微波三步提取-高效液相色谱-原子荧光法测定土壤中砷形态
钱晓燕1,马杰12,雷梅3,翁莉萍1,陈雅丽1,廖仲彬1,李永涛12
1.农业部环境保护科研监测所,天津 300191; 2.华南农业大学资源环境学院,广州 510642; 3.中国科学院地理科学与资源研究所,北京 100101
Determination of arsenic species in soils by three-step microwave extraction-HPLC-AFS
钱晓燕1,马杰12,雷梅3,翁莉萍1,陈雅丽1,廖仲彬1,李永涛12
1. Agro-Environmental Protection Institute, Ministry of Agriculture, Tianjin 300191, China; 2. College of Natural Resources and Environment, South China Agricultural University, Guangzhou 510642, China; 3. Institute of Geographic Sciences and Natural Resources Research, Chinese Academy of Sciences, Beijing 100101, China
摘要:采用高效液相色谱-原子荧光法对土壤中的砷形态进行分析,以了解其对土壤的污染程度。用1 mol/L磷酸-0.5 mol/L抗坏血酸混合提取剂对污染土壤样品进行三步微波提取,用高效液相色谱-原子荧光联用仪测定砷形态含量。As(Ⅲ)和As(V)标准工作曲线的线性范围均为8~100 μg/L,线性相关系数(r2)分别为0.999,0.996,检出限分别为0.11,0.72 μg /L。As(Ⅲ),As(V)测定结果的相对标准偏差分别7.6%和9.1% (n=11),加标回收回收率在82.2%~98.3%之间。多数土壤中砷形态以As(V)为主,As(Ⅲ)含量较低。该方法对土壤中的砷提取效果好,测定结果可靠,可为土壤砷污染的修复提供技术支撑。
Abstract:In order to evaluate arsenic contamination in soils, arsenic species in soils was analyzed by high-performance liquid chromatography-atomic fluorescence spectrometry (HPLC-AFS). Arsenic in soils was extracted by using three-step microwave extraction method with 1 mol/L phosphoric acid-0.5 mol/L ascorbic acid, and then the arsenic was determined by HPLC-AES. The linear range of standard working curve was 8-100 μg/L for As(Ⅲ) and As(V). The correlation coefficients were 0.999 and 0.996, and detection limits were 0.11 μg/L and 0.72 μg/L for As(Ⅲ) and As(V), respectively. The relative standard deviation of the results of AsAs(Ⅲ) and As(V) in the precision test were 7.6% and 9.1% (n=11), respectively. The spiked recoveries ranged from 82.2%-98.3%. For most soil samples, As(V) was predominant, the contents of As(Ⅲ) were low. This method is precise and accurate for arsenic species analysis in soil with good extraction effect, which can effectively supported the research of As-contaminated soils remediation.
关键词:砷形态;土壤;三步微波提取;高效液相色谱-原子荧光法
Keywords:arsenic species; soil; three-step microwave extraction; high performance liquid chromatography-atomic fluorescence spectrometry
本文引用格式:
钱晓燕,马杰,雷梅,等.微波三步提取-高效液相色谱-原子荧光法测定土壤中砷形态[J].化学分析计量,2018,27(6):5-10.
QIAN X Y,MA J,LEI M,et al. Determination of arsenic species in soils by three-step microwave extraction-HPLC-AFS[J]. Chemical analysis and meterage,2018,27(6):5-10
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