微波消解-石墨炉原子吸收光谱法测定痕量银的研究
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摘要
传统的应用石墨炉原子吸收光谱法测定化探样品中的痕量银,一般采用盐酸-硝酸-氢氟酸-高氯酸电热板加热溶样,使用铱、铂为基体改进剂,但存在分析流程繁琐、成本高等缺点。相比于电热板消解法,微波消解技术的高压密闭消解和微波快速加热等特点,具有酸用量少、消解完全、消解过程损失少等优点。本文对传统的微波消解和仪器工作参数进行了改良,确定了最佳测定条件。建立了HNO_3-H_2O_2高压密闭消解样品,石墨炉原子吸收法测定水系沉积物、土壤、岩石中痕量银的方法。采用65%的HNO_3和H_2O_2微波消解溶样,加入12 g/L硫脲为介质,消除了基体干扰。方法检出限为0.018μg/g,将所建立的分析方法用于沉积物标准物质(GBW07309、GBW07311)、土壤标准物质(GBW07402、GBW07404)和岩石标准物质(GBW07103、GBW07104)验证,结果显示测定值与推荐值吻合,准确度△lg C(GBW)≤±0.024、RE(GBW)≤±5.71%,精密度RSD(GBW)≤5.97%。该分析方法适用于大批化探样品中痕量银的测定。
A method for determination of trace silver in stream sediments,soils and rocks by graphite furnace atomic absorption spectrometry(HNO3-H2 O2) was developed in this study.The microwave digestion and instrument working parameters were optimized and the optimum conditions were determined.In traditional method,determination of trace silver in geochemical exploration samples is conducted by graphite furnace atomic absorption spectrometry through heating the hydrochloric acid nitric acid hydrofluoric acid and perchloric acid electric heating plate digestion,with iridium,platinum as matrix modifier; the analytical process is complex,and the cost is high.Compared with the electric heating plate digestion method,the microwave digestion technique is characterized by highpressure closed digestion with small amounts of acid,complete digestion and less loss in the digestion process.In this paper,HNO_3(65%) and H_2O_2 microwave digestion was used to dissolve the matrix interference by adding 12 g/L thiourea as the medium.The detection limit was 0.018 μg/g,and the analytical method was used for verification of sediment reference materials(GBW07309,GBW07311),soil standard substance(GBW07402,GBW07404) and rock reference materials(GBW07103,GBW07104).The measured results were consistent with the recommended values,the accuracy of lg C(GBW) is △lg C(GBW) ≤ ± 0.024,RE(GBW) ≤ ± 5.71%,the precision of RSD(GBW) is ≤5.97%.The method is suitable for the determination of trace silver in a large amount of geochemical samples.
A method for determination of trace silver in stream sediments,soils and rocks by graphite furnace atomic absorption spectrometry(HNO3-H2 O2) was developed in this study.The microwave digestion and instrument working parameters were optimized and the optimum conditions were determined.In traditional method,determination of trace silver in geochemical exploration samples is conducted by graphite furnace atomic absorption spectrometry through heating the hydrochloric acid nitric acid hydrofluoric acid and perchloric acid electric heating plate digestion,with iridium,platinum as matrix modifier; the analytical process is complex,and the cost is high.Compared with the electric heating plate digestion method,the microwave digestion technique is characterized by highpressure closed digestion with small amounts of acid,complete digestion and less loss in the digestion process.In this paper,HNO_3(65%) and H_2O_2 microwave digestion was used to dissolve the matrix interference by adding 12 g/L thiourea as the medium.The detection limit was 0.018 μg/g,and the analytical method was used for verification of sediment reference materials(GBW07309,GBW07311),soil standard substance(GBW07402,GBW07404) and rock reference materials(GBW07103,GBW07104).The measured results were consistent with the recommended values,the accuracy of lg C(GBW) is △lg C(GBW) ≤ ± 0.024,RE(GBW) ≤ ± 5.71%,the precision of RSD(GBW) is ≤5.97%.The method is suitable for the determination of trace silver in a large amount of geochemical samples.
引文
Chen Xue,Liu Yang,Nie Fenglian,et al.2011.Determination of trace silver in geochemical exploration samples by graphite furnace atomic absorption spectrometry[J].Gold,32(3):63~65(in Chinese with English abstract).
Chen Yujing,Wang Yubao and Li Guihua.2007.Determination of trace silver in geological samples of gold mine by microwave digestion-catalytic linetic spectrophotometry[J].Metallurgical Analysis,27(4):48~50(in Chinese with English abstract).
Dai Sufang and Zheng Hao.2000.Determination of silver in various ores by atomic absorption spectrometry in perchlorate+tartaric acid+thiourea medium[J].Rock and Mineral Testing,19(4):301~303(in Chinese with English abstract).
