Department of Chemistry, University of Jyväskylä, Finland.
Anal Chim Acta. 2011 Mar 18;689(2):178-83. doi: 10.1016/j.aca.2011.01.043. Epub 2011 Jan 26.
Hydride generation inductively coupled plasma optical emission spectrometry (HG-ICP-OES) was used in the determination of As and Sb concentrations in fly ash samples. The effect of sample pre-treatment reagents and measurement parameters used for hydride generation was evaluated. Due to memory effects observed, the appropriate read delay time was adjusted to 60s resulting in RSDs 0.6% and 2.3% for As and Sb, respectively. The most suitable volumes of pre-reduction reagents for 10 mL of sample were 4 mL of KI/ascorbic acid (5%) and 6 mL of HCl (conc.). The determination of Sb was significantly interfered by HF, but the interference could be eliminated by adding 2 mL of saturated boric acid and heating the samples to 60°C at least 45 min. The accuracy of the method was studied by analyses of SRM 1633b and two fly ash samples with the recovery test of added As and Sb. As high a recovery as 96% for SRM 1633b was reached for As using 193.696 nm with two-step ultrasound-assisted digestion. A recovery rate of 103% was obtained for Sb using 217.582 nm and the pre-reduction method with the addition of 2 mL of saturated boric acid and heating. The quantification limits for the determination of As and Sb in the fly ash samples using two-step ultrasound-assisted digestion followed with HG-ICP-OES were 0.89 and 1.37 mg kg(-1), respectively.
采用氢化物发生电感耦合等离子体原子发射光谱法（HG-ICP-OES）测定粉煤灰样品中的砷和锑浓度。评价了用于氢化物发生的样品预处理试剂和测量参数的影响。由于观察到记忆效应，适当调整了读取延迟时间为 60s，得到的砷和锑的相对标准偏差（RSD）分别为 0.6%和 2.3%。对于 10mL 样品，最适的预还原试剂体积分别为 4mL 的 KI/抗坏血酸（5%）和 6mL 的盐酸（浓）。HF 对 Sb 的测定有显著干扰，但通过添加 2mL 饱和硼酸并将样品加热至 60°C 至少 45min 可消除干扰。通过分析 SRM 1633b 和两个粉煤灰样品并进行砷和锑的加标回收试验，研究了该方法的准确性。采用两步超声辅助消解，在 193.696nm 处测定 SRM 1633b 中的砷，回收率高达 96%。采用添加 2mL 饱和硼酸和预还原方法，在 217.582nm 处测定 Sb 的回收率为 103%。采用两步超声辅助消解和 HG-ICP-OES 测定粉煤灰样品中砷和锑的定量限分别为 0.89 和 1.37mgkg-1。
