不同酸消解体系对微波消解测定土壤中重金属的影响
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摘要
为研究不同的酸消解体系对土壤中Cu、Zn、Pb、Cd、Cr、Ni、Co、V的消解效果,选择HNO_3+HF+H_2O_2、HNO_3+HCL+HF、HNO_3+HF+HCLO_4等不同酸体系,采用微波消解法对国家标准物质土壤进行处理,用电感耦合等离子体质谱仪(ICP-MS)对标准土壤样品中Cu、Zn、Pb、Cd、Cr、Ni、Co、V的含量进行了测定,以实验测定值和国家标准物质证书给定值进行比较,以3种酸消解准确度和精密度、加标回收率为依据,选出消解效果最好的酸消解体系。结果表明,以HNO_3+HF+HCLO_4酸体系的消解效果最佳,采用4 m L HNO_3+3 m L HF+1 m L HCLO_4消解,不仅节省酸的用量,而且可以保证消解完全。
To study the effects of different digestion system for the determination of Cu、Zn、Pb、Cd、Cr、Ni、Co and V in soil sample. The digestion liquid was compared with HNO3+HF+H_2O_2,HNO_3+HCL+HF and HNO_3+HF +HCLO_4,the microwave digestion and ICP-MS were applied to the analysis and determination of Cu、Zn、Pb、Cd、Cr、Ni、Co、V in national standard reference samples of soil. The optimal digestion system were selected of three different digestion reagents according to the contrast of experimental determination value and given value by National Standards Identified Centers,the accuracy and precision,spiked recoveries and digestion effects. The results showed that the optimal acid constitution was HNO_3+HF +HCLO_4,and adopted with 4 m L of HNO_3,2 m L of HF and 1 m L HCLO_4. It was not only save the amount of acid,but also dissolve completely.
To study the effects of different digestion system for the determination of Cu、Zn、Pb、Cd、Cr、Ni、Co and V in soil sample. The digestion liquid was compared with HNO3+HF+H_2O_2,HNO_3+HCL+HF and HNO_3+HF +HCLO_4,the microwave digestion and ICP-MS were applied to the analysis and determination of Cu、Zn、Pb、Cd、Cr、Ni、Co、V in national standard reference samples of soil. The optimal digestion system were selected of three different digestion reagents according to the contrast of experimental determination value and given value by National Standards Identified Centers,the accuracy and precision,spiked recoveries and digestion effects. The results showed that the optimal acid constitution was HNO_3+HF +HCLO_4,and adopted with 4 m L of HNO_3,2 m L of HF and 1 m L HCLO_4. It was not only save the amount of acid,but also dissolve completely.
引文
[1]蔡苹杨.电感耦合等离子体质谱法测定土壤中的铜锌铅镉[J].四川地质学报,2015,35(3):135-137.
[2]苏补拽,马建疆.常规消解与微波消解前处理方法测定土壤中重金属比较分析[J].内蒙古石油化工,2015,28(5):75-82.
[3]叶佩琳,胡银凤,朱宏斌,等.混合基体改进剂-石墨炉原子吸收光谱法测定速溶茶中的铅镉铬[J].食品安全质量检测学报,2015,6(5):1597-1602.
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[7]刘锟,周晓雪,土壤不同酸体系微波消解与电热板消解测试结果对比[J].化学计量,2015,8(2):27-30.
[8]蒋步云,柴振林.土壤中硒含量测定的消化方法探讨[J].土壤通报,2014,45(1):237-239.
[9]张琪,刘琳娟.高压密闭消解土壤砷、汞、铅、镉酸体系比较[J].中国环境监测,2009,25(5):48-50.
[10]倪张林,汤富彬,屈明华,等.微波消解-电感耦合等离子体质谱法测定油茶籽油中的5种重金属元素[J].食品科学,2013,34(4):169-173.
[11]黄薇,符式锦.微波消解-ICP-MS测定土壤及植物中硒的含量[J].广州化工,2014,12(1):146-148.
[12]任旭峰,王长智.微波消解-原子吸收法测定污泥中的铜、锌含量[J].广州化工,2015,43(4):120-122.
[13]高芹,邵劲松.微波消解原子吸收光谱法测定土壤中铅镉铬铜[J].监测分析,2011(2):99-101.
[14]刁晓东.微波消解-石墨炉原子吸收法测定土壤中钴[J].环境科学导刊,2014,3(33):137-140.
[2]苏补拽,马建疆.常规消解与微波消解前处理方法测定土壤中重金属比较分析[J].内蒙古石油化工,2015,28(5):75-82.
[3]叶佩琳,胡银凤,朱宏斌,等.混合基体改进剂-石墨炉原子吸收光谱法测定速溶茶中的铅镉铬[J].食品安全质量检测学报,2015,6(5):1597-1602.
[4]Kingston H M Standardization of sample Preparation for trace element determination through microwave enhanced chemistry[J].Atomic Spectroscopy,1998,19(2):27-30.
[5]朱振武,漾玉群.不同酸体系对微波消解法测量燃煤副产物中痕量元素的影响,(清华大学学报自然科学版)[J].2016,56(10):157-163.
[6]周燕琴.石墨炉原子吸收法测定土壤中痕量钴[J].污染防治技术,2015,28(2)51-54.
[7]刘锟,周晓雪,土壤不同酸体系微波消解与电热板消解测试结果对比[J].化学计量,2015,8(2):27-30.
[8]蒋步云,柴振林.土壤中硒含量测定的消化方法探讨[J].土壤通报,2014,45(1):237-239.
[9]张琪,刘琳娟.高压密闭消解土壤砷、汞、铅、镉酸体系比较[J].中国环境监测,2009,25(5):48-50.
[10]倪张林,汤富彬,屈明华,等.微波消解-电感耦合等离子体质谱法测定油茶籽油中的5种重金属元素[J].食品科学,2013,34(4):169-173.
[11]黄薇,符式锦.微波消解-ICP-MS测定土壤及植物中硒的含量[J].广州化工,2014,12(1):146-148.
[12]任旭峰,王长智.微波消解-原子吸收法测定污泥中的铜、锌含量[J].广州化工,2015,43(4):120-122.
[13]高芹,邵劲松.微波消解原子吸收光谱法测定土壤中铅镉铬铜[J].监测分析,2011(2):99-101.
[14]刁晓东.微波消解-石墨炉原子吸收法测定土壤中钴[J].环境科学导刊,2014,3(33):137-140.