Huang Jianhui and Lu Handi.2014.Determination of trace silver in geological samples by graphite furnace atomic absorption spectrometry[J].Minerals and Geology,28(3):381~384(in Chinese with English abstract).
Li Jian.1997.Study on cobalt and magnesium nitrate as universal matrix modifiers[J].Physical and Chemical Examination:Chemical Division,33(4):160~163(in Chinese with English abstract).
Li Wei and Yu Lincheng.2011.Continuous determination of six metals in drinking water by graphite furnace atomic absorption spectrometry[J].Chinese Journal of Health Laboratory Technology,21(8):2 094~2 095(in Chinese).
Niu Zhanhai,Lin Yan and He Duhu.2001.Determination of silver and cadmium in geochemical exploration samples by graphite furnace atomic absorption spectrometry[J].Metallurgical Analysis,21(6):61~63(in Chinese with English abstract).
Pan Wei.2016.Determination of trace silver in soil by microwave digestion-graphite furnace atomic absorption spectrometry[J].Pollution Control Technology,29(4):68~70(in Chinese with English abstract).
Su Dan,Liu Xiangdong and Zhang Kaige.2015.Determination of trace silver in geological samples by graphite furnace atomic absorption spectrometry[J].Gold,36(10):85~88(in Chinese with English abstract).
Wang Yunling,Sun Naiming and Chen Yuanmao.2013.Determination of silver in geological samples by microwave digestion-flame atomic absorption spectrometry[J].Spectral Laboratory,30(2):913~915(in Chinese with English abstract).
Xu Qiang,Qu Rongjun,Liu Yingxia,et al.2005.Determination of trace silver in geological samples by micro-column separation and enrichment with triethylenetetramine chelating resin-Flame atomic absorption apectrometry[J].Chemical World,46(3):151~154(in Chinese with English abstract).
Ye Jiayu and Jiang Baolin.2004.Analysis Methods of Regional Geochemical Exploration Samples[M].Beijing:Geological Publishing House,123,352(in Chinese).
Zhang Xuemei.2006.Determination of silver,boron,tin,molybdenum and lead in exploration geochemical samples by emission spectrometry[J].Rock and Mineral Testing,25(4):323~326(in Chinese with English abstract).
陈雪,刘烊,聂凤莲,等.2011.石墨炉原子吸收法测定化探样品中痕量银[J].黄金,32(3):63~65.
陈玉静,王玉宝,李桂华.2007.微波消解-催化动力学光度法测定金矿地质样品中痕量银[J].冶金分析,27(4):48~50.
代素芳,郑浩.2000.高氯酸+酒石酸+硫脲介质中原子吸收光谱法测定多种矿石中的银[J].岩矿测试,19(4):301~303.
黄俭惠,卢汉堤.2014.石墨炉原子吸收光谱法测定地质样品中痕量银[J].矿产与地质,28(3):381~384.
李建.1997.钴和硝酸镁作为通用基体改进剂的研究[J].理化检验:化学分册,33(4):160~163.
李维,余林成.2011.石墨炉原子吸收光谱法连续测定饮水中6种金属含量[J].中国卫生检验杂志,21(8):2 094~2 095.
牛占海,林焰,和督虎.2001.石墨炉原子吸收法测定化探样品中银和镉[J].冶金分析,21(6):61~63.
潘伟.2016.微波消解-石墨炉原子吸收法测定土壤中痕量银[J].污染防治技术,29(4):68~70.
苏丹,刘向东,张凯歌.2015.石墨炉原子吸收法测定地质样品中痕量银[J].黄金,36(10):85~88.
王云玲,孙乃明,陈远茂.2013.微波消解-火焰原子吸收光谱法测定地质样品中的银[J].光谱实验室,30(2):913~915.
徐强,曲荣君,刘英霞,等.2005.三乙烯四胺型螯合树脂微柱分离富集-火焰原子吸收光谱法测定地质样品痕量银[J].化学世界,46(3):151~154.
叶家瑜,江宝林.2004.区域地球化学勘查样品分析方法[M].北京:地质出版社,123,352.
张雪梅.2006.发射光谱法测定勘查地球化学样品中银硼锡钼铅[J].岩矿测试,25(4):323~326.
(1)国家地质实验测试中心. 2006. DZ/T0130. 4-2006《地质矿产实验室测试质量管理规范》第4部分:区域地球化学调查(1∶50 000)和(1∶20 000)样品化学成分分析.中国标准出版社发行.
Chen Yujing,Wang Yubao and Li Guihua.2007.Determination of trace silver in geological samples of gold mine by microwave digestion-catalytic linetic spectrophotometry[J].Metallurgical Analysis,27(4):48~50(in Chinese with English abstract).
