Polymorphism and stability of norfloxacin, (1-ethyl-6-fluoro-1,4-dihydro-4-oxo-7-(1-piperazinil)-3-quinolinocarboxylic acid

Norfloxacin was studied by thermal methods (TG and DSC), X-ray powder diffraction, and by FT-IR, UV-VIS and NMR spectroscopy. The drug substance can be prepared in two different crystalline forms and in amorphous state, depending on the experimental conditions of preparation. DSC examinations were carried out at various heating rates and by cycling the samples in the temperature range 50°–250°C. The unstable crystalline form undergoes two irreversible solid-solid phase transitions at 176.5° and 197.6°C. The polymorph melts in the temperature range 218.5°–220.0°C.

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Zusammenfassung Norfloxacin wurde mittels thermischer Methoden (TG und DSC), weiterhin mittels der Debye-Scherrer-Methode und FTIR-, UV-VIS-und NMR-Spektroskopie untersucht. Je nach den experimentellen Bedingungen bei der Herstellung kann die Wirkstoffsubstanz in zwei verschiedenen kristallinen und in einer amorphen Form hergestellt werden. Die DSC-Untersuchungen wurden bei zahlreichen Aufheizgeschwindigkeiten und durch abwechselnden Temperaturwechsel zwischen Raum- und Schmelztemperatur durchgeführt. Die unstabile kristalline Form unterliegt zwei irreversiblen Feststoff-Feststoff-Umwandlungen bei 176.5° und bei 195.6°C. Das polymorphe Material schmilzt im Temperaturbereich 218.5°–220.0°C.

     

Crystallochemical causes of the different thermal properties of [Cu(py)2(NCS)2] and [Cu(4-Mepy)2(NCS)2] complexes

The crystal structures and thermal behaviour of [Cu(py)₂(NCS)₂] (at 293) and [Cu(4-Mepy)₂(NCS)₂] and 180 K) complexes have been compared with their different temperature behaviour. It was found that the thermal stability of coordinated thiocyanate ligands in the course of thermal decomposition depends not only on the properties of the ligand L, but it is related to the arrangement of the thiocyanatocopper chains in the crystal structures.     

Partial Least-Squares Study of the Effects of Organic Modifier and Physicochemical Properties on the Retention of Some Thiazoles

JPC – Journal of Planar Chromatography – Modern TLC - Reversed-phase (RP) HPTLC with aqueous ammonia-organic modifier (acetonitrile, dioxane, acetone) mobile phases has been used to...     

Mechanism of the thermal decomposition of hydrophosphites of lithium,sodium and potassium

The thermal decomposition of some M ₂ ^I HPO₃ (M-Li, Na, K) phosphites under nitrogen atmosphere was investigated. A stepwise mechanism of thermal decomposition has been proposed.

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Zusammenfassung Es wurde die thermische Zersetzung von Phosphiten M ₂ ^I HPO₃ (M-Li, Na, K) in Stickstoffatmosphere untersucht. Die Schritte des Mechanismus der thermischen Zersetzung wurden vorgeschlagen.

     

On distribution of molecular weight in anionic polymerizates of caprolactam

Measurement has been made of the dependence of the molecular weight distribution on the ratio of the catalytic system components and on the polymerization time for polycaprolactam obtained by anionic polymerization. A bimodal character of the curves was observed for products made using molar ratios of activator (N-benzoylcaprolactam) to initiator (sodium dihydro-bis(methoxyethoxy)aluminate) of 1:1 and 1:3, when the polymerization times were less than 1 hr. This course is explained by the influence of fast side-reactions, mainly condensations. For a ratio of 3:1 of the components of the catalytic system, smooth integral distribution curves are obtained, accounting for a very fast decrease in the strong base concentration in the initial stages of the polymerization.     

Observation of a Doppler broadening of the 4438 keV gamma-line of12C in processes12C(n,n′γ)12C and9Be(α, nγ)12C

A Doppler broadening is described of the 4438 keV spectral gamma-line observed by means of a Ge(Li) detector during the deexcitation of nuclei of¹²C in an inelastic scattering¹²C(n, n′γ)¹²C using an²⁴¹Am−Be source as well as during the reaction⁹Be(α, nγ)¹²C taking place in the Am−Be source. The FWHM of the spectral line is equal to (90±4) keV in the latter reaction and (64±8) keV in the former process. Experimental values agree well with theoretical ones. Presented at the Instrumental Activation Analysis Conference, IAA 79, June 4–8, 1979, Klučenice, Czechoslovakia.     

