Sorbent for gas chromatography

 

(57) Abstract:

The sorbent can be used to determine the moisture in hydrocarbon gases C1-C4with the goal of certification as standard samples. Proposed sorbent composition, wt. %: copolymer of styrene 74-77; divinylbenzene, polyethylene glycol-400 23-26. 1 Il., table 1.

The invention relates to sorbents for gas chromatography that can be used in the determination of moisture in hydrocarbon gases WITH1-C4with the goal of certification as standard samples.

Known sorbent Polisorb 1 (a copolymer of styrene and divinylbenzene), used to determine the humidity of liquefied hydrocarbon gases.

However, due to insufficient selectivity of the sorbent cannot be used for analysis of propane and propylene on the moisture content.

Known sorbent on the basis of a copolymer of styrene and divinylbenzene containing the active charcoal in the following ratio, wt. the copolymer of styrene and divinylbenzene 75-90; active carbon 10-25. The sorbent allows you to define the water in propane.

However, this sorbent has the following disadvantages: due to the heterogeneity of the surface of the coal chromatogram poluchaya hydrocarbon gases; the inability to use sorbent for determination of water in all hydrocarbon gases WITH1-C4on one hand column.

The aim of the invention is the reduction of the detection limit, time of analysis and enabling determination of water in hydrocarbon gases WITH1-C4on one hand column.

This objective is achieved in that the sorbent on the basis of a copolymer of styrene and divinylbenzene as the stationary phase contains a polyethylene glycol-400 (PEG-400) in the following ratio, wt.

The copolymer of styrene and divinylbenzene 74-77

Polyethylene - glycol-400 23-26

When the content of polyethylene glycol-400 more than 26 wt. it turns out blurred rush of the water and increases the time of analysis. When the content is less than 23 wt. deteriorating the separation of water from Bhutan and as a consequence decreases the detection limit.

It is known that water is very strongly held and gives blurred peaks in the polar liquid phases, the molecules which form hydrogen bonds with water molecules. These phases is polyethylene glycol with a molecular weight of 400 (PEG-400) is widely used in gas chromatography.

The separation of the modified polymeric sorbents of Otley, the s 2-7% of the stationary phase. When applying the number of phases more than 100% efficiency of the column begins to fall due to the increase of the film thickness and deterioration of the process of mass transfer.

The effect of PEG-400 in number 23-26 wt. the Polisorb-1 is to maintain high efficiency speakers on the water and the simultaneous increase of selectivity with her determination in hydrocarbon gases. This leads to the surprising effect that enables the determination of water in hydrocarbon WITH1-C4with a relatively low detection limit. Thus, the proposed solution meets the criterion of "significant differences".

The sorbent is prepared as follows.

Polisorb-1 (TU-6-09-3602-74) FR. 0,2-0,315 mm placed in a round bottom flask and sequentially treated with a series of solvents (benzene, ethanol, acetone) and their subsequent removal. PEG-400 was dissolved in acetone, the resulting solution was poured to Polisorb-1. The acetone is removed by heating in an air bath at 50-60aboutWith subsequent vacuum treatment (5 h).

P R I m e R 1. On prepared as described above 7 g Polisorb-1 fraction of 0.2-0,315 mm put 3 g of polyethylene glycol-400, dissolved in acetone.

The composition Noi 1 m, diameter 3 mm

For analysis using GC Color-102".

The proposed method is illustrated by a drawing.

When the temperature of the column 90aboutAnd the speed of the carrier gas helium 60 ml/min analyze n-butane in water content. (1.2 air + butane; 3 water).

The table shows the values of limit of detectionminsimulation time t, KSthe asymmetry factor, criterion characterizing the completeness of the separation at different contents of Polisorb-1 and peg-400 in the analysis of propane (C3) and butane (S4) on the water content.

The table shows that, using the sorbent, 23-26% PEG-400 on Polisorb-1 achieved a complete separation of ( 1) water and hydrocarbon gases, so you can determine the admixture of water in all hydrocarbon gases WITH1-C4without changing columns. The limit of detection in comparison with the prototype reduced almost 4-5 times. The proposed sorbent almost complete symmetry of the peak water (see drawing) in contrast to the prototype. If you take the amount of PEG-400 is less than 23% of the degree of separation of the pair butane-water sharply decreases and consequently increases the detection limit. The increase in the number of glycols more than 26% leads to an increase in film thickness igasom, the proposed sorbent reduces the detection limit, reduce analysis time and allows you to define one column, the water content of hydrocarbon gases WITH1-C4.

SORBENT FOR GAS CHROMATOGRAPHY, containing a copolymer of styrene and divinylbenzene and the stationary liquid phase, characterized in that, to reduce the detection limit, time of analysis and determination of water on one column in hydrocarbon gases C1C4as stationary phase contains a polyethylene glycol-400 in the following ratio, wt.

The copolymer of styrene and divinylbenzene 74 77

The polyethylene glycol-400 23 26

 

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