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投稿时间:2021-12-09 修订日期:2022-07-20
投稿时间:2021-12-09 修订日期:2022-07-20
中文摘要: 为了提高土壤和沉积物中六价铬测定的灵敏度、精密度和正确度,建立了柱后衍生-离子色谱法测定六价铬的分析方法。样品经过预处理后,使用仪器进行定量分析。样品中的六价铬经过Prin-Cen Cr(VI)Spec Column型阴离子分析柱分离出来,分别使用硝酸铵体系溶液和二苯碳酰二肼溶液作为流动相和柱后衍生液,并使用TLD检测器进行六价铬的定量分析。结果表明,六价铬质量浓度在5~100 μg/L范围内线性关系较好,相关系数为1.0000,检出限为0.02 mg/kg。该方法在实际土壤和沉积物样品中的加标回收率为84.0%~94.0%,相对标准偏差为2.34%~11%。本方法与火焰原子吸收分光光度法(HJ1082-2019)相比,六价铬的测定不受试样盐分、pH值及三价铬影响,而且该方法具有灵敏度高、精密度好、正确度高和稳定性强的优点,适用于测定土壤和沉积物中的六价铬。
Abstract:In order to improve the sensitivity, precision and accuracy of the determination of hexavalent chromium in soil and sediment,an analytical method for the determination of hexavalent chromium by ion chromatography with post column derivatization was established. After pretreatment, the samples were quantitatively analyzed by instrument. In detail, the hexavalent chromium in the sample was separated by the Prin-Cen Cr(VI) Spec Column type anion analysis column, wherein the ammonium nitrate system solution and the diphenyl-carbazide solution were used as the mobile phase and the derivative reagent after column respectively. Then, the quantitative analysis of hexavalent chromium was carried out by the TLD detector. Experimental results showed that the mass concentration curve of Cr possessed a good linear relationship in the range of 5-100 μg/L, with the correlation coefficient of 1.0000 and the detection limit of 0.02 mg/kg. The recovery rate of this method in actual soil and sediment samples were 84.0%-94.0%. The relative standard deviations were 2.34%-11%. Compared with the flame atomic absorption spectrophotometry (HJ1082-2019), the determination of hexavalent chromium by this method was not affected by the salinity, pH value and trivalent chromium of sample. Moreover, the advantages of this method possessed high sensitivity, precision, accuracy and strong stability, which was suitable for the determination of hexavalent chromium in soil and sediment.
keywords: hexavalent chromium post-column derivatization ion chromatography soil sediment alkali digestion flame atomic absorption spectrophotometry
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作者 | 单位 | |
吴小龙 | 海南省生态环境监测中心 | a13807692160@163.com |
陈琴放* | 海南省生态环境监测中心 | chenqinfang1111@163.com |
符式锦 | 海南省生态环境监测中心 | 825416995@qq.com |
周女琬 | 海南省生态环境监测中心 | 372240308@qq.com |
陈京成 | 广州谱临晟科技有限公司 | jingcheng.chen@princensci.com |
引用文本:
吴小龙,陈琴放,符式锦,周女琬,陈京成.柱后衍生-离子色谱法测定土壤和沉积物中的六价铬[J].中国无机分析化学,2022,12(5):13-19.
WU Xiaolong,CHEN Qinfang,FU Shijin,ZHOU Nvwan,CHEN Jingcheng.Determination of hexavalent chromium in soil and sediment by ion chromatography with post-column derivatization[J].Chinese Journal of Inorganic Analytical Chemistry,2022,12(5):13-19.
吴小龙,陈琴放,符式锦,周女琬,陈京成.柱后衍生-离子色谱法测定土壤和沉积物中的六价铬[J].中国无机分析化学,2022,12(5):13-19.
WU Xiaolong,CHEN Qinfang,FU Shijin,ZHOU Nvwan,CHEN Jingcheng.Determination of hexavalent chromium in soil and sediment by ion chromatography with post-column derivatization[J].Chinese Journal of Inorganic Analytical Chemistry,2022,12(5):13-19.