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首页>《中国测试》期刊>本期导读>微波消解-ICP-MS法测定土壤及耕作物小麦中的8种重金属元素

微波消解-ICP-MS法测定土壤及耕作物小麦中的8种重金属元素

165    2019-05-28

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作者:徐聪1, 赵婷1, 池海涛1, 李琴梅1,2, 成永霞3, 赵小学3, 刘伟丽1,2, 高峡1,2

作者单位:1. 北京市理化分析测试中心, 北京 100094;
2. 有机材料检测技术与质量评价北京市重点实验室, 北京 100094;
3. 河南省土壤重金属污染监测与修复重点实验室, 河南 济源 459000


关键词:电感耦合等离子体质谱法;微波消解;土壤;重金属;小麦


摘要:

建立微波消解-电感耦合等离子体质谱(ICP-MS)法同时测定土壤及对应耕作物小麦中8种重金属元素(Cr、Ni、Cu、Zn、As、Cd、Hg、Pb)含量的方法,比较不同的酸消解体系对土壤消解效果的影响。通过优化仪器参数、选择103Rh作单一内标元素校正土壤基体的干扰及仪器信号漂移,并编辑校正方程消除质谱干扰等,实现对土壤、小麦籽粒及小麦粉中重金属元素的准确测定。结果表明:以HNO3-H2O2-HF (5∶2∶2)为消解液体系微波消解土壤时,样品消解完全且效果最佳;各元素均呈现良好的线性关系,相关系数(r2)≥0.999 5;检出限在0.005~0.15 μg/L之间。土壤标准物质GBW07454(GSS-25)和小麦标准物质GSB10046(GSB-24)的测定值与标准值吻合,加标回收率在93.4%~103.6%范围内,方法精密度和准确度高。实际样品结果显示,土壤中Cd、Pb达到3级中污染水平;对应小麦籽粒和小麦粉中重金属元素与土壤存在一定的同源性,重金属元素更易富集于小麦籽粒中,其中Cd污染最严重。


