Аналитический контроль получения экзо,экзо- и эндо,эндо- диметиловых эфиров норборнен-2,3-дикарбоновой кислоты
| Parent link: | Сорбционные и хроматографические процессы.— , 2000- Т 16, № 2.— 2016.— [С. 241-250] |
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| Other Authors: | , , , , |
| Summary: | Заглавие с экрана Представлен способ идентификации и количественного определения основных компонентов реакции Дильса-Альдера: исходных реагентов диметилмалеата и дициклопентадиена и продуктов их взаимодействия экзо,экзо- и эндо,эндо- диметиловых эфиров норборнен-2,3-дикарбоновой кислоты методом газовой хромато-масс-спектрометрии. Определены параметры идентификации анализируемых соединений (получены масс-спектры и линейные индексы удерживания). Установлено, что предлагаемый количественный метод является точным, правильным и воспроизводимым и может быть применен при аналитическом контроле технологии получения экзо,экзо- и эндо,эндо- диметиловых эфиров норборнен-2,3-дикарбоновой кислоты. The quality of raw materials and conditions of the Diels-Alder reaction between dimethyl maleate and dicyclopentadiene have a significant influence on the isomeric consist of the received dimethyl esters norbornene-2,3-dicarboxylic acid. Polymers (polyendicate) with different optical and physico-mechanical properties can be obtained by varying the ratio of exo,exo- and endo,endo- isomers in monomer. Thus, analytical control is extremely important for the production isomers dimethyl esters norbornene-2,3-dicarboxylic acid. Study was carried out to develop a simple gas chromatographic method for quantitative analysis of the main compounds of Diels-Alder reaction between dimethyl maleate and dicyclopentadiene. The qualitative analysis was performed by similarity searches in the National Institute of Standards and Technology (NIST) mass spectra database with the obtained pure mass spectrum of each component and by comparison of temperature-programmed retention indices (PTRI) with authentic standards included in our own laboratory database under construction. Quantitative parameters, such as the linear range, correlation coefficient were also investigated. The extracted standard curves obtained in the linear ranges showed excellent linearities with coefficients of correlation that were greater than 0.99. Accuracy of the method was determined using the six times analysis of the samples. The RSD values for accuracy was ? 1.74% and Fisher criterion for two days was not exceed the critical value of 5.05 for all compounds. To check the suitability the method was applied to determine reaction mixture consist in the standard mixes. The obtained results demonstrate good method recoveries, the RSD was less than 3 % in all cases. To check the suitability the method was applied to determine reaction mixture consist in the standard mixes. The obtained results demonstrate good method accuracy. Режим доступа: по договору с организацией-держателем ресурса |
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2016
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| Online Access: | http://www.sorpchrom.vsu.ru/articles/20160213.pdf http://elibrary.ru/item.asp?id=25794282 |
| Format: | Electronic Book Chapter |
| KOHA link: | https://koha.lib.tpu.ru/cgi-bin/koha/opac-detail.pl?biblionumber=648383 |