DETERMINATION OF ANIONS IN INTERMEDIATES AND PRODUCTS OF THE PRODUCTION OF m-PHTHALIC ACID BY ION CHROMATOGRAPHY
摘 要
建立了用离子交换色谱法同时测定间苯二甲酸生产工艺中中间物料及产品中F-、Cl-、Br-、OAc-、NO-3、PO3-4和SO2-4等7种阴离子的分析方法.采用A SUPP 5-250阴离子交换柱,以2.8 mmol·L-1 Na2CO3和1.2 mmol·L-1 NaHCO3混合溶液为流动相,在20 min内有效地分离和测定了样品中上述7种阴离子.采用抑制型电导检测,以S/N=3计算,F-、Cl-、Br-、OAc-、NO-3、PO3-4和SO2-4等离子的检出限分别为0.10,0.40,0.35,0.25,2.50,0.25和0.90 μg·L-1,相关系数在0.999 1~0.999 7范围内;峰面积的相对标准偏差小于1.3%,加标回收率在98.2 %~100.3%之间.
Abstract
Method of determination of 7 anions,including F-,Cl-,Br-,OAc-,NO-3,PO3-4 and SO2-4,by suppressed ion chromatography was proposed.Separation of the anions was performed by using the A-Supp.5-250 anion separation column (4 mm×50 mm) and a mixed solution of 2.8 mmol·L-1 Na2CO3 solution and 1.2 mmol·L-1 NaHCO3 solution was used as mobile phase,and the determination was done by conductivity detection.The 7 anions mentioned above were separated and determined within 20 min.Linear relationships between the peak area and concentration of the 7 anions were obtained with correlation coefficients in the range of 0.999 1 to 0.999 7,and RSD′s less than 1.3%.Detection limits (S/N=3) for the 7 anions obtained were 0.10,0.40,0.35,0.25,2.50,0.25 and 0.90 μg·L-1 in the above mentioned order.Values of recovery found were in the range from 98.2% to 100.3%.
中图分类号 O658
所属栏目 工作简报
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收稿日期 2005/7/5
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备注宋萍(1965-),女,山东长岛人,副教授,主要从事分析化学研究工作.
引用该论文: SONG Ping,WANG Qiao-e,DING Ming-yu,LIU Dong-lian,FAN hui. DETERMINATION OF ANIONS IN INTERMEDIATES AND PRODUCTS OF THE PRODUCTION OF m-PHTHALIC ACID BY ION CHROMATOGRAPHY[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2006, 42(12): 1016~1018
宋萍,王巧娥,丁明玉,刘冬莲,樊慧. 离子交换色谱法测定间苯二甲酸生产工艺中间物料及产品中的阴离子[J]. 理化检验-化学分册, 2006, 42(12): 1016~1018
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