电感耦合等离子体原子发射光谱法测定滑石粉中酸溶金属元素铬锰锌铜

Inductively coupled plasma atomic emission spectrometric determination of acid-soluble metal elements chromium,manganese,zinc and copper in talcum powder

以王水作溶剂,微波消解法消解样品,选择267.7、257.6、213.8和324.7nm波长的光谱线分别作为铬、锰、锌和铜的分析线,在发射功率为1 250W、辅助气流量为0.60L/min、雾化器压力为26psi的优化条件下以电感耦合等离子体原子发射光谱法(ICP-AES)测定了滑石粉中酸溶金属元素铬、锰、锌、铜含量。样品中的基体组分硅酸镁在王水中的溶解量很少,对测定没有影响。当测定待测元素浓度均为2.0μg/mL的溶液时,20.0μg/mL的铁、镁、钙、铝、锌、镍、铜对待测元素的干扰均小于5%。由于滑石粉中这些元素含量小于1%,因此它们对测定的影响可以忽略。铬、锰、锌、铜的检出限分别为0.004 8、0.003 8、0.001、0.002 6μg/mL。滑石粉样品分析结果的相对标准偏差(n=8)在1.1%～4.2%之间,回收率在93%～107%之间,测定结果与ICP-MS法基本吻合。

After digestion by aqua regia with microwave and selection of corresponding spectral lines at 267.7,257.6,213.8 and 324.7 nm as analytical lines,the acid-dissoluble metal elements including chromium,manganese,zinc and copper in talcum powder were determined by inductively coupled plasma atomic emission spectrometry（ICP-AES） under optimized conditions with radio frequency power of 1 250 W,auxiliary air flow rate of 0.60 L/min and atomizer pressure of 26 psi.When the concentration of each testing element was 2.0 μg/mL,the interferences caused by 20.0 μg/mL of iron,magnesium,calcium,aluminum,zinc,nickel and copper were all less than 5 %.Since the contents of these elements in talcum powder were less than 1 %,their influence on the determination could be ignored.The detection limits of chromium,manganese,zinc and copper were 0.004 8,0.003 8,0.001 and 0.002 6 μg/mL,respectively.This proposed method was applied in actual samples,and the determination results were consistent with those obtained by inductively coupled plasma mass spectrometry（ICP-MS） with relative standard deviations（RSD,n=8） of 1.1%-4.2% and recoveries of 93 %-107 %.