Synthesis of a New Triazene Reagent and Its Application to the Color Reaction with Gold(Ⅲ) Ion
摘 要
以4-氨基安替比林和对氨基苯磺酸为主要反应物,制备了1-(4-安替比林)-3-(对苯磺酸)三氮烯(ASTA)。采用红外光谱法对ASTA的分子组成及结构作了检测。研究了该试剂与金(Ⅲ)的显色反应。在含有Triton X-100的pH 10.3的硼砂-氢氧化钠缓冲溶液中,ASTA与金(Ⅲ)反应生成配合比为2∶1的橙红色配合物,在其最大吸收波长496 nm处的表观摩尔吸光率为1.8×105L·mol-1·cm-1。金(Ⅲ)的质量浓度在0.06~1.05 mg·L-1范围内与其吸光度呈线性关系,方法的检出限(3S/N)为0.02 mg·L-1。方法用于含金矿样品中金(Ⅲ)的测定,结果与原子吸收光谱法相一致,方法的回收率在109.0%~118.2%之间,相对标准偏差(n=6)小于4.0%。
Abstract
A new reagent, 1-(4-antipyrinyl)-3-(sulfanilic acid)-triazene (ASTA), was synthesized by the reaction between 4-antipyrine and sulfanilic acid. Molecular composition and structure of ASTA were determined by FT-IRS. It was found that in a Na2B4O7-NaOH buffer medium of pH 10.3 containing Triton X-100, a stable coordination complex (R∶Au3+=2∶1) was formed by the reaction of ASTA with gold ion, having the absorption maximum at 496 nm. Linear relationship between values of absorbance and concentration of Au(Ⅲ) ion was obtained in the range of 0.06-1.05 mg·L-1. Detection limit (3S/N) found was 0.02 mg·L-1. The apparent molar absorptivity of the color system was found to be 1.8×105L·mol-1·cm-1. The proposed method was applied to the determination of Au(Ⅲ) in gold ore samples, and the results obtained were in consistency with those obtained by AAS. Values of recovery were found in the range of 109.0%-118.2% and RSD (n=6) was less than 4.0%.
中图分类号 O657.32
所属栏目
基金项目 教育部重点试验室开放基金资助项目(CPEUKF06-04);淮海工学院江苏海洋资源开发研究院基金资助项目
收稿日期 2009/12/7
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备注陈文宾(1970-),男,山东黄县人,副教授,硕士,从事分析化学、环境监测教学与研究工作。
引用该论文: CHEN Wen-bin,ZHEN Qiu-xia,MA Wei-xing,XU Xing-you. Synthesis of a New Triazene Reagent and Its Application to the Color Reaction with Gold(Ⅲ) Ion[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2011, 47(1): 1~4
陈文宾,郑秋霞,马卫兴,许兴友. 一种新的三氮烯试剂的合成并应用于金(Ⅲ)离子的显色反应[J]. 理化检验-化学分册, 2011, 47(1): 1~4
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参考文献
【1】PEI Liang, ZHAO Qiong-ding. Multiwalled carbon nanotubes microcolumn preconcentration and determination of gold in geological and water samples by flame atomic absorption spectrometry[J]. Spectrochimica Acta Part B, 2008,63:714-717.
【2】郑景宜,吕文广.示波极谱珐测定矿石中的金[J].有色金属矿产与勘查, 1998,7(1):51-53.
【3】谭龙华,陈达士,林俊平,等.动力催化-离子选择电极法测定痕量金的研究及应用[J].黄金, 1997,18(5):51-54.
【4】韩鹤友,何治柯,罗庆尧.吐温-80固相化学发光测定痕量金的研究及其应用[J].分析化学, 1998,26(8):974-976.
【5】周文敞,沈友.巯基树脂富集硫代米蚩酮光度法测定矿石中的金[J].黄金, 2002,23(9):48-49.
【6】DEMETRIUS G T, ANASTASIOS V T, PARASKEVAS D T, et al. Highly selective flow injection spectrophotometric determination of gold based on its catalytic effect on the oxidation of variamine blue by potassium iodate in aqueous N,N-dimethylformamide medium[J]. Talanta, 2007,72:277-281.
【7】Al-MEREY R, HARIRI Z, HILAL J A. Selective separation of gold from iron ore samples using ion exchange resin[J]. Microchemical Journal, 2003,75:169-177.
【8】黄运瑞,高书燕.N-丙基-N′-2-(氨基对苯磺酸钠)硫脲与金的显色反应的研究和应用[J].黄金, 2005,26(6):45-47.
