Thermal analysis of renal stones

The chemical composition of 200 renal stones, collected from Taxila, Rawalpindi and Islamabad regions in Pakistan, was determined by thermogravimetric (TG) and differential thermal analysis (DTA) techniques. The thermal curves show weight losses at various temperatures indicating dehydration and decomposition phenomena of renal stones. Results were compared with qualitative data obtained by IR analysis which confirmed the chemical composition of various stones in the solid state. The thermal curves helped in the differentiation of various kinds of water held by stones and their chemical composition was obtained by weight loss during pyrolysis. It was found that 26.5% of the stones were pure whewellite, 3% weddellite, 13% uric acid anhydrous, 7.5% struvite, 2.5% ammonium acid urate, 0.5% cystine and 47% stones had mixed composition. In the mixed state the most frequent combinations were those of calcium oxalate with uric acid (14.5%) and with phosphates (27.5%).

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Zusammenfassung Mittels TG und DTA wurde die chemische Zusammensetzung von 200 Nierensteinen untersucht, die in den Gebieten Taxila, Rawalpindi und Islamabad in Indien gesammelt wurden. Die Thermogramme zeigen Masseverluste bei verschiedenen Temperaturen, die auf Dehydratation und Zersetzung der Nierensteine hinweisen. Die Ergebnisse wurden mit den qualitativen Resultaten aus der IR-Analyse verglichen, welche die chemische Zusammensetzung der verschiedenen Steine im festen Zustand bekräftigte. Die Thermogramme halfen bei der Unterscheidung von verschieden gebundenem Wasser, ihre chemische Zusammensetzung wurde durch Gewichtsverlust bei der Pyrolyse bestimmt. Man fand, daß 26.5 % der Steine aus reinem Whewellit bestanden, 3 % aus Weddellit, 13 % aus anhydrierter Harnsäure, 7.5 % aus Struvit, 2.5 % aus Ammmoniumhydrogenurat, 0.5 % aus Cystin und 47 % der Steine hatten eine gemischte Zusammensetzung. Die häufigsten Kombinationen der Mischzusammensetzungen waren Calciumoxalat mit Harnsäure (14.5 %) und mit Phosphaten (27.5 %).

     

两种以Znq2为基体的新型电致发光材料的合成与性能

以8-羟基喹啉为配体的金属配合物是一种性能优良的有机电致发光材料,其中有关8-羟基喹啉铝(Alq₃)研究已有大量报道,8-羟基喹啉锌(Znq₂)研究还有待发展。介绍了两种以Znq₂为基体的新型有机电致发光材料Znq₂(H₂O)₂和(Znq₂)₄的合成方法。用IR、XRD、TG、DTA和荧光测试方法进行表征与分析表明:Znq₂(H₂O)₂和(Znq₂)₄的玻璃化温度(T_g)分别为104.2℃和204.9℃;在161℃下Znq₂(H₂O)₂脱去水分子成为Znq₂,在361℃高温下四聚体(Znq₂)₄裂解为单体Znq₂;Znq₂(H₂O)₂和(Znq₂)₄具有很好的发光性能,在光致发光谱中λ_max分别是505,550nm。     

DTA and X-ray diffraction investigations of laser-irradiated CeO2 powders

The TG and DTA curves and diffractograms of powdered CeO₂ samples irradiated with a CO₂ laser beam with powers of 0.41–1.39 kW/cm² are presented. The laser treatment induced structural changes and probably generation of a metastable phase. X-ray diffraction coupled with thermal analysis was used to establish the structural modifications in the irradiated samples after heating.     

Thermoanalytical procedures to identify the morphology of polycrystalline materials

Polypropylenes of differing morphologies were examined by differential thermal analysis. The problems of reordering during the programmed heating are discussed. Four potential procedures by which the reordering could be inhibited are considered, and three of these are experimentally assessed. Their advantages and deficiencies are identified. Two pretreatments, an etching and a crosslinking, are recognised as able to qualitatively characterise the initial morphology, with a preference for the former. A test to identify the occurrence of reordering is identified. In celebration of the 60^th birthday of Dr. Andrew K. Galwey     

Activation energies for metastable to stable phase transition of 4,4'-di-n-heptyl- oxyazoxybenzene

Complexes of adenine, AdH, with cobalt, nickel and copper chlorides were prepared and their thermodynamic functions were determined. The complexing processes are endothermic in nature. The thermal behaviour of complexes was followed up by using TG and DTA analyses. The stoichiometry of thermal decomposition of the investigated complexes was suggested. This revised version was published online in August 2006 with corrections to the Cover Date.     

