多状态旋转阀的研制及其在自动分析中的应用

本文研制了在流动注射分析及其它自动分析中应用的８状态旋转阀。该阀用步进电机驱动，光电开关定位，单片微机系统控制。所研制的阀应用于自动溶剂萃取光度分析，取得满意效果。     

烷类特种气体分析装置的研制及其应用

研制烷类特种气体分析专用的多维气相色谱仪，特制的热导检测器，具有手动－自动功能。设计了输气－配气装置和多维气相色谱流程。以微机控制，可按编辑程序清洗系统。检查本底，自动进样，显示或打印谱图和分析结果。可检测多种烷类特种气体组份及其中氧，氮，一氧化碳和甲烷等痕量杂质。     

疲劳内耗仪的控制微机的更新及功能开发

介绍了对中法合作研制的疲劳内耗仪微机控制部分的改进，采用的ＩＢＭ－３８６，改进了控制及实验数据处理的方式，并扩展了仪器的功能。     

仪器分析标准物质

简述仪器分析标准物质的重要性及我国发展现状，指出了仪器分析标准物质研制中存在的问题。以光谱分析标准物质为例，介绍了仪器分析标准物质研制的特点，光谱分析标准物质的均匀性是研制的关键，其标准不确定度应由定值分析产生的标准不确定度、块状样品间的不均匀性产生的标准不确定度及块状样品内部的不均匀性产生的标准不确定度组成。     

全固态竹林胺传感器的研制和应用

全固态竹林胺传感器的研制和应用李荣华，乔宏斌（河南教育学院，郑州４５０００３）１引言竹林胺为ａ－肾上腺素受体阻滞药，现行分析标准为非水滴定法，不适于含碱性杂质的样品，而且手续繁复。本文首次报道了聚苯胺修饰竹林胺传感器的研制和应用。将具有较高导电性、良...     

磷钼杂多酸—碱性染料离子缔合物掺杂聚吡咯薄膜修饰石墨电极的研究

采用电化学聚合法研制了磷钼杂多酸－碱性染料离子缔合物掺杂聚吡咯薄膜修饰石墨电极，研究了修饰电极的电化学行为。     

气体分析用锡片和锡囊的研制与应用

本文提出了一种填补国内空白的新产品－气体分析用锡片和锡囊的研制方法。对锡片，锡囊的外观和内在质量检测结果证明，研制的锡片，锡囊完全达到了美国ＬＥＣＯ公司同类产吕的技术标准，而价格只有进口产品的四分之一左右。应用结果表明，该产品完全可以取代进口，完全适用于用事种金属及其俣金材料中气体分析的要求。     

单纯形自动优化的顺序注射分析系统

报道了具有自动优化功能的微机控制的顺序注射光度分析系统的研制。系统主要由注射汞、十位选择阀和带流通池的分光光度检测器构成。操作参数设定、数据采集和处理通过微机完成。采用改进单纯形方法进行系统优化,其算法集成到ＳＩＡ系统控制程序中使优化过程在微机的控制下自动完成。系统研究了ＳＩＡ钼蓝法测磷的操作条件对结果的影响。     

水质硬度测定仪的研制及应用

研制了一种便携式硬度测定仪，仪器检出限为０．２μｍｏｌ／Ｌ，，特别适用于锅炉罗化水等超低硬度水样的快速测定。     

YL－110型流动注射测金装置的研制

研制了一台流动注射测金装置。该装置由一台四道蠕动泵、两支旋转阀，一支８５３１纤维分离富集柱和有关电路组成一个整体，靠蠕动泵自动输送试样溶液，酸洗液和金洗脱液，使金在Φ３×４０ｍｍ的微型纤维柱上富集，由控制电路控制旋转阀切换自动完成柱平衡，进样，洗涤，洗脱过程，金洗脱液自动送入原子吸收分光光度计测定金。８５３１纤维是金的良好吸附剂，具有选择性容量大的优点。试样经王水分解后可直接进样测定。该装置与原子吸收分光光度计联用测定金。金的特征浓度可达０．６ｎｇ／ｍＬ每小时可测定４０～６０次。用本装置分析０．１６μｇ／ｍＬ金溶液，ＲＳＤ为０．８％。用于分析化探样品，铜精矿，电解铜等试样中金，得到满意的结果。     

