便携式X射线荧光光谱法同时测定氧化锌富集物中锌铁氯镉砷

氧化锌富集物的进口能弥补我国锌矿资源的不足,但要求ZnO>50%、Fe<10%、Cl<8%、Cd<0.25%、As<0.6%。目前常采用YS/T 1171.1～10-2017《再生锌原料化学分析方法》检测氧化锌富集物中锌铁氯镉砷含量,该系列检测方法均需要繁琐的湿法样品前处理,测量过程较为冗长,不能满足氧化锌富集物大量进口时快速通关的需求。故实验建立了采用便携式X射线荧光光谱法(PXRF)同时测定氧化锌富集物中锌铁氯镉砷的方法。采用YS/T 1171.3-2017和YS/T 1171.5-2017方法对氧化锌富集物样品进行定值,然后选取21个含量具有梯度的氧化锌富集物样品作为校准样品,建立起各元素X射线荧光强度值与含量的校准曲线。各曲线相关系数在0.8164～0.9999,方法检出限为0.013%～1.95%,各元素的相对标准偏差(RSD,n=11)均小于0.05%。采用本方法和化学方法分别检测氧化锌富集物样品,各元素的本方法检测值与化学分析方法检测值的相对误差均小于20%。本方法能应用到口岸现场进口氧化锌富集物快速筛查,检测一个样品仅需1分钟测量时间,极大地加快了进口氧化锌富集物通关速度。

Simultaneous Determination of Zn,Fe, Cl, Cd and As in Zinc Oxide Concentrate by portable X-ray fluorescence spectrometry

The import of zinc oxide concentrate can make up for the shortage of zinc ore resources in China, but it requires that ZnO > 50%, Fe < 10%, Cl < 8%, Cd < 0.25%, As < 0.6%. At present, YS / T 1171.1 ~ 10-2017 chemical analysis method of recycled zinc raw materials is often used to detect the content of zinc, iron, chloride, cadmium and arsenic in zinc oxide concentrate. This series of detection methods require complicated wet sample pretreatment, and the measurement process is lengthy, which can not meet the needs of rapid customs clearance when a large number of zinc oxide concentrate is imported. Therefore, a portable X-ray fluorescence spectrometry (pxrf) method was established for the simultaneous determination of zinc, iron, chloride, cadmium and arsenic in zinc oxide concentrate. The YS / T 1171.3-2017 and YS / T 1171.5-2017 methods were used to determine the value of zinc oxide concentrate samples, and then 21 zinc oxide enrichment samples with gradient content were selected as calibration samples to establish the calibration curve of each element X-ray fluorescence intensity value and content. The correlation coefficient of each curve was 0.8164-0.9999, and the detection limit was 0.013% - 1.95%. The relative standard deviation (RSD, n = 11) of each element was less than 0.05%. The relative error between the detection value of this method and that of chemical analysis method is less than 20%. This method can be applied to the rapid screening of imported zinc oxide concentrate at the port. It takes only one minute to detect a sample, which greatly speeds up the customs clearance of imported zinc oxide concentrate.