氢化物-原子荧光法测定锑精矿中痕量砷、汞的研究

Determination of Trace Arsenic and Mercury in Antimony Concentrates by Hydride Generation Atomic Fluorescence Spectrometry

研究了氢化物发生-原子荧光光谱测定锑精矿中痕量砷汞的分析方法，并对溶样方法及共存元素的干扰进行了研究。发现用王水溶解样品完全，砷汞溶出量最大；加入硫脲-抗坏血酸后，锑精矿中干扰元素的干扰基本消除；通过加入酒石酸抑制基体锑的水解，从而不需通过化学分离，直接测定锑精矿中的痕量砷汞，并用于实际样品的测定。方法的检出限分别为：砷0．220ng·mL^-1，汞0．002ng·mL^-1，相对标准偏差（RSD％n=11）分别为1．47％和0．52％，回收率分别为94．0％～103．0％和98．7％～102．8％。方法具有快速、准确、灵敏度高等优点。

A method for the determination of trace arsenic and mercury in antimony concentrates by hydride generation atomic fluorescence spectrometry was investigated. The method of dissolving sample and the effect of concomitant ion were studied. It was found that aqua regia can be used to dissolve the sample completely, with maximum quantities of dissolved arsenic and mercury. The interference of chemical elements in antimony concentrates was avoided by adding thiourea-Vc. The matrix of antimony was vaporized with tartaric acid during sample pre-treatment. Trace arsenic and mercury were determined in real samples. The detection limits of 0.220ng· mL^-1 and 0.002 ng· mL^-1 were obtained, the relative standard deviations（RSD%= 11） are 1.47% and 0.52%, and the recoveries are 94.0%-103.0%and 98.7%-102.8%for As and Hg respectively. This method has proved rapid, accurate and highly sensitive.