毛细管电泳进样技术新进展

评述了毛细管电泳进样技术新成果。对直接在线进样，二维分离体系中毛细管电泳分离的增样，相关毛细管电泳增样，超微量样品及单个分子的进样，近端进样，双向进样和高温下的进样装置的应用状况作了介绍。     

固体进样元素分析技术在农业领域的应用

重金属是农产品、农田土壤、肥料、饲料等农业样品中的重要污染物,传统的实验室分析方法需繁琐的前处理,耗时费力,无法满足重金属的快速检测需求。固体进样元素分析技术具有简化样品前处理、便捷、绿色、高效等优势,在农业领域中元素的快速检测分析中具有良好的应用前景。通过对固体进样元素分析技术,包括样品导入技术和电热蒸发、电感加热、激光烧蚀、X射线荧光光谱、激光诱导击穿光谱等固体进样分析系统进行综述,并对这些技术在农业领域中的应用做了进一步的梳理。固体进样分析技术已在农业样品中元素的快速检测、现场监测、风险评估等工作中发挥着举足轻重的作用,相信随着仪器研发、材料科学、机器学习等新兴技术的快速发展,其结构小巧、使用简单、分析迅速等优势将会充分发挥,为农业领域中质量安全监管提供一种更为有效、可靠的快速检测手段。     

石墨炉原子吸收光谱法测定海产品中镉含量

采用固体进样-石墨炉原子吸收光谱法测定海产品中镉的含量。以1.0 g·L^-1硝酸铅溶液为基体改进剂,灰化温度为950℃,原子化温度为1 900℃。镉的进样量在0.05～0.2 ng之间与其吸光度呈线性关系,检出限（3s）为0.015 ng。应用此法分析了海产品样品,加标回收率在60.0%～90.0%之间,测定结果与液体进样-石墨炉原子吸收光谱法测定结果基本一致。     

ICP-SSEA 法测定铸铝合金中8种元素

将固体进样装置与电感耦合等离子体发射光谱仪(ICP-SSEA)联用，采用固体进样，直接测定铸铝合金中的铜、铁、镁、锰、镍、钛、硅、锌等元素含量。研究表明，该法与火花光谱法比较，具有很宽的的动态范围，测量精度和普通化学分析方法相当，同时又有火花光谱分析的速度。能满足工厂冶炼控制的要求。     

大体积进样技术在环境分析中的应用

在毛细管气相色谱法(CGC)中,采用大体积进样技术(LVI),即使用能够容纳大体积样品的进样装置以及增加可控时间的溶剂蒸汽放空装置,可以满足环境样品中超痕量组分的分析要求,简化样品浓缩步骤以及实现液相色谱(LC)与CGC的在线联用。针对分析物的性质、毛细管柱的规格和分析的目的已发展了多种LVI。本文总结了几种常见的LVI,包括柱头进样(OCI)和程序升温进样(PTV),以及近年来发展的一些新技术,如在柱同时溶剂浓缩进样、样品直接引入进样/复杂基质进样和同时溶剂冷凝无分流进样,阐述了各种进样技术的基本原理及其与样品提取、LC纯化在线联用的方法在环境分析应用中的一些最新研究进展。     

固体直接进样石墨炉原子吸收法测定土壤中镉元素

固体直接进样是近年来石墨炉原子吸收分析领域发展较快的技术,它取代了繁冗的对固体样品的前处理,避免了样品的污染和损失,也保护了操作人员的身体健康。采用固体直接进样-石墨炉原子吸收光谱仪,结合使用持久化学改进剂对环境土壤样品中Cd元素进行测定,其结果表明,方法检出限为0.002 66ng,定量测定下限为0.008 87ng,相对标准偏差RSD≤10%,方法准确、可靠,均满足环境土壤测试方法的要求。     

原子吸收光度法中一种脉冲进样装置

矿岩中钾钠含量的分析多年来一直采用火焰光度法和原子吸收光度法.原子吸收光度法的简便和快速是其它化学法所不及的.但在样品处理时,因钾长石只能用氢氟酸溶解,而用氢氟酸和硝酸混酸溶样过程中部分钾钠与铝已形成胶体氟铝酸钠(Na_3AlF_6)和氟铝酸钾(K_3AlF_6),此氟化物难溶于水,测定时易阻塞原子化器的燃烧缝口.本文自制的脉冲进样装置,结构简单,操作方便.在常规进样的同时自行定量吸取微量样品再进行脉冲进样,可获得两种进样方法的分析结果,长时间应用没有阻塞缝口的现象,并进行了两种进样方法的效果评价.     

