Study of soils by thermal analysis

The study of soils is very important in the geological and geological engineering researches. A study of ten samples of soils was carried out by thermal analysis, and X-Ray Fluorescence Spectrometry to understand soil evolution in Angra dos Reis region, Rio de Janeiro State, Brazil. The sample collection sites were chosen based on geological characteristics, the soil layer thickness, the soil composition pattern, and whether or not it was moved either by erosion or by gravitational shifts. Because of the humid tropical climatic condition, natural soils tend to show great thickness of weathered mantles with formation of saprolites and saprolite soils. Kaolinite is an important secondary mineral which can be formed from many different minerals, like k-mica and k-feldspar and can be weathered to gibbsite. The results from TG/DTG and DTA indicated which soils had more weathering, and the same results were obtained by XRF, when silica/aluminum ratios from samples are compared with thermal analysis results.     

头发中无机元素分析方法及应用的研究进展

人体无机元素含量在头发中较其它体液或组织中高,易于检出。头发能够存储较长的时间信息,并且能提供其空间信息。通过分析其中的无机元素含量和同位素比例,可以说明元素在体内特定时间的变化以及反映人体的地理位置迁移。综述了头发中无机元素分析的前处理和仪器分析方法,重点介绍头发中无机元素分析在环境、医学及法医学研究中的应用,并对未来的技术发展和应用进行展望。     

Coordination chain polymeric assemblies of trivalent lanthanides with multidentate Schiff base synthetic, spectral investigation and thermal aspects

The coordination chain polymers of La(III), Ce(III), Pr(III), Nd(III) and Sm(III) with N,N’-di(o-thiophenyl)terephthalaldehydediimine have been prepared and characterized by elemental analysis, ¹H NMR, ¹³C NMR, magnetic measurements, infrared spectra, reflectance spectra and thermogravimetric analysis. A coordination number of seven around the metal ion is suggested. The thermal decompositions of the coordination polymers have been studied. The kinetic parameters have been calculated using Freeman-Carroll method. The thermodynamic activation parameters such as entropy (S*), preexponential factor (A), enthalpy (H*) and free energy of the decomposition (G*) have been evaluated.     

Literature survey on thermal analysis reference materials

Results of a literature search on thermal analysis reference materials are listed

---

Zusammenfassung Vorliegend werden die Ergebnisse einer Literaturrecherche über Referenz-substanzen für die thermische Analyse dargelegt.

     

The characterization of the thermal behaviour of inorganic fluorides using quasi-static thermoanalytical methods

Quasi-static thermal analysis is very useful for the characterization of the thermal behaviour of inorganic fluorides. The strong dependence of the thermal decomposition of hydroxonium fluorometallates, monofluorophosphates, and ammonium fluorometallates on the partial pressure is demonstrated. Non-reciprocal quasi-isobaric investigations are specially suitable to disclose this behaviour. The possibilities of characterization of the reaction mechanism using quasi-static thermal analytical methods as well as the use of these methods as synthetic variants for phase-pure fluorides are demonstrated by further examples. In this context the repression of the amount of hydrolysis products is discussed.

---

Zusammenfassung Quasi-statische thermoanalytische Methoden sind sehr gut für die Charakterisierung anorganischer Fluoride geeignet. Am Beispiel der termischen Zersetzung von Hydroxoniumfluorometallaten, Monofluorophosphaten und Ammoniumfluorometallaten wird der starke Einfluss von Partialdruckänderungen demonstriert. Besonders wichtig sind quasi-isobare, nicht-reziproke Verfahren für die Untersuchung dieses Verhaltens. An Beispielen wird auch die Möglichkeit der Reaktionsaufklärung mit quasi-statischen thermoanalytischen Methoden gezeigt. Die gleichen Methoden eignen sich darüber hinaus als Synthesevariante für phasenreine Fluoride. In diesem Zusammenhang werden die Möglichkeiten der Herstellung von Fluoriden mit geringem Hydrolysegrad ausführlich diskutiert.

     

Oxyreactive thermal analysis

The paper presents the applicability of Oxyreactive Thermal Analysis (OTA) for the investigation of different kinds of carbon matter. For comparative reasons and more precise interpretation, along with OTA some physico-chemical properties of analyzed materials were used as the methods commonly applied for the investigations. The carbon materials of both natural (anthracites, graphite and diamonds) and synthetic origin (active carbon, glass carbon, expanded graphite, soot and synthetic diamonds) were investigated. It was stated that there is close relationship between structure parameters and physico-chemical properties and the thermal reactivity within the investigated groups of carbon matters. The results show that OTA can be accepted as a good investigative way for such materials. This revised version was published online in July 2006 with corrections to the Cover Date.     

