火焰原子吸收光谱法测定高纯阴极铜,电解铜中的铅,铁,铋及钴矿中的铅

１引言纯铜中铁、铅的测定多采用石墨炉原子吸收法，而铋的测定采用氢化发生－原子荧光光谱法。本文论述了采用镧盐或铅盐作捕集剂，用过量氨水将铁、铅、铋与氢氧化镧或氢氧化锆共沉淀，硝酸或盐酸溶解后，用火焰原子吸收光谱法速测三元素，无需用价格昂贵的石墨炉原子吸收光谱仪和无色散原子荧光光谱仪，也不必去找高纯铜作基体，降低了综合分析的价格。而钻矿微量铅的分析，因共存元素多，分析难度大，本法采用在６ｍｏｌ／Ｌ盐酸介质中，用个甲基戊酮－（２）除去铁及部分其它共存离子，为下一步富集微量铅创造了良好的条件。实验证明，…     

色谱法分离富勒烯的研究

研究了用活性炭作固定相，ＣＳ２作流动相柱色谱法分离富勒烯混合物的方法，考察了用溶剂浸泡活性炭减活的时间、活性炭与富勒烯混合物配比、活性炭的粒度等因素对分离结果的影响，采用了索氏抽提器，可以很快地将固定相中的Ｃ７０等高级富勒烯提取出来，提高了回收率。     

植物和人发样品中痕量铅的氢化物原子荧光测定

以双电极高强度空心阴极灯作激发光源，于铁氰化钾碱性体系内进行铅的氢化反应。实验表明，原子化过程中石英炉芯对铅烷存在吸附。在最佳测试条件下，溶液检出限为０．１７μｇ／Ｌ，分析了国家一级植物标样和头发标样中痕量铅，取得令人满意的结果。     

中温煤焦油沥青的超临界溶剂抽提和分离

用超临界溶剂在半连续装置上对中温煤焦油沥青（ＭＣＴＰ）进行了抽提和分离，考察了抽提段的实验条件对灰分和吡啶不溶物（ＰＩ组分）脱除率的影响；在分离段使用升温和／或降压法、精馏法调节ＭＣＴＰ族组成分布，并用分步抽提法调节ＭＣＴＰ的族组成。实验表明：用甲苯为超临界溶剂抽提可脱除全部灰分，ＰＩ组分也可在较低的压力下选择性地脱除；采用升温和／或降压法对抽出物可进行一定程度的分离，但对庚烷可溶物（ＨＳ组分）分离的选择性不高；采用精馏法可选择性地脱除ＨＳ组分，但尚需改进设备进一步提高分离效率；采用分步抽提法用石油醚作一次抽提溶剂可高选择性地脱除ＨＳ组分，其选择性在９５％以上。     

化学衍生—高效液相色谱法同时测定铅（Ⅱ）和汞（Ⅱ）

从吡啶－２－乙醛苯甲酰腙作柱前衍生试剂，在优化了衍生和色谱条件下实现了用高效液相以谱法同时测定铅和汞离子，在ｐｈｅｎｏｍｅｎｅｘｓｐｈｅｒｅｘＣ１８色谱柱上，用甲醇－水（６５：３５，Ｖ／Ｖ），作流动相，于２４８ｎｍ处检测，得到线性良好的工作曲线，铅和汞的最低检测限分别为２．５５μｇ／Ｌ和７．２９μｇ／Ｌ。分析了环境水样品和合成水样，铅和汞的标准加入回收率分别为９８．３％～１０１．７％和９８．０～１     

环己酮抽提煤的研究

报道了环己酮在索氏抽提及回流抽提等条件下对不同煤队煤样的抽提行为，并探讨了抽提机理与特点，研究结果表明五己酮是一种良好的氢键受体，它与煤分子间相互作用同煤中羟基有密切关系。     

石墨炉原子吸收法直接测定含盐调味品中铅

用５００ｍｇ．Ｌ＾－１钯－２％砂酸作改进剂，直接测定含盐调味品中的铅，免去了复杂的前处理过程，消除了食盐的背景干扰，提高了效率，方法的平均回收率为１０２％±５．２８％，特征量为：铅２．５×１０＾－１１ｇ。     

石墨炉原子吸收光谱法测定全血中铅的方法改进

针对不同的石墨管测定全血中铅时，用铅标准溶液制作的标准曲线和以全血为基体制作的标准工作曲线斜率的不一致，提出以磷酸氢二铵、磷酸氢二钠和硝酸铵作基体改进剂，以全血为基体制作标准工作曲线来测定全血中铅含量的方法。试验表明，此法基本消除了全血基体对血铅测定的影响，适应各种石墨管，可快速、准确地测定全血中铅。     

石墨炉原子吸收法测定食品中痕量铅

样品经硝酸和高氯酸分解后，加入磷酸二氢铵作基体改进剂测定铅，方法快捷，准确，经济，精密度≤14％，回收率92％～104％，检出限0．4ng／mL，用于多种食品中铅的测定，结果令人满意。     

一种简单的抽提法

一种简单的抽提法王荣民张海涛何玉凤王云普（西北师范大学化学系兰州７３００７０）固体物质的抽提，一般是在所谓的索氏（Ｓｏｘｈｌｏｔ）抽提器中进行的。我们在实验过程中发现使用现成的磨口索氏抽提器有诸多不便：首先，索氏抽提器的成套性不好，这是因为索氏抽提器...     

