HNO_3-HClO_4消解-电感耦合等离子体质谱法测定粪肥中27种元素
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摘要
建立了电感耦合等离子体质谱仪(ICP-MS)测定粪肥中微量元素的分析方法。采用HNO_3-HClO_4[V(HNO_3)∶V(HClO_4)=3∶1]体系消解样品,利用普通/ORS混合模式-电感耦合等离子体质谱仪(ICP-MS)测定粪肥中Li、Be、Al、Ti、V、Cr、Mn、Fe、Co、Ni、Cu、Zn、Ga、As、Se、Sr、Mo、Ag、Cd、Sn、Sb、Te、Ba、Tm、Tl、Pb、U等27种微量元素。经标准物质和加标样品检测验证表明,测定结果与推荐值(或加标值)基本相符,回收率为80. 2%～112. 5%,相对标准偏差RSD<10%。27种元素的检测限(LOD)为0. 1～48. 3 mg/kg。该方法适用于实验室开展粪肥中27种微量元素的同步检测。
This paper describes a validation process for the simultaneous determination of 27 elements including Li,Be,Al,Ti,V,Cr,Mn,Fe,Co,Ni,Cu,Zn,Ga,As,Se,Sr,Mo,Ag,Cd,Sn,Sb,Te,Ba,Tm,Tl,Pb and U in manure samples by inductively coupled plasma mass spectrometry( ICP-MS) with octopole reaction system( ORS).Several criteria such as sample digestion condition,method linearity and limits of detection( LOD) are evaluated. A standard reference material and some spiked test samples are analyzed,and the recovery varies from 80. 2% to 112. 5%. Relative standard deviations RSD for this method are less than 10%.Limits of detection for 27 elements are obtained within the range of 0. 1 mg·kg-1( V,etc) to 48. 3 mg·kg-1( Fe).Results indicate that this method can be used in the laboratory for the routine determination of these 27 essential and nonessential elements in manure fertilizers.
This paper describes a validation process for the simultaneous determination of 27 elements including Li,Be,Al,Ti,V,Cr,Mn,Fe,Co,Ni,Cu,Zn,Ga,As,Se,Sr,Mo,Ag,Cd,Sn,Sb,Te,Ba,Tm,Tl,Pb and U in manure samples by inductively coupled plasma mass spectrometry( ICP-MS) with octopole reaction system( ORS).Several criteria such as sample digestion condition,method linearity and limits of detection( LOD) are evaluated. A standard reference material and some spiked test samples are analyzed,and the recovery varies from 80. 2% to 112. 5%. Relative standard deviations RSD for this method are less than 10%.Limits of detection for 27 elements are obtained within the range of 0. 1 mg·kg-1( V,etc) to 48. 3 mg·kg-1( Fe).Results indicate that this method can be used in the laboratory for the routine determination of these 27 essential and nonessential elements in manure fertilizers.
引文
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[2]李见云,侯彦林,化全县,等.大鹏设施土壤养分和重金属状况研究[J].土壤,2005,37(6):626-629.
[3]刘荣乐,李书田,王秀斌,等.我国商品有机肥料和有机废弃物中重金属的含量状况与分析[J].农业环境科学学报,2005,24(2):392-397.
[4]张树清,张夫道,刘秀梅,等.规模化养殖畜禽粪主要有害成分测定分析研究[J].植物营养与肥料学报,2005,11(6):822-829.
[5]赵文,潘运舟,兰天,等.海南商品有机肥中重金属和抗生素含量状况与分析[J].环境化学,2017,36(2):408-419.
[6]Honna T.Manuring effect on rice grain yield and extractable trace elements in soils[J].Journal of Plant Nutrition,2001,24(7):967-977.
[7]Sandrine Millour,Laurent Noe,Ali Kadar,et al. Simultaneous analysis of 21 elements in foodstuffs by ICP-MS after closed-vessel microwave digestion:Method validation[J].Journal of Food Composition and Analysis,2011,24(1):111-120.
[8]Guerin T,Chekri R,Vastel C,et al.Determination of 20 trace elements in fish and other seafood from the French market[J]. Food Chemistry,2011,127(3):934-942.
[9]中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.GB/T 13079—2006.饲料中总砷的测定[S].北京:中国标准出版社,2006.
[10]国家标准化管理委员会.GB/T 17138—1997土壤质量铜、锌的测定火焰原子吸收分光光度法[S].北京:中国标准出版社,1997.
[11]何飞飞,任涛,杨君.三元复混肥和鸡粪肥中重金属含量特征分析与评价[J].湖南农业大学学报(自科版),2011,37(6):665-668.
[12]吴国旭.电感耦合等离子体质谱(ICP-MS)对土壤中Cr、Ni、Cu、Zn、As、Cd、Hg、Pb分析方法研究[D].天津:南开大学,2004.
[13]Thompson J J,Houk R S.A study of internal standardization in inductively coupled plasma-mass spectrometry[J]. Applied Spectroscopy,1987,41(5):801-806.
[14]Kah Hin Low,Sharifuddin Md.Zain,Mhd.Radzi Abas.Evaluation of microwave-assisted digestion condition for the determination of metals in fish samples by inductively coupled plasma mass spectrometry using experimental designs[J].International Journal of Environmental Analytical Chemistry,2012,92(10):1161-1175.
[15]孙耀帆,李群,江志刚,等.电感耦合等离子体质谱法测定花生中34种元素[J].分析试验室,2012,(6):108-112.
[16]中华人民共和国国家质量监督检验检疫总局.JJF 1159—2006.四极杆电感耦合等离子体质谱仪校准规范[S].北京:中国计量出版社,2006.