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Simultaneous determination of arsenic(III) and arsenic(V) by flow injection-inductively coupled plasma-atomic emission spectrometry (ICP-AES) with ultrasonic nebulization

机译:流动注射-电感耦合等离子体原子发射光谱法(ICP-AES)超声雾化同时测定砷(III)和砷(V)

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摘要

A dual-column protocol for the sequential determination of As(III) and As(V) is described using inductively coupled plasma-atomic emission spectrometry (ICP-AES) with ultrasonic nebulization (USN). This procedure employed a 16-way valve containing two different homenmade mini columns for selective preconcentration of As(III) and As(V). One column was filled with Muromac A-1, which selectively preconcentrated As(III) at pH 3 after complexation with ammonium pyrrolidine dithiocarbamate (APDC, 0.05%). The effluent of the first column was then passed through the second column, which was filled with an anion-exchange resin to collect As(V). By using 0.6 M sodium hydroxide, both species were eluted sequentially and measured by ICP-AES. Enrichment factors of 136 (17 for micro column *8 for USN) for As(V) and 160 (20 for micro column *8 for USN) for As(III) were achieved with 4 min preconcentration. With the proposed procedure, the detection limits were calculated to be 0.7 μg L~(-1) for As(V) and 0.8 μg L~(-1) for As(III) based on (3σ) blank determination (N = 10). The relative standard deviations for 20 μg L~(-1) of As(V) and As(III) were 5.8% and 6.5%, respectively. The recovery for spiked water samples was in the range of 85-112%.
机译:使用感应耦合等离子体原子发射光谱法(ICP-AES)和超声雾化(USN),描述了用于顺序测定As(III)和As(V)的双柱协议。该程序使用了一个16通阀,该阀包含两个不同的国产微型柱,用于选择性预浓缩As(III)和As(V)。一根色谱柱装有Muromac A-1,它与吡咯烷二硫代氨基甲酸铵(APDC,0.05%)络合后,在pH 3时选择性地预浓缩了As(III)。然后使第一塔的流出物通过第二塔,该第二塔填充有阴离子交换树脂以收集As(V)。通过使用0.6 M氢氧化钠,将两种物质依次洗脱并通过ICP-AES测定。在进行4分钟的预浓缩后,As(V)的富集系数为136(对于USN,微柱为* 8 * 17),对于As(III)为160(对于USN的微柱为* 8 * 20)。根据建议的方法,基于(3σ)空白测定(N = 10),计算出As(V)的检出限为0.7μgL〜(-1),As(III)的检出限为0.8μgL〜(-1) )。 20μgL〜(-1)的As(V)和As(III)的相对标准偏差分别为5.8%和6.5%。加标水样的回收率在85-112%的范围内。

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