液相色谱法测定氯乙酸中乙酸、二氯乙酸的含量

提出了液相色谱法测定氯乙酸中乙酸和二氯乙酸含量的分析方法,计算出氯乙酸的含量,并与现行工业氯乙酸国标分析方法进行了比较,证明液相色谱分析方法简洁、快速,分析结果准确,在氯碱行业具有推广运用的价值。     

Studying local liquid velocity in liquid–solid packed bed using the newly developed X-ray DIR technique

Combination of X-ray Digital Industrial Radiography (DIR) and Particle Tracking Velocimetry (PTV) techniques for local liquid velocity measurement (V_LL) has been newly developed and successfully applied for trickle bed reactor (TBR). The technique was validated against newly developed fiber optical probe technique. This work attempts to highlight the applicability of this newly developed technique on a liquid–solid packed bed reactor. In this work, liquid was represented by water and solids were represented by EPS beads. The EPS beads were chosen because of its low density property. Three superficial liquid velocities (V_SL) were applied to the system. The experiment was replicated four times. The digital industrial radiography (DIR) consists of a complementary metal oxide semiconductor (CMOS) digital detector and X-ray source. Results of this work suggest that the technique has been successfully applied and comparable with previous work that has been done in the literature. It also suggests that there will be a maximum measurable interstitial liquid velocity when it travel inside the packed bed. The measured V_LL can have a maximum range that is between 4 and 4.7 times that of its V_SL. For V_SL=0.42±±2%, the V_LL-Max is in between 1.7 cm/s and 1.9 cm/s, V_SL=0.84±±2%, the V_LL-Max is in between 3.6 cm/s and 4.0 cm/s, and for V_SL=1.11±±2%, the V_LL-Max is in between 4.3 cm/s and 4.8 cm/s.     

UPLC法同时测定阿托伐他汀钙中15个杂质含量

目的建立超高效液相色谱法(UPLC)同时测定阿托伐他汀钙原料药中15个杂质含量的方法。方法采用岛津Shim-pack Velox PFPP(2.1 mm×100 mm,1.8μm)色谱柱,以3.9 g/L醋酸铵缓冲液(pH 5.0):乙腈:甲醇:四氢呋喃(无稳定剂)=67:21:6:6为流动相A,3.9 g/L醋酸铵缓冲液(pH 5.0):乙腈:甲醇:四氢呋喃(无稳定剂)=27:61:6:6为流动相B;梯度洗脱,流速0.43 ml/min,检测波长244 nm,柱温35℃,样品室温度10℃;进样量1.8μl。结果阿托伐他汀钙及各杂质峰间分离良好,在0.3~3μg/ml范围内15个杂质均呈良好的线性关系(r均>0.999,n=6),各杂质平均回收率分别为96.3%,99.1%,99.9%,102.4%,96.4%,99.8%,99.4%,104.9%,106.4%,105.4%,100.1%,98.9%,94.7%,94.4%,101.4%,且不同浓度间平行性良好。15个杂质重复性、进样精密度、中间精密度均良好,48 h内均较稳定。此法除对色谱柱要求较高外,耐用性良好。结论本方法简便、快速、分离度好、专属性强,经方法学验证可用于阿托伐他汀钙原料药杂质质量控制。     

Impact of non‐solvent on regeneration of cellulose dissolved in 1‐(carboxymethyl)pyridinium chloride ionic liquid

Cellulose dissolved in ionic liquid (1‐(carboxymethyl)pyridinium chloride)/water (60/40 w/w) mixture is regenerated in various non‐solvents, namely water, ethanol, methanol and acetone, to gain more insight into the contribution of non‐solvent medium to the morphology of regenerated cellulose. To this end, the initial and regenerated celluloses were characterized with respect to crystallinity, thermal stability, chemical structure and surface morphology using wide‐angle X‐ray diffraction, thermogravimetric analysis, Fourier transform infrared spectroscopy and scanning electron microscopy. According to the results, regardless of non‐solvent type, all regenerated samples have the same chemical structure and lower crystallinity in comparison to the initial cellulose, making them a promising candidate for efficient biofuel production based on enzymatic hydrolysis of cellulose. The reduction in crystallinity of regenerated samples is explained based on the potential of the non‐solvent to break the hydrogen bonds between cellulose chains and ionic liquid molecules as well as the affinity of water and non‐solvent which can be evaluated based on Hansen solubility parameter. The latter also determines the phase‐separation mechanism during the regeneration process, which in turn affects surface morphology of the regenerated cellulose. The pivotal effect of regenerated cellulose crystallinity on its thermal stability is also demonstrated. Regenerated cellulose with lower crystallinity is more susceptible to molecular rearrangement during heating and hence exhibits enhanced thermal stability. © 2019 Society of Chemical Industry     

