检测实验室如何开展管理评审工作

详细论述了管理评审的基本概念、如何开展管理评审工作以及中国实验室国家认可委员会的有关政策。     

Spectral studies of bridged bisindenylmetallocenes and products of their reactions with polymethylalumoxane in toluene and dichloromethane in the visible region

Quantitative characteristics of changes in the energy of charge transfer from -bonded ligands to metal are presented for the series of structurally similar ansa-metallocene complexes of IVB Group elements. The changes are caused by the solvation effect, replacement of -bonded chlorine ligands by methyl groups and of bridging ethylene groups by dimethylsilylene moieties, introduction of the methyl substituent into position 2 and phenyl substituent into position 4 of the indenyl system, variation of the transition metal in metallocene, and formation of complexes with polymethylalumoxane (MAO) at different Al_MAO/Zr ratios. These effects are found to be additive.     

Dehydrochlorination of monodisperse poly(vinylidene chloride) latex

The objective of the work described in this paper was to produce dispersions of small spherical carbon particles, having particle diameters in the region of 0.1 μm. To this end, the dehydrochlorination of poly(vinylidene chloride) (PVDC) latex particles was attempted. The PVDC latex was prepared by a dispersion polymerization route. Both chemical and thermal dehydrochlorination routes were attempted. Chemical dehydrochlorination, using a variety of base/solvent systems, led to nonporous, spherical black particles of the required size, but which contained only 60% carbon; most of the remainder was oxygen, introduced by nucleophilic substitution reactions. Thermal dehydrochlorination, at 700°C under a nitrogen atmosphere, using a fluidized bed arrangement, on the other hand, led to black particles, having 90% carbon and which retained their sphericity, but which were highly porous. Initial chemical dehydrochlorination, prior to thermal treatment, did not seem to reduce the porosity of the final carbons. Dispersions of the carbon particles in a variety of solvents were readily achieved.     

A supported gold catalyst for the elimination of hydrogen from CO2 feed gas in the production of urea

Supported gold catalyst for eliminating hydrogen from CO₂ feed gas in the production of urea is found to be superior to other industrial catalysts (e.g. Pt/Al₂O₃ and PdPt/Al₂O₃) in catalytic activity and resistance to sulfur poisoning.     

Unprecedented intermolecular aldol-type condensation involving CH-acid and the nitro group

The first evidence that α-acylnitrone is an intermediate in the base-promoted reaction of 4-nitro-N,N-diethylaniline with aceptophenome to give an enaminoketone was obtained. Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 8, pp. 1645–1647, August, 1998.     

Magnesium-butadiene addition compounds: Isolation,structural analysis and chemical reactivity

The magnesium-butadiene 1 : 1 (1), 1 : 2 (II) and 1 : 3 addition compounds obtained by the direct metalation of butadiene with metallic magnesium were isolated. These compounds have a polymeric structure. Structural analysis of these compounds by NMR and IR methods was carried out. The process for the formation of II via I and III via II was investigated. The results of protolysis and alkylation of the above magnesium compounds corresponded well to those of crotylmagnesium compounds.     

meso－四（4－磺酸苯基）卟啉与Co（Ⅱ）的显色反应的研究

本文研究了弱酸性介质中钴（Ⅱ）与ＴＰＰＳ４的显色反应条件。实验发现胺类化合物质子化后，不参与成络反应，而均能使ＴＰＰＳ４试剂的吸光度大大降低，从而提高了测定的灵敏度，Ｃｏ（Ⅱ）－ＴＰＰＳ４络合比为１：１，ε＿（４２６）＝３．５４×１０￣５，钴含量在０～５．０μｇ／２５ｍＬ范围内呈线性，并用于烟草、茶叶中痕量钴的测定，得到了满意的结果。     

Kinetic studies of nickel speciation in model solutions of a well-characterized humic acid using the competing ligand exchange method

Publications on the binding characteristics of metals with humic acid (HA) are sparse. Here we investigated the release of nickel from Ni(II)-HA complexes using model solutions of three different [Ni(II)]/[HA] mole ratios at three different pH values; we also compared the results with those of [Ni(II)]/[FA] complexes from previous work in this laboratory. Ligand exchange kinetics using the competing ligand exchange method (CLEM) were studied using two different techniques: graphite furnace atomic absorption spectrometry (GFAAS) with Chelex 100 resin as the competing ligand, and adsorptive cathodic stripping voltammetry (AdCSV) with dimethylglyoxime as the competing ligand to measure the rate of dissociation of Ni(II)-HA complexes. The results of the kinetic studies showed that as the [Ni(II)]/[HA] mole ratio was decreased, the rate of dissociation of Ni(II)-HA complexes decreased, and the proportion of free Ni²⁺ ions plus very labile nickel complexes decreased while the proportion of the less labile kinetically distinguishable components increased. Generally, the rate of dissociation of Ni(II)-HA complexes was slower than that of Ni(II)-FA complexes. Studies on the validity of the kinetic model showed that the concentrations of chemical species varied in a reasonable way with pH and the [Ni(II)]/[HA] mole ratios, indicating that the kinetically distinguishable components have chemical significance and the kinetic model is valid.