SU1247717A1 - Method of preparing specimen of pyrophoric alkyl compounds of elements for determining microimpurities in it - Google Patents
Method of preparing specimen of pyrophoric alkyl compounds of elements for determining microimpurities in it Download PDFInfo
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- SU1247717A1 SU1247717A1 SU843829680A SU3829680A SU1247717A1 SU 1247717 A1 SU1247717 A1 SU 1247717A1 SU 843829680 A SU843829680 A SU 843829680A SU 3829680 A SU3829680 A SU 3829680A SU 1247717 A1 SU1247717 A1 SU 1247717A1
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Abstract
Изобретение относитс к аналитической химии, а точнее, способу подготовки образца пирофорных алкильных соединений элементов дл определени в нем микропримесей. Цель изобретени - повьппение техники безопасности способа. Подготовку образца ведут гидролизо м анализируемой пробы водой в реакторе в атмосфере инертного газа. Навеску анализируемой пробы и воду помещают раздельно на.рассто нии 0,2-22 мм друг от друга. В полученных продуктах гидролиза определ ют микропримеси .известными способами. i (Л 1C 4 vj The invention relates to analytical chemistry, and more specifically, to a method for preparing a sample of pyrophoric alkyl compounds of elements for determining microimpurities therein. The purpose of the invention is to follow the safety method. Sample preparation is carried out by hydrolysis of the sample being analyzed with water in a reactor in an inert gas atmosphere. A sample of the analyzed sample and water are placed separately at a distance of 0.2–22 mm from each other. In the resulting hydrolysis products, trace impurities are determined by known methods. i (L 1C 4 vj
Description
Изобретение относитс к аналитической химии, а именно к способам подготовки образцов пирофорных ап- кильных соединений.элементов.This invention relates to analytical chemistry, in particular, to methods for preparing samples of pyrophoric acyl compounds.
Целью изобретени вл етс позы- шение техники безопасности за счет улучшени контрол за ходом реакции.The aim of the invention is the safety posturing by improving the control of the reaction course.
Изобретение иллюстрируетс следующими пример . .The invention is illustrated by the following example. .
пример 1. Через реактор, разделенный на цва отсека и отделенный от атмосферы гидрозатвором, продувают осушенный и очищенный на цеолитах и алюмогеле азот. Помещают в один отсек 2 г триметилгалли , в другой 2 г воды. Рассто ние между поверхност ми жидкостей 0,2 мм. Газообразные продукты реакции пропускают через барботеры с поглотительной смесью (алифатический или алицикли- ческий углеводород с высокой степенью чистоты по отношению к анализируемым примес м) дл улавливани примесей. Врем проведени разложени около 6 мин. Окончание процесса газовыделени фиксируют визуально по прекращению барботажа выдел ющихс газов в поглотительных барботерах. Твердые продукты разложени раствор ют в особо чистой сол ной кислоте дл после- дующего анализа на содержание микропримесей . Получают 1,5 г оксида галли . Example 1. Through the reactor, divided into the color of the compartment and separated from the atmosphere by a hydraulic seal, nitrogen is drained and purified on zeolites and aluminum gel. Place in one compartment 2 g of trimethylgalli, in the other 2 g of water. The distance between the surfaces of liquids is 0.2 mm. The gaseous reaction products are passed through spargers with an absorption mixture (an aliphatic or alicyclic hydrocarbon with a high degree of purity with respect to the impurities to be analyzed) to trap impurities. Decomposition time is about 6 minutes. The end of the gassing process is recorded visually upon the termination of the bubbling of the evolved gases in the absorption bubblers. The solid decomposition products are dissolved in especially pure hydrochloric acid for subsequent analysis of the content of microimpurities. 1.5 g of gallium oxide are obtained.
Пример 2. Провод т процесс аналогично примеру 1 с тем отличием, что через реактор посто нно продувают осушенный аргон (система разомкнута ) . Определено, что произошёл унос 70-80% определ емой микропримеси серыExample 2. The process is carried out analogously to example 1 with the difference that dried argon is continuously purged through the reactor (the system is open). It was determined that 70-80% of the detected sulfur trace was carried off.
Пример 3. Провод т аналогич- но примеру 1. Помещают в один отсек 2 г диметилцинка, а в другой 2 г воды.Example 3. It is carried out similarly to Example 1. 2 g of dimethyl zinc are placed in one compartment, and 2 g of water in the other.
Рассто ние между поверхност ми жидкостей 25 мм. После окончани га- зовыделени (0,6 ч) реактор вкрывают и вьщелившийс твердый продукт подвергают термообработке в среде очи- щенного при 900-1 . Получают 1,5 г оксида цинка.The distance between the surfaces of liquids is 25 mm. After termination of the gas release (0.6 h), the reactor is covered and the solid product which has leaked out is subjected to heat treatment in the medium cleaned at 900-1. 1.5 g of zinc oxide are obtained.
Пример 4. Провод т процесс аналогично примеру 3 с тем отличием, что рассто ние между поверхност ми жидкостей 30 мм. Процесс разложени идет 4,5 ч. Получают 1,6 г оксида цинка. . Example 4. The process is carried out as in Example 3 with the difference that the distance between the surfaces of the liquids is 30 mm. The decomposition process takes 4.5 hours. 1.6 g of zinc oxide are obtained. .
Пример 5. Провод т процесс аналогично примеру 3 с тем отличием, что рассто ние между поверхност ми . жидкостей 0,2 мм. Врем проведени разложени 0,1 ч. Получено 1,6 г оксида цинка.Example 5. The process is carried out as in Example 3 with the difference that the distance between the surfaces. liquids 0.2 mm. The decomposition time was 0.1 h. 1.6 g of zinc oxide was obtained.
Пример 6. Провод т процесс аналогично примеру 3 с тем отличием,, что рассто ние между поверхност ми О,1 мм. Процесс проходит с сильным разогревом и выбросом реагентов. Получено 0,5 г оксида цинка.Example 6. The process is carried out as in Example 3 with the difference that the distance between the surfaces is 0, 1 mm. The process takes place with a strong heating and emission of reagents. Received 0.5 g of zinc oxide.
Подготовка обр азцов алкильных соединений элементов, таких как триме- тилгаллий, диметилцинк и др., по известному способу приводит к возгоранию и взрыву с потерей анализируемых соединений.Preparation of samples of alkyl compounds of elements, such as trimethylgallium, dimethylzinc, etc., by a known method leads to fire and an explosion with the loss of the analyzed compounds.
Предлагаемый способ может быть использован при экспресс-анализе на содержание микропримесей в алкилме- таллах, получении высокочистых эталонных образцов оксидов и гидроксид- ных элементов, примен емых в новых отрасл х науки и техники. Применение предлагаемого способа позвол ет повысить , технику безопасности за счет улучшени контрол за ходом реакции.The proposed method can be used for the rapid analysis of the content of microimpurities in alkyl metals, the preparation of high-purity reference samples of oxides and hydroxide elements used in new fields of science and technology. The application of the proposed method allows an increase in safety engineering by improving the control over the course of the reaction.
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SU843829680A SU1247717A1 (en) | 1984-12-21 | 1984-12-21 | Method of preparing specimen of pyrophoric alkyl compounds of elements for determining microimpurities in it |
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SU843829680A SU1247717A1 (en) | 1984-12-21 | 1984-12-21 | Method of preparing specimen of pyrophoric alkyl compounds of elements for determining microimpurities in it |
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SU1247717A1 true SU1247717A1 (en) | 1986-07-30 |
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1984
- 1984-12-21 SU SU843829680A patent/SU1247717A1/en active
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