基于氧弹燃烧-气体吸收-离子色谱法测定危险废物可燃组分中氟、氯和硫的含量

Determination of F,Cl and S in hazard waste by oxygen bomb combustion-gas absorption and ion chromatography

建立基于氧弹燃烧-气体吸收-离子色谱法测定危险废物中氟、氯、硫含量的分析方法。采用氧弹燃烧法对危险废物进行预处理,采用碳酸钠、碳酸氢钠和过氧化氢作为吸收液,目标物转化为氟化物、氯化物和硫酸盐,并用离子色谱法对吸收液中氟离子、氯离子和硫酸根含量进行测定,通过计算可得到氟、氯和硫的含量。结果表明,该方法定量检测限为13.5~32.7 mg/kg,在0.1~5 mg/L(氟化物)、1~50 mg/L(氯化物、硫酸根)线性范围良好,相关系数大于0.999,精密度为2.2%~3.5%。样品加标回收率在93.6%~102.4%,并用控制混合物质控样品对方法进行了验证,该方法快速、准确、回收率高,重复性好,适合危险废物样品可燃组分中氟、氯和硫含量的测定。

An oxygen bomb combustion-gas absorption analytical method for determination of fluorine,chlorine and sulfur in hazardous waste by ion chromatography was established.The hazard waste samples was pretreated by oxygen bomb combustion method,and Na_(2)CO_(3),NaHCO_(3) and H_(2)O_(2) were used as absorbents(the targets converted into fluoride,chloride and sulfate),the contents of fluoride,chloride and sulfate in the absorbent solution were determined by ion chromatography.The content of fluorine,chlorine and sulfur in the sample could be obtained by calculations.The results showed that the detection limits of the method were within 13.5~32.7 mg/kg.The linear range of fluoride,chloride and sulfate were 0.1~5 mg/L,1~50 mg/L with favorable linear relationship,and the correlative coefficients were greater than 0.999.The relative standard deivations were in the range of 2.2%~3.5%.The recoveries in the sample were between 93.6%~102.4%.This method was also verified by the control mixtures quality control samples.It was a rapid and accurate method with high recovery and good repeatability,suitable for the determination of fluorine,chlorine and sulfur elements content in hazard waste sample.