Capillary electrophoretic separation of protease inhibitors used in human immunodeficiency virus therapy

A new capillary electrophoretic method for trace analysis of gamma-cyclodextrin, gamma-CD, in a sample of beta-CD has been developed, building on our recent work in which the tetraphenylborate ion, Ph4B-, was found to bind to gamma-CD three orders of magnitude more strongly than to beta-CD. The method involves measurement of the change of net electrophoretic mobility of Ph4B- and its CD complexes in a background electrolyte containing a fixed concentration of beta-CD. Good linearity was found between 1/deltamu and 1/Cgamma where deltamu is the difference in the mobility of Ph4B- in the beta-CD solution at a given and at zero concentration of gamma-CD, and Cgamma the gamma-CD concentration. The limit of detection for gamma-CD in a beta-CD sample was found to be 0.020% (w/w), and high precision and accuracy were obtained.     

铀的三元协萃规律研究-HTTA-HPMBA-(C8H5)4AsCl三元协萃高氯酸铀酰的机理

本文研究α-噻吩甲酰三氟丙酮(HTTA),1-苯基-3-甲基-4-苯甲酰基-5吡唑啉酮(HPMBP)与四苯基砷氯(C5H5)4AsCl的氯仿溶液从高氯酸中萃取U(VI).该体系属螯合,离子缔合AAC类,测定了其二元及三元协同萃取体系平衡常数.用亚甲基蓝光度法测定了萃合物中ClO4^-的存在,用斜率法确定二元协萃物组成为(C6H5)4As^+[UO2(ClO4)(TTA)2]^-和C6H5)4As^+[UO2(ClO4)(PMBP)2]^-三元协萃配合物为(C6H5)4As^+[UO2(ClO4)(TTA)(PMBP)]^-.     

Palladium fluoride complexes: one more step toward metal-mediated C-F bond formation

The first molecular complexes of palladium containing a Pd-F bond, both fluorides and bifluorides, were synthesized and fully characterized in the solid state and in solution. Reactivity studies of the Pd fluoride complexes revealed their unexpected stability and unusual chemical properties, different from the hydroxo, chloro, bromo, and iodo analogues. A novel efficient method to generate "naked fluoride" was developed using [(Ph(3)P)(2)Pd(F)Ph]. The naked fluoride from the Pd source fluorinated dichloromethane, deprotonated chloroform, and catalyzed di- and trimerization of hexafluoropropene under uncommonly mild conditions.     

TREATMENT AND RESOURSE REUSE OF INDUSTRIAL WASTEWATER FROM PRODUCTION PROCESS OF PHENYL ACETIC ACID

The effluent from phenyl acetic acid (Ph CH2COOH) production process can be treated with NDA-999 macroporous polymeric adsorbent with about 100% remopval efficiency of Ph CH2COOH,benzyl alcohol(PhCH2OH) and benzaldehyde(PhCOHO)as well as the decrease in Total Organic Carbon(TOC)from 4691mg/l to <300mg/L.3.7kg phCH2COOH and 120kg NaCl will be recovered from per m^3 wastewater and the adsorbent can be reused after being regenerated by NaOH aqueous solution and methanol.Good economic,social and environmental results can be achieved with this method.     

银合金中银、铜含量的示波滴定

报道了用示波滴定银合金中银、铜的含量。试样酸溶后,取部分试液,在pＨ５～６的ＨＡc－ＮaＡc缓冲介质中用四苯硼钠（Ｎa－ＴＰＢ）法示波滴定银。另取部分试液,加Ｖe使Ｃu＾２＋还原为Ｃu＾＋,用Ｎa－ＴＰＢ法示波滴定铜,而Ａg＋被还原为Ａa,避免了测定铜的干扰。该方法标准加入回收率为９９．８％～１００．２％,ＲＳＤ〈０．２％。     

Protein extraction from Phoenix dactylifera L. leaves, a recalcitrant material, for two-dimensional electrophoresis

This work was aimed at optimizing a protein extraction procedure for date palm (Phoenix dactylifera L.) leaves, a highly recalcitrant plant tissue for 2-DE. Five protein extraction protocols based on different protein precipitation agents (TCA/acetone vs. phenol (Ph) methods) and protein resolubilization methods (physical treatments, e.g., sonication, shaking and/or heating) were tested. Ph/SDS extraction with methanol/ammonium acetate precipitation, followed by DOC preincubation and TCA/acetone precipitation and, finally, solubilization by shaking in rehydration solution was found to be the best protein extraction method. We conclude that DOC with TCA/acetone precipitation step eliminates interfering compounds, thus allowing efficient resolubilization of date palm leaf proteins. This method could be appropriate for proteomic studies such as date palm colonization by entomopathogenic fungi.     

