High performance liquid chromatography analysis of p-aminophenol synthesized by nitrobenzene transfer hydrogenation using formic acid as hydrogen sourceEI北大核心CSCD

Qualitative analysis of the main by-product of 4-hydroxybenzamide in the synthesis of p-aminophenol bynitrobenzene transfer hydrogenation with formic acid as hydrogen source was carried out by electrospray ionization mass spectrometry. The reaction system was quantitatively analyzed by high performance liquid chromatography. The chromatographic conditions were shown as followsShim pack VP-ODS column250 mm× 4.6 mm5 μµmdetection wavelength of 254 nmVmethanolVbuffer solution=114.8 mmol/L sodium dihydrogen phosphate solution1.9 mmol/L dibasic sodium phosphate solutionas the mobile phase and the flow rate of 0.8 mL/min with a column temperature of 35. Nitrobenzenep-aminophenolaniline and formylaniline in the reaction system were quantitatively analyzed by standard curve method with methyl N-phenylcarbamate as internal standard. The correlation coefficientsR2were 0.99930.99950.9998 and 0.9992 for these analytes respectively. The relative standard deviations RSDs were less than 1.0% 0.3% 0.2% and 0.4% respectively. The recoveries were in the ranges of 95.5%-102.6%101.2%-104.8%95.1%-99.8% and 95.7%-101.1%respectively. This method can be used for the simultaneous determination of main and by-products in the transfer hydrogenation of nitrobenzene with formic acid as hydrogen source. © 2022, Youke Publishing Co.,Ltd. All rights reserved.     

高效液相色谱-紫外检测法测定水产品中氨苯砜及其代谢物残留量EI北大核心CSCD

建立了水产品中氨苯砜及其代谢产物N-乙酰氨苯砜残留量同时测定的高效液相色谱-紫外检测法(HPLC-UV)。样品经1%氨化乙腈提取,正己烷去脂,MCX阳离子固相萃取柱富集净化,氮吹浓缩,定容过膜后测定。以甲醇和水为流动相,ZORBAX SB-C_(18)色谱柱梯度洗脱分离,采用保留时间定性,外标法定量。在最佳检测条件下,目标化合物质量浓度在5~200 ng/mL范围内线性关系良好(R^(2)> 0.999),检出限(LOD)为10.0μg/kg,定量限(LOQ)为20.0μg/kg。以不同类型的水产品为空白基质,在20,50,100μg/kg加标水平下,氨苯砜的回收率为70.1%~81.7%,N-乙酰氨苯砜的回收率为84.2%~109.5%,相对标准偏差(RSD)均小于10%。该方法能够实现大批量水产品中氨苯砜及其代谢物残留量的检测。     

Enhanced Electrochemical Nitrate-to-Ammonia Performance of Cobalt Oxide by Protic Ionic Liquid Modification

Electrochemical conversion of nitrate to ammonia is an appealing way for small-scale and decentralized ammonia synthesis and waste nitrate treatment. Currently, strategies to enhance the reaction performance through elaborate catalyst design have been well developed, but it is still of challenge to realize the promotion of reactivity and selectivity at the same time. Instead, a facile method of catalyst modification with ionic liquid to modulate the electrode surface microenvironment that mimic the role of the natural MoFe protein environment is found effective for the simultaneous improvement of NH₃ yield rate and Faradaic efficiency (FE) at a low NaNO₃ concentration of 500 ppm. Protic ionic liquid (PIL) N-butylimidazolium bis(trifluoromethylsulfonyl)imide ([Bim]NTf₂) modified Co₃O_4−x is fabricated and affords the NH₃ yield rate and FE of 30.23±4.97 mg h⁻¹ mg_cat.⁻¹ and 84.74±3.43 % at −1.71 and −1.41 V vs. Ag/AgCl, respectively, outperforming the pristine Co₃O_4−x. Mechanistic and theoretical studies reveal that the PIL modification facilitates the adsorption and activation of NO₃⁻ as well as the NO₃⁻-to-NH₃ conversion and inhibits hydrogen evolution reaction competition via enhancing the Lewis acidity of the Co center, shuttling protons, and constructing a hydrogen bonded and hydrophobic electrode surface microenvironment.     

Rational Design of Porous Ionic Liquids for Coupling Natural Gas Purification with Waste Gas Conversion

Removal of trace impurities for natural gas purification coupled with waste gas conversion is highly desired in industry. We here report a type of porous ionic liquids (PILs) that can realize the continuous flow separation of CH₄/CO₂/H₂S and the conversion of the captured H₂S to useful products. The PILs are synthesized through a step-by-step surface modification of ionic liquids (ILs) onto UiO-66-OH nanocrystals. The introduction of free tertiary amine groups on the nanocrystal surface endows these PILs with an exceptional ability to enrich H₂S from CO₂ and CH₄ with impressive selectivity, while the permanent pores of UiO-66-OH act as containers to store an exceptionally higher amount of the selectively captured H₂S than the corresponding nonporous ILs. Simultaneously, the tertiary amines as dual functional moieties offer effective catalytic sites for the conversion of the H₂S stored in PILs into 3-mercaptoisobutyric acid, a key intermediate required for the synthesis of Captopril (an antihypertensive drug). Molecular dynamics, density functional theory calculations and Grand Canonical Monte Carlo simulations help understand both the mechanisms of separation and catalysis performance, confirming that the tertiary amines as well as the permanent pores in UiO-66-OH play vital roles in the whole procedure.     

