氢化物发生-原子吸收光谱法测定萤石粉中砷

提出了以氢化物发生-原子吸收光谱法测定萤石粉中砷的方法,研究了酸介质、还原剂、载气流量等因素对测定的影响,并选择出最佳工作条件.砷的检出限为0.052μg·g-1,线性范围为0.10～6.00 μg·L-1,回收率在90.0%～102.0%之间,相对标准偏差为9.8%.     

氢化物—原子荧光光光谱法同时测定黄铜中的砷与锑

试样用硝酸－硫酸分解,试验了酸度、还原剂浓度以及黄铜中常见元素对测定结果的影响,砷、锑的回收率分别为：９６％～１０９％,９０％～９３％,砷、１锑的检出限分别为０．１９ｎｇ＝ｍＬ、０．３１ｎｇ＝ｍＬ,砷、锑的线性范围分别为０．５～２５０ｎｇ／ｍＬ、０．５～５００ｎｇ／ｍＬ。本法用于黄铜标准样品中的砷、锑。结果与标准值吻合。     

氢化物发生－缝管原子捕集－原子吸收法测定钢铁和地质试样中的砷

介绍简易的氢化物发生原子吸收测砷的方法。喷雾器负压将ＫＢＨ_４吸入反应器，并将生成的ＡｓＨ_３吸入乙炔－空气焰原子化。石英缝管使灵敏度提高３．５倍。方法的检测限（３σ）为１．８ｎｇ／ｍＬ（５ｍＬ试样）。２０ｎｇ／ｍＬＡｓ（Ⅲ）标准液１０次测定的ＲＳＤ为３．８％。本法成功地应用于钢铁和地质标样中微量砷的测定。     

Advances in On-Line Hydride Generation Atomic Spectrometric Determination of Arsenic

Flow analysis has played a major role in many areas of chemical analysis, making operations more robust and precise. It facilitates experimental studies opening new areas of research. In the field of arsenic research, there are various examples of surveys concerning arsenic determination and its species with the use of flow injection analysis (FIA) and sequential injection analysis (SIA). The increasing concern over the human exposure to arsenic and its species has necessitated the development of rapid, highly sensitive, precise, and accurate analytical methods for its determination in trace levels in environmental and biological samples. This review provides a literature survey on the automatic on-line hydride generation methodologies coupled to atomic spectrometry for determination of inorganic and organic arsenic species, during the last decades. All advances in on-line manifolds are categorized and highlighted. There are several reports of manifolds and setup instrumentation concerning hydride generation including continuous flow analysis (CFA), FIA, SIA, lab-on-valve (LOV), multicommutation flow systems, and hyphenated techniques. On-line preconcentration and pretreatment methodologies coupled with hydride generation such as solid phase extraction, co-precipitation and trapping are also discussed, as they are of particular interest in the development of fully automated methods.     

Determination of Inorganic and Total Arsenic in Wines by Hydride Generation Atomic Absorption Spectrometry

A method is described for the determination of inorganic arsenic species and total arsenic in wines by means of hydride generation atomic absorption spectrometry (HGAAS). Simple ethanol evaporation is the only pretreatment procedure proposed for wine samples prior to direct measurement of inorganic arsenic (AsIII) and As(V) species by HGAAS. The total arsenic content is determined after microwave digestion of the wine samples. The optimal parameters for the microwave digestion procedure and the next HGAAS measurement of arsenic are established. The detection limits achieved are 0.1µgL^–1 for inorganic and total arsenic determination. The relative standard deviation for both procedures and for ten independent determinations varied between 8 and 15% for arsenic species in the range of 1–30µgL^–1. The accuracy of the procedure for total arsenic determination was proved by comparative analysis using electrothermal atomic absorption spectrometry.     

Single Laboratory Validation of a Method for the Determination of Total Inorganic Arsenic by Hydride Generation Atomic Absorption Spectrometry

The purpose of this study consists in reporting of single laboratory validation of a method for the determination of total inorganic arsenic by hydride generation atomic absorption spectrometry from natural and residual water samples. Applicability, fitness for purpose, selectivity, and sensitivity were discussed. A calibration study was realized, linear working range (0.4–4 μg·L^?1), detection (0.11 μg·L^?1), and quantification (0.38 μg·L^?1) limits being determined. It was also proven that the method is accurate and precise. Following the bottom-up approach measurement, uncertainty was estimated (method validation data were used).     

