Chromatographic device for determining the projected values of the retention

 

(57) Abstract:

Usage: in chromatography for identification of individual compounds or individual components of chemical mixtures. The inventive chromatographic device for determining the projected values hold contains two separation column, the preparation unit gas regulators costs and pressure of carrier gas in each column, automatic dispenser, there are a number of doses of a fixed volume, and the input of each of the columns simultaneously connected to two respective fixed dose and lines of carrier gas through the locking elements of the dispenser, and outputs the speakers connected to the detector via adjustable pnevmoobrushenija and automation of the analysis with the additional computing device to calculate the extrapolated value of the deduction. The invention provides improved accuracy and reduced labor costs and time when determining the projected values hold for infinitely large percentage of impregnating a solid carrier stationary liquid phase, the zero value samples, zero in column etc. 1 C.p. f-crystals, 1 Il.

The invention relates to chromeline mixtures in various industries: chemical, oil, gas, petrochemical, metallurgy, medicine, biology, ecology, etc.

Known chromatograph to determine the extrapolated value of the holding on which spend several consecutive analyses of individual compounds or individual components of complex mixtures with standard substances comparison and rezorbiruetsa component alternately on two columns with different content of the stationary liquid phase (page) on solid media [1] based On the test results determine the retention time rezorbiruetsa and analyzed components, standards (substances comparison), and calculates a relative or interpolation value retention, the values of which extrapolate to the infinitely large to the percentage of impregnation of the solid carrier stationary liquid phase, the zero value samples or zero pressure in the column formula

Ie=100+Z

or

re= , (1) where reand Ieextrapolated values of the relative retention index and Kovacs;

to, t, t,t,t the retention time rezorbiruetsa and analyzed components, standard (substances comparison) and normal paraffin hydrocarbons with the number of carbon atoms in the values of the specified parameters for extrapolation value retention at 1-St and 2-nd separation columns (content page, the volume of the sample, pressure, and others).

A disadvantage of the known device is that to determine the extrapolated values of the relative retention or index Kovacs use the results rezorbiruetsa component identified substances and standards of several cycles of chromatography was carried out, which reduces the accuracy and reliability of the information received and greatly increases the complexity of the measurement process [2]

The closest to the essential features of the claimed device is selected as a prototype chromatographic device for determining the projected values holding, containing connected in series to the source of carrier gas, the preparation unit gas flow regulators and pressure gauges on two parallel independent streams of carrier gas, automatic dosing of gases and liquids, detector, differential amplifier, automation system analysis and Registrar [3] Extrapolated values of the relative retention reand index Kovacs Iedetermined by the formula.

The disadvantages of the known device are as follows.

The low accuracy of the measurement because of the kih cycles chromatography was carried out. Thereby are not fully specific features chromatography, associated with the mutual correlation of the errors of the measured values of the retention component.

The impossibility of simultaneous input of two samples (gas and liquid) of different sizes in each column; the inability to work two identical columns in the same mode of flow of carrier gas, but at different pressure values in each column.

The automation system of analysis does not allow the calculation of relative and interpolation values, retention, and extrapolate their values to the infinitely large to the percentage of impregnation page, the zero value samples or zero pressure in the column.

The aim of the invention is to improve the accuracy of determining the projected values of retention.

The purpose is due to the fact that the chromatographic device for determining the projected values holding, containing connected in series to the source of carrier gas, the preparation unit gas flow regulators and pressure measurements on two parallel between the lines a carrier gas, automatic dispenser, two parallel connected of razdelitel amplifier and recorder, added two adjustable pnevmoobrushenija located between the output of each of the separation column and the detector, and automatic dispenser is equipped with a number of different doses of a fixed volume, and the input of each of the columns is connected simultaneously with two fixed doses and line the carrier gas through the locking elements of the dispenser. In addition, automation of the analysis is further provided with a computing device to calculate the extrapolated values hold by the formula (1).

When the task is created technical result, which is the simultaneous chromatographicaliy in the period of one cycle analysis of fixed sample volumes rezorbiruetsa component, such as methane, in the case of using a flame ionization detector identified compounds and standards on two separation columns. While the modes of columns set in accordance with one of the parameters extrapolation, for example, different content page, different sample volumes and pressure for each column in the constancy of the two other parameters, including the flow of carrier gas.

Comparative analysis of the prototype pok the b input of two identical or different samples of a fixed amount in each of the separation column, adjustable pnevmoapparatury output columns to change the pressure in the columns while maintaining the constancy of the flow rate of the carrier gas and the additional computing device to calculate the extrapolated values of the relative retention or index Kovacs.

The proposed device is characterized by a new set of essential features that enhance the accuracy and reduce labor costs and time when determining the projected values of retention.

The drawing shows the proposed device.

