董云渊,王滢,史君齐,岳跃振,骆华英,郑启富,张敏,廖建明,陈晓彬.磁性固相萃取结合气质联用仪检测造纸废水中的氯酚类化合物[J].中国造纸学报,2023,38(4):41-47 |
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磁性固相萃取结合气质联用仪检测造纸废水中的氯酚类化合物 |
Magnetic Solid-phase Extraction Combined with GC-MS for Chlorophenols Analysis in Papermaking Wastewater |
投稿时间:2022-09-07 |
DOI:10.11981/j.issn.1000-6842.2023.04.41 |
中文关键词: 磁性聚苯乙烯微球 气质联用 造纸废水 氯酚 |
Key Words:Fe3O4@PS GC-MS papermaking wastewater chlorophenols |
基金项目:衢州市科技计划项目(2023K230、2018K38);浙江省基础公益计划项目(LGN21C030001);浙江大学衢州研究院科技计划项目(IZQ2019-KJ-028);衢州市重点研发计划项目(2021Z01);衢江区科技计划项目(QJ2019J001、QJ2020012、QJ2020022、QJ2021038,QJ2021040)。 |
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中文摘要: |
以聚苯乙烯包覆的四氧化三铁微球(Fe3O4@PS)作为磁性固相萃取(MSPE)的吸附剂,结合气质联用仪(GC-MS)测定造纸废水中的氯酚类(CPs)化合物。通过透射电子显微镜(TEM)、X射线衍射仪(XRD)和傅里叶变换红外光谱仪(FT-IR)对吸附剂材料进行表征分析。优化了MSPE过程中材料用量、超声萃取时间和洗脱条件等影响因素。结果显示,20 mg吸附剂材料、超声萃取7 min、2 mL乙醇作为洗脱溶剂是最佳的MSPE条件。在最优条件下进行方法学评价和实际水样加标试验,结果显示,在2.5~2000 μg/L的浓度范围内线性关系较好,检出限在0.076~0.207 μg/L之间,相关系数介于0.9966~0.9994之间。实际水样加标结果显示两种氯酚物质的加标回收率介于83.39%~109.40%之间。实验结果表明,以Fe3O4@PS作为MSPE吸附剂,可以较大程度提高CPs化合物的萃取效率并简化操作流程。 |
Abstract: |
In this study, magnetic polystyrene (Fe3O4@PS) microspheres were used as adsorbents in solid phase extraction combined with GC-MS to evaluate the efficiency of extracting chlorophenols (CPs) from papermaking wastewater. The novel microspheres were characterized by transmission electron microscope (TEM), X-ray diffraction (XRD) and fourier-transform infrared spectroscopy (FT-IR). The main influence parameters of the magnetic solid-phase extraction (MSPE), such as the amount of sorbent, extraction time and elution condition, were investigated and optimized. The results demonstrated that 20 mg of sorbent, 7 min of desorption time and 2 mL of eluent solvent were chosen as the optimum conditions. Under the optimum conditions, an excellent linearity was observed in the range of 2.5~2000 μg/L. The LODs for chlorophenols were in the range of 0.076~0.207 μg/L and the correlation coefficients ranging from 0.9966~0.9994. The proposed method was successfully applied for the analysis of papermaking wastewater samples with recoveries ranging from 83.39%~109.40%. The above results demonstrated that Fe3O4@PS as a MSPE absorbent performed effective extraction efficiency and simplified operation process in the trace analysis of CPs. |
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