吹扫捕集/气相色谱-质谱法测定石油炼制工艺废催化剂浸出液中挥发性有机物

Determination of volatile organic compounds in waste catalyst leaching liquor in petroleum refining process using P&T-GC-MS method

采用吹扫捕集/气相色谱-质谱法,建立了石油炼制工艺废催化剂浸出液中挥发性有机物(VOCs)的检测方法.该方法标准曲线线性范围为5—200μg L^(−1),线性相关系数R2>0.99,方法检出限为0.1—2.0μg L^(−1).催化裂化(FCC)废催化剂浸出液、吸附脱硫(S Zorb)废催化剂浸出液和渣油加氢废催化剂浸出液的测定结果显示各组分的相对标准偏差(RSD)分别为0.2%—0.6%、0.7%—3.9%和0.9%—4.3%,基体加标回收率分别为78.7%—161.0%、64.9%—145.6%和74.0%—167.6%.所建立的方法可以满足废催化剂浸出液中VOCs的检测要求.FCC废催化剂浸出液中大部分VOCs的含量低于检出限.S Zorb废催化剂浸出液、渣油加氢废催化剂浸出液检出的化合物分别以C_(9)—C_(11)芳烃和C_(10)—C_(12)芳烃为主.所选取的3种废催化剂浸出液中目标VOCs含量均低于GB5085.3—2007中浸出毒性鉴别限值.

A method was established for the determination of volatile organic compounds(VOCs)in waste catalyst leaching liquor in petroleum refining process by gas chromatography-mass spectrometry(GC-MS)with purge and trap(P&T)pretreatment.The linear ranges were 5—200μg L^(−1) and linear correlation coefficients were more than 0.99.The detection limits were 0.1—2.0μg L^(−1).3 kinds of waste catalysts from the semi synthetic fluid catalytic cracking(FCC),S Zorb and residue hydrotreating refinery process were investigated for leaching experiment.The recoveries of leaching liquors were 78.7%—161.0%,64.9%—145.6%and 74.0%—167.6%with RSD of 0.2%—0.6%,0.7%—3.9%and 0.9%—4.3%respectively.This method was suitable for the analysis of VOCs in waste catalyst leaching liquor.The concentration of most VOCs were below the detection limits in waste catalyst leaching liquor from FCC.C_(9)-C_(11) aromatic hydrocarbons and C_(10)-C_(12) aromatic hydrocarbons were the main compounds detected in waste catalyst leaching liquors from S Zorb and residue hydrotreating respectively.The contents of target VOCs in the leaching solution of the three waste catalysts selected were all lower than the limiting values for the identification of leaching toxicity in GB5085.3—2007.