过氧化钠碱熔-电感耦合等离子体质谱法测定原生矿石中的锡
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摘要
原生锡矿石主要存在的矿床类型有矽卡岩型锡矿、斑岩型锡矿、锡石硅酸盐脉型锡矿、锡石硫化物脉型锡矿、石英脉及云英岩型锡矿。锡矿石一般不溶于盐酸、硝酸及王水体系,采用硫酸、氢氟酸处理时无法全部溶解。苯芴铜分光光度法和碘量法等传统测试方法存在受样品中伴生元素干扰大、稳定性差、检出限高、分析效率低等不足。本文建立了电感耦合等离子体质谱法测定原生矿石中锡元素含量的分析方法,用过氧化钠对样品进行熔融分解处理,热水浸取后用酒石酸-盐酸酸化,采用铑作为内标进行仪器信号漂移校正,同时用高倍稀释的方式来克服基体干扰。方法检出限为0.1μg/g,精密度小于5%,最低检出浓度为0.4μg/g,测试范围为12.5～12700μg/g。本方法操作简便,分析速度和数据质量都优于传统分析方法。
BACKGROUND: The main types of primary tin ore occur in skarn, porphyry, cassiterite silicate vein, cassiterite sulfide vein, quartz vein and greisen tin deposits. Tin ores are generally insoluble in hydrochloric acid, nitric acid and aqua regia, and tin ores cannot be dissolved completely when treated with sulfuric acid or hydrofluoric acid. Traditional measurement methods such as phenylfluorone-cetyltrimethyl ammonium bromide spectrophotometry and iodometry have disadvantages, such as the serious interference of the associated elements in the sample, poor stability, high detection limit and low analysis efficiency.OBJECTIVES: To establish a method for the determination of tin in primary ore by Inductively Coupled Plasma-Mass Spectrometry.METHODS: The sample was melted and decomposed by sodium oxide, and leached by hot water, followed by tartaric acid and hydrochloric acid acidification. ~(103)Rh was used as the internal standard element to correct instrument signal drift, and the matrix effect was overcome by high-dilution factors.RESULTS: The detection limit of the method was 0.1μg/g for tin, the precision was less than 5%, the minimum detection concentration was 0.4μg/g, and the measurement range was 12.5-12700μg/g.CONCLUSIONS: The method has simple pretreatment and operation. The analysis efficiency and data quality are an improvement over traditional methods.
BACKGROUND: The main types of primary tin ore occur in skarn, porphyry, cassiterite silicate vein, cassiterite sulfide vein, quartz vein and greisen tin deposits. Tin ores are generally insoluble in hydrochloric acid, nitric acid and aqua regia, and tin ores cannot be dissolved completely when treated with sulfuric acid or hydrofluoric acid. Traditional measurement methods such as phenylfluorone-cetyltrimethyl ammonium bromide spectrophotometry and iodometry have disadvantages, such as the serious interference of the associated elements in the sample, poor stability, high detection limit and low analysis efficiency.OBJECTIVES: To establish a method for the determination of tin in primary ore by Inductively Coupled Plasma-Mass Spectrometry.METHODS: The sample was melted and decomposed by sodium oxide, and leached by hot water, followed by tartaric acid and hydrochloric acid acidification. ~(103)Rh was used as the internal standard element to correct instrument signal drift, and the matrix effect was overcome by high-dilution factors.RESULTS: The detection limit of the method was 0.1μg/g for tin, the precision was less than 5%, the minimum detection concentration was 0.4μg/g, and the measurement range was 12.5-12700μg/g.CONCLUSIONS: The method has simple pretreatment and operation. The analysis efficiency and data quality are an improvement over traditional methods.
引文
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[2] 何小虎,周素莲,韦莉,等.碘量法测定铟锡氧化物靶材废料中锡[J].冶金分析,2013,33(9):65-69.He X H,Zhou S L,Wei L,et al.Determination of tin in indium tin oxide target waste by iodometry[J].Metallurgical Analysis,2013,33(9):65-69.
