【引用本文】 薛静, 安帅, 汪寅夫, 等. 王水水浴消解-电感耦合等离子体质谱法测定土壤中的硒[J]. 岩矿测试, 2020, 39(5): 725-730. doi: 10.15898/j.cnki.11-2131/td.202003050025
XUE Jing , AN Shuai , WANG Yin-fu , et al. Determination of Selenium in Soil by Inductively Coupled Plasma-Mass Spectrometry with Aqua Regia Digestion in Water Bath[J]. Rock and Mineral Analysis, 2020, 39(5): 725-730. doi: 10.15898/j.cnki.11-2131/td.202003050025

王水水浴消解-电感耦合等离子体质谱法测定土壤中的硒

1. 中国地质调查局沈阳地质调查中心, 辽宁 沈阳 110032;

2. 辽宁省有色地质勘查总院有限责任公司, 辽宁 沈阳 110121

收稿日期: 2020-03-05  修回日期: 2020-04-20 

作者简介: 薛静,硕士,工程师,主要从事土壤、岩石矿物等无机元素的分析工作。E-mail:may927@163.com。。

Determination of Selenium in Soil by Inductively Coupled Plasma-Mass Spectrometry with Aqua Regia Digestion in Water Bath

1. China Geological Survey Shenyang Geological Survey Center, Shenyang 110032, China;

2. Liaoning Nonferrous Geological Exploration Institute Limited Liability Company, Shenyang 110121, China

Received Date: 2020-03-05
Revised Date: 2020-04-20

摘要:随着富硒产品关注度越来越高,对土壤中硒含量测定的研究也越来越受到人们的重视。应用传统电感耦合等离子体质谱法(ICP-MS)测定土壤样品中的硒时,受到的基体效应和多原子离子干扰比较显著,准确测定硒含量的难度较大。本文建立了采用50%王水-沸水浴消解体系,ICP-MS测定土壤样品中硒含量的方法,采用动能歧视模式(KED)消除质谱干扰,选用103Rh元素作为在线加入内标以消除仪器信号漂移。用该方法对有证土壤标准物质进行分析,其结果均在不确定度范围内,方法相对误差介于-2.01%~2.99%之间,相对标准偏差(RSD)小于6.60%,检出限为0.012μg/g,测定下限为0.048μg/g。应用该方法与国家环境保护标准方法(HJ680—2013)对20个土壤实际样品进行比对分析,其结果基本一致。该方法适合于地质等行业大批量分析测定土壤样品中的硒。

关键词: 水浴消解, 电感耦合等离子体质谱法, 土壤, , 动能歧视模式

Determination of Selenium in Soil by Inductively Coupled Plasma-Mass Spectrometry with Aqua Regia Digestion in Water Bath

KEY WORDS: water bath digestion, inductively coupled plasma-mass spectrometry, soil, selenium, kinetic energy discrimination

本文参考文献

[1]

刘金巍,刘雪松,边超,等.甲烷动态反应电感耦合等离子体质谱法测定地下水中痕量硒[J]岩矿测试,2019,38(1):85-91.

Liu J W,Liu X S,Bian C,et al.Determination of trace selenium in groundwater by DRC ICP-MS[J].Rock and Mineral Analysis,2019,38(1):85-91.

[2]

王俊伟,钱蜀,李海霞,等.电感耦合等离子体质谱法测定土壤样品中的痕量硒元素[J].中国环境监测,2012,28(3):97-100.

Wang J W,Qian S,Li H X,et a1.Determination of trace selenium in soils by inductively coupled plasma-mass spectrometry[J].Environmental Monitoring in China,2012,28(3):97-100.

[3]

钱薇,唐昊冶,王如海,等.一次消解土壤样品测定汞、砷和硒[J].分析化学,2017,45(8):1215-1221.

Qian W,Tang H Y,Wang R H,et al.Determination of mercury,arsenic and selenium in soils by one-time digestion[J].Chinese Journal of Analytical Chemistry,2017,45(8):1215-1221.

[4]

谭芳维,黄菲,唐秀龙,等.水浴消解-原子荧光法测定土壤中硒、锑的研究[J].广州化工,2019,47(6):103-105.

Tan F W,Huang F,Tang X L,et al.Determination of selenium and antimony in soil by water bath digestion-atomic fluorescencel[J].Guangzhou Chemical Industry,2019,47(6):103-105.

[5]

陈海英.王水水浴消解-双道原子荧光光谱法(AFS)同时测定土壤中的汞和硒[J].农业科技与装备,2013,10(10):13-15.

