地质分析的历史发展及当今热点

简要回顾了地质分析技术的历史与发展,分析了当代地学研究对地质分析提出的新要求和当前分析科学所能提供的基础条件,评价和展望了现代地质分析的重要领域和热点技术：整体分析,显微分析技术的发展及对气体地球化学分析、现场分析、地质标准物质和“绿色”分析技术的需求。“地质分析”从“岩析分析”走来,并将向涉及更广领域的“天然材料分析”扩展。整体分析、显微分析、有机和无机生化分析将是其3个重要发展方向。     

面向新世纪的冶金材料分析

21世纪冶金材料分析面临复杂体系中痕量元素分析、冶金材料原位分析以及在线实时分析等三大问题。本文对这三方面的发展趋势进行了评述。     

冶金分析

本文是《分析试验室》定期评述“冶金分析”的续篇。对１９９３－１９９５年我国在该领域发表的工作进行评述，国内几种主要期刊１９９６年１季度发表的工作也包括其中。     

食品分析

本文对 1 998～ 1 999年间国内食品分析进展作了简介 ,内容包括食品的元素分析、化合物分析、添加剂分析、毒物、药物残留分析、食品色香味品质分析、营养分析、快速检测、打假防伪分析、微生物检验和有关基础研究与新食源开发分析等。引入文献338篇。     

高速分析进展

介绍近年来高速分析研究的一些新成果，提出了高速分析发展的方向。     

质谱应用心得

有机化合物四大谱(质谱、核磁、红外、紫外)已成为有机化学学科中很重要的分析鉴定手段。从大学二年级起,我们学习了《仪器分析》、《仪器分析实验》、《有机化合物的光谱鉴定》等课程,但这些理论上的学习只在我们脑海中留下不明的,笼统的概念。直至做毕业论文时,我们将自己亲手合成的化合物进行质谱分析来鉴定证实,才对质谱有了进一步的较清晰的了解,巩固     

仪器分析中的定量方法

在目前国内使用的仪器分析教材中,当介绍每一种仪器分析方法的应用时,均要涉及到它的定量分析方法。与经典的化学分析不同,除少数仪器方法(如:库仑分析、电重法、热分析等)外,一般都需要有与待测物质相同的标准样品,并以如下关系式为基础进行定量分析:     

化工,石油产品及硅酸盐分析

本文是《分析试验室》定期评述中“化工、石油产品及硅酸盐分析”课题的第六次评述，它评述了１９９５年７月至１９９７年６月国内关于化工产品、石油产品、硅酸盐的分析进展情况，共引用文献６７５篇。     

发光分析

本文是《分析试验室》定期评述中“发光分析”课题的第篇评述文章，它评述在１９９１年１月－１９９４年１２月间我国发光分析的发展概况，内容包括：概述、荧光分析、磷光分析化学发光和生物发光分析。     

顶空进样GC-SIM-MS测定硝唑尼特中溶剂残留甲醇含量

利用气相色谱-选择离子监测质谱联用仪(GC-SIM-MS)测定硝唑尼特样品中溶剂残留甲醇的含量,顶空进样,温度为70℃,时间为20 min.SIM定量离子m/z 32,参考离子m/z 31,30和29.甲醇质量浓度在0.5~100μg/m L内呈良好的线性(R~2=0.999 92).方法相对标准偏差为2.49%~4.85%,样品加标回收在94.5%~102.8%之间,检测限为0.5μg/m L,符合定量分析的要求.     

