利用电感耦合等离子体质谱法测定肥料重金属砷、镉、铅、铬含量
作者:
作者单位:

(1.北方干旱半干旱耕地高效利用全国重点实验室/ 中国农业科学院农业资源与农业区划研究所,北京 100081;2.国家化肥质量检验检测中心(北京),北京 100081;3.农业农村部农产品质量安全肥料源性因子风险评估实验室(北京),北京 100081;4.青岛市农业科学研究院,山东 青岛 266109)

作者简介:

李亚丽(1996-),在读硕士研究生,主要从事重金属测试和离子组学研究工作。E-mail:2720194554@qq.com。

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基金项目:

基金项目:国家重点研发计划项目(2022YFD1700603);国家农产品质量安全风险评估项目(GJFP2019035,GJFP2019037);中央级公益性科研院所基本科研业务费专项(Y2019PT20-04,1610132019018)。


The determination of arsenic,cadmium,lead and chromium in fertilizer by inductively coupled plasma mass spectrometer method
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(1.State Key Laboratory of Efficient Utilization of Arid and Semi-arid Arable Land in Northern China/Institute of Agricultural Resources and RegionalPlanning,ChineseAcademy of Agricultural Sciences,Beijing100081;2.China National Center for Quality Supervision and Test of ChemicalFertilizers(Beijing),Beijing10081;3.Laboratory of Quality and Safety Risk Assessment for Agricultural Products from FertilizerSources(Beijing),Ministry of Agriculture and RuralAffairs,Beijing100081;4.Qingdao Academy of AgriculturalSciences,Qingdao Shandong266109)

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    摘要:

    选取7 个不同的肥料样品,采用硝酸- 盐酸(王水)消解,消解液中砷(As)、镉(Cd)、铅(Pb)、铬(Cr)重金属元素含量采用电感耦合等离子体质谱(ICP-MS)法氦碰撞模式测定。 结果显示,根据固体称重量为0.2 g,定容体积50 mL,Cr、As、Cd、Pb 方法检出限分别为0.018、0.008、0.005、0.021 mg/kg,定量限分别为0.061、0.025、0.016、0.069 mg/kg,根据液体称重量1.0 g,定容体积50 mL,Cr、As、Cd、Pb 方法检出限分别为0.004、0.002、0.001、0.004 mg/kg,定量限分别为0.012、0.005、0.003、0.014 mg/kg,待测样品分别进行6 组重复测定,结果显示Cr 相对标准偏差(RSD)在3.8% ~ 16.8% 之间,As 的RSD 为3.9% ~ 56.5%,Cd 的RSD 为0.0% ~ 25.7%,Pb 的RSD 为4.2% ~ 24.5%,样品加标回收率为67.4% ~ 122.0%。4 家实验室对不同肥料种类抽取样品进行实验室比对测定,分析显示所有参与实验室测试值之间存在一致性,经柯克伦检验剔除离群值,保留歧离值后,将格拉布斯检验应用于通过柯克伦检验后的单元平均值,各元素均未发现有单个或成对歧离值或离群值存在。方法精密度和准确度满足要求,结论认为ICP-MS 可用于肥料中As、Cd、Pb、Gr 含量的测定分析。

    Abstract:

    Seven different fertilizer samples were selected for digestion by nitric acid-hydrochloric acid(aquaregia). The contents of heavy metals such asarsenic(As),cadmium(Cd),lead(Pb)andchromium(Cr)in the digestion solution were determined by helium collision mode using an inductively coupled plasma massspectrometer(ICP -MS)method. The resultsshowed that:based on the solid weight of 0.2 g and the constant volume of 50mL,the detection limits of Cr,As, Cd and Pb were0.018,0.008,0.005 and 0.021mg/kg,respectively,and the limits of quantification were0.061,0.025,0.016 and 0.069mg/kg,respectively. According to the liquid weight of 1.0 g and the constant volume of 50mL,the detectionlimits ofCr,As,Cd and Pb were0.004,0.002,0.001 and 0.004mg/kg,respectively,and the limits of quantification were0.012,0.005,0.003and 0.014 mg/kg,respectively. The relative standard deviationof Cr,As,Cdand Pb( n=6)were 3.8%-16.8%,3.9%-56.5%,0-25.7% and 4.2%-24.5%,respectively. The recoveries were 67.4%-122.0%. Samples of different fertilizer types wereextracted from four laboratories for laboratorycomparison,and the analysis showed that there was consistency between the test values of all the participating laboratories. After the outliers were removed by the Cochran test and the outliers wereretained,the Grubbs test wasapplied to the unit average after passing the Cochrantest,and no single or pairs of outliers or outliers were found for each element. The precision and accuracy of the method meet the requirements. Conclusion suggested that ICP-MS could be used for the determination ofAs,Cd,Pb and Cr in fertilizer.

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李亚丽,刘蜜,郭伟,王孝钢,汪洪.利用电感耦合等离子体质谱法测定肥料重金属砷、镉、铅、铬含量[J].中国土壤与肥料,2024,(2):235-243.

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  • 收稿日期:2023-02-15
  • 最后修改日期:
  • 录用日期:2023-03-08
  • 在线发布日期: 2024-05-22
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