高效液相色谱法测定环孢素A含量

提出了高效液相色谱法测定环孢素A含量的方法。以Agilent Extend C18色谱柱(250mm×4.6mm,5μm)为固定相,以乙腈、水、叔丁基甲醚和磷酸按体积比500比500比50比1的混合溶液为流动相,用紫外检测器检测,检测波长为210nm。环孢素A的质量浓度在0.025～2.00g.L-1范围内与其峰面积呈线性关系。方法应用于环孢素原料药分析,测定结果的相对标准偏差(n=6)小于1.0%,用标准加入法做回收试验,回收率在99.3%～101%之间。     

高效液相色谱法测定透明质酸中乙二胺四乙酸

提出了高效液相色谱法测定透明质酸中乙二胺四乙酸(EDTA)含量的方法。用ZOR-BAX Eclipse XDB-C18(4.6mm×150mm,5μm)色谱柱分离,以乙腈-pH 6.5的100g.L-1四丁基氢氧化铵-水(20+20+60)混合溶液为流动相,用紫外检测器在波长260nm处测定。EDTA的质量浓度在0.037 2～1.86mg.L-1范围内呈线性,检出限(3S/N)为4.745μg.L-1。方法用于分析透明质酸样品,回收率在87.2%～93.6%之间,测定值的相对标准偏差(n=5)小于5%。     

电子能量对沿面介质阻挡放电等离子体化学产物的影响

基于光电倍增管研制了一套无触发信号的双通道光学探测系统, 并组装了测试样机, 实现了对沿面介质阻挡放电(SDBD)等离子体约化电场的测量, 进而通过BOLSIG+软件获得了电子能量. 采用原位紫外吸收光谱和傅里叶变换红外光谱, 研究了SDBD等离子体在不同电压和频率下的化学产物的浓度变化, 并结合空气等离子体化学反应揭示了产物相互作用的微观机理. 结果表明, 电子能量能够改变电子碰撞反应的速率系数, 调控化学反应的源头活性粒子的浓度, 进而影响到化学产物的生成和猝灭.     

Zr-MOF空心纳米球固载离子液体对CO2环加成反应的催化性能

通过后合成修饰方法(PSM)构筑了空心纳米球(Void@UiO-66-Ⅰ)和实心块(UiO-66-Ⅰ) 2种形貌的季铵盐功能化UiO-66-NH₂(Zr), 得到兼具酸碱活性位点和氢键给体的新型功能化金属-有机框架材料. 通过一系列表征证明2种催化剂的成功合成, 并将它们用于催化转化CO₂和氧化苯乙烯的环加成反应. 由于Void@UiO-66-Ⅰ催化剂的季铵盐部分含有大量的羟基和卤素阴离子, 可以通过氢键和亲核攻击与环氧化合物连接, 诱导环氧化合物开环, 促使反应顺利进行, 且催化剂的中空结构有利于物质进出催化剂, 起到加快反应速率的作用, 使得该催化剂在CO₂与氧化苯乙烯环加成反应中表现出比实心块UiO-66-Ⅰ催化剂更好的催化性能. Void@UiO-66-Ⅰ催化剂在120 ℃, CO₂压力为1.2 MPa, 反应时间为6 h, 无溶剂和助催化剂的反应条件下, 碳酸苯乙烯酯的收率和选择性分别为85.5%和95%.     

Recent advances in the improvement of g-C3N4 based photocatalytic materials

g-C₃N₄ have been widely used in the fields of photocatalytic hydrogen production,photocatalytic degradation of dyes and oxidative degradation of toxic gases due to their excellent performance.It has attracted extensive attention in recent years due to its highly efficient photocatalytic capacity of hydrogen generation,water oxidation,carbon dioxide reduction and degradation of organic pollutants.Because of the abundant carbon and nitrogen composition of the earth,large-scale production and industrial applications of this material are possible.The modification of this material makes its performance more excellent so that this new material can obtain a steady stream of vitality.These outstanding works have become important materials and milestones on the road to mankind's photocatalytic hydrogen production.This review will begin with the basic idea of designing,synthesizing and improving g-C₃N₄ based photocatalytic materials,and introduce the latest development of g-C₃N₄ photocatalysts in hydrogen production from four aspects of controlling the carbon/nitrogen ratio,morphology,element doping and heterojunction structure of g-C₃N₄ materials.     

