杨占菊,李颜君,隆英兰,韩俊丽，王景凤

(青海省高原矿物加工工程与综合利用重点实验室，西部矿业集团科技发展有限公司分析检测中心，西宁 810007）

氢化物发生-原子荧光光谱法同时测定锌锭中砷和锑

杨占菊,李颜君,隆英兰,韩俊丽，王景凤

(青海省高原矿物加工工程与综合利用重点实验室，西部矿业集团科技发展有限公司分析检测中心，西宁 810007）

建立用氢化物发生-原子荧光光度计同时测定锌锭样品中砷和锑含量的方法。采用硝酸一次溶样，加入酒石酸防止锑水解。加入硫脲-抗坏血酸混合溶液作为还原剂和掩蔽剂，消除干扰元素的影响，对实验条件进行了优化。砷和锑的负高压分别为220，200 V，灯电流分别为80，60 mA，还原剂为1%硼氢化钾溶液(含0.5% KOH)，载流为10%盐酸溶液，还原时间为30 min。测定砷的线性范围为0～80 ng/mL，相关系数r=0.999 8，检出限为0.35 μg/L，测定结果的相对标准偏差为3.18%(n=11)；测定锑的线性范围为0～80 ng/mL，相关系数r=0.999 6，检出限为0.42 μg/L，测定结果的相对标准偏差为4.32%(n=11)，砷和锑的加标回收率在97.46%～100.30%之间。用该方法对标准样品进行测定，测定结果与标准值相符。该方法基体干扰少，灵敏度高，适合于锌锭中砷和锑的日常测定。

锌锭；砷；锑；原子荧光光谱法

AbstractThe method for the simultaneous determination of arsenic and antimony in zinc ingot sample by hydride atomic fluorescence spectrophotometry was established. Nitric acid digestion was used， tartaric acid was added to prevent hydrolysis. Thiourea-ascorbic acid was used as reducing agent and masking agent to eliminate interference effects. Experimental conditions were optimized，arsenic and antimony negative high voltage were 220, 200 V,respectively, lamp current were 80, 60 mA, respectively, reducing agent was 1% potassium borohydride solution (include 0.5% KOH)，current carrying was 10% hydrochloric acid solution，and the reduction time was 30 min. The linear range of arsenic was 0-80 ng/mL with the correlation coef ficient (r) of 0.999 8，the detection limit was 0.35 μg/L，and the relative standard deviation was 3.18%(n=11). The linear range of antimony was 0-80 ng/mL with the correlation coef ficient (r)of 0.999 6，the detection limit was 0.42 μg/L， and the relative standard deviation was 4.32%(n=11).The standard addition recoveries of arsenic and antimony were in the range of 97.46%-100.30%. The method was used to determine the standard sample, the detection result was consistent with the standard value. This method has high sensitivity, less matrix interference, it is suitable for the routine determination of arsenic and antimony in zinc ingot sample.

Keywordszinc ingot; arsenic; antimony; atomic fluorescence spectrophotometry

锌锭作为重要的工业产品，主要用于压铸合金、电池业、印染业、医药业、橡胶业、化学工业等，锌与其它金属的合金在电镀、喷涂等行业得到广泛的应用，是镀锌工艺的重要原料，其杂质含量是确定产品质量的一项关键指标。而锌锭中砷和锑的含量会影响其性能，其中砷、锑的杂质含量对提高镀锌层的附着力以及提高镀锌板的性能起关键作用。……