无水磷脂DHPC的相变及水含量影响的DSC研究

利用差示扫描量热法,研究了无水及含水的1,2-双正十七烷酰基磷脂酞胆碱(DHPC)的相变特性.实验发现,无水DHPC初次受热时,首先发生玻璃态转变,接着像通常的晶体一样熔化.因此是玻璃性晶体.从熔体中结晶的DHPC是通常的晶体.从可以冻结水的总熔化培Q_f和水含量h的关系断定:在含水DHPC中,水可以存在于3种热力学上可区分的状态.第1种是不可冻结水,它是与磷脂头基直接结合的水,是一级水合水.每个头基最多可结合7个这样的水分子.第2种是二级水合水,其熔点接近于纯水但其比熔比焓dQ_f/dh比纯水的低.每个DHPC分子最多可保有约6个这样的水分子.当h再增大时,体系中有熔点及比熔化焓接近于纯水的体相水.实验发现,h增加,DHPC熔化峰向低温方向移动;当h>16.2%时,其凝胶-液晶相变温度T_tr及相交焓面△H_tr基本上不随h变化.T_tr、△H_tr及相变熵△S_(tr)的实验值和从偶数碳酰基磷脂酰胆碱同系物中得到的Huang(1981)方程组的计算值吻合.     

不同实验条件对DSC峰形的影响以及相变温度的确定

本文通过深入分析实际的ＤＳＣ过程，阐述了ＤＳＣ曲线上各个特征点以及这些点所对应的物理意义。在理论上分析各种不同的实验条件对ＤＳＣ曲线形状的影响，指出目前在ＤＳＣ分析中所用的确定试样熔点的方法以及用高纯金属ＤＳＣ变曲线上熔融峰峰前沿的斜率修正试样相变温度所存在的问题，指出ＤＳＣ相变曲线刚开始偏离基线的那点所相应试样盒的温度即为试样的熔点，本文还提出了通过提高试样，试样盒以及试样支座之间的热导率，来提     

磷脂DHPC和短杆菌肽D相互作用的DSC研究

Changes of the behavior of the thermotropic phase transitions of the phospholipid DHPC by the action of miniprotein gramicidin D (G.D) have been studied by differential scanning calorimetry. The experimental results demonstrated that G.D could not remove the pretransition of DHPC, but the pretransition peak and the main transition peak of DHPC were incorporated into a broad peak. The pretransition temperature and the main transition temperature of DHPC decreased to different ex-tent. The sums of the pretransition and main transition enthalpies of DHPC showed a lineally decreasing relationship with increasing the mole fraction x_g of gramicidin D.     

过量水中脑磷脂假二元系相变的DSC研究

运用差示扫描量热法研究了过量水中脑磷脂 (DMPE和DHPE)假二元系的凝胶 液晶相变 ,给出该假二元系的相图 .实验表明 ,至少在DHPE的摩尔分数低于0 1时可能出现部分相分离现象 .理想溶液模型分析表明 ,既在凝胶相 ,又在液晶相 ,这两个脑磷脂都不理想混溶 ;正规溶液模型分析表明 ,凝胶相的非理想性参数更大     

Eu3+对DMPC人工膜脂双层主相变温度的影响

利用付里叶变温红外光谱和核磁共振谱研究了Ｅｕ３＋离子与人膜ＤＭＰＣ脂双层配位作用的影响，实验发现Ｅｕ３＋离子对ＤＭＰＣ脂双层影响不局限于界面区域，而且扩展到整个酰基链，因而使ＤＭＰＣ脂双层的主相变温度提高了６℃。     

癸二醇和十二烷二醇及其混合物的液固相变研究

使用差示扫描量热法（DSC）和红外光谱法（IR）对1,10-癸二醇（1,10-C10H22O2,A）与1,12-十二烷二醇（1,12-C12H26O2,B）及其二元混合物系统液固相变进行研究。测定了该二元混合系统的相变温度、相变焓和液固平衡相图。该二元系统存在低共熔混合物,其组成为xB=0．333,低共熔温度为328K。该二元混合系统的IR图谱显示存在氢键缔合现象,长链烷烃中的亚甲基在晶格中是有序规则排列的。该系统具有较低的相变温度和较高的相变焓,是一种潜在的低温储能材料。     

