一种X荧光分析熔片法脱模剂的改进研究

Improvement of a Molten Release Agent for X-Ray Fluorescence Analysis

熔片法在X荧光分析中比压片法更精准,所得数据能用于财务结算,被大量运用于厂矿,科研院校等。磷矿及磷化工熔片法一直用溴化铵和碘化铵作为脱模剂,但使用这种脱模剂,经常导致自动熔片机导轨和滑轨堵塞,3~5 d就要停机清扫,一个季度传动装置就大修一次;熔片时肉眼可见烟尘,环境污染大,对机器部件腐蚀严重。改用碘化锂做脱模剂,腐蚀情况相应变小,变成一个月清扫吹扫一回,熔片时观察不到明显的烟雾。用正交法找到了碘化锂最佳浓度配比,优化了脱模剂的配比。改进后方法的加标回收率在90.00%~102.50%之间,方法的检出限0.31 mg/kg,具有简单易于推广的特点。

The analysis result of the fused sheet method in the X-ray fluorescence analysis is more accurate than that of the pressed sheet method,and the generated data can be used for financial settlement,which is widely used in factories,mines,scientific research institutions,etc.The fused sheet method of phosphate rock and phosphate chemical industry has always used ammonium bromide and ammonium iodide as the release agent.The use of this release agent has led to the frequent blockage of the guide rail and slide rail of the automatic fused sheet machine.On average,the machine will be shut down for cleaning,purging and oiling in 3-5 days,and the transmission device will be overhauled once a quarter.Smoke and dust are visible to the naked eye during the melting process,which causes great environmental pollution and serious corrosion to machine parts.After inquiry and data review,lithium iodide is used as the release agent in the experiment,and the corrosion condition is correspondingly reduced,turning into a monthly cleaning and purging,and no obvious smoke can be observed during the melting process.The optimal concentration ratio of lithium iodide was found by orthogonal method,and the ratio of mold release agent was improved.The recovery rate of standard addition of the improved method was between 90.00%and 102.50%.The detection limit of the method was 0.31 mg/kg,and the method was simple and easy to popularize.