| 242 | 1 | 59 |
| 下载次数 | 被引频次 | 阅读次数 |
在用电感耦合等离子体质谱法（ICP-MS）对土壤中的痕量重金属进行测定时，易受到土壤复杂基质所引发的基体效应的干扰，进而影响测定数据的准确性。本文通过分析基体效应机理，创新性地在截取锥与传统提取透镜之间额外增设了一个提取透镜，构建双提取透镜装置，同时，对该双提取透镜装置以及作为碰撞气的氦气进行了优化调节，旨在最大程度地降低基体效应的影响。基于此，成功建立起在双提取透镜及碰撞气条件下，用于测定土壤中痕量重金属元素的应用方法。为充分验证该方法的准确性与可靠性，本文选取GSS-9湖积物土壤成分分析标准物质展开测定实验，通过对比有无双提取透镜配置时的线性关系、检出限、精密度、加标回收率以及内标波动比等关键指标，全面评估所建方法的性能。结果表明：相较无双提取透镜的内标下降至40%，配置1内标波动能够维持在70%～130%；各配置下的线性相关系数均在0.999以上；由于双提取配置下的灵敏度较低，导致其检出限略高于无双提取透镜时，但均低于检出要求；相较无双提取的透镜的7%～38%，配置1的测定值相对误差最小，在0.4%～15%，各元素进行6次测定所得结果的RSD处于5%以内；配置1和配置2的加标回收率稳定保持在80%～120%，而无双提取透镜和配置3的加标回收率波动较为显著，超出80%～120%的区间。实验结果表明，双提取透镜装置能显著减少基体带来的内标波动，有效降低基体效应，提高分析准确性，为土壤环境监测和污染治理提供准确数据支持，也为ICP-MS在复杂基体分析中的应用提供了新的思路和方法。
Abstract：Inductively coupled plasma mass spectrometry(ICP-MS) is sensitive to interference from matrix effects caused by the complex soil matrix. These matrix effects may affect the accuracy of measurement data. This article analyzes the mechanism behind matrix effects and introduces an innovative approach by adding an additional extraction lens between the skimmer cone and the traditional extraction lens. This results in the construction of a dual extraction lens system. Combined with helium gas as collision gas,the dual extraction lens device has been optimized to minimize the impact of matrix effects. Based on this,an application method for determining trace heavy metals in soil under dual extraction lens and collision gas conditions has been successfully established. To ensure the accuracy and reliability of the method,experiments were performed using the GSS-9 lake sediment soil composition analysis standard material. By comparing key indicators such as linear relationship,detection limit,precision,spiked recovery rate,and internal standard fluctuation ratio with and without the dual extraction lens,the performance of the established method was comprehensively evaluated. In terms of internal standard fluctuations,the internal standard of configuration 1 decreased to 40% compared to the non-dual extraction lens setup,with fluctuations maintained between 70% and 130%. In terms of linear relationship,the linear correlation coefficients for all configurations were above 0. 999. In terms of detection limit,the detection limit for the dual extraction configuration was slightly higher than that without dual extraction lenses but still met the detection requirements. In terms of precision,the relative error of configuration 1 was between 0. 4% and 15%,compared to 7%-38% for the non-dual extraction lens. The RSD of the results obtained from six measurements of each element was within 5%. For spiked recovery rates,the recovery rates of configuration 1 and configuration 2 remained stable between 80% and 120%,while the recoveries of the non-dual extraction lens and configuration 3 showed significant fluctuations beyond this range. The experimental results indicate that the dual extraction lens device effectively reduces internal standard fluctuations caused by the matrix and minimizes matrix effects. This improves analytical accuracy and provides reliable data support for soil environmental monitoring and pollution control. The study also offers new ideas for the application of ICP-MS in analyzing complex matrices.
[1] SOODAN R K,PAKADE Y B,NAGPAL A,et al.Analytical techniques for estimation of heavy metals in soil ecosystem:a tabulated review[J]. Talanta,2014,125:405-410.
[2] MOOR C,LYMBEROPOULOU T,DIETRICH V J.Determination of heavy metals in soils,sediments and geological materials by ICP-AES and ICP-MS[J].Mikrochim Acta,2001,136:123-128.
[3] SHAHEEN M E,TAWFIK W,MANKOULA A F,et al.Determination of heavy metal content and pollution indices in the agricultural soils using laser ablation inductively coupled plasma mass spectrometry[J]. Environmental Science and Pollution Research,2021,28:36039-36052.