Determination of eight kinds of heavy metal elements in cultivated soil and the wheat by microwave digestion-ICP-MS method
XU Cong1, ZHAO Ting1, CHI Haitao1, LI Qinmei1,2, CHENG Yongxia3, ZHAO Xiaoxue3, LIU Weili1,2, Gao Xia1,2
1. Beijing Center for Physical & Chemical Analysis, Beijing 100094, China;
2. Organic Material Testing Technology and Quality Evaluation of the Key Laboratory of Beijing, Beijing 100094, China;
3. Key Laboratory for Monitoring and Remediation of Heavy Metal Polluted Soils of Henan Province, Jiyuan 459000, China
Abstract: A method was established to determine eight kinds of heavy metal elements (Cr, Ni, Cu, Zn, As, Cd, Hg, Pb) in soil and the wheat by microwave digestion-inductively coupled plasma mass spectrometry (ICP-MS), and the effects of different acid digestion reagent systems on soil digestion were investigated. The heavy metal elements in soil, the wheat grains and the wheat flour were accurately determined by optimizing instrument parameters, selecting 103Rh as interior standard to correct the matrix interference and instrument signal drift, and editing correction equation to eliminate mass spectrum interference. The results indicated that the samples was dissolved completely with best effects when using HNO3-H2O2-HF (5:2:2) as digestion reagent system. Each element presented a good linear relationship with correlation coefficient (r2) ≥ 0.999 5, and the detection limit was between 0.005-0.15 μg/L. The method has high precision and accuracy because the determination results of GBW07454 (GSS-25) and GSB10046 (GSB-24) were consistent with the standard values and the recovery ranged between 93.4%-103.6%. The practical sample results showed that Cd, Pb reached the 3 level pollution in soil and the heavy metals in the soil were homologous with the corresponding wheat grains and wheat flour, and which are more likely to be enriched in wheat grain, among which the pollution of Cd was the most serious.
Keywords: inductively coupled plasma mass spectrometry method;microwave digestion;soil;heavy metal;wheat
2019, 45(5):85-92  收稿日期: 2019-01-17;收到修改稿日期: 2019-03-03
基金项目: 河南省土壤重金属污染监测与修复重点实验室开放基金资助项目(2017205)
作者简介: 徐聪(1990-),女,山西河津市人,硕士,研究方向光谱质谱分析
参考文献
[1] 王雪梅, 杜彤彤, 王娟, 等. 微波消解/ICP-MS同时测定粮食、蔬菜中的11种重金属元素[J]. 分析测试学报, 2017, 36(12):1522-1525
[2] CAI M F, LI K M, XIE D P, et al. The status and protection strategy of farmland soils polluted by heavy metals[J]. Environmental Science & Technology, 2014, 37(120):223-230
[3] PENG Y, WU J, CHAO J B, et al. A methods for the accurate determination of 14 metal elements in soils/sediments by ICP-MS[J]. Environmental Chemistry, 2017, 36(1):175-182
[4] 土壤环境质量标准:GB15618-2008[S]. 北京:中国标准出版社, 2008.
[5] 冉景, 王建德, 王灿, 等. 便携式X射线荧光光谱法与原子吸收、原子荧光法测定土壤重金属的对比研究[J]. 光谱学与光谱分析, 2014, 34(11):3113-3118
[6] GARCIA R, MAIZ I, MILLAN E. Heavy metal contamination analysis of roadsoils and grasses from Gipuzkoa (Spain)[J]. Environmental Technology, 1996, 17(7):763-770
[7] SENG C P, NORHAYATI M T, HAFIZA M Z, et al. Heavy metal contents in soil of major towns in the east coast of Peninsular Malaysia[J]. Chinese Journal of Geochemistry, 2006, 25(1):56-56
[8] CHRISTOPH M, THEOPISTI L, VOLKER J D. Determination of heavy metals in soils, sediments and geological materials by ICP-AES and ICP-MS[J]. Mikrochimica Acta, 2001, 136(3-4):123-128
[9] 张洪文, 张永辉, 韩康琴, 等. 多道全自动原子荧光光谱法测定土壤中的砷和汞[J]. 中国无机分析化学, 2014, 4(1):18-21
[10] 陈江, 姚雨鑫, 费勇, 等. 微波消解等离子体发射光谱法和石墨炉原子吸收光谱法联合测定土壤中多元素[J]. 岩矿测试, 2009, 28(1):25-28
[11] BENDAKOVSKÁ L, KREJČOVÁ A, ČERNOHORSKÝ T. Development of ICP-MS and ICP-OES methods for determination of gadolinium in samples related to hospital waste water treatment[J]. Chemical Papers, 2016, 70(9):1155-1165
[12] 孙秀敏, 雷敏, 李璐, 等. 微波消解-ICP-MS法同时测定土壤中8种重(类)金属元素[J]. 分析试验室, 2014, 33(10):1177-1180
[13] 韩张雄, 马娅妮, 陶秋丽. 微波消解样品-电感耦合等离子体质谱法测定小麦中铜、锌、镉、镍和铅[J]. 理化检验-化学分册, 2013, 46(10):1199-1201
[14] 闫学全. 一种自动石墨消解-ICP-MS法监测工业区土壤中微量砷、汞、硒、锑元素残留方法的建立[J]. 中国测试, 2018, 44(11):77-80
[15] ETTLER V, MIHALJEVIC M, KOMÁREK M. ICP-MS measurements of lead isotopic ratios in soils heavily contaminated by lead smelting:tracing the sources of pollution[J]. Analytical and Bioanalytical Chemistry, 2004, 378(2):311-317
[16] 袁静. 微波消解-ICP-MS法测定土壤和底泥中的12种金属元素[J]. 中国环境监测, 2012, 28(5):96-99
[17] 龙加洪, 谭菊, 吴银菊, 等. 土壤重金属含量测定不同消解方法比对研究[J]. 中国环境监测, 2013, 29(1):123-126
[18] FALCIANI R, NOVARO E, MARCHESINI M. Multi-element analysis of soil and sediment by ICP-MS after a microware assisted digestion method[J]. Journal of Analytical Atomic Spectrometry, 2000, 15:561-565
[19] 刘传娟, 刘凤枝, 蔡彦明, 等. 不同前处理方法-ICP-MS测定土壤中的重金属[J]. 分析实验室, 2009, 28:91-94
[20] 土壤质量铅、镉的测定石墨炉原子吸收分光光度法:GB/T 17141-1997[S]. 北京:中国标准出版社, 1997.
[21] 鲁照玲, 胡红云, 姚洪. 土壤中重金属元素电感耦合等离子体质谱定量分析方法的研究[J]. 盐矿测试, 2012, 31(2):241-246
[22] 陈岩, 赵晓丽, 杨慧, 等. 湿法消解ICP-MS法测定紫菜和海带中15种元素[J]. 分析试验室, 2015, 34(7):803-806
[23] 赵小学, 赵宗生, 陈纯, 等. 电感耦合等离子体质谱法内标元素选择的研究[J]. 中国环境监测, 2016, 32(1):84-87
[24] 陈京都, 戴其根, 许学宏, 等. 江苏省典型区农田土壤及小麦中重金属含量与评价[J]. 生态学报, 2012, 32(11):3487-3796
[25] XU Q, GUO W, JIN L L. Determination of cadmium in geological samples by aerosol dilution ICP-MS after inverse aqua regia extraction[R]. Electronic Supplementary Material (ESI) for Journal of Analytical Atomic Spectrometry, 2015.
[26] 粮食(含谷物、豆类)及制品中铅、铬、镉、汞、硒、砷、铜、锌等八种元素限量:NY861-2004[S]. 北京:中国农业出版社, 2004.
[27] 邵云, 李春喜, 李向力, 等. 土壤-小麦系统中5种重金属含量的相关分析[J]. 河南农业科学, 2007, 5:25-28
[28] 顾志荣, 王亚丽, 陈晖, 等. 当归药材与产地土壤中无机元素的相关分析研究[J]. 土壤通报, 2014, 45(6):1410-1415