Frequency-modulated simultaneous Atomic Absorption Spectrometry (FremsAAS): Determination of As, Se and Sb

The evaluation of accuracy and efficiency of the frequency-modulated simultaneous Atomic Absorption Spectrometry (FremsAAS) has been extended to an arrangement with EDL as light sources. Fundamental calibrations have been worked out for As, Se and Sb using a graphite furnace as well as hydride generation in combination with a heated quartz tube as atomization unit. The characteristic data are in good agreement with results obtained by conventional single-channel AAS instruments. Determinations in three standard reference materials with different complex matrices resulted in complete agreement with the certified values.     

Determination of As and Sb in Steels by Electrothermal Atomic Absorption Spectrometry after Reduction, Complexation and Sorption on Activated Carbon

 A method for the preconcentration and separation of As and Sb in steel sample solutions is proposed. The analytes are reduced to their trivalent oxidation states with a mixture of ascorbic acid and potassium iodide and complexed by the ammonium salt of dithiophosphoric acid O,O-diethyl ester. The complexes are sorbed onto carbon. After desorption in a small volume of nitric acid solution, As and Sb are determined by electrothermal atomic absorption spectrometry. Iron(III) is also reduced to Fe(II), which is not complexed and is about 99.9% eliminated by the preconcentration procedure. Enrichment factors of 5 and 10 were obtained for As and Sb, respectively. The method was applied to the analysis of four certified steel samples, after acid dissolution in a microwave system and good agreement was obtained with the certified values. Received May 4, 1998. Revision February 22, 1999.     

Iridium and Rhodium as Permanent Chemical Modifiers for the Determination of Ag, As, Bi, Cd, and Sb by Electrothermal Atomic Absorption Spectrometry

Performance of graphite platforms coated with Ir, Rh, and a mixture of both, as permanent modifiers for Ag, As, Bi, Cd, and Sb, was evaluated. The coating process is very simple: a solution containing Ir, Rh, or a mixture of both is pipetted on the platform inserted in a graphite tube, and this is submitted to a temperature program. High pyrolysis temperatures are allowed, especially for As and Bi, 1400°C, in the Ir + Rh-coated platform. The sensitivity remains about the same for all analytes with different coatings, except for As in the Ir-coated platform, for which a remarkable gain was obtained in comparison to the other coatings. The lifetimes of the treated tubes were in the range 50 to more than 1000 cycles, being especially long for Sb and Ag in the Rh-coated platform, more than 600 and 1000 cycles, respectively. The Rh coating could not be used for Bi and Cd. Analysis of a certified reference water and of acid oyster tissue digests showed the absence of interference and good precision. Advantages of the permanent coatings are the possibility of low blanks byin situcleaning of the modifier and shorter analysis time.     

在线双毛细管-氢化物火焰原子吸收光谱法测定砷、锑、铋、汞、硒和锡

1引言使用氢化物原子吸收光谱(HG-AAS)法测定As、Sb、B、iHg、Se和Sn已有报道。但将氢化物在线引入空气乙炔焰,用火焰法快速测定这些元素的方法少见报道。本实验利用双毛细管装置,建立了在线HG-AAS测定As、Sb、B、iHg、Se和Sn的方法,该方法具有简便、快速、灵敏度高,干扰少和KBH4用量少的优点。2实验部分2.1仪器及试剂GGX-9型原子吸收分光光度计;微型多功能进样装置(自制专利产品);空心阴极灯;盐酸(1 1);硫脲溶液(5%);抗坏血酸溶液(5%);KBH4溶液(1%,2%);邻二氮菲溶液(1%);As、Sb、B、iHg、Se、Sn的标准溶液;蒸馏水;其余试剂…     

氢化物原子荧光光谱法测定水中微量砷和硒

研究了氢化物发生-原子荧光光度法测定水中微量砷和硒的方法。结果表明,检出限:砷为0.0518μg/L,硒为0.0524μg/L;11次测定的相对标准偏差为0.36％～0.62％;标准回收率:砷为96.8％～100.9％;硒为95.9％～103.7％。方法简便、快速、灵敏,适于生活饮用水、地表水和水源水中微量砷、硒的同时测定。     

