电感耦合等离子体发射光谱(ICP-OES)法测定废催化剂及浸取渣中7种有价元素  

Determination of Seven Valuable Elements in Spent Catalyst and Leaching Residue by Inductively Coupled Plasma Optical Emission Spectrometry

作　　者：田坤 徐臣松 罗昊楠 TIAN Kun;XU Chensong;LUO Haonan(Guizhou Wylton Catalyst Technology Co.,Ltd.,Tongren,Guizhou 554300,China)

机构地区：[1]贵州威顿催化技术有限公司,贵州铜仁554300

出　　处：《中国无机分析化学》2024年第10期1431-1436,共6页Chinese Journal of Inorganic Analytical Chemistry

基　　金：贵州省科技支撑项目(黔科合支撑[2021]一般302号);贵州省科技成果应用及产业化项目(黔科合支撑[2023]一般015)。

摘　　要：工业硫酸废催化剂中含有大量的钒、钠、钾、硫及少量铝、铁、砷物质,常作为钒和碱金属盐提取的重要原料。快速准确测定废催化剂及浸取渣中相关组分含量对其分离提取至关重要。在柱层析分离的基础上,浸取处理后样品中V、Na、S、K的浸出率分别为95.28%、98.39%、98.88%、97.82%,S扫描电子显微镜(SEM)表征结果表明,载体表面及孔道中沉积物溶解消失。同时,采用电感耦合等离子体发射光谱(ICP-OES)法进行测定,并确定了各元素的谱线(V 309.311 nm、Na 589.490 nm、K 766.490 nm、S 180.731 nm、Al 394.401 nm、Fe 238.204 nm、As 189.042 nm)。结果表明,各元素的质量浓度在一定范围内与发射强度呈线性、校准工作曲线的线性相关系数除砷为0.999 7外,均大于0.999 9,各元素的检出限为0.004~0.017μg/g,测定结果相对偏差(RSD,n=11)除砷为2.2%,其余元素均小于0.90%,且加标回收率在98.9%~102%。方法准确度及精密度均可以满足工业硫酸废催化剂中多种元素测试要求,为废催化剂浸取分离过程中各元素含量提供数据参考。Industrial sulfuric acid waste catalysts contain a large amount of vanadium,sodium,potassium,sulfur,and a small amount of aluminum,iron,and arsenic.They are often used as important raw materials for extracting vanadium and alkali metal salts.Rapid and accurate determination of relevant components in waste catalysts and leaching residues is crucial for their separation and extraction.On the basis of column chromatography separation,this article investigated the leaching rates of V,Na,S,and K in the samples after leaching treatment,which were 95.28%,98.39%,98.88%,and 97.82%,respectively.SEM showed that the sediment dissolved and disappeared on the surface of the carrier and in the pores.At the same time,the inductively coupled plasma emission spectroscopy(ICP-OES) method was used for determination,and the spectral lines of each element(V 309.311 nm,Na 589.490 nm,K 766.490 nm,S 180.731 nm,Al 394.401 nm,Fe 238.204 nm,As 189.042 nm) were determined.The results showed that the mass concentration of each element was linear with emission intensity within a certain range,and the linear correlation coefficient of the calibration working curve was greater than 0.999 9,except for arsenic,which was 0.999 7,The detection limit of each elementwas 0.004—0.017 μg/g,and the relative deviation(RSD,n=11) of the determination results excluding As was 2.2%.The other elements were less than 0.90%,and the recovery of the added standard was between 98.9% and 102%.The accuracy and precision of the method can meet the requirements for testing various elements in industrial sulfuric acid waste catalysts,providing data reference for the content of each element in the leaching and separation process of waste catalysts.

关 键 词：废催化剂 柱层析浸取 微波消解 电感耦合等离子体发射光谱法 

分 类 号：O657.31[理学—分析化学] X132[理学—化学]