磷酸提取-高效液相色谱-氢化物发生原子荧光光谱法分析垃圾焚烧飞灰中无机砷形态  

Determination of Inorganic Arsenic Speciation in Municipal Solid Waste Incineration Fly Ash by High Performance Liquid Chromatography-Hydride Generation-Atomic Fluorescence Spectroscopy with Phosphoric Acid as Extracting Agent

作　　者：徐章[1] 胡红云[1] 陈敦奎 曹金秀[1] 姚洪[1] 

机构地区：[1]华中科技大学煤燃烧国家重点实验室,武汉430074

出　　处：《分析化学》2015年第4期490-494,共5页Chinese Journal of Analytical Chemistry

基　　金：国家重点基础研究发展计划(No.2011CB201505);湖北省科技支撑项目(No.2014BCB040)资助~~

摘　　要：以H3PO4为提取剂,通过微波提取的方法,采用高效液相色谱-氢化物发生原子荧光光谱联用技术（HPLC-HG-AFS）实现了垃圾焚烧飞灰中砷的价态测定。重点探究了H3PO4存在下,使用HPLC-HG-AFS测定无机砷（As（Ⅲ）和As（Ⅴ）价态的色谱条件。结果表明,当使用（NH4）2HPO4为流动相时,H3PO4的存在会对As？的分析造成不利影响,增大流动相流速对改善这种状况几乎没有效果;而使用Na2HPO4-KH2PO4混合溶液（p H 6.864）作为流动相时,可以显著降低H3PO4对As（Ⅴ）分析的干扰。在优化的色谱条件下,As（Ⅲ）和As（Ⅴ）可在5 min内实现分离,检出限分别为0.063和0.110μg/L。在标准物质加标回收实验中,各价态回收率良好（86.5%-102.5%）。利用本方法对来自4个垃圾焚烧电厂的飞灰样品进行分析,发现垃圾焚烧飞灰中的砷主要以As？的形式存在。A method for the determination of arsenic speciation in municipal solid waste incineration fly ash was developed by high performance liquid chromatography（ HPLC） coupled with hydride generation atomic fluorescence spectroscopy（ HG-AFS）. Before the determination,various forms of arsenic were extracted by phosphoric acid through microwave digestion. The effect of phosphoric acid in the extracted solution on the speciation analysis of inorganic arsenic（ As （Ⅲ） / As （Ⅴ）） was studied. The results showed that when using diammonium phosphate as mobile phase,the determination of As ？ was adversely affected. The increasing flow rate of mobile phase hardly reduced adverse influence caused by phosphoric acid. The adverse influence was effectively suppressed when a mixed solution of disodium hydrogen phosphate / potassium dihydrogen phosphate（ p H = 6. 864） was used as the mobile phase. By using the improved method,As（Ⅲ） and As （Ⅴ）could be separated in 5 minutes and the detection limits of As （Ⅲ） and As （Ⅴ） were 0. 063 μg / L and 0. 110 μg / L,respectively. The recovery rate of As （Ⅲ） and As （Ⅴ）in spiked standard sample was satisfactory（ 86. 9%- 102. 6%）. The determination of arsenic species in fly ashes sampled from four different municipal solid waste incineration plants was successfully accomplished by using the developed method. The results showed that the arsenic was predominant in the form of As（Ⅴ）.

关 键 词：无机砷 形态分析 高效液相色谱-氢化物发生原子荧光光谱技术 垃圾焚烧飞灰 

分 类 号：X831[环境科学与工程—环境工程] O657[理学—分析化学]