高温燃烧水解氟电极法测定骨氟化物水平实验条件的研究

Study on experimental conditions for the method of high temperature combustion and fluoride electrode hydrolysis in determining fluoride contents in bone

目的建立一种较为准确、实用的测定骨等生物样品中氟化物水平的测定方法。方法采用高温燃烧水解-氟电极法,使用拉丁方设计,以回收率作为选择实验条件的指标,对骨等生物样品的氟化物水平测定方法进行了温度、时间、消化液收集量3个处理因素和4个水平的实验研究。结果选择出温度为1100℃,时间为30 min,消化液收集量为75 ml的最佳测定条件,同时还推出了一种新的助燃剂-金刚砂(Sic),对缓冲液常规使用方法也进行了改进。结论高温燃烧水解-氟电极法具有良好的准确度和精密度,回收率为97．6％- 101．7％,变异系数均为2．0％以下,且简单易行。

Objective To establish a simple and suitable method for determining the contents of fluoride in bone and other samples. Methods The samples were eombusted under high temperature and hydrolyzed with fluoride electrode and then the fluoride contents were determined in 4 parallel tests under different treatment of time, temperature and the collected volume of digestive liquid, adopting Latin square design and the rate of recovery as the index of the research. Results 1 100 ℃ of temperature, 30 min of reacting time and collecting 75 ml of digestive liquid were the best conditions for determining fluoride content. At the same time, a new combustionaiding agent-Sin was put out, and the regular way of using buffer was improved. Conclusions The method described above is simple and suitable with better accuracy and precision. In this research, the rate of recovery is from 97.6% to 101.7%, and the coefficient variation is under 2.0%.