JOURNAL OF CHROMATOGRAPHY A
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2021
·
IF 4.759
Yuanyuan Fu,Zhentao Li,Qiaoyan Li,Changjun Hu,Yikun Liu,Wenqi Sun,Zilin Chen
Covalent organic frameworks (COFs), considered as a series of newly emerging porous organic materials, have been widely utilized in separation fields. Herein, a novel COF (TFPB-BD) was first employed as stationary phase for high-efficiency capillary electrochromatographic separation. Benzidine (BD) and 1,3,5-Tris-(4-formylphenyl)benzene (TFPB) were selected as organic linkers and then introduced into the aldehyde group modified capillary for the in situ growth of TFPB-BD onto the capillary inner wall at room temperature. The morphology and formation of TFPB coated capillary column were confirmed by a variety of tools including Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM) and energy dispersive X-ray spectrometry (EDS). It's interesting that the TFPB globular crystals with nanoscale were uniformly and densely modified on the capillary inner surface. Hence, the prepared column exhibited prominent separation performance for the test analytes including alkylbenzenes, chlorobenzenes and phenolic compounds with high efficiency and high resolution. The maximum column efficiency can reach about 1.8 × 10 5 plates•m −1 . Additionally, the high resolutions of anilines, amino acids and parabens were also achieved on the TFPB modified capillary. The precisions (RSDs) of the retention times of alkylbenzenes of intra-day runs ( n = 3), inter-day runs ( n = 3) and parallel columns ( n = 3) were all less than 2.83%. This innovative COF-based stationary phase gives great promise for the chromatographic separation field.
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JOURNAL OF CHROMATOGRAPHY A
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2021
·
IF 4.759
Changjun Hu,Zhenkun Mao,Zhentao Li,Qiaoyan Li,Zilin Chen
Hydrophilic column combined with mobile phase containing high content of water is a green method for the separation of polar compounds, but there are few related studies, and the separation efficiency and performance of existing columns still needs to be improved. In this work, a novel monolithic column for separation of hydrophilic compounds under both high water content and HILIC condition, was prepared by in-situ polymerization using 4-vinylbenzoic acid (VBA) and 1-(Acryloyloxy)-3-(methacryloyloxy)-2-propanol (AMAP) as functional monomers. The poly(VBA- co -AMAP) monolithic column showed good separation performance towards various polar compounds under different chromatographic conditions based on the π-interaction, hydrophobic and hydrogen bonding interactions provided by 4-vinylbenzoic acid functional monomer. The highest column efficiency for adenine was over 2.15 × 10 5 plates m −1 (theoretical plate, N). In addition, the monolith showed good stability and reproducibility, the relative standard deviations (RSDs) of retention times within days (n = 5), between days (n = 5), between columns (n = 3) and between batches (n = 3) were 0.47-1.13%, 1.20-2.68%, 0.59-1.78% and 1.54-3.60%, respectively. This novel type of monolith has great application potential in the separation of hydrophilic compounds.
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JOURNAL OF CHEMICAL AND ENGINEERING DATA
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2021
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IF 2.694
Xiaohui Qiao,Xue Sun,Hansen Yang,Hualiang An,Fang Li,Wei Xue,Yanji Wang
In this work, choline chloride/urea (1:2), choline chloride/oxalic acid (1:1), choline chloride/ethylene glycol (1:2), benzyltriphenylphosphonium chloride/ethylene glycol (1:11), tetrabutylammonium bromide/ethylene glycol (1:4), tetrabutylammonium bromide/diethylene glycol (1:4), and tetrabutylammonium bromide/triethylene glycol (1:4) were examined as deep eutectic solvents (DESs). The melting points and dynamic viscosities of these solvents were determined, and the solubilities of benzene, toluene, and ethylbenzene in each were assessed using the cloud point method between T = 303.15 and 353.15 K at atmospheric pressure. The solubilities of each of these three aromatic compounds in these DESs were found to increase with increases in temperature. Both the hydrogen bond acceptors and hydrogen bond donors in the DESs were also shown to affect solubility, with the former having a greater effect and this effect decreasing in the order of tetrabutylammonium bromide > benzyltriphenylphosphonium chloride > choline chloride. The simplified dual-parameter equation and the Apelblat empirical equation were used to correlate the experimentally determined solubilities of benzene, toluene, and ethylbenzene in the seven DESs, and the latter equation generated higher correlations.
