基于特级初榨橄榄油两种不同特性的DSC掺假分析方法研究

该文基于油脂物理特性与氧化稳定性2种特性,利用差示扫描量热法(differential scanning calorimetry,DSC)对市面上常见的特级初榨橄榄油(extra virgin olive oil,EVOO)中大豆油掺假问题进行研究。在物理特性方面,采用DSC冷却曲线来分析EVOO掺假。随着大豆油掺假比例升高,油样在-40~-60℃结晶焓值ΔH由EVOO的29.78 J/g减小为40%掺假混合油的6.133 J/g,对EVOO质量比构建的一元回归方程Y=57.556X-28.44(R2=0.997)。在氧化稳定性方面,氧化温度160℃下,不同油样诱导氧化时间随大豆油掺假比例上升逐渐变短,由EVOO的25.8 min逐渐减小为40%掺假混合油的17.8 min,Y=-19.4X+25.64(R^(2)=0.996),掺假模型相关性较好。这2种DSC检验掺假分析方法都能有效鉴别EVOO中大豆油的掺假且各有特点,可根据实际情况选取合适的方法更好处理EVOO掺假问题。

DIFFERENTIAL SCANNING CALORIMETRY AND X-RAY DIFFRACTION STUDIES ON AGING BEHAVIOR OF Zn-Al ALLOYS

Decomposition processes of the quenched Zn-Al alloys were studied by differential scanning calorimetry (DSC), X-ray diffraction (XRD) and transmission electron microscopy (TEM). The results show that the stabilities of supersaturated solid solution (SSS) of Zn-Al alloy and α' phase formed by quenching would reduce with the increase of Zn content and the precipitation of η-Zn phases even when aging at ambient temperature, so that the exothermic precipitation peak in DSC curve would disappear. The activation energy of the η-Zn precipitation and the reaction enthalpy were calculated and measured. The kinetics of α' decomposition or η-Zn formation was determined by XRD. The microstructure change during aging was observed by TEM.

Synthesis kinetics of Mg_2Sn in Mg-Sn powder mixture using non-isothermal differential scanning calorimetry

The non-isothermal heating process of Mg-Sn powder mixture was studied by differential scanning calorimetry(DSC) technique and the synthesis kinetics of Mg2Sn was evaluated by the model-free and model-fitting methods.The activation energy and conversion function of Mg2Sn synthesis reaction are calculated to be 281.7 kJ/mol and g(α)=[-ln(1-α)] 1/4,respectively.The reaction mechanism of 2Mg+Sn→Mg2Sn under non-isothermal condition is regarded as "nucleation and growth" .During the non-isothermal heating process,the phase transformation occurred in the Mg-Sn powder mixture was analyzed by XRD and the microstructure evolution of Mg2Sn was observed by optical microscopy,which is in good agreement with the reaction mechanism of 2Mg+Sn→ Mg2Sn deduced from the kinetic evaluation.

Studies of the Energy Release of Mitochondria from Sporophyte Cytoplasmic Male Sterile Rice by Differential Scanning Calorimetry

The differential scanning calorimetric (DSC)curves of the mitochondria isolated from two varieties of sporophyte cytoplasmic male sterile and their fertile lines of Yie Bai and Ma Xie type rice have been determined. The curves show that the energy is released continuously as temperature rise to 70℃. Some thermodynamic and kinetic parameters of the energy release of the mitochondria have been obtained. The presented results showed that the mitochondria from cytoplasmic male sterile rice released more heat and they had higher energy barrier, less rate, and more complicated mechanism than that of their fertile lines in the energy release process.

Measurement of Crystallinity of Acrylic Copolymer by Swelling Differential Scanning Calorimetry

In this paper the measurement of crystallinity(C)ofacrylic copolymer(PAC),by Swelling Differential Scan-ning Calorimetry(SDSC)is discussed.Common DSC isonly used for measuring the crystallinity of polymers withmelting point,(T_m),below their decomposition temper-ature,(T_d).As temperature rises,polymers with swell-ing agent added become swollen and dissolved,goingthrough whole process of breaking solid structures.Thus,SDSC makes it possible to measure the crystallini-ty of polymers even with T_d below T_m.But the C mea-sured by WAXD and the total endothermal melting(swelling)heat in SDSC thermograms,(△H_l),are notlinearly correlated.It has been found that,instead of the△H_l,△H_l’obtained from the △H_l by subtracting the en-dothermal heat,△H_l,and the C measured by WAXDare linearly correlated.On the basis of this linear rela-tion,the unknown C of another PAC sample is measuredby SDSC.The result is in good accordance with thatmeasured by WAXD.