Monitoring hydration state conversion by TG-DTA

Characterization of the solid-state form (hydrate or polymorph) of a pharmaceutical active is a key scientific and regulatory requirement during development of and prior to seeking approval for marketing of the drug product. A variety of analytical methods are available to perform this task. By nature of the fundamental information it provides, TG-DTA offers advantages over other methods in regards to monitoring and quantitation of hydration state changes. In a single experiment with only a few milligrams of sample, TG-DTA perceives minor changes in phase, quantitates total water content and percent conversion, and illustrates hydrate type. All of this is accomplished without the necessity of generating time-consuming standard curves representing the differing ratios of hydrated to anhydrous forms. This study describes the use of TG-DTA to monitor and quantitate humidity induced solid–solid phase conversion of nitrofurantoin and risedronate. Percent conversion was qualitatively observed by both TG and DTA signals and quantitated by the TG.     

Thermal evolution of ferromagnetic metallic glasses

A traditional TG apparatus was modified by placing two permanent magnets producing a controlled magnetic field (TG(M): Magneto Thermogravimetry). This technique proved to be useful to study both structural relaxation and crystallisation of ferromagnetic metallic glasses. Results obtained for the amorphous alloys Fe₄₀Ni₄₀P₁₄B₆ and Fe_62.5Co₆Ni_7.5Zr₆Nb₂Cu₁B₁₅, are reported in this paper. Structural relaxation can be evaluated by measuring changes in Curie temperature induced by thermal treatments. Crystallisation in TG(M) is detected through a change in the measured apparent mass (difference between the sample mass and magnetic force driving it upward). These results were confirmed by DSC analysis. Whether the obtained crystalline phase is ferromagnetic, it can be identified through its Curie temperature, measured by TG(M). In fact the value of 770°C measured as Curie temperature of crystallised Fe_62.5Co₆Ni_7.5Zr₆Nb₂Cu₁B₁₅led to conclude that the only ferromagnetic crystalline phase is a-Fe. These hypothesis was confirmed by XRD analysis, showing that the first crystallisation yields to a-Fe nanocrystals. This revised version was published online in July 2006 with corrections to the Cover Date.     

Thermal analysis of anhydrous and hydrated Cholesterol

Cholesterol constitutes the major component of most gallstones. It was identified and determined, in gallstones, issued from eleven patients, by thermal analysis: differential scanning calorimetry (DSC), with the use of the melting temperature and enthalpy, thermogravimetry (TG), with the mass loss of water. Anhydrous cholesterol (ChA) was characterized by two endothermic peaks (polymorphic, melting) and cholesterol monohydrate (ChH) by two endothermic peaks (dehydration, melting), too. Cha needle and Chh plate crystals were observed under polarizing light microscopy. The numerous stones obtained from nine patients were cholesterol stones: the ChA was higher 45 and lower 96%. ChH was present in stones of three patients. This revised version was published online in July 2006 with corrections to the Cover Date.     

五硼酸钾部分高温特性的研究

研究了高温下水蒸汽及氯化钠或氯化钾对五硼酸钾的影响。借助自行设计的反应器与XRD、Raman光谱分析高温水蒸汽气氛下五硼酸钾的结构变化，证明了无论在其熔融态还是固态都会与水蒸汽发生反应，使产物中的K₂O含量升高，B₂O₃与水结合从五硼酸钾中脱离。利用DTA、XRD分析绘制了KB₅O₈-MCl（M＝K、Na）体系熔度图，属简单低共熔型，低共熔点分别为x_KCl=50%、 742 ℃，x_NaCl=20%、 689 ℃。     

差热分析(DTA)法研究五水硫酸铜的失水过程

关于五水硫酸铜的失水过程有不同的说法。归纳起来,主要有以下几种:1.五水硫酸铜的失水过程分三步进行,即