The surface energetics of a powder plays an important role in the ease of preparation, stability and dissolution of pharmaceutical products. Existing techniques for assessing surface energetics of powders (i.e. liquid penetration and contact angles) suffer from practical and theoretical limitations as well as being somewhat subjective. The objective of this study was to evaluate the data obtained by microcalorimetric techniques from which ?H and other kinetic parameters of adsorption can be determined. Results were supplemented by data obtained by vacuum microbalance methods.

A common technique for sampling organic solvents in workplace air is the use of preconcentration of vapors on adsorbents. The most widely used adsorbent is activated carbon, due to its large sampling capacity. After desorption (thermal or displacement by other solvents such as carbon disulfide), analysis is made by gas chromatography. In order to avoid breakthrough, the collected amount is usually <10% of the maximum capacity (total pore volume).

在经济快速发展进程，对化学品的生产及使用逐渐走向多样化、大量化、复杂化，化学品的性质也趋于复杂及高危害性。失控反应最终可能导致火灾、爆炸甚至外泄等安全议题，造成巨大的生命财产损失，因此也日益受到关注。国家十三五规划中也表明应提供安全生产的工作环境，建立良好之物质管理体系，有效推动灾害防范；充分知悉工作场所危害物质的特性及危害，并依各项安全规定工作，维持生产安全。本文与国际知名热分析厂家美国TA仪器合作，浅谈在国际上及个人研究经验对热分析技术研究失控反应的案例介绍及心得。

对高分子材料常常用熔体流动速率（熔融指数MI）表示材料熔体的流动性，这种测试完全忽略了材料的流动模型，所以对每一个被研究的材料所施加应变历史都不相同。这种单点的数值是粘性和弹性共同贡献的结果。这种完全经验的数值完全没有定义确定的变形，一般而言仅仅作为材料的等级或窗口数值。由于其测量方法的限制，它不可能区分粘性和弹性。很多情况下具有同样MI的材料却表现出截然不同的加工性能。所以熔体流动速率（MI）测试只能用于质量控制，它无法提供材料的基本性能信息或于加工过程相关联。 不过在控制应力/应变流变仪上的动态测试对材料流动行为可以提供非常有价值的信息。流变仪可以通过单一实验准确的测得弹性和粘性响应。 我们研究的样品为三种硬质PVC样品，分别以A，B和C样品来标记。每一种样品PVC样品在稳定剂类型和浓度及基本PVC树脂类型等方面均有明显的不同。

热分析技术在橡胶领域应用得越来越广泛，本文简要介绍了示差扫描量热仪DSC、热重分析仪TGA、动态力学分析仪DMA和热机械分析仪TMA的基本原理和在橡胶领域的应用实例。

Conventional transducers measure the strain in a compliant member and based on their stiffness, determine the torque resp. normal force (Fig. 1a). This method has several inherent disadvantages. Since the compliant member is strained, the strain has to be accounted for in determining actual sample strain. In dynamic the inertia of the moving mass of the transducer, affects the measured results at high frequences. Further, viscoelastic materials which develop normal forces, drive the cone and plate apart. This effect generates secondary flow fields and the result is an inaccurate transient normal force measurement. To overcome these problems of conventional transducer, all developments have been made towards stiffer transducers. The stiffness however is directly related to the resolution of the strain measurement of the compliant member i.e. the torque resp. force measurement. This implies that the stress resolution decreases with increasing stiffness.

Linear viscoelastic measurements are often taken for granted. Many users are not aware that systematic errors such as instrument compliance may significantly corrupt the test results, especially at high frequency when the sample becomes stiff in comparison to the instrument itself. Instrument compliance effects can be demonstrated, when running high modulus materials in different size plate geometries. Figure 1 shows the complex modulus of PIB measured at -20°C using 8mm and 25mm plates. With increasing frequency, the complex modulus of the test run with 25mm plate geometry deviates significantly from the result obtained with the 8mm plate geometry. In the same graph, the measured sample deformation is plotted versus frequency. While the strain amplitude for the test performed with 8mm parallel plates is virtually constant and close to the 2% command value, does the actual sample strain for the tests performed with 25mm plates, decrease with frequency. This shows that for these tests, the deformation amplitude applied by the actuator is not fully transferred onto the sample. The smaller the sample strain in relation to the command strain, the higher the compliance effect of the instrument.

传统的旋转流变仪是在理想流动条件（黏度流动）下工作的，使用板、椎板或同心圆筒表征复杂材料，尤其在线性黏弹区域更好。但往往复杂流体在这种条件下最难测量的。测试或滑动过程中采样工具界面上的沉降有明显的效果，且能够减少仪器的操作范围。 Traditional rotational rheometry has been dealing with ideal flow conditions (viscometric flows) using plate, cone-plate or concentric cylinder geometries to characterize complex materials, preferably in the linear viscoelastic region. Complex fluids, however are often difficult to measure under these conditions. Sedimentation during testing or slippage at the sample-tool interface have a significant effect on the results and reduce the operation range of the instruments. ?Furthermore do viscoelastic flows by no means represent the real flow situation in batch or continuous reactors and processing machines during mixing and/or incorporation of additives, etc. For example, in order to simulate and to understand the gelatinization of starch, a mixing element is used as the standard geometry to avoid settling of the non soluble starch particles since the early days of rheological testing.

