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摘要:本论文采用HNO3:H2O2为1:1作为消解试剂,以高压消解法消解样品,以载流溶液盐酸酸度、还原剂KBH4浓度、负高压为正交试验因素,选三水平做正交试验,在正交试验的优化条件下,得出实验最优条件为5%的盐酸、负高压为270V、KBH4浓度为20g/L;根据实验优化条件,绘制砷、汞标准曲线,砷的相关系数为R=0.9993,汞的相关系数为R=0.9997,并以5%的盐酸做载流液,加入10g/L硫脲做预还原掩蔽剂,20g/LKBH4为还原剂,用原子荧光法测定云黄连中砷的含量为0.1347mg/kg,汞的含量为0.0112mg/kg。该方法测得的回收率为94%-100.5%之间,砷的检出限为0.0691µg/L,汞的检出限为0.0253µg/L。 关键词:黄连;砷;汞;原子荧光光谱法
ABSTRACT:This paper adopted HNO3:H2O2 1:1 as negate reagents, with High-pressure digestion method digested samples, In current-carrying solution acidity, reductant concentration of hydrochloric acid KBH4 and negative high-pressure for orthogonal experiment factors, Chosen three levels for orthogonal experiment, In the optimized conditions of orthogonal test, Obtain the optimal conditions for 5% of hydrochloric acid, negative high pressure for 270V, KBH4 concentration for 20g/L, According to the experimental optimized conditions , Drawn arsenic and mercury standard curve,Arsenic and the correlation coefficient was R = 0.9993, Mercury and the correlation coefficient was R = 0.9997,And hydrochloric acid at 5% current-carrying liquid, Joined in 10g/L thiourea masking agent for prereduction,20g/L KBH4 masking agent for reductant, By atomic fluorescence spectrometry cloud the content of arsenic coptis chinensis for 0.1347 mg/kg, mercury content was 0.0112 mg/kg. This method for measurement of the recovery 100.5% between, arsenic 94 percent - the detect limited for 0.0691 µg/L, mercury detect limit for 0.0253 µg/L. Keywords: Coptis, Arsenic , Mercury, Atomic fluorescence spectrometry. |