火焰原子吸收光谱法测定粗锡中铋的含量
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摘要
为了准确、快速测定粗锡中铋的含量,对火焰原子吸收光谱法测定粗锡中铋的条件进行了研究,并建立了测定方法。确定了用盐酸、硝酸、高氯酸、氢氟酸进行溶解粗锡,经盐酸-氢溴酸除掉大量的锡、锑和砷,在盐酸-硝酸混合酸的介质中,用火焰原子吸收光谱法于223.1nm处测定粗锡中铋的含量。通过条件实验研究了溶样方法、共存元素干扰、仪器条件等因素对测定结果的影响,在选定仪器参数条件下,加标回收率为98.9%～105%,且测定值与电感耦合等离子体发射光谱法结果一致;相对标准偏差(RSD,n=11)为1.6%和1.2%,结果准确性和重复性较高,适合粗锡等物料中铋的测定。
In order to accurately and rapidly determine the content of bismuth in crude tin,the determination conditions by flame atomic absorption spectrometry were investigated.The samples were digested with HCl-HNO3-HClO4-HF,evaporated them to dryness.Tin,stibonium and arsenic were volatilized by adding HCl-HBr,determination of bismuth content by flame atomic absorption spectrometry at 223.1 nm with the HCl-HNO3.Digest method,influence of coexisting elements and instrument condition were discussed in this paper.This method has high determination recovery and repeatability,the determination recovery of bismuth was 98.9%-105%,and compared with ICP-AES method,the measured values was in agreement with the certified values.The determination RSD were 1.6% and1.2%,when the samples were repeatedly measured(n=11)with this method.
In order to accurately and rapidly determine the content of bismuth in crude tin,the determination conditions by flame atomic absorption spectrometry were investigated.The samples were digested with HCl-HNO3-HClO4-HF,evaporated them to dryness.Tin,stibonium and arsenic were volatilized by adding HCl-HBr,determination of bismuth content by flame atomic absorption spectrometry at 223.1 nm with the HCl-HNO3.Digest method,influence of coexisting elements and instrument condition were discussed in this paper.This method has high determination recovery and repeatability,the determination recovery of bismuth was 98.9%-105%,and compared with ICP-AES method,the measured values was in agreement with the certified values.The determination RSD were 1.6% and1.2%,when the samples were repeatedly measured(n=11)with this method.
引文
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[7]何桥云.锡矿石中铋的测定---火焰原子吸收光谱法[J].云南化工(Yunnan Chemical Technology),2017,44(5):67-70.
[8]王嘉盛.火焰原子吸收光谱法测定锡锭中痕量杂质元素[J].蓄电池(Storage Battery),2003,40(3):143-144.
[9]全国有色金属标准化技术委员会.锡化学分析方法第3部分:铋量的测定火焰原子吸收光谱法:GB/T3260.3-2013[S].北京:中国标准出版社,2013.
[10]全国有色金属标准化技术委员会,锡阳极泥化学分析方法第3部分:铜量、铅量和铋量的测定火焰原子吸收光谱法:YS/T1116.3-2016[S].北京:中国标准出版社,2016.
[2]范丽新,陆青.EDTA滴定法测定粗锡中铅[J].冶金分析(Metallurgical Analysis),2017,37(5):68-72.
[3]李振昊,李文乐,孔繁华,等.掺杂二氧化锡的应用研究进展[J].化工进展(Chemical Industry and Engineering Progress),2010,29(12):2324-2329.
[4]北京矿冶研究总院测试研究所.有色冶金分析手册[M].北京:冶金工业出版社,1998.
[5]魏雅娟,吴雪英,江荆,等.火焰原子吸收光谱法(AAS)测定银精矿中铋元素的含量[J].山东工业技术(Shandong Industrial Technology),2018(7):225-226.
[6]何洁,贺与平.火焰原子吸收光谱法测定锡基轴承合金中的铋[J].云南化工(Yunnan Chemical Technology),2006,33(2):61-62.
[7]何桥云.锡矿石中铋的测定---火焰原子吸收光谱法[J].云南化工(Yunnan Chemical Technology),2017,44(5):67-70.
[8]王嘉盛.火焰原子吸收光谱法测定锡锭中痕量杂质元素[J].蓄电池(Storage Battery),2003,40(3):143-144.
[9]全国有色金属标准化技术委员会.锡化学分析方法第3部分:铋量的测定火焰原子吸收光谱法:GB/T3260.3-2013[S].北京:中国标准出版社,2013.
[10]全国有色金属标准化技术委员会,锡阳极泥化学分析方法第3部分:铜量、铅量和铋量的测定火焰原子吸收光谱法:YS/T1116.3-2016[S].北京:中国标准出版社,2016.