微波消解-ICPMS法测定不同肥料中镍含量
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摘要
试验选用了有机肥、生物有机肥和复合微生物肥料三种肥料,利用微波消解法和常压酸解法两种方法前处理样品,建立了用电感耦合等离子体质谱仪测定肥料中镍含量的方法。试验结果表明:微波消解法和常压酸解法的线性相关系数均大于0.9995,方法检出限在0.0059～0.0065 mg/kg之间,相对标准偏差均小于5%,各梯度质量浓度加标回收率在92.3%～104.2%之间。两种方法的线性范围、精密度和回收率良好,都符合要求。但微波消解法相对而言更加简便和快速,能够缩短样品前处理时间并且减少试剂用量,可大大提高工作效率,减少试验成本,更适合于肥料中镍含量的测定。
Three kinds of fertilizers, including organic fertilizer, bio-organic fertilizer and compound microbial fertilizer, were used to pretreat by microwave digestion and atmospheric acid digestion. A method for the determination of nickel in fertilizers by inductively coupled plasma mass spectrometry(ICP-MS) was established. The experimental results show that the linear correlation coefficients of microwave digestion and atmospheric acid digestion are greater than 0.9995. The detection limit of the method is between 0.0059 mg/kg and 0.0065 mg/kg. The relative standard deviations are less than 5 %, and the recovery rates of gradient mass concentration are between 92.3 % and 104.2 %. The linear range, precision and recovery of the two methods are satisfactory and meet the requirements. However,microwave digestion is relatively simple and fast, which can shorten the sample pretreatment time and reduce the amount of reagents. It can greatly improve work efficiency, reduce test costs, and is more suitable for the determination of nickel content in fertilizers.
Three kinds of fertilizers, including organic fertilizer, bio-organic fertilizer and compound microbial fertilizer, were used to pretreat by microwave digestion and atmospheric acid digestion. A method for the determination of nickel in fertilizers by inductively coupled plasma mass spectrometry(ICP-MS) was established. The experimental results show that the linear correlation coefficients of microwave digestion and atmospheric acid digestion are greater than 0.9995. The detection limit of the method is between 0.0059 mg/kg and 0.0065 mg/kg. The relative standard deviations are less than 5 %, and the recovery rates of gradient mass concentration are between 92.3 % and 104.2 %. The linear range, precision and recovery of the two methods are satisfactory and meet the requirements. However,microwave digestion is relatively simple and fast, which can shorten the sample pretreatment time and reduce the amount of reagents. It can greatly improve work efficiency, reduce test costs, and is more suitable for the determination of nickel content in fertilizers.
引文
[1]张西科,张福锁,李春俭.植物生长必需的微量营养元素--镍[J].土壤,1996(4):176-179.
[2]张秀玲,宋光煜.植物的镍素营养[J].中国土壤与肥料,2004(6):33-36.
[3]王鹏新.土壤和植物中的镍及其相互关系[J].农业环境保护,1993(5):213-216.
[4]吴玉萍,林小峰,孔光辉,等.微波消解ICP-MS测定有机肥中的砷、铅、镉、镍和铬[J].光谱实验室,2016,31(06):000751-755.
[5]NY/T 305.1-1995有机肥料铜的测定[S].北京:中国标准出版社,1995.
[2]张秀玲,宋光煜.植物的镍素营养[J].中国土壤与肥料,2004(6):33-36.
[3]王鹏新.土壤和植物中的镍及其相互关系[J].农业环境保护,1993(5):213-216.
[4]吴玉萍,林小峰,孔光辉,等.微波消解ICP-MS测定有机肥中的砷、铅、镉、镍和铬[J].光谱实验室,2016,31(06):000751-755.
[5]NY/T 305.1-1995有机肥料铜的测定[S].北京:中国标准出版社,1995.