SU1033181A1 - Method of treating polymeric sorbent for chromatography - Google Patents
Method of treating polymeric sorbent for chromatography Download PDFInfo
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- SU1033181A1 SU1033181A1 SU823394244A SU3394244A SU1033181A1 SU 1033181 A1 SU1033181 A1 SU 1033181A1 SU 823394244 A SU823394244 A SU 823394244A SU 3394244 A SU3394244 A SU 3394244A SU 1033181 A1 SU1033181 A1 SU 1033181A1
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- sorbent
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- inert gas
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Abstract
СПОСОБ ОБРАБОТКИ ПОЛИМЕРНОГО СОРБЕНТА ДЛЯ ХРОМАТОГРАФИИ, преимущественно на основе сополимера стирола и дивинилбензола путем его нагревани в токе инертного газа, о тл и чают и и с тем, что, с целью повышени термостойкости сорбента, предварительно сорбент облучают гамма-излучением изото- . па экспозиционной дозой 2«10 :о 3 -10 рентген,A METHOD FOR TREATING POLYMERIC SORBENT FOR CHROMATOGRAPHY, mainly based on a copolymer of styrene and divinylbenzene by heating it in a stream of inert gas, about tl, and with the fact that, in order to increase the heat resistance of the sorbent, the sorbent is irradiated with gamma radiation isotope. PA exposure dose of 2 "10: about 3 -10 x-ray,
Description
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СдЭ Изобретение относитс к способам обработки полимерного сорбента дл хроматографии и может быть испольэо ваноу.дл анализа нормальных углеводородов , спиртов, органических кисЗТот , ароматических углеводородов, их смесей и водных растворов в различных отрасл х химической проквд ленности . Известен способ обработки полиме ного сорбента дл хроматографии на основе сополимера стирола и дивинил бензола путем его нагревани в токе инертного газа при 1бО-250°С в течение 18-24 ч 1}. Недостатком способа вл етс недостаточна термостойкость сорбента (250°С). Цель изобретени - повышение тер мостойкости сорбента. Поставленна цель достигаетс согласно способу, включающему облучение полимерного сорбента на основе сополимера стирола и дивинилбензола гамма-излучейием экспозиционной дозой 2 «10 - 310 Р с по ледующим нагреванием в токе инертного газа. При экспозиционной дозе облуче-ни менее 21о9 рентген температура начала разложени ниже 2бО°С, а при увеличении экспозиционной до зы сверх 3-10 наблюдаетс уменьшение термостабильности сорбента (ниже 270°С). Пример 1. Берут фракцию 0,25-0,5 мм полимерного сорбента полисорб-1 (ТУ-б-09-3602-74) и заполн ют им газохроматографичёскую колонку. Сорбент в колонке облучаю гамма-излучением изотопа Со экспо зиционной ДОЗОЙ 4 После чего прогревают в токе инертного газа Л гели ) в течение 5 ч при 200°С. Затем определ ют температу эу на чала разложени сорбента по термогравиметрическим кривым, полученны на дериватографе при скорости нагре- ва З с/мин в атмосфере инертного гаэа (гели ). В качестве эталона сравнени используют предварительно прокаленную окись алюмини (). Температура начала разложени сое-, тавл ет З20с. Затем колонку помещают в термостат хроматографа (ЛХМ-8МД 5 модификации ) с детектором по теплопроводности . Анализ провод т при 300±1 С. В. качестве объекта- Дл анализа используют такие смеси, как смесь состава: метанол; этанолу пропанол/ бутанол; пентанол и,смесь состава: н-пентан, н -гексан н -гептан; н -октан; М-нонан н-декан. Объем вводимой пробы 0,2 мкм Ло- полученным хроматограммам провод т расчет эффективности колонки (по ГОСТ 17567-727 по компонентам смеси (таблица). Пример 2. Берут фракцию 0,25-0,5 мм полимерного сорбента полисорб-1 (ТУ-б-09-3602-74) и заполн ют им газохроматографичёскую 1Солонку . Сорбент в колонке облучают гамма-излучением изотопа Со экспозиционной дозой Р, после чего прогревают в токе инертного газа (гели )в течение 4 ч при . Температура начала разложени сорбента составл ет 340Рс. Затем колонку помещают в термостат хроматографа (ЛХМ-8МД 5 модификации) с детектором по теплопроводности. Анализ провод т при 300±1 С. В качестве объекта анализа используют такие смеси, как смесь состава: метанол ( этанол, пропанол j бутанол; пентанол и смесь состава: Н-пентан Н-гексан) н-гептан; н-октан; н-нонан; н-декан. Объем вводимой пробы 0,2 мкм. В таблице приведены результаты расчетов по полученным хроматограммам эффективности колонки по компонентам смеси.Sde The invention relates to methods for treating a polymeric sorbent for chromatography and can be used to analyze normal hydrocarbons, alcohols, organic acids, aromatic hydrocarbons, their mixtures and aqueous solutions in various chemical fields. A known method of treating a polymeric sorbent for chromatography based on a copolymer of styrene and divinyl benzene by heating it in a stream of inert gas at IBO-250 ° C for 18-24 hours 1}. The disadvantage of this method is the insufficient heat resistance of the sorbent (250 ° C). The purpose of the invention is to increase the sorbent capacity. The goal is achieved according to a method that includes irradiating a polymeric sorbent based on a copolymer of styrene and divinylbenzene with gamma radiation with an exposure dose of 2-10-310 P, followed by heating in an inert gas flow. With an exposure dose of irradiation not less than 21-10 X-ray, the temperature of the onset of decomposition below 2 ° C, and with an increase in