Effect of radiation dose on the thermal decomposition of sodium bromate

Influence of radiation dose in the range of 0.5–2.0 MGy of⁶⁰Co -rays on the isothermal decomposition of sodium bromate at 633.0 K shows that irradiation increases the initial gas evolution {ie37-1}, shortens the induction period (I), enhances the rate of reaction in the accelerating and decay stages. The data fit well the Prout-Tompkins relationship, indicating that nucleation occurs in a chain branching manner during the process. The fraction decomposed, , increases with increasing radiation dose.     

Determination of thiol groups with o-diacetoxy-iodobenzoate

o-Diacetoxyiodobenzoate is used for determining thiol groups by two procedures. In the first, thiols are titrated directly with the reagent at pH 6-8, with leuco-2,6-dichlorophenolindophenol and potassium iodide as indicator. In the second, thiols are treated at pH 7 with an excess of the reagent, the surplus being determined by reaction with excess of mercaptoacetic acid followed by back-titration of the latter with iodine. Both procedures yield results within 0.2% of the theoretical.     

Untersuchung der OberflÄchenspannung der Systeme:

Zusammenfassung Die Oberfl?chenspannungen der Systeme: 1. Wasser/propionsaures Natrium mit verschiedenen Alkoholen; 2. Wasser/buttersaures Natrium mit verschiedenen Alkoholen; 3. Wasser/crotonsaures Natrium mit verschiedenen Alkoholen und 4. Wasser/caprylsaures Natrium mit verschiedenen Alkoholen wurden gemessen, und die Ergebnisse werden im Sinne der in früheren Arbeiten (3, 4) ver?ffentlichten Hypothese diskutiert.

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Summary The surface tension of the systems (1) water-sodium propionate and different alcohols, (2) water-sodium butyrate and different alcohols, (3) water-sodium crotonate and different alcohols and (4) water-sodium caprylate and different alcohols has been determined and the results have been discussed on the basis of the hypothesis suggested in previous papers (3, 4).

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übersetzt von Dr. K, Jaeckel (Marburg/L.)

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Wir danken Herrn Dr. A. Chatterji, Head of the Chemistry Department, für sein Entgegenkommen. Einer von uns (J. M.) dankt dem Scientific Research Grants Committee für ein Stipendium zur Durchführung der Arbeit.     

Synthesis of α-hydroxy-β-lactams

A convenient synthesis of α-hydroxy-β-lactams has been devised that involves the annelation of an inline with benzyloxyacetyl chloride and triethylamine and subsequent hydrogenolysis in the presence of palladium on carbon. In most cases a cis-β-lactam was obtained. A thioimidate can also be used as the imino component in the annelation reaction but the hydrogenolysis step fails. The annelation of the appropriate thiazoline to a 6-epi-penicillin derivative occurred much more readily with benzyloxyacetyl chloride than with azidoacetyl chloride.     

Kinetics and mechanism of oxidation of cyclopentanone by N-bromosuccinimide

N-bromosuccinimide oxidation of cyclopentanone in acidic media in presence of mercuric acetate has been made. A zero order dependance to N-bromosuccinimide and a first order dependence to cyclopentanone and hydrogen ion concentration has been observed. Ionic strength, mercuric acetate and succinimide has negligible effect while methanol addition has a positive effect. Various rate parameters have been computed and 1,2-cyclopentanedione identified as the end product. A suitable mechanism in confirmity with the above observations has been proposed.With 2 Figures     

Therapeutic monitoring of imipramine and desipramine by micellar liquid chromatography with direct injection and electrochemical detection

A micellar liquid chromatographic (MLC) procedure was developed for the clinical monitoring of imipramine and its active metabolite, desipramine. The determination of these highly hydrophobic substances was carried out after direct injection of the serum samples using a mobile phase composed of 0.15 m SDS--6% (v/v) pentanol buffered at pH 7, pumped at 1.5 mL/min into a C(18) column (250 x 4.6 mm), and electrochemical detection at 650 mV. Using this MLC method, calibration was linear (r > 0.995) and the limits of detection (ng/mL) were 0.34 and 0.24 for imipramine and desipramine, respectively. Repeatabilities and intermediate precision were tested at three different concentrations in the calibration range and a CV (%) below 2.2 was obtained. In this MLC procedure, the serum is determined without treatment, thus allowing repeated serial injections without changes in retention factors, and reducing the time and consumables required to carry out the pretreatment process. The assay method can be applied to the routine determination of serum imipramine and its metabolite in therapeutic drug monitoring.     

(Z)-3-p-tolylsulfinylacrylonitrile as a chiral dienophile: diels-alder reactions with furan and acyclic dienes

The behavior of (Z)-3-p-tolylsulfinylacrylonitrile (1) as a chiral dienophile has been evaluated from its reactions with furan and acyclic dienes. Electrostatic interactions of the cyano group with the sulfinyl one restrict the conformational mobility around the C-S bond, thus controlling the pi-facial selectivity, which is almost complete in all cases, the approach of the diene from the less-hindered face of the dienophile (that bearing the lone electron pair) in the predominant rotamer being the favored one. The regioselectivity is also completely controlled by the cyano group. Additionally, the reactivity of compound 1 as well as its endo-selectivity are both higher than those observed for the corresponding (Z)-3-sulfinylacrylates, thus proving the potential of sulfinylnitriles as chiral dienophiles.     

Determination of thiourea and its organic derivatives with iodine trichloride

Thiourea and its organic derivatives and thiosemicarbazide are determined in water, methanol or glacial acetic acid medium by reaction with an excess of iodine trichloride in the presence of mercuric chloride. The reaction is complete in 15 min. The excess of iodine trichloride is evaluated by adding potassium iodide and titrating the liberated iodine with thiosulphate. A variety of organic thioureas can be determined with an average accuracy and precision of 0.2%.     

A study of conductivity of the systems: Water-0.2 N sodium salts of fatty acids and Butanol-I in presence of free acids and alkali (Part II)

Summary From the study of the electrical conductance of the systems: Water-0.2N sodium salts of fatty acids and Butanol-I containing different amounts of free acids, it has been concluded that two types of micelles exist in such systems. Above 50% Butanol-I concentration lipophilic hydromicelles exist, whereas below 50% Butanol-I concentration hydrophilic oleomicelles are formed. It has also been observed that the concentration at which the change in the micelle structure takes place depends on the chain length of the soap. The conductance of the solutions of all the systems goes on decreasing with the increase in Butanol-I concentration as well as with the increase in the chain length of the soap. The results are in agreement with viscosity and surface tension results obtained in the previous communications.

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Zusammenfassung Aus Untersuchungen der elektrischen Leitf?higkeit eines Systems: Wasser/0,2 n Natriumsalze der Fetts?uren und Butanol-I, das verschiedene Betr?ge an freien S?uren enth?lt, wurde auf die Anwesenheit von zwei verschiedenen Mizelltypen in solchen Systemen geschlossen. Bei Konzentrationen von mehr als 50% Butanol-I existieren lipophile Hydromizellen, w?hrend unterhalb 50% Butanol-I hydrophile ?lmizellen gebildet werden. Es wurde beobachtet, da? die Konzentration bei der der Strukturwechsel der Mizellen stattfindet, von der Kettenl?nge der Seife abh?ngt. Die Leitf?higkeit der L?sungen aller Systeme beginnt abzunehmen mit der Zunahme der Konzentration von Butanol-I, wie auch mit dem Wachsen der Kettenl?nge der Seife. Die Ergebnisse sind in übereinstimmung mit den früher erhaltenen bei Untersuchungen von Viskosit?t und Oberfl?chenspannung.