Director field configurations around a spherical particle in a nematic liquid crystal

We study the director field around a spherical particle immersed in a uniformly aligned nematic liquid crystal and assume that the molecules prefer a homeotropic orientation at the surface of the particle. Three structures are possible: a dipole, a Saturn-ring, and a surface-ring configuration, which we investigate by numerically minimizing the Frank free energy supplemented by a magnetic-field and a surface term. In the dipole configuration, which is the absolutely stable structure for micron-size particles and sufficiently strong surface anchoring, a twist transition is found and analyzed. We show that a transition from the dipole to the Saturn ring configuration is induced by either decreasing the particle size or by applying a magnetic field. The effect of metastability and the occurrence of hysteresis in connection with a magnetic field are discussed. The surface-ring configuration appears when the surface-anchoring strength W is reduced. It is also favored by a large saddle-splay constant K₂₄. A comparison with recent experiments [#!itapdb:Poulin1997!#,#!itapdb:Poulin1998!#] gives a lower bound for W, i.e., for the interface of water and pentylcyanobiphenyl (5CB) in the presence of the surfactant sodium dodecyl sulfate. Received 2 November 1998     

Dielectric properties of side chain liquid crystalline elastomers: influence of crosslinking on side chain dynamics

Dielectric response, from 1 Hz to 10 MHz, of liquid crystalline side chain elastomers has been compared to the one of analogous uncrosslinked materials. Results are discussed in terms of mobility of the mesogens. Two different systems have been investigated: smectic A elastomers allow to determine the influence of crosslinking on the relaxation (i.e. the reorientation of the whole mesogen around the chain), a S _C ^* elastomer shows the drastic influence of the polymer network on the Goldstone mode. Received 12 October 1998     

液体中溶解气体的普适分析方法-声致发光法

液体中溶解气体的量的分析一直是分析化学中的难题。迄今为止,只是发展了水体中溶解氧的化学分析与仪器分析方法,而其他的气体如N2,CO2,CH4的分析方法至今仍很缺乏,特别是液体中溶解的稀有气体,如：Ar,He,Ke的分析方法至今仍然是空白,文章介绍了声致发光分析气体溶解于液体（包括非水溶液）的新方法。     

Synthesis and characterization of TiO2 powders by the double-nozzle electrospray pyrolysis method. Part 2. Material evaluation

Here we report the synthesis and characterization of anatase TiO₂ powders by the double-nozzle electrospray pyrolysis method. Titanium(IV) bis(ammonium lactato) dihydroxide (TALH) aqueous solution (2.0 wt%) and pure H₂O were separately injected into capillaries by using two syringe pumps, and were electrosprayed by using positive (+4 kV) and negative (−4 kV) DC voltage, respectively. Under a stream of dry clean air, the droplets were carried to the stainless steel tube heated with a tubular furnace at 350–450 °C. Thanks to the neutralization of droplets by the double-nozzle electrospray, the final TiO₂ powder yield after pyrolysis was much improved from 6% (by single nozzle) to 55.4% (in this study), although the particle size distribution became wider due to the electrical neutralization and coalescence of the droplets. Photocatalytic activity for H₂ evolution was studied.     

Determination of eugenol and isoeugenol in aquaculture water by ultra performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometryEI北大核心CSCD

An analytical method was established for the determination of eugenol and isoeugenol in aquaculture water by ultra performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry UPLC-Q-TOF-MS. Water samples were derivatized with dansyl chloride. The derivatization products were separated on a ThermoAccucore C18 column100 mm×2.1 mm2.6 μµm under gradient elution condition utilizing acetonitrile and 0.1% formic acid as mobile phases. Q-TOF-MS operating in mass data using alternating collision cell energyMSEmode with positive electrospray ionization was used for the identification of analytes. The results showed that the calibration curves for eugenol and isoeugenol were linear in the range of 0.1-20 μµg/L with the correlation coefficientsrhigher than 0.995. Their recoveries in aquaculture water were 83.2%-102% and 91.8%-104%respectivelywith relative standard deviationsRSDsless than 15%. The limits of detection were 0.02 and 0.05 μµg/L and the limits of quantitation were 0.05 and 0.1 μµg/Lrespectively. The method can be applied to the determination of eugenol and isoeugenol in real water samples. © 2022, Youke Publishing Co.,Ltd. All rights reserved.     

Solvent effectiveness factor: A new correlation to study the influence of solvent,temperature, and stirring rate on synthesis yield of Ionic Liquids

The main objective of this study is to investigate the effect of solvent, temperature, and stirring on synthesis yield of Ionic Liquids (ILs). A representative Ionic Liquid [BMIM][BF₄] is prepared using seven different solvents and their influence on percentage yield is explained using a new correlation; solvent effectiveness factor (SEF). The SEF of solvent is governed by nature of solvent, operating temperature and stirring rate. Acetone has the highest SEF 1.275 and affords maximum IL yield 88.11% while toluene has the least SEF 0.674 and produces minimum IL 63.21%. When synthesis temperature is increased from 50 to 80 °C, synthesis yield is substantially increased from 76.7 to 93.08% because rise in temperature increases the SEF from 1.234 to 1.333, mainly due to the decrease in solvent viscosity. Similarly, when stirring rate is increased from 80 to 200 RPM, IL yield slightly increased from 87.37 to 91.35% due to addition of mechanical energy in the reaction mixture which in turn reduced solvent viscosity and increased SEF from 1.278 to 1.297.