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利用LC-AFS与ICP-OES测定污泥中砷形态及总砷含量
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作者单位
江晖,廖天宇,李广鹏,袁玲玲,耿文华 南京工业大学生物与制药工程学院 
基金项目:国家自然科学基金(21703134);陕西省自然科学基础研究计划面上项目(2018JM2040);商洛市科技局项目(SK2015-37)
中文摘要:应用液相色谱和原子荧光联用(LC-AFS)技术以及在线紫外消解技术分析了污泥中三价砷(As(Ⅲ))、一甲基砷(MMA)、二甲基砷(DMA)、五价砷(As(Ⅴ))和砷甜菜碱(AsB)5种砷形态含量,并利用电感耦合等离子体发射光谱(ICP-OES)测定了总砷(T-As)含量。通过对液相色谱分离、柱后衍生条件的优化,确定流动相为15 mmol/L (NH4)2HPO4,pH 6.0,载流5%(体积分数) HCl,还原剂为含5 g/L NaOH的10 g/L KBH4溶液,5种砷形态可在10 min内得到分离、测定。结果表明,总砷含量与各形态砷总和接近,相对标准偏差(RSD)在5%之内;As(Ⅲ)、As(Ⅴ)、MMA、DMA、AsB的检出限(以As计)分别为 0.3、2.1、1.4、1.1、0.7 μg/L,总砷的检出限为0.8 μg/L,且在线性范围内各砷形态和总砷标准曲线的相关系数均大于0.999。该方法前处理便捷,结果准确、重复性好,可为环境污泥中砷形态分析提供技术基础。
中文关键词:环境危害  污泥    形态测定  液相色谱-原子荧光联用(LC-AFS)  电感耦合等离子体发射光谱(ICP-OES)
 
Determination of Arsenic Speciations and Total Arsenic Content in Sludge by LC-AFS and ICP-OES
Abstract:The contents of five kinds of arsenic speciations in sludge,i.e.As(Ⅲ),monomethylarsenic(MMA),dimethylarsenic(DMA),As(Ⅴ) and arsenicbetaine(AsB) were determined by liquid chromatography hydride generation atomic fluorescence spectrometry(LC-AFS) with UV online digestion.The content of total arsenic(T-As) was determined by inductively coupled plasma optical emission spectrometry(ICP-OES).Under the optimized conditions for liquid phase separation and post column derivatization,the five arsenic speciations were separated and determined in 10 min with 15 mmol/L (NH4)2HPO4 as mobile phase at pH 6.0,5%(by volume) HCl as carrier and 5 g/L NaOH and 10 g/L KBH4 as reducing agents.In this experiment,the T-As was close to the sum of five arsenic speciations,and the relative standard deviations for them each other were less than 5%.The detection limits for As(Ⅲ),As(Ⅴ),MMA,DMA,AsB and T-As were 0.3,2.1,1.4,1.1,0.7 and 0.8 μg/L,respectively.The correlation coefficients for five arsenic speciations and T-As were larger than 0.999 in the linear range.With the advantages of convenient pretreatment,accuracy and reproducibility,the proposed method could provide a technical basis for the analysis of arsenic speciation in sludge.
Key Words:environmental hazards  sludge  arsenic  speciation analysis  liquid chromatography-atomic fluorescent spectrometry(LC-AFS)  ICP-OES
引用本文:江晖,廖天宇,李广鹏,袁玲玲,耿文华.利用LC-AFS与ICP-OES测定污泥中砷形态及总砷含量[J].分析测试学报,2018,37(9):1034-1039.
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