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MOLECULES · 2022 ·Vol. 27 ·期 6 ·1950 · IF 4.927

Determination of Methyl Methanesulfonate and Ethyl Methylsulfonate in New Drug for the Treatment of Fatty Liver Using Derivatization Followed by High-Performance Liquid Chromatography with Ultraviolet Detection

Yue Wang,Jing Feng,Song Wu,Huihui Shao,Wenxuan Zhang,Kun Zhang,Hanyilan Zhang,Qingyun Yang

A new derivatization high-performance liquid chromatography method with ultraviolet detection was developed and validated for the quantitative analysis of methanesulfonate genotoxic impurities in an innovative drug for the treatment of non-alcoholic fatty liver disease. In this study, sodium dibenzyldithiocarbamate was used as a derivatization reagent for the first time to enhance the sensitivity of the analysis, and NaOH aqueous solution was chosen as a pH regulator to avoid the interference of the drug matrix. Several key experimental parameters of the derivatization reaction were investigated and optimized. In addition, specificity, linearity, precision, stability, and accuracy were validated. The determined results of the samples were consistent with those obtained from the derivatization gas chromatography–mass spectrometry analysis. Thus, the proposed method is a reliable and practical protocol for the determination of trace methanesulfonate genotoxic impurities in drugs containing mesylate groups.

研究领域: 药物分析 · 毒理学 · 分析化学
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Metals · 2024 ·Vol. 14 ·期 1 ·87 · IF 2.6

Electrochemistry of Tin Deposition from Methanesulfonic Acid

Yuantao Yang,Junli Wang,Xuanbing Wang,Jinlong Wei,Xiaoning Tong,Ruidong Xu,Linjing Yang

The electrolytic refining of crude tin is generally carried out in the fluorosilicic acid (H2SiF6) system with the assistance of bone glue and β-naphthol. However, the high saturated vapor pressure and low stability of H2SiF6present environmental concerns and do not align with sustainable development goals. In this paper, the electrochemical behavior of tin on a glassy carbon (GC) electrode was studied in a relatively green and environmentally friendly methanesulfonic acid (MSA) system. Bone glue, sodium lignosulfonate, and β-naphthol were used as additives to make the deposit morphology smooth and to ensure grain refinement. The electrochemical reduction process of Sn2+in an MSA system is a quasi-reversible process controlled by diffusion. The apparent activation energyEa= 14.189 kJ/mol for the ion diffusion of Sn2+was further calculated. The results of chronoamperometry showed that the electrocrystallization of Sn2+on the GC electrode gradually tended to three-dimensional instantaneous nucleation with the increase in applied potential. The morphology and phase of the deposits were analyzed using scanning electron microscopy (SEM) and X-ray diffraction (XRD). The results showed that the deposits were uniform and dense pure tin. This work elucidates the electrochemical behavior of tin in a methanesulfonic acid system.

研究领域: 电化学 · 材料科学
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POLYMER DEGRADATION AND STABILITY · 2024 · IF 6.3

Amphiphilic molecules affording efficient aqueous degradation of unsaturated polyester resin

Peng Zhao,Xiaojing Cui,Chizhou Wang,Xiaojie Shao,Hongyan Li,Ning Zhang,Xianglin Hou,Tiansheng Deng

Enormous challenges have been encountered in the degradation and recycling of unsaturated polyester resin (UPR) in water, primarily due to its water resistance. Herein, a novel, efficient and green catalytic system of methanesulfonic acid (MSA)/sodium laurylsulfonate (SLS) was proposed to aqueously degrade UPR under mild conditions (200°C). This method is considerably milder compared to other reported works based on aqueous hydrolysis (230°C-380°C). What's more, amphiphilic SLS as a phase transfer reagent enhanced the concentration of catalyst at the H 2 O-UPR interface, which facilitated the mass transfer between organic motifs with inorganic reagents and thus accelerated the reaction. The NMR and FT-IR characterizations indicated the ester bonds were cleaved via hydrolysis with H 2 O catalyzed by MSA, and high value-added products, i.e., copolymer of styrene and maleic anhydride (SMA) and phthalic acid (PA), were reclaimed by a simple separation process, with the yield of 86.77% and 84.37%, respectively. Furthermore, a viable mechanism for degradation was proposed through the degradation performance of the model compounds. This study provides a practical approach for the chemical degradation and conversion of other resins containing ester bonds.