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。     

流动注射-氢化物发生原子吸收光谱法测定香烟接装纸中的痕量砷

将流动注射-氢化物发生和原子吸收光谱法有机的结合起来,探讨了流动注射-氢化物发生-原子吸收光谱法测定香烟接装纸中砷的最佳条件。样品经消解后,加入还原剂,使五价砷还原为三价,在盐酸介质中和硼氢化钾反应生成砷化氢,进入电热石英管原子化测定。检测结果相对标准偏差小于5%,加标回收率为96.7%~104%,方法检出限为0.18μg/L。     

原子吸收原子荧光和火焰光谱分析

原子吸收原子荧光和火焰光谱分析何华＊１９５８年中山大学物理系毕业，现任中国广州分析测试中心研究员。中国仪器仪表学会分析仪器学会理事。《分析测试学报》、《光谱学与光谱分析》、《分析仪器》以及《分析测试仪器通讯》等期刊编委。多年来主要从事原子光谱分析新...     

原子吸收,原子荧光和火焰光谱分析

本文根据1988～1990年国内主要分析刊物所发表的文章,以及第三届北京分析测试学术报告会及展览会(BCEIA)、中国化学会第三届原子光谱会的主要论文,对我国原子吸收、原子荧光和火焰光谱分析的进展进行了评述,对于国外有关的重要文章也简单地加以介绍。     

原子吸收和原子荧光光谱分析

本文是《分析试验室》期刊定期评述中关于原子吸收光谱(AAS)及原子荧光光谱(AFS)分析的第10篇综述文章。文中对2002年12月～2004年11月期间我国在AAS/AFS领域所取得的主要进展进行评述。内容包括概述、仪器装置与数据处理、火焰原子吸收光谱法、电热原子吸收光谱法、化学蒸气发生技术以及原子荧光光谱法等。收集文献511篇。     

原子吸收、原子荧光和火焰光谱分析

本文主要根据1991～1993年第一季度国内重要分析刊物所发表的文章以及在此期间重要全国性会议的主要论文,对我国原子吸收光谱法,原子荧光光谱法以及火焰发射光谱分析法的进展作一综述。文中共收集文献692篇。     

氢化物发生-原子荧光光谱法测定海洋沉积物中砷、锑、铋、汞、硒

提出了用盐酸-硝酸-水(3+1+4)混合酸消解样品,氢化物发生-原子荧光光谱法测定海洋沉积物样品中砷、锑、铋、汞、硒的方法。考察了原子荧光光谱仪的最佳工作条件。在最佳条件下砷、锑、铋、硒的检出限(3s/k)分别为0.018,0.004,0.001,0.003μg.g-1,汞的检出限(3s/k)为0.604ng.g-1。应用于3种海洋沉积物标准物质的测定,测定值与标准值吻合。     

氢化物生成原子荧光法快速测定锑精矿中的砷、汞、硒、铋和锡

锑精矿;砷;汞;硒;铋;锡;氢化物发生 原子荧光     

蒸气发生–原子荧光法连续测定化探样品中微量砷、锑、铋、汞、硒、碲

建立了连续测定化探样品中微量砷、锑、铋、汞、硒、碲的原子荧光光谱法。研究了酸度、KBH4溶液浓度、基体改进剂等条件对荧光强度的影响。在优化的实验条件下,砷、锑、铋、汞、硒、碲的检出限分别为0.011,0.006,0.020,0.002 5,0.005,0.002 mg/L,测定结果的相对标准偏差分别为1.30%,4.64%,3.76%,5.46%,2.04%,3.41%(n=11),准确度大于98%。该方法简便,成本低,检测结果准确,检出限、准确度及精密度均能达到行业规范要求,可用于化探样品中微量元素测试。     

