本文以六甲基二硅胺烷(HMDSA)为衍生化试剂，建立了 HMDSA-GC测氟的新方法。在15%01-3色谱柱上，衍生产物三甲基氟硅烷(TMFS) 得到很好的分离(Te=120℃，N230ml/min)采用Youden实验设计找出了影响能测氟灵敏度与准确复的因素，对此作了进一步的研完并对HMDSA-GC法测氟的实验条件作了详尽的探查与讨论。方法的 枝幺限量为 5ng/g;线性工作范围为QO5-25Mg/g;对At.S;等九种元素的干扰试验证明这些元素并不影响氟的准确检出。应用该法测定了牙膏、茶叶及人发挥品中的氟，结果令人满意。本文还将 HMDSA法与 TMCS 法和F-ISE法作，较为详细的比较，并在氟离子选择电极测氟难确度方面进行了一些探讨。

In this article,a new method for determination of fluoride with hexamethyldisilazane-gas-chromatograph has been researched detaily.Thrimethylfluorosilane produced from hexamethyldisilazane and hydrofluoride in acid condition was separated on l5% 0V-3 column at l20*c with N2 as carrier gas(30ml/min)and FID.The sensitive factors were picked out by using Youden's ruggedness test,and experimental conditions were optimized by detailed experiments.The detection limit was 5 ng/g(2.6Xl0~7M),linear range from 0.05 to 25 mg/g and aluminum ion,silicate ion etc.did not interfere the determination.Compared with trimethylsilane-gas- chromatograph method and fluoride ion-selective-electrode method,this new method expressed higher sensitivity. The precision and accuracy of fluoride ion-selective- electrode method have been investigated and contents of fluoride in anti-dental caries toothpastes,tea and human hair were reported.