RU1838332C - Method of preparing of polymeric sorbent for chromatography - Google Patents
Method of preparing of polymeric sorbent for chromatographyInfo
- Publication number
- RU1838332C RU1838332C SU915015825A SU5015825A RU1838332C RU 1838332 C RU1838332 C RU 1838332C SU 915015825 A SU915015825 A SU 915015825A SU 5015825 A SU5015825 A SU 5015825A RU 1838332 C RU1838332 C RU 1838332C
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- RU
- Russia
- Prior art keywords
- chromatography
- sorbent
- sulfuric
- mixture
- preparing
- Prior art date
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- Treatment Of Liquids With Adsorbents In General (AREA)
Abstract
Использование: синтез сорбентов дл газохроматографического анализа, дл кон- центрировани и разделени смесей пол рных органических соединений. Сущность изобретени : жидкофазное нитрование сополимера стирола с дивинилбензолом смесью 94%-ной серной и 56%-ной азотной кислот в соотношении 1:1. Одновременное облучение рентгеновским излучением экспозиционной дозой 800-2400 рентген. 1 табл,Usage: synthesis of sorbents for gas chromatographic analysis, for the concentration and separation of mixtures of polar organic compounds. SUMMARY OF THE INVENTION: liquid phase nitration of a styrene-divinylbenzene copolymer with a mixture of 94% sulfuric and 56% nitric acids in a 1: 1 ratio. Simultaneous x-ray irradiation with an exposure dose of 800-2400 x-rays. 1 tab
Description
Изобретение относитс к способам получени полимерных сорбентов дл молекул рной хроматографии, и может быть использовано в хроматографическом анализе дл концентрировани и разделени пол рных органических соединений.The invention relates to methods for producing polymer sorbents for molecular chromatography, and can be used in chromatographic analysis to concentrate and separate polar organic compounds.
Целью изобретени вл етс повышение хроматографической пол рности полимерного сорбента дл хроматографии на основе сополимера стирола-дивинилб ензо- ла.An object of the invention is to increase the chromatographic polarity of a polymer sorbent for chromatography based on a styrene-divinylbenzene copolymer.
Поставленна цель достигаетс путем смешени полимерного сорбента со смесью 94% серной и 56% азотной кислот с последующей экспозицией в поле рентгеновского излучени экспозиционными дозами 800- 2400 Рентген.This goal is achieved by mixing the polymer sorbent with a mixture of 94% sulfuric and 56% nitric acids, followed by exposure to the x-ray field with exposure doses of 800-2400 X-rays.
Сопоставительный анализ предлагаемого решени с прототипом показывает, что за вл емый способ отличаетс от известного тем, что нитрование производ т смесьюA comparative analysis of the proposed solution with the prototype shows that the claimed method differs from the known one in that nitration is carried out with a mixture
серной и азотной кислот в процессе рентгеновского облучени .sulfuric and nitric acids during x-ray irradiation.
Технический результат, получаемый при использовании за вл емого решени выражаетс в повышении величины хроматографической пол рности получаемого сорбента.The technical result obtained by using the claimed solution is expressed in an increase in the chromatographic polarity of the resulting sorbent.
П р и м е р 1. Навеску фракции 0,25-0,50 мм полимерного сорбент., полисорб-1 ( 09-3602-74) помещают в полиэтиленовый бюкс, затем заливают смесью серной (94%) и азотной (56%) кислот (в соотношении 1:1) в количестве, по объему равном обьему сорбента , и герметично облучают. Затем сосуд выдерживают в поле рентгеновского излучени аппарата РАП 150/30.0-14 с нэпр же- . нием на трубке 100-300 кВ при токе 10,«А до достижени экспозиционной дозы 800 Рентген. После этого бюкс вскрывают, сорбент отмывают водой до нейтральной реакции , затем сушат. Из сухого сорбента готов т газохроматографическую насадочt/s СPRI me R 1. A portion of the fraction of 0.25-0.50 mm polymer sorbent., Polysorb-1 (09-3602-74) is placed in a polyethylene bottle, then pour a mixture of sulfuric (94%) and nitrogen (56% ) acids (in a ratio of 1: 1) in an amount equal to the volume of the volume of the sorbent, and hermetically irradiated. Then the vessel is kept in the X-ray field of the RAP apparatus 150 / 30.0-14 with NEP. with a tube of 100-300 kV at a current of 10, A until the exposure dose of 800 X-rays is reached. After this, the bucks are opened, the sorbent is washed with water until neutral, then dried. A gas chromatographic packing / s C is prepared from a dry sorbent
00 00 00 CJ СО ГчЭ00 00 00 CJ SO GCE
СО With
ную колонку (0,5 м х 3 мм) и помещают в термостат хроматографа, оснащенного детектором по теплопроводности, Дл определени пол рности сорбента провод т анализ тестовых соединений по Роршнай- деру - Мак Рейнольдсу и рассчитывают коэффициенты пол рности A Ix, у, z, и, s и общую пол рности ЈД. Расчет коэффициентов пол рности дл облученных сорбентов (RESN), прототипа, полисорба-1 и контрольного образца, полученного нитрованием полис рба-Ч смесью серной и азотной кислот в тех же услови х, что и за вл емое решение, но без облучени (KN) провод т относительно неспецифического, непол рного полимерного сорбента пора- пак Q.a column (0.5 mx 3 mm) and placed in a thermostat of a chromatograph equipped with a thermal conductivity detector. To determine the polarity of the sorbent, test compounds are analyzed by the Rorschneider – Mac Reynolds test and the polarity coefficients A Ix, у, z are calculated , and, s and the general polarity ЈД. Calculation of polarity coefficients for irradiated sorbents (RESN), prototype, polysorb-1 and a control sample obtained by nitrating polys-rba-Ch with a mixture of sulfuric and nitric acids under the same conditions as for the claimed solution, but without irradiation (KN) a relatively non-specific, non-polar polymeric sorbent Q-Q is carried out.
