新试剂2-(5-碘-2-吡啶偶氮)-5-二甲氨基苯胺 分光光度法测定矿石中的钴
Spectrophotometric Determination of Cobalt in Ores with a New Regent 2-(5-Iodine-2-Pyridylazo)-5-Dimethylaminoaniline
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摘要: 对新试剂2-(5-碘-2-吡啶偶氮)-5-二甲氨基苯胺(5-I-PADMA)与钴(Ⅱ)的显色反应进行试验。结果表明,在pH为4.2~9.2时,钴(II)与试剂形成1∶2红紫色配合物,配合物有两个吸收峰,分别位于554 nm和602 nm处;钴配合物形成后非常稳定,当以无机酸酸化,由于质子化作用,配合物转化成另一种具有较高吸收特性绿蓝色稳定的双质子化型体,其吸收峰分别红移至568 nm和614 nm,适宜的酸浓度范围分别为:0.3~7.0 mol/L 盐酸、0.3~6.0 mol/L 高氯酸、0.3~4.2 mol/L硫酸和0.7~7.3 mol/L磷酸。配合物表观摩尔吸光系数ε614 nm为1.21×105 L/(mol·cm)。钴含量在0~0.5 μg/mL内遵循比尔定律。方法简便,快速,且具有良好的选择性,已成功地应用于矿样中微量钴的测定,结果满意。
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关键词:
- 2-(5-碘-2-吡啶偶氮)-5-二甲氨基苯胺 /
- 钴 /
- 矿石 /
- 分光光度法
Abstract: High sensitive color reaction of a new reagent of 2-(5-iodine-2-pyridylazo)-5-dimethylaminoaniline (5-I-PADMA) with cobalt (Ⅱ) has been studied. In pH 4.2~9.2 medium, 5-I-PADMA reacts with cobalt (Ⅱ) to form a violet-red complex exhibiting two absorption peaks at 554 nm and 602 nm respectively. This complex can be changed into another stable blue-green diproton species after acidification with mineral acids, and the two absorption peaks shift to 568 nm and 614 nm respectively. This species possesses a higher absorption characteristic. The optimal acidification conditions were found to be 0.3~7.0 mol/L HCl, 0.3~6.0 mol/L HClO4, 0.3~4.2 mol/L H2SO4 and 0.7~7.3 mol/L H3PO4, respectively. The apparent molar absorptivity ε614 nm is 1.21×105 L /( mol· cm). Beer's law is obeyed in the range of 0~0.5 μg/mL for Co. The method provides high sensitivity, high selectivity and less interference. The method has been successfully applied to the determination of cobalt in ores with satisfactory results.-
Keywords:
- 2-(5-iodine-2-pyridylazo)-5-dimethylaminoaniline /
- cobalt /
- ore /
- spectrophotometry
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杨晓慧,韩权,李海维.4-(5-硝基-2-吡啶偶氮)-1,3-二氨基苯的合成及其与钴的显色反应[J].冶金分析,2008,28(4):23-26. Yamini Y, Hosseini M H, Morsali A. Soild phase extraction and flame atomic absorption spectrometric determination of trace amounts of zinc and cobalt ions in water samples[J]. Mikrochimica Acta,2004,146:67-72. Yamini Y, Hosseini M H, Morsali A. Soild phase extraction and flame atomic absorption spectrometric determination of trace amounts of zinc and cobalt ions in water samples[J]. Mikrochimica Acta,2004,146:67-72.
Baghban N, Shabani A M H, Dadfarnia S, Jafari A A. Flame atomic absorption spectrometric determination of trace amounts of cobalt after cloud point extraction as 2- phenol complex[J].Journal of the Brazilian Chemical Society, 2009,20(5):832-838. Baghban N, Shabani A M H, Dadfarnia S, Jafari A A. Flame atomic absorption spectrometric determination of trace amounts of cobalt after cloud point extraction as 2- phenol complex[J].Journal of the Brazilian Chemical Society, 2009,20(5):832-838.
El-Defrawy M M M, Posta J, Beck M T. Elimination of the interfering effects of ligands in the determination of cobalt by atomic absorption spectrometry[J].Analytica Chimica Acta,1980,115:155-161. El-Defrawy M M M, Posta J, Beck M T. Elimination of the interfering effects of ligands in the determination of cobalt by atomic absorption spectrometry[J].Analytica Chimica Acta,1980,115:155-161.
Rao K S, Balaji T, Rao T P, Babu Y, Naidu G R K. Determination of iron, cobalt, nickel, manganese, zinc, copper, cadmium and lead in human hair by inductively coupled plasma-atomic emission spectrometry[J]. Spectrochimica Acta:Part B,2002,57(8):1333-1338. Rao K S, Balaji T, Rao T P, Babu Y, Naidu G R K. Determination of iron, cobalt, nickel, manganese, zinc, copper, cadmium and lead in human hair by inductively coupled plasma-atomic emission spectrometry[J]. Spectrochimica Acta:Part B,2002,57(8):1333-1338.
