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  • 1
    Electronic Resource
    Electronic Resource
    Amsterdam : Elsevier
    Journal of Pharmaceutical and Biomedical Analysis 12 (1994), S. 889-893 
    ISSN: 0731-7085
    Keywords: IR spectroscopy. ; Mefloquine hydrochloride ; X-ray diffraction ; polymorphism ; solid-state investigation ; thermal analysis
    Source: Elsevier Journal Backfiles on ScienceDirect 1907 - 2002
    Topics: Chemistry and Pharmacology , Medicine
    Type of Medium: Electronic Resource
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  • 2
    Electronic Resource
    Electronic Resource
    Springer
    Journal of thermal analysis and calorimetry 9 (1976), S. 241-250 
    ISSN: 1572-8943
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Résumé On a étudié à l'aide d'un Derivatograph, sous diverses conditions, la réaction de mélanges binaires et ternaires des carbonates alcalins avec l'oxyde d'aluminium. L'identification des produits formés a été effectuée par diffraction des rayons X. Si les mélanges binaires et ternaires de carbonates contiennent du carbonate de lithium, il se forme toujours 1'α-métaaluminate de lithium, qui, à température plus élevée, se transforme en la formeγ. Si la carbonate de lithium est utilisé seul, on peut obtenir aussi l'ortho-dialuminate.
    Abstract: Zusammenfassung Die Reaktionen binärer und ternärer Alkalikarbonatmischungen mit Aluminiumoxid wurden mittels eines Derivatographen unter verschiedenen Bedingungen untersucht. Die Reaktionsprodukte wurden durch Röntgendiffraktion identifiziert. In Gegenwart Li2CO3-haltiger binärer und ternärer Karbonatmischungen war das Produkt stets α-Lithium-meta-aluminat, das bei höheren Temperaturen in dieγ-Form überging, während bei Einsatz von Li2CO3 auch Orthodialuminat erhalten werden konnte.
    Notes: Abstract Reactions of binary and ternary alkali metal carbonate mixtures with aluminium oxide were studied by means of a derivatograph under different conditions. Reaction products were identified by X-ray diffraction. In the presence of binary and ternary carbonate, mixtures containing Li2CO3 the product was alwaysα-lithium metaaluminate, transforming to theγ-form at higher temperatures, while using only Li2CO3 the orthodialuminate could be obtained too.
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  • 3
    Electronic Resource
    Electronic Resource
    Springer
    Journal of thermal analysis and calorimetry 48 (1997), S. 515-525 
    ISSN: 1572-8943
    Keywords: cyclodextrin ; mandelic acid ; stability constant ; stoichiometry ; UV photometry
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract In the present study the solid and liquid phase behaviour of mandelic acid cyclodextrin systems were studied. The samples were prepared using dry grinding/kneading technique in the absence of any solvent. Thermoanalytical methods (TG, DSC, EGD) were used to characterise the solid compounds. In liquid phase the stoichiometry and the stability constants of the complexes formed were determined using UV spectrophotometry. Partial complex formation was found in case of all cyclodextrins used. The amount of uncomplexed mandelic acid varied between 10–20% of the total guest content.
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  • 4
    Electronic Resource
    Electronic Resource
    Springer
    Journal of thermal analysis and calorimetry 50 (1997), S. 431-440 
    ISSN: 1572-8943
    Keywords: salicylaldehyde S-methylisothiosemicarbazone ; thermogravimetry ; uranyl complexes
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Solvate complexes of UO 2 2+ andN(1), N(4)-bis(salicylidene)-S-methylisothiosemicarbazone, (H2Me-L1), of general formula [UO2(Me-L1)S] (S= H2O, MeOH, EtOH, Py, DMF and DMSO) were synthesized. The methanolic UO 2 2+ ” adducts of N(1)-benzoylisopropylidene-N(4)-salicylidene-S-alkylisothiosemicarbazone, (H2R-L2,R=Me, Prn) of general formula [UO2(R-L2)· MeOH], were also prepared. Thermal decomposition of the complexes was investigated in air and argon. The complexes decompose to α-U3O8 in air, while in argon the decomposition is not completed up to 1000 K. The temperature and the mechanism of decomposition of the complexes are a function of the solvent belonging to the inner coordination sphere.
