氟硅酸回收法无水氟化氢磷含量测定方法研究

Study on determination method of phosphorus content of anhydrous hydrogen fluoride prepared by recycling fluosilicic acid

采用氟硅酸回收法制取的无水氟化氢是一种资源回收利用产品,在相关国家标准没有发布前尚无检测标准可以执行。本项目制定了该产品国家推荐性标准,对其中测定磷含量的方法做了研究,并建立方法。主要研究了样品前处理、最佳检测波长、磷标准曲线的浓度范围、精密度、加标回收、检出限等方面,建立了氟硅酸回收法无水氟化氢中磷含量的检测方法。通过加标回收、重复性实验等方式验证了该方法的可靠性。结果表明,该方法检出限低(0.005 mg/L)、精密度高(1.41%)、加标回收率好(95.0%~102.5%),完全适用于氟硅酸回收法无水氟化氢中磷含量的测定。

Anhydrous hydrogen fluoride prepared by recycling fluosilicic acid is a kind of resource recycling process in the production of products,the relevant standards for products that were not produced before the release of the national standard are not available.This project has developed the national recommence standard of the product,studied the method of determination of phosphorus content,and established the method.The sample pretreatment,the best detection wavelength,phosphorus concentration range of standard curve,precision and standard addition recovery,detection limit and so on,were mainly studied.The determination method of phosphorus content of anhydrous hydrogen fluoride prepared by recycling fluosilicic acid was established.The reliability of the method was verified by means of standard recovery and repeatability experiment.Results showed that the methods detection limit was completely low（0.005 mg/L）,precision was high（1.41%） and the high standard addition recovery rate was good（95.0%～102.5%）.The method was suitable for the determination of phosphorus content in anhydrous hydrogen fluoride by recycling fluosilicic acid.