FI-Catalytic Photometric Determination of Trace Amounts of Oxalate
摘 要
在1.8×10-2mol·L-1硫酸介质中,于30 ℃加热160 s时,草酸根对重铬酸钾、碘化钾和罗丹明6G之间的褪色反应具有显著的催化作用。结合流动注射技术,提出了一种催化光度法测定痕量草酸根的方法。草酸根的线性范围为0.10~1.20 mg·L-1,检出限(3s/k)为0.03 mg·L-1,进样频率18次·h-1。对0.30及0.80 mg·L-1 草酸根标准溶液进行平行测定,其相对标准偏差(n=11)分别为2.7%和1.6%。该方法用于菠菜、尿液中草酸根含量的测定,并以此样品为基体进行回收试验,测得回收率在93.3%~96.7%之间。
Abstract
In 1.8×10-2mol·L-1 H2SO4 medium and heated at 30 ℃ for 160 s, the color-fading reaction among K2Cr2O7, KI and rhodamine 6G was significantly catalyzed by oxalate. By applying flow-injection technique, a FI-catalytic photometric method for determination of trace amount of oxalate was proposed. Linearity range was kept in the range of 0.10-1.20 mg·L-1, and limit of detection (3s/k) found was 0.03 mg·L-1, when the sampling frequency was 18 times per hour. Precision of the method was tested by addition of standard oxalate solutions with concentration of 0.30 and 0.80 mg·L-1 for 11 determinations, giving values of RSD′s 2.7% and 1.6% respectively. The proposed method was applied to the analysis of samples of spinach and urine, and using these samples as matrixes, recovery was tested by the standard addition method. Values of recovery found were in the range of 93.3%-96.7%.
中图分类号 O657.32
所属栏目
基金项目 国家自然科学基金项目(20977025);河南省教育厅自然科学基金项目(2009A150016);河南师范大学青年科学基金(2008qk12)
收稿日期 2010/7/18
修改稿日期
网络出版日期
作者单位点击查看
备注叶存玲(1973-),女,河南洛阳人,副教授,主要从事分析化学方向的教学和科研工作。
引用该论文: YE Cun-ling,WANG Zhi-ke,FENG Su-ling. FI-Catalytic Photometric Determination of Trace Amounts of Oxalate[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2011, 47(8): 963~965
叶存玲,王治科,冯素玲. 流动注射-催化光度法测定痕量草酸根[J]. 理化检验-化学分册, 2011, 47(8): 963~965
被引情况:
【1】彭慧仙, "离子色谱法测定硫酸氧钒中的Cl-和C2O2-4",理化检验-化学分册 51, 1364-1368(2015)
共有人对该论文发表了看法,其中:
人认为该论文很差
人认为该论文较差
人认为该论文一般
人认为该论文较好
人认为该论文很好
参考文献
【1】REDDY S M, HIGSON S P, VADGAMA P M. Amperometric enzyme electrode for the determination of urine oxalate[J]. Anal Chim Acta, 1997,343(1/2):59-68.
【2】CHAMJANGALI M A, SHARIF-RAZAVIAN L, YOUSEFI M, et al. Determination of trace amounts of oxalate in vegetable and water samples using a new kinetic-catalytic reaction system[J]. Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy, 2009,73(1):112-116.
【3】胡伟华,翟庆洲,王馨莹.利用对三溴偶氮胂-锆(Ⅳ)络合物的置换反应光度法测定草酸[J].理化检验-化学分册, 2008,44(4):352-354.
【4】周全法,吴煜,王琪.催化光度法测定微量草酸盐[J].理化检验-化学分册, 1997,33(8):352-354.
【5】张德良,曾序玲.动力学分光光度法测定微量草酸的研究[J].分析化学, 1995,23(4):395-397.
【6】冯素玲,李彬,樊静,等.食品及生物样品中痕量草酸的荧光动力学法测定[J].分析化学, 1997,25(11):1274-1277.
【7】宋功武.流动注射荧光法测定微量草酸根研究[J].湖北大学学报:自然科学版, 1993,15(2):176-179.
【8】HNOW R, HESSE A. Comparison of extraction methods for the determination of soluble and total oxalate in foods by HPLC-enzyme-reactor[J]. Food Chemistry, 2002,78(4):511-521.
【9】武汉大学.分析化学实验[M].4版.上海:高等教育出版社, 2001.
【2】CHAMJANGALI M A, SHARIF-RAZAVIAN L, YOUSEFI M, et al. Determination of trace amounts of oxalate in vegetable and water samples using a new kinetic-catalytic reaction system[J]. Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy, 2009,73(1):112-116.
【3】胡伟华,翟庆洲,王馨莹.利用对三溴偶氮胂-锆(Ⅳ)络合物的置换反应光度法测定草酸[J].理化检验-化学分册, 2008,44(4):352-354.
【4】周全法,吴煜,王琪.催化光度法测定微量草酸盐[J].理化检验-化学分册, 1997,33(8):352-354.
【5】张德良,曾序玲.动力学分光光度法测定微量草酸的研究[J].分析化学, 1995,23(4):395-397.
【6】冯素玲,李彬,樊静,等.食品及生物样品中痕量草酸的荧光动力学法测定[J].分析化学, 1997,25(11):1274-1277.
【7】宋功武.流动注射荧光法测定微量草酸根研究[J].湖北大学学报:自然科学版, 1993,15(2):176-179.
【8】HNOW R, HESSE A. Comparison of extraction methods for the determination of soluble and total oxalate in foods by HPLC-enzyme-reactor[J]. Food Chemistry, 2002,78(4):511-521.
【9】武汉大学.分析化学实验[M].4版.上海:高等教育出版社, 2001.
相关信息