Zhang Guijiang, Li Zhi, Zang Xiaohuan, Wang Chun, Wang Zhi
Department of Chemistry, College of Science, Agricultural University of Hebei, Baoding, China.
J Sep Sci. 2014 Feb;37(4):440-6. doi: 10.1002/jssc.201301183. Epub 2014 Jan 6.
In this work, a graphene composite was coated onto etched stainless-steel wire through a sol-gel technique and it was used as a solid-phase microextraction (SPME) fiber. The prepared fiber was characterized by SEM, which revealed that the fiber had a highly porous structure. The application of the fiber was evaluated through the headspace SPME of five halogenated aromatic hydrocarbons (chlorobenzene, bromobenzene, 1,3-dichlorobenzene, 1,2-dichlorobenzene, and 1,2,4-trichlorobenzene) in water samples followed by GC with flame ionization detection. The main factors influencing the extraction efficiency, including headspace volume, extraction time, extraction temperature, stirring rate, ionic strength of sample solution, and desorption conditions, were studied and optimized. Under the optimum conditions, the linearity of the method ranged from 2.5 to 800.0 μg/L for 1,2,4-trichlorobenzene and from 2.5 to 500.0 μg/L for chlorobenzene, bromobenzene, 1,3-dichlorobenzene, and 1,2-dichlorobenzene, with the correlation coefficients (r) ranging from 0.9962 to 0.9980, respectively. The LODs (S/N = 3) of the method for the analytes were in the range between 0.5 and 1.0 μg/L. The recoveries of the method for the analytes obtained for the spiked water samples at 50.0 and 250.0 μg/L were from 76.0 to 104.0%.
在本研究中，通过溶胶 - 凝胶技术将石墨烯复合材料涂覆在蚀刻不锈钢丝上，并将其用作固相微萃取（SPME）纤维。通过扫描电子显微镜（SEM）对制备的纤维进行表征，结果表明该纤维具有高度多孔的结构。通过对水样中五种卤代芳烃（氯苯、溴苯、1,3 - 二氯苯、1,2 - 二氯苯和1,2,4 - 三氯苯）进行顶空固相微萃取，随后采用带有火焰离子化检测的气相色谱法对该纤维的应用进行评估。研究并优化了影响萃取效率的主要因素，包括顶空体积、萃取时间、萃取温度、搅拌速率、样品溶液的离子强度和解吸条件。在最佳条件下，该方法对于1,2,4 - 三氯苯的线性范围为2.5至800.0μg/L，对于氯苯、溴苯、1,3 - 二氯苯和1,2 - 二氯苯的线性范围为2.5至500.0μg/L，相关系数（r）分别在0.9962至0.9980之间。该方法对分析物的检测限（S/N = 3）在0.5至1.0μg/L范围内。对于加标浓度为50.0和250.0μg/L的水样，该方法对分析物的回收率为76.0%至104.0%。
