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COMPARISON AND VERIFICATION OF HEXAVALENT CHROMIUM DETECTION METHODS IN SOLID SAMPLES
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摘要: 采用碱溶液提取/火焰原子吸收法(HJ 687—2014《固体废物六价铬的测定 碱消解/火焰原子吸收分光光度法》和HJ 1082—2019《土壤和沉积物 六价铬的测定 碱溶液提取-火焰原子吸收分光光度法》)测定了固体废物和土壤样品中六价铬含量,比对和验证了2种方法实验流程、分析方法性能及不确定度评定结果。结果表明:HJ 687—2014的方法检出限相对较高,不适合测定浓度较低的土壤;HJ 1082—2019要求按照试样制备的步骤配置工作曲线,考虑了基体干扰的影响。HJ 687—2014的检出限为0.28 mg/kg,相对标准偏差为0.69%~0.93%,样品加标回收率为95.7%~97.2%;HJ 1082—2019的检出限为0.17 mg/kg,相对标准偏差为0.6%~3.0%,样品加标回收率为76.0%~83.1%。对于同一实际样品,2种方法的测定结果相近,HJ 687—2014和HJ 1082—2019的测定结果分别为(48.1±4.2),(46.6±5.4) mg/kg。比对发现,影响HJ 687—2014和HJ 1082—2019不确定度的最主要环节分别为曲线拟合和样品消解。Abstract: This paper used two kinds of alkaline solution extraction/flame atomic absorption methods, Solid Waste-Determination of Hexavalent Chromium-by Alkaline Digestion/Flame Atomic Absorption Spectrophotometic (HJ 687—2014) and Soil and Sediment-Determination of Cr(Ⅵ)-Alkaline Digestion/Flame Atomic Absorption Spectrometry (HJ 1082—2019). The content of hexavalent chromium in solid waste and soil samples was measured and the experimental procedures, analytical method performance and uncertainty evaluation results of the two methods were compared and verified. The results showed that the detection limit of the HJ 687—2014 method was relatively higher, which was not suitable for the determination of soil with lower concentration. In HJ 1082—2019, it was required to configure the working curve according to the steps of sample preparation, which considered the influence of matrix interference. The detection limit of HJ 687—2014 was 0.28 mg/kg, the relative standard deviation was 0.69%~0.93%, and the sample recovery rate was 95.7%~97.2%. And the detection limit of HJ 1082—2019 was 0.17 mg/kg, the relative standard deviation was 0.6%~3.0%, and the sample recovery rate was 76.0%~83.1%. For the analysis of the same actual sample, the results of the two methods were similar. The detecting results of HJ 687—2014 and HJ 1082—2019 were (48.1±4.2), (46.6±5.4) mg/kg. After comparison, it was found that the main processes affecting the uncertainty of HJ 687—2014 and HJ 1082—2019 were curve fitting and sample digestion, respectively.
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Key words:
- hexavalent chromium /
- alkaline digestion /
- flame atomic absorption /
- solid sample
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