液态危废中总氟、总氯、总溴及总硫含量的测定

Determination of Total Fluorine, Total Chlorine, Total Bromine and Total Sulfur in Liquid Hazardous Waste

建立了液态危废中总氟、总氯、总溴及总硫含量的氧弹燃烧-离子色谱法快速测定的方法。液态危废种类多且成分复杂,采用充有高压氧气的氧弹可将其灼烧完全并且防止了目标物的挥发,灼烧后产生的挥发物在密闭体系中被一定比例的碳酸钠、碳酸氢钠及双氧水的混合吸收液充分吸收,转化为氟化物、氯化物、溴化物及硫酸盐,此吸收液进离子色谱仪可以同时将氟离子、氯离子、溴离子及硫酸根快速测出,通过计算可得到总氟、总氯、总溴及总硫的含量。实验表明,方法中总氟、总氯、总溴及总硫的线性相关系数均高于0.999;方法的检出限分别为27.30、25.14、3.70、10.11 mg/kg;样品加标回收率均在93.64%~105.45%之间;RSD均在1.7%~3.1%之间。方法操作简单、准确性高、精密度好,实现了液态危废中总氟、总氯、总溴及总硫含量的同步快速测定。

A rapid determination method of total fluorine, total chlorine, total bromine, and total sulfur in liquid hazardous waste was established by using oxygen bomb combustion and ion chromatography techniques.The liquid hazardous waste in high pressure oxygen during oxygen bomb combustion could by completely burnt and the volatilization of the targets could be prevented.The volatiles produced after burning were fully absorbed by a certain proportion of sodium carbonate, sodium bicarbonate, and hydrogen peroxide in a sealed system and converted into fluoride, chloride, bromine, and sulfur.The content of total fluorine, total chlorine, total bromine, and total sulfur could be obtained by calculations.The results showed that the linear correlation coefficients were all higher than 0.999;the detection limits of the method for total fluorine, total chlorine, total bromine, total sulfur were 27.30,25.14,3.70,and 10.11 mg/kg;the recoveries of the method at different concentrations were all between 93.64% and 105.45%;the relative standard deviation(RSD) were all between 1.7% and 3.1%.The method was simple, accurate, and precise, it can realize simultaneous and rapid determination of total fluoride, total chlorine, total bromine and total sulfur in liquid hazardous wastes.