[4] PAN F,YU Y,YU L,et al. Quantitative assessment on soil concentration of heavy metal-contaminated soil with various sample pretreatment techniques and detection methods[J]. Environ Monit Assess,2020,192(12):800. DOI:10. 1007/s10661-020-08775-4.
[5] NIMELAN V,KUMAR S S,RAJAMANICKAM M,et al.ICP-MS Measurement of trace and rare earth elements in beach pacer-deposit soils of odisha,east coast of India,to estimate natural enhancement of elements in the environment[J]. Molecules,2021,26(24):7510. DOI:10. 3390/molecules26247510.
[6] MENG R,DU J H,LIU Y H,et al. Exploration of digestion method for determination of heavy metal elements in soil by ICP-MS[J]. Spectroscopy and Spectral Analysis,2021,41:2122-2128.
[7] NASR E G,EPOVA E N,ALBERT D,et al. Trace elements analysis of Tunisian and European extra virgin olive oils by ICP-MS and chemometrics for geographical discrimination[J]. Foods,2021,11(1):82. DOI:10. 3390/foods11010082.
[8] PANDEY S,GUPTA S,SHARMA S K. Plasmonic nanoparticle's anti-aggregation application in sensor development for water and waste water analysis[J].Environ Monit Assess,2023,195(7):874. DOI:10. 1007/s10661-023-11355-x.
[9] PATRIC L,GRZEGORZ O,MATSTOTAL F.Dissolution of environmental samples for the determination of uranium and thorium by ICP-MS and alpha-particle spectrometry[J]. Applied Radiation and Isotopes,2022,181:110103. DOI:10. 1016/j. apradiso. 2022. 110103.
[10] POTOCNIK D,HUDOBIVNIK M J,MAZEJ D,et al.Optimization of the sample preparation method for determination of multi-elemental composition in fruit samples by ICP-MS analysis[J]. Measurement:Sensors,2021,18:100292. DOI:10. 1016/j. measen.2021. 100292.
[11] SPANU A,LANGASCO I,VALENTE M,et al.Tuning of the amount of Se in rice(Oryza Sativa)grain by varying the nature of the irrigation method:development of an ICP-MS analytical protocol,validation,and application to 26 different rice genotypes[J]. Molecules(Basel,Switzerland),2020,25(8):1861. DOI:10. 3390/molecules25081861.
[12] WEBSTER A B,GANSWINDT A,SMALL C,et al.Optimised ICP-MS quantification method for using animal faeces as a measure of protected area ecosystem health[J]. MethodsX,2021,8:101441. DOI:10. 1016/j. mex. 2021. 101441.
[13] ZHOU L H,JIN Y J,MA L F,et al. Multi-isotope calibration for determination of nickel,molybdenum,barium,and lead in soil samples by inductively coupled plasma mass spectrometry[J]. Spectroscopy Letters,2022,55(4):278-283.
[14] CATENZA K F,DONKOR K K. Determination of heavy metals in cannabinoid-based food products using microwave-assisted digestion and ICP-MS[J]. Food Analytical Methods,2022,15:2537-2546.
[15] ROMANOVSKIY K A,BOLSHOV M A,MUNZ A V.A novel photochemical vapor generator for ICP-MS determination of As,Bi,Hg,Sb,Se and Te[J]. Talanta,2018,187:370-378.
[16] TANG X,LI B,LU J,et al. Gold determination in soil by ICP-MS:comparison of sample pretreatment methods[J].Journal of Analytical Science and Technology,2020,11:45. DOI:10. 1186/s40543-020-00245-3.
[17] BRAYSHER E C,BROWN R J C,BROWN A S.Investigation of internal standard use for short-term drift correction in ICP-MS/MS[J]. Accreditation and Quality Assurance,2025,30:221-231.
[18] LANOT T,LAVIT M,GANDIA P,et al. Optimization of ICP-MS internal standardization for 26 elements by factorial design experiment[J]. Journal of Trace Elements in Medicine and Biology,2023,78:127178.DOI:10. 1016/J. JTEMB. 2023. 127178.
[19] TAKATA N,BOTHA A,NOMNGONGO P N.Development of a method for the determination of total selenium in soil,maize plants,and maize flour by inductively coupled plasma tandem mass spectrometry(ICP-MS/MS)[J]. Analytical Letters,2023,57:2200-2214.