Comparison between Glass and Stainless-Steel Vessels in Differential Scanning Calorimetry Estimation

Differential scanning calorimetry (DSC) provides easy screening for thermal hazard evaluation. Here, we investigate the difference between using glass and stainless-steel vessels on the DSC measurement of exothermic decomposition energy (QDSC) for 41 chemical substances (containing nitro, halogen, peroxide, and sulfur groups, and hydrazine bonds). Two borosilicate glass vessels (capillary and ampule) and one stainless-steel vessel were used. All QDSC values obtained were investigated with reference to the permissible fluctuation range specified by the ASTM (American Society for Testing and Materials) international Both glass vessels produced very similar QDSC values, despite different sample scales. The QDSC values obtained with the glass vessels were generally roughly within the variation tolerance range of the stainless-steel vessel. Notable exceptions were halogen- or sulfur-containing compounds;these exhibited smaller QDSC values with glass vessels in almost all cases. We will investigate whether certain structures in compounds react with stainless steel. The vessel material choice is crucial in evaluating the true reactivity of a substance.

Application of Single Scan Differential Scanning Calorimetry Technique for Determination of Kinetic Parameters of Crystallisation in Se-Sb-Ag

A single scan has been performed in Differential Scanning Calorimetry (DSC) at a heating rate of 15oC/min under non-isothermal conditions to investigate the crystallization kinetics of glassy Se90Sb10-xAgx alloys (where x = 2, 4, 6, 8). For this purpose, Handerson’s theory based on non-isothermal method for thermal analysis of single-scan DSC data has been used. The activation energy of crystallization and order parameter has been determined and composition dependence of these parameters has been discussed.

Thermal Diffusivity and Thermal Conductivity of Epoxy-Based Nanocomposites by the Laser Flash and Differential Scanning Calorimetry Techniques

Nanocomposites were fabricated by using a commercial two part epoxy as a matrix and multiwalled carbon nanotubes, graphite fibers and boron nitride platelets as filler materials. Multiwalled carbon nanotubes (MWCNTs) that were produced by chemical vapor deposition were found to produce nanocomposites with better thermal diffusivity and thermal conductivity than the MWCNTs that were produced by the combustion method. Compared to the MWCNTs produced by both methods and graphite fibers, boron nitride produced nanocomposites with the highest thermal conductivity. Specific heat capacity was measured by using differential scanning calorimetry and thermal diffusivity was measured by using the laser flash.

DSC法测定PET/PTT混纺产品中PTT纤维含量的不确定度评定

文中以差式扫描量热法(DSC)测定PTT(聚对苯二甲酸丙二醇酯)纤维含量为实验依据,分析实验过程中的不确定度来源并进行具体量化,得出差式扫描量热仪系统误差和热量求积是不确定度主要来源的结论。DSC法测定PTT纤维含量的相对扩展不确定度为3.58%(k=2)。根据笔者在实验室长期检测的经验,给出提高检测结果准确性的建议。

Application of differential scanning calorimetry to study the interpretation on herbal medicinal drugs:a review

Background:Differential scanning calorimetry as a method of investigating and monitoring the kinetics of herbal medicinal plants.Some instrumental and experimental aspects are discussed.Methods:A brief survey is made of herbal medicinal plants and results of differential scanning calorimetry studies are reviewed and this discussion is presented the effects of the instrumental conditions like heating rate and the sample conditions like sample particle size,sample mass,sample purity,sample stability in the melting region and property of impurities.Conclusion:This study suggests that application of differential scanning calorimetry to study the interpretation on herbal medicinal drugs.

