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41.
R.L. Ammlung D.F. Shriver M. Kamimoto D.H. Whitmore 《Journal of solid state chemistry》1977,21(3):185-193
The new compound Tl2ZnI4 has been prepared and characterized by Raman spectroscopy, powder X-ray diffraction, elemental analyses, and a partial binary phase diagram. The compounds In4CdI6, Tl4CdI6, and In2ZnI4, for which phase diagrams are available in the literature, were characterized by Raman spectroscopy and their identities were confirmed by elemental analyses and X-ray powder diffraction. Each of these materials, except Tl4CdI6, undergoes a sharp order-disorder phase transition at elevated temperatures that can be detected by the measurement of Raman spectra as a function of temperature. Conductivity measurements as a function of temperature, using both reversible and blocking electrodes, reveal a high ionic conductivity in the disordered, high-temperature phase. This work suggests that indium(I) and thallium(I) ionic conductors may exist, analogous to some well-known double salt conductors based on simple silver(I) and copper(I) halides. In addition, the present study demonstrates the usefulness of Raman spectroscopy in the characterization of heavy-metal ionic conductors. 相似文献
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The specific formation of LFe(CO)4 (L = PPh3, P(OPh)3, P(OMe)3 can be achieved by the reaction of Fe(CO)5 with L in the presence of a catalytic amount of iron carbonyl anion. A convenient synthetic procedure was developed in which the iron carbonyl anion catalyst is generated in situ. It is shown that the mechanism does not proceed by the simple cleavage of the Fe2(CO)82? or Fe3(CO)112? anions, because triphenylphosphine reacts with these anions in the absence of Fe(CO)5 to produce (PPh3)2Fe(CO)3. 相似文献
43.
Schoeller DA Colligan AS Shriver T Avak H Bartok-Olson C 《Journal of mass spectrometry : JMS》2000,35(9):1128-1132
The doubly labeled water method is commonly used to measure total energy expenditure in free-living subjects. The method, however, requires accurate and precise deuterium abundance determinations, which can be laborious. The aim of this study was to evaluate a fully automated, high-throughput, chromium reduction technique for the measurement of deuterium abundances in physiological fluids. The chromium technique was compared with an off-line zinc bomb reduction technique and also subjected to test-retest analysis. Analysis of international water standards demonstrated that the chromium technique was accurate and had a within-day precision of <1 per thousand. Addition of organic matter to water samples demonstrated that the technique was sensitive to interference at levels between 2 and 5 g l(-1). Physiological samples could be analyzed without this interference, plasma by 10000 Da exclusion filtration, saliva by sedimentation and urine by decolorizing with carbon black. Chromium reduction of urine specimens from doubly labeled water studies indicated no bias relative to zinc reduction with a mean difference in calculated energy expenditure of -0.2 +/- 3.9%. Blinded reanalysis of urine specimens from a second doubly labeled water study demonstrated a test-retest coefficient of variation of 4%. The chromium reduction method was found to be a rapid, accurate and precise method for the analysis of urine specimens from doubly labeled water. 相似文献
44.
D. F. Shriver 《Journal of Cluster Science》1992,3(4):459-467
Some analogies between organometallic chemistry and surface chemistry are developed. Comparison of Lewis acid promoted CO insertion and Zn2+ promotion of oxygenates in the hydroformylation of C2H4 over Rh, suggests that Zn2+ interaction with Rh-CO may promote migratory insertion which favors hydroformylation over hydrogenation of alkenes. CCO, which is observed in metal clusters should be a viable surface species. Finally, parallels can be found between the positioning of oxygen in clusters and on surfaces. 相似文献
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46.
Thorsen T Shriver T Racine N Richman BA Schoeller DA 《Rapid communications in mass spectrometry : RCM》2011,25(1):3-8
The doubly labeled water method provides an objective and accurate measure of total energy expenditure in free‐living subjects and is considered the gold‐standard method for this measurement. Its use, however, is limited by the need to employ isotope ratio mass spectrometry (IRMS) to obtain the high‐precision isotopic abundance analyses needed to optimize the dose of expensive 18O‐labeled water. Recently, cavity‐ring down spectroscopy (CRDS) instruments have become commercially available and may serve as a less expensive alternative to IRMS. We compared the precision and accuracy of CRDS with those of IRMS for the measurement of total energy expenditure from urine specimens in 14 human subjects. The relative accuracy and precision (SD) for total body water was 0.5 ± 1% and for total energy expenditure was 0.5 ± 6%. The CRDS instrument displayed a memory between successive specimens of 5% for 18O and 9% for 2H. The memory necessitated carefully ordering of specimens to reduce isotopic disparity, performance of several injections of each specimen to condition the analyzer, and use of a mathematical memory correction on subsequent injections. These limited the specimen throughput to about one urine specimen per hour. CRDS provided accuracy and precision for isotope abundance measurements of urine that were comparable with those of IRMS. The memory problems were easily recognized by our experienced laboratory staff, but future efforts should be aimed at reducing the memory of the CRDS so that it would be less likely to result in poor reproducibility in laboratories using doubly labeled water for the first time. Copyright © 2010 John Wiley & Sons, Ltd. 相似文献
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