Structural diversity in a family of copper(I) thioether complexes

Copper(I) complexes of the tridentate thioether ligands [PhB(CH(2)SCH(3))(3)] (abbreviated PhTt), [PhB(CH(2)SPh)(3)] (PhTt(Ph)), [PhB(CH(2)S(t)()Bu)(3)] (PhTt(t)()(Bu)), and [PhB(CH(2)S(p)()Tol)(3)] (PhTt(p)()(Tol)) and bidentate thioether ligands [Ph(2)B(CH(2)SCH(3))(2)] (Ph(2)Bt), [Et(2)B(CH(2)SCH(3))(2)] (Et(2)Bt), and [Ph(2)B(CH(2)SPh)(2)] (Ph(2)Bt(Ph)) have been prepared and characterized. The solution and solid state structures are highly sensitive to the identity of the borato ligand employed. Ligands possessing the smaller (methylthio)methyl donors, [PhTt] and [Ph(2)Bt], yielded tetrameric species, [(PhTt)Cu](4) and [(Ph(2)Bt)Cu](4), containing both terminal and bridging thioether ligation. The ligands containing the larger (arylthio)methyl groups, [PhTt(Ph)] and [PhTt(p)()(Tol)], form monomeric [PhTt(Ar)]Cu(NCCH(3)) in solution and one-dimensional extended structures in the solid state. Each complex type reacted cleanly with acetonitrile, pyridine, or triphenylphosphine generating the corresponding four-coordinate monomer, of which [PhTt(Ph)]Cu(PPh(3)), [PhTt(p)()(Tol)]Cu(PPh(3)), and [Et(2)Bt]Cu(PPh(3))(2) have been structurally characterized.     

Palladium doping of magic gold cluster Au38(SC2H4Ph)24: formation of Pd2Au36(SC2H4Ph)24 with higher stability than Au38(SC2H4Ph)24

A phenylethanethiolate-protected Pd(2)Au(36)(SC(2)H(4)Ph)(24) cluster, which is a two-Pd atom-doped cluster of the well studied magic gold cluster Au(38)(SC(2)H(4)Ph)(24), was synthesized in high purity and its stability was investigated. The results demonstrate that Pd(2)Au(36)(SC(2)H(4)Ph)(24) is more stable than Au(38)(SC(2)H(4)Ph)(24) against degradation in solution and core etching by thiols.     

Reversible H2 addition across a nickel-borane unit as a promising strategy for catalysis

We report the synthesis and characterization of a series of nickel complexes of the chelating diphosphine-borane ligands ArB(o-Ph(2)PC(6)H(4))(2) ([(Ar)DPB(Ph)]; Ar = Ph, Mes). The [(Ar)DPB(Ph)] framework supports pseudo-tetrahedral nickel complexes featuring η(2)-B,C coordination from the ligand backbone. For the B-phenyl derivative, the THF adduct [(Ph)DPB(Ph)]Ni(THF) has been characterized by X-ray diffraction and features a very short interaction between nickel and the η(2)-B,C ligand. For the B-mesityl derivative, the reduced nickel complex [(Mes)DPB(Ph)]Ni is isolated as a pseudo-three-coordinate "naked" species that undergoes reversible, nearly thermoneutral oxidative addition of dihydrogen to give a borohydrido-hydride complex of nickel(II) which has been characterized in solution by multinuclear NMR. Furthermore, [(Mes)DPB(Ph)]Ni is an efficient catalyst for the hydrogenation of olefin substrates under mild conditions.     

Ge(9)=Ge(9)=Ge(9)](6-): a linear trimer of 27 germanium atoms

The title anion was synthesized by oxidation of nido-Ge94- with Ph3P or Ph3As in ethylenediamine solution. It was structurally characterized in the compound (Rb-2,2,2-crypt)6[Ge9=Ge9=Ge9].3en (2,2,2-crypt = 4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo[8.8.8]hexacosane) crystallized from the solution. The anion is a linear trimer of nine-atom clusters with the shape of tricapped trigonal prisms elongated along two of the three prismatic edges. Each pair of clusters is connected by two exo-bonds.