利用LC-AFS与ICP-OES测定污泥中砷形态及总砷含量  

Determination of Arsenic Speciations and Total Arsenic Content in Sludge by LC-AFS and ICP-OES

作　　者：江晖[1] 廖天宇 李广鹏[1] 袁玲玲 耿文华[1] JIANG Hui;LIAO Tian-yu;LI Guang-peng;YUAN Ling-ling;GENG Wen-hua(College of Biotechnology and Pharmaceutical Engineering,Nanjing Tech University,Nanjing 211816,China)

机构地区：[1]南京工业大学生物与制药工程学院,江苏南京211816

出　　处：《分析测试学报》2018年第9期1034-1039,共6页Journal of Instrumental Analysis

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 (NH_4)_2HPO_4,pH 6. 0,载流5%(体积分数) HCl,还原剂为含5 g/L NaOH的10 g/L KBH_4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. 7μg/L,总砷的检出限为0. 8μg/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。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(NH 4)2HPO 4 as mobile phase at pH 6.0,5%(by volume)HCl as carrier and 5 g/L NaOH and 10 g/L KBH 4 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 0.8μg/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.

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) 

分 类 号：O657.3[理学—分析化学] X132[理学—化学]