Photometric Determination of Trace Amount of Lead in Pure Zinc with Polybromo-Phenylfluorone
摘 要
研究了多溴代苯基荧光酮显色剂3′,5′-二溴-4′-羟基-4,5-二溴苯基荧光酮(DBHDBPF)与铅(Ⅱ)的显色反应,结果表明:在十六烷基三甲基溴化铵微乳液存在下及pH 10.0的硼砂-氢氧化钠缓冲溶液中,显色剂DBHDBPF与铅形成2比1的稳定络合物。其最大吸收波长位于波长592 nm处,表观摩尔吸光率为1.58×105L·mol-1·cm-1。据此提出了甲基异丁基酮萃取分离、DBHDBPF光度法测定纯锌中铅含量的方法。铅的质量浓度在1.8 mg·L-1以内符合比耳定律,方法的检出限(3S/N)为0.12 mg·L-1。应用此方法测定了GBW 02701和GBW 02702纯锌标准物质中微量铅的含量,测定结果与认定值相一致。
Abstract
The color reaction between a polybromo-phenylfluorone chromagenic reagent, 3′,5′-dibromo-4′-hydroxy-4,5-dibromophenylfluorone (DBHDBPF), and Pb(Ⅱ) was studied. In a Na2B4O7-NaOH buffer solution of pH 10.0, and in the CTMAB microemulsion, a stable coordination complex with the molar ratio (DBHDBPF∶Pb) of 2 to 1, was formed, with its absorption maximum at the wavelength of 592 nm. Value of apparent molar absorptivity was found to be 1.58×105L·mol-1·cm-1. Based on these facts, a method of spectrophotometry for the determination of lead in pure zinc was proposed using 4-methyl-2-pentanone (MIBK) to extract Pb(Ⅱ) from sample solution. Beer′s law was held in the range within 1.8 mg·L-1, with detection limit (3S/N) of 0.12 mg ·L-1. The proposed method was applied to the determination of Pb in CRM′s of pure zinc (GBW 02701 and GBW 02702), giving results in consistency with the certified values.
中图分类号 O657.3
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收稿日期 2010/10/22
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备注李兴伟(1984-),男,湖北黄冈人,硕士研究生,从事有毒重金属的分析试剂及测定方法研究。
引用该论文: LI Xing-wei,CAO Jin-xing,OU Zhong-ping. Photometric Determination of Trace Amount of Lead in Pure Zinc with Polybromo-Phenylfluorone[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2011, 47(10): 1146~1148
李兴伟,曹金星,欧忠平. 多溴代苯基荧光酮光度法测定纯锌中痕量铅[J]. 理化检验-化学分册, 2011, 47(10): 1146~1148
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参考文献
【1】高琳,姚军龙,晏高华.二溴对甲基偶氮磺光度法测定铝合金中微量铅[J].冶金分析, 2005,25(2):54-55.
【2】李兴扬,张栋.二苯硫腙-CCl4-萃取-分光光度法连续测定水样中铜和铅[J].理化检验-化学分册, 2007,43(7):561-563.
【3】范晓燕,董杰.Pb(Ⅱ)-双硫腙-PAR水相光度法测定样品中铅[J].理化检验-化学分册, 2001,37(6):258-260.
【4】LI Zai-jun, YANG Yu-ling, TANG Jian, et al. Spectrophotometric determination of trace lead in water after preconcentration using mercaptosephadex[J]. Talanta, 2003,60(1):123-130.
【5】LI Zai-jun, TANG Jian, PAN Jiao-mai. The determination of lead in preserved food by spectrophotometry with dibromohydroxyphenylporphyrin[J]. Food Control, 2004,15(7):565-570.
【6】周晚云,周春山,刘星星,等.锌基体分离及纯锌中杂质成分的ICP-MS测定[J].矿冶, 1999,8(1):98-101.
【7】申明乐,刘万峰.氢化物发生-原子荧光光谱法测定锌锭中锡铅锑铋[J].冶金分析, 2008,28(7):69-71.
【8】何家洪,徐强,宋仲容.分光光度法测定铅(Ⅱ)的研究进展[J].冶金分析, 2010,30(3):34-44.
【9】RAO T P, REDDY M L P, PILLAI A P. Application of ternary and multicomponent complexes to spectrophotometic and spectrofluorimetric analysis of inorganics[J]. Talanta, 1998,46,765-813.
【10】李在均.新苯基荧光酮试剂合成及在食品分析中应用[D]. 2004:16-20.
【11】朱振中,李在均,潘教麦.Meso-四-(3,5-二溴-4-羟基苯)卟啉分光光度测定食品中微量铅[J].分析科学学报, 1999,15(2):43-46.
【2】李兴扬,张栋.二苯硫腙-CCl4-萃取-分光光度法连续测定水样中铜和铅[J].理化检验-化学分册, 2007,43(7):561-563.
【3】范晓燕,董杰.Pb(Ⅱ)-双硫腙-PAR水相光度法测定样品中铅[J].理化检验-化学分册, 2001,37(6):258-260.
【4】LI Zai-jun, YANG Yu-ling, TANG Jian, et al. Spectrophotometric determination of trace lead in water after preconcentration using mercaptosephadex[J]. Talanta, 2003,60(1):123-130.
【5】LI Zai-jun, TANG Jian, PAN Jiao-mai. The determination of lead in preserved food by spectrophotometry with dibromohydroxyphenylporphyrin[J]. Food Control, 2004,15(7):565-570.
【6】周晚云,周春山,刘星星,等.锌基体分离及纯锌中杂质成分的ICP-MS测定[J].矿冶, 1999,8(1):98-101.
【7】申明乐,刘万峰.氢化物发生-原子荧光光谱法测定锌锭中锡铅锑铋[J].冶金分析, 2008,28(7):69-71.
【8】何家洪,徐强,宋仲容.分光光度法测定铅(Ⅱ)的研究进展[J].冶金分析, 2010,30(3):34-44.
【9】RAO T P, REDDY M L P, PILLAI A P. Application of ternary and multicomponent complexes to spectrophotometic and spectrofluorimetric analysis of inorganics[J]. Talanta, 1998,46,765-813.
【10】李在均.新苯基荧光酮试剂合成及在食品分析中应用[D]. 2004:16-20.
【11】朱振中,李在均,潘教麦.Meso-四-(3,5-二溴-4-羟基苯)卟啉分光光度测定食品中微量铅[J].分析科学学报, 1999,15(2):43-46.
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