摘要
为建立ICP-AES同时快速稳定测定土壤、水系沉积物中锰、钒、钛方法,开展了样品前处理方法、分析谱线的筛选、共存离子和基体干扰、方法准确度精密度检出限和加标回收试验。采用HCl-HNO_3-HClO_4-H_2SO_4-HF五酸加热溶样;以Mn259.37 nm、Ti338.3 nm,V292.40 nm为分析谱线;以水系沉积物国家标准样品绘制标准曲线进行基体匹配,减小试液基体、介质不一对测试结果的影响;方法检出限为Mn 0.096μg/g、Ti 0.125μg/g、V 0.098μg/g,经国家一级标准物质分析验证,分析值均与推荐值相符,方法精密度(RSD%)小于1.5%,相对误差小于3.0%,进行样品加标回收试验三种元素回收率为94.7%~105.2%。所建立的方法抗干扰能力强,稳定性高,线性范围宽,精密度高,结果准确,适用于土壤、水系沉积物及相关地质样品中Mn、V、Ti的快速分析。
In order to establish a method for simultaneous and rapid determination of Mn, V and Ti in soil and water sediments by ICP-AES, the pretreatment method of sample and the suitable analytical spectral lines has been selected, the coexistence ions and matrix interference and accuracy of the method of precision detection limit and the standard addition recovery test have been completed. The HCl-HNO_3-HCl O_4-H_-2SO_4-HF was used to dissolve the sample; The Mn259.37 nm, Ti338.3 nm, V292.40 nm was used as analytical spectral lines; The standard curve was drawn by the national standard of stream sediments samples matrix matching, to reduce the impact of test solution matrix, the different medium on the test results; Method detection limit were Mn 0.096 μg/g, Ti 0.125 μg/g, V 0.098 μg/g, it has been verified by national standard substances analysis, analysis of the values are in conformity with recommended value, method precision（RSD %） is less than 1.5%, the relative error less than 3.0%, the sample standard addition recovery experiment was carried out three elements recovery were 94.7% ~105.2%. The method has strong anti-jamming capability, high stability, wide linear range, high precision, accurate, applicable to the soil, stream sediment and the related geological samples fast analysis of Mn, V and Ti.
出处
《浙江化工》
CAS
2017年第3期47-51,共5页
Zhejiang Chemical Industry
