土壤样品中痕量价态金石墨炉原子吸收光谱法的测定及分离方法实验研究
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摘要
在前人研究泡塑吸附金分离的基础上,用聚氨酯泡沫塑料吸附,利用石墨炉原子吸收法测定了痕量价态金的含量,探讨了溶矿介质、解脱时间、吸附温度、Fe~(3+)加入量等对测定结果的影响,确定了最佳测定条件,详细讨论了Fe~(3+)在溶矿和吸附过程中的作用,并将该方法用于土壤中痕量价态金的测定。方法检出限为0. 01 ng/g,测定范围为0. 03～300 ng/g,价态金回收率分别是Au~(3+)97. 3%、Au~+95. 8%、Au098. 9%,价态金分离精密度(RSD,n=12)为7. 3%～18. 8%。用石墨炉原子吸收光谱法测定价态金,不但有效地抑制了共存元素的干扰,而且能降低检出限,提高灵敏度和准确度,自动化进样减少了劳动强度,提高了分析测试效率,适合大批量样品的测试。
The effects of dissolution medium,liberation time,adsorption temperature and Fe~(3+)addition amount on the determination results were discussed in this paper. The best determination conditions were determined,and the role of Fe~(3+)in ore dissolution and adsorption was discussed in detail. A trace amount of valence gold was separated and adsorbed by polyurethane foam. Gold was directly determined by graphite furnace atomic absorption spectrometry with thiourea solution to remove gold. The method is suitable for the determination of trace valence gold in stream sediments,soil and rocks. The detection limit of the method is 0. 01 ng/g,the determination range is 0. 03～ 300 ng/g,the recovery rates of valence gold are Au~(3+)97. 3%,Au~+95. 8%,Au098. 9%,respectively,and the separation precision( RSD,n = 12) of valence gold is 7. 3% ～ 18. 8%. Determination of valence gold by graphite furnace atomic absorption spectrometry can not only effectively inhibit interference of coexisting elements,but also reduce detection limit and improve sensitivity and accuracy. Automatic sample introduction reduces labor intensity and improves analysis and testing efficiency,thus suitable for testing large quantities of samples.
The effects of dissolution medium,liberation time,adsorption temperature and Fe~(3+)addition amount on the determination results were discussed in this paper. The best determination conditions were determined,and the role of Fe~(3+)in ore dissolution and adsorption was discussed in detail. A trace amount of valence gold was separated and adsorbed by polyurethane foam. Gold was directly determined by graphite furnace atomic absorption spectrometry with thiourea solution to remove gold. The method is suitable for the determination of trace valence gold in stream sediments,soil and rocks. The detection limit of the method is 0. 01 ng/g,the determination range is 0. 03～ 300 ng/g,the recovery rates of valence gold are Au~(3+)97. 3%,Au~+95. 8%,Au098. 9%,respectively,and the separation precision( RSD,n = 12) of valence gold is 7. 3% ～ 18. 8%. Determination of valence gold by graphite furnace atomic absorption spectrometry can not only effectively inhibit interference of coexisting elements,but also reduce detection limit and improve sensitivity and accuracy. Automatic sample introduction reduces labor intensity and improves analysis and testing efficiency,thus suitable for testing large quantities of samples.
引文
Gong Meiling.1991.Discussion on determination of trace gold by foam adsorption chemical spectrometry[J].Metallurgical Analysis,11(3):1~5(in Chinese with English abstract).
Sha Yanmei and Zhou Yingfen.1997.Improvement of separation and analysis methods of trace gold in geochemical exploration samples[J].Geological Laboratory,13(2):16~18(in Chinese with English abstract).
Song Lihua and Jin Yi.2009.Determination of trace gold in geochemical exploration samples by graphite furnace atomic absorption spectrometry[J].Physical and Chemical Examination(Chemical Division),45(6):692~694(in Chinese with English abstract).
Sun Xiaoling,Yu Zhaoshui and Zhang Qin.2002.Determination of ultra trace gold in exploration geochemical samples by foam adsorption enrichmentgraphite furnace atomic absorption spectrometry[J].Rock and Mineral Testing,19(4):266~270(in Chinese with English abstract).
Wang Zhu,Shao Bei,Wu Guodong,et al.2010.Determination of trace gold in geochemical exploration samples by foam adsorption-graphite furnace atomic absorption s Spectrometry under low oxygen and low partial pressure environment[J].Rock and Mineral Testing,29(3):282~286(in Chinese with English abstract).
Xiong Zhaochun.1993.Study on adsorption and separation of trace valuable gold on carbon foam[J].Rock and Mineral Testing,12(4):255~258(in Chinese with English abstract).
Xiong Zhaochun.1998.Discussion on valence separation of trace gold in natural medium[J].Rock and Mineral Testing,14(4):261~263(in Chinese with English abstract).
Xiong Zhaochun,Peng Zhenying and Zhou Yingfen.1995.Separation and analysis of trace gold and its role in exploration geochemistry[J].Henan Geology,13(2):145~150(in Chinese with English abstract).
Yang Liqin,Wei Wanshun,Lu Yanming,et al.2002.Analysis and research of valence gold in stream sediments and soils in Plateau Lakes and Marshes[J].Gold Science and Technology,10(16):39~44(in Chinese with English abstract).
Zhao Hong.2001.Determination of trace gold in foam with chemical spectrometric method[J].Nonferrous Metals and Metallurgy,17(4):39~41(in Chinese with English abstract).
Zou Haifeng,Tian Liyu,Jiang Guilan,et al.2001.Study and application of adsorption properties of polyurethane foam to gold with different valence[J].Rock and Mineral Testing,20(3):187~190(in Chinese with English abstract).