研究领域: 材料科学 · 环境科学
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JOURNAL OF SEPARATION SCIENCE · 2019 ·Vol. 43 ·期 2 ·398-405 · IF 2.516

Ultrasensitive high-performance liquid chromatography determination of tetracycline antibiotics and their 4-epimer derivatives based on dual effect of methanesulfonic acid

Xiaojing Lai,Jing Liu,Xin Xu,Jie Li,Baojun Zhang,Lijun Wei,Hongping Cai,Xianglei Cheng

In reversed-phase liquid chromatography, tetracycline antibiotics yield broad and asymmetrical peaks, as a result of their ionic interaction with the anionic free silanol groups and metal ion present in the silica-based stationary phases (commonly derivatized with C18 groups). These frequently encountered difficulties were absolutely eliminated based on dual effect when methanesulfonic acid was employed as an eluent additive. The study revealed that the performance of methanesulfonic acid to minimize the “silanol effect” is mainly explained by both direct neutralization of the anionic silanol sites and electrostatic attraction with analytes. Based on these dual action mechanisms, an ultrasensitive method has been successfully developed for the simultaneous determination of tetracycline antibiotics and their derivatives (minocycline, oxytetracycline, tetracycline, chlortetracycline, metacycline, doxycycline, 4-epitetracycline, and 4-epichlortetracycline) in bovine milk with convenient ultraviolet detection within 15 min. Under the optimal conditions, the calibration curves showed good linearity ( r 2 > 0.999) for all analytes in the range of 1∼200 ng/mL with the instrument limits of detection as low as 0.3 ng/mL. The study sheds new light on suitable additives to analyze basic compounds with the advantage of good compatibility with MS detection.

研究领域: 分析化学 · 药物分析 · 食品安全
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FUEL PROCESSING TECHNOLOGY · 2015 · IF 3.352

Microwave-assisted nickel and vanadium removal from crude oil

Hui Shang,Yu Liu,Jin-Chun Shi,Quan Shi,Wen-Hui Zhang

Most crude oils contain traces of metal complexes, among which vanadium (V) and nickel (Ni) compounds are the most harmful poisons to the catalysts of fluid catalytic cracking (FCC) and hydrogenation units. These metals are proven to be extremely hard to remove, since they exist in crude oil as stable oil-soluble complexes. The microwave technology provides a new way for Ni/V removal, their removal efficiency using chemical reagents and the mechanism of microwave-assisted demetallization were studied in this paper. It was concluded that the demetallization efficiency can be highly enhanced under microwave irradiation . There is no specific structural selectivity for vanadium porphyrins during microwave treatment process. The demetallization agent — methanesulfonic acid , containing a sulfonyl acid group was found to react with VO 2   + and Ni 2   + . Ni and V were removed from porphyrin ring without destroying the ring structure, corresponding water soluble inorganic salts were formed, thus can be successfully separated from crude oil by washing or desalting process.

研究领域: 化学工程 · 石油加工 · 环境科学
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JOURNAL OF THE ELECTROCHEMICAL SOCIETY · 2019 ·Vol. 166 ·期 13 ·D638 · IF 3.12

Fabrication of Ti/SnO2-Sb/Ce-PbO2 Anode from Methanesulfonate Bath and Its Electrocatalytic Activity

Pengfei Xu,Xiaohong He,Junwei Mao,Yongming Tang

In this paper, Ti/SnO2-Sb/Ce-PbO2 anode is electrodeposited from MSA bath, and the effect of Ce3+ concentration in bath on the phase composition and morphology of lead dioxide electrode is elucidated. It is found that with the addition of 2 mM Ce3+ ion to the bath the Ce-PbO2 anode exhibits highest stability in 0.5 M H2SO4, and cerium exists as Ce (IV) in the PbO2 film. The electrocatalytic activity of lead dioxide anode for phenol removal is slightly enhanced by the inclusion of Ce. The significant improvement in electrocatalytic activity can be achieved by the addition of small amount of Bi3+ ion to the bath containing Ce3+ ion. In this study, electrocatalytic activities of various anodes follow the order: Ce,Bi-PbO2 > Ce-PbO2 > undoped PbO2 > Bi-PbO2.

