SU285328A1 - PREPARATION GAS LIQUID CHROMATOGRAPH - Google Patents

Description

Preparative gas-liquid chromatographs are known that contain a hot thermostat zone, a carrier gas supply, a heating column, a sample introduction unit, separation chromatographic columns, a detector, a heated output, a sampling device. The separable mixture is introduced through the sample introduction unit into the chromatographic columns in which the gas mixture is divided into separate concentration zones. Separation may be complete or incomplete. Concentration zones in the form of chromatographic peaks are recorded by a detector mounted at the outlet of the columns. In accordance with the shape of the peaks, the operator or machine connects to the heated output a sampling device, in which the individual components of the mixture to be separated are collected.

The purpose of the invention is to improve the separation capacity of the device and increase the purity of the fractions. It is achieved by the fact that the chromatograph is equipped with a parallel main line of separation columns with an additional gas-carrier line, which is connected between the column sections by means of shut-off valves, and an additional solvent inlet is installed at the inlet to the sampling device.

littelny columns; in fig. 3 and 4 are chromatograms of the fraction obtained respectively without washing and with washing of communications. The chromatograph contains a hot zone of thermostat 1, an inlet 2 of carrier gas, a heating column 3, a sample inlet 4, which communicates with several series-connected sections of chromatographic columns A, B, B ....

After each section of the chromatographic columns, detectors a, b, c ... and inputs 5, 6, 7 ... of carrier gas are included in the gas line. The locking devices I, II, III ... on the gas line of the chromatograph allow the carrier gas to be supplied either to the first and all subsequent sections, or only to the second and all subsequent sections, or to the fifth and all subsequent sections, mine all previous but with

the prerequisite for alternate transmission in the form of individual portions of all concentration zones through all sections of separation columns up to the sampling device.

Particularly high purity of the selected substances is achieved by the fact that, in the proposed chromatograph, there is an inlet 8 of carrier gas with a backing device, connected through an additional evaporator 9 with the output of the latter

After each concentration zone is taken, in order to obtain the next component in a pure form, a portion of the solvent is introduced into the additional evaporator and, opening the valve 8, the solvent pairs are driven into the separate trap of the sampling device 10 by flowing a carrier gas current, thus flushing the entire output communication 11. Thereafter the specks 8 are closed again.

A mixture of tridecane 12, an unknown, difficult to separate impurity 13 and tetradecane 14, when divided on a conventional chromatograph preparative chromatograph, gave the chromatogram shown in FIG. 3. Separation conditions: thermostat temperature 150 ° C, gel consumption 100 ml / min, columns 8 mm in diameter, 3 m long, nozzle 7% polyethylene glycol adipate at a spherochrome, mix weight 80-100 µl. The same mixture, when divided into columns of the same length and diameter, with the same packing, under the same conditions, separated by a preparative chromatograph of the proposed design, gave the chromatogram shown in FIG. four.

Subject invention

A preparative gas-liquid chromatograph containing a device for injecting several series-connected

separator column sections with different sorbents and detectors at the exit of each section, sampling device, characterized in that, in order to increase the separating ability and increase the purity

fractions, the chromatograph is provided with a parallel main line of separation columns with an additional line of carrier gas, connected by means of shut-off valves between the sections of the separation columns, and at the inlet

an additional solvent input unit is installed in the sampling unit.

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