污水监测过程的质量控制

在污水监测过程中，采用测定全程序空白值、进行平行双样测定、对样品进行复测、考察加标回收率、使用标准物质、分析同一样品不同指标的相关性等多种控制方法，从不同方面对分析过程进行控制，可大大提高分析结果的科学性、准确性、可靠性。     

同位素稀释热电离质谱法测定人血清中痕量铜和锌

采用热电离同位素稀释质谱法(ID-TIMS)准确测定了欧盟标准物质与测量研究院(EC-JRC-IRMM)组织的国际测量评估计划IMEP-17人血清样品中的痕量铜和锌。由于锌和铜都是易受污染的元素,本工作建立了仅用少量硝酸消解的低流程本底和适于热电离质谱测量的生物基体血清中痕量铜和锌的样品前处理方法;采用适当比例的硅胶和磷酸作为电离增强剂,在热电离质谱(TIMS)测量时获得了较高强度且稳定的铜和锌离子束;血清中痕量铜和锌的测量结果可直接溯源到国际单位mole。2种人血清样品中铜和锌测量结果的不确定度(k=2)分别为0.94%、0.83%和0.49%,测量值被EC-JRC-IRMM采用作为该样品的标准值。     

Determination of trace lead by hydride generation-inductively coupled plasma-mass spectrometry

A newly developed hydride generation-inductively coupled plasma-mass spectrometry (HG-ICP-MS) system was employed to determine trace amounts of lead in geological and biological samples. Laboratory-made single-stage and double-stage gas-liquid separators (GLSs) were investigated in order to replace the consumable membrane-GLS. Possible reasons were given why double-stage GLSs were superior over the single-stage ones according to the factors such as GLS volume and configuration, carrier gas inlet mode and flow rate. Interferences in liquid and vapor phase from concomitant ions and their products were investigated employing different flow mani-folds. Memory effects contributed to the blank values, but could be reduced employing a special wash protocol. Internal and external standardization were combined to improve the accuracy of the method, with bismuth as the internal standard according to its similarity with lead in the HG-ICP-MS system. Compared with ICP-MS and hydride generation-atomic fluorescence spectrometry (HG-AFS) methods, the system performance of HG-ICP-MS was characterized with improved detection limit to 0.002 ng/ml and acceptable short- and long-term stabilities. The linear dynamic range of this method was up to 50 ng/ml lead. Three Chinese national certified reference materials: poplar leaves, human hair and copper ore, were analyzed for method validation, and the results agreed well with the certified values. At last, the method was also employed to determine wide range of lead concentrations in lightweight limestone and nervous tissue samples from infants of albino rats with recoveries between 95 and 105% (n=10).     

电感耦合等离子体原子发射光谱法(ICP-AES)测定玄武岩中的8种微量元素

采用硝酸-盐酸-氢氟酸高压封闭消解样品,电感耦合等离子体原子发射光谱法测定玄武岩中的8种微量元素。实验确定了方法的分解条件以及测定元素的检出限及干扰条件。用国家一级标准物质GBW07105(玄武岩)进行方法验证,检测结果与标准值基本吻合,符合地质矿产开发的要求。     

Trueness, precision, and detectability for sampling and analysis of organic species in airborne particulate matter

Recovery, precision, limits of detection and quantitation, blank levels, calibration linearity, and agreement with certified reference materials were determined for two classes of organic components of airborne particulate matter, polycyclic aromatic hydrocarbons and hopanes, using typical sampling and gas chromatography/mass spectrometry analysis methods. These determinations were based on initial method proficiency tests and on-going internal quality control procedures. Recoveries generally ranged from 75% to 85% for all target analytes and collocated sample precision estimates were generally better than 20% for polycyclic aromatic hydrocarbons and better than 25% for hopanes. Results indicated substantial differences in data quality between the polycyclic aromatic hydrocarbons and hopanes. Polycyclic aromatic hydrocarbons demonstrated better collocated precision, lower method detection limits, lower blank levels, and better agreement with certified reference materials than the hopanes. The most serious area of concern was the disagreement between measured and expected values in the standard reference material for hopanes. With this exception, good data quality was demonstrated for all target analytes on all other data quality indicators.     

