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INTERNATIONAL JOURNAL OF ENVIRONMENTAL ANALYTICAL CHEMISTRY · 2018 · IF 1.372

Dispersive solid-phase extraction based on mesoporous melamine-formaldehyde polymer for sensitive determination of five chlorinated herbicides residues in water by high-performance liquid chromatography

Yanfang Zhao,Lubin Xu

In this work, a low-cost melamine-formaldehyde polymer with large-surface-area mesoporous structure was prepared and applied as an efficient solid sorbent for pre-concentration of five kinds of chlorinated herbicides including fomesafen, atrazine, pyrithiobac-sodium, benazolin and acifluorfene from water samples. Extraction parameters such as pH of the sample solution, amount of mesoporous melamine-formaldehyde polymer (mMFP), extraction time, type of desorption solv-ent and volume of the sample were systematically investigated. Combining dispersive solid-phase extraction with high-performance liquid chromatography (HPLC), the detection limits (S/N = 3) of the five herbicides were ranged from 0.04 to 0.18 μg L−1 with good linearity (R2 ≥ 0.9908). Then the tap water and river water samples were analysed by the developed method, and the obtained results indicated that this method provides acceptable recoveries and precisions. mMFP can be prepared through one-pot catalyst-free polymerisation from low-cost starting materials, so that they could be easily scaled up for the sample pre-treatment and have the powerful potentiality in purification of contaminated water.

研究领域: 环境科学 · 分析化学 · 水处理
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MICROCHEMICAL JOURNAL · 2019 · IF 3.206

Accelerated solvent extraction combined with GC–MS: A convenient technique for the determination and compound-specific stable isotope analysis of phthalates in mine tailings

Ning Min,Jun Yao,Meseret Amde,Langping Wu,Geoffrey Sunahara,Hao Li,Yafei Chen,Jiakang Liu,Viktor G. Mihucz

A reliable, simple and fast method was developed to detect four phthalic acid esters (PAEs) including dimethyl phthalate (DMP), diethyl phthalate (DEP), dibutyl phthalate (DBP) and diethylhexyl phthalate (DEHP) in mine tailings based on the accelerated solvent extraction (ASE) combined with gas chromatography-mass spectrometry (ASE/GC–MS). Evaluation of extraction parameters including choice of extraction solvent, temperature, extraction time, and number of extraction cycles showed that dichloromethane, 120 °C, 3 min, and 2 cycles were optimal, respectively. Under these conditions, the limit of detection (LOD) and limit of quantitation (LOQ) values were in the range of 1.2–2.0 µg kg –1 and 3.0–4.6 µg kg –1 , respectively, and precision of the analytical data, RSD ≤ 7.0% were determined. This method was used to analyze the PAEs-spiked mine tailing samples (100 µg kg –1 of each analyte). Acceptable recovery values of 71.3–77.1%, 100–110%, 105–116%, and 101–115% were obtained for DMP, DEP, DBP and DEHP, respectively. The technique was also successfully applied for the extraction of the PAEs in real samples collected from mine tailing pond. Finally, stable C and H isotope analyses were conducted using GC coupled to isotope ratio MS to investigate effect of the ASE method on H and C isotopic compositions of the target analytes. Results showed that the ASE procedure did not lead to significant isotope fractionation of the compounds. Overall, the major advantages of this method are: automated operation, high sensitivity, short extraction time, less solvent consumption, and compatibility with a variety of detecting equipment. Combined with CSIA, it could be used to study the degradation mechanisms of target PAEs in mine tailing environments.

研究领域: 环境科学 · 分析化学 · 同位素地球化学
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JOURNAL OF SEPARATION SCIENCE · 2014 · IF 2.594

Preparation of monolithic fibers for the solid-phase microextraction of chlorophenols in water samples

Xiaojia Huang,Yong Zhang,Meng Mei,Dongxing Yuan

Monolithic fibers were synthesized and applied for the solid-phase microextraction and determination of chlorophenols in environmental water samples by coupling with HPLC. The fibers were prepared by copolymerization of vinylimidazole and ethylene dimethacrylate as functional monomer and cross-linker, respectively. The effect of the preparation conditions of monolithic fibers on the extraction efficiencies was investigated in detail. Several characteristic techniques, such as elemental analysis, infrared spectroscopy, mercury-intrusion porosimetry, and SEM were used to characterize the monolithic material. The effect of the extraction parameters, including desorption solvent, extraction and desorption time, pH values, and ionic strength in sample matrix on the extraction performance was investigated thoroughly. Under the improved extraction conditions, the linear ranges of 2-chlorophenol, 2,4-dichlorophenol and pentachlorophenol were 1.0–200 μg/L and 2.0–200 μg/L for 2,4,6-trichlorophenol. The detection limits (S/N = 3) were in the range of 0.16–0.45 μg/L, the RSDs for intraday and interday precisions were <7.0%. Finally, the proposed method was successfully used to detect different environmental water samples. The recoveries of spiked water samples were ranged from 90.0 to 115%. At the same time, satisfactory repeatability was achieved with RSDs < 9.0%.

CAS / MDL: 95-57-8 120-83-2 88-06-2
研究领域: 分析化学 · 环境科学 · 材料科学
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SEPARATION AND PURIFICATION TECHNOLOGY · 2021 · IF 7.312

Microemulsion system constructed with a new cyano-functionalized ionic liquid for the extraction of Pd(II) and preparation of palladium nanoparticles

Min Shao,Muhan Chen,Mei Fan,Guoting Luo,Ci Jin,Zhangjie Huang

In this study, based on a cyano-functionalized ionic liquid, 1-nitrile-1-octylpyrrole bromide ([C 8 Y 3 Pr]Br), a [C 8 Y 3 Pr]Br/cyclohexane/tributyl phosphate (TBP)/NaCl microemulsion system was constructed and used for the extraction of Pd(II) and preparation of Pd nanoparticles from multimetal solutions. The key extraction parameters including vibration time, [C 8 Y 3 Pr]Br concentration, phase ratio ( R W/O ), and HCl concentration were evaluated. Compared with other ionic-liquid microemulsion systems, the cyano-functionalized ionic liquid [C 8 Y 3 Pr]Br microemulsion system showed excellent extraction performance for Pd(II). Almost all Pd(II) was extracted (>98.0%) from a multimetal solution using the microemulsion system, while the separation factors ( β Pd/M ) of [C 8 Y 3 Pr]Br-based microemulsions for Pd(II) with Cu 2+ , Fe 3+ , Ni 2+ , Zn 2+ , Co 2+ , and Mg 2+ exceeded 1.0 × 10 3 . The mechanism extracting Pd(II) using [C 8 Y 3 Pr]Br was confirmed to be an anion-exchange reaction via Job’s method, spectral analysis (UV, FTIR), and DFT calculations. Alcohols and hydrazine hydrate were used as demulsifiers, and Pd nanoparticles were directly obtained from the microemulsion phase. The Pd nanoparticles were identified by TEM, XPS, and XRD analyses. The chemical structures of extracted species based on the microemulsion system and the mechanism of demulsification of alcohols were studied. Thus, an effective new process was developed in this study for the direct preparation of Pd nanoparticles from mixed metal solutions via solvent extraction.

CAS / MDL: 126-73-8
研究领域: 化学 · 材料科学 · 纳米技术 · 分析化学
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