Determination of bismuth in atmospheric particulate matter by hydride generation and atomic absorption spectrometry

The particulates are collected on Whatman 41 cellulose filters and decomposed with sulfuric acid and hydrogen peroxide; bismuth is then measured by hydride generation/atomic absorption spectrometry. The detection limis is 0.08 ng m^?3 if 500 m³ of air is filtered through an 11-cm filter. Generally, the precision is better than 10%. The concentrations found in Ghent, Belgium varied between 0.1 and 0.8 ng m^?3. Bismuth was also determined in NBS Orchard leaves (SRM 1571); a value of 98.5 ± 15 ng g^?1 was found.     

Ultratrace determination of tin by hydride generation in-atomizer trapping atomic absorption spectrometry

A quartz multiatomizer with its inlet arm modified to serve as a trap (trap-and-atomizer device) was employed to trap tin hydride and subsequently to volatilize collected analyte species with atomic absorption spectrometric detection. Generation, atomization and preconcentration conditions were optimized and analytical figures of merit of both on-line atomization as well as preconcentration modes were quantified. Preconcentration efficiency of 95 ± 5% was found. The detection limits reached were 0.029 and 0.14 ng mL⁻¹ Sn, respectively, for 120 s preconcentration period and on-line atomization mode without any preconcentration. The interference extent of other hydride forming elements (As, Se, Sb and Bi) on tin determination was found negligible in both modes of operation. The applicability of the developed preconcentration method was verified by Sn determination in a certified reference material as well as by analysis of real samples.     

氢化物发生原子吸收法测定卡托普利

根据卡托普利与醋酸铅反应定量生成沉淀的特点 ,通过用氢化物发生原子吸收法测定沉淀中的铅 ,可间接测定卡托普利的含量。平均回收率 99.8% ,RSD值为 1 .6%     

Determination of serum selenium by hydride generation flame atomic absorption spectrometry

Serum is rapidly digested with a mixture of nitric and perchloric acids at a temperature of 180 +/- 10 degrees C, and hydrochloric acid is used to reduce selenium(VI) to selenium(IV). Selenium is determined by hydride generation flame atomic absorption spectrometry. The results show that this method has the advantages of being sensitive, accurate, rapid and simple. After the serum is digested and diluted, 4.0 ml is taken for the determination. The characteristic concentration, detection limit, variation coefficient, recovery rate and linear range are 2.93 mug 1(-1), 1.55 mug l(-1), 1.6-5.0%, 97.3-99.2% and 0.0-320.0 mug l(-1) respectively. Serum at 4 degrees C and in frozen state can be preserved for at least 7 and 14 days, respectively.     

Determination of selenium in fish flesh by hydride generation atomic absorption spectrometry

Selenium was determined in freeze-dried fish flesh from perch, pike-perch and the fish flesh reference materials MA-A-2 No. 1174 and MA-B-3 No. 151 (both from the International Atomic Energy Agency) by hydride generation atomic absorption spectrometry. Four different decomposition procedures were tested. They yielded consistent results for the four specimens, but the certified concentration level of selenium in the reference material MA-A-2 was not reached. This indicated losses or the presence of very stable selenium-containing compounds in this fish flesh. Neutron activation analysis of the reference material, however, was in agreement with those results obtained.     

氢化物-原子吸收光谱法测定冶金企业废水中的砷

采用HNO3/HClO4(体积比10∶1)消解冶金废水样品,经6mol.L-1 HCl溶液酸化后,加入碘化钾(3%)、抗坏血酸(1%)及硫脲(1%)混合溶液进行还原,用氢化物-原子吸收光谱法(HG-AAS)测定了样品中的As含量.结果表明,该方法的检出限为0.297μg/L,相对标准偏差RSD为5.463%,样品加标回收率为93%～108%;其操作方便、选择性好、灵敏度高、干扰少,适合于复杂废水中微量和痕量As的测定.     

Determination of lead in wines by hydride generation atomic absorption spectrometry.

The optimization of lead hydride generation in aqueous ethanolic media and the influence on its generation of the wine components, both white and red, have been studied. These interferences were overcome by careful control of the parameters affecting hydride generation and the procedure was applied to the determination of Pb in wines. The method is fast, accurate and sensitive and can be used to quantify 24 ppb of Pb in wines.     