[3] 叶家瑜.区域地球化学勘查样品分析方法[M].北京:地质出版社,2004.Ye J Y.Sample Analysis Method for Regional Geochemical Exploration[M].Beijing:Geological Publishing House,2004.
[4] 胡永玫.碘量法测定掺锑二氧化锡粉中锡[J].冶金分析,2018,38(11):66-70.Hu Y M.Determination of tin in antimony-doped tin oxide powder by iodometry[J].Metallurgical Analysis,2018,38(11):66-70.
[5] 苏洋,刘红英.苯芴酮-溴化十六烷基三甲基铵分光光度法测定钛铁中锡[J].冶金分析,2015,35(4):65-76.Su Y,Liu H Y.Determination of tin in ferrotitanium by phenylfluorone-cetyl trimethyi ammonium bromide spectrophotometry[J].Metallurgical Analysis,2015,35(4):65-76.
[6] 谭仪文.苯芴酮-溴代十六烷基三甲胺分光光度法测定析出铅中的锡[J].中国有色冶金,2005,4(2):23-25.Tan Y W.Determining tin in deposited lead by benzfluorenone-bromo-hexadecyl-trimethylamine spectrophotometry[J].China Nonferrous Metallurgy,2005,4(2):23-25.
[7] 姚建贞,郝志红,唐瑞玲,等.固体发射光谱法测定地球化学样品中的高含量锡[J].光谱学与光谱分析,2013,33(11):3124-3127.Yao J Z,Hao Z H,Tang R L,et al.Determination of high content of tin in geochemical samples by solid emission spectrometry[J].Spectroscopy and Spectral Analysis,2013,33(11):3124-3127.
[8] 刘江斌,武永芝.原子发射光谱法快速测定矿石中锡[J].冶金分析,2013,33(3):65-68.Liu J B,Wu Y Z.Rapid determination of tin in ore by atomic emission spectrometry[J].Metallurgical Analysis,2013,33(3):65-68.
[9] 辛文芳,李伟,乌晓蒙.发射光谱法测多目标区域地球化学调查中银、硼、锡三元素的分析总结[J].地质与资源,2016,25(4):401-403.Xin W F,Li W,Wu X M.Determination of silver,boron and tin from multi-purpose regional geochemical survey by emission spectrometry[J].Geology and Resources,2016,25(4):401-403.
[10] 胡长春,王沿方,陈作王.电感耦合等离子体原子发射光谱法测定锡铅合金中的锡[J].化学分析计量,2018,27(5):72-75.Hu C C,Wang Y F,Chen Z W.Determination of tin in tin-lead alloy by inductively coupled plasma atomic emission spectrometry[J].Chemical Analysis and Meterage,2018,27(5):72-75.
[11] 李超,刘英波,韩豫萍,等.发射光谱法测定地球化学物料中的微量银锡硼[J].云南冶金,2018,47(3):84-88.Li C,Liu Y B,Han Y P,et al.The determination of trace amount silver,tin,boron in geochemical materials by emission spectrography[J].Yunnan Metallurgy,2018,47(3):84-88.
[12] Roncevic S,Nemet I,Svedruzic L P,et al.Chemical vapour generation for tin determination in high-content calcium matrix by inductively coupled plasma atomic emission spectrometry[J].Croatica Chemica Acta,2014,87(1):17-22.
[13] Afonso D D,Baytak S,Arslan Z.Simultaneous generation of hydrides of bismuth,lead and tin in the presence of ferricyanide and application to determination in biominerals by ICP-AES[J].Journal of Analytical Atomic Spectrometry,2010,25(5):726-729.
[14] Uemoto M,Nagaoka M,Fujinuma H.Interlaboratory testing for the determination of trace amounts of tin and lead in magnesium and magnesium alloys by inductively coupled plasma atomic emission spectrometry[J].Analytical Sciences,2009,25(5):717-721.