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AICHE JOURNAL
·
2021
·Vol. 67
·期 6
·e17197
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IF 3.993
Liyun Huang,Kui Wu,Qian He,Chao Xiong,Tao Gan,Xiaohui He,Hongbing Ji
Single atom catalysts (SACs), featured with atomically dispersed metal species, have been considered as one of the most promising catalytic materials because of the excellent performance in various high-value-added reactions. However, the large-scale and continuous-type production of such SACs is still challenging. Herein, a novel and facile microcapsule strategy for the quasi-continuous synthesis of iron SACs supported on S, N co-doped carbon (Fe/SNC) is developed, and the Fe species are presented as isolated active sites and stabilized as the FeN 3 S-like structure. The as-prepared Fe/SNC catalysts exhibit excellent catalytic properties for selective oxidation of arylalkanes, which followed pseudo-first-order kinetics with an E a = 41.5 kJ/mol. More importantly, the two Fe/SNC catalysts synthesized at different continuous times showed essentially identical catalyst structure and catalytic performance, demonstrating the superior reliability of our microcapsule strategy for the quasi-continuous production of SACs, which can be easily scaled up to industrial application.
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SENSORS AND ACTUATORS B-CHEMICAL
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2020
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IF 7.1
Yanhui Zhong,Zhaoxia Shi,Taoxiao Wen,Xiaohua Xiao,Gongke Li,Yufei Hu
In this work, a novel cataluminescence(CTL) strategy was developed for fast differentiation of sunscreen cosmetics. The CTL reactions occurring on the surface of sunscreen cosmetics whose characteristic composition served as catalyst. Normalization methodology was utilized to process sensor array signals, we developed a dimensionless quantity called “relative signal ( S kr )” to characterize the sensor response. Firstly, aldehydes are eligible for triggering CTL reactions on the surface of TiO 2 , so they served as probe in the CTL sensor. Then, with four aldehydes as sensor elements, the obtained four S kr of a catalytic material constitute as digital code for rapid screening of nanomaterials. Further, the CTL S kr of different brands and colors of sunscreen cosmetics were obtained. The CTL S kr functioned as digital code which can be used to distinguish sunscreen cosmetics. Intersecting, the CTL signals of the array could be applied to normalize, and identify sunscreen cosmetics of different brands and colors through linear discrimination analysis (LDA). It provides a rapid and convenience platform for distinguishing sunscreen cosmetics, and avoid cumbersome sample preparation. The strategy is a new idea for rapid distinguishing the complex samples based on its special ingredient.
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JOURNAL OF CHROMATOGRAPHY A
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2020
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IF 4.049
Gaoyi Yi,Jingxia He,Baian Ji,Die Gao,Kailian Zhang,Lujun Wang,Jing Zeng,Zhining Xia,Qifeng Fu
In recent years, mussel-inspired polydopamine (PDA) based materials have been widely used as stationary phases for open-tubular capillary electrochromatography (OT-CEC) because of their various excellent properties. Nevertheless, the traditional synthesis routes of functionalized PDA-based capillary columns usually are time-consuming and limited in aqueous solutions. Herein, we report a facile and rapid route to prepare octadecylamine (ODA) functionalized PDA coated OT-CEC columns in organic solvents via a novel one-step in situ solvothermal-assisted coating strategy. Through this developed solvothermal-assisted approach, the growth rate of ODA/PDA coating was significantly speeded up and their hybrid coating process on the capillary inner surface could be rapidly completed in 60 min. The successful preparation of the solvothermal-assisted ODA/PDA hybrid coating were systematically characterized and confirmed by several methods. The influence of the preparation parameters on the formation of hybrid coating and the separation ability of the ODA/PDA modified columns were systematically explored. Consequently, the high-efficiency baseline separation of four kinds of neutral, acidic and basic analytes were achieved based on the ODA/PDA modified columns. The repeatability of the solvothermal-assisted ODA/PDA coated column was also studied, and the relative standard deviations for intra-day, inter-day and column-to-column were all less than 5%. Additionally, the solvothermal-assisted ODA/PDA modified column exhibited good stability and long lifetime.
