新型碳分子筛在工业源挥发性有机物测定中的应用  

Application of New Carbon Molecular Sieve in Determination of Volatile Organic Compounds from Industrial Sources

作　　者：齐乔鑫 许守聪 杨黎忠 李玉婷 李琳[1] QI Qiaoxin;XU Shoucong;YANG Lizhong;LI Yuting;LI Lin(Engineering Research Center of Health Food Design&Nutrition Regulation,School of Life and Health Technology,Dongguan University of Technology,Dongguan 523808,China;Labinno Application Technology(Guangzhou)Co.,Ltd.,Guangzhou 511348,China)

机构地区：[1]东莞理工学院生命健康技术学院食品营养健康工程与智能化加工研究中心,东莞523808 [2]莱创应用(广州)科技发展有限公司,广州511348

出　　处：《理化检验（化学分册）》2024年第7期649-659,共11页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：东莞理工学院引进人才科研启动专项经费项目(GC300502-36);东莞理工学院高层次人才(创新团队)科研启动项目(KCYCXPT2017007)。

摘　　要：制备新型碳分子筛Scalpha 1500,并采用Scalpha 1500代替进口碳分子筛Carboxen 1000组合成新的吸附管(CB1500吸附管)。采用扫描电子显微镜(SEM)、X射线能谱法(EDS)、氮气吸附-脱附等温线法和X射线衍射法(XRD)对两种碳分子筛的表观形貌、元素组成、孔隙结构以及晶相构成进行表征。利用热脱附-气相色谱-质谱法(TD-GC-MS),比较CB1500吸附管与HJ 734-2014推荐组合三吸附管(Carbon 300吸附管)对挥发性有机物(VOCs)的测试性能。吸附管的最优解吸参数为解吸温度300℃、解吸时间6 min、解吸流量50 mL·min^(−1),在该条件下,两种吸附管具有相近的本底值、解吸性能及穿透性能。结果表明,CB1500及Carbon 300吸附管中24种VOCs的质量在5~100 ng内与对应的峰面积呈线性关系,检出限(3S/N)分别为0.4~4.8μg·m^(−3)和0.4~4.6μg·m^(−3)。按照标准加入法进行回收试验,CB1500及Carbon 300吸附管中24种VOCs的回收率分别为93.0%~107%和92.0%~113%,除乳酸乙酯外其他23种VOCs测定值的相对标准偏差(n=7)均小于5.0%。采用两种吸附管对广州某工业园区固定污染源废气进行采样分析,CB1500及Carbon 300吸附管中24种VOCs均有检出,检出量分别为2.3~21.1μg·m^(−3)和2.4~21.3μg·m^(−3)。上述结果说明新型碳分子筛Scalpha 1500可代替进口碳分子筛Carboxen 1000组合成新的吸附管采集VOCs,可极大降低采样成本。A new carbon molecular sieve Scalpha 1500 was prepared,and Scalpha 1500 was applied to replace the imported molecular sieve Carboxen 1000 to form a new adsorption tube(CB1500).The apparent morphology,elemental composition,pore structure and crystal phase composition of two carbon molecular sieves were analyzed by scanning electron microscopy(SEM),energy dispersive X-ray spectroscopy(EDS),N_(2)adsorption-desorption isotherms and X-ray diffraction(XRD).The testing performance of CB1500 adsorption tube and HJ 734-2014 recommended combination triple adsorption tube(Carbon 300 adsorption tube)in volatile organic compounds(VOCs)determination was compared by thermal desorption-gas chromatography-mass spectrometry(TD-GC-MS).The optimal desorption parameters for the adsorption tubes were desorption temperature of 300 ℃,desorption time of 6 min,and desorption flow rate of 50 mL·min^(−1).Under these conditions,the two types of adsorption tubes had similar background values,desorption performance,and penetration performance.As shown by the results,linear relationships between values of the corresponding peak area and mass of 24 VOCs in CB1500 and Carbon 300 adsorption tubes were found in the range of 5-100 ng,with detection limits(3S/N)in the range of 0.4-4.8μg·m^(−3)and 0.4-4.6μg·m^(−3),respectively.Test for recovery was made by the standard addition method,giving results in the range of 93.0%-107%for CB1500 adsorption tube and 92.0%-113%for Carbon 300 adsorption tube,with RSDs of the determined values(n=7)of 23 VOCs except for ethyl lactate less than 5.0%.Two types of adsorption tubes were used to sample and analyze the exhaust gas from stationary pollution source of an industrial park in Guangzhou.24 VOCs were detected in CB1500 and Carbon 300 adsorption tubes,with detection amounts of 2.3-21.1μg·m^(−3)and 2.4-21.3μg·m^(−3),respectively.It was shown by the above results that the new carbon molecular sieve Scalpha 1500 could replace the imported carbon molecular sieve Carbon 1000 to form a new adsorpti

关 键 词：热脱附-气相色谱-质谱法(TD-GC-MS) 挥发性有机物 新型碳分子筛 吸附管 

分 类 号：O657.63[理学—分析化学]