【9】李英,张玉泉.新试剂N-烯丙基-N′-2-安替比林基硫脲光度法测定矿样中微量金[J].贵金属, 2006,27(1):46-49.
【10】黄桂芳,王晓艳.四-(4-磺酸基苯基)卟啉与金显色反应研究及其应用[J].分析试验室, 1994,13(1):42-45.
【11】殷志禹,徐其亨.5-(4-羧基苯偶氮)-8-(对甲苯磺酰氨基)喹啉与金显色反应研究及应用[J].岩矿测试, 1996,15(2):117-119.
【12】王海青,岳志劲,刘永文,等.新显色剂2-羟基-3-磺酸基-5-硝基苯基重氮氨基偶氮苯与汞的显色反应研究[J].光谱实验室, 2005,22(5):966-968.
【13】王贵方,刘立新.2,4,4′-三硝基苯基重氮氨基偶氮苯光度法测定微量钯[J].冶金分析, 2007,27(2):48-50.
【14】宾高远,曹秋娥,李崇宁,等.1-(4-氨替比林)-3-(2-噻唑)-三氮烯的合成及其光度法测定钯(Ⅱ)[J].分析试验室, 2006,25(5):19-21.
【15】王贵芳,邢云.4-(4-氯苯重氮氨基)-硝基偶氮苯的合成及其与镉(Ⅱ)的显色反应[J].冶金分析, 2009,29(5):20-23.
【16】赵霞,刘鹏,丁中涛,等.新试剂1-(4-安替比林)-3-(对苯甲酸)-三氮烯的合成及其应用研究[J].黄金, 2007,28(9):53-55.
【2】郑景宜,吕文广.示波极谱珐测定矿石中的金[J].有色金属矿产与勘查, 1998,7(1):51-53.
【3】谭龙华,陈达士,林俊平,等.动力催化-离子选择电极法测定痕量金的研究及应用[J].黄金, 1997,18(5):51-54.
【4】韩鹤友,何治柯,罗庆尧.吐温-80固相化学发光测定痕量金的研究及其应用[J].分析化学, 1998,26(8):974-976.
【5】周文敞,沈友.巯基树脂富集硫代米蚩酮光度法测定矿石中的金[J].黄金, 2002,23(9):48-49.
【6】DEMETRIUS G T, ANASTASIOS V T, PARASKEVAS D T, et al. Highly selective flow injection spectrophotometric determination of gold based on its catalytic effect on the oxidation of variamine blue by potassium iodate in aqueous N,N-dimethylformamide medium[J]. Talanta, 2007,72:277-281.
【7】Al-MEREY R, HARIRI Z, HILAL J A. Selective separation of gold from iron ore samples using ion exchange resin[J]. Microchemical Journal, 2003,75:169-177.
【8】黄运瑞,高书燕.N-丙基-N′-2-(氨基对苯磺酸钠)硫脲与金的显色反应的研究和应用[J].黄金, 2005,26(6):45-47.
【9】李英,张玉泉.新试剂N-烯丙基-N′-2-安替比林基硫脲光度法测定矿样中微量金[J].贵金属, 2006,27(1):46-49.
【10】黄桂芳,王晓艳.四-(4-磺酸基苯基)卟啉与金显色反应研究及其应用[J].分析试验室, 1994,13(1):42-45.
【11】殷志禹,徐其亨.5-(4-羧基苯偶氮)-8-(对甲苯磺酰氨基)喹啉与金显色反应研究及应用[J].岩矿测试, 1996,15(2):117-119.
【12】王海青,岳志劲,刘永文,等.新显色剂2-羟基-3-磺酸基-5-硝基苯基重氮氨基偶氮苯与汞的显色反应研究[J].光谱实验室, 2005,22(5):966-968.
【13】王贵方,刘立新.2,4,4′-三硝基苯基重氮氨基偶氮苯光度法测定微量钯[J].冶金分析, 2007,27(2):48-50.
【14】宾高远,曹秋娥,李崇宁,等.1-(4-氨替比林)-3-(2-噻唑)-三氮烯的合成及其光度法测定钯(Ⅱ)[J].分析试验室, 2006,25(5):19-21.
【15】王贵芳,邢云.4-(4-氯苯重氮氨基)-硝基偶氮苯的合成及其与镉(Ⅱ)的显色反应[J].冶金分析, 2009,29(5):20-23.
【16】赵霞,刘鹏,丁中涛,等.新试剂1-(4-安替比林)-3-(对苯甲酸)-三氮烯的合成及其应用研究[J].黄金, 2007,28(9):53-55.
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