毛细管气相色谱法测定腈纶布料中苯、甲苯和二甲基甲酰胺残留

 建立了同时定量测定腈纶布料及其服装中的苯、甲苯和二甲基甲酰胺残留的毛细管气相色谱分析方法。测得的回收率分别为 93 .3 % ,1 0 1 .8% ,94.9% ;变异系数为 3 .4% ,2 .0 % ,2 .8%。方法简便、快速、准确。     

采用二维气相色谱及毛细管色谱柱分析汽油中苯和甲苯的含量

采用微板流路控制技术(Deans Switch)和常见的商品毛细管柱HP-5 (30 m×0.32 mm×0.25 μm)和Rtx-TCEP (30 m×0.25 mm×0.4 μm),建立了一种全新的分析车用汽油中苯和甲苯含量的二维气相色谱方法。用该方法分析汽油中0～5%的苯和0～20%的甲苯,两者校正曲线的线性关系良好,相关系数分别为0.9994和0.9999;标准样品5次重复测定的相对标准偏差均小于1.5%;车用汽油实际样品中苯和甲苯的加标回收率在96.8%～103.8%之间。车用汽油实际样品测定结果和SH/T 0713-2002标准方法测定结果一致。该方法是车用汽油中苯和甲苯含量测定的一种简便快捷、准确可靠的分析方法。     

用大口径毛细管气相色谱法快速测定塑料食品包装袋中有机残留物

采用５３０μｍ大口径毛细管色谱柱,顶空气相色谱－火焰电离检测器测定,建立了一种塑料食品包装袋中有机溶剂———甲苯、乙酸乙酯、丁酮和异丙醇残留的气相色谱快速分析方法,回收率为９４．８％～１０１．６％,相对标准偏差为０．８％～２．７％。方法简便、灵敏、准确、重现性好。     

Determination of fuel dialkyl ethers and BTEX in water using headspace solid-phase microextraction and gas chromatography-flame ionization detection

A simple procedure for the determination of methyl tert-butyl ether (MTBE), ethyl tert-butyl ether (ETBE), ethyl butyl ether (EBE), tert-amyl methyl ether (TAME), benzene, toluene, ethylbenzene, and xylenes (BTEX) in water using headspace (HS) solid-phase microextraction (HS-SPME) was developed. The analysis was carried out by gas chromatography (GC) equipped with flame ionization detector (FID) and 100% dimethylpolysiloxane fused capillary column. A 2 Plackett-Burman design for screening and a central composite design (CCD) for optimizing the significant variables were applied. Fiber type, extraction temperature, sodium chloride concentration, and headspace volume were the significant variables. A 65 microm poly(dimethylsiloxane)-divinylbenzene (PDMS-DVB) SPME fiber, 10 degrees C, 300 g/l, and 20 ml of headspace (in 40 ml vial) were respectively chosen for the best extraction response. An extraction time of 10 min was enough to extract the ethers and BTEX. The relative standard deviation (R.S.D.) for the procedure varied from 2.6 (benzene) to 8.5% (ethylbenzene). The method detection limits (MDLs) found were from 0.02 (toluene, ethylbenzene, and xylenes) to 1.1 microg/l (MTBE). The optimized method was applied to the analysis of the rivers, marinas and fishing harbors surface waters from Gipuzkoa (North Spain). Three sampling were done in 1 year from June 2002 to June 2003. Toluene was the most detected analyte (in 90% of the samples analyzed), with an average concentration of 0.56 microg/l. MTBE was the only dialkyl ether detected (in 15% of the samples) showing two high levels over 400 microg/l that were related to accidental fuel spill.     

Flow injection analysis of copper diethyldithiocarbamate in high resistance toluene media using a microelectrode detector

Flow injection (FI) analysis of copper as the copper diethylthiocarbamate complex (Cu(Et₂dtc)₂) has been performed in a high resistance toluene carrier stream. The method is based on the oxidation of the copper complex at a platinum microelectrode fabricated to fit a Metrohm wall-jet flow cell. Electrodes of sizes 5 to 25 μm radii were tested in toluene-based carriers containing either 0.03 M tetrahexylammonium perchlorate (Hex₄NClO₄) or 35% acetonitrile. Detection limits (3 : 1 signal to noise ratio) in the range 1 × 10⁻⁷ M (5 μm radius electrode) to 5 × 10⁻⁸ M (25 μm radius electrode) were achieved, which are comparable to detection limits reported in lower resistance media under similar conditions. The system was applied to the analysis of copper in water samples after extraction of the metal as its diethyldithiocarbamate into toluene and good agreement was found with data obtained by other voltammetric methods.     

