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991.
Danielle Giron S. Monnier M. Mutz P. Piechon T. Buser F. Stowasser K. Schulze M. Bellus 《Journal of Thermal Analysis and Calorimetry》2007,89(3):729-743
Adequate very sensitive quantification methods are needed for the development and are also now required for the monitoring
of undesirable solid form(s) as routine tests. The pre-requisite for quantitation are selectivity, sensitivity and most important
the purity of standards and their proper storage, what is a challenge for metastable forms.
Several analytical techniques are available such as X-ray diffraction, spectroscopy, thermal analysis and microcalorimetry.
The different steps of the validation of the analytical methods and problems to be solved are discussed. Examples illustrate
the different techniques and compare their possible advantages and limits. The relative standard deviation of measurements
should allow for checking the homogenization procedure of mixtures for calibration. The validation should be carried out following
ICH guidelines for validation of analytical methods. Comparison of different techniques in adequate concentration range add
confidence in the analytical results. 相似文献
992.
V. G. Badelin E. Yu. Tyunina G. V. Girichev N. I. Giricheva O. V. Pelipets 《Journal of Structural Chemistry》2007,48(4):647-653
This paper reports on our mass spectrometric study of sublimation of glycine and DL-alanyl-glycine (Ala-gly). The sublimation enthalpy of Ala-gly has been determined by generalization of the data obtained and the results of AM1 quantum-chemical calculations. A relationship has been found between the sublimation enthalpy (ΔH subl), heat capacity (C P), and the sum of bond lengths (Σn i l i ) in 17 α-amino acid and 9 dipeptide molecules. Correlations are suggested for evaluating ΔH subl of amino acids and peptides. 相似文献
993.
用计算机多元分析研究冠心病微量元素谱,识别冠心病患者与健康者;非线性映射法判别率男性86.6%,女性96.2%;SIMCA差别法正确回判率男性85.0%,女性88.3%。 相似文献
994.
猴头菇微量元素含量的分析 总被引:5,自引:6,他引:5
用电感耦合等离子体发射光谱仪(ICP-AES)测定了湛江市栽培的猴头茹微量元素的含量,发现其磷、硫、钙、镁、锌、铁、铜等元素的含量都比较丰富,并讨论了这些有益元素与人体健康的关系。 相似文献
995.
The thermal analysis of CoC2O4·2H2O, Co(HCOO)2·2H2O and Co(CH3COO)2·4H2O was carried out with simultaneous TG-DTG-DTA measurements under non-isothermal conditions in air and argon atmospheres.
The intermediates and the end products of decomposition were characterised by X-ray diffraction and IR and UV-VIS spectroscopy.
The decomposition of the studied compounds occur in several stages. The first stage of dissociation of each compound is dehydration
both in air and argon. The next stages differ in air and argon. The final product of the decomposition of each compound in
air is Co3O4. In argon it is a mixture of Co and CoO for cobalt(II) oxalate and cobalt(II) formate but CoO for cobalt(II) acetate.
This revised version was published online in August 2006 with corrections to the Cover Date. 相似文献
996.
The present paper covers the reaction ergodography for the addition of AlH3 to acetylene investigated by ab initio calculation with RHF/3-21G basis set. The changes in some physical properties along the reaction path (IRC) are presented. The formations of FMOs of the transition state have been analyzed according to the Fukui' s method. On the basis of the perturbation theory and Wolfsborg Helmholtz formula, we calculated the FMO' s energy orders of TS and its formation that shows the HOMO of TS consists of LUMO, HOMO of AlH3 and HOMO of HCCH. 相似文献
997.
By means of model calculations it could be shown for an irreversible surface reaction of 1st order that the determination of the activation energy of the desorption of the reactant or, respectively, of the surface reaction is possible by application of the method of variation of the heating rate to the desorption curve of the reactant, according to circumstances whether the ratio of the activation energy of the surface reaction and of the desorption of the reactant is greater or smaller than one.The possibilities of the kinetic evaluation are applied to the isomerization of cyclopropane on a NaX-zeolite catalyst. The resulting heat of adsorption of cyclopropane and the activation energy of the reaction agree well with the values of literature obtained by isothermal measurements in a pulse reactor.
Zusammenfassung Mit Modellrechnungen für eine irreversible Oberflächenreaktion 1. Ordnung konnte gezeigt werden, daß durch Anwendung der Methode der Variation der Heizgeschwindigkeit auf die Desorptionskurve des Ausgangsstoffes die näherungsweise Bestimmung der Aktivierungsenergie der Desorption des Ausgangsstoffes bzw. der Oberflächenreaktion möglich ist, je nachdem ob das Verhältnis der Aktivierungsenergien für die Oberflächenreaktion und der Desorption des Ausgangsstoffes größer oder kleiner als eins ist.Die Möglichkeiten der kinetischen Auswertung werden auf die isomerisierung von Cyclopropan an einem NaX-Zeoliten angewendet. Die erhaltene Adsorptionswärme für Cyclopropan und die Aktivierungsenergie für die Reaktion stimmen gut mit Literatur-werten von isothermen Messungen im Impulsreaktor überein.相似文献
998.
固定pH滴定法测定弱酸弱碱性药物 总被引:8,自引:0,他引:8
报道一种水溶液吕测定弱酸弱碱性药物的新型滴定分析方法-固定pH滴定法,其理论基础是弱酸弱碱在水溶液中各种存在形式的分布系数在pH值固定时为常数,对甲硝唑,盐酸美西律等离散常数在10^-8至10^-11范围内的7种弱酸弱碱性药物进行测定。结果与药典法吻合,回收率在99.4%~100.6%,方法简便,快速,准确,制剂中的赋形剂及色物不影响测定。 相似文献
999.
1000.
A relationship is derived to enable the comparison of the dispersion heights of normal and reverse flow injection analysis (FIA). A single channel flow system is employed in the absence of a chemical reaction. The stopped-flow injection method is used to probe the influence of molecular diffusion on the overall dispersion of normal and reverse FIA, which appeared to demonstrate fundamentally different diffusion behaviors. Small discrepancies are observed between the dispersion heights, which are enhanced by the stopped-flow period, especially when unmatched matrix ionic compositions of the indicator and counter solutions were involved. For these conditions, the diffusion flux rate is enhanced considerably, displaying a peak, in addition to the transient, for both methods. The influence of diffusion on the dispersion characteristics of normal and reverse FIA is discussed theoretically. Diffusion in the proposed model is postulated to oppose dispersion by convection. The latter initiates concentration gradients in the injection zone and propagates it with flow time over the dispersion zone profile. The diffusion flux then reacts in order to confine the indicator dispersion for normal FIA and to enhance it for reverse FIA. This model is consistent with the experimental results and accounts for most of the phenomena encountered. Probably owing to the influence of secondary flow phenomena, the use of coiled tubes has suppressed the effects of diffusion on the overall dispersion behavior.Part of the experimental work was performed at IMI Institute for Research and Development, Haifa, Israel. 相似文献