辉光放电质谱法测定高纯锆中36种痕量杂质元素
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摘要
测定锆及锆合金中杂质元素的研究较为常见,而针对高纯锆中化学成分检测的相关研究较少。在讨论各杂质元素质谱干扰的基础上,通过选择合适的同位素及分辨率,建立了辉光放电质谱法(GDMS)测定高纯锆中Na、Al、Si、P、Ti、V、Cr、Fe等36种痕量杂质元素的分析方法。对仪器参数进行了优化,最终选择氩气流量为370mL/min,放电电流为32mA,预溅射时间为15min。利用建立的实验方法对高纯锆样品中痕量杂质元素进行了测定,测定结果的相对标准偏差(RSD,n=7)均小于30%,质量分数大于0.1μg/g的杂质元素的RSD(n=7)均小于10%。采用电感耦合等离子体质谱法(ICP-MS)进行了方法比对,实验方法与ICP-MS的结果具有一致性。
The impurity elements in zirconium and zirconium alloy were commonly studied,but there were few reports on the analysis of chemical composition in high purity zirconium.On the basis of discussing the mass spectrometric interferences of various impurity elements,the determination method of 36 trace impurities such as Na,Al,Si,P,Ti,V,Cr and Fe in high purity zirconium by glow discharge mass spectrometry(GDMS)was established by selecting the proper isotopes and resolution rates.The instrumental parameters were optimized and the final conditions were selected:the argon flow rate was 370 mL/min,the discharge current was 32 mA,and the pre-sputtering time was 15 min.Trace impurity elements in high purity zirconium sample was determined according to the experimental method.The relative standard deviations(RSD,n=7)of determination results were less than 30%.For the impurity elements with mass fraction higher than 0.1μg/g,the RSDs(n=7)were all less than 10%.The determination results were compared with those obtained by inductively coupled plasma mass spectrometry(ICP-MS).The results showed good consistence.
The impurity elements in zirconium and zirconium alloy were commonly studied,but there were few reports on the analysis of chemical composition in high purity zirconium.On the basis of discussing the mass spectrometric interferences of various impurity elements,the determination method of 36 trace impurities such as Na,Al,Si,P,Ti,V,Cr and Fe in high purity zirconium by glow discharge mass spectrometry(GDMS)was established by selecting the proper isotopes and resolution rates.The instrumental parameters were optimized and the final conditions were selected:the argon flow rate was 370 mL/min,the discharge current was 32 mA,and the pre-sputtering time was 15 min.Trace impurity elements in high purity zirconium sample was determined according to the experimental method.The relative standard deviations(RSD,n=7)of determination results were less than 30%.For the impurity elements with mass fraction higher than 0.1μg/g,the RSDs(n=7)were all less than 10%.The determination results were compared with those obtained by inductively coupled plasma mass spectrometry(ICP-MS).The results showed good consistence.
引文
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[13]胡芳菲,王长华,李继东.直流辉光放电质谱法测定氧化铝中的杂质元素[J].质谱学报,2017,35(4):335-340.HU Fang-fei,WANG Chang-hua,LI Ji-dong.Impurities concentration detection in oxide aluminum by direct current glow discharge mass spectrometry[J].Journal of Chinese Mass Spectrometry Society,2017,35(4):335-340.
[14]ASTM International.ASTM F2405-04(2011)Standard test method for trace metallic impurities in high purity copper by high-mass-resolution Glow Discharge Mass Spectrometer[S].Pennsylvania:ASTM,2011.
[15]ASTM International.ASTM F1709-97(2016)Standard specification for high purity titanium sputtering targets for electronic thin film applications[S].Pennsylvania:ASTM,2016.
[16]ASTM International.ASTM F1593-08(2016)Standard test method for trace metallic impurities in electronic grade aluminum by high mass-resolution Glow-Discharge Mass Spectrometer[S].Pennsylvania:ASTM,2016.
[2]中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.GB/T 13747.15-2017锆及锆合金化学分析方法第15部分:硼量的测定姜黄素分光光度法[S].北京:中国标准出版社,2008.
