流动注射氢化物发生与动态反应池-电感耦合等离子体质谱法分析镍基超合金中锗砷硒  

Determination of germanium,arsenic,selenium in nickel-base superalloy by flow injection hydride generation and dynamic reaction cell-inductively coupled plasma mass spectrometry

作　　者：干宁[1] 李天华[1] 王鲁雁[1] 徐伟民[1] 

机构地区：[1]宁波大学材化学院新型功能材料及其制备科学国家重点实验室,浙江宁波315211

出　　处：《冶金分析》2007年第11期7-11,共5页Metallurgical Analysis

基　　金：浙江省自然科学基金(Y106725);浙江省科技攻关项目(No.2006C31040);浙江省教育厅基金(20061697);宁波市自然科学基金(No2006A610048)资助项目

摘　　要：建立了流动注射(FI)氢化物发生(HG)与动态反应池(DRC)-电感耦合等离子体质谱法(CP-MS)分析镍基超合金样品中锗、砷、硒的方法。采用动态反应池-氢化物生成技术富集锗、砷、硒,选择半胱氨酸(L-Cys)以及使用气液分离装置,降低了Ni,Co基体在三种元素氢化物生成时的干扰。探讨了氢化物生成的最佳条件、气体流速及基质氧化物对测定的影响。结果表明,以2.0 g/L NaBH4作为氢气发生剂,20 g/L L-Cys作为掩蔽和增敏剂,控制气体流速为0.95 mL/min时,三种元素都有最佳的氢化物发生效率,且Ni,Co对分析干扰可忽略不计。实验求得锗、砷、硒检测限分别为0.003 pg/L,0.001 pg/L,0.002 pg/L。测定1μg/g锗、砷、硒的RSD分别为1.5%,2.9%,2.2%,回收率分别为91.3%,91.4%,112.0%。应用该法于镍基合金标准样品中Ge,As,Se的测定,结果与认定值相吻合。A new method for determination of Ge,As,Se in nickel base superalloy samples was established by flow injection hydride generation-dynamic reaction cell-inductively coupled plasma mass spectrometry（FI-HG--DRC-ICP-MS）. Hydride generation technology was employed for enrichment of Ge,As,Se in samples. L-cysteine was chosen to reduce the interference of Ni and Co to form hydride. The optimum experimental conditions were discussed. The results showed that three elements have the best hydrogen generation efficiency and the interference of Ni,Co matrix can be neglected with 2.0 g/L NaBH4 as hydrogen generating agent,20 g/L L-Cys as masking agent,and gas flow rate of 0.95 mL/min. Under the optimum experimental conditions,the detection limits of Ge,As,Se were 0. 003 pg/L,0. 001 pg/L,0. 002 pg/L respectively. The RSDs at the 1μg/g level for Ge,As,Se were 1.5%,2.9%,2.2% and recoveries were 91.3%, 91.4%, 112.0% , respectively. The method was employed to determine Ge,As,Se in standard nickel based alloys. The results were comparable with the certified values.

关 键 词：流动注射氢化物发生系统 动态反应池-电感耦合等离子体质谱仪 镍基超合金 锗 砷 硒 

分 类 号：TG115.3[金属学及工艺—物理冶金]