Modification of adsorbent for chromatography and device for its implementation

 

(57) Abstract:

Use: in the production of modified polymeric sorbents. The inventive method includes the handling of sorbent in the plasma electric discharge in the presence of a plasma-forming gas. Processing of polymer sorbent is subjected to chromatography on the basis of styrene and divinylbenzene at a pressure of plasma gas 1 - 130 PA. As a plasma-forming gas using oxygen. The device has a reservoir partially filled with sorbent and fitted with electrodes and socket for connection to a vacuum pump, a generator of electrical voltage connected to the electrodes, and the ultrasonic vibrator of the type connected with capacity for sorbent. 2 S. and 2 C.p. f-crystals, 1 Il.

The invention relates to the field of gas chromatography and, in particular, to methods for producing modified polymer sorbents that can be used to analyze complex mixtures of polar and nonpolar compounds.

There is a method of modifying an inert carrier for gas chromatography, in which a layer of particles of the sorbent is heated at a temperature of 200 - 300oTo insure flow of inert gas, nasiminskoy media pure inert gas at a temperature of 20 30oWith higher than by passing the gas mixture.

A device for implementing this method is a reactor with electrodes that are connected to the voltage source for plasma processing chromatograph solid media (soot) deposition on him modifier which is used as polyacrylnitril, and its polymerization on the surface of the carrier. The reactor is equipped with means for mixing the media. The modification is carried out in argon [1]

The known method of thermochemical modification applies for modification of inert carriers, but is not applicable for the modification of polymeric sorbents for gas chromatography.

The closest in technical essence and the achieved result for the proposed method is a method of plasma processing of materials in a plasma reactor with electrodes placed on the outer part of the reactor, with the possibility of rotation and the nozzle for supplying a gas environment [2]

A device for implementing this method adopted for the prototype contains a sealed container partially filled modified sorbent and provided with a socket for connection to a vacuum, the electrodes established by vitalcom known method and device for its implementation, what it does not provide uniformity modification of the sorbent particles in the particle bed of the sorbent. Processed mainly in the surface layer of the sorbent, facing the electrodes. The inner layers of the sorbent almost not processed, because they are closed from the effects of plasma external (outer) layers of the particles of the sorbent. For this reason, the known method is applicable only for the processing of thin layers of sorbent, the share of thin-layer chromatography. The objective of the invention was to develop such a method and device for its implementation, which provide a uniform (homogeneous) processing of sorbent particles in the layer of sorbent.

This task is solved in that a method of modification of the adsorbent for chromatography by processing in the plasma electric discharge in a sealed vessel in the presence of a plasma-forming gas, which according to the invention the treatment machine polymeric sorbent for gas chromatography based on the vinyl derivatives of divinylbenzene with continuous stirring of the particles of sorbent in a confined space air-tight container and the pressure of the plasma gas 1 130 PA, and as a plasma-forming gas used color is collected by rotating the housing air-tight container.

In a preferred embodiment of the method, the mixing of the particles of the sorbent is carried out by vibration layer of the sorbent with the creation of a fluidized bed of sorbent particles.

Another distinctive feature of the proposed method is that during the processing of the sorbent adds vapors of organic substances containing functional groups selected from the series: HE; -NH2; -SLEEP; -COOH; -C=O.

This task is solved in that the device for modification of the adsorbent for chromatography, containing tank partially filled with modified sorbent and fitted with electrodes and socket for connection to a vacuum pump, and the generator voltage connected to the electrodes, which according to the invention is equipped with a device for mixing particles of a sorbent layer during processing in a plasma electric discharge. 2 In one possible embodiment of the device of the device for modification of the particles of sorbent made in the form of a sealed container made of elektroprovodyashchego material (glass), which is connected with the motor shaft, and the electrodes, for simplicity of construction are external and motionless.

In shemy polymeric sorbent Polisorb-1" is placed in the middle part of the housing 1 (see the drawing) through the loading hole, which is then hermetically closed by a plug 8. The internal volume of the housing 1 is connected through pipe 7 to a vacuum pump (Fig. not shown) and are pumping out of the internal volume to a pressure of 1 130 PA.

Then use the generator 4 to the electrodes 3 is energized, sufficient for ignition between the electrodes 3 in the internal volume of the housing 1 glow electric discharge. Developing this generator 4, the power density is 0.001 to 0.1 W/see through drive, for example, an electric motor (Fig. not shown), the shaft 2 and the housing 1 are rotated 1 120 revolutions per minute.

In the presence of low-temperature plasma glow discharge plasma-forming gas (oxygen) affects the surface of the polymer particles of the sorbent, forming its covalently grafted functional groups. In this case, the change in chemical surface properties of the sorbent particles is carried out by plasma-forming gas without the use of vapors of organic compounds containing grafted functional groups. To ensure the modification of the sorbent by imparting to the surface defined functional groups in the internal volume of the housing 1 of the device is the modification of the adsorbent for chromatography by processing in the plasma electric discharge in a sealed container in the presence of plasma gas, characterized in that the processing of the polymer sorbent is subjected to chromatography on the basis of styrene and divinylbenzene at a pressure of plasma gas 1-130 PA, and as a plasma-forming gas using oxygen.

2. Sposo under item 1, characterized in that the mixing of the particles of the sorbent is carried out by vibration layer of sorbent with frequency 10 105Hz with creating a fluidized bed of sorbent.

3. The method according to PP. 1 and 2, wherein the plasma-forming gas add of vapors of organic substances containing functional groups selected from the series-HE; -NH2; -SLEEP; -COOH; -C=0.

4. The device for modification of the adsorbent for chromatography, containing tank, partially filled with modified sorbent and fitted with electrodes and socket for connection to a vacuum pump, and the generator voltage connected to the electrodes, characterized in that it is provided with an ultrasonic vibrator type connected with capacity for sorbent with the aim of mixing particles of a sorbent layer during processing in a plasma electric discharge.

 

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FIELD: analytical instrumentation engineering; chromatographic analysis of composition of substances.

SUBSTANCE: proposed method includes delivery of carrier gas to evaporation chamber through gas supply line, introduction of sample into evaporation chamber, delivery of part of gas flow from evaporation chamber to chromatographic column and discharge of remaining of gas flow to atmosphere. Delivery of carrier gas to evaporation chamber is effected in direction opposite to motion of evaporated sample to chromatographic column. Device proposed for introducing the sample into chromatograph has sample introducing line, evaporation chamber, chromatographic column, carrier gas supply and carrier gas discharge line which are connected with evaporation chamber. Carrier gas discharge line is connected with evaporation chamber in area of introduction of sample and carrier gas supply line is connected with opposite end of evaporation chamber.

EFFECT: enhanced accuracy of dosing the sample; improved quality of separation of components; enhanced reliability; simplified construction.

11 cl, 3 dwg

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