SU826225A1 - Method of gasochromatic separation of organic and organo-silicon compounds - Google Patents

Description

polynkalic radykalys containing dinin

The purpose of the invention is to improve the separation of a mixture of organic and organosilicon substances.

This circuit is achieved by gas chromatography of the organic separation of orgHif4ecKHX and organosilicon compounds by dropping the mixture to be separated through a chromatographic column with a stationary phase — opi-methyl-f5-ethyl-adamantylsiloxane of the general formula

Ad

(

VL

where t "1O-75,

(CHfyj A - is ethlada-mantyl radical. The presence of bulk ethylamine

radicals in the oligoorganosiloxane chain provides better solubility in them of compounds containing polycyclic radicals, which contributes to increased separation. The best separation of isomers is due to the structure and rheological properties of oligoorganoethyl-man-methyls-oceans.

The table shows the properties used as a stationary phase oligomethyl-P-etaladantilsiloksanov general formula

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I

(sn)

-9.-0 - BlSnL, (I)

SiO I

O-si j

CHoJ

m (CHj)

where ro 10-75, n-1-10, (CH2.) 2Adl25P is etladating the radical

567

1052

nineteen

MDRT - the maximum allowable working temperature. The stationary phases are tested for gas-liquid chromatography. They can be used under isothermal conditions and in temperature programming mode with a katharometer and a flame ionization detector. Example. A sorbent for gas liquid chromatography using olomethyl-0-ethyl damantilsiloxane is prepared as follows. The compound of formula (1), where tn (, p 5, P 67 is applied to a solid carrier chromatone H-AW-HMDS with a grain size of 0.2 0, 315 mm, in the amount of 30% from solution in diethyl ether. Excess solvent was removed with constant stirring without heating, the conditioning of the sorbent is carried out in a stream of pure and dry inert gas in the following mode: at - 1 h, 2bo ° C - 1 h, 300 ° C2 h, 350 ° C - 2 h, - 2 After conditioning, the remaining amount of the stationary phase is 11%. i The prepared sorbent is loaded into a chromatographic column with a diameter of 4 mm and a length of 0.5 m. Sorbent they are poured into the column in small portions and compacted by tapping until they are completely filled. Both ends of the column are closed with glass fiber tempos and connected to an LCM-72 chromatograph. detector, columns (initial) and 350 ° C (final). Program speed in C / min 562 A mixture of oligometry, (ethyl) adamantylsiloxanes formed by the hydrolytic condensation reaction of dimethyldichlorosilane followed by rearrangement of the hydrol product is subjected to analysis. behind. The resulting chromatogram is shown in FIG. 1. j Peaks 1-16 are dimetypcyclosiloxanes of the general formula t () SiOj p where n: 3-14. The peaks of 1726 are oligomethyl-li-ethyladamantylsiloxanes. The identification is carried out by the dependence of the retention time on the number of silicon atoms. The separation of these components in a known stationary phase does not occur in a cavity and the total number of peaks is 11 instead of 26. Example 2. In analogy to example 1, a sorbent is obtained when a compound of formula (1) in which X 52, rt, p; c5 is applied to a solid carrier . The mixture formed during the pyrolytic interaction of orthooxide (zenine with trichlorosilane and representing siloxanofenanthrene derivatives) is separated on a chromatographic column 0.5 m long and 4 mm in diameter. The temperature in the evaporator, in the thermostat of the detector is 300 C. The heating rate is U C / min. The resulting chromatogram is shown in Fig. 2. Compounds (Identified by mass spectrometry, average: Peak 1 - solvent Peak 2 - C Peak 3 - X Peak 4- X ,, Peak 5 Peak 6,

Peak 7 Peak 8 Peak 9 SiCl

At the known stationary phase, the separation of this complex mixture was not obtained.

Example 3. Analogously to example 1, a sorbent is obtained when a compound of formula (1) is applied, in which PS, 9, on a solid support chromate NAW-HMDS, separates the mixture of isomers - pentafenne ether.

Claims (2)

Column length 1 m, diameter 4 mm. The temperature in the column thermostat 325 ° C detector evaporator. The velocity of the carrier gas gels is 60 ppm / min, the sample size is 0.4 µl of the ether solution of pentafet llovy ether. The 1 chromatograph is shown in FIG. 3. Peak 1 — meta-isomer, peak 2 — orthoisomer, peak 3 para-isomer. At the known stationary phase, only partial separation takes place between the meta-isomer and the unseparated mixture of ortho and para isomers. . The examples given show a high selectivity in the separation of organic and organosilicon compounds containing lol-diclic radicals in the danry stationary phase. CLAIMS A method for gas chromatographic Section laziness organic and organosilicon soedascheny separable by passing the mixture through a chromatography column with a stationary phase - oligoorganosiloksanom, yuschiys differs in that in order to improve the separation of the mixture, as used oligorrganosiloksana oligometil- -etiladamaitilsiloksan ob- boiling formula wherein m 10-75,, - (СН,),, - is ethadantamyl radical. Sources of information taken into account in the examination 1. Organic silicone stationary phases for gas-liquid chromatography, Central Scientific Research Laboratory, Moscow, 1969. 2. USSR author's certificate number 538293, cl. Q O1 N 31 / O8, 1975 (prototype).