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| 碱性微波提取-ICP/MS法测定土壤中六价铬 |
| Determination of Hexavalent Chromium in Soil by Microwave-assisted Alkaline Digestion ICP/MS |
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| DOI： |
| 中文关键词: 六价铬 正交试验 碱性微波提取 ICP/MS法 土壤 |
| 英文关键词: Hexavalent chromium Orthogonal experiment Microwave-assisted alkaline digestion ICP/MS Soils |
| 基金项目:南通市“基于空间异质性模型的南通市土壤重金属溯源及污染源解析”科技基金资助项目 (JC2021167) |
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| 中文摘要: |
| 采用碱性微波提取法处理土壤样品，用电感耦合等离子体质谱（ICP/MS）法测定试样中的六价铬，以标准物质测定相对误差的绝对值作为试验指标建立正交模型，确定碱性微波消解的提取温度95 ℃、提取时间30 min、氯化镁用量005 g、提取液体积6 mL为最佳试验条件，采用He碰撞池技术和在线内标分别消除基体带来的质谱和非质谱干扰。条件优化后,方法检出限为0.10 mg/kg，实际样品6次测定结果的RSD分别为13.0%和5.7%，加标回收率为120%和106%。将该方法用于有证标准土壤样品的测定，测定结果均在标准值范围内。 |
| 英文摘要: |
| The soil was treated by microwave assisted alkaline digestion, and Cr6+ in the samples was determined by ICP/MS. An orthogonal model was established by taking the absolute value of relative error of reference material measurements as test indexes, the optimum conditions of microwave assisted alkaline digestion were determined as extraction temperature of 95 ℃, extraction time of 30 min, dosage of magnesium chloride of 0.05 g and extracting solution of 6 mL. He collision cell technology and on line internal standard were used to eliminate the interference of mass spectrometry and non mass spectrometry caused by matrix respectively. Under the optimized conditions, the method detection limit was 0.10 mg/kg. The RSD of 6 measurements of actual samples were 13.0% and 5.7%, and the spiked recoveries were 120% and 106%, respectively. This method was applied to the determination of certified standard soil samples, and the results were all within the range of standard values. |
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