大体积进样不分流气-质联用测定二噁英

利用大体积进样技术结合气相色谱-质谱仪器,对二噁英的测定效果进行了研究．对进样量1,5,10,25,50μL和100μL的色谱图进行了分析,同时与传统分流／不分流进样技术进行了对比．对比和研究表明：使用大体积进样方式完全可以代替传统分流／不分流进样技术,并且不影响色谱分离度,又可以大幅度提高仪器分析的灵敏度．     

毛细管电泳序列分析技术用于在线酶分析研究进展

毛细管电泳技术具有操作简单、样品消耗量少、分离效率高和分析速度快等优势,不仅是一种高效的分离分析技术,而且已经发展成为在线酶分析和酶抑制研究的强有力工具。酶反应全程的实时在线监测,可以实现酶反应动力学过程的高时间分辨精确检测,以更准确地获得反应机制和反应速率常数,有助于更好地了解酶反应机制,从而更全面深入地认识酶在生物代谢中的功能。此外,准确、快速的在线酶抑制剂高通量筛选方法的发展,对加快酶抑制类药物的研发以及疾病的临床诊断亦具有重要意义。电泳媒介微分析法（EMMA）和固定化酶微反应器（IMER）是毛细管电泳酶分析技术中常用的在线分析方法。这两种在线酶分析法的进样方式通常为流体动力学进样和电动进样,无法实现酶反应过程中的无干扰序列进样分析。近年来,基于快速序列进样的毛细管电泳序列分析技术已经发展成为在线酶分析的另一种强有力手段,以实现高时间分辨和高通量的酶分析在线检测。该文从快速序列进样的角度,综述了近年来毛细管电泳序列分析技术在线酶分析的研究进展,并着重介绍了各种序列进样方法及其在酶反应和酶抑制反应中的应用,包括光快门进样、流动门进样、毛细管对接的二维扩散进样、流动注射进样、液滴微流控进样等。     

应用响应曲面试验设计法研究克百威气相色谱测定中的色谱行为

应用响应曲面试验设计法研究了气相色谱不同的进样方式,包括常规分流不分流进样以及柱头进样对克百威色谱行为的影响。通过构建模型,对试验的影响因子包括进样口温度、初始柱温和栽气流速对克百威色谱行为的相对重要性进行了评价。并利用面积归一化方法,对进样口温度和初始柱温对克百成分解的影响进行了定量评价和探讨。结果表明：在常规进样方式中,进样口温度和初始柱温是影响克百威分解的主要因素。通过色谱条件的优化,解决了常规进样不能解决的克百威的热分解问题。     

Solid sampling analysis by means of autoprobe-GFAAS

Summary A recently developed solid sampling graphite system for automatic probe atomisation (SAP-GFAAS) was applied for the direct determination of Pb and Cd in untreated bovine liver matrix.The study was based on 30 livers with a low content of lead (0.045 to 0.27 g Pb/g fresh matter) and of cadmium (0.031–0.24 g Cd/g fresh matter). The basic comparative data for the evaluation of the SAP-GFAAS method were supplied by a standardized GFAAS method with preliminary sample homogenization and matrix decomposition. Additionally, data were obtained by two further solid sampling methods: a front entry graphite system with direct Zeeman effect background correction and a side entry graphite system with high-energy deuterium continuum background correction. The combination of the autoprobe technique and solid sampling was shown to provide analytical results — in terms of handling, accuracy and precision — comparable to those obtained by means of the conventional solid sampling systems. Differences between the results of the sample decomposition method and the solid sampling methods, as well as between the three solid sampling methods must be regarded as being of no practical significance. Part I: see [1].     

Determination of element concentrations in biological reference materials by solid sampling and other analytical methods

Summary Using solid sampling with graphite furnace atomic absorption spectrometry (GFAAS), values for cadmium, copper, lead and zinc in six biological reference materials were obtained from up to four laboratories participating in three collaborative studies. These results are compared with those obtained with other methods used in routine analysis from laboratories of official food control. Under certain conditions solid sampling with GFAAS seems to be suitable for routine analysis as well as conventional methods.     