[20] BOLEA F E,RUAIBARZ A,RESANO M,et al. To shift,or not to shift:Adequate selection of an internal standard in mass-shift approaches using tandem ICP-mass spectrometry(ICP-MS/MS)[J]. Journal of Analytical Atomic Spectrometry,2021,36(6):1135-1149.
[21] BOTHA A. A comparison of different calibration strategies for the trace analysis of soil samples by inductively coupled plasma mass spectrometry(ICPMS)[J]. Metrologia,2020,57(6):065013. DOI:10. 1088/1681-7575/abac52.
[22] MAO J C,LIU X Y,CHEN B,et al. Determination of heavy metals in soil by inductively coupled plasma mass spectrometry(ICP-MS)with internal standard method[J].Electronics Science Technology and Application,2017,4(1):23-31.
[23]朱志刚，李美丽，井永军，等.单提取法-动能甄别型碰撞模式-电感耦合等离子体质谱（ICP-MS）法测定土壤中8种有效态元素的含量[J].中国无机分析化学，2023,13(6):590-597.ZHU Zhigang,LI Meili,JING Yongjun,et al.Determination of eight available elements in soil by inductively coupled plasma mass spectrometry with single extraction method-kinetic energy discrimination collision mode[J]. Chinese Journal of Inorganic Analytical Chemistry,2023,13(6):590-597.
[24]刘向磊，孙文军，文田耀，等.三酸分步消解-电感耦合等离子体质谱法测定土壤详查样品中23种金属元素[J].岩矿测试，2020,39(5):793-800.LIU Xianglei,SUN Wenjun,WEN Tianyao,et al.Determination of 23 metal elements in detailed soil survey samples by inductively coupled plasma-mass spectrometry with three acid stepwise digestion[J]. Rock and Mineral Analysis,2020,39(5):793-800.
[25] NAKAMURA A,KUBOTA K,OHTA A. Multielement analysis of geological samples using ICP-MS equipped with integrated sample introduction and aerosol dilution systems[J]. Bulletin of the Geological Survey of Japan,2023,74(2):71-85.
[26] NYIKA A,OLUMANA M,BHARDWAJ S,et al.A comparison of reproducibility of inductively coupled spectrometric techniques in soil metal analyses:a comparison of reproducibility of inductively coupled spectrometric techniques in soil metal analyses[J]. Air,Soil,and Water Research,2022,12:1-9.
[27] FANG W,TANG H,ZHOU J. A green digestion method for minor elemental analysis of egg samples by ICP-MS[J]. Journal of Analytical Chemistry,2023,78:728-736.
[28] UPADHYAY K,VIRAMGAMI A,BALACHANDAR R,et al.Development and validation of an ICP-MS method and its application in assessing heavy metals in whole blood samples among occupationally exposed lead smelting plant workers[J]. Journal of Biological Inorganic Chemistry,2024,29:763-771.
[29] BAJAJ A O,PARKER R,FARNSWORTH C,et al.Method validation of multi-element panel in whole blood by inductively coupled plasma mass spectrometry(ICPMS)[J]. Journal of Mass Spectrometry and Advances in the Clinical Lab,2023,27:33-39.
[30] TANNER S D. Space charge in ICP-MS:calculation and implications[J]. Spectrochimica Acta,1992,47(6):809-823.
[31] TANNER S D,COUSINS L M,DOUGLAS D J.Reduction of space charge effects using a three-aperture gas dynamic vacuum interface for inductively coupled plasma-mass spectrometry[J]. Applied Spectroscopy,1994,48(11):1367-1372.
[32] NIU H S,HOUK R S. Langmuir probe measurements of the in extraction process in inductively coupled plasma mass spectrometry-I,spatially resolved determination electron density and electron temperature[J]. Spectrochim Acta Part B,1994,49(12/13/14):1283-1303.
基本信息:
DOI：10.20236/j.CJIAC.2025.12.005
中图分类号:O657.63;X833
引用信息:
[1]李凯,王雷,方哲,等.双提取透镜-电感耦合等离子体质谱(ICP-MS)法测定土壤中重金属元素[J].中国无机分析化学,2025,15(12):1942-1950.DOI:10.20236/j.CJIAC.2025.12.005.
基金信息:
超高纯金属痕量测试电感耦合等离子体质谱仪项目; 国家重点研发计划项目(2021YFF0700103)