A reexamination of the degradation of polyvinylchloride by thermal analysis

Degradation of polyvinylchloride has been reexamined in the light of its DT-DSC-TG analytical behavior up to a temperature of 1000°C in an inert atmosphere. Four distinct stages of degradation have been identified. The first stage is almost eventless with no change in weight for untreated PVC samples. The second stage is almost exclusively dehydrochlorination. The third stage appears to be a structural reorganization involving such processes as cis-trans isomerization, aromatization, and crosslinking. The fourth stage appears to be a structural degradation and is associated with the evolution of hydrocarbons. The role of liberated hydrogen chloride has been better appreciated in catalyzing the above secondary reactions on the polyene residue obtained on partial or total dehydrochlorination. The effect of the particle dimension and chemical and physical pretreatments of the samples, such as low temperature dehydrochlorination by an alkali and vacuum heat treatment, respectively, on the degradation pattern has been studied. © 1994 John Wiley & Sons, Inc.     

Study on electro-conductance and thermal analysis of lithium carnallite

Lithium carnallite is a hydrated double salt containing lithium and magnesium chlorides. The processes of thermal dehydration and thermal decomposition of lithium carnallite during heating has been studied by the conductance-thermoanalysis which was designed according to Berg and-Wendlandt, and an interpretation of the conductance-thermoanalytical curve has been suggested.     

Differential thermal analysis of montmorillonite

The paper provides an overview of publications on the DTA of montmorillonites (in the temperature range 20–1100°C), starting with the first experiments of Le Chatelier (1887) and ranging up to the present. Consideration is given to the dehydration, dehydroxylation, amorphization and rehydration of montmorillonite (42 references).     

Synthesis,characterization, and thermal studies of cardanol-based polyphosphate esters

Polyphosphate esters were synthesized from derivatives of cardanol phosphorodichloridateates and dihydric phenols by interfacial polycondensation using a phase transfer catalyst. The polymers were characterized by IR, ¹H-, ¹³C-, and ³¹P-NMR spectroscopy, and GPC. The thermal stability and thermal degradation kinetics of the polymers were determined by thermogravimetry. The flammability of the polymers was evaluated by limiting oxygen index values. © 1993 John Wiley & Sons, Inc.     

Polymer melting and polymer powder sintering by thermal analysis

Sintering of polymeric powders is a peculiar characteristic of many processing technologies, including rotational moulding and selective laser sintering (SLS). During polymer sintering, viscosity reduction in the melt state promotes densification of polymer powders, through a double stage mechanism, involving powder coalescence and bubble removal. In particular, sintering of semi-crystalline polymers is strongly influenced by the melting behaviour. Nevertheless, melting itself in absence of pressure is not necessarily accompanied by powder sintering, unless low viscosities are achieved. In this work, the melting and sintering behaviour of recycled high density polyethylene (rHDPE) have been analysed through differential scanning calorimetry (DSC) and Thermomechanical Analysis (TMA). Efficient models capable of describing the melting temperature distribution and rate of sintering of rHDPE powders have been developed, highlighting the inherent differences between the two distinct processes. This revised version was published online in July 2006 with corrections to the Cover Date.     

Optimization of firing parameters for ceramic wares by thermal analysis

Aesthetic and utilitarian properties of traditional ceramic wares as well as engineering properties of modern advanced ceramics are attained by maintaining an optimum temperature-time-atmosphere relationship, called firing schedule, in the kiln. The contribution of modern thermal analysis (TA) techniques such as TG/DTG, TG/EGA, TG/MS, DTA, DSC, TDA, etc. in 1) optimizing production steps by raw material quality control, by studying binder burn out, product densification, 2) in simulating appropriate preheating, firing and cooling schedules as well as 3) in developing shorter firing cycles has been extensively reported in recent literature. The paper will first discuss theoretical curves and energy required for ceramic firing and present from the literature selected examples of applications of thermal analysis in ceramic technology.     

Solid-state Compounds of 4-chloro-benzylidenepyruvate With Lanthanides. Preparation and thermal studies

Solid-state compounds Ln-4Cl-BP, where Ln represents lighter trivalent lanthanides and 4Cl-BP is 4-chlorobenzylidenepyruvate, were prepared. Thermogravimetry, derivative thermogravimetry (TG and DTG), differential scanning calorimetry (DSC) and other methods of analysis were used to characterize and to study the thermal behaviour of these compounds. This revised version was published online in July 2006 with corrections to the Cover Date.     