Chen H Y.Simultaneous determination of mercury and selenium in soil with aqua regia digestion in water bath and double channel atomic fluorescence spectrometry (AFS)[J].Agricultural Science & Technology and Equipment,2013,10(10):13-15.

[6]

林海兰,朱日龙,于磊,等.水浴消解-原子荧光光谱法测定土壤和沉积物中砷、汞、硒、锑和铋[J].光谱学与光谱分析,2020,40(5):1528-1533.

Lin H L,Zhu R L,Yu L,et al.Determination of arsenic,mercury,selenium,antimony and bismuth in soil and sediments by water bath digestion-atomic fluorescence spectrometry[J].Spectroscopy and Spectral Analysis,2020,40(5):1528-1533.

[7]

黄薇,符式锦,王旭日,等.微波消解-ICP-MS测定土壤及植物中硒的含量[J].广州化工,2014,42(23):146-148.

Huang W,Fu S J,Wang X R,et al.Determination of selenium in soil and plant by microwave digestion-ICP-MS[J].Guangzhou Chemical Industry,2014,42(23):146-148.

[8]

刘芸,曹国松,程佩,等.微波消解-ICP-MS法测定土壤中的硒含量[J].化学与生物工程,2017,34(11):67-70.

Liu Y,Cao G S,Cheng P,et al.Determination of selenium content in soil by microwave digestion-ICP-MS[J].Chemistry & Bioengineering,2017,34(11):67-70.

[9]

田敏,刘畅.两种消解土壤中硒的方法对比分析[J].黑龙江环境通报,2007,31(3):33-34.

Tian M,Liu C.Comparative analysis of two digestion method of selenium in soil[J].Heilongjiang Environmental Journal,2007,31(3):33-34.

[10]

屈明华,陈雄弟,倪张林,等.DRC-ICP-MS法测定土壤硒前处理方法研究[J].土壤通报,2019,50(3):698-703.

Qu M H,Chen X D,Ni Z L,et al.Pretreatment for determination of soil selenium by ICP-MS with dynamic reaction cell[J].Chinese Journal of Soil Science,2019,50(3):698-703.

[11]

严进.双氧水氧化1-(2-吡啶偶氮)-2-萘酚动力学光度法测定痕量硒[J].广州化工,2016,44(21):132-134.

Yan J.Determination of selenium by catalytic kinetic spectrophotometry in hydrogen peroxide-PAN system[J].Guangzhou Chemical Industry,2016,44(21):132-134.

[12]

韩亚,郭伟,汪洪.电感耦合等离子体质谱(ICP-MS)法与氢化物发生-原子吸收光谱(HG-AAS)法测定土壤中硒含量的对比研究[J].中国无机分析化学,2020,10(3):28-32.

Han Y,Guo W,Wang H.Methodcomparison for determination of selenium in soil by ICP-MS and HG-AAS[J].Chinese Journal of Inorganic Analytical Chemistry,2020,10(3):28-32.

[13]

冯永明,邢应香,刘洪青,等.微波消解-电感耦合等离子体质谱法测定生物样品中微量硒的方法研究[J].岩矿测试,2014,33(1):34-39.

Feng Y M,Xing Y X,Liu H Q,et al.Determination of trace selenium in biological samples by inductively coupled plasma-mass spectrometry with microwave digestion[J]. Rock and Mineral Analysis,2014,33(1):34-39.

[14]

程秀花,王海蓉,黎卫亮,等.电感耦合等离子体质谱法测定硒时多元素干扰的碰撞/反应研究及其在地质样品中的应用[J].冶金分析,2015,35(12):5-9.

Cheng X H,Wang H R,Li W L,et al.Study on collision/reaction for multielement interference in determination of selenium by inductively coupled plasma mass spectrometry and its application to geological sample[J].Metallurgical Analysis,2015,35(12):5-9.

[15]

徐鹏,孙亚莉.Carius管密封溶样-等离子体质谱法测定环境样品中镓、锗、砷、硒、镉、锡、锑、碲、汞、铅和铋[J].分析化学,2010,38(4):581-584.

Xu P,Sun Y L.Determination of Ga,Ge,As,Se,Cd,Sn,Sb,Te,Hg,Pb and Bi in environmental samples by inductively coupled plasma mass spectrometry combined with Carius tube digestion[J].Chinese Journal of Analytical Chemistry,2010,38(4):581-584.

[16]

D'Ilio S,Violante N,Majorani C,et al.Dynamic reaction cell ICP MS for determination of total As,Cr,Se and V in complex matrices:Still a challenge? A review[J].Analytica Chimica Acta,2011,698(1):6-13.

