to gain information about the metabolic degradative pathway employed by a microorganism, routine isotopic analyses on a range of analytes have been performed. Quantities of sample producing mass-44 ion beam signal (I(44)) of 2 x 10(-10) to 1 x 10(-8) A were analysed. When the IRMS was tuned for high sensitivity, ion source nonlinearities were overcome by peak height correction from an algorithm that was produced using known isotopic standards of varying concentrations. This led to sample accuracy of <0.01 per thousand and sample precision of 0.1 per thousand. Copyright 1999 John Wiley & Sons, Ltd.     

Frequency scan for the analysis of high mass ions generated by matrix-assisted laser desorption/ionization in a paul trap

An ion trap has been modified for the analysis of high mass ions generated by matrix-assisted laser desorption/ionization. Samples are deposited on a probe tip and introduced directly onto the hyperbolically shaped surface of one endcap. All three electrodes - both the endcaps and the ring electrode - are insulated so that the radio frequency (Rf) voltage may be applied to the center ring electrode and the inverted Rf voltage to the endcaps. By using low frequencies (below 100 kHz) and low amplitudes (below 200 V), high mass singly charged ions may be trapped and analyzed by a frequency sweep at constant amplitude. In the high mass range (60-160 kDa), this instrument showed good sensitivity, signal-to-noise ratios, and mass resolution. Copyright 1999 John Wiley & Sons, Ltd.     

79Br NMR spectroscopy as a practical tool for kinetic analysis

⁷⁹Br NMR spectroscopy has been used to monitor a series of reactions in which the bromide ion is produced, including the Menschutkin reaction of pyridine with a range of substituted benzyl bromides and a Heck coupling process. In cases where the process could also be monitored using ¹H NMR spectroscopy, the kinetic analyses using heteronuclear magnetic resonance spectroscopy were shown to be completely consistent. Both the utility of the process in following reactions which may be difficult to analyse using other techniques and the practical limitations associated with solvent choice are discussed. Copyright © 2009 John Wiley & Sons, Ltd.     

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