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61.
A review of sample preparation methods for organic acids in biological fluids, in particular serum and urine, is presented. It covers techniques on organic acid determination without sample preparation, release of organic acids from binding locations, removal of proteins by protein precipitation and ultrafiltration, isolation of the organic acids by liquid-liquid and liquid-solid extraction, purification of the extract, derivatization and pre-fractionation. The various alternative sample preparation steps are compared and critically discussed. Examples of applications including profile analysis of organic acids by gas chromatography (GC), determination of particular organic acids by GC or liquid chromatography and determination of fatty acids as a distinct chemical class of acids demonstrate that the kind of sample preparation chosen depends strongly on the analytical aims. 相似文献
62.
有机溶剂对镧和钇ICP光谱信号的增敏机理研究 总被引:2,自引:0,他引:2
本文考察了有机溶剂(乙酸丁酯)及有机试剂(PMBP)引入ICP-AES对稀土元素镧和钇光谱信号的影响。实验结果表明,有机溶剂的引入明显增大了待测物的传质效率,从而导致分析灵敏度的改善。与水相相比,有机相的引入对ICP激发温度未产生明显影响,但使线对强度比(LogI^ /I)增强,有利于待测物的电离。 相似文献
63.
Nitrogen-15 labeled pyrroles have been prepared from commercially available 15N glycine or sodium nitrite using the Barton-Zard, Knorr, and Kleinspehn approaches. These pyrroles were used as intermediates in the synthesis of per-15N labeled porphyrins needed for the analysis and assignment of vibrational spectra for sedimentary porphyrins. Etioporphyrin-I was prepared via pyrromethene intermediates, while etioporphyrins II-V and a related tetrahydrobenzoporphyrin were synthesized via stepwise routes involving the copper(II) mediated cyclization of a,c-biladienes as the key step. Detailed analyses of both the proton and carbon-13 NMR spectra provide nitrogen-15 coupling constants for these important structures. 相似文献
64.
65.
Eu5Ge3 and EuIrGe2 were prepared from the elements in tantalum tubes, and their crystal structures were determined from single crystal X-ray data. Eu5Ge3 adopts the structure of Cr5B3: I4/mcm, a = 799.0(1)pm, c = 1 536.7(1)pm, Z = 4, wR2 = 0.0421 for 669 F2 values and 16 variables. The structure of Eu5Ge3 contains isolated germanium atoms and germanium atom pairs with a Ge? Ge distance of 256.0 pm. Eu5Ge3 may be described as a Zintl phase with the formulation [5 Eu2+]10+[Ge]4?[Ge2]6?. Magnetic investigations of Eu5Ge3 show Curie-Weiss behaviour above 50 K with a magnetic moment of μexp = 7.6(1) μB which is close to the free ion value of μeff = 7.94 μB for Eu2+. EuIrGe2 is isotypic with CeNiSi2: Cmcm, a = 445.5(2) pm, b = 1 737.4(4) pm, c = 426.6(1) pm, Z = 4, wR2 = 0.0507 for 295 F2 values and 18 variables. The structure of EuIrGe2 is an intergrowth of ThCr2Si2-like slabs with composition EuIr2Ge2 and AlB2-like slabs with composition EuGe2 in an AB stacking sequence. Both slabs are distorted when compared to the symmetry of the prototypes. The Ge? Ge distance of 256.6 pm in the AlB2-like fragment is comparable to that in Eu5Ge3. 相似文献
66.
Alejandro Marcó Ramón Compañó Roser Rubio Pilar Domènech Albert Palangues Miguel Maestro 《Mikrochimica acta》2002,140(1-2):131-139
Four inter-comparison exercises on organic elemental analysis were carried out between 1997 and 2001 by the Department of
Analytical Chemistry of the University of Barcelona, together with the Microanalysis Service and the Institute of the Marine
Sciences, which both belong to the CSIC in Barcelona, and the University of A Coru?a. More than sixty laboratories participated
in these exercises. Here we describe the design and characteristics of the trials, the samples and the homogeneity tests applied.
We report the results obtained for the analysis of carbon, hydrogen, nitrogen, sulphur and oxygen, their statistical analysis,
and the most relevant aspects of the technical discussion meetings.
Received December 20, 2001; accepted March 18, 2002; published online July 22, 2002 相似文献
67.
The change in semiconductive properties of β-apo-8′-carotenal, astacene and methyl bixin on adsorption of various vapours
on the crystallite surfaces has been studied at a constant sample temperature. The adsorption of vapours enhances the semiconductivity
of the polyenes appreciably. This enhancement depends on the chemical nature and also on the pressure of the adsorbed vapour.
The adsorption and desorption kinetics follow the modified Roginsky-Zeldovich relation. A two stage desorption process, the
first stage of which gives a Lennard-Jones potential energy curve and is followed by a rate-determining transition over a
potential energy barrier to the second stage of adsorption forming weakly bound complexes between the vapour molecules and
the polyene crystallites, can explain satisfactorily the experimentally observed kinetic data. 相似文献
68.
氟阴离子在有机合成中的应用:Ⅱ.无水氟化钾催化乙酐与苯甲醛的Perkin反应 总被引:4,自引:0,他引:4
用无水醋酸盐催化苯甲醛与乙酐的Perkin反应,一般反应时间较长,产率最高为55—60%.用三乙胺、吡啶和无水碳酸钾等作催化剂,产率也无明显提高.近年来氟阴离子在有机合成中的应用迅速发展,我们曾用无水氟化钾催化成功地实施了丙二酸二乙酯与苯甲醛的Knoevenagel缩合,并研讨了该反应的微环境效应.本工作首次用无水氟 相似文献
69.
Stephen de Mora Jean-Pierre Villeneuve Eric Wyse 《Accreditation and quality assurance》2007,12(11):587-592
Aspects of the International Atomic Energy Agency (IAEA) Analytical Quality Control Services (AQCS) for marine environmental
studies are discussed, focusing on recent laboratory performance studies (LPS) and the production of reference materials for
trace metals and organic compounds in various marine matrices. The IAEA has organized seventeen global interlaboratory studies
for a range of organic contaminants. Of note has been the inclusion of numerous polychlorinated biphenyl congeners (PCBs)
and some sterols of anthropogenic origin. Concurrently, there have been eleven worldwide intercomparison exercises for trace
metals in the marine environment, most of which included methylmercury. Although such interlaboratory studies can help improve
performance in individual laboratories and regional laboratory networks, the results reveal that problems remain in the determination
of some metals and many organic contaminants. 相似文献
70.