[17]

陈波,刘洪青,邢应香.电感耦合等离子体质谱法同时测定地质样品中锗硒碲[J].岩矿测试,2014,33(2):192-196.

Chen B,Liu H Q,Xing Y X.Simultaneous determination of Ge,Se and Te in geological samples by inductively coupled plasma-mass spectrometry[J].Rock and Mineral Analysis,2014,33(2):192-196.

[18]

刘征宙,曹丽丽,陈浩云,等.电感耦合等离子体质谱法-碰撞反应池技术测定高纯度磷酸二氢钾中痕量金属元素[J].化学试剂,2015,37(9):809-811

,842. Liu Z Z,Cao L L,et al.Chen H Y,Detection of trace metal elements in potassium dihydrophate with ICP-MS(CCT) method[J].Chemical Reagents,2015,37(9):809-811,842.

[19]

余兴.电感耦合等离子体四极杆质谱碰撞/反应池技术现状与进展[J].冶金分析,2013,33(3):14-23.

Yu X.The present situation and advance in collision/reaction cell technique of inductively coupled plasma quadrupole mass spectrometry[J].Metallurgical Analysis,2013,33(3):14-23.

[20]

章连香,冯先进.八极杆碰撞/反应池(ORS)-电感耦合等离子体质谱(ICP-MS)法测定复杂矿物中的稀土元素[J].中国无机分析化学,2017,7(2):22-26.

Zhang L X,Feng X J.Determination of rare earth elements in complex minerals by octopole reaction system (ORS)-inductively coupled plasma mass spectrometry (ICP-MS)[J].Chinese Journal of Inorganic Analytical Chemistry,2017,7(2):22-26.

[21]

韩建华,孙传强,汪曣,等.电感耦合等离子体质谱中碰撞反应池的模拟探讨[J].冶金分析,2014,34(9):1-7.

Han J H,Sun C Q,Wang Y,et al.Discussion on the simulation of collision reaction cell in inductively coupled plasma mass spectrometry[J].Metallurgical Analysis,2014,34(9):1-7.

[22]

陕红,孙宝利,黄金丽,等.DRC-ICP-MS测定蜂王浆中硒的方法研究[J].分析测试学报,2016,35(9):1191-1194.

Shan H,Sun B L,Huang J L,et al.Analysis of selenium in royal jelly by ICP-MS with dynamic reaction cell[J].Journal of Instrumental Analysis,2016,35(9):1191-1194.

[23]

杏朝刚,袁京群,李士敏.微波消解-动态反应池电感耦合等离子体质谱测定农产品中的痕量硒[J].浙江农业学报,2018,30(8):1414-1419.

Xin C G,Yuan J Q,Li S M.Determination of trace selenium in agricultural products with microwave digestion-dynamic reaction cell inductively coupled plasma mass spectrometry[J].Acta Agriculturae Zhejianggensis,2018,30(8):1414-1419.

[24]

徐进力,邢夏,唐瑞玲,等.动能歧视模式ICP-MS测定地球化学样品中14种痕量元素[J].岩矿测试,2019,38(4):394-402.

Xu J L,Xing X,Tang R L,et al.Determination of 14 trace elements in geochemical samples by ICP-MS using kinetic energy discrimination mode[J].Rock and Mineral Analysis,2019,38(4):394-402.

[25]

黄子敬,陈孟君,邓华阳,等.微波消解-ICP-MS混合模式测定动植物源食品中11种金属元素[J].分析试验室,2017,36(1):24-28.

Huang Z J,Chen M J,Deng H Y,et al.Determination of 11 trace elements in animal and plant origin food by microwave digestion with ICP-MS in mixed mode[J].Chinese Journal of Analysis Laboratory,2017,36(1):24-28.

[26]

林珍,黄超冠,卢燕平,等.沸水浴-氢化物发生原子荧光光谱法测定土壤中的硒[J].广州化学,2017,42(3):34-37.

Lin Z,Huang C G,Lu Y P,et al.Boilingwater bath-determination of selenium in soil by hydride generation atomic fluorescence spectrometry[J].Guangzhou Chemistry,2017,42(3):34-37.

[27]

郑欣.X Series 2 ICP-MS CCTED在食品样品超痕量元素分析中的应用[J].环境化学,2009,28(3):467-468.

Zheng X.Application of X Series 2 ICP-MS CCTED in analysis of ultra-trace elements of food samples[J].Environmental Chemistry,2009,28(3):467-468.

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王水水浴消解-电感耦合等离子体质谱法测定土壤中的硒

薛静, 安帅, 汪寅夫, 高慧莉, 史佳铭