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Improved determination of arsenic in environmental and geological specimens using HG-AFS

机译:使用HG-AFS改进了环境和地质样品中砷的测定

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A sensitive and robust analytical procedure for the determination of arsenic in plant, coal, and sediment samples using hydride generation-atomic. uorescence spectrometry (HG-AFS) has been developed. The optimised concentrations of NaBH4 and HCl required for arsine generation were 1% (m/v) and 4.5 M, respectively. Seven certified plant reference materials (CTA-OTL-1 Oriental Tobacco Leaves, CTA-VTL-2 Virginia Tobacco Leaves, GBW 07602 Bush Branches and Leaves, NIST 1547 Peach Leaves, NIST 1573a Tomato Leaves, NIST 1575 Pine Needles and NIST 1515 Apple Leaves), two certified coal reference materials (NIST 1632c Bituminous Coal and NIST 1635 Subbituminous Coal), and one marine sediment reference material ( GBW 07316 Marine Sediment) were analysed for quality control purposes. Sample digestion was carried out on 200 mg sample aliquots with 3 ml HNO3 and 0.1 ml HBF4, heated in a microwave autoclave up to a temperature of 240 degreesC. After digestion, no evaporation of HNO3 to remove acid from the digests is needed before arsine generation can be carried out. External standard solutions were matched for the HNO3 concentration in the analyte solutions (0.042 M HNO3). Potassium iodide was found to be the ideal reagent for the quantitative reduction of As( V) to As( III), in contrast to L-cysteine. The detection limit (3sigma) for As(III) was 6 ng l(-1), which is 1 - 2 orders of magnitude lower than that reported recently by other authors using HG-AFS. This sensitive, robust and low-cost analytical procedure will be applied to the determination of As in sediment samples to help understand the mechanisms of both natural and anthropogenic As accumulation in wetlands.
机译:使用氢化物​​发生原子法测定植物,煤和沉积物样品中的砷的灵敏而稳定的分析程序。荧光光谱法(HG-AFS)已开发。生成砷化氢所需的NaBH4和HCl的最佳浓度分别为1%(m / v)和4.5M。七种经过认证的植物参考材料(CTA-OTL-1东方烟叶,CTA-VTL-2弗吉尼亚烟叶,GBW 07602布什树枝和树叶,NIST 1547桃叶,NIST 1573a番茄叶,NIST 1575松针和NIST 1515苹果叶),为了质量控制目的,对两种认证的煤炭参考物质(NIST 1632c烟煤和NIST 1635亚烟煤)和一种海洋沉积物参考物质(GBW 07316海洋沉积物)进行了分析。样品消化是在200毫克样品等分试样中加入3毫升HNO3和0.1毫升HBF4进行的,然后在微波高压釜中加热到240摄氏度。消化后,无需进行HNO3蒸发即可从消化液中去除酸,然后才能进行砷化氢生成。使外标溶液与分析物溶液中的HNO3浓度匹配(0.042 M HNO3)。与L-半胱氨酸相比,碘化钾是将As(V)定量还原为As(III)的理想试剂。 As(III)的检出限(3sigma)为6 ng l(-1),比其他使用HG-AFS的作者最近报道的检出限低1-2个数量级。这种灵敏,可靠且低成本的分析方法将用于测定沉积物样品中的砷,以帮助了解湿地中自然和人为砷的积累机理。

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