摘要
称取经冷冻粉碎的橡胶样品0.2g,用硝酸6mL和过氧化氢2mL在密闭的聚四氟乙烯(PTFE)消解罐中进行微波消解,所得溶液定容至50mL。分取此溶液5.00mL,加盐酸(5+95)溶液至10mL,用氢化物发生-原子荧光光谱法测定此溶液中的汞含量。经试验选定分析条件:1用0.5g·L-1硼氢化钾溶液(溶于2g·L-1氢氧化钠溶液中)作还原剂;2以盐酸(5+95)溶液作载流;3光电倍增管负高压为260V;4灯电流为15mA;5原子化器高度为10mm;6载气和屏蔽气流量依次为300,800mL·min-1。方法的检出限(3s/k)为3μg·L-1。用标准加入法做回收试验,测得平均回收率为95.7%,测定值的相对标准偏差(n=11)为4.3%。选取含汞高及低量的样品各1个,分别由10家实验室对所提出的方法做验证,结果较好。
The rubber sample was smashed with a frozen grinder,and a portion of 0.2g of sample was taken and digested with 6mL of HNO3 and 2mL of H2O2 in a closed PTFE digester.The solution obtained was made up to 50 mL,and an aliquot of 5.00 mL after diluting to 10 mL with HCl(5+95)was used for HG-AFS determination of its Hg-content.Analytical conditions were optimized as follows:1 0.5g·L-1 solution of KBH4 dissolved in2g·L-1 NaOH solution was used as reductant;2 HCl(5+95)solution was used as carrier;3 negative high voltage of photomultiplier:260V;4lamp current:15mA;5 height of atomizer:10mm;6flow-rate of carrier gas and shielding gas:300,800mL·min-1 respectively.Detection limit(3s/k)found was 3μg·L-1.Value of average recovery found by standard addition method was 95.7%,with RSD(n=11)of 4.3%.Accuracy and precision of this method were further verified by an inter laboratory program among 10 laboratories,and satisfactory results were obtained.
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2014年第12期1567-1570,共4页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
国家质量监督检验检疫总局科研制标项目(2009B661)