Simultaneous determination of monomethylmercury, monobutyltin, dibutyltin and tributyltin in environmental samples by multi-elemental-species-specific isotope dilution analysis using electron ionisation GC-MS

In this work, the simultaneous determination of four organometallic species (monomethylmercury, monobutyltin, dibutyltin and tributyltin) in environmental samples by using a GC-MS system with electron ionisation has been established. The measurement of isotope ratios in each species was accomplished by selecting the most adequate molecular cluster, and simple mathematical equations were applied to correct the contributions of 13C from the organic groups attached to the tin and mercury atoms. The influence of different parameters such as dwell time on the precision and accuracy of the measured isotope ratios in each target species has also been studied. The determination and the sample preparation procedures presented in this work were first individually validated by analysing several certified reference materials for butyltin compounds (mussel tissue CRM-477 and marine sediment SOPH-1) and for monomethylmercury (tuna fish CRM-464) using an innovative focused microwave technology for the extraction of the species from the solid samples. Additionally, the simultaneous determination of the four species was successfully validated by obtaining quantitative recoveries in spiked natural waters and by analysing the certified reference material BCR-710 (certified in tributyltin and monomethylmercury). The values obtained in such certified tissue were fully in agreement not only with the certified mass fractions but also with the proposed indicative values for mono- and dibutyltin.     

Preconcentration and determination of lead, cadmium and nickel from water samples using a polyethylene glycol dye immobilized on poly(hydroxyethylmethacrylate) microspheres.

A simple and sensitive preconcentration analysis-atomic absorption spectrometric procedure is described for the determination of lead, cadmium and nickel. The method is based upon on-line preconcentration of metal ions on a minicolumn of Cibacron Blue F3-GA immobilized on poly(hydroxyethylmethacrylate), poly(HEMA). The enrichment factors obtained were 42 for lead, 52 for cadmium and 63 for nickel (sample volume 10 mL and sample flow rate 5 mL/min). The relative standard deviations (n = 10), in 10 mL sample solutions containing 100 microg/L Pb(2+), 10 microg/L Cd(2+) and 100 microg/L Ni(2+) were 8.9, 3.7 and 3.5%, respectively. The limits of detection (blank + 3s) (n = 10), were found to be 12.01 microg/L for Pb(2+), 1.34 microg/L for Cd(2+) and 28.73 microg/L for Ni(2+). The accuracy of the system was checked with certified and tap water samples spiked with known amounts of metal ions. No significant difference was found between the achieved results and the certified values.     

Atomic fluorescence spectrometry combined with reduction aeration for the determination of mercury in biological samples

A sensitive atomic fluorescence system for the determination of mercury was optimized. The system consists of a continuous-flow mercury vapour generator coupled to a fluorescence spectrometer specific for mercury. A new gas-liquid separator was developed. A detection limit of 0.9 ng Hg 1^?1 was obtained. The system was combined with a microwave oven for dissolving samples in closed Teflon PFA vessels. Accurate results were obtained for certified reference materials, and biological samples such as urine and hair were analysed.     

Quality assurance for the analytical data of micro elements in food

The micro element content of food is an important quality index due to the action of these elements on human health. In this article, we discuss how to ensure the reliability of analytical data on micro elements in order to truly represent the condition of food. Sampling, treatment of the analytical sample, selection of the analytical method, standard solution, and certified reference material, blank test, calibration of the instrument and equipment, application of the quality control chart, assessment of the final analytical result, and quality assurance system are briefly described. Received: 5 July 2001 Accepted: 19 November 2001     

石墨炉原子吸收光谱法测定保健品松花粉中痕量铅

实验通过采用优级纯以上试剂降低本底,多道程序清洗器皿控制污染,通过控制酸量改善测定铅的信噪比,降低检出限,引入基体改进剂磷酸二氢铵消除基体干扰.优化石墨炉检测条件下,松花粉样品中铅的加入平均回收率达到90％以上.使用标准物质(茶叶GBW10016)对该方法进行了验证,结果表明铅的测定值在标准物质的保证值范围内.该方法能...