免试剂离子色谱法测定入境冶炼渣浸出液中阴阳离子

Determination of anion and cation in leaching solution of imported smelting slag by reagent free ion chromatography

用免试剂离子色谱法对冶炼渣中阴、阳离子(F-,Cl-,NO2-,Br-,NO3-,SO42-,PO43-,Li+,Na+,NH4+,K+,Mg2+和Ca2+)进行了测定。阴离子分离条件:阴离子交换柱Ion Pac AS19,氢氧化钾溶液梯度淋洗,抑制电导检测,流速为1mL/min;阳离子分离条件:阳离子交换柱Ion Pac CS16,甲基磺酸溶液梯度淋洗,抑制电导检测,流速为1.3mL/min。同一天内的待测离子峰保留时间、峰高和峰面积的相对标准偏差分别小于0.35%,1.8%和1.1%,连续5天的待测离子峰保留时间、峰高和峰面积的相对标准偏差分别小于0.78%,2.4%和1.6%。被测离子的浓度与峰面积具有良好的线性,相关系数r=0.999 0～0.999 9,检出限低于20μg/L。对入境氧化铁皮渣、钒渣、富锰渣浸出液中阴、阳离子进行测定,加标回收率在86%～110%之间。

Abstract： The anion and cation （F^-,C1^-,NO2^-,Br^-,NO3^-,SO4^2-,PO4^3-,Li^＋,Na^＋,NH4^＋,K^＋,Mg^2＋andCa^2＋） in leaching solution of smelting slag were determined by reagent free ion chro- matography. The separation conditions of anion： cation exchange column Ion Pac AS19, gradient elution with potassium hydroxide solution, suppressed conductance detection, flow rate of 1 mL/min; separation conditions of cation, anion exchange column Ion Pac CS16, gradient elution with methanesulfonic acid solution, suppressed conductance detection, flow rate of 1. 3 mL/min. The relative standard deviations （RSDs） of retention time, peak height and peak area of testing ions within one day were less than 0.35 %, 1.8 % and 1.1%, respectively. The RSDs of retention time, peak height and peak area of testing ions in continuous five days were less than 0.78 %, 2.4 % and 1.6 %, respectively. The concentration of determined ions with its peak area had good linearity （r=0. 999 0-0. 999 9）. The detection limit was lower than 20 μg/L. The anion and cation in leaching solution of imported scale slag, vanadium slag and manganese-rich slag were determined with recoveries of standard addi- tion in the range 86 %-110 %.