基于CdSe/ZnS量子点薄膜结构的高双折射光子晶体光纤的色散与损耗控制

基于有限元法,设计了一种六边形排列含CdSe/ZnS量子点薄膜结构的高双折射光子晶体光纤,分析了具有不同厚度CdSe/ZnS量子点薄膜光子晶体光纤的色散及损耗特性.结果表明,含CdSe/ZnS量子点薄膜结构的光子晶体光纤在x和y方向均存在基模.当泵浦光波长逐渐增加时,具有相同厚度CdSe/ZnS量子点薄膜光子晶体光纤的双折射值逐渐增大,x和y方向总色散先增大后减小且存在两个零色散点,损耗逐渐增大并在可见光波段趋近于零;具有不同厚度CdSe/ZnS量子点薄膜光子晶体光纤随CdSe/ZnS量子点薄膜厚度的增加,在相同泵浦光波长处,双折射值逐渐减小,x和y方向总色散逐渐减小且两个零色散点逐渐靠近,损耗逐渐增大.通过沉积不同厚度CdSe/ZnS量子点薄膜和选择合适泵浦光波长,可有效控制光子晶体光纤的色散和损耗.     

Influence of fineness on the cementitious properties of steel slag

In this paper, the influence of fineness on the cementitious properties of steel slag and the properties of cement containing steel slag with different finenesses were investigated. The results show that increasing the fineness can significantly enhance the early as well as the late cementitious properties of steel slag. However, the early hydrations of cement and steel slag tend to hinder each other especially in the case of large steel slag replacement and high fineness of steel slag. Therefore, increasing fineness of steel slag cannot improve the early cementitious properties of the cement containing steel slag. At 28 days, the hydrations of steel slag and cement tend to promote each other. Increasing the fineness of steel slag enhances the late cementitious properties of the cement containing steel slag significantly.     

Comparing study on hydration properties of various cementitious systems

The hydration properties of slag sulfate cement (SSC), slag Portland cement (PSC), and ordinary Portland cement (POC) were compared in this study by determining the compressive strength of pastes, the hydration heat of binders within 72 h, the pore structure, the hydration products, and the hydration degree. The results indicated that main hydration products of PSC paste and POC paste are calcium hydroxide and C–S–H gel, while those of SSC paste are ettringite and C–S–H gel from the analyses of XRD, TG–DTA, and SEM. At the early curing age, the compressive strength depends on the clinker content in the cementitious system, while at the late curing age, which is related to the potential reactivity of slag. From hydration heat analysis, the cumulative hydration heat of PSC is lower than that of POC, but higher than that of SSC. Slag can limit chemical reaction and the delayed coagulation of gypsum, which also plays a role in the early hydration. So SSC shows the lowest heat release and slag can’t be simulated without a suitable alkaline solution. Based on MIP analysis, the porosity of POC paste is the smallest while the average pore size is the biggest. At the age of 90 days, the compressive strength of SSC can get higher development because of its relative smaller pore size than that of PSC and POC paste.     

反相高效液相色谱法同时测定壮阳类保健品中达泊西汀和4种PDE5抑制剂

提出了反相高效液相色谱法同时测定壮阳类保健品中4种PDE5抑制剂和达泊西汀含量的方法。样品溶于水中,再加甲醇提取。分取10μL提取液进样,并用Inertsil ODS-SP色谱柱为分离柱和由(A)三乙胺-乙酸-水(8+4+988)混合液,(B)乙腈和(C)0.02%(φ)磷酸溶液三者按不同比例相混的混合液作流动相进行梯度淋洗和分离。在检测波长290nm处进行测定。他达那非的质量浓度在1.25~25.0mg·L-1范围内与其峰面积呈线性关系,其余4种化合物的质量浓度在5.0~100mg·L-1范围内与其峰面积呈线性关系,方法的检出限(3S/N)在0.05~0.2mg·L-1之间。加标回收率在94.1%~109%之间,测定值的相对标准偏差(n=6)均小于1.0%。     

基于不同还原剂体系银粉的可控制备

以硝酸银为原料,在不同温度条件下,分别以无机和有机还原剂,制备了不同形貌的银粉颗粒,采用扫描电子显微镜以及X射线衍射对其形貌与结构进行了表征。在此基础上,重点研究了不同还原体系对银粉颗粒形貌的影响,并提出了相应的机理。研究结果表明,以七水合硫酸亚铁作为还原剂时,银颗粒形貌由铁离子浓度控制,在高浓度,低反应速度条件下可得到花状银颗粒。随着体系浓度的下降,表面由粗糙花状变为光滑球状,导电性能并随之升高。以抗坏血酸作为还原剂,硫酸根为保护剂时,硫酸根浓度对银粉形貌有着很大的影响,随着硫酸根浓度的增加,银颗粒由球形变为枝片状。导电性能有所升高。