首页> 中文期刊> 《冶金分析》 >免试剂离子色谱法测定入境冶炼渣浸出液中阴阳离子

免试剂离子色谱法测定入境冶炼渣浸出液中阴阳离子

         

摘要

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1 mL/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1.3 mL/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20 μg/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.%The anion and cation (F- , Cl- , NO2- , Br- , NO3- , SO42- , PO43- , Li+ , Na+ , NH4 + , K+ , Mg2+ and Ca2+ ) 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 elu-tion 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 methane-sulfonic 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 addition in the range 86 % -110 %.

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