摘要
采用响应曲面优化-原子荧光光谱法(AFS)测定铅锌矿中微量汞。基于对AFS测汞时10项因素,即盐酸-硝酸(3+1)混合酸所需的体积、还原剂的质量浓度(ρ)、辅助气的流量、消解时间及温度、载流的体积分数(φ)、原子化器温度、光电倍增管的负高压、灯电流及载气流量的PlackettBurman试验设计,筛选出前3项为显著因素,并通过中心复合设计对此3项因素进行响应曲面法优化,从而得到上述3个因素的优化值依次为10mL,0.3g·L^(-1)和450mL·min^(-1)。汞的线性范围在10.00μg·L^(-1)以内。方法应用于3个国家标准物质(GBW 07165,GBW 07162,GBW 07163)的分析,测定值与认定值相符,测定值的相对标准偏差(n=6)在0.38%~5.5%之间。
AFS was applied to the determination of trace amount of Hg in lead-zinc ore by response camber optimization. Based on the designing by the Plackett-Burman testing of 10 factors in AFS of Hg, i. e. , volume of mixed acid of HCl-HNO3 （3 ＋ 1）, mass concentration （p） of reductant, flow-rate of auxiliary gas, time and temperature of digestion, volume fraction （φ） of carrying current, temperature of atomizer, negative high voltage of photomultiplier, lamp current and flow-rate of carrying gas, the first 3 factors were found to be the significant ones; giving their optimum values of 10 mL, 0.3 g · L-1 and 450 mL · min-1 repeetively found by optimization of the 3 factors through central composite designing. Linearity range of Hg was found in the range within 10. 00μg · L-1. The proposed method was applied to the analysis of 3 CRM＇s of GBW 07165, GBW 07162 and GBW 07163, giving results in consistency with the certified values and values of RSD＇s （n=6） found from the analytical results were in the range of 0. 38%--5.5%.
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2016年第8期922-927,共6页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