Solubility Study of Nimodipine Inclusion Complexation with α- and β-Cyclodextrin and some Substituted Cyclodextrins

The solubility of nimodipine was measured in aqueous solutions of the following cyclodextrins: -cyclodextrin (-CD), hydroxypropyl--CD (HP--CD), -cyclodextrin (-CD), random substituted methyl--CD (M--CD), three hydroxypropyl--CDs (HP--CD) with mutually different average degree of substitution, and hydroxypropyl--cyclodextrin (HP--CD). From the determined linear solubility diagrams the values of the binding constant K₁₁ of the inclusion complexes of nimodipine with the respective CDs were evaluated. The -CDs efficiently solubilized sparingly soluble nimodipine, the highest value of K₁₁ was found for M--CD (1680 M^-1), followed by -CD (550 M^-1) and HP--CDs, where the higher degree of substitution lowered K₁₁. Only slight solubilization of nimodipine was observed in the solutions of the -CDs and HP--CD.     

Conductivity Studies of Dilute Aqueous Solutions of Oxalic Acid and Neutral Oxalates of Sodium, Potassium, Cesium, and Ammonium from 5 to 35°C

Conductivity measurements of oxalic acid and neutral oxalates (disodium oxalate, dipotassium oxalate, dicesium, and diammonium oxalate) were performed on dilute aqueous solutions, c < 3 × 10^–3 mol-dm^–3, from 5 to 35°C. These data and those available from the literature were analyzed in terms of dissociation steps of oxalic acid, the Onsager conductivity equation for neutral oxalates, the Quint–Viallard conductivity equation for the acid, and the Debye–Hückel equation for activity coefficients, to give the limiting equivalent conductances of bioxalate anion ;(HC₂O₄ ^–) and oxalate anion (1/2C₂O₄ ^2–) and the corresponding dissociation constants K ₁ and K ₂.     

Determination of boron in boron-alloyed steels by inductively coupled plasma atomic emission spectrometry

An inductively coupled plasma atomic emission spectrometry (ICP-AES) procedure has been developed and examined for the determination of boron content (0.01 up to about 2% B) in boron-alloyed steels such as POLDI ATA BOR (65% Fe, 19%Cr, 12% Ni, 1.5% Mn, 1% B), POLDI ATA BOR EXTRA (62% Fe, 18% Cr, 13% Ni, 2.5% Mo, 1.5% Mn, 1% B) and POLDI ATA BOR-R (75% Fe, 18% Cr, 3.5% Ti, 1.8% B). The steel sample is dissolved with a mixture of hydrochloric, nitric, sulfuric and phosphoric acids in a quartz vessel. Borides of alloyed metals, especially of iron and chromium, are quantitatively decomposed. The presence of phosphoric acid in a sample solution reduces the volatility of boric acid with water vapour.Presented in part at the 1989 European Winter Conference on Plasma Spectrochemistry, Reutte, Austria     

Influence of the pyridine methyl substituent position on the chemical changes of the NCS groups in the thermal decomposition of coordination compounds of the type Cu(NCS)2L2

The influence of the position of the CH₃ group in picoline and lutidine ligands on the degree of chemical change of the NCS groups in coordination compounds of the type Cu(NCS)₂L₂ (whereL=2-, 3- and 4-picoline, and 2,3-, 2,4-, 2,5-, 2,6-, 3,4- and 3,5-lutidine) is dealt with. The most marked effect of the CH₃ group is found to be exerted in position 4. This effect of the methyl group on the degree of chemical change points to the mutual influence of the ligands in coordination compounds of Cu(II).

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Zusammenfassung Der Artikel befaßt sich mit dem Einfluß der Lage der CH₃ Gruppe in Pikolinen und Lutidinen als Liganden auf den Grad der chemischen Änderungen der Gruppen NSC in Koordinationsverbindungen des Typs Cu(NCS)₂L₂ (L=2-, 3- und 4-Pikoline, 2,3-, 2,4-, 2,5-, 2,6-, 3,4- und 3,5-Lutidine). Der ausgeprägteste Effekt der CH₃ Gruppe wurde in der Position 4 beobachtet. Dieser Einfluß der Methylgruppe auf das Ausmaß der chemischen Änderungen deutet auch auf die gegenseitige Wirkung der Liganden in Koordinationsverbindungen von Cu(II).

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Résumé L'article a trait à l'influence de la position du groupe CH₂ dans les picolines et lutidines, en tant que ligands, sur le degré des changements chimiques des groupes SCN dans les composés de coordination du type Cu(SCN)₂L₂ (L=2-, 3 et 4-picoline, 2,3-, 2,4-,2,5-, 2,6-, 3,4- et 3,6-lutidine). L'effet le plus prononcé du groupe CH₃ s'observe en position 4. Cette influence du groupe méthyle sur le degré des changements chimiques indique aussi l'influence mutuelle des ligands dans les composés de coordination du Cu(II).

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- , , NCS Cu(NCS)₂,L₂, L=2-, 3- 4- , 2.3-, 2.4-, 2.5-, 2.6-, 3.4- 3.5-. , 4. Cu(II).