固体分层取样方案的最优化设计

本文首次从理论上探讨了取得量对分层取样误差的影响,提出了总取样量一定时各层的最佳取样量和最小取样方差的计算公式,从而为分层取样的最佳取样方案设计提供了理论依据。     

Analytical quality control by solid sampling GFAAS in the production of animal tissue reference materials: lead and cadmium in bovine liver reference materials

Summary The function of solid sampling graphite furnace atomic absorption spectrometry (SS-GFAAS) in the laboratory-internal preparation, production and standardization of bovine liver reference material is described. Analytical quality assurance was achieved by using a wet digestion decomposition procedure and GFAAS (WD-GFAAS) as well as three different methods of SS-GFAAS. It will be shown, that SS-GFAAS is an adequate and efficacious method of analytical quality control in the production of reference materials. Details are given about the preliminary steps of sample selection and preparation, applying SS-GFAAS both as a screening method and for the detection of contamination during the production of the reference materials. The element contents of the four bovine liver materials measured after decomposition with nitric acid in the open system by GFAAS and also by Flame-AAS, using the slotted tube atom trap, are compared statistically with the results obtained by SS-GFAAS. In solid sampling analyses three different systems were applied: a solid sampling ZAA-spectrometer with platform-boat, a D₂AA-spectrometer with solid sampling graphite tube and platform-drawer and an autoprobe-D₂AA-spectrometer with solid sampling autoprobe and graphite tube.     

在线采样技术在中国的发展

在线采样技术能实时采样,满足在线监测的采样要求。按照采样进样介质的不同分为气体、液体、固体三类。对气体中有毒气体、大气颗粒物、VOCs,液体中水样、原油,固体中煤的机械化采样技术进行了概述,旨在帮助了解在线采样技术在国内矿业、环境行业的发展和应用。随着5G时代的到来,在线采样技术一定会发挥越来越重要的作用。     

Graphite furnace atomic absorption analysis of marine samples for trace metals

Trace element determinations by graphite furnace atomic absorption spectrometry which are pertinent to the analysis of marine samples are highlighted. Results for the direct introduction of solids, slurries and dissolved samples of fauna, sediments and saline waters are discussed. Examples drawn from recent literature show that typical samples which benefit most from direct solid sampling are those that do not require the very highest accuracy or precision. No clear consensus amongst users of this technique has emerged regarding the choice between peak height or area recording or the need to standardize by aqueous calibration, the method of additions or use of matrix matched solids. Slurry sampling overcomes several limitations associated with direct solid sampling and whereas generalizations serve little purpose in assessing the applicability of the direct solid sampling approach, slurry sampling holds great promise for widespread use. Examples of external and in situ concentration techniques necessary to augment the relative detection power of the system for the analysis of saline waters are also given. These include an examination of “classical” procedures utilizing chelation-solvent extraction, immobilized ligands and precipitation methods as well as techniques which rely on sequestration in the furnace of volatile analyte species generated in external cells.     

Solid sampling AAS methods in industrial product control

Summary The present-day capabilities of the solid sampling AAS are faced with the profile of requirements of the industrial practice on chemical trace analysis. It is shown that solid sampling AAS is a reasonable alternative to conventional techniques for a lot of types of analytical problems. A survey of solid sampling AAS applications in German industry up to 1986 is given and briefly discussed.

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M?glichkeiten der direkten Feststoff-AAS in der industriellen Produktionskontrolle

     

Evaluation of the solid sampling technique for the determination of aluminium in biological materials by atomic absorption and atomic emission spectrometry

Summary Results for the determination of aluminium in several biological materials by atomic absorption and atomic emission spectrometry using the solid sampling technique in connection with a constant temperature furnace are given. A comparison was made with a dissolution procedure and good agreement was generally obtained. With the solid sampling technique it was possible to calibrate against aqueous standards and to achieve a precision of better than 10% r.s.d. for NBS 1577a Bovine Liver and IAEA H-4 Animal Muscle, providing that the sample mass was greater than 1.3 mg and that the peak area was evaluated. Laboratory air and the solid sampling procedure were identified as possible sources of contamination.

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Auswertung der Feststofftechnik für die Bestimmung von Aluminium in biologischen Materialien durch AAS und AES

     

Experiments in solid sampling gas chromatography

The influence of probe material on the total evaporation time of compounds injected into the gas chromatograph by solid sampling has been investigated. A quartz needle was found to give the shortest evaporation time. The type of analysis will, however, to some extent determine the probe material to be chosen. A comparison of solid sampling with liquid sampling showed that the former has a higher degree of reproducibility.