Farhadi Khalil, Tahmasebi Raheleh, Maleki Ramin
Department of Chemistry, Faculty of Science, Urmia University, Urmia, Iran.
Talanta. 2009 Feb 15;77(4):1285-9. doi: 10.1016/j.talanta.2008.09.009. Epub 2008 Sep 13.
A novel titania sol-gel coating, including tetrabutyl orthototitanat (TBOT) as initial alkoxide, triethanolamine (TEA) as stabilizer, nitric acid as acid catalyst, and polyethylene glycol (PEG, 6000) as binder was prepared for the first time on an anodized aluminium wire and subsequently applied to headspace solid phase microextraction (HS-SPME) of benzene, toluene, ethylbenzene and xylenes (BTEX) with gas chromatography flame ionization detection (GC-FID). The analytical characteristics of the proposed porous titania sol-gel derived TBOT/PEG/TEA (41.6:16.0:42.4) fiber were comparable with reported fibers. The extraction temperature, extraction time, effect of salt addition, desorption temperature and desorption time were optimized. Under the optimized conditions and for all BTEX components, the linearity was from 20 to 800 microg L(-1), the RSD was below 8.2% and limit of detections (LODs) were between 5.4 and 14.8 microg L(-1). The recovery values were from 86.7% to 94.2% in water samples. The proposed HS-SPME-GC-FID method was successfully applied for the analysis of BTEX compounds from petrochemical wastewater samples.
首次在阳极氧化铝丝上制备了一种新型二氧化钛溶胶 - 凝胶涂层，该涂层以原钛酸四丁酯（TBOT）为起始醇盐，三乙醇胺（TEA）为稳定剂，硝酸为酸催化剂，聚乙二醇（PEG，6000）为粘结剂，随后将其应用于苯、甲苯、乙苯和二甲苯（BTEX）的顶空固相微萃取（HS - SPME），并采用气相色谱火焰离子化检测（GC - FID）。所提出的由多孔二氧化钛溶胶 - 凝胶衍生的TBOT/PEG/TEA（41.6:16.0:42.4）纤维的分析特性与已报道的纤维相当。对萃取温度、萃取时间、加盐效果、解吸温度和解吸时间进行了优化。在优化条件下，对于所有BTEX组分，线性范围为20至800 μg L⁻¹，相对标准偏差低于8.2%，检测限（LOD）在5.4至14.8 μg L⁻¹之间。水样中的回收率为86.7%至94.2%。所提出的HS - SPME - GC - FID方法成功应用于石化废水样品中BTEX化合物的分析。