Eu3＋对DMPC人工膜脂双层主相变温度的影响

利用付里叶变温红外光谱和核磁共振谱研究了Eu     

Eu3+和Al3+离子对DPPC人工膜脂双层主相变温度的影响

天然生物膜组成复杂,直接用于研究困难较大.由于天然生物膜中脂分子的行为与人工脂双层膜的行为十分类似,故我们用单一磷脂制备人工脂双层膜来研究金属离子对其主相变温度的影响.     

固态磷脂相变行为的红外和拉曼光谱研究

用红外和拉曼光谱方法在２９０～４０５Ｋ的温度范围内考察了无水二肉豆蔻酰磷脂酰乙醇胺的分子构象随温度的变化。结果表明，该磷脂在３６５Ｋ附近的熔化相变过程中，不仅酰链的构象和堆积发生了有序－无序转变，而且极性头部基团和接界区域基团也发生了结构重排；逆相变过程中，烷基链构象重新恢复了有序，但头部基团和甘油骨架构象没有恢复原始有序状态。     

Study of Calcium Sulfate Crystallization by the Differential Scanning Calorimetry

The state of water in calcium chloride and sodium sulfate solutions, as well as during the crystallization of calcium sulfate from solutions with concentrations of 0.68–7.08 g dm^–3 was studied by the differential scanning calorimetry. One clearly detectable endothermic peak was revealed in the DSC curves of ice melting of CaCl₂ and Na₂SO₄ solutions. An increase in the concentration of these solutions does not lead to the appearance of any additional peaks or shoulders on the DSC curves. Thermograms for sodium sulfate and calcium chloride mixed solutions change their patterns: a low-temperature peak appears and peaks with asymmetric shoulders or splitted principal peak are registered. These changes are presumably related to the water structuring by the surface of forming calcium sulfate crystals.     

DSC法研究液晶物质2-(4-烷氧苯基)6-取代苯并噻唑的相变热性质

The phase transitions of a new group of mesogens, 2-(4-alkoxyphenyl)-6-substituted benzothiazoles were thermodynamically studied by DSC, and their transition temperatures and enthalpy changes were measured, from which the transition entropy changes were calculated. The results obtained were discussed. In addition, the phe-nomenon of super-cooling of the compounds were quantitatively observed.     

Investigations of the Sub-Ambient Transitions in Frozen Sucrose by Modulated Differential Scanning Calorimetry (MDSC®)

40% w/w sucrose/water solutions were analyzed by Modulated Differential Scanning Calorimetry [1] in the sub-ambient temperature region. At these temperatures, the solutions exhibit a complex, two-step thermal event. The lower-temperature event is believed to be the glass transition of the amorphous sucrose phase. The nature of the higher-temperature event is the subject of controversy. This event has been shown to have distinct second-order characteristics, and as such is believed to be a second T_g. Others feel that this event is the onset of melting. The temperature region between these events contains a devitrification exotherm. Through the use of MDSC, both in scanning and stepwise quasi-isothermal modes, improved sensitivity and resolution of MDSC provides new insight into the nature of these transitions.This revised version was published online in November 2005 with corrections to the Cover Date.     

Study on the Stability of GaF3-based Glasses by Differential Scanning Calorimetry

The glass formation and devitrification of GaF₃-based glasses were studied by differential scanning calorimetry. A comparison of various simple quantitative methods to assess the level of stability of multicomponent fluoride glass systems is presented. Most of these methods are based on critical temperatures. In this paper a new parameter k _b(T) is added to the stability criteria. The stability of several GaF₃-based glasses were experimentally evaluated and correlated with the activation energies of crystallization via this new kinetic criterion and compared with those evaluated by other criteria. This revised version was published online in August 2006 with corrections to the Cover Date.     

