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Ordered nanoporous carbon (CMK-3) coated fiber for solid-phase microextraction of benzene and chlorobenzenes in water samples

机译:有序纳米孔碳(CMK-3)涂层纤维用于固相微萃取水样品中的苯和氯苯

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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.
机译: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。制备的材料通过扫描电子显微镜(SEM),X射线衍射(XRD)和N 2吸附/解吸等温线表征。使用气相色谱(GC)系统评估了纤维的效率,该系统用于从水性样品的顶部空间提取苯(B)和氯苯(CBs)。将制备的纳米材料涂覆到铜线上以制造SPME纤维。这些纤维具有易于制备,快速,高热稳定性和机械稳定性等优点。为了优化影响萃取效率的不同参数,例如样品量,萃取温度,萃取时间,离子强度和搅拌速度,使用了Taguchi OA16(45)正交阵列实验设计。根据方差分析(ANOVA)获得的结果,确定最佳提取条件为:12 mL样品量;实验室温度20%(w / v)氯化钠; 35分钟的提取时间和600 rpm的搅拌速度。在B和CB的最佳条件下,线性范围为2.5至800μg/ L,方法的相对标准偏差(RSD%)在5.2至9.3%之间,检出限(LOD)在0.09至0.28μg之间/升水样品中的回收率从85.40%到104.20%。最后,通过水样中B和CB的提取和测定,评价了该方法的适用性。

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