[3]中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.GB/T 13747.9-2017锆及锆合金化学分析方法第9部分:镁量的测定火焰原子吸收光谱法[S].北京:中国标准出版社,2008.
[4]中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.GB/T 13747.17-2017锆及锆合金化学分析方法第17部分:镉量的测定极谱法[S].北京:中国标准出版社,2008.
[5]中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.GB/T 13747.20-2017锆及锆合金化学分析方法第20部分:铪量的测定电感耦合等离子体原子发射光谱法[S].北京:中国标准出版社,2008.
[6]中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.GB/T 13747.27-2017锆及锆合金化学分析方法第27部分:痕量杂质元素的测定电感耦合等离子体质谱法[S].北京:中国标准出版社,2008.
[7]邓传东,廖志海,乔洪波,等.电感耦合等离子体原子发射光谱法测定核纯级海绵锆中锂钠镁钙[J].冶金分析,2018,38(12):36-40.DENG Chuan-dong,LIAO Zhi-hai,QIAO Hong-bo,et al.Determination of lithium,sodium,magnesium,calcium in sponge zirconium of nuclear grade by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2018,38(12):36-40.
[8]李洁,安身平,宁伟,等.电感耦合等离子体原子发射光谱法测定核纯级海绵锆中17种微量杂质元素[J].理化检验:化学分册,2017,53(9):1047-1051.LI Jie,AN Shen-ping,NING Wei,et al.ICP-AES determination of 17kinds of trace impurity elements in sponge zirconium of nuclear purity grade[J].Physical Tests and Chemical Analysis Part B:Chemical Analysis,2017,53(9):1047-1051.
[9]王金磊,罗琳,李波,等.ICP-MS法核级海绵锆中痕量杂质含量的测定[J].河南化工,2017,34(7):48-51.WANG Jin-lei,LUO Lin,LI Bo,et al.ICP-MS determination of trace impurity elements in sponge zirconium of nuclear purity grade[J].Henan Chemical Industry,2017,34(7):48-51.
[10]王鹏,龙绍军,廖志海,等.电感耦合等离子体质谱法测定核级海绵锆中钨[J].理化检验:化学分册,2017,53(11):1322-1324.WANG Peng,LONG Shao-jun,LIAO Zhi-hai,et al.ICP-MS determination of W in nuclear grade sponge zirconium[J].Physical Tests and Chemical Analysis Part B:Chemical Analysis,2017,53(11):1322-1324.
[11]杨海岸,罗舜,闫豫昕,等.辉光放电质谱法测定高纯镍中16种痕量杂质元素[J].冶金分析,2015,35(5):1-6.YANG Hai-an,LUO Shun,YAN Yu-xin,et al.Determination of sixteen trace impurity elements in high purity nickel by glow discharge mass spectrometry[J].Metallurgical Analysis,2015,35(5):1-6.
[12]刘元元,胡净宇.辉光放电质谱法测定棒状高纯镁中12种杂质元素[J].冶金分析,2018,38(4):16-21.LIU Yuan-yuan,HU Jing-yu.Determination of twelve impurities in rod like high-purity magnesium by glow discharge mass spectrometry[J].Metallurgical Analysis,2018,38(4):16-21.
[13]胡芳菲,王长华,李继东.直流辉光放电质谱法测定氧化铝中的杂质元素[J].质谱学报,2017,35(4):335-340.HU Fang-fei,WANG Chang-hua,LI Ji-dong.Impurities concentration detection in oxide aluminum by direct current glow discharge mass spectrometry[J].Journal of Chinese Mass Spectrometry Society,2017,35(4):335-340.
[14]ASTM International.ASTM F2405-04(2011)Standard test method for trace metallic impurities in high purity copper by high-mass-resolution Glow Discharge Mass Spectrometer[S].Pennsylvania:ASTM,2011.
[15]ASTM International.ASTM F1709-97(2016)Standard specification for high purity titanium sputtering targets for electronic thin film applications[S].Pennsylvania:ASTM,2016.
[16]ASTM International.ASTM F1593-08(2016)Standard test method for trace metallic impurities in electronic grade aluminum by high mass-resolution Glow-Discharge Mass Spectrometer[S].Pennsylvania:ASTM,2016.
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