微波消解-电感耦合等离子体原子发射光谱法测定银精矿中铅锌铜砷锑铋镉

Determination of lead,zinc,copper,arsenic,antimony,bismuth and cadmium in silver concentrate by inductively coupled plasma atomic emission spectrometry after microwave digestion

采用盐酸-硝酸-氢氟酸并采用微波消解处理样品,高氯酸冒烟至尽干,加盐酸溶解盐类,选择Pb 220.353nm、Zn 206.200nm、Cu 327.393/Cu 324.752nm、As 193.696nm、Sb206.836nm、Bi 190.171nm、Cd 214.440nm/Cd 226.502nm为分析谱线,使用电感耦合等离子体原子发射光谱法(ICP-AES)同时测定铅、锌、铜、砷、锑、铋、镉,从而建立了银精矿中铅、锌、铜、砷、锑、铋、镉等杂质元素的分析方法。铅、锌、锑在0.50%~5.00%,铜、铋在0.10%~5.00%,砷在0.10%~3.00%,镉在0.050%~0.50%范围内校准曲线呈线性,线性相关系数r均大于0.999 9。方法中各元素的检出限为0.001%~0.014%。实验方法用于测定两个银精矿样品中铅、锌、铜、砷、锑、铋、镉,结果的相对标准偏差(RSD,n=11)为0.74%~2.9%,并与相应的国标方法测定值相吻合(其中铅和锌采用火焰原子吸收光谱法(YS/T 445.9—2001),铜采用火焰原子吸收光谱法(YS/T 445.2—2001),砷和铋采用氢化物发生-原子荧光光谱法(YS/T 445.3—2001),锑参照采用氢化物发生-原子荧光光谱法(YS/T 445.3—2001),镉采用原子吸收光谱法(YS/T 445.8—2001))。按照实验方法测定两个银精矿样品中铅、锌、铜、砷、锑、铋、镉,并进行加标回收试验,回收率为96%~105%。

The sample was treated by microwave digestion in hydrochloric acid-nitric acid-hydrofluoric acid system.After perchloric acid fuming to dryness,the salts were dissolved with hydrochloric acid.Pb220.353 nm,Zn 206.200 nm,Cu 327.393/Cu 324.752 nm,As 193.696 nm,Sb 206.836 nm,Bi 190.171 nm and Cd 214.440 nm/Cd 226.502 nm were selected as the analytical lines.The simultaneous determination method of lead,zinc,copper,arsenic,antimony,bismuth and cadmium in silver concentrate by inductively coupled plasma atomic emission spectrometry（ICP-AES）was established.The linearity of calibration curves was good for lead,zinc and antimony（0.50%-5.00%）,copper and bismuth（0.10%-5.00%）,arsenic（0.10%-3.00%）and cadmium（0.050%-0.50%）.The linear correlation coefficients（r）were all higher than 0.999 9.The detection limits of elements were in range of 0.001%-0.014%.The experimental method was applied for the determination of lead,zinc,copper,arsenic,antimony,bismuth and cadmium in two silver concentrate samples.The relative standard deviations（RSD,n=11）of measured results were between 0.74%and 2.9%.The found results were consistent with those obtained by national standard methods：flame atomic absorption spectrometry（YS/T 445.9-2001）for lead and zinc,flame atomic absorption spectrometry（YS/T 445.2-2001）for copper,hydride generation-atomic fluorescence spectrometry（YS/T445.3-2001）for arsenic and bismuth,reference of hydride generation-atomic fluorescence spectrometry（YS/T 445.3-2001）for antimony,and atomic absorption spectrometry（YS/T 445.8-2001）for cadmium.The contents of lead,zinc,copper,arsenic,antimony,bismuth and cadmium in two silver concentrate samples were determined according to the experimental method.Meanwhile,the recovery tests were also conducted.The recoveries were between 96% and 105%.