Аналогичным способом провод т облучение и тестирование сорбентов дл других экспозиционных доз в указанном интервале (800-2400 Р). Результаты приведены в таблице .The sorbents were irradiated and tested in a similar way for other exposure doses in the indicated range (800-2400 R). The results are shown in the table.
Как видно из таблицы, использование предлагаемого способа получени полимерного сорбента дл хроматографии позвол ет достигать величины хроматографической пол рности ( JA ) в 2 раза большей, чем у способа-п рототи па.As can be seen from the table, the use of the proposed method for producing a polymer sorbent for chromatography allows achieving a chromatographic polarity (JA) of 2 times greater than that of the method of prototyping.
Техническа осуществл емость предлагаемого изобретени достаточно очевидна, поскольку используетс серийно производимый рентгеновский аппарат РАП 150/300-14The technical feasibility of the present invention is quite obvious, since a commercially available x-ray apparatus RAP 150 / 300-14 is used.
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и товарно производимые компоненты: сополимер стирола-дивинилбензола (полисорб- 1) ТУ-б-09-3602-74 и серна (94%) и азотна (56%) кислоты.and commercially produced components: styrene-divinylbenzene (polysorb-1) copolymer TU-b-09-3602-74 and sulfuric acid (94%) and nitric acid (56%).
Пол рные полимерные сорбенты, полученные за вл емым способом, найдут широкое применение в аналитических, санитарно-эпидемиологических службах, экологических, природоохранных, заводских лаборатори х, подразделени х технического контрол технологических процессов, исходного сырь , готовой продукции, при определении степени загр знени сточных вод, воздуха производственных и бытовых помещений в качестве материала дл сорбционно- го концентрировани (пробоотбора) микропримесей токсичных органических соединений . Такие сорбенты могут использоватьс в качестве насадок газохроматографических колонок дл разделени смеси пол рных и непол рных органических веществ.Polar polymer sorbents obtained by the claimed method will find wide application in analytical, sanitary and epidemiological services, environmental, environmental, factory laboratories, units of technical control of technological processes, feedstock, finished products, in determining the degree of pollution of wastewater air of industrial and domestic premises as a material for sorption concentration (sampling) of microimpurities of toxic organic compounds. Such sorbents can be used as packing gas chromatographic columns to separate a mixture of polar and non-polar organic substances.
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SU915015825A RU1838332C (en) | 1991-12-06 | 1991-12-06 | Method of preparing of polymeric sorbent for chromatography |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SU915015825A RU1838332C (en) | 1991-12-06 | 1991-12-06 | Method of preparing of polymeric sorbent for chromatography |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| RU1838332C true RU1838332C (en) | 1993-08-30 |
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ID=21591172
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| SU915015825A RU1838332C (en) | 1991-12-06 | 1991-12-06 | Method of preparing of polymeric sorbent for chromatography |
Country Status (1)
| Country | Link |
|---|---|
| RU (1) | RU1838332C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1321736C (en) * | 2003-08-14 | 2007-06-20 | 江苏工业学院 | Resin adsorbent for desulfurizing hydrocarbon and its prepn |
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1991
- 1991-12-06 RU SU915015825A patent/RU1838332C/en active
Non-Patent Citations (1)
| Title |
|---|
| Llndsay-Smlth J.R., Tameesh А.Н.Н., Waddlngton D.I, J.Chromatogr. 1978, Vol.148, P.353-363. Llndsay-Smith J.R., Tameesh A.H.H., Waddington D.I. J.Chromatogr. 1978, Vol.151, p.21-26. * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1321736C (en) * | 2003-08-14 | 2007-06-20 | 江苏工业学院 | Resin adsorbent for desulfurizing hydrocarbon and its prepn |
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