摘要
建立了同时从沉积物中提取亚砷酸盐As(Ⅲ)、砷酸盐As(Ⅴ)、一甲基砷酸(MMA)和二甲基砷酸(DMA)4种砷形态的提取方法以及HPLC-ICP-MS联用测定沉积物中4种砷形态化合物的检测方法.探讨了磷酸、抗坏血酸、水浴时间等前处理条件,以及C8色谱柱和Hamilton PRP-X100色谱柱的色谱分离条件,由此建立了沉积物中砷形态的检测方法.结果表明,在95℃条件下水浴60 min,提取剂选择0.3 mol/L磷酸和0.5 mol/L抗坏血酸的混合溶液,4种砷形态化合物加标回收率在70%-110%之间,相对标准偏差(RSD)小于6%.选用Hamilton PRP-X100(5μm×15 cm)色谱柱进行4种砷形态的分离,以15 mmol/L磷酸氢二铵溶液(用甲酸调节pH=6.0)为流动相,在7 min内同时分析检测4种砷形态化合物,As(Ⅲ)、DMA、MMA和As(Ⅴ)的检出限依次为0.22、0.60、0.28和0.78μg/L.该方法实现了对沉积物中常见的不同形态砷的同时分析,具有灵敏度高、精密度好的特点.
A method for determining arsenite(As(Ⅲ)),arsenate(As(Ⅴ)),monomethyl arsenic acid(MMA)and dimethyl arsenic acid(DMA)in the sediment by water bath extraction and HPLC-ICP-MS is established.The pretreatment conditions were compared such as phosphoric acid,ascorbic acid,and water bath time,as well as the chromatographic separation conditions of the C8 column and the Hamilton PRPX100 column,thereby a method for detecting the speciation of arsenic in the sediment was established.A mixed solution of 0.3 mol/L phosphoric acid and 0.5 mol/L ascorbic acid was selected as the extractant,and the samples were bathed at 95℃for 60 min.The results show that the recoveries were between 70%and 110%,and the relative standard deviation was less than 6%.Four speciations of arsenic were separated by Hamilton PRP-X100 column.The mobile phase was 15 mmol/L(NH4)2HPO4 solution(adjusted the pH to 6.0 with formic acid).The peaks of four speciations of arsenic appeared within 7 min.The detection limits of As(Ⅲ),DMA,MMA and As(Ⅴ)were 0.22,0.60,0.28 and 0.78μg/L,respectively.The method realizes simultaneous analysis of different speciations of arsenic commonly found in sediments,with high sensitivity and good precision.
作者
赵彤
陈翠红
Zhao Tong;Chen Cuihong(College of Environmental Science and Engineering,Key Laboratory of Pollution Process and Environmental Criteria(Ministry of Education),Tianjin Engineering Center of Environmental Diagnosis and Contamination Remediation,Nankai University,Tianjin 300350,China)
出处
《南开大学学报（自然科学版）》
CAS
CSCD
北大核心
2020年第3期97-101,共5页
Acta Scientiarum Naturalium Universitatis Nankaiensis
基金
天津市自然科学基金(17JCQNJC08400)。