研究领域: 材料科学 · 电化学
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JOURNAL OF POWER SOURCES · 2019 · IF 7.467

Recycling LiCoO2 with methanesulfonic acid for regeneration of lithium-ion battery electrode materials

Bin Wang,Xin-Ye Lin,Yuanyuan Tang,Qiang Wang,Michael K.H. Leung,Xiao-Ying Lu

With the massive consumption of lithium-ion batteries in portable consumer electronics and electric vehicles, proper disposal of spent batteries is of paramount importance for sustainable development. In this study, biodegradable organic methanesulfonic acid (MSA) is investigated for the first time to leach valuable metals from waste LiCoO 2 powders for battery material regeneration. Under the optimal conditions, leaching efficiencies of lithium and cobalt are achieved at nearly ∼100% and ∼100%, respectively. Comparison experiment indicates that MSA can achieve better leaching performance than previously reported organic acids (e.g. citric acid , malonic acid , succinic acid , oxalic acid) under the same conditions. Besides, strong leaching capability of MSA at high solid-to-liquid ratios (e.g. 81.2 g L −1 and 163 g L −1 ) is confirmed with satisfactory leaching efficiencies (ca. 92.4%–100%). Feasibility test of MSA utilization for proper treatment of spent batteries is demonstrated at the optimized conditions. Importantly, regeneration study suggests that the as-obtained leachate can be employed to synthesize Co 3 O 4 anode and LiCoO 2 cathode materials with micro/nanostructures. Excellent cycling performance and rate capability of the regenerated electrode materials are demonstrated in the repeated charge-discharge cycles. Overall, the proposed recycling strategy is of great significance for rational resource utilization of spent lithium-ion batteries.

CAS / MDL: 144-62-7 34819-78-8
研究领域: 材料科学 · 环境科学
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Lubricants · 2023 ·Vol. 11 ·期 4 ·156 · IF 3.5

Synthesis of Multi-butylnaphthalene Base Oils Catalyzed by Trifluoromethanesulfonic Acid and Its Lubricating Properties

Yuanyuan Li,Chen Chen,Qiong Tang,Lei Liu,Jinxiang Dong

Alkylnaphthalene as base oils are widely applied in the production of high-performance lubricating oils. Here, we report the synthesis of multi-butylnaphthalenes by alkylation of naphthalene andn-butene with trifluoromethanesulfonic acid as catalyst. Trifluoromethanesulfonic acid exhibited excellent catalytic performance with naphthalene conversion, as high as 98.5%, and the multi-butylnaphthalenes selectivity of 98.8% under optimum conditions. To investigate the effects of the side-chain numbers on naphthalene on the lubrication performance, two kinds of alkylnaphthalenes were obtained by controlling catalyst dosage, denoted as MBN-1 (90.3% mono/di-butylnaphthalenes) and MBN-2 (98.2% tri/tetra/penta/hexa-butylnaphthalenes), respectively. The primary physiochemical properties of the synthetic oils were tested, and their tribological performance was evaluated. MBN-2, with more side chains on naphthalene, displayed more effective friction reduction and anti-wear properties than MBN-1 and the commercial alkyl naphthalene base oil AN5.Keywords:naphthalene;trifluoromethanesulfonic acid;alkylation;synthetic lubricating base oil

研究领域: 化学工程 · 材料科学
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ACS Sustainable Chemistry & Engineering · 2022 · IF 9.224

Green Electrorefining of Crude Lead with High-Quality Deposits in an Additive-Assisted Methanesulfonic Acid System

Changliu Xiang,Sijun Zhu,Jinbo Song,Yougang Li,Tao Luo,Cong Chang,Junjie Qu,Shenghai Yang,Changhong Wang,Yongming Chen

The conventional electrorefining process of crude lead (Pb)─employing a bone glue (BG)- and calcium lignosulfonate (CL)-synergistically assisted fluosilicic acid (H2SiF6) system─suffers the undesired environment burden caused by the high saturated vapor pressure and low stability of H2SiF6. Herein, we propose an additive-assisted methanesulfonic acid (MSA) system for green and efficient electrorefining of crude Pb based on the low volatility and high stability of MSA. Combinations of MSA with additives are evaluated and screened using photographic images, SEM observations, XRD, white light interference, etc. The electrochemical analysis of cyclic voltammetry and chronoamperometry elucidates the Pb deposition behavior in the Lugalvan BNO12-assisted MSA system, in which a three-dimensional nucleation model is applicable. Using MSA as the solvent and β-naphthol ethoxylate (Lugalvan BNO12) as the assisted additive, the bench-scale operation of crude Pb electrorefining experimentally achieves an electric energy requirement (W) of 87 kWhe/t Pb and a cathodic current efficiency (η) of 99.6%. This is very competitive with the W of 120 kWhe/t Pb and η of 95.0% for the BG-CL-assisted H2SiF6 system. Also, the bench-scale operation obtains a plat and dense deposit sample with a Pb purity of >99.99%. The distribution behavior of elements shows that most of the Pb element is recovered in the form of the cathodic Pb, elements Sn, Zn, and Fe mainly accumulate in the electrolyte, and elements As, Sb, Bi, Ag, and Cu remain in the anode slime. This work opens new directions for more technically and economically feasible Pb electrorefining.

