摘要
为了更精确地评估地质样品化学分析过程中背景值的高低,利用ICP-MS对在百级超净工作台内浓缩10倍的无机酸(优级纯盐酸、硝酸和氢氟酸)中38种痕量杂质元素进行了测定。测试过程中采用惰性气体(氦气)碰撞反应界面技术降低多原子干扰,考察了氦气流速对^(89)Y信号强度和CeO/Ce氧化物产率的影响。在最优实验条件下,各元素标准曲线的线性相关系数均不低于0.9990、检出限优于20.58 ng·L^(-1);加标回收实验的回收率在97.21%~103.55%、RSD为0.89%~4.96%。分析结果显示,在3种优级纯无机酸中杂质铁的含量普遍较高,盐酸、硝酸和氢氟酸分别达到10.28、8.60和34.81μg·L^(-1)。对二次纯化后氢氟酸的测定结果显示,除铁元素外的金属离子均未检出。
In order to better evaluate the background value during the chemical analysis of geological samples,this article concentrated the inorganic acid sample 10 times in a class 100 ultra-clean bench.ICP-MS was used to analyze the high-quality pure hydrochloric acid,nitric acid and hydrofluoric acid.The trace impurity elements were accurately determined.During the test,inert gas(He)collision reaction interface technology was used to reduce polyatomic interference.The influence of helium flow rate on the signal strength of ^(89)Y and the yield of CeO/Ce oxide was investigated.Under the optimal experimental conditions,element standards of the linear correlation coefficients of the curves were all better than 0.9990,and the detection limit was better than 20.58 ng·L^(-1).The recoveries and RSDs of the spiked recovery experiments were between 97.21%to 103.55%and 0.89%to 4.96%,respectively.The analysis results of the samples showed that the content of impurity iron was generally high in the three excellent grades of pure inorganic acids,with hydrochloric acid,nitric acid and hydrofluoric acid reaching 10.28,8.60 and 34.81μg·L^(-1),respectively.The measurement results of hydrofluoric acid after the second purification showed no metal ions except iron.
作者
杨锋
袁永海
李政林
余红霞
丁姗姗
YANG Feng;YUAN Yong-hai;LI Zheng-lin;YU Hong-xia;DING Shan-shan(Guangxi Key Laboratory of Hidden Metallic Ore Deposits Exploration,Guilin University of Technology,Guilin 541006,China)
出处
《桂林理工大学学报》
CAS
北大核心
2020年第4期828-832,共5页
Journal of Guilin University of Technology
基金
国家重点研发计划项目(2020YFA0714800)
广西高校中青年教师科研基础能力提升项目(2019KY0291,2019KY0297)。
关键词
ICP-MS
无机酸
预富集
杂质元素
ICP-MS
inorganic acid
preliminary enrichment
impurity element