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TALANTA
·
2020
·
IF 5.339
Xue Li,Yuan-Yuan Cui,Cheng-Xiong Yang
Microporous organic networks (MONs) have shown great promise in separation science recently. Exploring novel, simple and convenient strategy to fabricate MONs coated capillary columns for gas chromatography (GC) still remains challenging but desirable for the development of MONs in chromatographic separation. To extend the potential application of MONs in separation science and to further develop novel method for the fabrication of MONs-based capillary columns, here we demonstrate a novel covalent coupling strategy to fabricate uniform MONs bonded capillary columns for GC separation of position isomers and hydrocarbons. The bare capillary column was firstly modified with (3-bromopropyl)trimethoxysilane to provide bromine sites for coupling with alkynyl monomers . The amino- and hydroxyl-functionalized MONs (MON-NH 2 and MON-OH) were then directly grown onto the inner wall of the brominated capillary columns via the covalent coupling between bromine and alkynyl groups. The uniform MON-NH 2 and MON-OH bonded capillary columns were obtained and showed good resolution for GC separation of dichlorobenzene , chlorotoluene, bromotoluene, and propylbenzene position isomers and many other hydrocarbons including linear alkanes, alkylbenzenes , pinene isomers, cyclohexane and benzene, ketones and aldehydes. The MONs bonded capillary columns also owned good lifetime and precision for dichlorobenzene isomers with the relative standard deviations (RSDs) of 0.2–0.3%, 1.2–2.1%, and 1.7–2.5% for retention time, peak height and peak area, respectively. In addition, the fabricated MON-NH 2 and MON-OH bonded capillary columns offered better resolution than commercial InertCap-1, InertCap-5, InertCap-1701 and InertCap-WAX capillary columns for the separation of chlorotoluene and bromotoluene position isomers. These results revealed the feasibility of covalent coupling strategy to fabricate MONs-based stationary phases in GC, highlighting the potential of MONs in separation science.
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JOURNAL OF CHROMATOGRAPHY A
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2020
·
IF 4.049
Xingyun Zhao,Hongyan Zhang,Xiaoyu Zhou,Li Wang,Lihong Wan,Ren'an Wu
Hydrothermally cross-linked polyvinylpyrrolidone (PVP) immobilized SiO 2 stationary phase (CPVP-Sil) was prepared via a green and facile one-pot method which was demonstrated for hydrophilic interaction liquid chromatography (HILIC) as well as reverse phase chromatography(RP). A water or organic solvent-insoluble permanent CPVP immobilizing on the silica particle surface can be formed simply by dipping silica particles into PVP solution and low temperature hydrothermal treatment. The cross-linked PVP network coating on SiO 2 endow it ring lactam functional groups which exhibited excellent separation ability of polar compounds by a typical HILIC retention mechanism at higher organic solvent contents (>55% ACN) and additionally polyvinyl groups for separation of alkylbenzenes in RP mode(<25% ACN). A high column efficiency of about 7 × 10 4 plates per meter was obtained for the test catechol compound. Remarkably, the CPVP-Sil packing materials showed good stability in acid (at pH 3.5) or basic (at pH 9.5) conditions, with 5400-fold column volumes and 3500-fold column volumes respectively.
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ANALYTICA CHIMICA ACTA
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2020
·
IF 5.977
Yueru Shi,Luyi Chen,Junlong Huang,Zhiwei Ma,Qingkun Hu,Fang Zhu,Juan Zheng,Gangfeng Ouyang
Binders are significant components for the preparation of solid-phase microextraction (SPME) fibers. However, little attention has been paid to the effect of different binders. Considering their diverse properties, in this work, we select three kinds of commonly used binders including polydimethylsiloxane (PDMS), polyacrylonitrile (PAN) and Nafion, as well as introduce a new binder of poly (vinylidene fluoride) (PVDF) to synthetically study the influence of binders. By using the commercial active carbons (ACs) with different binders, four SPME fibers with uniform morphologies and comparative thicknesses ( i.e. , ACs-PDMS-coated, ACs-PAN-coated, ACs-Nafion-coated and ACs-PVDF-coated fibers) have been prepared successfully. The effect of binders on the pore structure of ACs is firstly investigated. It is found that PDMS and PAN would cause pore blocking, and the specific surface area of ACs coatings decreases from 1362 m 2 g −1 to 280 and 196 m 2 g −1 , respectively. While the specific surface area of ACs-PVDF composite remains 940 m 2 g −1 . Based on SPME, the influences of acid/alkali, high temperature and matrix towards different fibers are further systematically surveyed. Finally, the enrichment performance of prepared fibers towards various organic pollutants is preliminarily discussed. The comparison results show that PVDF demonstrates outstanding stability in all aspects. Therefore, PVDF might be an excellent candidate for the preparation of SPME fiber. Moreover, all obtained results are expected to provide the reference value for the further development of novel SPME fibers.
