优化作业方式提高始极片质量

针对某厂铜电解种板工序存在的始极片质量波动较大的问题,从种板系统体积控制和添加剂匹配的角度出发,分析各种因素对始极片质量的影响,做出了相应的改进措施,使种板系统运行更加稳定,始极片质量得到进一步提升。     

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。     

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.     

高效液相色谱法测定多环芳烃的出峰顺序探讨

目的探讨水﹑气﹑土壤中多环芳烃检测标准(HJ 478-2009﹑HJ 647-2013、HJ 784-2016)的正确出峰时间和顺序。方法用高效液相色谱来对苊烯、芴、苊、?、苯并(a)蒽进行定性分析,并与3个标准中的出峰顺序进行比较。结果苊烯、苊、芴、苯并(a)蒽、?的出峰时间分别为6.450、7.923、8.233、17.760、18.740min,与标准HJ478-2009﹑HJ647-2013的出峰顺序存在差异。结论在使用标准HJ478-2009﹑HJ647-2013、HJ 784-2016同时测定16种多环芳烃时,多环芳烃的出峰顺序及时间应以HJ 784-2016为准。     

环形通道内液态铅铋合金流动换热特性实验研究

通过对环形通道内液态铅铋合金的流动换热特性进行实验研究，得到了气泡泵注气对液态金属流动的影响，并拟合出环形通道内液态铅铋合金的摩擦系数关系式和换热特性关系式。结果表明：采用气泡泵注气能有效提升铅铋合金的质量流速；相同Reynolds数下环形通道内液态铅铋合金的摩擦系数大于由布拉休斯公式计算得到的摩擦系数；液态铅铋合金对流换热过程中，导热项占主导地位，并且Nusselt数随Peclet数的增大而增大。     

Liquid Marble Patchwork on Super-Repellent Surface

Liquid marble (LM) is a droplet that is wrapped by hydrophobic solid particles, which behave as a non-wetting soft solid. Based on these properties, LM can be applied in fluidics and soft device applications. A wide variety of functional particles have been synthesized to form functional LMs. However, the formation of multifunctional LMs by integrating several types of functional particles is challenging. Here, a general strategy for the flexible patterning of functional particles on droplet surfaces in a patchwork-like design is reported. It is shown that LMs can switch their macroscopic behavior between a stable and active state on super-repellent surfaces in situ by jamming/unjamming the surface particles. Active LMs hydrostatically coalesce to form a self-sorted particle pattern on the droplet surface. With the support of LM handling robotics, on-demand cyclic activation–manipulation–coalescence–stabilization protocols by LMs with different sizes and particle types result in the reliable design of multi-faced LMs. Based on this concept, a single bi-functional LM is designed from two mono-functional LMs as an advanced droplet carrier.     

[Zr0.73(Cu0.59Ni0.41)0.27]87Al13合金过冷液相区热塑性成形研究

为探究[Zr_(0.73)(Cu_(0.59)Ni_(0.41))_(0.27)]_(87)Al_(13)非晶合金的热塑性成形性能以及绘制其对应的热加工图谱,用Gleeble3500型热模拟压缩实验机对该非晶合金进行不同参数下的热模拟压缩实验。结果表明,合金在压缩过程中变形行为由牛顿流变演变为非牛顿流变;同时,过高或过低的热加工温度均能导致合金晶化;进一步对数据分析得到该合金在不同热塑性成形参数下的功率耗散图与流变失稳图,并绘制出相应的热加工谱图,谱图分析结果表明,该合金在温度为420与430℃、应变速率为10~(-3) s~(-1)时具有较高功率耗散系数且没有失稳区域,因此,合金可选的热塑性加工参数为温度420～430℃,应变速率10~(-3) s~(-1)。     

液相色谱法快速检测染色梅鱼中日落黄、柠檬黄的含量

目的建立一种快速、低成本检测染色梅鱼中日落黄、柠檬黄的方法。方法将染色梅鱼剥皮,鱼皮经70%甲醇氨水提取液提取,经EclipseXDB-C_(18)色谱柱分离,以甲醇和乙酸铵水溶液为流动相,进行梯度洗脱,流速为1.0 mL/min,柱温35℃,利用紫外检测器检测日落黄、柠檬黄的含量。结果日落黄、柠檬黄在1.25、2.5、12.5、25 mg/kg添加水平的加标回收率为80%～90%,相对标准偏差小于10%(n=6),柠檬黄检出限为0.05 mg/kg,日落黄检出限为0.025 mg/kg。结论该方法快速、准确、成本低,适合染色梅鱼中日落黄、柠檬黄的快速检测。     

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