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  • 5
    Electronic Resource
    Electronic Resource
    Springer
    Journal of thermal analysis and calorimetry 38 (1992), S. 1017-1025 
    ISSN: 1572-8943
    Keywords: pharmaceutical substances ; polymorphism ; pseudopolymorphism
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Zur Untersuchung des physikalisch-chemischen Verhaltens binärer Gemische wird ein komplexes System, bestehend aus thermoanalytischen Methoden, IR und Röntgendiffraktion nach dem Debye-Scherrer-Verfahren, beschrieben. Dieses System wurde an binären Gemischen von Amphetaminhydrochloridsalzen getestet. Die Untersuchungen zeigten, daß von den gewählten Verbindungen die Hydrochloride der primären und sekundären Amine eine Tendenz zur Konglomeratbildung zeigen, während die Hydrochloride der tertiären Amine Molekülverbindungen (Racemate) bilden. Für p-Fluoramphetamin-Hydrochlorid wurde die Existenz von zwei polymorphen Modifikationen nachgewiesen.
    Notes: Abstract A complex system including thermoanalytical methods, infrared spectroscopy and X-ray powder diffraction for studying physico-chemical behaviour of binary mixtures is described. This system has been tested by investigating binary mixtures of amphetamine hydrochloride salts. These studies have proved that among the selected compounds the primary and secondary amine hydrochloride salts exhibit conglomerate forming tendency, while the tertiary amine hydrochloride salts form molecular compounds (racemates). For thep-fluoro amphetamine hydrochloride the existence of two polymorphic modifications has been detected.
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  • 6
    ISSN: 1572-8943
    Keywords: 2-benzylamino-butanol ; DSC ; mandelic acid ; melting phase diagram ; optical resolution
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The optical resolution of racemic mandelic acid (I) by S-2-benzylamino-butanol (II) was performed in water, ethyl acetate, and water saturated ethyl acetate. It was found that the efficiency of the resolution is three times higher in water saturated ethyl acetate than in either water or ethyl acetate. The salt mixtures produced during the resolutions and the pure diastereoisomeric salts were analyzed by TG, DSC and X-ray powder diffraction measurements. The R-(-)-I×S-(+)-II salt has the higher melting point and heat of fusion value which indicates that this is the more stable salt. Though the general assumption is that diastereoisomeric salt pairs of successful optical resolutions form eutectic systems, the R-mandelic acid-S-2-benzylamino-butanol and the S-mandelic acid-S-2-benzylamino-butanol system was found to behave in a different way. Melting did not start at or near the estimated eutectic temperature. The difference can be explained either by miscibility in the solid phase (solid solution) or by a blocked interaction between the crystals of the two solid salts. This unusual behaviour of the salt pair should be responsible for the unusual difference in the efficiency of the resolutions performed in different solvents
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  • 7
    ISSN: 1572-8943
    Keywords: diastereoisomeric salt formation ; mechanism of optical resolutions
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The optical resolution of α-phenylethylamine (1) by 2R,3R-tartaric acid (2) was studied in different solvents, the precipitated salts were subjected to thermoanalytical measurements and X-ray powder diffraction. The most efficient resolution can be accomplished by using methanol, the precipitate, an unsolvated salt containing the S-(-)-1⋅2R,3R-(+)-2 salt in abundance, is not a simple mixture of the diastereoisomeric salt pair, but a new modification. In water, ethanol and acetonitrile a reversed, but less effective resolution can be accomplished by precipitation of a hydrate which contains the R-(+)-1 in abundance. The precipitates from water and ethanol also proved to be new modifications. Only the precipitate from acetonitrile is the mixture of the diastereoisomeric salt pair, which can be expected in fractional crystallization of an eutectic forming diastereoisomeric salt pair. The number of different modifications found by changing the solvent in case of this particular salt pair seems surprisingly high, but may occur for other diastereoisomeric salt pairs, too. The existing but not investigated polymorphism can be the explanation for the sometimes very poor reproducibility of the preparative resolutions.
