SU883712A1 - Method of qualitative determination of impurityes in tetrachlorethylene - Google Patents

Method of qualitative determination of impurityes in tetrachlorethylene Download PDF

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Publication number
SU883712A1
SU883712A1 SU792777187A SU2777187A SU883712A1 SU 883712 A1 SU883712 A1 SU 883712A1 SU 792777187 A SU792777187 A SU 792777187A SU 2777187 A SU2777187 A SU 2777187A SU 883712 A1 SU883712 A1 SU 883712A1
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SU
USSR - Soviet Union
Prior art keywords
tetrachlorethylene
qualitative determination
impurityes
processing
determination
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SU792777187A
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Russian (ru)
Inventor
Станислав Витальевич Рыков
Борис Данилович Свиридов
Григорий Алексеевич Никифоров
Людвига Исх-Бен-Юминовна Петровская
Альфред Зиновьевич Янкелевич
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Предприятие П/Я А-7815
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Priority to SU792777187A priority Critical patent/SU883712A1/en
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Publication of SU883712A1 publication Critical patent/SU883712A1/en

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  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
  • Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)

Description

(54)СПОСОБ КАЧЕСТВЕННОГО ОПРЕДЕЛЕНИЯ ПРИМЕСЕЙ В ТЕТРАХЛОРЭТИЛЕНЕ(54) METHOD FOR QUALITATIVE DETERMINATION OF IMPURITIES IN TETRACHLORETHYLENE

1one

Изобретение относитс  к аналитической химии, в именно к способам качественного определени  примесей в тетрахлорэтилене. .сThe invention relates to analytical chemistry, in particular to methods for the qualitative determination of impurities in tetrachlorethylene. .with

Известен способ качественного определени  примесей в тетрахлорэтилене, заключающийс  в обработке анализируемой пробы смесью крахмала, едкого кали, йодистого кали, при кип чении JQ до получени  синей окраски tl}.A known method for the qualitative determination of impurities in tetrachlorethylene, which consists in treating the sample being analyzed with a mixture of starch, potassium hydroxide, and potassium iodide, while boiling JQ to obtain a blue color tl}.

Недостатками способа  вл етс  длительность определени  - 35-40 мин.The disadvantages of this method are the duration of determination - 35-40 minutes.

Наиболее близким к описываемому изобретению по технической сущности и достигаемому результату  вл етс  5 способ качественного определени  примесей в тетрахлорэтилене, заключающийс  в обработке анализируемой пробы :НОнаном с последующим хроматографи- . рованием полученного раствора Г2. 20The closest to the described invention by its technical essence and the achieved result is 5 methods for the qualitative determination of impurities in tetrachlorethylene, which consists in processing the sample being analyzed: NOHNAN, followed by chromatography. the obtained solution G2. 20

Недостатком способа  вл етс  длительность определени .The disadvantage of this method is the duration of the determination.

Цель изобретени  - сокращение времени определени .25The purpose of the invention is to reduce the time to determine .25

Поставленнёш цель достигаетс  тем, что в качестве органического реагента дл  обработки анализируемой пробы используют хинондиазид и при температуре 90-100°С регистрируют спектры 30The goal is achieved by using quinone diazide as an organic reagent for processing the sample being analyzed and spectra are recorded at a temperature of 90-100 ° C

 дерного магнитного резонанса раствора , полученного после обработки.nuclear magnetic resonance of the solution obtained after processing.

Пример 1. КО,5 МП тетрахлорэтилена особой очистки добавл етс  10 мг хинондиазида, ампула помещаетс  в датчик спектрометра ЯМР, имеющий температуру , и затем снимаетс  спектр ПМР в области 5-8 м.д. Сигналы отрицательной пол рности отсутствуют , что .свидетельствует об отсутствии (210-4 м/л) . Врем  анализа 10-15 мин.Example 1. KO, 5 MP of tetrachlorethylene of special purification, 10 mg of quinone diazide is added, the ampule is placed in the sensor of the NMR spectrometer, which has a temperature, and then the PMR spectrum is taken in the range of 5-8 ppm There are no negative polarity signals, indicating a lack of (210-4 m / l). Analysis time 10-15 min.

Пример 2. КО,5 мл ТХЭ, насыщенного газообразным хлором, добавлено 20 мг хинондиазида. В спектре ПМР, сн том при 100°С, видны сигналы отрицательной пол рности мета-протонов продукта реакции карбена с хлором , что свидетельствует о загр зненности тетрахлорэтилена. Продукт можетExample 2. KO, 5 ml of TCE, saturated with chlorine gas, added 20 mg of quinone diazide. In the PMR spectrum, taken at 100 ° С, there are visible signals of the negative polarity of the meta-protons of the reaction product of carbene with chlorine, which indicates that the tetrachlorethylene is contaminated. Product can

быть идентифицирован как Оbe identified as o

количеству образовани  которого можно судить,что хлор в растворе содержитс  в кон1;ентрации 10 м/л. Врем  полного анализа 15 минут. 38837 Так как и предлагаемый и известный способ  вл ютс  качественными, то главное преимущество предлагаемого способа  вл етс  экспрессность. Врем  анализа сокращаетс  до 20 минут. Кроме того, предлагаекий способ поз-, вол ет определить наличие примесей в количестве 10 -10 м/л.the amount of the formation of which can be judged that the chlorine in the solution is contained in conen; concentration of 10 m / l. Full analysis time is 15 minutes. 38837 Since both the proposed and the known method are qualitative, the main advantage of the proposed method is expressivity. The analysis time is reduced to 20 minutes. In addition, the proposed method allows to determine the presence of impurities in the amount of 10 -10 m / l.

Claims (2)

1.ТУ 6-09-4084-75.1. TU 6-09-4084-75. 2.Ту 6-09-4084-75 (прототип). 24 Ьбработки анализируемой пробы органическим реагентом, отличающийс  тем, что, с целью сокращени  времени определени , в качестве органического реагента используют хинондиазид и при температуре 90ЮС С регистрируют спектры  дерного магнитного резонанса раствора, полученного после обработки.2. That 6-09-4084-75 (prototype). 24 processing the sample with an organic reagent, characterized in that quinone diazide is used as an organic reagent to reduce the determination time and nuclear magnetic resonance spectra of the solution obtained after processing are recorded at a temperature of 90 ° C.
SU792777187A 1979-06-06 1979-06-06 Method of qualitative determination of impurityes in tetrachlorethylene SU883712A1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
SU792777187A SU883712A1 (en) 1979-06-06 1979-06-06 Method of qualitative determination of impurityes in tetrachlorethylene

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
SU792777187A SU883712A1 (en) 1979-06-06 1979-06-06 Method of qualitative determination of impurityes in tetrachlorethylene

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SU883712A1 true SU883712A1 (en) 1981-11-23

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