牛、羊乳粉的DSC热学性质比较及掺假分析

为明确羊乳粉、牛乳粉的热学特征,采用差示扫描量热法(differential scanning calorimetry,DSC)对真空冷冻干燥制备的全脂羊、牛乳粉样品以及高比例掺假(75%、50%、25%)和低比例掺假(10%、5%、3%、1%)牛乳粉的混合羊乳粉样品进行热力学分析。结果表明,全脂羊乳粉和全脂牛乳粉在DSC热学指标上存在差异,全脂牛乳粉相比全脂羊乳粉缺失一个脂肪特征熔融吸热峰b,蛋白质熔融吸热峰c峰值温度和热焓值较低,而乳糖熔化分解峰e热焓值较高。对于掺入不同比例牛乳粉的羊乳粉,通过检测是否存在吸热峰b及其热焓值,可判断样品掺假牛乳粉比例是否在25%以下及判断掺入牛乳粉的量;在不同比例掺假样品中检测乳糖熔化分解峰e的焓值可判断羊乳粉掺入牛乳粉的掺假量。因此,DSC技术可以实现对羊乳粉、牛乳粉热学性质的分析和评价,也可作为乳制品行业质量保证和真实性鉴别的潜在分析工具。

ATR-FTIR结合DSC法快速鉴别食品接触用塑料包装制品

研究了一种衰减全反射红外光谱(ATR-FTIR)结合差示扫描量热法(DSC)快速鉴别食品接触用塑料包装制品单一材质的方法。红外光谱图能准确反应塑料制品的内部结构,结合DSC曲线得出其具体成分。该方法快速、准确且几乎不破坏样品。

城市生活垃圾热解特性的TG-DSC分析

Seven typical components in municipal solid wastes (MSWs)--paper,food,textile,wood,straw,plastic and rubber were chosen as the thermogravimetric analysis samples in this paper to study the pyrolysis characteristics. By the thermogravimetry and differential scanning calorimetry (TG-DSC) analysis,pyrolysis characteristics of MSWs’ components and pyrolysis endothermal enthalpy were obtained.The kinetic parameters of pyrolysis were determined with the Doyle method and a multi-stage first order pyrolysis model was proposed.The simulated results by this model showed good agreement with the TG experimental data.The pyrolysis characteristics provide significant parameters to a new concept of circulating fluidized bed incinerator,which can simultaneously restrain the high-temperature HCl corrosion and emission of dioxins.

DSC对苯基苯酚改性酚醛树脂固化机理研究

采用DSC技术、Kissinger法对苯基苯酚改性酚醛树脂的固化过程进行了研究,得到放热峰顶活化能为169.3 kJ/mol,远大于普通酚醛树脂(约70 kJ/mol)。理论近似凝胶温度、固化温度及后处理温度分别为414.5 K、448.9 K和483.9K。酚醛树脂的固化通常由化学反应控制和扩散控制两阶段组成。通过Ozawa法得到活化能与转化率(E-a)的变化关系表明,2种树脂固化历程存在明显差异。普通酚醛树脂固化反应进行到10%(a=10%),粘度迅速增大,反应转向扩散控制;而苯基苯酚改性酚醛树脂固化反应时粘度变化小,直至a=70%,才较快增长。这将有利于小分子的逃逸和各基团充分反应。同时高活化能也表明,反应形成了高键能的化学键,有利于提高树脂的残炭率和烧蚀性能。

DSC法测定生物质的比热

将DSC技术应用于5种林业废弃物及低温热解焦炭的比热测定,通过分析标准样——刚玉(Al2O3)与生物质样品在升温过程中的吸热特性,可得到样品的比热,同时利用前人经验公式进行了对比分析。生物质样品的比热为1.55～1.62 J/(g.℃),焦炭的比热为0.83～0.99 J/(g.℃),与文献报道一致,这也证明了DSC测定生物质比热的可行性。