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  • 8
    Electronic Resource
    Electronic Resource
    Springer
    Journal of thermal analysis and calorimetry 29 (1984), S. 1083-1093 
    ISSN: 1572-8943
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung VerÄnderungen des Wassergehalts von Aluminiumsulfat-Hydrat bei Zimmertemperatur in Luft unterschiedlicher relativer Feuchtigkeit wurden gravimetrisch untersucht. Die auf diese Weise konditionierten Proben wurden durch thermoanalytische (TG, DTG, DSC) und röntgendiffraktometrische Messungen charakterisiert. Durch Erstarren der Schmelze erhaltenes industrielles Aluminiumsulfat-Hydrat ist teilweise kristallin. Nach dem Mahlen kristallisiert dieses Material wÄhrend der Lagerung. Dieser Proze\ erfordert eine feuchte AtmosphÄre, wobei sich der Kristallisationsgrad mit steigender relativer Feuchtigkeit erhöht. Es wurde festgestellt, da\ die Kristallisation des Aluminiumsulfats durch einen höheren Wassergehalt der Schmelze gefördert wird.
    Abstract: РЕжУМЕ ИжМЕНЕНИЕ сОДЕРжАНИ ь ВОДы В гИДРАтЕ сУльФ АтА АлУМИНИь БылО ИсслЕД ОВАНО гРАВИМЕтРИЧЕскИ пРИ кОМНАтНОИ тЕМпЕРАтУ РЕ В АтМОсФЕРЕ ВОжДУхА с Р АжлИЧНОИ ОтНОсИтЕль НОИ ВлАжНОстьУ. пОлУЧЕНН ыЕ тАкИМ пУтЕМ ОБРАжц ы БылИ ОхАРАктЕРИжОВАНы МЕ тОДОМ тг, Дтг, Дск И МЕтОДОМ Д И ФРАкцИИ РЕНтгЕНОВс к Их лУЧЕИ. тЕхНИЧЕскИИ гИДРАт с УльФАтА АлУМИНИь, пОлУЧЕННыИ жАМОРАжИВАНИЕМ РАсп лАВА, ИМЕл ЧАстИЧНО кРИстАллИЧ ЕскУУ стРУктУРУ. пОслЕ ИжМЕльЧЕНИь ВЕ ЩЕстВО пРИ хРАНЕНИИ кРИстАллИжУЕтсь. пРО цЕсс кРИстАллИжАцИИ тРЕБУЕт ВлАжНОИ АтМО сФЕРы, пРИЧЕМ УВЕлИЧЕ НИЕ ОтНОсИтЕльНОИ ВлАжН ОстИ ВыжыВАЕт БОлЕЕ ИНтЕНсИВНУУ кР ИстАллИжАцИУ. НАИДЕН О, ЧтО кРИстАллИжАцИь сУль ФАтА АлУМИНИь Иж РАсплАВА УскОРьЕт сь пРИ БОлЕЕ ВысОкОМ с ОДЕРжАНИИ ВОДы В жАМЕсЕ.
    Notes: Abstract Changes in the water content of aluminium sulphate hydrate were investigated gravimetrically at room temperature in air with different relative humidities. The samples conditioned in this way were characterized by thermoanalytical (TG, DTG, DSC) and X-ray diffraction measurements. Industrial aluminium sulphate hydrate obtained by freezing the melt has a partly crystalline structure. After grinding, this material crystallizes during storage. This process requires a humid atmosphere; increasing relative humidity brings about more intensive crystallization. It was found that the crystallization of aluminium sulphate from the melt is facilitated by a higher water content of the melt.