电感耦合等离子体原子发射光谱法测定粗锑中的As、Bi、Cd、Cu、Fe、Pb和Se元素

通过样品处理、谱线选择、准确度和精密度测定、加标回收实验及与其他测定方法的比对实验,建立了电感耦合等离子体原子发射光谱法(ICP-AES)测定粗锑中As、Bi、Cd 、Cu、Fe、Pb、Se 7种元素的定量分析方法。实验结果表明,该方法准确度高,稳定可靠,相对标准偏差(RSD,n=6)均小于3%,方法的加标回收率在95~105%之间,分析结果与分光光度法、原子吸收光谱法(AAS)及原子荧光光谱法(AFS)分析结果相吻合,能够满足日常对粗锑中杂质元素含量测定的要求。     

间接原子吸收分光光度法测定锆

研究了空气－乙炔火焰原子吸收光谱法间接测定微量锆的方法,在弱酸性溶液中钢与Ｎ－亚硝基苯胲（铜铁试剂）形成１：２络合物可被氯仿定量萃取,Ｚ ｒ（Ⅳ）定量置换Ｎ－亚硝基苯胲钢中的铜,原子吸收光谱法测铜间接测锆,特征浓度为 ０．０７ × １０－６ ｇ／ｍＬ／１％,线性范围为 ０～５ｍｇ／Ｌ,方法简便、快速、灵敏度高,选择性好,用于瓷釉和α－βＡｌ２Ｏ３中氧化锆的测定,结果满意。     

原子吸收法间接测定微量锆

间接原子吸收光谱法的研究受到人们的普遍重视,主要有利用杂多酸的“化学放大”效应间接测定磷、砷、锗;沉淀反应间接测定氯离子、硫酸根,化学干扰效应间接测定钛、铝及络合效应间接测定钒、硼、硝酸根等,但在间接测锆方面未见报道,本文用Mg-8-羟基喹啉(MgL_2)沉淀锆置换出定量的镁,通过测镁间接测锆,建立了空气-乙炔火焰原子吸收光谱法间接测定锆的新体系,方法的特征浓度为0.018mg/L/1%,较氧化亚氮乙炔火焰(10mg/L/1%)提高500倍,该方法灵敏、快速、体系稳定,经萃取分离除去干扰元素,用于实际样品中氧化锆的测定,结果满意.2 实验部分     

Indirect Determination of Vanadium by Atomic Absorption Spectrometry

Abstract

An indirect atomic absorption spectrometric method for vanadium has been developed on the basis of heteropoly chemistry. Molybdovanadophosphoric acid is formed, extracted and stripped by a basic buffer solution. The resulting molybdate, which is equivalent to a specific amount of vanadium, is determined by atomic absorption spectrometry.     

对喷式氢化物发生原子荧光光谱法同时测定烟叶中痕量砷和锑

提出了一种提高氢化物生成效率的新方法——对喷式氢化物发生(HG)原子荧光光谱法(AFS),并同时测定烟叶中痕量砷和锑。样品和还原剂(KBH4)从相对的方向高速喷出在近雾化状态下发生反应生成氢化物。同常规HG-AFS相比,灵敏度提高了15倍。在最优的实验条件下,砷和锑的检出限分别为6.3ng/L和19.2ng/L;相对标准偏差(RSD)分别为3.2%和1.8%;线性范围为0.019~3.2μg/L(As)和0·058~9.6μg/L(Sb)。本方法成功地用于测定烟叶中痕量砷和锑,回收率为92%~106%。     

原子吸收光谱法测定痕量铕

探讨了痕量铕的富集、解吸条件及测定时的干扰情况.实验表明适量Fe²⁺的存在才能满足分析要求.利用浸钽液热解镀层石墨管和光温控制技术以保证方法的灵敏度和重现性.方法操作简便、结果准确,适合大批岩石、矿物中Eu₂O₃大于1×10^-5%的测定.