Advances in nano thermal analysis of coatings

This article discusses AFM-based localized thermal analysis of crosslinked polymer coatings based on a recent breakthrough in nanoscale thermal probe technology. The addition of a thermal tip to a conventional AFM adds a new and valuable capability of spatially resolved thermal analysis to the AFM. It is particularly useful for thin films since it enables the measurement of transition temperatures (melting (T _m) or glass (T _g)) on selected regions of the sample aiding in the identification and characterization of phases on the length scales approaching macromolecular dimensions. Examples include the monitoring of the softening point of automotive clearcoat systems, as a function of cure time and cure temperature and characterization of degradation and embrittlement of weathered acrylic-polyurethane coatings. Comparison of nano thermal analysis with bulk DSC and MDSC is made and its inherent advantages over DSC in analyzing surfaces, is demonstrated.     

Study of the NaBr–DyBr3 phase diagram by differential thermal analysis

The phase diagram of the quasi binary NaBr–DyBr₃ system was determined by differential thermal analysis (DTA) applied to 27 samples covering the complete composition range of the system. The 3NaBr*DyBr₃(s) compound is present in the solid-phase in addition to the pure component halides NaBr(s) and DyBr₃(s). The DyBr₃(s) and 3NaBr*DyBr₃(s) phases showed a polymorphic transition at 1112 and at 733 K, respectively. The {DyBr₃(s) + 3NaBr*DyBr₃(s)} eutectic mixture melts at 709 K giving a liquid of the molar composition x(NaBr) = 0.62. The 3NaBr*DyBr₃(s) phase melts peritectically at 765 K. The phase diagram obtained in the present study virtually agrees with the calculated one available in literature.     

Techniques of thermal analysis applied to the study of cultural heritage

It is increasingly important that chemistry reaches people who have not studied directly this field of science but that, daily, have practices where chemistry is involved in various extents. This is what happens, for instance, in the activities related with the study and the preservation of cultural heritage. In this sense, the present work is a short review of the particular case of techniques based on the thermal analysis and calorimetry applied within the context of the characterization of art and archeological objects, exemplified by various case studies, as the characterization of mortars, preparatory grounds, ancient painting materials and drying oils.     

火焰原子吸收法测定鸡尾木中无机元素的含量

鸡尾木(ExcoecariaVenenataS.LeeetF.N.Wei)属大戟科,海漆属,为民间药用珍贵植物,用于治疗牛皮癣、慢性湿疹等,疗效颇佳[1]。鸡尾木中无机元素,尤其是医学微量元素的测定对其药理效的研究有重要的参考价值。1　实验部分1 1　仪器及试剂TAS 986原子吸收分光光度计(北京普析通用仪器有限责任公司);空心阴极灯:Fe、Cu、Ni、Cr、Cd、Zn、Co、Ba、Ca(北京瑞利普光电器厂);Mg、Pb(北京真空电子技术总公司);Mn(北京市朝阳天宫电器厂);AdventurerTM电子天平(奥豪斯国际贸易〈上海〉有限公司)。标准储备液:配制Zn2+、Mg2+、Fe3+、Mn2…     

混合高级醇固-液相变储热材料的研究

相变储热材料研究与开发是国内外的一个新兴领域[1-6]。为了解决一些仪器的内部散热问题,本文研究了混合高级醇固-液相变储热材料的凝固和熔化特性、相变焓值、固液相体积以及石墨粉对材料的导热性能。1实验部分1·1试剂与仪器CDR-1型差动热分析仪-配微机处理系统,上海天平仪器     

Applications of thermal analysis in some solid-state reactions

TG-DTG-DTA has been used to characterize various isomers of CoCl₂·2(CH₃C₆H₄NH₂). Thermal analysis is further used to analyse the binary mixtures of these isomers. DTA recorded after different elapsed times follows the progress of reaction between cobalt chloride and benzocaine where progressively small endotherms are associated with starting materials. The application of thermal analysis to following the solid-solid reactions between metal acetates and 8-hydroxyquinoline was highlighted. The stoichiometry of such reactions was confirmed from the decrease in intensity of an endotherm as one increases the stoichiometry.Thanks are due to Drs. Keshav Chander, K. Kaur, Rajinder Singh and G. S. Chopra for helpful discussions and experimental work.