摘要
采用激光剥蚀固体进样和电感耦合等离子体质谱(ICP-MS)相结合的技术测定了纯铜中Fe、Zn、As、Sn、Sb、Pb、Bi共7种痕量元素。对激光剥蚀参数进行了优化,确定实验条件如下所示:激光能量为100%,剥蚀孔径为200μm,扫描速率为50μm/s,载气流量为0.4L/min。在优化的实验条件下,对纯铜标准样品进行测定,根据标准样品的认定值确定了测定元素的相对灵敏度因子(RSF),各元素仪器检出限为0.006 5～0.31μg/g。将实验方法应用于纯铜样品中痕量杂质的测定,测得结果的相对标准偏差(RSD,n=6)为6.6%～26%。参照国家标准方法GB/T 5121.28—2010中的ICP-MS以及实验方法分别对纯铜实际样品中的杂质元素进行定量分析,同时对两种方法的测定结果进行一致性检验,结果表明,对于Fe、Zn、Sn、Bi这4个元素,t<t_(0.05,9),说明这两种方法测定结果的一致性较好,具有可比性。由于其余3个元素的含量低于国家标准方法 GB/T 5121.28—2010检出限,因此未做平均值一致性检验。
Seven trace elements in pure copper,including Fe,Zn,As,Sn,Sb,Pb,Bi,were determined by laser ablation solid injection combined with inductively coupled plasma mass spectrometry(ICP-MS).The laser ablation parameters were optimized and the following experimental conditions were adopted:the laser energy was100%,the spot size was200μm,the scan rate was50μm/s,and the carrier gas flow rate was0.4L/min.The certified reference material of pure copper was determined under the optimum experimental conditions.The relative sensitivity factors(RSF)of tested elements were obtained based on the certified values of certified reference material.The detection limits of elements were0.0065-0.31μg/g.The trace impurities in pure copper sample were determined according to the experimental method,and the relative standard deviations(RSD,n=6)of results were between6.6%and26%.The contents of impurity elements in pure copper actual sample were quantitatively analyzed respectively according to ICP-MS in GB/T5121.28-2010of national standard method and the proposed method.Meanwhile,the consistency test of determination results by the above two methods was conducted.For these four elements including Fe,Zn,Sn and Bi,the results showed that t was less than t0.05,9,which indicated good consistency for the two methods with comparability.Since the contents of other elements were lower than the detection limit of GB/T5121.28-2010of national standard method,the consistency test of average value was not performed.
作者
陈晓峰
胡芳菲
张煦
臧慕文
童坚
CHEN Xiao-feng;HU Fang-fei;ZHANG Xu;ZANG Mu-wen;TONG Jian(Guobiao (Beijing) Testing & Certification Co., Ltd., Beijing 100088, China)
出处
《冶金分析》
CAS
CSCD
北大核心
2018年第12期1-6,共6页
Metallurgical Analysis