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JOURNAL OF CHROMATOGRAPHY A
·
2020
·
IF 4.049
Shenling Wang,Yanling Geng,Xiaowei Sun,Rongyu Wang,Zhenjia Zheng,Shenghuai Hou,Xiao Wang,Wenhua Ji
In this work, a single cross-linking functional monomer, 2,5-divinylterephthalaldehyde, was designed and synthesized to simplify the preparation of molecularly imprinted polymers (MIPs). In the presence of estradiol as a template, MIPs were successfully prepared using 2,5-divinylterephthalaldehyde along with a solvent and initiator. This method reduced most of the complex variables encountered in the traditional synthesis. Characterization of the morphology and structure of the MIPs was performed by scanning electron microscopy, Fourier transform infrared spectroscopy, and Brunauer-Emmett-Teller analysis. Compared with non-imprinted polymers, the MIPs had higher adsorption capacities for five estrogens with imprinting factors above 2.9. The MIPs had high extraction efficiencies, good functional properties, long lifetimes, and good reproducibility, which made them suitable for solid-phase microextraction (SPME). Coupled with ultra-high performance liquid chromatography tandem mass spectrometry, the MIP-based fibers were applied to SPME for the analysis of five estrogens in milk samples. Under the best conditions, the established method had a wide linear range (0.5–10000 ng kg −1 ), low limits of detection (0.08–0.26 ng kg −1 ) and quantification (0.26–0.87 ng kg −1 ), good precision (3.2–8.1%, n = 6), and fiber-to-fiber reproducibility (4.3%–8.8%, n = 3). The MIPs-based fibers can be reused at least 60 times without apparent loss of extraction efficiency. Finally, this method was applied to the determination of target estrogens in milk samples with satisfactory relative recoveries (84.3%–105%, relative standard deviation ≤ 7.8%).
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JOURNAL OF CHROMATOGRAPHY A
·
2020
·
IF 4.049
Zhentao Li,Zhenkun Mao,Changjun Hu,Qiaoyan Li,Zilin Chen
Fluorous affinity means remarkably specific interaction between highly organic fluorides. This work aims to explore the potential of fluoro-functionalized stationary phase for the separation of organic fluorides by means of fluorous-fluorous interaction. Here, by using the Michael addition strategy between 1H,1H,2H,2H-perfluorodecanethiol (PFDT) and polydopamine (PD), a novel fluoro-functionalized stationary phase was synthesized for open-tubular capillary electrochromatography (OT-CEC). The PFDT@PD was characterized by scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR) and X-ray Photoelectron Spectrometer (XPS). The PFDT@PD@capillary exhibited outstanding separation performance towards neutral compounds (such as alkylbenzenes and chlorobenzenes) and organic fluorides (such as fluorobenzenes and perfluoroalkyl methacrylates etc.) with high resolution and high separation efficiency by hydrophobic interaction and fluorous-fluorous interaction. In addition, the column shows good stability and reproducibility. The relative standard deviations (RSDs) of the retention time for intra-day (n = 5) and inter-day (n = 3) runs and between columns (n = 3) are less than 0.39%, 1.22% and 3.87%, respectively. This novel type of fluoro-functionalized stationary phase represents a great application potential in organic fluorides separation field.
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Molecular Catalysis
·
2020
·
IF 3.687
Hongbing Song,Yule Liu,Yongjie Wang,Bingxiao Feng,Xin Jin,Tingting Huang,Meng Xiao,Hengjun Gai
In this study, a series of hypercrosslinked poly(ionic liquid)s (HCPILs) formed from imidazolium tetrachloropalladate were successfully fabricated for selective hydrogenation of phenylacetylene. Its textural properties can be tuned by the different molar ratios of reactants, thereby adjusting its active sites. The synthetic HCPILs were analyzed using various characterization techniques. Due to the constraint of the microporous structure and the charge effect of ionic liquid moieties in the HCPILs, palladium nanoparticles generated from HCPILs were reduced in situ during hydrogenation of phenylacetylene and highly dispersed. Amongst which catalyst a-4 with the largest pore-volume performed the best selectivity (97.3 %) to styrene at 96 % phenylacetylene conversion under the conditions of 308 K and 1 atm H 2 pressure. Furthermore, the activity and selectivity of the catalyst did not change considerably in solvents with different polarities. Even after repeated the catalytic experiments for five times, the catalyst displayed no significant loss for activity and selectivity. This work shows industrial application potential and a developing direction in the selective hydrogenation process.
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