氢化物-原子荧光光谱法测定大气沉降物中砷含量

大气沉降物中砷的测定传统方法干扰多,本文针对大气沉降物样品的复杂性,在样品中加入盐酸、硝酸、高氯酸于电热板上加热消解,能有效的消除大量有机质对测量结果的干扰,为大气沉降物研究工作提供更为精准的检测数据。该方法能有效的消除基体干扰,分析成本低,测定的精密度高、准确性好,相对标准偏差(RSD)低于2.0%,样品加标回收率高于90%。     

Determination of tin and methyltin species by hydride generation and detection with graphite-furnace atomic absorption or flame emission spectrometry

A method for the determination of tin and organotin species by hydride generation is described. Tin hydrides are detected by graphite-furnace atomic absorption, quartz-cuvette atomic absorption, or flame emission spectrometry with detection limits of 50, 50, and 20 pg as tin, respectively. Germanium interferences are eliminated with a dual-detector flame photometer with an electronic cancellation circuit.     

Determination of antimony in wine by hydride generation graphite furnace atomic absorption spectrometry

 A method was developed for the determination of Sb in wine by electrothermal atomic absorption spectrometry, based on preconcentration by hydride generation with collection directly in the graphite furnace. Thiourea was added for prereduction of Sb(V) to Sb(III). The hydride was directly generated from diluted wine. Palladium was used as modifier in the collection step; the overall efficiency of the hydride/trapping system was found to be 67%. Sb was determined in several samples of red wine; the concentrations found were in the range 0.6 to 5.7 μg/L Sb. The detection limit of the method was 39 pg Sb, corresponding to 0.13 μg/L Sb in wine when 0.3 mL wine was analyzed. Received: 3 November 1995/Revised: 22 February 1996/Accepted: 24 February 1996     

Determination of antimony in wine by hydride generation graphite furnace atomic absorption spectrometry

 A method was developed for the determination of Sb in wine by electrothermal atomic absorption spectrometry, based on preconcentration by hydride generation with collection directly in the graphite furnace. Thiourea was added for prereduction of Sb(V) to Sb(III). The hydride was directly generated from diluted wine. Palladium was used as modifier in the collection step; the overall efficiency of the hydride/trapping system was found to be 67%. Sb was determined in several samples of red wine; the concentrations found were in the range 0.6 to 5.7 μg/L Sb. The detection limit of the method was 39 pg Sb, corresponding to 0.13 μg/L Sb in wine when 0.3 mL wine was analyzed. Received: 3 November 1995/Revised: 22 February 1996/Accepted: 24 February 1996     

Determination of trace arsenic in hydrofluoric acid by hydride generation and atomic absorption spectrometry

Practical procedures are given for determination of arsenic(III) and (V) in hydrofluoric acid by means of hydride generation and atomic absorption spectrometry. Arsenic(III) can be determined by direct generation of arsine with sodium borohydride in hydrochloric/hydrofluoric acid medium, arsenic(V) being only slightly reduced under the conditions used. For its determination, arsenic(V) has to be prereduced with potassium iodide, and even then its reduction to arsenic(III) and then arsine is far from complete. It is possible to determine it in presence of arsenic(III) by a difference method, but this is recommended only if the As(V)/As(III) ratio is greater than 1. Total arsenic can be determined after oxidation of As(III) and evaporation of most of the hydrofluoric acid. The limit of determination is 5 g/l for arsenic(III) and 0.25 g/l for total arsenic; the relative standard deviation is about 10%.     

Determination of antimony in steel by hydride generation and by electrothermal zeeman atomic absorption spectrometry

Procedures are described for the determination of antimony in steel. Samples by decomposed with a nitric/perchloric acid mixture and antimony is determined either by a.a.s. after hydride generation with sodium tetrahydroborate or by graphite-furnace a.a.s. with Zeeman background correction. Some reference steel samples were analyzed by both methods and by instrumental neutron activation. The results obtained (45–680 μg g^?1 antimony) were in very good agreement; detection limits were about 3 μg g^?1. The relative standard deviation for samples with > 50 μg g^?1 antimony was 〈 5%.     

Determination of arsenic by hydride generation with a long absorption cell for atomic absorption spectrometry

A method is described for the determination of arsenic involving hydride generation and atomic absorption spectrometry with an improved long graphite-tube furnace capable of considerably higher temperatures than the conventional quartz-tube heaters. Arsine is generated with sodium tetrahydroborate, held in a nitrogen-cooled trap and then swept with helium into an alumina tube (19 cm long) placed within the graphite furnace. The optimum conditions for determination of arsenic are given. The detection limit is 0.2 ng ml^?1 with RSD of 2–3%. Results for various NBS Standard Reference Materials agreed well with expected values and were as follows: orchard leaves, 10 ± 1 μg g^?1; tomato leaves, 0.28 ± 0.03 μg g^?1; bovine liver, 0.046 ± 0.005 μg g^?1.     

