有序纳米孔碳(CMK-3)涂层纤维固相微萃取水样中苯和氯苯

M. Anbia, Naser kakoli khataei, S. Salehi
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引用次数: 2

摘要

制备了纳米多孔碳(CMK-3),并将其用作顶空固相微萃取(HS-SPME)的纤维涂层。采用扫描电镜(SEM)、x射线衍射(XRD)和N2吸附/脱附等温线对制备的材料进行了表征。利用气相色谱(GC)系统从水样品的顶空气中提取苯(B)和氯苯(CBs),评价了纤维的效率。将制备的纳米材料涂覆在铜线上制备SPME纤维。这些纤维具有制备简单、快速、热稳定性和机械稳定性高的优点。采用田口OA16(45)正交实验设计,对影响提取效率的样品体积、提取温度、提取时间、离子强度和搅拌速率等参数进行优化。根据方差分析(ANOVA)得到的结果,确定最佳提取条件为:进样量12 mL;实验室温度;20% (w/v) NaCl;提取时间35 min,搅拌速度600 rpm。在优化条件下,B和CBs的线性范围为2.5 ~ 800µg/L,相对标准偏差(RSD %)为5.2 ~ 9.3%,检出限(lod)为0.09 ~ 0.28µg/L。在水样中回收率为85.40% ~ 104.20%。最后,通过对水样中B和CBs的提取和测定,对该方法的适用性进行了评价。
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Ordered nanoporous carbon (CMK-3) coated fiber for solid-phase microextraction of benzene and chlorobenzenes in water samples
Nanoporous carbons (CMK-3) were prepared and have been used as a fiber coating for headspace solid phase microextraction (HS-SPME). The prepared materials were characterized by Scanning Electron Microscopy (SEM), X-Ray Diffraction (XRD) and N2 adsorption/desorption isotherms. The efficiency of the fiber was evaluated using a gas chromatography (GC) system for the extraction of benzene (B) and chlorobenzenes (CBs) from the headspace of aqueous samples. The prepared nanomaterial was coated onto a copper wire for fabrication of the SPME fiber. These fibers featured advantages like easy and fast preparation, high thermal and mechanical stability. To optimize different parameters which influence the extraction efficiency such as sample volume, extraction temperature, extraction time, ionic strength and stirring rate, a Taguchi OA16 (45) orthogonal array experimental design was used. Based on the results obtained from the analysis of variance (ANOVA), the optimum conditions for extraction were established as: 12 mL sample volume; laboratory temperature; 20 % (w/v) NaCl; 35 min extraction time and stirring rate of 600 rpm. Under the optimized conditions for B and CBs, the linearity was from 2.5 to 800 µg/L, the relative standard deviation (RSD %) of the method was between 5.2 and 9.3% and limit of detections (LODs) was between 0.09 and 0.28 µg/L. The recovery values were from 85.40% to 104.20 % in water samples. Finally, the applicability of the proposed method was evaluated by the extraction and determination of B and CBs in the water samples.
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