Density functional theory study on dehydrogenation of methylcyclohexane on Ni–Pt(111)

Methylcyclohexane is a very promising liquid organic hydrogen carrier, but its dehydrogenation mechanism on Pt-based bimetallic catalysts is not yet clear. In order to understand the catalytic dehydrogenation of methylcyclohexane on Ni–Pt(111), DFT calculations were performed and the calculation results were compared with the corresponding values on Pt(111). It is shown that because the electronegativity of Ni atoms is less than that of Pt atoms, electrons transfer from Ni atoms to Pt atoms. Compared with Pt(111), the binding energy (the absolute value of the adsorption energy) of related species on Ni–Pt(111) surface was smaller, indicating that the binding strength between these species and the surface metal atoms on Ni–Pt(111) is weaker. In the stable adsorption configurations on Ni–Pt(111), almost all the metal atoms forming chemical bonds with the adsorbates were Pt atoms, indicating that Pt was the main active component. Although the actual catalytic reaction is more complicated, this study provided some insights into one of the important aspects.     

The control of paracetamol particle size and surface morphology through crystallisation in a spray dryer

The parameters governing the crystallisation of paracetamol using various conventional techniques has been extensively studied, however the factors influencing the drug crystallisation using spray drying is not as well understood. The aim of this work was to investigate the crystallisation of an active pharmaceutical ingredient through evaporative crystallisation using a spray dryer to study the physicochemical properties of the drug and to use semi-empirical equations to gain insight into the morphology and particle size of the dried powder. Paracetamol solutions were spray dried at various inlet temperatures ranging from 60 °C to 120 °C and also from a series of inlet feed solvent compositions ranging from 50/50% v/v ethanol/water to 100% ethanol and solid-state characterisation was done. The size and morphology of the dried materials were altered with a change in spray drying parameters, with an increase in inlet temperature leading to an increase in particle Sauter mean diameter (from 3.0 to 4.4 µm) and a decrease in the particle size with an increase in ethanol concentration in the feed (from 4.6 to 4.4 µm) as a result of changes in particle density and atomised droplet size. The morphology of the dried particles consisted of agglomerates of individual crystallites bound together into larger semi-spherical agglomerates with a higher tendency for particles having crystalline ridges to form at higher ethanol concentrations of the feed.     

融合前沿研究的液体电介质击穿教学研究

针对《高电压与绝缘技术》课程中液体电介质的教学难点，提出了融合前沿研究的液体电介质击穿教学方法。基于前沿的液体放电应用背景与先进的液体放电研究平台，形象地展示液体电介质的动态击穿过程，在教学内容、教学方法、考核方式等方面进行科教融合改进，实施“以学生为中心”理念的课程教学设计。该教学方式取得了较好的教学效果，能够为其它知识点的教学质量提升提供参考。     

High-Performance Unidirectional Manipulation of Microdroplets by Horizontal Vibration on Femtosecond Laser-Induced Slant Microwall Arrays

The high-performance unidirectional manipulation of microdroplets is crucial for many vital applications including water collection and bioanalysis. Among several actuation methods (e.g., electric, magnetic, light, and thermal actuation), mechanical vibration is pollution-free and biocompatible. However, it suffers from limited droplet movement mode, small volume range (V_Max/V_Min < 3), and low transport velocity (≤11.5 mm s⁻¹) because the droplet motion is a sliding state caused by the vertical vibration on the asymmetric hydrophobic microstructures. Here, an alternative strategy is proposed—horizontal vibration for multimode (rolling, bouncing/reverse bouncing, converging/diffusing, climbing, 90^o turning, and sequential transport), large-volume-range (V_Max/V_Min ≈ 100), and high-speed (≈22.86 mm s⁻¹) unidirectional microdroplet manipulation, which is ascribed to the rolling state on superhydrophobic slant microwall arrays (SMWAs) fabricated by the one-step femtosecond laser oblique ablation. The unidirectional transport mechanism relies on the variance of viscous resistance induced by the difference of contact area between the microdroplet and the slant microwalls. Furthermore, a circular, curved, and “L”-shaped SMWA is designed and fabricated for droplet motion with particular paths. Finally, sequential transport of large-volume-range droplets and chemical mixing microreaction of water-based droplets are demonstrated on the SMWA, which demonstrates the great potential in the field of microdroplet manipulation.