由导电性颗粒和非导电液体混合而成的电流变液的微观结构状态在有无外电场作用差异巨大，从而表现出显著不同的流变特性。这类体系有着广泛应用前景，对电流变液流变特性的系统表征有十分重要的意义和实用价值，TA仪器最新研制的电流变附件是研究这类流变的理想工具。

拉伸流变仪的根是是在20世纪初被发现的。Trouton在测试沥青和鞋匠所用蜡时，在这些材料上进行“扭转”和“牵引”变形。通过巧妙的实验他发现，单轴拉伸黏度是剪切黏度的三倍。

在当今日益激烈的竞争环境下，高性能先进材料的开发尤为重要。许多材料制造商不在专注于单一产品领域，而是越来越趋向于多元化。以至于现在开发研究实验室经常研究一系列有明显的不同物理和化学性质的材料。因为这个原因，分析仪器必须非常灵活，它必须能够容纳存在各种各样的物理状态的样品且不影响其灵敏度和重现性。动态力学分析（DMA）也不例外，本文将讨论使用DMA测量系列材料的粘弹性特征，包括液体、聚脂薄膜、乳胶、预浸料坯和复合材料。

分析流变学是确定材料微观结构从而测量粘弹性响应的学科。分析流变学是分析化学在相同意义上与其他作为其他分析方法基础上的流变性能测试的延伸。固有粘度分析技术是一种分析流变学。分析流变学可适用于任何材料系统的流变响应，这种响应很大程度上取决于微观结构分析。?

流变光学是指将光学技术应用于变形系统的结构、取向和压力测量。光学测量可以是对流变力学测试的一个重要的补充，因为他们可以帮助理解表现在聚合物和胶体材料上的机制控制的流动性能。光学分析模块OAMII采用偏振测定或测量光的偏振，以确定在主体流动和变形材料的折射率的各向异性。与流变仪相反，光学方法不需要接触材料，且可以专注于极小体积的材料的测试。

震荡中的流变测量无论在应力还是应变通常都会形成强烈的信号。随着材料复杂度的增加，在样本测试中更加需要能够覆盖广泛范围的样品弹性模量（个和应力及应变）。对于动态范围由于106的，必须消除随机噪声和系统误差修正，以确保准确的结果。高速数据采集与灵活的相关技术结合，以提高低端性能流变仪。

从1970到1980，美国对塑料的需求从200亿磅增加到了500亿磅。塑料的成功主要是由于其广泛的应用，由于其广泛的性能，塑料可以替代金属、玻璃、陶瓷、纸张、天然纤维、包装材料、消费产品、管道、家具，等等…… 塑料最重要的性能在于其重量轻，耐破损，能巩固功能部件，想对便宜，易于自动化生产，生产成本较低……

ARES DETA（介电配件）是一种扩展ARES应变控制流变仪测试能力的配件，包括材料介电响应的研究。这种能力探测所测材料的导电和电容性能，扩大了ARES流变仪作为表征材料性能的通用仪器的应用范围。

粉末涂料是一种先进的提供装饰和保护的方法，广泛应用于各种材料领域以及同时适用于工业客户和普通消费者。加工过程中使用的粉末是一种颜料和树脂混合物，可喷到表面涂层。带电粉末粒子年粘附在接地表面，直至在固化炉中加热和通话呈平滑涂层。

一般炸药和推进剂的稳定性和兼容性的调查需要远远超出了讨论范围。 在过去的100多年里，硝基一直被用作推进剂，设定了大量的测试来调查其稳定性。大多数的这些测试在本质上都很非常简单和实证的。然而，在过去10年左右的时间里，现代分析方法已被引入炸药领域，且常与旧方法一起使用。现代研究方法提供了有关该组分研究的更真实信息，但其结果是稳定的、兼容的且保持复杂混合物的稳定性，这在推进剂研究中是不容易的。

本文运用热分析分析热塑性材料的物理性质。热分析是一系列的传统测量技术用于确定材料特性随温度的变化的技术。对两个工程热塑性塑料的短期和长期的物理性质研究的实验结果表明，热分析对描述热塑性材料的物理性质很有家价值。

热机械分析仪（TMA）历来都是被用来测量固体材料的尺寸变化。然而，这项技术也可扩展到评估液体样品上，提供一种替代差示扫描量热仪（DSC）确定相变和玻璃化转变温度的方法。

