以四苯基卟啉(TPP)和硫酸为原料,微波法合成了四对磺酸苯基卟啉(TPPS4),产率高达94.7%,通过紫外可见吸收光谱(UV)、红外光谱(IR)、核磁共振(1HNMR)验证了其结构.在pH 6.5的HAc-NaAc的缓冲溶液中和Hg2+存在下,于沸水浴中TPPS4和铜、铬、镍反应15 min可实现柱前衍生.以四乙基溴化铵(TEABr)作离子对试剂,在C18柱上采用甲醇-水(体积比为40:60)体系作流动相,在420 nm处检测,实现了高效液相色谱法分离和测定铜、铬、镍,络合物和反应试剂在15 min内出峰完毕.铜、铬、镍的检测限分别为0.01 μg/L,0.50 μg/L,0.10 μg/L.此法可用于集中处理后的电镀废液中铜、铬、镍的测定.
参考文献
[1] | Manfred Doss .Conversion of porphyrin methyl esters to zinc and copper chelates for spectrophotometric analysis[J].Analytical Biochemistry,1971,39(01):7-14. |
[2] | 陈阳,马金石.水溶性光疗药物TPPS4的合成及提纯的研究[J].武汉科技大学学报(自然科学版),2003(03):254-255. |
[3] | 张松,潘超,乔庆东.四苯基卟啉及其衍生物的合成和可见光谱的研究[J].化工科技,2003(05):15-17. |
[4] | 丁学军 .meso-四对磺酸苯基卟啉的合成[J].化学世界,1990,31(04):164-166. |
[5] | 黎先超,胡景,孙小梅.原卟啉-吐温80-硫酸铵液固体系分离和测定铜、镍的研究[J].冶金分析,2006(03):72-74. |
[6] | Amit Chatterjee;Hiroaki Tao;Yasuyuki Shibata .Determination of selenium compounds in urine by high-performance liquid chromatography-inductively coupled plasma mass spectrometry[J].Journal of Chromatography A,2003,997(1-2):249-257. |
[7] | Zhihong Shi;Chengguang Fu .Porphyrins as ligands for trace metal analysis by high-performance liquid chromatography[J].Talanta: The International Journal of Pure and Applied Analytical Chemistry,1997(4):593-604. |
[8] | Qiufen Hu;Guangyu Yang;Haitao Li;Xi Tai;Jiayuan Yin .Study on Determination of Seven Transition Metal Ions in Water and Food by Microcolumn High-Performance Liquid Chromatography[J].Bulletin of the Korean Chemical Society,2004(5):694-698. |
[9] | Kashiyama Y;Kitazato H;Ohkouchi N .An improved method for isolation and purification of sedimentary porphyrins by high-performance liquid chromatography for compound-specific isotopic analysis[J].Journal of chromatography, A: Including electrophoresis and other separation methods,2007(1/2):73-83. |
[10] | 赵春杰;黄东萍;张仲元 等.HPLC同时测定人血清和人发中微量铬锌铜铅的含量[J].中国药学杂志,1995,30(03):162-165. |
[11] | 刘波 .发光材料四苯基卟啉及其金属配合物的合成及性能[D].西北工业大学,2007. |
[12] | 王涛 .卟啉化合物的合成及与铜、铅显色反应的研究[D].河北师范大学,2005. |
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