A method of obtaining a polymer sorbents for chromatography

 

(57) Abstract:

Usage: the synthesis of sorbents for gas chromatography. The inventive mixing polymeric sorbent with nitric acid, followed by irradiation with gamma radiation isotope With60the exposure dose 25106- 200106the x-ray. table 1.

The present invention relates to methods of producing polymeric sorbents for molecular chromatography and can be used in various fields of national economy for the preparation of polar sorbents.

A method of obtaining a polar polymer sorbents for chromatography on the basis of a copolymer of 4-nitrostyrene, divinylbenzene and ethylvinylbenzene by the chemical interaction of these monomers (1).

The disadvantage of this method is low chromatographic polarity determined by the coefficients of Arsagera Mack Reynolds.

Closest to the proposed invention to the technical essence and the achieved result is a method for preparing polymeric sorbent by nitration of the sorbent on the basis of a copolymer of divinylbenzene - ethylvinylbenzene "fuming" (concentrated) nitric acid is sny anhydride, acetic acid and fuming" nitric acid, and therefore the necessary pre-treatment reagents, constant control over the course of the reaction, obmyvka ready sorbent residues from acid to neutral reaction. In addition, the resulting sorbent is characterized by a low value of chromatographic polarity on Arsagera Mack Reynolds.

The aim of the invention is to increase the chromatographic polarity polymeric sorbents for chromatography on the basis of a copolymer of styrene-divinylbenzene.

This goal is achieved by mixing the polymeric sorbent with concentrated nitric acid with the simultaneous irradiation of gamma radiation With60exposure doses (25-200) x 106the x-ray.

Comparative analysis of the proposed solutions with the prototype shows that the inventive method differs from the known fact that the nitration occurs during irradiation of gamma radiation With60and it is due to activation of polymer sorbent and nitric acid under the action of radiation chromatographic polarity of a copolymer of styrene-divinylbenzene increases. Therefore, the claimed method meets critera: increase chromatographic polarity 2 times, in relation to the original copolymer matrix 20 times.

The study of other known technical solutions in this field, the features distinguishing the claimed invention from the prototype, were not identified and therefore they provide the technical solution according to the criterion of "significant differences".

Example.

Take the fraction of 0.25-0.50 mm polymeric sorbent Polisorb-1 (TU-6-09-3602-74), put in a metal Cup, then pour a concentrated nitric acid in a quantity in terms of volume equal to the volume of the sorbent, and hermetically closed. The vessel is then irradiated with gamma radiation isotope With60before exposure dose of 25 x 106x-ray for 25 hours (when power used setup 106R) at a temperature of 20-60oWith, which is the temperature of the natural heat due to the reaction. After this, the vessel is opened and exposed the sorbent is washed with water until neutral, then dried. Dry sorbent prepared Packed gas chromatography column (1 m x 3 mm) and placed in a thermostat chromatograph equipped with a thermal conductivity detector. To determine the polarity of the sorbent analyze test connections Arsagera Mack Reynolds the General polarity of the I (2,3). The calculation of the coefficients of the polarity of Arsagera Mack Reynolds for irradiated sorbents, analog, prototype and Polisorb-1 spend relatively polymeric sorbent porapak-Q. Chromatographic analysis on irradiated materials is performed according to the conditions specified in the method-prototype (2), the results are shown in the table. For comparison are also factors polarity to the original sorbent matrix Polisorb-1, as well as sorbent, obtained by the action of concentrated nitric acid on Polisorb-1 for 200 hours, but without irradiation (control sample, in the table marked KP). The selected time corresponds to the maximum exposure sorbents in gamma setting, and thus the radiation dose in the table corresponds to the time of irradiation, as the power of 106R.

Similarly spend irradiation, cooking columns, analysis of test compounds and calculation of coefficients polarity for sorbents with exposure doses (40 70 100 200) x 106the x-ray. The results are shown in the table.

Thus, as can be seen from the above data, the use of the proposed method of polymeric sorbents for chromatography even at the lowest exposure dose (for sorbent, prepared according to the method prototype, which also is the base object. Irradiation to a dose of 70 x 106R allows you to bring the total polarity of I to 2-fold excess relative to the prototype and 20-fold compared to was used as the source matrix sorbent Polisorb-1 (see table).

The necessity of application of gamma radiation With60and its positive effect on the process of nitration of polymer sorbents perfectly clearly emerges from comparing the values of the total chromatographic polarity of the I samples, obtained by the proposed method with the value defined for the control sorbent KP treated with the same acid in identical conditions, but without radiation.

It should be noted that the selected interval exposure doses due to the fact that at doses less than 25 x 106R, increased polarity relative to the prototype does not occur, and increase the dose more than 200 x 106R is impractical because the polarity of the sorbent relative dose-for (70 x 106p) no longer increases, although superior values for the prototype method.

A method of obtaining a polymer sorbents for chromatography put the clinical topics what, with the aim of increasing the polarity of the sorbent, the nitration is carried out in the process - irradiation from a source of the isotope With60the exposure dose 25106200106R.

 

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