摘要
建立了以HG-AFS测定铅基合金样品中砷的简单方法,研究了共存元素可能引起的干扰并成功地加以解决,优化了氢化物发生条件及仪器的工作参数。KBH4最优浓度为1.0%(m/V),样品溶液和载流中HCl的最优浓度分别为10%(V/V)和5%(V/V)。实验表明,当硫脲存在时,Cu不干扰As的测定;Sb、Sn和Bi引起的干扰可以通过0.5%(m/V)KMnO4溶液在线吸收相应的氢化物加以消除。通过测定铅基合金标准样品以检验方法的准确性,由标准加入法得到的结果与标准值吻合。本方法的检出限为0.17μg/L,对40μg/LAs标准溶液连续测定11次的相对标准偏差为1.45%。
A simple method based on hydride generation (HG) -AFS for the determination of As in lead-based alloys was developed. Interferences caused by co-existing elements were investigated and minimized success- fully. The conditions for the hydride generation technique and instrumental parameters were also optimized. KBH4 concentration was fixed in 1.0% (m/V). Optimized HC1 concentration in the sample and carrier solu- tion was 10% (V/V) and 5% ( V/V), respectively. Experiments showed that no interference caused by Cu was observed when thiourea existed and interferences caused by Sb, Sn and Bi could be eliminated by absorbing their corresponding hydrides using 0.5% (m/V) KMnO4 solution on-line. Feasibility of this method was demonstrated by determination of two certified lead-based alloys, and the results obtained by standard addition agreed well with certified values. The method detection limit was 0.17 μg/L and RSD was 1.5% for 11 consecutive determinations of 40 μg/L As standard solution.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2007年第8期1183-1186,共4页
Chinese Journal of Analytical Chemistry
基金
国家自然科学基金(No20605021
2067705)资助
关键词
砷
铅基合金
氢化物发生
原子荧光
Arsenic, lead-based alloy, hydride generation, atomic fluorescence spectrometry