电感耦合等离子体原子发射光谱法测定黑钨精矿中痕量硫磷

以过氧化钠为熔剂在高温下熔融矿样，用酒石酸提取，在最佳的实验条件下，选用紫外区的180．669 nm 和 178．221 nm 光谱线分别作为硫和磷的分析线，用电感耦合等离子体原子发射光谱法（ICP-AES）同时测定了黑钨精矿中硫和磷。为了避免在酸性条件下产生的大量钨酸沉淀对硫、磷的吸附，加入了酒石酸络合钨。钨、铁、硅、锰、钙产生的基体效应通过选择较低的观测高度和基体匹配的方法克服。硫、磷的检出限分别为0.007 0 mg/L和0.004 8 mg/L，线性范围均为0.01～100 μg/mL。建立的方法用于标准样品的测定，测定结果与认定值吻合。样品分析结果的相对标准偏差（RSD）为1.7%～2.8%。

Determination of trace sulfur and phosphorus in wolframite concentrate by inductively coupled plasma atomic emission spectrometry

Under the optical experiment conditions，the spectral line of 178.221nm and 180.669 nm in ultraviolet band were selected as analytical lines of sulfur and phosphorus respectively, and sulfur and phosphorus in wolframite concentrate were determined simultaneously by inductively coupled plasma atomic emission spectrometry with sodium peroside as flux for melting mining sample at high temperature and tartaric acid as extractant. Tartaric acid was added for the complexation of tungsten in order to avoid the adsorption of sulfur and phosphors by large amount of tungstic acid precipitates which generated in acid condition. The matrix effect produced by tungsten, iron, silicon, manganese and calcium were overcome by selection of relatively low observation height and matrix matching method. The detection limit of sulfur and phosphorous was 0.007 0 mg/L and 0.004 8 mg/L,respectively, and the linear range was the same as 0.01-100 μg/mL. The proposed method was applied for the determination of certified reference materials, and the determination results were consistent with the certified value. The relative standard deviations (RSDs) for sample analysis results were 1.7%-2.8%.