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A non-oxidative alkaline sample digestion procedure using tetramethylammonium hydroxide and a high pressure, microwave assisted
autoclave digestion system was developed. The silicon concentrations of the digested samples were measured by inductively
coupled axial plasma optical emission spectrometry (ICP-OES). Details of the digestion conditions as well as the optimised
instrumental parameters for ICP-OES are described. The method was developed and tested using silicon-spiked ascorbic acid
and applied to samples of animal tissue and organs. The total silicon content of two different reference materials, NIST 1577b
Bovine liver and BCR 184 Bovine Muscle having neither certified nor informational values for Si was determined. The results
obtained are compared with the results of independent methods such as wavelength dispersive x-ray fluorescence spectrometry
(WDXRF) and solid sampling electrothermal atomic absorption spectrometry (ETAAS). The method described achieves a limit of
detection of 2 mg kg–1 using 100 mg of solid biological or organic material and covers a concentration range of up to 500 mg kg–1.
Received: 27 October 2000 / Revised: 31 January 2001 / Accepted: 2 February 2001 相似文献
85.
Kopel Pavel Trávníček Zdeněk Kvítek Libor Biler Martin Pavlíček Marek Šindelář Zdeněk Marek Jaromír 《Transition Metal Chemistry》2001,26(3):282-286
NiII mixed-ligand complexes of compositions [Ni(pmdien)(ttcH)] (1), [Ni(baphen)2(ttcH)] · 4H2O (2), [Ni-(dpa)(ttcH)(H2O)] (3), [Ni(cyclam)(ttcH)] · 2H2O (4), [Ni(hexaa)](ttcH) (5) and [Ni(hexab)(ttcH)] · 2H2O (6), (baphen = 4,7-diphenyl-1,10-phenanthroline, dpa = 2,2-dipyridylamine, cyclam = 1,4,8,11-tetraazacyclotetradecane, hexaa = 1,3,6,9,11,14-hexaazatricyclo[12.2.1.16,9]-octadecane, hexab = 1,8-dimethyl-1,3,6,8,10,13-hexaazacyclotetradecane) have been prepared and characterized by means of i.r., u.v.–vis. spectroscopies and magnetochemical measurements. The redox properties of the complexes were studied by cyclic voltammetry. The crystal and molecular structure of [Ni(pmdien)(ttcH)] was determined. The nickel atom is penta-coordinated by three N atoms of pmdien, and by S and N atoms of trithiocyanurate(2–) anion. 相似文献
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Gosteva Alevtina N. Plyusnin Pavel E. Semushina Yulya P. Pechenyuk Sofiya I. Filatov Evgeny Yu. Kyrtova Olga Yu. 《Journal of Thermal Analysis and Calorimetry》2018,134(1):253-260
Journal of Thermal Analysis and Calorimetry - The thermal behavior of double complex compounds (DCC) [Cr(ur)6][Co(CN)6]·4H2O (I), [Cr(ur)6][Co(C2O4)3]·3.5H2O (II),... 相似文献
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A simple convenient protocol for the synthesis of diethyl α,α-diaryl methylphosphonate derivatives 5a-f, 6b-f, 7a-f and 8a-f, diethyl α-alkenyl α-aryl methylphosphonates 9a-d and 10a-d and α-(oxoalkyl) α-aryl methylphosphonate 11a-d and 12a-d is described. Trichloroacetimidates 3a-d were treated with activated arenes, styrene, allyltrimethylsilane or silylenol ethers C-nucleophiles in the presence TMSOTf to afford the desired products in good yields and short reaction time. 相似文献
90.
Milan Jakubek Zdeněk Kejík Robert Kaplánek Hana Veselá David Sýkora Pavel Martásek 《Supramolecular chemistry》2018,30(3):218-226
Perimidine-based chelators 1 and 2 were prepared, and their structures were confirmed by 1H and 13C NMR, MS spectroscopy and elemental analysis. These compounds were studied as specific synthetic receptors for the recognition of transition metal ions. They exhibited high affinity and selectivity towards Cu(II) ions. The conditional binding constants, linear dynamic range and detection limit were determined by UV–vis spectroscopy. These parameters demonstrated high potential of the prepared synthetic receptors for the recognition and determination of Cu(II) ions. The minimum detectable concentrations of Cu(II) ions for the synthetic receptors 1 and 2 were 270 and 75 nM (R 2 = 0.9915 and 0.9964) in aqueous medium (water/DMSO; 99:1 (v/v)), respectively. 相似文献