液相色谱-原子荧光光谱法测定地表水中的价态砷  

Determination of Valent Arsenic in Surface Water by Liquid Chromatography Atomic FluorescenceSpectroscopy

作　　者：杜江 向文礼 张玲艳 张妍 DU Jiang;XIANG Wen-li;ZHANG Ling-yan;ZHANG Yan(Yunnan Provincial Ecological Environment Monitoring Center,Kunming 650034,China)

机构地区：[1]云南省生态环境监测中心,云南昆明650034

出　　处：《精细化工中间体》2024年第2期75-80,共6页Fine Chemical Intermediates

摘　　要：建立地表水中价态砷(As^(3+)、As^(5+))的液相色谱-原子荧光光谱分析方法,采用Hamilton PRP-X100色谱柱,以磷酸二氢钾和磷酸氢二钠溶液为流动相,流速1.2 mL/min,进样体积100μL,等度洗脱。As^(3+)和As^(5+)的方法检出限分别为0.60、0.69μg/L,相对标准偏差分别为3.6%~11.0%、4.9%~9.0%,加标回收率分别为85.5%~93.6%、84.8%~96.4%,并对某受污染地表水体进行实样测试,验证该方法的可行性。该方法在测定地表水中三价砷和五价砷时,样品前处理简单,只需用0.45μm滤膜过滤;分析速度快,1个样最多只需8 min;仪器灵敏度高,性能稳定;精密度、准确度优;标曲线性良好(r≥0.999);试剂用量少;分离效果好;操作简单,适用于地表水中价态砷(As3+、As5+)的测定。By establishing liquid chromatography-atomic fluorescence spectrometry method,a Hamilton PRPX100 chromatographic column was used,a solution of potassium dihydrogen phosphate and disodium hydrogen phosphate was used as mobile phase;the flow rate was 1.2 mL/min;injection volume was of 100μL,and isocratic elution mode was used for testing.The detection limits of As3+and As5+were 0.60μg/L and 0.69μg/L,respectively.The relative standard deviations were 3.6%~11.0%and 4.9%~9.0%,respectively.The recovery rates of spiking were 85.5%~93.6%and 84.8%~96.4%,respectively,and the feasibility of this method was verified by conducting real sample testing on a polluted surface water body.Experimental results showed that this method had the advantages of simple sample pretreatment and only required 0.45μm filter membrane filtration when determining trivalent and pentavalent arsenic in surface water.This analysis process is fast with 8 minutes for each sample.The instrument has high sensitivity and stable performance,excellent precision and accuracy,good linearity of the standard curve(r≥0.999),low reagent usage,good separation effect.The instrument has the advantages of simple operation and is suitable for the determination of valence arsenic(As3+,As5+)in surface water.

关 键 词：液相色谱-原子荧光光谱法 地表水 三价砷 五价砷 

分 类 号：O657.31[理学—分析化学]