龚美菱.1991.地质样品中痕量金的物相分析[J].冶金分析,11(3):1~5.
沙艳梅,周应芬.1997.化探样品中痕量金价态分离与分析方法改进[J].地质实验室,13(2):16~18.
宋丽华,金一.2009.石墨炉原子吸收光谱法测定化探样品中痕量金[J].理化检验(化学分册),45(6):692~694.
孙晓玲,于照水,张勤.2002.泡沫塑料吸附富集-石墨炉原子吸收光谱法测定勘查地球化学样品中超痕量金[J].岩矿测试,19(4):266~270.
王祝,邵蓓,邬国栋,等.2010.低氧低分压环境下泡塑吸附-石墨炉原子吸收光谱法测定化探样品中的痕量金[J].岩矿测试,29(3):282~286.
熊昭春.1993.痕量价态金的载炭泡塑吸附分离研究[J].岩矿测试,12(4):255~258.
熊昭春.1998.关于天然介质中痕量金的价态分离的讨论[J].岩矿测试,14(4):261~263.
熊昭春,彭振英,周应芬.1995.痕量金价态分离与分析及在勘查地球化学研究中的作用[J].河南地质,13(2):145~150.
杨理勤,卫万顺,路彦明,等.2002.高原湖沼区水系沉积物和土壤中价态金的分析研究[J].黄金科学技术,10(16):39~44.
赵虹.2001.泡塑吸附化学光谱法测定痕量金的探讨[J].有色矿冶,17(4):39~41.
邹海峰,田丽玉,姜桂兰,等.2001.聚氨酯泡塑对不同价态金吸附性能的研究及应用[J].岩矿测试,20(3):187~190.
Sha Yanmei and Zhou Yingfen.1997.Improvement of separation and analysis methods of trace gold in geochemical exploration samples[J].Geological Laboratory,13(2):16~18(in Chinese with English abstract).
Song Lihua and Jin Yi.2009.Determination of trace gold in geochemical exploration samples by graphite furnace atomic absorption spectrometry[J].Physical and Chemical Examination(Chemical Division),45(6):692~694(in Chinese with English abstract).
Sun Xiaoling,Yu Zhaoshui and Zhang Qin.2002.Determination of ultra trace gold in exploration geochemical samples by foam adsorption enrichmentgraphite furnace atomic absorption spectrometry[J].Rock and Mineral Testing,19(4):266~270(in Chinese with English abstract).
Wang Zhu,Shao Bei,Wu Guodong,et al.2010.Determination of trace gold in geochemical exploration samples by foam adsorption-graphite furnace atomic absorption s Spectrometry under low oxygen and low partial pressure environment[J].Rock and Mineral Testing,29(3):282~286(in Chinese with English abstract).
Xiong Zhaochun.1993.Study on adsorption and separation of trace valuable gold on carbon foam[J].Rock and Mineral Testing,12(4):255~258(in Chinese with English abstract).
Xiong Zhaochun.1998.Discussion on valence separation of trace gold in natural medium[J].Rock and Mineral Testing,14(4):261~263(in Chinese with English abstract).
Xiong Zhaochun,Peng Zhenying and Zhou Yingfen.1995.Separation and analysis of trace gold and its role in exploration geochemistry[J].Henan Geology,13(2):145~150(in Chinese with English abstract).
Yang Liqin,Wei Wanshun,Lu Yanming,et al.2002.Analysis and research of valence gold in stream sediments and soils in Plateau Lakes and Marshes[J].Gold Science and Technology,10(16):39~44(in Chinese with English abstract).
Zhao Hong.2001.Determination of trace gold in foam with chemical spectrometric method[J].Nonferrous Metals and Metallurgy,17(4):39~41(in Chinese with English abstract).
Zou Haifeng,Tian Liyu,Jiang Guilan,et al.2001.Study and application of adsorption properties of polyurethane foam to gold with different valence[J].Rock and Mineral Testing,20(3):187~190(in Chinese with English abstract).
龚美菱.1991.地质样品中痕量金的物相分析[J].冶金分析,11(3):1~5.
沙艳梅,周应芬.1997.化探样品中痕量金价态分离与分析方法改进[J].地质实验室,13(2):16~18.
宋丽华,金一.2009.石墨炉原子吸收光谱法测定化探样品中痕量金[J].理化检验(化学分册),45(6):692~694.
孙晓玲,于照水,张勤.2002.泡沫塑料吸附富集-石墨炉原子吸收光谱法测定勘查地球化学样品中超痕量金[J].岩矿测试,19(4):266~270.
王祝,邵蓓,邬国栋,等.2010.低氧低分压环境下泡塑吸附-石墨炉原子吸收光谱法测定化探样品中的痕量金[J].岩矿测试,29(3):282~286.
熊昭春.1993.痕量价态金的载炭泡塑吸附分离研究[J].岩矿测试,12(4):255~258.
熊昭春.1998.关于天然介质中痕量金的价态分离的讨论[J].岩矿测试,14(4):261~263.
熊昭春,彭振英,周应芬.1995.痕量金价态分离与分析及在勘查地球化学研究中的作用[J].河南地质,13(2):145~150.
杨理勤,卫万顺,路彦明,等.2002.高原湖沼区水系沉积物和土壤中价态金的分析研究[J].黄金科学技术,10(16):39~44.
赵虹.2001.泡塑吸附化学光谱法测定痕量金的探讨[J].有色矿冶,17(4):39~41.
邹海峰,田丽玉,姜桂兰,等.2001.聚氨酯泡塑对不同价态金吸附性能的研究及应用[J].岩矿测试,20(3):187~190.