Abstract：In national standards GB/T 4103.2—2012 and GB/T 4103.6—2012, different sample dissolution methods were used for the determination of arsenic and antimony in lead and lead alloys by hydride generation-atomic fluorescence spectrometry (HG-AFS). The determination procedures were complicated. The sample was dissolved with nitric acid. The sulfuric acid was added to precipitate out and remove the lead matrix. Meanwhile, the hydrolysis of antimony was avoided by heating sulfuric acid to control the solution acidity. And accordingly the simultaneous determination method of arsenic and antimony in sample by HG-AFS was established. The experimental results showed that the correlation coefficients of calibration curves of arsenic and antimony were higher than 0.9997 under the optimal working conditions. The detection limits of method were 0.0005μg/L and 0.0007μg/L for arsenic and antimony, respectively. The interference tests indicated that the coexisting elements in sample did not interfere with the determination. The experimental method was applied for the determination of arsenic and antimony in actual lead ingot sample. The found results were basically consistent with those obtained by national standard methods (GB/T 4103.2—2012, GB/T 4103.6—2012 or IREAC-ZY-PB01). The relative standard deviations (RSD, n=6) of determination results for arsenic and antimony were between 1.8% and 2.0%.
李颜君, 杨占菊, 董更福, 隆英兰. 氢化物发生-原子荧光光谱法同时测定铅锭中砷锑[J]. 冶金分析, 2017, 37(11): 75-79.
LI Yan-jun, YANG Zhan-ju, DONG Geng-fu, LONG Ying-lan. Simultaneous determination of arsenic and antimony in lead ingot by hydride generation-atomic fluorescence spectrometry. , 2017, 37(11): 75-79.
热孜万古丽,全小盾,秦婷,等.电感耦合等离子体原子发射光谱法(ICP-AES)测定铅锭中11种杂质元素[J].中国无机分析化学,2012,2(1):74-76.RE ZI Wan-gu-li,QUAN Xiao-dun, QIN Ting,et al.Determination of 11 impurity elements in lead ingot by inductively coupled plasma atomic emission spectrometry(ICP-AES)[J].Chinese Journal of Inorganic Analytical Chemistry,2012 ,2(1):74-76.
[2]
唐斯田,周时建.电感耦合等离子体原子发射光谱法测定铅锭中8种杂质元素含量[J].理化检验:化学分册(Physical Testing and Chemical Analysis Part B: Chemical Analysis),2008 ,6(44):576-577.
[3]
刘梦影,吉国强,汪照玮,等.火焰原子吸收光谱法测定高纯铅中微量锑铋[J].广东化工,2016,43(11):246-247.LIU Meng-ying,JI Guo-qiang,WANG Zhao-wei,et al.Flame atomic absorption spectrometry determination of trace antimony and bismuth in high purity lead[J].Guangdong Chemical Industry,2016,43(11):246-247.
[4]
张遴,卢玉琦,高若煜,等.氢化物发生-原子荧光光谱法测定铅锭中砷锑铋[J].理化检验:化学分册,2000,36(1):26-28.ZHANG Lin,LU Yu-qi, GAO Ruo-yu,et al.Determination of arsenic antimony bismuth in lead ingots by hydride generation atomic fluorescence spectrometry[J].Physical Testing and Chemical Analysis Part B: Chemical Analysis,2000,36(1):26-28.
[5]
王丽,陆建平,张云飞,等.聚环氧琥珀酸掩蔽基体-氢化物发生原子荧光光谱法测定铅锭中砷和汞[J].冶金分析,2011,31(9):34-37.WANG Li,LU Jian-ping,ZHANG Yun-fei,et al.Simultaneous determination of arsenic and mercury in lead ingot by polyepoxysuccimic acid masking matrix-hydride generation atomic fluorescence spectrometry[J].Metallurgical Analysis,2011,31(9):34-37.
[6]
蔡玉曼,李明,陆丽君,等.盐酸-硝酸水浴消解氢化物发生原子荧光光谱法测定钨矿石和钼矿石中的砷[J].岩矿测试,2015,34(3):325-329.CAI Yu-man,LI Ming,LU Li-jun,et al.Determination of arsenic in tungsten and molybdenum ores by hydride generation-atomic fluorescence spectrometry with hydrochloric acid-nitric acid water-bath digestion[J]. Rock and Mineral Analysis,2015, 34(3): 325-329.
[7]
唐琼,陆建平,庞洁,等.氢化物发生原子荧光光谱法测定铅锭中硒[J].分析科学学报(Journal of Analytical Science),2014(1):123-126.
[8]
王雪芹,鲁丹,刘金华,等.快速去除硝酸和亚硝酸对氢化物发生原子荧光法测定砷的干扰[J].分析化学,2009,37(2):288-291.WANG Xue-qin,LU Dan,LIU Jin-hua,Rapid removal of interference from nitric and nitrous acid on the determination of arsenic with hydride generation atomic fluorescence spectrometry[J].Chinese Journal of Analytical Chemistry,2009,37(2):288-291.
任占军,郝贵奇,尹长田,等.微波消解-氢化物发生原子荧光光谱法测定污泥中汞和砷[J].冶金分析,2014,34(3):52-56.REN Zhan-jun,HAO Gui-qi,YIN Chang-tian,et al.Determination of mercury and arsenic in sludge by microwave digestion-hydride generation atomic fluorescence spectrometry[J].Metallurgical Analysis,2014,34(3):52-56.
[11]
金宇,刘曙,李晨,等.氢化物发生-原子荧光光谱法测定氟石中锑[J].冶金分析,2014,34(5):64-67.JIN Yu,LIU Shu,LI Chen,et al.Determination of antimony in fluorspar by hydride generation-atomic fluorescence spectrometry[J].Metallurgical Analysis,2014,34(5):64-67.
[12]
韩宗才,关弘弢.原子荧光光谱法测定合金钢中锑[J].光谱实验室(Chinese Journal of Spectroscopy Laboratory),2014,31(2):281-283.
