固相萃取-离子色谱法分析硫铁矿区酸性水中阴离子  

Determination of Anions in Acidic Mine Water from Pyrite Ore Mining Area Using Solid Phase Extraction and Ion Chromatography

作　　者：柳玲 王丽香 吴宇鑫 LIU Ling;WANG Li‑xiang;WU Yu‑xin(Shaanxi Academy of Environmental Sciences,Xi’an 710061,China)

机构地区：[1]陕西省环境科学研究院,陕西西安710061

出　　处：《中国给水排水》2025年第6期130-136,共7页China Water & Wastewater

基　　金：陕西省重点研发计划项目(2021ZDLSF05-10)。

摘　　要：为快速准确测定硫铁矿区酸性水中5种阴离子(F^(-)、Cl^(-)、NO_(2)^(-)、NO_(3)^(-)和SO_(4)^(2-))浓度,对ICS-1100离子色谱仪、流动相配比等色谱条件进行改进优化,选择亲水性强的IonPac AS19阴离子分离柱(250 mm×4 mm),IonPac AG19阴离子保护柱(50 mm×4 mm)以及AERS 500自动再生抑制器(4 mm);采用20.0 mmol/L的KOH为流动相,流速为1.0 mL/min,进样量为25μL。采用固相萃取前处理,以标准色谱图各组分保留时间定性,以色谱峰面积外标法定量。该方法能够在9 min内快速完成检测,分析效率较常规离子色谱法提高了40%,优化后的方法相关性好(r>0.999),检出限低(0.006~0.016 mg/L),精密度高(相对标准偏差0.2%~3.9%),加标回收率范围为89.2%~103.0%,有证标准物质测定结果在其置信区间内,相对误差范围为1.9%~4.8%。该方法简单快速,灵敏度高,适用于批量复杂基体酸性水质样品中阴离子的检测。To rapidly and accurately determine the concentrations of F^(-),Cl^(-),NO_(2)^(-),NO_(3)^(-)and SO_(4)^(2-)in acidic water from a pyrite ore mining area,the chromatographic conditions such as ICS-1100 ion chromatograph and flow compatibility ratio were improved and optimized.Specifically,the hydrophilic IonPac AS19 anion exchange column(250 mm×4 mm),the IonPac AG19 anion protection column(50 mm×4 mm)and the AERS 500 automatic regeneration inhibitor(4 mm)were selected.A 20.0 mmol/L KOH solution was employed as the mobile phase,with a flow rate of 1.0 mL/min and an injection volume of 25μL.Solid phase extraction pretreatment was adopted,and the retention time of each component in the standard chromatogram was used for qualitative analysis,while the chromatographic peak area external standard method was used for quantitative analysis.Compared to traditional ion chromatography,this method achieved rapid detection within 9 minutes,thereby enhancing analysis efficiency by 40%.The optimized method exhibited excellent correlation(r>0.999),a low detection limit(0.006-0.016 mg/L),high precision(relative standard deviation was 0.2%-3.9%),and a recovery rate range of 89.2%-103.0%.The determined results of the certified reference materials fell within the confidence interval,with a relative error range of 1.9%to 4.8%.The proposed method is characterized by its simplicity,rapidity,and high sensitivity,making it particularly suitable for the detection of anions in acidic water samples with complex matrix.

关 键 词：离子色谱法 固相萃取 酸性矿井水 阴离子 改进优化 

分 类 号：TU992[建筑科学—市政工程]