超高效液相色谱-串联质谱法同时检测糕点中6种甜味剂

目的建立超高效液相色谱-串联质谱法同时测定糕点中6种常用合成甜味剂的分析方法。方法选用超纯水作为提取溶剂,涡旋和超声提取后,低温离心,取部分上清液加入正己烷除脂,Waters Atlantis■T3色谱柱、甲醇-5 mmol/L甲酸铵(含0.1%甲酸)作为流动相、亲水亲脂平衡型固相萃取柱HLB(hydrophile-lipophile balance)净化。结果6种甜味剂在质量浓度为10~200 ng/mL的曲线范围内呈良好线性关系,相关系数r均大于0.999,平均加标回收率在85.0%-98.2%之间,相对平均偏差(relative standard deviation,RSD)为1.3%~6.7%。结论该方法具有前处理简单、灵敏度高、检测速度快等优点,适合糖精钠、甜蜜素、三氯蔗糖、阿斯巴甜、阿力甜、纽甜的检测,但不适用于安赛蜜的检测。     

Effects of structural parameters on water film properties of transpiring wall reactor

Corrosion and salt deposition problems severely restrict the industrialization of supercritical water oxidation. Transpiring wall reactor can effectively weaken these two problems by a protective water film. In this work, methanol was selected as organic matter, and the influences of vital structural parameters on water film properties and organic matter removal were studied via numerical simulation. The results indicate that higher than 99% of methanol conversion could be obtained and hardly affected by transpiration water layer, transpiring wall porosity and inner diameter. Increasing layer and porosity reduced reactor center temperature, but inner diameter's influence was lower relatively. Water film temperature reduced but coverage rate raised as layer, porosity, and inner diameter increased. Notably, the whole reactor was in supercritical state and coverage rate was only approximately 85% in the case of one layer. Increasing reactor length affected slightly the volume of the upper supercritical zone but enlarged the subcritical zone.     

Effects of Ti,Y, and Hf additions on the thermal properties of ZrB2

Reactive hot pressing was utilized to synthesize and densify four ZrB₂ ceramics with impurity contents low enough to avoid obscuring the effects of dopants on thermal properties. Nominally pure ZrB₂ had a thermal conductivity of 141 ± 3 W/m K at 25 °C. Additions of 3 at% of Ti, Y, or Hf decreased the thermal conductivity by 20 %, 30 %, and 40 %, respectively. The thermal conductivity of (Zr,Hf)B₂ was similar to ZrB₂ synthesized from commercial powders containing the natural abundance of Hf as an impurity. This is the first study to demonstrate that Ti and Y additions decrease the thermal conductivity of ZrB₂ ceramics and report intrinsic values for thermal conductivity and electrical resistivity of ZrB₂ containing transition metal additions. Previous studies were unable to detect these effects because the natural abundance of Hf present masked the effects of these additions.     

生物可降解PCL/PLA开孔发泡材料制备及吸油性能

以聚己内酯（PCL）为基体，添加不同含量聚乳酸（PLA）熔融共混制备具有不同分散相形态的PCL/PLA共混物，利用超临界二氧化碳（scCO₂）微孔发泡工艺制备不同发泡倍率和开孔率的PCL/PLA多孔材料用于吸油应用。针对边长3 mm正方体样品溶解度实验发现100 min后CO₂在PCL中已达到饱和吸附状态。PLA分散相含量的增加显著增大了PCL/PLA共混物泡孔密度，并使共混泡孔尺寸减小且分布更加均匀；发泡温度升高6℃，泡孔尺寸增大50%，发泡倍率增大38%，开孔率减小了20%。PCL/PLA开孔材料具有明显的亲油疏水性，发泡倍率越高，疏水性越好；针对花生油和硅油的吸油实验发现材料吸油率与发泡倍率和开孔率整体呈正比，实际吸油量高于理论计算值，10次循环吸油测试后样品吸油率仅降低8.5%，材料吸油量与油品特性黏度关系不大。     

超临界流体萃取技术生产重交通道路沥青的研究

研究了采用超临界流体萃取技术(SFEF),以减压渣油和催化裂化油浆为原料,制备重交通道路沥青产品的可行性.结果表明:当原料中油浆掺入量为10%～30%时,可以生产出牌号为AH70,AH90,AH110的重交通道路沥青产品.工业试验表明,生产牌号为AH70,AH90的重交通道路沥青,采用此技术方案是可行的.     

甘油三乙酸酯超临界酯交换反应及其动力学研究

研究了在超临界条件下甘油三乙酸酯与甲醇或乙醇的酯交换反应,分别考察了超临界状态下醇油摩尔比和温度对反应的影响。实验结果表明,甲醇或乙醇与甘油三乙酸酯的摩尔比为14、反应温度为350℃、反应时间为20m in时,乙酸甲酯或乙酸乙酯的收率分别达100%和60%。对超临界状态下动力学的研究结果表明,甘油三乙酸酯与甲醇或乙醇的酯交换反应为拟一级反应,在相同的反应条件下,采用甲醇时酯交换反应速率比用乙醇时快,相应的甘油三乙酸酯的转化率也高;甘油三乙酸酯在超临界甲醇或乙醇中酯交换反应的表观活化能分别为58.7 kJ/mol和75.1 kJ/mol,甘油三乙酸酯与甲醇酯交换反应的活化能低于与乙醇酯交换反应的活化能,表明碳链短的醇更易进行酯交换反应。     

Analysis of supersaturation and nucleation in a moving solution droplet with flowing supercritical carbon dioxide

A supercritical antisolvent (SAS) process is employed for production of solid nanoparticles from atomized droplets of dilute solution in a flowing supercritical carbon dioxide (SC CO₂) stream by attaining extremely high, very rapid, and uniform supersaturation. This is facilitated by a two‐way mass transfer of CO₂ and solvent, to and from the droplet respectively, rendering rapid reduction in equilibrium solubility of the solid solute in the ternary solution. The present work analyses the degree of supersaturation and nucleation kinetics in a single droplet of cholesterol solution in acetone during its flight in a flowing SC CO₂ stream. Both temperature and composition are assumed to be uniform within the droplet, and their variations with time are calculated by balancing the heat and mass transfer fluxes to and from the droplet. The equilibrium solubility of cholesterol with CO₂ dissolution has been predicted as being directly proportional to the Partial Molar Volume Fraction (PMVF) of acetone in the binary (CO₂–acetone) system. The degree of supersaturation has been simulated up to the time required to attain almost zero cholesterol solubility in the droplet for evaluating the rate of nucleation and the size of the stable critical nuclei formed. The effects of process parameters have been analysed in the pressure range of 7.1–35.0 MPa, temperature range of 313–333 K, SC CO₂ flow rate of 0.1136–1.136 mol s^?1, the ratio of the volumetric flow rates of CO₂‐to‐solution in the range of 100–1000, and the initial mole fraction of cholesterol in acetone solution in the range of 0.0025–0.010. The results confirm an extremely high and rapid increase in degree of supersaturation, very high nucleation rates and stable critical nucleus diameter of the order of a nanometre. Copyright © 2005 Society of Chemical Industry     

连续式超临界流体萃取进卸料装置

概括了超临界流体萃取技术和包括连续式操作在内的超临界流体萃取装置的研究现状 ,提出了一种通过球形进、卸料器完成固相物料超临界流体萃取连续化进卸料的装置 ,介绍了该装置的结构和工作原理 ,给出装置中各主要部件的计算方法。