SU247608A1 - METHOD OF ANALYSIS OF POLYMERS - Google Patents
METHOD OF ANALYSIS OF POLYMERSInfo
- Publication number
- SU247608A1 SU247608A1 SU1191816A SU1191816A SU247608A1 SU 247608 A1 SU247608 A1 SU 247608A1 SU 1191816 A SU1191816 A SU 1191816A SU 1191816 A SU1191816 A SU 1191816A SU 247608 A1 SU247608 A1 SU 247608A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- polymers
- pyrolysis
- analysis
- polymer
- metal filament
- Prior art date
Links
- 229920000642 polymer Polymers 0.000 title description 16
- 238000004458 analytical method Methods 0.000 title description 5
- 238000000197 pyrolysis Methods 0.000 description 10
- UHOVQNZJYSORNB-UHFFFAOYSA-N benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 239000003990 capacitor Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229920001195 polyisoprene Polymers 0.000 description 2
- 239000005977 Ethylene Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 238000009432 framing Methods 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 230000003301 hydrolyzing Effects 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- -1 methylvinylsiloxane Chemical class 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 238000010517 secondary reaction Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 125000005373 siloxane group Chemical group [SiH2](O*)* 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
Description
Изобретение относитс к способам анализов полимеров, преимущественно к способам анализов состава продуктов, образующихс при гидролизе полимеров в инертной атмосфере с помощью газовой хроматографии.The invention relates to methods for analyzing polymers, preferably to methods for analyzing the composition of products formed by hydrolyzing polymers in an inert atmosphere using gas chromatography.
Известен способ анализа полимеров путем пиролиза их на металлической нити и последующего газохроматографического анализа. Однако известный способ не позвол ет получить воспроизводимых результатов и представительного характеристического спектра продуктов пиролиза, так как врем пиролиза при этом, как правило, велико, что осложн ет и искажает пиролиз за счет протекани побочных реакций.There is a method of analyzing polymers by pyrolysis of them on a metal filament and subsequent gas chromatographic analysis. However, the known method does not allow to obtain reproducible results and a representative characteristic spectrum of pyrolysis products, since the pyrolysis time is, as a rule, long, which complicates and distorts pyrolysis due to side reactions.
Цель изобретени - упрощение анализа полимеров.The purpose of the invention is to simplify the analysis of polymers.
С этой целью на металлическую нить, содержащую тонкую пленку полимера, подают контролируемый по длительности и энергии импульсный разр д от конденсатора.To this end, a pulsed discharge from a capacitor, controlled in duration and energy, is supplied to a metal filament containing a thin film of polymer.
Сущность изобретени заключаетс в том, что производ т сожжение микрограммовых навесок полимера, наносимых из разбавленных ра.створов на вольфрамовую нить, в короткое врем за счет разр да от конденсатора.The essence of the invention is that the microgram samples of the polymer are applied, which are applied from the diluted solutions to the tungsten filament, in a short time due to the discharge from the capacitor.
Способ по сн етс примерами.The method is illustrated by examples.
1%-;ный бензольный ра:твор полиизопрена регул рного строени . После удалени растворител образец полимера сжигают в потоке аргона непосре.дственно перед колонкой хроматографа «Хром-2 (пламенно-ионизационного детектора) путем разр да батареи конденсаторов общей емкостью до 3000 мф, зар жаемых до потенциала 30 в. Выдел ема в импульсе энерги достигает 1,35 дж. Врем пиролиза и параметры импульса, привод щие к пиролизу полиизопрена до мономера, подбирают опытным путем (табл. 1).1%; benzene: benzene polyisoprene with a regular structure. After removing the solvent, the polymer sample is burned in an argon stream immediately before the Chrom-2 chromatograph column (flame ionization detector) by discharging a battery of capacitors with a total capacity of up to 3000 mf charged to 30 volts. The energy released in a pulse reaches 1.35 j. The time of pyrolysis and the pulse parameters leading to the pyrolysis of polyisoprene to the monomer are selected empirically (Table 1).
Таблица 1Table 1
1515
2020
Таким образом, становитс возможным вести направленный пиролиз полимера дл получени наиболее полной информации о строеНИИ основного звена цепи Полимера.Thus, it becomes possible to conduct directional pyrolysis of the polymer to obtain the most complete information about the structure of the main chain link of the Polymer.
Пример 2. Параметры нити соответствуют указанным в примере 1. Пиролиз метилвинилсилоксановых полимеров осуществл ют при энергии импульса 0,6 дж. В этих услови хExample 2. The parameters of the thread correspond to those given in Example 1. The pyrolysis of methylvinylsiloxane polymers is carried out with a pulse energy of 0.6 J. Under these conditions
центрации образа.равщихс этилена к метану, рассчитанное из хроматограммы, пропорционально срдержаний винильных групп в полимере . Способ позвол ет получать количественнУе да;нные по составу боковых групп, обрамл ющих силоксановую цепь (табл. 2).the concentration of ethylene to methane, calculated from the chromatogram, is proportional to the vinyl groups in the polymer. The method allows to obtain quantitative; the composition of the side groups framing the siloxane chain (Table 2).
Та блица 2Table 2
Отношение концентрацииConcentration ratio
С,Н4C, H4
в газах пиролизаin pyrolysis gases
СНдSnd
0,50 0,85 1,20 1,850.50 0.85 1.20 1.85
Таким образом, отсутствие .вторичных реакций при пиролизе полимеров, осуществл емом предлагаемым способом, позвол ет производить анализ полимеров, который наиболее полно отражает строение и состав полимера.Thus, the absence of secondary reactions during the pyrolysis of polymers, carried out by the proposed method, allows the analysis of polymers to be carried out, which most fully reflects the structure and composition of the polymer.
Предмет изобретени Subject invention
Способ анализа, полимеров путем термического разложени на металлической нити с последующим хроматографическим разделением продуктов разложени и детектированием их, отличающийс тем, что, с целью унрощени анализа, на металлическую нить подают контролируемый по энергии и длительности импульсный разр д.The method of analysis of polymers by thermal decomposition on a metal filament, followed by chromatographic separation of decomposition products and their detection, characterized in that, in order to simulate the analysis, a pulsed discharge controlled by energy and duration is applied to the metal filament.
Publications (1)
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