Hydride Generation Atomic Fluorescence Spectrometric Determination of Ultratrace Arsenic in High Purity Indium Oxide

A simple, sensitive, and interference free method was proposed for the determination of total arsenic in high purity indium oxide by hydride generation atomic fluorescence spectrometry (HG-AFS). Preconcentration was carried out by distillation of volatile arsenic trichloride. Hydrazine sulfate was used as a prereductant to reduce As (V) to As (III). The volatile arsenic trichloride generation was based on the reaction between As (III) and hydrochloric acid, and vapors were absorbed with water. The method provides a linear response range of 2 ng/mL–70 ng/mL, a detection limit of 0.1 ng/mL, a recovery of 96%–113%, and an average relative standard deviation of 2.42%. The method was validated by means of interlaboratory comparative analysis with the proposed method HG-AFS, and the comparison of data by using proposed method HG-AFS and reference methods of ICP-OES and spectrophotometry.     

流动注射分光光度法测定砷的研究

本文采用自行设计制造的氢化物发生及吸收装置,将流动注射技术同氢化物发生分光光度法结合在一起,设计了一种不使用载气的流动注射分析系统并对该系统的测定条件进行了实验研究,实验用HNO_3-AgNO_3-聚乙烯醇-乙醇混合液作吸收液,结果证明该系统具有操作简便,成本低廉,分析速度快(30次/小时),灵敏度高,重现性好及线性范围可调的优点。     

氢化物发生ICP-AES测定各种形态砷

本文研究了用萃取分离环境样品中的有机砷和无机砷,用氢化物发生ICP-AES法测定的方法。As(Ⅲ)、As(Ⅴ)、DMA、MMA检测限在0.6～0.8ppb之间。各形态砷的浓度在1ppb～10ppm之间时工作曲线呈良好线性关系,相对标准偏差为1.4～2.2%。     

顺序注射-氢化物发生原子吸收法测定砷

通过在气液分离器的液体出口处增置微型电磁阀,延长样品和还原剂NaBH4在气液分离器中的反应时间,实现了单注射泵顺序注射-氢化物发生原子吸收法测定砷。本法自动化程度高,分析速度112次／h,样品消耗量为0．4mL;4μg/L As测定10次的相对标准偏差为2．0％;检出限0．09μg/L。用于标样中砷的测定,结果满意。     

氢化物原子荧光光谱法测定虾中砷和汞

建立了氢化物原子荧光法同时测定虾中砷和汞的方法。研究了样品前处理及实验条件对测定砷、汞的原子荧光强度的影响，并探讨了共存离子对测定砷、汞的干扰和消除的方法。本方法具有操作简便、快速、灵敏度高等优点，砷和汞的检出限分别为0．026μg/L和0．020μg／L；相对标准偏差分别为1．7％～9．4％和1．2％～9．4％；回收率为98％～106％。     

氢化物-原子荧光法测定粮食中的砷

研究了氢化物－原子荧光法测定粮食中砷的适宜条件,试验了酸介质和还原剂的用量对测定砷的影响,选择了仪器的最佳工作条件及氢化物发生条件,试验了生成氢化物元素及粮食中常见元素对测定的干扰情况。在测定条件下,砷的线性范围为０～８０μｇ／Ｌ,检出限为０．３μｇ／Ｌ。用该法测定了标准物质小麦粉及大米,结果与推荐值吻合。方法快速、准确,应用于进口粮食中砷的检测,获得满意结果     

Effect of the Mineralization Method on Arsenic Determination in Marine Organisms by Hydride Generation Atomic Fluorescence Spectroscopy

The efficiency of several mineralization methods for As determination in marine organisms has been evaluated. Wet mineralization in closed reactors at 150°C with acids (HNO₃/HClO₄/H₂SO₄) and K₂S₂O₈ and microwave-assisted digestion with HNO₃/H₂O₂ or with HNO₃/H₂O₂/HCl does not quantitatively destroy the organic matter of fish. This was ascertained by comparing the As content obtained by HG-AFS with that obtained by ICP-MS. Dry-ashing destroys organic As species and the resulting As recovery when HG-AFS is applied is similar to that obtained by ICP-MS. Similar arsenic contents were obtained for all the mineralization methods tested when arsenic was analysed by ICP-MS. These results indicate that when HG-AFS is applied for arsenic determination, the organic matter should be completely oxidised (e.g. by UV photo-oxidation and K₂S₂O₈) to transform organic arsenic compounds into those able to generate hydrides. The results have been validated with a fish candidate reference material (CRM) (EU SEAS plaice) with a known content of total arsenic. Arsenic speciation after 1:1 methanol-water extraction (which provides quantitative arsenic recovery after two consecutive extractions) by HPLC-ICP-MS shows that cuttlefish only contains arsenobetaine, which explains the difficulty of mineralization.     

