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作 者:墨淑敏 李娜 王长华 邱长丹 潘元海 杨飞宇 MO Shu-min;LI Na;WANG Chang-hua;QIU Chang-dan;PAN Yuan-hai;YANG Fei-yu(Guobiao(Beijing)Testing&Certification Co.,Ltd.,Beijing 100088,China)
机构地区:[1]国标(北京)检验认证有限公司,北京100088
出 处:《冶金分析》2019年第9期21-25,共5页Metallurgical Analysis
摘 要:锡铅焊料中的杂质元素对焊点的抗氧化性、润湿性、扩展面积有重要影响,因此对其进行测定意义重大。采用硝酸、氢氟酸溶解样品,选择H 2动态反应池模式测定Fe,标准模式测定Al、P、Cu、Zn、As、Cd、Ag、Sb、Au、Bi,同时以Sc校正Al、P、Fe、Cu,以Cs校正Zn、As、Ag、Cd,以Tl校正Sb、Au、Bi,实现了电感耦合等离子体质谱法(ICP-MS)对锡铅焊料中这11种杂质元素含量的测定。在优化的实验条件下,11种杂质元素校准曲线的相关系数均大于0.999,方法的检出限在0.002~0.80μg/g范围内,测定下限在0.007~2.73μg/g范围内。用建立的实验方法测定锡铅焊料样品中Al、P、Fe、Cu、Zn、As、Cd、Ag、Sb、Au、Bi,平行测定11次结果的相对标准偏差(RSD)为0.85%~3.5%,加标回收率为90%~110%。将实验方法应用于锡铅焊料标准物质YT9302中Al、Fe、Cu、Zn、As、Sb、Bi共7种杂质元素的测定,结果与认定值一致。The impurity elements in tin-lead solder had an important influence on the oxidation resistance,wettability and expansion area of solder joints.Therefore,the accurate determination of these impurities was of great significance.The sample was dissolved with nitric acid and hydrofluoric acid.The content of Fe was determined at H 2 dynamic reaction cell mode,and the contents of Al,P,Cu,Zn,As,Cd,Ag,Sb,Au and Bi were determined at standard mode.Meanwhile,Sc was selected for the correction of Al,P,Fe and Cu;Cs was selected for the correction of Zn,As,Ag and Cd;Tl was selected for the correction of Sb,Au and Bi.Thus,a determination of eleven impurity elements in tin-lead solder by inductively coupled plasma mass spectrometry(ICP-MS)was realized.Under the optimized experimental conditions,the correlation coefficients of calibration curves of 11 impurity elements were all higher than 0.999.The detection limits were in the range of 0.002-0.80μg/g,and the low limit of determination were in the range of 0.007-2.73μg/g.The proposed method was applied for the determination of Al,P,Fe,Cu,Zn,As,Cd,Ag,Sb,Au and Bi in tin-lead solder sample.The relative standard deviations(RSDs,n=11)were between 0.85%and 3.5%,and the recoveries were between 90%and 110%.The experimental method was also applied for the determination of seven impurity elements(Al,Fe,Cu,Zn,As,Sb and Bi)in the certified reference material of tin-lead solder.The results were consistent with the certified values.
关 键 词:电感耦合等离子体质谱法(ICP-MS) 锡铅焊料 杂质
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