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机构地区:[1]长安大学环境科学与工程学院,西安710054 [2]西北大学化学工程学院,西安710069
出 处:《理化检验(化学分册)》2006年第4期278-280,共3页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
摘 要:基于Cr(Ⅵ)-8-羟基喹啉对鲁米诺-H2O2化学发光体系的催化作用,建立了测定Cr(Ⅵ)的化学发光法。检出限为1.2×10^-3mg·L^-1,线性范围为3.0×10^-3~4.0×10^-2mg·L^-1,回归方程为ICL=3.6+1.68×10^6C(g·L^-1),相对标准偏差2.8%(n=11);将该法应用于丙酸钙、动物蛋白粉等生化产品中痕量铬的测定,加标回收率96%~105%,5次测定平均值与苯二碳酰二肼光度法相比较,相对偏差小于5%,并探讨了化学发光反应机理。It was found that in an alkaline medium of KOH, the chemiluminescence (CL) reaction between luminol and H2O2 was catalyzed by the complex formed by Cr(Ⅵ ) with 8-hydroxyquinoline, and that linear relationship between the intensity of CL and the concentration Cr(Ⅵ) ion was kept in the range of 3.0× 10^-3 to 4 .0× 10^-2 mg· L^-1, having its linear regression equation as ICE = 3. 6+1. 68 ×10^6 C (g · L^-1 ) with correlation coefficient of 0. 999. Detection limit of this method was found to be 1.2 ×10^- 3mg · L^-1 for Cr(Ⅵ ), under the condition of K=3 and confidential level of 99. 6%. Test of precision was made at the concentration level of 2× 10^-2mg · L^-1 of Cr(Ⅵ) for 11 multiplicate determinations, and the RSD's obtained was 2. 8%. In the application of this method to the determination of Cr(Ⅵ ) in samples of calcium propionate and animal protein powder, results obtained were in consistency with the results obtained by photometry. RSD's (n= 5) found were less than 3.2%, and recovery tested by the standard addition method gave results in the range of 96% to 105%. A brief discussion on the reaction methanism was also given.
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