| 利用LC-AFS与ICP-OES测定污泥中砷形态及总砷含量 |
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| 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） |
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| 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 砷 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) |
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| Determination of Arsenic Speciations and Total Arsenic Content in Sludge by LC-AFS and ICP-OES |
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| 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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