Method of obtaining sulphur-labelled compounds by reaction of ''hot'' sulphur-35 atoms with cyclic hydrocarbons
Creators
Description
The authors discuss methods of obtaining sulphur-labelled compounds, such as aliphatic and cyclic mercaptans and sulphides, by direct synthesis employing recoil atoms from the reaction Cl35 (n, p) S35. Hot S35 atoms were obtained in the middle of the target substance by exposing mixtures of C Cl4 and a cyclic hydrocarbon (cyclopentane, cyelohexane) to neutrons in a reactor. A method is given for irradiating the mixtures and then separating the various sulphur-bearing compounds by specific chemical methods, rectification, and paper and gas-liquid chromatography. The purpose of the exchange is clarified. The relation of the yield of the separated sulphur-labelled products to the composition of the mixture and type of exposure was investigated, and an active-sulphur balance settled. New types of atomic sulphur reactions were established: the CH2-group is replaced and implanted on the C-C link. The cyclic molecule is destroyed in the interaction with the hot sulphur atoms. Hot sulphur atoms can initiate the formation of polymers containing sulphur. The yields of these reactions were established. Up to 98% of the active sulphur is linked in the form of organic sulphur compounds. It was shown that sulphur-labelled thiophene, tetrahydrothiopyrane, cyclopentyl-mercaptan, cyclohexylmercaptan, ethyl-propyl-butyl-mercaptans, dicyclopentyl-sulphide, polymeric mercaptans and sulphides could be synthesized by heat. I t is possible to regulate within broad limits the yield of various labelled compounds by changing the decelerating properties of the medium. (author)
Abstract (French)
Les auteurs examinent les methodes permettant d'obtenir des composes marques au soufre (mercaptans et sulfures aliphatiques et cycliques) par synthese directe a l'aide des atomes de recul obtenus par la reaction 35Cl (n, p) 35S. Des atomes fortement excites de 35S ont ete obtenus au milieu de la substance cible par irradiation neutronique de melanges de CCl4 et d'un hydrocarbure cyclique (cyclopentane, eyclohexane) dans un reacteur. Les auteurs exposent la methode d'irradiation des melanges et les procedes chimiques permettant de separer ensuite les divers composes contenant du soufre (rectification, chromatographie sur papier et chromatographie gaz-liquide). Ils expliquent le role de l'echange, examinent la mesure dans laquelle le rendement pour les divers produits marques au soufre depend de la composition du melange et de la nature de l'irradiation et etablissent le bilan du soufre actif. Ils determinent de nouveaux types de reaction atomique du soufre : substitution du groupe CH2 et incorporation dans les unions C-C. Apres avoir constate la destruction de la molecule cyclique dans l'interaction avec les atomes excites du soufre, ils font ressortir l'aptitude de ces atomes a amorcer la formation de polymeres contenant du soufre. Ils ont determine les rendements de ces reactions et demontre que jusqu'a 98% du soufre actif se lie sous forme de composes organiques du soufre. Les auteurs montrent la possibilite de realiser la synthese a chaud des produits suivants, marques au soufre: thiophane, tetrahydrothiopyrane, cyclopentylmercaptan, cyclohexylmercaptan, ethyl-propyl-butyl-mercaptans, sulfure de dicyclopentyle, mercaptans et sulfures polymeres. Ils indiquent egalement la possibilite de regler dans des limites assez larges le rendement des divers composes marques, en modifiant les proprietes de ralentissement du milieu. (author)Abstract (Spanish)
La memoria estudia metodos para obtener compuestos marcados con azufre, como sulfuros y mercaptanos alifaticos, y ciclicos, mediante sintesis directa empleando atomos de retroceso obtenidos por la reaccion 35Cl (n, p) 35S. Se obtuvieron atomos excitados de azufre-35 en la misma sustancia blanco, irradiando con neutrones en un reactor mezclas de CCl4 y un hidrocarburo ciclico (ciclopentano, ciclohexano). La memoria indica un procedimiento para irradiar las mezclas y separar despues los compuestos que contengan azufre utilizando metodos quimicos especificos, destilacion fraccionada, cromatografia sobre papel y cromatografia gas-liquido. Tambien explica la finalidad del intercambio. Los autores estudiaron la relacion entre el rendimiento de los diversos productos marcados con azufre y la composicion de la mezcla y el