Dai Sufang and Zheng Hao.2000.Determination of silver in various ores by atomic absorption spectrometry in perchlorate+tartaric acid+thiourea medium[J].Rock and Mineral Testing,19(4):301~303(in Chinese with English abstract).
Huang Jianhui and Lu Handi.2014.Determination of trace silver in geological samples by graphite furnace atomic absorption spectrometry[J].Minerals and Geology,28(3):381~384(in Chinese with English abstract).
Li Jian.1997.Study on cobalt and magnesium nitrate as universal matrix modifiers[J].Physical and Chemical Examination:Chemical Division,33(4):160~163(in Chinese with English abstract).
Li Wei and Yu Lincheng.2011.Continuous determination of six metals in drinking water by graphite furnace atomic absorption spectrometry[J].Chinese Journal of Health Laboratory Technology,21(8):2 094~2 095(in Chinese).
Niu Zhanhai,Lin Yan and He Duhu.2001.Determination of silver and cadmium in geochemical exploration samples by graphite furnace atomic absorption spectrometry[J].Metallurgical Analysis,21(6):61~63(in Chinese with English abstract).
Pan Wei.2016.Determination of trace silver in soil by microwave digestion-graphite furnace atomic absorption spectrometry[J].Pollution Control Technology,29(4):68~70(in Chinese with English abstract).
Su Dan,Liu Xiangdong and Zhang Kaige.2015.Determination of trace silver in geological samples by graphite furnace atomic absorption spectrometry[J].Gold,36(10):85~88(in Chinese with English abstract).
Wang Yunling,Sun Naiming and Chen Yuanmao.2013.Determination of silver in geological samples by microwave digestion-flame atomic absorption spectrometry[J].Spectral Laboratory,30(2):913~915(in Chinese with English abstract).
Xu Qiang,Qu Rongjun,Liu Yingxia,et al.2005.Determination of trace silver in geological samples by micro-column separation and enrichment with triethylenetetramine chelating resin-Flame atomic absorption apectrometry[J].Chemical World,46(3):151~154(in Chinese with English abstract).
Ye Jiayu and Jiang Baolin.2004.Analysis Methods of Regional Geochemical Exploration Samples[M].Beijing:Geological Publishing House,123,352(in Chinese).
Zhang Xuemei.2006.Determination of silver,boron,tin,molybdenum and lead in exploration geochemical samples by emission spectrometry[J].Rock and Mineral Testing,25(4):323~326(in Chinese with English abstract).
陈雪,刘烊,聂凤莲,等.2011.石墨炉原子吸收法测定化探样品中痕量银[J].黄金,32(3):63~65.
陈玉静,王玉宝,李桂华.2007.微波消解-催化动力学光度法测定金矿地质样品中痕量银[J].冶金分析,27(4):48~50.
代素芳,郑浩.2000.高氯酸+酒石酸+硫脲介质中原子吸收光谱法测定多种矿石中的银[J].岩矿测试,19(4):301~303.
黄俭惠,卢汉堤.2014.石墨炉原子吸收光谱法测定地质样品中痕量银[J].矿产与地质,28(3):381~384.
李建.1997.钴和硝酸镁作为通用基体改进剂的研究[J].理化检验:化学分册,33(4):160~163.
李维,余林成.2011.石墨炉原子吸收光谱法连续测定饮水中6种金属含量[J].中国卫生检验杂志,21(8):2 094~2 095.
牛占海,林焰,和督虎.2001.石墨炉原子吸收法测定化探样品中银和镉[J].冶金分析,21(6):61~63.
潘伟.2016.微波消解-石墨炉原子吸收法测定土壤中痕量银[J].污染防治技术,29(4):68~70.
苏丹,刘向东,张凯歌.2015.石墨炉原子吸收法测定地质样品中痕量银[J].黄金,36(10):85~88.
王云玲,孙乃明,陈远茂.2013.微波消解-火焰原子吸收光谱法测定地质样品中的银[J].光谱实验室,30(2):913~915.
徐强,曲荣君,刘英霞,等.2005.三乙烯四胺型螯合树脂微柱分离富集-火焰原子吸收光谱法测定地质样品痕量银[J].化学世界,46(3):151~154.
叶家瑜,江宝林.2004.区域地球化学勘查样品分析方法[M].北京:地质出版社,123,352.
张雪梅.2006.发射光谱法测定勘查地球化学样品中银硼锡钼铅[J].岩矿测试,25(4):323~326.
(1)国家地质实验测试中心. 2006. DZ/T0130. 4-2006《地质矿产实验室测试质量管理规范》第4部分:区域地球化学调查(1∶50 000)和(1∶20 000)样品化学成分分析.中国标准出版社发行.
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