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5′-硝基水杨基荧光酮胶束增敏分光光度法测定微量钯

Micellar Sensitization Spectrophotometry for Determination of Microamounts of Palladium with 5′_Nitrosalicyl Fluorone

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【作者】 郭忠先陈华明冯翔远张淑云

【Author】 Guo Zhongxian, Chen Huaming, Feng Xiangyuan, Zhang Shuyun ( Department of Chemical Engineering, Sichuan Institute of Light Industry and Chemical Technology, Zigong, 643033 )

【机构】 四川轻化工学院化学工程系

【摘要】 于pH67~76的磷酸盐缓冲介质中,溴化十六烷基三甲铵存在下,Pd(Ⅱ)与5′_硝基水杨基荧光酮30min内反应完全,生成组成比1∶2的紫红色配合物。λmax=582nm,Δλ=56nm,表观ε为104×105L·mol-1·cm-1,配合物至少稳定36h。测Pd(Ⅱ)的线性范围在0~080mg/L。结合丁二酮肟_氯仿萃取分离,方法可用于试样中微量钯的测定,结果与5_Br_PADAB光度法一致,标准加入回收率为932%~1004%,相对标准偏差为17%(n=10)。

【Abstract】 In phosphate buffer medium of pH 6.7~7.6, and in the presence of cetyltrimethylammonium bromide(CTMAB), palladium(Ⅱ) forms a 1∶2 soluble complex with 2,6,7trihydroxy92′hydroxy5nitrophenylfluorone3. The complex has a maximum absorption at 582 nm with contrast Δ λ =56 nm, and the apparent molar absorptivity is 1.04×10 5 L·mol -1 ·cm -1 . The chromogenic reaction is complete in 30 min and the color is stable for at least 36 h. Beer′s law is obeyed in the range of 0~0.80 mg/L for palladium. The effect of other metal ions on the determination of Pd has also been investigated. The method has been applied to the determination of palladium in an alloy after separating the interfering ions from the sample by extraction with dimethyl glyoxime and chloroform in acidic medium. The recovery is 93.2%~100.4% with precision of 1.7% RSD( n =10). The result is in good agreement with that provided by 5BrPADAB spectrophotometry.

  • 【文献出处】 岩矿测试 ,ROCK AND MINERAL ANALYSIS , 编辑部邮箱 ,1997年03期
  • 【分类号】TG115.335
  • 【被引频次】7
  • 【下载频次】32
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