微波常压法合成水杨酸酯

在浓硫酸催化下，采用微波常压法由水杨酸分别与正丁醇、异丁醇、正戊醇和异戊醇反应合成相应的水杨酸酯。结果表明：当水杨酸：醇：Ｈ２ＳＯ４＝１：５．５：０．３（摩尔比）时，采用５６０Ｗ微波辐射２２ｍｉｎ，水杨酸酯的产率可达８８．７％￣９６．４％，反应速度至少是常规反应的１４倍。     

兖州高硫煤的加氢热解脱硫及脱硫动力学

在加压热天平上，考察了氢气和氮扬气氛下高硫煤的热解脱硫。利用气相色谱在线分析研究了硫化氢氢气的逸出规律。结果表明，加氢热解比氮气下的热解有着更显著的脱友作用，脱硫率可达９０％以上。而且加氢热解下６５％的脱除硫转化为气相硫化氢，而氮气下热解是有８０％的硫转化为液相。     

Study on fluorescence property of dopamine and determination of dopamine by fluorimetry

In this study, a rapid and sensitive high performance liquid chromatography-inductively coupled plasma-mass spectrometry (HPLC-ICP-MS) determination of primary As species in fish tissues and urine is reported. The separation was achieved on an Altima C18 column with a mobile phase containing citric acid and hexanesulfonic acid (pH 4.5). As(V), monomethylarsonic acid (MMA), As(III), dimethylarsinic acid (DMA) and arsenobetaine (AsB) were separated in less than 4 min with retention times of 83, 99, 130, 166 and 208 s, respectively. This separation of five species in less than 4 min should be attractive to those interested in As speciation. The quantification limits were 44, 56, 94, 64, 66 ng l(-1) and the relative standard deviations (R.S.D.) for day-to-day injections of As at 2 mug l(-1) were 2.0, 3.1, 2.4, 3.8 and 4.0%. The procedure was tested using two reference materials (DORM-2 dogfish muscle tissue, NIST SRM 2670 Freeze-dried Urine, normal level) and then applied to real-world samples. The results obtained demonstrate the suitability of the procedure for screening and quantification at physiological levels of primary As species in biological samples.     

N-α-Benzyloxyacetyl derivatives of (S)-4-benzyl-5,5-dimethyloxazolidin-2-one for the asymmetric synthesis of differentially protected α,β-dihydroxyaldehydes

α-Dibenzylamino- and α-benzyloxy- derivatives of N-acetyl-(S)-4-benzyl-5,5-dimethyloxazolidin-2-one readily undergo highly stereoselective boron mediated syn-aldol reactions with a range of aromatic and aliphatic aldehydes, generating the syn-aldol products in good to excellent yields as single diastereoisomers after purification. In the α-dibenzylamino series, deprotection of the functionalised aldol fragments to the corresponding α-amino-β-hydroxy methyl ester or α-amino-β-hydroxyaldehyde proved problematic, with a range of N- and O-protecting groups giving mixtures of products arising from endocyclic and exocyclic cleavage pathways. However, in the α-benzyloxy series, O-silyl protection of the aldol products, and subsequent DIBAL reduction gives stereoselectively the corresponding N-1′-hydroxyalkyloxazolidin-2-ones, which undergo base promoted fragmentation to the desired highly functionalised and differentially protected α,β-dihydroxyaldehydes in good yields and without loss of stereochemical integrity.     

A novel three-dimensional coordination polymer [Cd2(C3H2O4)2(H2O)2(μ 2-hmt)] n (hmt = hexamethylenetetramine): synthesis and crystal structure

The self-assembly of the Cd^II ion, hexamethylenetetramine (hmt) and malonate ligand yields a three-dimensional (3D) coordination polymer [Cd₂(C₃H₂O₄)₂(H₂O)₂( ₂-hmt)] _n with channels. The Cd^II ion is located in a octahedral coordination environment, composed of four oxygen atoms from three malonates, one oxygen atom of water and one nitrogen atom of hmt. Two oxygen atoms of each malonate coordinate to the same Cd^II ion and the other two oxygen atoms connect to adjacent two Cd^II ions respectively to form a two-dimensional infinite network, these networks are bridged by ₂-hmt coordinated to Cd^II ions to product a 3D architecture.     

β-羧基乙基锗倍半氧化物及其衍生物

本文综述了β-羧基乙基锗倍半氧化物及其衍生物的生物活性、合成方法以及该领域最新研究动向。     

Comparison of procedures for correction of matrix interferences in the multi-element analysis of soils by ICP-AES with a CCD detection system

Three procedures, matrix matching, plasma optimisation and single-point standard-addition, have been evaluated to ascertain the best procedure for simultaneous multi-element analysis of industrial soils by ICP-AES with CCD detection. A standard reference material, CRM143 from the Bureau Communautaire de Réference (BCR), has been analysed for Cd, Cr, Cu, Mn, Ni and Pb using the three different matrix interference correction procedures. All three procedures give comparable results which are in good agreement with the BCR values, except for Cr. The single-point standard addition procedure was chosen, on the basis of economy and ease of implementation, to correct for matrix interferences in the determination of Cd, Co, Cr, Cu, Mn, Mo, Ni, Pb, Sn and V in soil samples collected from an industrial site in England. Concentrations of some of the elements were found to vary greatly with sampling depth. For example, the concentration of Mn, determined using the atomic line at 279.920 nm, increased from 426 ± 3 g/g at a depth of 18–28 cm to 5996 ± 144 g/g at 60–85 cm.     

用亚铁氰化钛钾从模拟高放废液中吸附Cs研究

本文研究了溶胶-凝胶法合成的无机离子交换剂亚铁氰化钛钾的耐酸性和辐照稳定性等性能，测定了从模拟酸性高放废液中主要常量组分离子相对于Cs的分离系数，研究了流速对Cs吸附曲线的影响。实验结果表明，该交换剂具有良好的辐照稳定性，交换剂经2×106Gy的辐照，亚铁氰化钛钾对Cs的表观交换容量下降6～7％，为0．873mmolCs／g干交换剂。在0．5～1．5mol／LHNO3中具有良好的化学稳定性。在模拟酸性高放废液中对几种离子的选择吸附顺序为：Cs＞＞M＞Fe＞Sr＞Na＞Cr＞Nd，Mn，该交换剂具有较高的吸附容量，对Cs具有良好的选择性，有希望用作从酸性高放废液中去除Cs的材料。     

反相液体色谱中饱和醇保留行为的研究 Ⅰ.低碳醇保留行为与溶质分子结构的关系

本文从吸附-疏溶剂理论出发,根据热力学平衡观点,导出了一定固定相和流动相时,描述溶质保留行为与其分子结构关系的理论模型,并用之预测了饱和醇的保留值,获满意结果。从而表明本模型不但能用于同系物,而且亦可用于同分异构体及立体异构体保留行为的预测。