杜芳艳,郑保炜,张亚.钴(Ⅱ)与3-噻唑偶氮-氨基苯酚生成的络合物的极谱吸附波[J].理化检验:化学分册,2008,44(3):255-257. 刘彬,孙家娟,王晓玲,杨连利,赵群会.钴(Ⅱ)与5-(5-硝基-2-吡啶偶氮)-2,4-二氨基甲苯络合物吸附波及其应用[J].分析测试学报,2003,22(1):48-51. Khuhawar M Y, Laniwani S N. High performance liquid chro-matographic liquid chromatographic separation and UV determination of cobalt, copper iron and platinum in pharmaceutical preparation using bis(isovalerylacetone)ethylenedimine as complexing reagent[J]. Mikrochimica Acta, 1998,129:65-70. Khuhawar M Y, Laniwani S N. High performance liquid chro-matographic liquid chromatographic separation and UV determination of cobalt, copper iron and platinum in pharmaceutical preparation using bis(isovalerylacetone)ethylenedimine as complexing reagent[J]. Mikrochimica Acta, 1998,129:65-70.
Barany E, Bergdahl I A, Bratteby L E, Lundh T, Samuelson G, Schütz A, Skerfving S, Oskarsson A. Trace element levels in whole blood and serum from Swedish adolescents[J].Science of the Total Environment,2002,286(1-3):129-141. Barany E, Bergdahl I A, Bratteby L E, Lundh T, Samuelson G, Schütz A, Skerfving S, Oskarsson A. Trace element levels in whole blood and serum from Swedish adolescents[J].Science of the Total Environment,2002,286(1-3):129-141.
李俊,张兆威,张华山.meso-四(3-氯-4磺酸苯基)卟啉与钴(Ⅱ)显色反应的光度法研究[J].分析科学学报,2001,17(5):387-390. 汤福隆,王莉红.meso-四(2-氨基-5-磺酸苯基)卟啉的合成及其与钴显色反应的研究[J].化学试剂,1993,15(6):324-326. 周能,赵书林,李舒婷.1-(6-硝基-2-苯并噻唑)-3-(5-溴-8-喹啉)-三氮烯与钴(Ⅱ)的高灵敏显色反应及其应用[J].分析试验室,2007,26(3):66-68. 章汝平,何立芳,蔡玲燕.1-(5-硝基-3-苯并异噻唑)-3- -三氮烯的合成及与钴的显色反应[J].冶金分析,2006,26(5):48-50. 杨明华,王智敏,张春牛,王慕华.1-(6-硝基-2-苯并噻唑)-3-(4-硝基苯)-三氮烯与钴的显色反应[J].浙江师范大学学报:自然科学版,2004,27(3):265-267. Li Z, Guanyu Y, Wang B, Jiang C, Yin G. Study of 2-(2-quinolinylazo)-5-dimethylamino-benzoic acid as a new chromogenic reagent for the spectrophotometric determination of cobalt[J].Analytical and Bioanalytical Chemistry, 2002,374(7):1318-1324. Li Z, Guanyu Y, Wang B, Jiang C, Yin G. Study of 2-(2-quinolinylazo)-5-dimethylamino-benzoic acid as a new chromogenic reagent for the spectrophotometric determination of cobalt[J].Analytical and Bioanalytical Chemistry, 2002,374(7):1318-1324.
Zyryanov A B, Baykov A A. Determination of Mn(Ⅱ) and Co(Ⅱ) with arsenazo (Ⅲ) [J].Biochemistry,2002,67(6):635-639. Zyryanov A B, Baykov A A. Determination of Mn(Ⅱ) and Co(Ⅱ) with arsenazo (Ⅲ) [J].Biochemistry,2002,67(6):635-639.
刘彬,孙家娟.吡啶偶氮类试剂在分析化学中的应用进展[J].冶金分析,2001,21(5): 36-44. Shibata S, Furukawa M, Goto K. Spectrophotometric studies on the reaction of cobalt with 4-(2-pyridylazo)-1,3-diaminobenzene and its halogen derivatires[J].Analytica Chimica Acta,1974,71(1):85-96. Shibata S, Furukawa M, Goto K. Spectrophotometric studies on the reaction of cobalt with 4-(2-pyridylazo)-1,3-diaminobenzene and its halogen derivatires[J].Analytica Chimica Acta,1974,71(1):85-96.
韩权,李娟,杨晓慧,单露,霍燕燕. 5-(5-氟-2-吡啶偶氮)-2,4-二氨基甲苯的合成及其与钯的显色反应[J].岩矿测试,2009,28(10):491-493. 韩权,吴启勋. 2-(3,5-二氯-2-偶氮吡啶)-5-二甲氨基苯胺与钴显色反应研究及其应用[J].化学试剂,1992,14(4):241-242. Shibata S, Furukaw M, Kamata E.Syntheses and spectrophoto-metric studies of 5-(2-pyridyl-azo)-2,4-diaminotoluene and its derivatives as analytical reagents: Spectrophotometric determination of cobalt with 5- -2,4-diaminotoluene [J].Analytica Chimica Acta, 1974,73:107-118. Shibata S, Furukaw M, Kamata E.Syntheses and spectrophoto-metric studies of 5-(2-pyridyl-azo)-2,4-diaminotoluene and its derivatives as analytical reagents: Spectrophotometric determination of cobalt with 5- -2,4-diaminotoluene [J].Analytica Chimica Acta, 1974,73:107-118.
Kiss E.Pyridylazo-diaminobenzenes as reagents for cobalt: Spectrophotometric determination of cobalt in silicates and meteorites[J].Analytica Chimica Acta, 1973,66(3):385-396. Kiss E.Pyridylazo-diaminobenzenes as reagents for cobalt: Spectrophotometric determination of cobalt in silicates and meteorites[J].Analytica Chimica Acta, 1973,66(3):385-396.
刘彬,张光,张小玲.新显色剂5-(5-硝基-2-吡啶偶氮)-2,4-二氨基甲苯与钴高灵敏显色反应的研究[J].分析化学,1995,23(8):981.
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