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电导-紫外可见串联离子色谱法测定水样中痕量的IO_3^-、ClO_2^-、ClO_3^-、BrO_3^-、Br^-和NO_2^- 被引量:4

Determination of iodate,chlorite,chlorate,bromide,bromate,nitrite in water using ion chromatography with the suppressed conductivity detection and the visible detection
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摘要 目的:建立离子交换-电导-柱后衍生紫外可见串联离子色谱法同时测定样品中痕量的IO-3、ClO-2、ClO-3、BrO-3、Br-和NO-2。方法:采用高容量柱IonPacAS9-HC,以9.0mmol/LNa2CO3作淋洗液,外接水自动抑制,0.5g/L邻二甲氧基联苯胺盐酸盐+5g/L溴化钾+20%甲醇+5.6%硝酸作衍生剂,反应温度60℃,450nm波长检测。结果:方法的线性范围广、相关好(r>0.999),相对标准偏差(RSD)0.84%~5.4%,样品平均加标回收率91.3%~107.7%,检出限0.023~2.0μg/L,电导检测法与柱后衍生法比较测定表明,后者灵敏度更高。样品的酸度、共存离子对测定无影响。结论:本方法准确、灵敏、适用性广,可满足μg/L级痕量组分的测定。 Objective: To develop a method for simultaneously determinating iodate, chlorite, chlorate, bromide, bromate nitrite in water samples. Methods: A high capacity anion exchange Ion Pac 9 - HC column was used. 9 mmol/L sodium carbonate was used as eluent, an auto - suppression external water mode was selected,0. 5 g/L o - dianisidine. 2HCl(ODA) + 5 g/L KBr +20% methanel + 5. 6% nitric acid was used for post column reagent. The post column reaction (PCR) temperature was 60℃ ,and the visible absorbance detected at 450 nm. Results:The sample's pH and coexist anion had no influence on determination. The method enjoyed a wide linear range and good relativity ( r 〉 0. 999 ). The method detection limit (MDL) was 0. 023 - 2. 0 μg/L. The average recoveries were 91.3% - 109. 4% , and the relative standard deviation (RSD) were 0. 84% - 5.4%. The analytical results by the method of post column addition of reagent to enhance visible absorbance detection of anion was compared with that of the suppressed conductivity detection and was proved to be better in sensitivity. Conclusion: The results showed that the method was accurate and sensitive and might be good for application and suitable for trace analysis (μg/L) of samples.
出处 《中国卫生检验杂志》 CAS 2005年第8期914-917,共4页 Chinese Journal of Health Laboratory Technology
关键词 离子色谱法 卤素含氧酸盐 亚硝酸盐 自来水 矿泉水 瓶装水 Ion chromatography, Iodate, Chlorite, Chlorate, Bromide, Bromate, Nitrite Tap Water Spring Water Bottled Water
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