应用衍生气相色谱法测定含氟稀土精矿焙烧逸出气体中的氟化物。焙烧逸出气体经过NaOH溶液吸收,三甲基氯硅烷衍生气化,生成气态氟硅烷(TMFS),在气相色谱仪中利用氢火焰离子化检测器(FID)检测,以峰高外标法测定其氟含量。实验表明,在500μg/mL范围内,FID检测器的响应值与TMFS的浓度成正比,其相关系数r=0.99941;且在合理选择吸收气体流量的前提下,测量的相对标准偏差(RSD)为1.43%,加标回收率在96.9%~103.3%之间,其RSD为2.75%,具有较高的精密度和准确度。此法也可用于稀土矿物中含氟率的测定。
Derivative gas chromatography is used to analyze the fluorinated compound derived from the gas out of the rare earth concentrates containing fluorine. After absorbed by the NaOH solution, the trimethylchlorosilane is added into gas and the TMFS being generated. Then, used FID detector to analyze it in gas ctu'omatography and analyze the content of fluorine. The experiments show that in the category of 0.5g/L, the response value of FID detector is direedy proportional to the concentration of TMFS, and the relative rate r= 0.99941. Furthermore, under the state that the absorbing gas is in a proper flowrate, the relative standard deviation (RSD) is 1.43% ; the indexed recovery ratio is between 96.9% and 103.3%, with RSD at a rate of 2.75%, which has a relatively high degree of precision and accuracy. This method can also be used to measure the fluorine containing rate in rare earth ore.