摘要
本文研究了电感耦合等离子体质谱法(ICP-MS)分析铁矿石中的钾、钠,相较于常规检测方法,该方法具有更低的检出限。通过对消解参数、试剂纯度影响、加酸量、等离子体功率、雾化器流量、采样深度等条件因素进行优化,并通过干扰实验、检出限、方法精密度和回收率实验对方法进行了评价。结果表明,最佳的溶样条件为:消解温度达到210℃且保温时间超过20 min,溶样过程使用的硝酸、盐酸、氢氟酸需经过纯化,最佳加酸量为2.0 mL盐酸,0.5 mL氢氟酸,1.0 mL硝酸。最优的分析条件为:等离子体功率为900 W、雾化气流量为1.00 L/min、采样深度为150×102µm。本方法钾、钠的检出限达到1.02、1.53μg/L,测定下限达到4.40、5.10μg/L,回收率在90%~110%之间,精密度为(RSD)<5%。
In this paper,inductively coupled plasma mass spectrometry(ICP-MS)for the determination of potassium and sodium in iron ore was studied.Compared with conventional detection methods,this method has a lower detection limit.The parameters of digestion,the influence of reagent purity,the amount of acid added,plasma power,atomizer flow and sampling depth were optimized,and the method was evaluated by interference experiment,detection limit,precision and recovery experiment.The results show that the optimal dissolution conditions are as follows:the digestion temperature reaches 210℃and the holding time exceeds 20 min.The nitric acid,hydrochloric acid and hydrofluoric acid used in the dissolution process need to be purified.The optimal amount of acid added is 2.0 mL hydrofluoric acid,0.5 mL hydrofluoric acid and 1.0 mL nitric acid.The optimal analysis conditions are:plasma power of 900 W,atomizing gas flow rate of 1.00 L/min,sampling depth of 150×102µm.The detection limits of potassium and sodium were 1.02μg/L and 1.53μg/L,and the detection limits were 4.40μg/L and 5.10μg/L.The recoveries were between 90%and 110%,and the precision(RSD)was<5%.
作者
王贵玉
Wang Guiyu(Beijing Shougang Co.,Ltd.,Qian'an 064404,China)
出处
《冶金标准化与质量》
2024年第3期14-18,共5页
Metallurgical Standardization & Quality
关键词
电感耦合等离子体质谱法
铁矿石
钾
钠
inductively coupled plasma mass spectrometry
iron ore
potassium
sodium
