TiO_2纳米线的生长和热处理及水样中多环芳烃的固相微萃取
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摘要
采用水热法在酸处理的钛丝(Ti)基体上自制备生成了二氧化钛纳米线(TiO_2NWs),接着对其在800℃进行热处理,形成了石纹状的TiO_2涂层,并将其作为固相微萃取(SPME)纤维涂层,与高效液相色谱-紫外检测器(HPLC-UV)联用测定环境水样中的5种多环芳烃(PAHs).与商用聚二甲基硅氧烷(PDMS)纤维相比,所制备的纤维对PAHs具有良好的萃取选择性.对于每种分析物浓度为50μg·L~(-1)的加标水样,检测限为0.013～0.065μg·L~(-1),用单支纤维与HPLC-UV联用方法的日内和日间的相对标准偏差分别低于5.4%和6.2%(n=5).该方法成功应用于环境水样中PAHs的萃取、富集和定量分析,回收率为83.8%～109%,相对标准偏差为4.8%～9.1%.而且,该纤维的制备精密可控,可稳定使用300次.
TiO_2 nanowires(TiO_2NWs) were in-situ grown on the Ti wire by hydrothermal process in alkali solution.Thereafter,the TiO_2NWs coated Ti(Ti@TiO_2NWs) fiber was annealed at 800 ℃,and the rock-like TiO_2 coating was fabricated on the Ti fiber substrate.Coupled to high-performance liquid chromatography with ultraviolet detection,the solid-phase microextraction performance of the rock-like TiO_2 coating was comparatively studied using typical aromatic compounds as model analytes.As compared with the commercial polydimethylsiloxane(PDMS) fiber,the rock-like TiO_2 coated Ti fiber showed high extraction capability and good extraction selectivity for polycyclic aromatic hydrocarbons(PAHs).Under the optimized conditions,the developed method presents linear ranges from 0.05 to 400 μg·L~(-1) with correlation coefficients higher than 0.999 and limits of detection from 0.013 to 0.065 μg·L~(-1).Relative standard deviations(RSDs) were below 5.4% and 6.2% for intra-day and inter-day analyses of PAHs at the spiking level of 50 μg·L~(-1) with the single fiber(n=5),respectively.The developed method was successfully applied to the selective enrichment and determination of target PAHs in environmental water samples with recoveries from 83.8% to 109% and RSDs from 4.8% to 9.1%.Moreover,the fabrication of the rock-like TiO_2 coated Ti fiber precisely controllable and is stable for at least 300 extraction and desorption cycles.
TiO_2 nanowires(TiO_2NWs) were in-situ grown on the Ti wire by hydrothermal process in alkali solution.Thereafter,the TiO_2NWs coated Ti(Ti@TiO_2NWs) fiber was annealed at 800 ℃,and the rock-like TiO_2 coating was fabricated on the Ti fiber substrate.Coupled to high-performance liquid chromatography with ultraviolet detection,the solid-phase microextraction performance of the rock-like TiO_2 coating was comparatively studied using typical aromatic compounds as model analytes.As compared with the commercial polydimethylsiloxane(PDMS) fiber,the rock-like TiO_2 coated Ti fiber showed high extraction capability and good extraction selectivity for polycyclic aromatic hydrocarbons(PAHs).Under the optimized conditions,the developed method presents linear ranges from 0.05 to 400 μg·L~(-1) with correlation coefficients higher than 0.999 and limits of detection from 0.013 to 0.065 μg·L~(-1).Relative standard deviations(RSDs) were below 5.4% and 6.2% for intra-day and inter-day analyses of PAHs at the spiking level of 50 μg·L~(-1) with the single fiber(n=5),respectively.The developed method was successfully applied to the selective enrichment and determination of target PAHs in environmental water samples with recoveries from 83.8% to 109% and RSDs from 4.8% to 9.1%.Moreover,the fabrication of the rock-like TiO_2 coated Ti fiber precisely controllable and is stable for at least 300 extraction and desorption cycles.
引文
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[3] CAO D D,LU J X,LIU J F,et al.In situ fabrication of nanostructured titania coating on the surface of titanium wire:a new approach for preparation of solid-phase microextraction fiber[J].Analytica Chimica Acta,2008,611(1)56.
[4] XU H L,LI Y,JIANG D Q,et al.Hydrofluoric acid etched stainless steel wire for solid-phase microextraction[J].Analytical Chemistry,2009,81(12):4971.
[5] SUN M,FENG J J,QIU H M,et al.CNT-TiO2 coating bonded onto stainless steel wire as a novel solid-phase microextraction fiber[J].Talanta,2013,114:60.
[6] 彭英,庄园,何欢,等.硫酸改性聚(甲基丙烯酸缩水甘油酯-乙二醇二甲基丙烯酸酯)固相微萃取涂层-高效液相色谱检测水中4种药品及个人护理用品[J].分析化学,2014,42(9):1359.
[7] JIA J,LIU S J,QIU H D,et al.Supported nanohydroxyapatite on anodized titanium wire for solid-phase microextraction[J].Analytical and Bioanalytical Chemistry,2014,406(8):2163.
[8] 李晴,黄晓兰,林晓珊,等.选择性吸附地沟油杂质的不锈钢固相微萃取头研究[J].分析化学,2015,43(9):1422.
[9] 杜稼健,张敏,甄琦,等.镍钛合金纤维基体表面纳米多孔复合氧化物的可控生长及其对多环烃的选择性固相微萃取[J].分析化学,2017,45(11):1662.
[10] WANG F X,ZHENG J,QIU J L,et al.In situ hydrothermally grown TiO2@C core-shell nanowire coating for highly sensitive solid phase microextraction of polycyclic aromatic hydrocarbons[J].ACS Applied Materials & Interfaces,2017,9(2):1840.
[11] CHEN X B,SAMUEL S M.Titanium dioxide nanomaterials:synthesis,properties,modifications,and applications[J].Chemistry Review,2007,107(7):2891.
[12] LIU H M,WANG D A,JI L,et al.A novel TiO2 nanotube array/Ti wire incorporated solid-phase microextraction fiber with high strength,efficiency and selectivity[J].Journal of Chromatography A,2010,1217(12):1898.
[13] LI Y,ZHANG M,YANG Y X,et al.Electrochemical in situ fabrication of titanium dioxide-nanosheets on a titanium wire as a novel coating for selective solid-phase microextraction[J].Journal of Chromatography A,2014,1358:60.
[14] SUN Y,SUN S P,LIAO X M,et al.Effect of heat treatment on surface hydrophilicity-retaining ability of titanium dioxide nanotubes[J].Applied Surface Science,2018,440:440.