本文详细介绍了目前国内国外常用的热物理性质数据的手册和数据库，以及查阅和使用中的单位换算和注意事项。供广大设计人员，材料研究和开发人员，测试人员参考使用。

? 安全 ? 您再也不需要液氮或其他冷却气体，远离窒息、冻伤或其他危险 ? 方便 ? 再不需要采购、更换、填充液氮， 只要有电，您的ACS永远候命 ！ ? 小巧 ? ACS将节约您36% 到 75% 的实验室空间 ? 安静 ? 有效和耐久的设计带给您完全可以被忽略的噪音. ? 物超所值 ? ACS只需要您2-3年的液氮消耗成本*（取决您的实际液氮消耗情况）

该附件是在原DMA上增加了一个密封的样品室，额外增加一个湿度发生及控制器，从而使温度达到5°C–120°C，湿度达到5-95%。从而使材料耐受严酷的温湿度双85考验成为可能！

In the past few decades calcium sulfate based building products have become materials of choice for various interior construction purposes, The basis of gypsum technology is the ability of gypsum to transform into various calcium sulfates (hemihydrale, anhydrite) when being heated. When hemihydrate or anhydrite is mixed with water calcium sulfale dihydrate is formed again due to re-hydralion. During re-hydration of hemihydrate, the following exothermic reaction occurs:

Solution calorimetry measures the heat of solution of a solid dissolving into a solvent. Hogan & Buckton (2000) have shown there is a measurable difference in the enthalpies of solution between the amorphous and crystalline form of a material. Typically, the dissolution of a crystalline material is an endothermic process and exothermic for an amorphous material. Such an ability to differentiate between the amorphous and crystalline form of a material is important to formulators of solid dosage forms for drug delivery. In all of these forms the assessment of the order or possible disorder associated with the solid material is vital for stability and compatibility testing. Generally the presence of amorphous material influences the physical integrity and usually the kinetics of degradation. Often, only a small amount of amorphous material can produce severe effects on the stability of a particular formulation.

Since the introduction of the first commercial (temperature servo) device for quantitatively measuring heat flow into (or out of) a sample as it undergoes a transition, there has been considerable confusion about what name should be used to describe this analytical measurement (1). A wide variety of labels has been applied including Quantitative Differential Thermal Analysis (QDTA) (1,2,3), Dynamic Differential Calorimetry (DDC), Dynamic Enthalpic Analysis (DEA) and, of course, Differential Scanning Calorimetry (DSC). DSC has been the most accepted name largely because instrument manufacturers have used the term. With the introduction of other commercial devices, which also measure differential heat flow but are not based on the temperature servo approach , the confusion has increased. This confusion has been aggravated by the instrument manufacturers themselves who have often claimed unspecified advantages for their particular instrument. The manufacturer of the original commercial device, understandably, has attempted to limit the DSC definition exclusively to his design. He continues to claim that his instrument is the only “true DSC”.?

The purpose of this paper is to assist DSC users with interpretation of unusual or unexpected transitions in DSC results. The transitions discussed in the paper are several of the ones that most frequently create problems for the new user, and which can also fool even an experienced thermal analyst. By applying some of the recommended procedures and solutions, most laboratories will be able to improve the overall quality and interpretation of DSC results.

Two common problems in the TG-DTG analysis of unknown elastomer vulcanizates and probable solutions are discussed. The first problem concerns the difficulty in quantitatively determining the oil and elastomer in the compound in cases where their volatilization temperature range overlaps. After a review of the published works which studied this problem, isothermal TG (with or without vacuum) along with the use of "High Resolution" TG equipment is recommended. The second problem concerns separate determination of carbon residue from the elastomers and added carbon black in the compound, which very often oxidizes together. Subtraction of the carbon residue formed by the elastomers, determined by previous analyses, from the total weight loss in oxygen, was suggested in the literature. However, the quantity of char depends on type of the elastomer, as well as its concentration, curative type and amount and rate of heating. The problem is not, therefore, fully resolved. Experiments under slow feed of lean oxygen gas and isothermal temperature were also suggested in the literature. Under this condition, oxidation of carbon black and char may occur at slightly different temperatures and overlapping is minimized. However, this could be achieved only for large and medium particle size blacks (soft blacks) which oxidize at higher temperatures and not for the smaller particle size blacks, (used mostly in tire treads). Further work under slow feed of lean oxygen with a superimposed isothermal program and/or vacuum is recommended. The capability of the recently announced "High Resolution Thermogravimetric Analyzer" should also be explored.?

Differential Scanning Calorimetry (DSC) is used to measure heat flow into or out of a sample as it is exposed to a controlled thermal profile. DSC provides both qualitative and quantitative information about material transitions such as the glass transition, crystallization, curing, melting, and decomposition. For some of these transitions, DSC can provide not only the temperature at which the transition (reaction) occurs and how much total heat is involved, but DSC can also provide valuable information about the rate (kinetics) of reaction. Furthermore, with the advent of easy-touse computer based data analysis programs, the ability to obtain such kinetic information has become more practical.?

Manufactures have been listening. In growing numbers, they have been hearing the rising voices of dissatisfied customers, outspoken consumer advocates, government watchdogs, and litigious lawyers. The message: The public wants products that work, that last a reasonable length of time, and that are safe to use.?