Study by Differential Scanning Calorimetry of Water-in-Oil Emulsions Stabilized by Clays and CTAB

In this work, we have tested various formulations in order to get emulsions containing pure water, Tunisian olive oil, Tunisian clays, and an ammonium salt. Two different types of clays: smectite and kaolinite and the cethyltrimethylamonium bromide (CTAB) were tested. CTAB is used as surfactant and a compound modifying the clays properties. The amount of CTAB being fixed at 0.66 w/w, the proportions of clays were varied from 0 to 9% for each of the following proportions of water: 10, 20, 30%. To the aqueous phase obtained by mixing two separate aqueous phases: water + CTAB and water + clay, the oil was added drop by drop, the agitation being maintained at 5000 rpm. The obtained mixtures were analyzed by Differential Scanning Calorimetry (DSC), optical microscopy and bottle tests. An optimized formulation containing water (30%), smectite clay (5.3%) and CTAB (0.66%) was found to give W/O emulsions which kinetic stability is greater than 75 days regarding coalescence and greater than 700 hours regarding sedimentation.     

甘露醇纯度的差示扫描量热法测定

使用差示扫描量热法(DSC)对甘露醇纯度进行测定。密封式铝坩埚封装样品,最佳实验条件为升温速率约0.7℃·min-1,样品量约2.5mg,氮气流速为20～40mL·min-1;纯度测定的RSD为0.016,纯度准确测定的下限为98%,通过F检验及t检验,该方法与药典法无显著差异。该方法简便、快速、准确,适合甘露醇等高纯度药品的纯度测定。     

High-Resolution Calorimetry: New Perspectives for the Study of Phase Transitions

Only 7 pg of substance are needed to measure solid–solid phase transitions in n-alkanes with a new type of calorimeter (see schematic picture). This corresponds to a transition heat of only 500 pJ. The small time constant of the calorimeter additionally permits the observation of dynamic effects in the examined phase transitions.     

示差扫描量热法进展及其在高分子表征中的应用

示差扫描量热法(DSC)是表征材料热性能和热反应的一种高效研究工具,具有操作简便、应用广泛、测量值物理意义明确等优点.近年来DSC技术的发展大大拓展了高分子材料表征的测试范围,促进了对高分子物理转变的热力学和动力学的深入研究.温度调制示差扫描量热法(TMDSC)是DSC在20世纪90年代的标志性进展,它在传统DSC的线性升温速率的基础之上引入了调制速率,从而可将总热流信号分解为可逆信号和不可逆信号两部分,并能测量准等温过程的可逆热容.闪速示差扫描量热法(FSC)是DSC技术近年来的创新性发展,它采用体积微小的氮化硅薄膜芯片传感器替代传统DSC的坩埚作为试样容器和控温系统,实现了超快速的升降温扫描速率以及微米尺度上的样品测试,使得对于高分子在扫描过程中的结构重组机制的分析以及对实际的生产加工条件的直接模拟成为可能.本文从热分析基础出发,依次对传统DSC、TMDSC和FSC进行了介绍,内容覆盖其发展历史、方法原理、操作技巧及其在高分子表征中的应用举例,最后对DSC未来的发展和应用进行了展望.本文希望通过综述DSC原理、实验技巧和应用进展,帮助读者加深对DSC这一常用表征技术的理解,进一步拓展DSC表征高分子材料的应用.     

Literature Status on Temperature-Modulated Differential Scanning Calorimetry

Journal of Thermal Analysis and Calorimetry -     

差示扫描量热法测定除草剂绿麦隆的纯度

研究了用差示扫描量热法(DSC)测定绿麦隆的纯度。该法测定最佳条件为升温速率0.5 K.min-1,样品量2~3 mg,保护气流速20 mL.min-1。用本法测得绿麦隆原药的纯度为98.35%,相对标准偏差(RSD)为0.034%,测定结果与已知纯度相符。并将测定结果与高效液相色谱(HPLC)法进行了比较。该法具有操作简便,样品用量少,准确度和精密度均较高等优点。