串联电导及紫外检测器-离子色谱法测定土壤中6种有机酸根和无机阴离子  

IC Determination of 6 Organic and Inorganic Anions in Soil with Conductivity Detector and UV-Detector in Series

作　　者：王文佳[1] 刘娟[1] 尹雪梅[1] 李桂香 施超欧[1] 

机构地区：[1]华东理工大学化学与分子工程学院,上海200237 [2]澳实分析检测(上海)有限公司,上海201206

出　　处：《理化检验（化学分册）》2014年第1期19-22,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：应用离子色谱法测定土壤样品中正丁酸根、草酸根、溴离子、碘离子、氯离子及硫酸根等6种有机酸根和无机阴离子的含量.样品(10.00 g)用50 mmol·L-1氢氧化钠溶液50 mL超声提取60 min,离心分离.取上清液,经0.22 μm滤膜过滤和OnGuardⅡP柱净化.流出液稀释5倍后通过IonPac AG18柱分离,用不同浓度的氢氧化钾溶液进行梯度淋洗,用串联的电导检测器和紫外检测器(236 nm)进行检测.前者用于除碘离子外的5种阴离子的测定,后者用于碘离子的测定.上述6种阴离子的峰面积分别在一定范围与其质量浓度呈线性关系,其检出限(3S/N)在0.013～0.095 μg·g-1之间.加标回收率在92.0％～112％之间,测定值的相对标准偏差(n=6)在1.2％～7.2％之间.Six organic and inorganic anions including n-butyrate,oxalate,bromide,iodide,chloride and sulfate in soil were determined by ion chromatography (IC) with conductivity detector and UV-detector connected in series.The sample (10.00 g) was extracted ultarsonically with 50 mmol · L-1 NaOH solution (50 mL) for 60 min.After centrifugation,the supernatant was filtered with 0.22 μm membrane and purified on OnGuard ⅡP column.The eluate after diluting 5 times with water was separated on IonPAC AG18 column using KOH solutions of different concentrations as mobile phase in gradient elution.The 5 anions besides I-were detected with conductivity detector and iodide ion was detected by UV detector at 236 nm.Linear relationships between values of peak area and mass concentration of the 6 anions were kept in definite ranges with values of detection limits (3S/N) in the range of 0.013-0.095 μg · g-1.Values of recovery given by standard addition method were in the range of 92.0％-112％,with values of RSD's (n=6) ranged from 1.2％ to 7.2％.

关 键 词：离子色谱法 土壤 有机酸根 无机阴离子 电导检测器 紫外检测器 

分 类 号：O657.1[理学—分析化学] X832.02[理学—化学]