Determination and interference studies of bismuth by tungsten trap hydride generation atomic absorption spectrometry

The determination of bismuth requires sufficiently sensitive procedures for detection at the μg L⁻¹ level or lower. W-coil was used for on-line trapping of volatile bismuth species using HGAAS (hydride generation atomic absorption spectrometry); atom trapping using a W-coil consists of three steps. Initially BiH₃ gas is formed by hydride generation procedure. The analyte species in vapor form are transported through the W-coil trap held at 289 °C where trapping takes place. Following the preconcentration step, the W-coil is heated to 1348 °C; analyte species are released and transported to flame-heated quartz atom cell where the atomic signal is formed. In our study, interferences have been investigated in detail during Bi determination by hydride generation, both with and without trap in the same HGAAS system. Interferent/analyte (mass/mass) ratio was kept at 1, 10 and 100. Experiments were designed for carrier solutions having 1.0 M HNO₃. Interferents such as Fe, Mn, Zn, Ni, Cu, As, Se, Cd, Pb, Au, Na, Mg, Ca, chloride, sulfate and phosphate were examined. The calibration plot for an 8.0 mL sampling volume was linear between 0.10 μg L⁻¹ and 10.0 μg L⁻¹ of Bi. The detection limit (3 s/m) was 25 ng L⁻¹. The enhancement factor for the characteristic concentration (C_o) was found to be 21 when compared with the regular system without trap, by using peak height values. The validation of the procedure was performed by the analysis of the certified water reference material and the result was found to be in good agreement with the certified values at the 95% confidence level.     

微型氢化物发生-原子吸收光谱法测定纺织品中的痕量砷和锑

采用三毛细管微型在线氢化发生技术和装置, 建立了氢化物发生-电热石英管原子吸收法测定纺织品中痕量As、 Sb的分析方法. 研究了共存离子对As、 Sb检测的干扰及消除方法. 结果表明: 该方法除Co、 Sn对As和Ni对Sb有干扰外, 其它干扰元素允许量都较大. 采用酒石酸和KI混合掩蔽剂可抑制Co、 Sn对As和Ni对 Sb的干扰. As和Sb的检出限分别为0.7和0.4 ng/L, 已用于测定纺织品中痕量As和Sb的分析.     

Determination of bismuth in geological materials by automated hydride generation and electrothermal atomic absorption spectrometry

The rapid and precise determination of bismuth (>5 μg kg^?1 in geological materials is described. The sample is decomposed with a HClO₄/HNO₃/HF mixture; interferences are eliminated by addition of aluminium chloride, ascorbic acid and thiourea. Bismuth hydride is introduced into a quartz cell atomizer.     

Determination of selenium in sediments by hydride generation atomic absorption spectrometry. Elimination of interferences

Summary The hydride generation/atomic absorption spectrometry (AAS) with an automated flow system is useful for the routine analysis of selenium in environmental samples. This method is, however, subject to interferences from transition metal ions and other hydride forming ions. The conditions to minimize the interferences were established: the concentration of hydrochloric acid 6 mol/l; the concentration of tetrahydroborate 0.5%. Iron(III) chloride released the depression of selenium signals by metal ions such as copper(II) and bismuth(III). Selenium in several standard reference materials including sediment samples was determined by the present method and by fluorimetry with 2,3-diaminonaphthalene. The results obtained by the two methods agreed with an acceptable precision. This means that hydride generation/AAS offers good precision and accuracy in the determination of selenium in sediment samples as well as DAN fluorimetry. However, the former is much simpler in operation. The method was applied to the determination of selenium in estuarine sediments collected in Nagoya harbor and Ise Bay. The results can be used to assess the pollution state of these places.

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Selenbestimmung in Sedimenten durch AAS mit Hydriderzeugung. Eliminierung von Störungen

     

Determination of arsenic in sea water by sorbent extraction with hydride generation atomic absorption spectrometry

A rapid and sensitive sorbent extraction hydride generation-flow injection analysis atomic absorption spectrometric (HG-FIAS-AAS) method is described for the determination of As(III) and As(V) based upon online preconcentration on a microcolumn packed with activated alumina. In the present procedure these arsenicals are complexed with quinolin-8-ol-5-sulphonic acid from neutral solutions in the flow injection system and adsorbed on the column. The preconcentrated species are eluted with 10% HCl, mixed with 0.5% sodium borohydride and carried to the HG-FIAS cell with a carrier gas flow rate of 75 ml min(-1). The retention efficiency is found to be better than 98% with sensitivity enhancement of 12 and 10 for As(III) and As(V), respectively, for a 20 s preconcentration period. The respective detection limits are 0.05 and 2 ng ml(-1) for As(III) and As(V). The throughput of the samples is found to be 60 h(-1), with a loading time of 20 s. The method has been applied to sea water samples.