The device comprises a source 1 of carrier gas, unit 2 gas with two controllers 3 flow and two 4 pressure gauges, one on the appropriate line of carrier gas, automatic dispenser 5 with a range of doses 6-13, various fixed volume, four channels 14 for supplying a carrier gas in the column when the set of samples at doses of 6, 8, 10 and 12, three locking elements 15 and the actuator 16 at three points, two separation columns 17 and 18, two adjustable pnevmoobrushenija 19, the detector 20, the differential amplifier 21, system 22 automation of the analysis, additional computing device 23 and the Registrar 24, line 25 set Pro is ogenyi I drive 16 connection channels of the dispenser 5 correspond to the drawing and nenormiruemym component lines 25 fills doses of 6 and 8, and the analyzed component and standards on the lines 26 fill in the doses of 10 and 12. Columns 17 and 18 are blown through the carrier gas through the channels 14 from source 1 carrier gas through the unit 2 gas and line the carrier gas.

When the position of the second actuator 16 moving parts of the dispenser with 5 doses are moved to the left in the drawing and in column 17 are dosed simultaneously to analyze the gas sample (dose 6) and the liquid sample (dose of 10), and in column 18, respectively, the dose of 8 gas and dose 12 of the liquid. The volume of the dose of 6 is equal to the dose volume 8 and volume dose of 10 is equal to the dose volume 12. At the same time a set of samples through lines 25 and 26 of the gas and the liquid in doses of 7, 9, 11 and 13.

When the position of the third actuator is movable elements are moved still further to the left on the drawing and in columns 17 and 18 simultaneously dosed, respectively, of the sample gas (dose 7 and 9) and liquid (dose 11 and 13), and the amount of dose 7 is not equal to the dose volume 9 and volume dose 11 is not equal to the dose volume 13.

Modes of analysis to determine the extrapolated values of retention following.

Extrapolation to infinitely large percentage of impregnating a solid carrier stationary liquid phase.

Columns 17 and 18 are made of stainless steel tubes (length 1 m, inner diameter 3 opinions. Regulators 3 consumption and adjustment pnevmoapparatury 19 install the same flow rate and pressure of carrier gas in both columns. The analysis is carried out in the position II of the actuator of the dispenser. In this column enter the same sample gas (doses of 6 and 8) and liquid (doses of 10 and 12). Thus there is only one variable parameter extrapolation of the content of the page in columns.

Extrapolation to zero pressure.

Columns 17 and 18 are identical and filled with sorbent with the same content page. The flow of carrier gas in the columns is set equal, and the pressure is different due to changes in the magnitude of pnevmoobrushenija 19 in one of the columns. The analysis is performed in the position II of the actuator of the dispenser.

Extrapolation to the zero value samples.

Columns 17 and 18 are identical and filled with sorbent with the same content page. The flow rate and pressure of carrier gas in the columns set by regulators 3 and pnevmoobrushenija 19 is also the same. The analysis is performed in the position III of the actuator of the dispenser. In columns 17 and 18 impose different amounts of gas (dose 7 and 9) and liquid (dose 11 and 13).

Eluruume of the columns 17 and 18 components enter into the chamber of the detector 20 which signals through the diff is s and simultaneously fed to the system 22 automation of the analysis with the additional processing unit 23 to calculate the extrapolated values of the relative retention or index Kovacs analyzed components.

The output time of the chromatographic peak rezorbiruetsa component at equal cost carrier gas in identical columns 17 and 18 should be the same, and the detector generates one total peak component at the same time with two columns. Criterion validation of the peak shape (no its razdaivaniya) is the signal of the differentiating amplifier 21 with bipolar characteristic. In the case of obtaining a double peak, you need to slightly change the flow of carrier gas in one of the columns using knob 3 flow.

The values of the retention time rezorbiruetsa component identified compounds and standards obtained while chromatographicaliy samples on two columns, are measured and stored in the storage device system 22 automation of analysis, where do the additional computing device 23, is made with the use of microprocessor-based equipment. Computing device 23 calculates the extrapolated values hold by the formulas (1). Parameter values extrapolation and1and a2specified by the operator. The results of the calculation of reor Iedepending on the statement registriruyetsia TO determine the EXTRAPOLATED VALUES of RETENTION, contains one United source of carrier gas, the preparation unit gas flow regulators and pressure gauges on two parallel lines carrier gas, automatic dispenser, two parallel connected separation column, a detector, the output of which is connected to the automation system analysis, as well as from the differentiating amplifier and recorder, characterized in that it additionally introduced two adjustable pnevmoobrushenija located between the output of each of the separation column and the detector, and automatic dispenser consists of two movable parallel spaced elements connected to the actuator, in each above each of the columns is made of doses of different sizes, and one of the items announced two lines nesorbiruyushchegosya gas, and the other two lines of the analyzed liquid substances-standards, and the entrance of each of the columns is connected simultaneously with two doses and a line of carrier gas through the locking elements of the dispenser.

2. The device under item 1, characterized in that the automation system analysis is further provided with a computing device to calculate the extrapolated value retention.

 

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