[15] 陈安明.电感耦合等离子体原子发射光谱法测定碳钢及生铁中痕量砷锑铋锡铅[J].冶金分析,2007,27(3):68-70.Chen A M.Determination of trace As,Sb,Bi,Sn and Pb in steel and pig iron by inductively coupled plasma-atomic emission spectrometry[J].Metallurgical Analysis,2007,27(3):68-70.
[16] Seco-Gesto E M,Moreda-Pineiro A,Bermejo-Barrera A,et al.Multi-element determination in raft mussels by fast microwave-assisted acid leaching and inductively coupled plasma-optical emission spectrometry[J].Talanta,2007,72(3):1178-1185.
[17] 陈波,胡兰,陈园园,等.地质样品中总锡测定方法的研究进展[J].理化检验(化学分册),2017,53(2):236-241.Chen B,Hu L,Chen Y Y,et al.Recent progress of research on methods for determination of total tin in geological samples[J].Physical Testing and Chemical Analysis (Part B:Chemical Analysis),2017,53(2):236-241.
[18] 郝原芳,刘新,宋丽华,等.电感耦合等离子体质谱法测定铅合金中的微量杂质元素镉和锡[J].岩矿测试,2016,35(4):378-383.Hao Y F,Liu X,Song L H,et al.Determination of trace cadmium and tin in lead alloys by inductively coupled plasma-mass spectrometry[J].Rock and Mineral Analysis,2016,35(4):378-383.
[19] 罗艳,杨侨.碱熔、分离沉淀-电感耦合等离子体质谱法快速测定地球化学样品中的锡[J].分析试验室,2017,36(7):827-830.Luo Y,Yang Q.Alkaline fusion,separate precipitation-inductively coupled plasma spectrometry and rapid measurement of tin from planet chemical samples[J].Chinese Journal of Analysis Laboratory,2017,36(7):827-830.
[20] 侯艳霞,刘庆彬,胡净宇,等.电感耦合等离子体质谱法测定锡粉基体的记忆效应研究[J].冶金分析,2015,35(12):1-4.Hou Y X,Liu Q B,Hu J Y,et al.Study on memory effect of tin powder matrix by inductively coupled plasma mass spectrometry[J].Metallurgical Analysis,2015,35(12):1-4.
[21] 王铁,亢德华,于媛君.电感耦合等离子体质谱法测定锰铁中痕量铅锡锑[J].冶金分析,2013,33(5):13-16.Wang T,Kang D H,Yu Y J.Determination of trace lead,tin and antimony in ferromanganese by inductively coupled plasma mass spectrometry[J].Metallurgical Analysis,2013,33(5):13-16.
[22] Hosick T J,Ingamells R L,Machemer S D.Determina-tion of tin in soil by continuous hydride generation and inductively coupled plasma mass spectrometry[J].Analytica Chimica Acta,2002,456(2):263-269.
[23] Brügmann G,Berger D,Pernicka E.Determination of the tin stable isotopic composition in tin-bearing metals and minerals by MC-ICP-MS[J].Geostandards and Geoanalytical Research,2017,41(3):437-448.
[24] Latkoczy C,Prohaska T,Stingeder G,et al.Simultaneous multi-element analysis of trace elements in soil samples by means of high-resolution inductively coupled plasma sector field mass spectrometry (SF-ICP-MS)[J].Fresenius Journal of Analytical Chemistry,2000,368(2-3):256-262.
[25] Duan H,Gong Z,Yang S.Online photochemical vapour generation of inorganic tin for inductively coupled plasma mass spectrometric detection[J].Journal of Analytical Atomic Spectrometry,2015,30(2):410-416.
[26] 黄超冠,蒙义舒,郭焕花,等.过氧化钠碱熔-电感耦合等离子体发射光谱法测定钛铝合金中的铬铁钼硅[J].岩矿测试,2018,37(1):30-35.Huang C G,Meng Y S,Guo H H,et al.Determination of chromium,iron,molybdenum and silicon in Ti-Al alloy by inductively coupled plasma-optical emission spectrometry with sodium peroxide alkali fusion[J].Rock and Mineral Analysis,2018,37(1):30-35.
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