the exposure dose above 3-10, a decrease in the thermal stability of the sorbent (below 270 ° C) is observed. Example 1. A fraction of 0.25-0.5 mm of the polymer sorbent Polysorb-1 (TU-B-09-3602-74) is taken and a gas chromatography column is filled with it. The sorbent in the column is irradiated with gamma radiation from the Co isotope by exposure dose 4 and then heated in a stream of inert gas L helium) for 5 hours at 200 ° C. Then, the temperature Eu of the beginning of decomposition of the sorbent is determined by thermogravimetric curves obtained on a derivatograph at a heating rate of 3 s / min in an inert atmosphere (gels). Pre-calcined alumina () is used as a reference standard. The temperature of the onset of decomposition is equal to that of C20c. Then the column is placed in a thermostat of the chromatograph (LHM-8MD 5 modifications) with a thermal conductivity detector. The analysis is carried out at 300 ± 1 C.V. as an object. For the analysis, mixtures such as: mixture of methanol are used; ethanol, propanol / butanol; pentanol and, a mixture of composition: n-pentane, n-hexane n-heptane; n-octane; M-nonan n-dean. The volume of the injected sample was 0.2 µm. The obtained chromatograms were used to calculate the column efficiency (according to GOST 17567-727 for the components of the mixture (table). Example 2. Take a fraction of 0.25-0.5 mm of the polymeric sorbent Polysorb-1 (TU- b-09-3602-74) and fill them with gas chromatographic Solon. The sorbent in the column is irradiated with gamma radiation from the Co isotope with an exposure dose of P, and then heated in a stream of inert gas (gels) for 4 hours at the start of decomposition of the sorbent 340 Ps. Then the column is placed in a chromatograph thermostat (LHM-8MD 5 modifications) with a thermal conductivity detector. The analysis is carried out at 300 ± 1 C. Mixtures of the composition: methanol (ethanol, propanol j, butanol; pentanol and the mixture: H-pentane; H-hexane) n-heptane are used as the object of analysis; n-octane, n-nonane, n-decane. The volume of the injected sample is 0.2 μm. The table shows the results of calculations on the obtained chromatograms of the column efficiency by mixture components.
Известный (t анализа 200°С) 260 500 475 500 510 600 Предлагаеккзй по примерам 370 350 440 1310 400 21445 1075 1025 1025 720 Known (t analysis 200 ° C) 260 500 475 500 510 600 Offered in examples 370 350 440 1310 400 21445 1075 1025 1025 720
9,5 15 140 190 270. 300 270 740 2,8:780 950 700 620 600 2,6 1100 1,5 92о 1080 720 780 740 1,49.5 15 140 190 270. 300 270 740 2.8: 780 950 700 620 600 2.6 1100 1.5 92o 1080 720 780 740 1.4
J1033181J1033181
Таким образом, предлагаемый ело-разделение органических веществ приThus, the proposed organic organic separation at
соб позвол ет повысить термостой-более высокой температуре заit allows you to increase the heat resistance to a higher temperature
кость сорбента -до 340®С и проводитьболее короткий промежуток вреэффвктизное газохроматографическоемени.the sorbent's bone is up to 340 ° C and conduct a shorter interval in the gas-chromatographic effect.
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SU823394244A SU1033181A1 (en) | 1982-02-02 | 1982-02-02 | Method of treating polymeric sorbent for chromatography |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SU823394244A SU1033181A1 (en) | 1982-02-02 | 1982-02-02 | Method of treating polymeric sorbent for chromatography |
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| Publication Number | Publication Date |
|---|---|
| SU1033181A1 true SU1033181A1 (en) | 1983-08-07 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| SU823394244A SU1033181A1 (en) | 1982-02-02 | 1982-02-02 | Method of treating polymeric sorbent for chromatography |
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| SU (1) | SU1033181A1 (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2001048470A1 (en) * | 1999-12-28 | 2001-07-05 | Amersham Biosciences Ab | The manufacture of improved support matrices |
| RU2809157C2 (en) * | 2018-08-31 | 2023-12-07 | Джензим Корпорейшн | Sterile chromatographic resin and its application in production methods |
| US11839861B2 (en) | 2014-01-17 | 2023-12-12 | Genzyme Corporation | Sterile chromatography resin and use thereof in manufacturing processes |
| US11912739B2 (en) | 2014-01-17 | 2024-02-27 | Genzyme Corporation | Sterile chromatography and manufacturing processes |
-
1982
- 1982-02-02 SU SU823394244A patent/SU1033181A1/en active
Non-Patent Citations (1)
| Title |
|---|
| 1. Сакодынскйй К.И., Панина Л.И. Полимерные сорбенты дл молекул рной хроматографии. М., Наука, 1977, с. 117 (прототип). * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2001048470A1 (en) * | 1999-12-28 | 2001-07-05 | Amersham Biosciences Ab | The manufacture of improved support matrices |
| US11839861B2 (en) | 2014-01-17 | 2023-12-12 | Genzyme Corporation | Sterile chromatography resin and use thereof in manufacturing processes |
| US11912739B2 (en) | 2014-01-17 | 2024-02-27 | Genzyme Corporation | Sterile chromatography and manufacturing processes |
| RU2809157C2 (en) * | 2018-08-31 | 2023-12-07 | Джензим Корпорейшн | Sterile chromatographic resin and its application in production methods |
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