研究领域: 冶金工程 · 环境科学
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JOURNAL OF MOLECULAR LIQUIDS · 2019 · IF 4.561

Prediction of viscosity for high-concentrated ternary solution (CH3SO3H + VOSO4 + H2O) in vanadium flow battery

Xiangrong Li,Chenglin Jiang,Jianguo Liu,Ye Qin,Zhongyu Zhang,Zaibo Liu,Jiazhen Yang,Chuanwei Yan

In this paper, a model for viscosity of high-concentrated additive (methanesulfonic acid) in vanadium electrolyte is reported. Methanesulfonic acid was evaluated as a possible stabilizing agent for the thermal precipitation of supersaturated V(V) solutions at elevated temperatures. Viscosity ( η ) of the ternary solution CH 3 SO 3 H + VOSO 4  + H 2 O was measured between the temperatures 283.15 K and 318.15 K under atmospheric pressure. Based on the viscosity, viscosity B -coefficient, activation energy (Δ μ 0 ≠ 0 ) and Gibbs free energy of activation (Δ G ≠ ) were further calculated. With the help of these paraments, a semi-empirical predicting function is established to estimate the viscosity of high-concentrated additive, i.e. methanesulfonic acid in vanadium electrolyte. AARD of this semi-empirical method is 0.22%, which demonstrates that viscosity estimation for high-concentrated ternary solution CH 3 SO 3 H + VOSO 4  + H 2 O can be achieved.

研究领域: 化学工程 · 能源科学
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JOURNAL OF THE ELECTROCHEMICAL SOCIETY · 2018 ·Vol. 165 ·期 16 ·D783 · IF 3.662

Electrochemical Nucleation and Growth of Cobalt from Methanesulfonic Acid Electrolyte

Delong Kong,Zhen Zheng,Fanyu Meng,Ning Li,Deyu Li

Electrochemical nucleation and growth of cobalt onto glassy carbon electrode (GCE) from methanesulfonic acid (MSA) electrolyte was investigated, the influence of pH and cobalt concentration on the electrocrystallization mechanism was also examined. Cyclic voltammetry experiments indicate a pH and cobalt concentration dependence of the onset potential and a deposit phase change with decreasing pH was also noted. From analysis of current transients, the diffusion coefficient of cobalt ion was estimated as 1.89 × 10−5 cm2s−1. The electrocrystallization mechanism for 0.6 mol/L Co2+ follows the instantaneous nucleation with kinetic controlled growth and is independent of the bath pH while the mechanism for 0.2 mol/L Co2+ follows the progressive nucleation with diffusion controlled growth at pH = 2.0 and then goes to instantaneous nucleation with kinetic controlled growth at pH = 1.5 and exhibits a process of progressive nucleation with kinetic controlled growth with lower pH of 1.0.

研究领域: 电化学 · 材料科学
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MATERIALS LETTERS · 2024 · IF 2.7

A facile approach to the preparation of S-doped porous carbons for CO2 adsorption

Hongmin Cui,Jianguo Xu,Nanfu Yan,Runhan Yan,Jinsong Shi

In the current work, we explored the direct synthesis of S-doped porous carbons employing cesium methanesulfonate as a novel bifunctional chemical activator. The obtained carbons showed high surface area (654–2264 m 2 /g) and high S content (6.56–15.13 wt%). Effects of activation temperature and cesium methanesulfonate amount on the carbons’ properties were also studied. The obtained carbons showed CO 2 uptake of 3.58–4.76 mmol/g at 0 °C and 1 bar. Effects of textural properties and S-doping on CO 2 adsorption performances were discussed.

CAS / MDL: 9004-34-6
研究领域: 材料科学 · 环境科学
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