采用密闭消解多晶硅样品,然后利用磷钼蓝光度法测定多晶硅中磷含量.探讨了酸度、显色剂用量、还原剂用量等因素对测定的影响,并优化了实验参数.在最大吸收波长829nm处,磷的线性范围为0~4.0μg/mL,相关系数为0.999 8,检出限为0.04 μg/mL.用本文确定的方法测定多晶硅样品中磷时,大量硅在溶样时加入氢氟酸挥发而除去,过量的氢氟酸用硼酸络合,对磷的测定没有影响.该方法操作简便,具有较高的灵敏度,样品中磷分析结果的相对标准偏差为2.5%~3.5%,加标回收率在93.3%~99.8%之间.
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