电感耦合等离子体原子发射光谱法测定氟化氢气体中16种金属元素
Determination of 16 Metal Elements in Hydrogen Fluoride Gas by Inductively Coupled Plasma Atomic Emission Spectrometry
摘 要
基于电子工业对氟化氢气体中金属离子含量的严格要求，以自制的简单的气体吸收装置吸收氟化氢气体，通过吸收前后吸收液的质量变化得到氟化氢的质量，采用附带耐氢氟酸进样系统的电感耦合等离子体原子发射光谱仪（ICP-AES）在最优的仪器工作条件下测定吸收液中的钾、镁、铝、钡、锌、铬、钴、镉、铁、铜、镍、铅、锰、钠、钙和锡等16种金属元素的含量。结果表明：16种金属元素的质量浓度均在一定范围内与其对应的光谱强度呈线性关系，相关系数均大于0.999 0，检出限（3s）为0.10~6.0 μg·L-1，测定值的相对标准偏差（n=11）为0.96%~5.0%。
自制气体吸收装置
金属元素
氟化氢气体
inductively coupled plasma atomic emission spectrometry
self-made adsorption device
metal element
hydrogen fluoride gas
Abstract
Based on the strict quality requirements in the electronic industry, a method for determination of metal impurities in hydrogen fluoride gas was developed by inductively coupled plasma atomic emission spectrometry (ICP-AES) with a hydrofluoric acid-resistant sampling system. A simple self-made absorption device was designed for absorbing hydrogen fluoride gas, and the mass of absorbed hydrogen fluoride was obtained by the mass changes of absorption solution. The 16 metal elements including potassium, magnesium, aluminum, barium, zinc, chromium, cobalt, cadmium, iron, copper, nickel, lead, manganese, sodium, calcium and tin were determined under the optimal instrumental conditions. As found by results that linear relationships between mass concentrations of 16 metal elements and their corresponding spectral intensities were all in the definite ranges, with correlation coefficients greater than 0.999 0. The detection limits (3s) were ranged from 0.10-6.0 μg·L-1, and RSDs (n=11) of the measured values were in the range of 0.96%-5.0%.
中图分类号 O657.31 DOI 10.11973/lhjy-hx202008007
所属栏目 工作简报
基金项目 国家重点研发计划项目课题（2017YFB0405803）
收稿日期 2020/11/23
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备注钟军,教授级高级工程师,主要从事含氟电子化学品、含氟精细化学品的检测技术研究及标准化工作,zhongjun-6@163.com
引用该论文: ZHONG Jun,LI Jun,YE Lin,TAN Hui,ZHENG Hongmei. Determination of 16 Metal Elements in Hydrogen Fluoride Gas by Inductively Coupled Plasma Atomic Emission Spectrometry[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2020, 56(8): 888～892
钟军,李军,叶林,谭慧,郑红梅. 电感耦合等离子体原子发射光谱法测定氟化氢气体中16种金属元素[J]. 理化检验－化学分册, 2020, 56(8): 888～892
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【8】MOTZ K L, FREIRE F J, EDWARDS E G, et al. Process for purifying hydrogen fluoride:US, 5108559 A[P]. 1992-04-28.
【9】张丹辉,唐安江,韦德举,等.四氟化硅气体中杂质的检测及净化研究进展[J].应用工, 2019,48(2):486-489.
【10】张文娟.高纯电子气体中金属杂质分析方法概述[J].广州化工, 2015,43(14):19-20.
【11】BULANOV A D, PIMENOV V G. Determination of impurities in monoisotopic silicon tetrafluoride[J]. Inorganic Materials, 2004,40(7):754-759.
【12】郑秋艳,王少波,李绍波,等.电感耦合等离子体原子发射光谱法测定高纯六氟化钨中13种金属元素[J].理化检验-化学分册, 2010,46(8):952-954.
【13】JAHL M J, BARNES R M. Analysis of silane with a sealed inductively coupled plasma discharge[J]. Journal of Analytical Atomic Spectrometry, 1992,7(6):833-838.
【14】JACKSIER T, BARNES R M. Quantitative analysis of electronic-grade anhydrous hydrogen chloride by sealed inductively coupled plasma atomic emission spectroscopy[J]. Journal of Analytical Atomic Spectrometry, 1994,9(11):1299-1303.
【15】孟蓉,李红华,黄志齐,等.膜去溶剂化进样ICP-MS法直接测定电子级高纯过氧化氢中痕量金属杂质[J].化学试剂, 2002,24(4):208-210.
【16】郭峰,谭红,何锦林,等.改进的挥发硅-ICP-MS法测定测定高纯四氯化硅中金属杂质[J].福建分析测试, 2006,15(4):7-9.
【17】林宇巍.SEMI标准关于电子气分析方法概述[J].质量技术监督研究, 2011(3):18-21.
【18】HUTTON R C, BRIDENNE M, COFFRE E, et al. Investigations into the direct analysis of semiconductor grade gases by inductively coupled plasma mass spectrometry[J]. Journal of Analytical Atomic Spectrometry, 1990,5(6):463-466.
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