ICP-MS Determination of W in Nuclear Grade Sponge Zirconium
摘 要
0.100 0 g核级海绵锆样品用氢氟酸0.5 mL,硝酸2 mL于150℃左右溶解后,用水定容至100 mL。采用电感耦合等离子体质谱法测定样品溶液中钨的含量。184W为分析核素,以232Th为内标物。钨的线性范围在100.0 μg·L-1以内,方法的检出限(3s)为0.003 μg·L-1。以2.00,50.00 μg·L-1浓度水平进行加标回收试验,回收率为91.5%,93.5%,测定值的相对标准偏差(n=6)为5.0%,2.4%。
Abstract
The sample (0.100 0 g) of nuclear grade sponge zirconium was dissolved with HF (0.5 mL) and HNO3 (2 mL) at temperature of 150℃ or so,and then was diluted to 100 mL with water. ICP-MS was applied to the determination of W in the sample solution. 184W was used as the analytical nuclide, 232Th was used as internal standard. Linearity range of W was found in the range within 100.0 μg·L-1 with detection limit (3s) of 0.003 μg·L-1. Tests for recovery was made by standard addition method at the concentration levels of 2.00, 50.00 μg·L-1, values of recovery found were 91.5%,93.5%, with RSD's (n=6) of 5.0%, 2.4%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201711017
所属栏目 工作简报
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收稿日期 2016/11/5
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备注王鹏(1982-),男,甘肃正宁人,助理研究员,研究方向为核燃料及材料化学分析,13518103539@163.com
引用该论文: WANG Peng,LONG Shaojun,LIAO Zhihai,QIAO Hongbo,WANG Zhanming,ZHAO Feng,NING Wei. ICP-MS Determination of W in Nuclear Grade Sponge Zirconium[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2017, 53(11): 1322~1324
王鹏,龙绍军,廖志海,乔洪波,王占明,赵峰,宁伟. 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
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参考文献
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【7】高洪波,禄妮,李波,等.ICP-AES法测定锆合金中常量及微量元素[J].现代科学仪器, 2007(2):87-89.
【8】YIM S A, CHOI M S, CHAE J S. Direct determination of gold in rock samples using collision cell quadrupole ICP-MS[J]. J Am Soc Mass Spectrom, 2012,23(1):171-178.
【9】龙绍军,廖志海,安身平,等.电感耦合等离子体质谱法测定铀铌混合氧化物中的钐、铕、钆、镝[J].核化学与放射化学, 2014,36(6):352-356.
【2】ASTM B349/B349M-2009 Zirconium sponge and other forms of virgin metal for nuclear application[S].
【3】康慨,王训银,王树安,等.海绵锆中钨的分析测定-二硫酚锌盐-氯仿萃取分光光度法[J].核动力工程, 2001,22(1):70-74.
【4】李刚,陈苏,李艳,等.电感耦合等离子体原子发射光谱法测定核级锆合金中17种常量及痕量元素[J].冶金分析, 2012,32(11):56-60.
【5】侯列奇,王树安,李洁.ICP-AES测定核纯海绵锆中17个杂质元素方法研究[J].光谱实验室, 1996,13(5):42-46.
【6】侯列奇,李洁,卢菊生.电感耦合等离子体原子发射光谱法测定核纯海绵锆中微量铪[J].理化检验-化学分册, 2008,44(2)142-143.
【7】高洪波,禄妮,李波,等.ICP-AES法测定锆合金中常量及微量元素[J].现代科学仪器, 2007(2):87-89.
【8】YIM S A, CHOI M S, CHAE J S. Direct determination of gold in rock samples using collision cell quadrupole ICP-MS[J]. J Am Soc Mass Spectrom, 2012,23(1):171-178.
【9】龙绍军,廖志海,安身平,等.电感耦合等离子体质谱法测定铀铌混合氧化物中的钐、铕、钆、镝[J].核化学与放射化学, 2014,36(6):352-356.
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