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  • 9
    Electronic Resource
    Electronic Resource
    Springer
    Journal of thermal analysis and calorimetry 27 (1983), S. 315-324 
    ISSN: 1572-8943
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Die Thermogravimetrie wurde zur Untersuchung von Aluminiumfolien für Elektrolytkondensatoten angewandt. Zur Interpretation der Ergebnisse wurden auch durch Raster Elektronenmikroskopie, Röntgendiffraktometrie und Oberflächenmessungen erhaltene Daten herangezogen. Sowohl die spezifische Oberfläche als auch die Kapazität der Folien verhalten sich proportional zur Höhe der thermogravimetrisch gemessenen Oxydationsstufe, die sich zur Verfolgung des Prozesses der anodischen Oxydation und der thermischen Behandlung der Folien als geeignet erwiesen hat.
    Abstract: Резюме Термогравиметрия бы ла использована для и зучения алюминиевой фольги электролитических к онденсаторов. Наряду с этим, была использована сканир ующая электронная микроск опия, рентгеновская д иффракция и определение площади поверхности. Значения удельной пл ощади поверхности и е мкостная способность фольги н аходились в линейной зависимос ти от степени окислен ия, измеренной методом Т Г. Было установлено, что метод ТГ является приемлемым также для последующих процесс ов анодного окисления фольги и ее термической обработ ки.
    Notes: Abstract Thermogravimetry was applied in studies of aluminium foils for electrolytic capacitors. Scanning electron microscopy, X-ray diffraction and surface area determination were also used in the interpretation of the results. Both the specific surface area and the capacity of the foils showed a linear relationship to the height of the oxidation step measured by TG, which was found suitable for following the processes of anodic oxidation and thermal treatment of the foils as well.
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  • 10
    Electronic Resource
    Electronic Resource
    Springer
    Journal of thermal analysis and calorimetry 33 (1988), S. 765-769 
    ISSN: 1572-8943
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Die Zersetzung von Hydrargillit zuχ-Aluminiumoxid in Luft und die Umwandlung vonχ-Aluminiumoxid zu Böhmit unter hydrothermalen Bedingungen bei isothermer Versuchsführung wurden untersucht. Die Reaktionsprodukte wurden mittels Thermogravimetrie und Röntgenbeugung charakterisiert. Die Geschwindigkeit der Umsetzung von Hydrargillit zuχ-Aluminiumoxid unterhalb 250 °C wird durch Keimbildung und Wachstum bestimmt. Die Geschwindigkeit der hydrothermalen Umsetzungχ-Al2O3→Böhmit hängt von der Mahldauer und der Teilchengrössen des Hydrargillits ab, aus dem dasχ-Al2O3 präpariert worden war. Während letztere Reaktion wird bei tieferer Temperatur partiell Hydrargillit gebildet, das Endprodukt war stets Böhmit.
    Abstract: Резюме Изотермически иссле довано разложение гиббсита доχ-окиси а люминия в атмосфере воздуха и превращени е его до боэмита в гидротермических ус ловиях. Методом ТГ и рентгенофазового ан ализа охарактеризов аны продукты реакции. Скорость реа кции разложения гиббсита доχ-окиси а люминия ниже 250° соотве тствует механизму образован ия центров кристаллизации и их к онтролируемому рост у. Гидротермическое пр евращениеχ-окиси алюминия до боэмита з ависит от времени изм ельчения и размера частиц гиббс ита, из которых был полученχ-оксид а люминия. Во время этой реакции при более низкой темп ературе вновь наблюдалось образов ание гиббсита, но коне чным продуктом реакции во всех случаях был боэмит.
    Notes: Abstract The gibbsite →χ-alumina decomposition (in air) and theχ-alumina → boehmite transformation (under hydrothermal conditions) were investigated isothermally. Reaction products were characterized by TG and X-ray diffraction. The rate of the gibbsite →χ-alumina reaction below 250 °C appears to be nucleation and growth controlled. That of the hydrothermal transformation ofχ-alumina to boehmite depends on the time of grinding and the particle size of the gibbsite from which theχ-oxide has been prepared. During this reaction, partial re-formation of gibbsite was observed at lower temperatures, but the final product was always boehmite.
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