电感耦合等离子体原子发射光谱法同时测定锑矿石中14种元素的含量

Simultaneous Determination of 14 Elements in Antimony Ores by Inductively Coupled Plasma-Atomic Emission Spectrometry

锑矿石样品(0.100 0g)加入盐酸-硝酸(3+1)混合酸5 mL,氢氟酸5 mL,高氯酸0.5mL和硫酸(1+1)溶液1mL的混酸体系,加热(200℃)分解,蒸发至近干时,冷却,加入盐酸-硝酸-水(3+1+4)混合酸10mL,加热至盐类完全溶解,冷却,用盐酸-硝酸-水(3+1+36)混合液稀释至50mL。此溶液可供电感耦合等离子体原子发射光谱法同时测定14种元素,并选择了合适的分析谱线。部分微量元素分析谱线的光谱干扰,运用背景扣除或干扰元素校正系数法等予以校准。测得各元素的检出限[3s×500(稀释因子)]为0.81~123μg·g-1。按上述方法测定CRM(GBW07174),其相对标准偏差(n=11)为0.51%~7.1%。

0. 1000 g of antimony ore sample was added an acid mixture composed of 5 mL of HCl-HNO3 （3＋ 1） mixed acid, 5 mL of HF, 0. 5 mL of HC104 and 1 mL of H2SO4 （1＋1） solution, and heated with the acid mixture （under 200 ℃）, and the solution obtained was evaporated to near dryness. After cooling, 10 mL of a mixed acid of HCl-HNO3-H2O （3 ＋ 1 ＋ 4） were added and heated to dissolve the salts completely. After cooling, the solution was diluted to 50 mL with an acid solution of HC1-HNO3-H2O （3＋ 1＋36）, and used for ICP-AES determination of 14 elements simultaneously. Analytical spectral lines were selected. Spectral interferences of several trace elements with the chose spectral lines, were overcome by background correction or correction coefficients. Values of detection limits （3s× 500, 500 is the dilution factor） found for the 14 elements were in the range of 0. 81-123 μg · g^-1. A CRM （GBW 07174） was analyzed by the proposed method, with values of RSDs （n = 11） ranged from 0.51% to 7.1%.