2,4,6‐trichlorophenyl acrylate emulsion‐templated porous polymers (PolyHIPEs). Morphology and reactivity studies

A series of monolithic crosslinked polymers with 2,4,6‐trichlorophenyl acrylate as a reactive component was prepared by free radical polymerization of the internal phases of high internal phase emulsions (HIPEs). The volume ratio of water to oil phase (void volume; 60–90%), crosslinker type (divinylbenzene or ethylenglycol dimethacrylate) and quantity (30–50 mol %) and type of porogenic solvent (chlorobenzene, toluene, chloroform, dichloroethane) were altered to study these effects on the structure and reactivity of the monolithic polymers. The polymer supports were characterized by scanning electron microscopy (SEM), FTIR spectroscopy, elemental analysis and mercury intrusion porosimetry. SEM images revealed an open cellular structure with voids between 1 and 12 μm and window sizes between 0.3 and 3 μm. The porogen had an influence on the surface area, being larger with added porogen and the influence being highest with toluene. Adding toluene also influenced the void size, increasing the average diameter from ～2 μm (no porogen) to ～12 μm (added toluene). Monolithic supports were functionalized by reaction of the ester moieties with tris(2‐aminoethyl)amine derivative and by hydrolysis of the ester groups to carboxylic acids. © 2007 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 45: 4043–4053, 2007     

Mercapturic acids derived from toluene in rat urine samples: identification and measurement by gas chromatography–tandem mass spectrometry

Toluene is one of the most widely used CMR chemicals in industry. Worker exposure to this compound is regulated in France, but new, more sensitive methods are required to effectively monitor this exposure. A gas chromatography-tandem mass spectrometry (GC-MS/MS) method was developed and fully validated for the simultaneous determination of urinary toluene mercapturic acids derived from side chain and ring oxidation, i.e., benzylmercapturic acid and the three isomers o-, m- and p-toluylmercapturic acids, respectively. The method involves a simple and efficient two-step preparation procedure consisting of liquid-liquid extraction of the urinary acids followed by a microwave-assisted esterification of the isolated compounds using 2-propanol. The method meets all the required validation criteria: high selectivity, intra-day and inter-day precision ranges between 1.0?% and 12.4?%, with close to 100?% recovery. Linearity has been shown over the reduced concentration range 0.03-0.5?mg/L whereas a multiplicative model (ln-ln transformation) had to be used to describe the full range of concentrations 0.03-20?mg/L. The limits of detection for the four analytes, ranging from 2.8 to 5.5?μg/L, made the method suitable for their identification and quantification in urine from rats inhaling toluene in the 2 to 200?ppm concentration range. All urine samples from exposed rats contained measurable amounts of all metabolites. This is the first time that o- and m-toluylmercapturic acids have been shown to occur. Our results confirm the hypothesis that toluene mercapturic acids derived from ring oxidation exist in three forms.     

顶空气相色谱法测定盐酸司他斯汀中6种残留溶剂

建立了顶空气相色谱法(HS-GC)测定盐酸司他斯汀中乙醚、丙酮、异丙醇、四氢呋喃、甲苯与二甲苯6种有机溶剂残留量的方法.样品用二甲基亚砜溶解,在110 ℃加热20 min,使气液平衡,采用氢火焰离子化检测器(FID),以DB-1701(60 m x 0.320 mm,1.00 μm)为分析柱,程序升温测定.在优化的气相...     

Spectrophotometric determination of NO(2) in the working atmosphere

A method is described for determining NO(2) in workplace atmospheres, based on its reaction with bis(diethyldithiocarbamato)copper(II) in toluene. NO(2) is absorbed from an air sample by a toluene solution of Cu(dtc)(2) and the decrease in the initial absorbance at 437 nm is measured. The method has been compared with the Saltzman method. The interference of NO, Cl(2), O(3), SO(2) and other gases has been studied. The NO(2) concentration range of the method is 1-500 mg m (3).