氢化物发生原子荧光光谱法测定临床样品微量砷和硒

研究了氢化物原子荧光法测定临床床样品全血，血清，胎盘，头发，指甲和尿液中微量Ａｓ和Ｓｅ的方法。线性范围为Ａｓ１．３＊１０＾－９－２．５＊１０＾－７ｇ／ｍＬ，Ｓｅ２．８＊１０＾１０－７．５＊１０＾－８ｇ／ｍＬ；相对标准偏差（ｎ＝１３）Ａｓ２．６－３．６％，Ｓｅ２．８－４．２％；Ａｓ、Ｓｅ的标准加入回收率为９６．７－１０４．２％，用于６种临床样品中Ａｓ、Ｓｅ测定，获得满意的结果。     

Determination of Phosphorus by Inductively Coupled Plasma Atomic Emission Spectroscopy after Hydride Generation

Thehydridegenerationtechniquehascontributedmuchtotheimprovementofthesensitivityinatomicabsorption,emissionandfluorescencespectroscopyofAs.Sb.Bi.Se.Te.Ge.SnandPh"=.ManyworkershavesuccessfullyappliedthistechniquetodeterminationofCu.Zn.Cd3'4'5.KazukoMatsumotostudiedphosphinegenerationcoupledwithICPatomicemissionspectrometry,wherephosphateinaqueoussolutionwasfirstprecipitatedbyaddingCaCI,ascalciumphosphate,whichwasthenreducedtoCa,P,byheating(ca,1100'C)togetherwithaluminumpowder'.Thedetecti…     

流通式电化学氢化物发生法原子吸收测定硒的研究

采用自行研制的以铅作阴极、石墨作阳极无隔膜分隔的流通式电化学氢化物发生器,电解产生的气体经气液分离器后直接送入火焰原子吸收进行测定,因无外加载气减少了稀释提高了灵敏度。研究了各种影响因素,选择了最佳条件,以0．5mol／L硫酸作电解液,以1．3mL／min流速通过氢化物发生器,电解电流为2．0A。结果表明硒质量浓度在0～5μg／mL范围内呈良好的线性关系,其相关系数为0．9988,相对标准偏差为4．4％,特征质量浓度为0．0397μg／mL,检出限为0．084μg／mL。     

氢化物发生-分光光度法连续测定砷和铅

本文提出了以氢化物与硝酸银反应为基础的在一份试样溶液中连续测定微量砷和铅的分光光度法。利用硝酸银-聚乙烯醇-乙醇溶液吸收砷化氢显色测定砷,硝酸银-明胶-乙醇溶液吸收铅化氢显色测定铅。方法灵敏快速,通过稀释有色吸收液可测定砷与铅含量相差较大的样品。应用于沉积物和土壤中砷和铅的分析,获得满意的结果。     

连续氢化物发生—微波等离子体炬原子发射光谱法测定砷

对连续氢化物发生－微波等离子炬原子履地测定砷进行了研究，对这一方法的分析性能考察结果表明，本法对砷的检出限（３σ）ｎｇ／ｍＬ线性范围达三个数量级，大多数共存离子的干扰很小，对实际样品是一种简便、快速、准确的分析方法。     

连续流动氢化物发生—原子吸收光谱法测定地质样品中痕量硒

经试验研究，选定了分析地质样品中痕量硒的测定体系，建立了切实可行的分析方法，该方法不需分离，直接测定，灵敏度高，干扰少，方法测定下限可达０．０２μｇ／ｇ，进行了部分样样分析，结果令人满意。     

氢化物发生-冷阱捕获-色谱分离-原子吸收法测定天然水中砷的形态

研究建立了氢化物发生－冷阱捕获－色谱分离－原子吸收方法测定天然水中四种主要砷形态。测试系统自行组装，色谱住填料采用ChromosorbGAW－DMCS（粒径0．3～0．45mm），其上涂布3％OV－101。方法的检出限以砷计分别为：As（V）0．51ng，As（Ⅲ）0．43ng，MMA0．38ng，DMA067ng；12ng砷标准偏差As（Ⅴ）4．21％，As（Ⅲ）3．56％，MMA3．23％，DMA5．46％。在0～50ng砷量范围标准曲线线性关系良好。该法适用性广，已用于湖水、河水、海水和地下水等不同水样神形态测定，加标回收率93．5％～104．9％。给出了上述水样四种砷形态的分析结果。