SU1370553A1 - Method of preparing silica gel for separating gas mixtures containing ozone by means of gas chromatography - Google Patents

Abstract

The invention relates to sorbents for gas analysis by gas chromatography and allows the selectivity of the separation of gas mixtures containing ozone to be increased. A column filled with mesoporous silica gel (by whom, KCC, KSK-2) is heated in a flow of carrier gas for 5–10 hours at 40–70 C. Separation of mixtures containing ozone, oxygen, carbon dioxide, and nitrous oxide , hydrocarbons. 4 il.

Description

but

WITH

C71 SP OS

13

The invention relates to sorbents for the analysis of gases and can be used for the separation and analysis of mixtures containing ozone.

The aim of the invention is to increase the selectivity of separation of gas mixtures containing ozone.

The gas chromatography analysis was carried out on an LHM-8M instrument, a katharometer detector, the carrier gas (gels) speed was 4U ml / min, the temperature of the temperature of the sample was 30 cm, the volume of the injected sample was 1 cm, the column was 1 m, and the internal diameter was 3 mm.

Example 1. A column filled with silica gel KSM (310 m / g) with dia

3 mm pore meter, 0.2-0.3 mm particle size, heated in a stream of carrier gas at 40 ° C for 5 hours. A mixture containing oxygen, ozone and carbon dioxide is analyzed.

As can be seen from Fig. 1, all components of the mixture are separated. The retention time is: 0 - 37 s; Oz - 2 min 18 s; COj - A min 55 sec.

PRI mme R 2. The column with the sorbent of example 1 is heated for 10 hours at 60 ° C. The mixture in the column of Example 1 is separated on a column. All components of the mixture are separated. The retention time is: Oi — 25 s; O - 1 min A5 s; COj - 2 min. 15 s.

Example 3: A column with a sorbent of Example 1 is heated for 8 hours at 70 ° C. Figure 2 shows a chromatogram from which it is clear that the separation of oxygen and ozone is deteriorating, but remains sufficient to determine ozone in mixtures .

SOG

Oz

and

(Da ".f

II p and mep 4. The column with the sorbent of Example 1 is heated at 30 and 80 C. In the first case, the ozone peak is sharply broadened and becomes asymmetric, which does not allow quantitative analysis of the ozone content. When heated to 80 seconds, the ozone and oxygen peaks are practically not separated.

Example5. The column with the sorbent prepared according to Example 1 is used to separate the mixtures, containing 1 C1x nitrous oxide (Fig. 3) and ethane (Fig. 4). As can be seen from the chromatograms, complete separation of the components of the mixture is achieved.

On silica gel prepared by the prototype method, the selectivity of separation in an oxygen-ozone pair is low, which does not provide complete separation of components and the possibility of quantitative analysis.

The proposed method can be used to prepare silica gel for determination in ozone gas mixtures at a level of 0.1% and higher. You can use mesoporous silica gel KSM; KSS, KSK-2.

Claims (1)

Invention Formula The method of preparing silica gel for the separation of gas mixtures containing ozone by gas chromatography, including the heat treatment of mesoporous silica gel for 5-10 hours, characterized in that, with increasing separation selectivity, heat treatment is carried out at 40-70 C. FIG. 2 fig.Z Phie.