四硝基并哌嗪(TNAD)与推进剂组分相容性的DSC法评估

采用差示扫描量热法(DSC),研究了四硝基并哌嗪(TNAD)与奥克托今(HMX)、黑索今(RDX)、二硝基哌嗪(DNP)、1.25/1-NC/NG混合物、3-硝基-1,2,4-3-己基铅(NTO-Pb)、铝粉(13.8μm)和吉钠(D INA)等含能组分的相容性;同时也研究了TNAD与聚乙二醇(M=10000)、二异氰酸酯(N-100)、2-硝基二苯胺(2-NDPA)、1,3-二甲基-1,3-二苯基脲(C2)、炭黑(C.B.)、三氧化二铝(A l2O3)、2,4-二羟基苯甲酸铜(β-Cu)、己二酸铜(AD-Cu)和邻苯二甲酸铅(φ-Pb)等惰性材料的相容性。研究表明:TNAD与NC+NG、RDX、NTO-Pb和PET相容性较好;与D INA、HMX轻微敏感;而对2-NDPA,φ-Pb,-βCu,AD-Cu和A l2O3等惰性材料敏感,与DNP、PEG,N-100,C2和C.B.等不相容。由此可见,TNAD能与推进剂主要组分相容,可在NC+NG体系的改性双基推进剂中应用。

冷冻干燥过程中溶液冻结特性的DSC研究

利用差示扫描量热仪(DSC)研究了蔗糖水溶液的冻结特性,分析了溶液浓度和热历史对冻干过程的影响。DSC实验结果表明,过冷度和最大冻结浓缩溶液的玻璃化转变温度Tg’均与热历史有关;降温时溶液中的水分能否充分结晶受浓度和降温速率的共同影响。降温过程中的结晶热可用来确定溶液降温后的冻结水含量以及最大冻结浓缩溶液中的水分含量。

DSC方法在特级初榨橄榄油掺假鉴别中的应用

采用差示扫描量热法(DSC)对进口特级初榨橄榄油中葵花籽油的掺假鉴别进行了系统研究。由橄榄油入手考察了升降温循环实验条件下油品的重复性及数据可靠性,以此为基础提出采用程序降温的方法研究油品的结晶特性。统计了研究体系内的8种特级初榨橄榄油、6种其他食用油以及5种比例的模拟掺假油的结晶峰温度值,建立了回归方程。结果表明:进口特级初榨橄榄油在-60^-46℃区间内具有尖锐的结晶峰;随着掺入葵花籽油比例的升高,模拟掺假油的结晶温度逐渐向低温区移动,结晶峰形由尖锐逐渐变平坦;由结晶起始温度和结晶峰值温度分别相对于掺假油体积分数建立的回归方程具有很好的相关性,可以快速准确地鉴别特级初榨橄榄油。

牛半腱肌肉结缔组织胶原蛋白热力特性热诱导变化DSC分析(英文)

探讨牛半腱肌肉结缔组织胶原蛋白热力特性的热诱导变化。牛半腱肌肉分别采用水浴和微波加热到内部终点温度分别为40、50、60、70、80℃和90℃,研究结缔组织滤渣和热力特性在热处理过程中的变化。结果表明:结缔组织滤渣含量随着热处理温度的升高而增加,当加热温度分别为60、70℃和80℃时,结缔组织滤渣含量在两种热处理方式间存在显著差异(P<0.05)。在两种热处理方式中,40℃至60℃的内部终点温度是影响结缔组织胶原蛋白热收缩温度的关键加热温度。热诱导的结缔组织胶原蛋白热力特性的变化是水浴和微波加热牛肉胶原蛋白热收缩温度存在差异的主要原因。

NiTi形状记忆合金加热相变过程的DSC研究

采用差示扫描量热法研究了时效处理对N iTi形状记忆合金加热相变过程的影响规律。结果表明:当时效温度低于T0(特征转折温度)时,相变温度(AS和Af)随时效温度的升高而升高;当时效温度高于T0时,相变温度随时效温度的升高而下降。对于AS,当时效15m in时,T0=500℃,当时效30m in时,T0=400℃;对于Af,T0均为400℃。在300℃、400℃和500℃时效15m in,加热相变过程为M→R和R→P两阶段,在600℃和700℃时效15m in时,加热相变过程为M→P一阶段;当时效时间延长至30m in时,加热相变过程由M→R和R→P两阶段相变过程变为M→P一阶段。时效温度为500℃和700℃时,体积转变率与温度关系曲线的斜率较大。