tipo de irradiacion, y determinaron el balance de azufre activo. Establecieron nuevos tipos de reacciones de azufre atomico: la sustitucion del grupo CH2 y la inclusion en el enlace C-C. La molecula se destruye en la interaccion, con atomos de azufre excitados. Estos atomos pueden iniciar la formacion de polimeros que contienen azufre. Se determino el rendimiento de estas reacciones. Hasta el 98% del azufre excitado aparece en forma de compuestos organicos de azufre. Se demostro que, en caliente, es posible sintetizar tiefeno, tetrahidrotiopirano, ciclopentilmercaptano, ciclohexilmercaptano, etilpropilbutilmercaptanos, sulfuro de diciclopentilo, mercaptanos polimerizados, etc., marcados con azufre. El rendimiento de varios compuestos marcados puede regularse dentro de amplios limites modificando las propiedades moderadoras del medio. (author)Abstract (Russian)
Rassmatrivayutsya metody polucheniya mechennykh po sere soedinenij - otkrytykh i tsiklicheskikh merkaptanov i sul'fidov, - osnovannye na pryamom sinteze s uchastiem atomov otdachi, poluchaemykh po reaktsii Cl35 (n, p) S35. Poluchenie goryachikh atomov S35 v srede veshchestva misheni osushchestvlyalos' putem oblucheniya v reaktore nejtronami smesej CCl4 i tsiklicheskogo uglevodoroda (tsiklopentan, tsiklogeksan). Izlagaetsya metodika oblucheniya smesej i posleduyushchego razdeleniya razlichnykh serosoderzhashchikh soedinenij s ispol'zovaniem spetsificheskikh khimicheskikh metodik, rektifikatsii, bumazhnoj i gazo-zhidkostnoj khromatografii. Vyyasnena rol' obmena. Issledovana zavisimost' vykhoda otdel'nykh mechennykh po sere produktov ot sostava smesi i kharaktera oblucheniya. Sveden balans po aktivnoj sere. Ustanovleny novye tipy reaktsij atomarnoj sery: zameshcheniya CH2-gruppy, vnedrenie po svyazi C-C. Obnaruzhena destruktsiya tsiklicheskoj molekuly pri vzaimodejstvii s goryachimi atomami sery. Pokazana sposobnost' goryachikh atomov sery initsiirovat' obrazovanie serosoderzhashchikh polimerov. Ustanovleny vykhody ehtikh reaktsij. Pokazano, chto do 98 % aktivnoj sery okazyvaetsya svyazannoj v forme seroorganicheskikh soedinenij. Pokazana vozmozhnost' goryachego sinteza mechennykh po sere tiofana, tetragidrotiopirana, tsiklopentilmerkaptana, tsiklogeksilmerkaptana, ehtilpropilbutilmerkaptanov, ditsiklopentilsul'fida, polimernykh merkaptanov i sul'fidov. Pokazana vozmozhnost' regulirovaniya v shirokikh predelakh vykhoda razlichnykh mechenykh soedinenij putem izmeneniya zamedlyayushchikh svojstv sredy. (author)Additional details
Additional titles
- Original title (Russian)
- Обтентион де cомпосес марqуес ау соуфре пар реаcтион дьатомес де соуфре-35 еxcитес авеc дес хыдроcарбурес cыcлиqуес; Получение меченных по сере соединений в результате реакции ''горячих'' атомов серы-35 с циклическими углеводородами; Методос пара обтенер cомпуестос марcадос cон азуфре медианте ла реаccион де атомос еxcитадос де азуфре-35 cон хидроcарбурос
Publishing Information
- Publisher
- Globus, Druck- und Verlagsanstalt
- Imprint Place
- Vienna (International Atomic Energy Agency (IAEA))
- Imprint Title
- Radioisotopes in the Physical Sciences and Industry. Proceedings of the Conference on the Use of Radioisotopes in the Physical Sciences and Industry. V. III
- Imprint Pagination
- 652 p.
- Series
- Proceedings Series
- Journal Page Range
- p. 27-41
- ISSN
- 0074-1884
Conference
- Title
- Conference on the Use of Radioisotopes in the Physical Sciences and Industry
- Dates
- 6-17 Sep 1960
- Place
- Copenhagen (Denmark)
INIS
- Country of Publication
- International Atomic Energy Agency (IAEA)
- Country of Input or Organization
- International Atomic Energy Agency (IAEA)
- INIS RN
- 43113000
- Subject category
- S37: INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY; S07: ISOTOPES AND RADIATION SOURCES;
- Resource subtype / Literary indicator
- Conference
- Descriptors DEI
- HYDROCARBONS; INTERACTIONS; LABELLED COMPOUNDS; LIQUID COLUMN CHROMATOGRAPHY; POLYMERS; RECOILS; SULFIDES; SULFUR; SULFUR 35; SYNTHESIS; THIOLS
- Descriptors DEC
- BETA DECAY RADIOISOTOPES; BETA-MINUS DECAY RADIOISOTOPES; CHALCOGENIDES; CHROMATOGRAPHY; DAYS LIVING RADIOISOTOPES; ELEMENTS; EVEN-ODD NUCLEI; ISOTOPES; LIGHT NUCLEI; NONMETALS; NUCLEI; ORGANIC COMPOUNDS; ORGANIC SULFUR COMPOUNDS; RADIOISOTOPES; SEPARATION PROCESSES; SULFUR COMPOUNDS; SULFUR ISOTOPES
Optional Information
- Notes
- 6 figs, 2 tabs, 4 refs
- Secondary number(s)
- STI/PUB--20(Vol.3)