Chromatograph

 

(57) Abstract:

Use: in analytical techniques, in particular in the chromatograph for quantitative analysis of individual components of different mixtures in different industries - chemical, gas, petrochemical, metallurgical, medical, biological and other inventive chromatograph includes a source of carrier gas, three dosing with dosing volumes, the first column, the flow divider, the detector, the second column with a concentration detector output and the third dosing with dosing volume at the entrance. There are also cumulative column for the designated components of the device maintain the desired temperature desorption, United switch gas flows from the outlet of the first column and dosing volumes respectively of the second and third or the third and fourth dispensers through additional gas valve. Chromatograph provides a separate source components of the analyzed mixture and putting two of them in mixture with carrier gas in the separation column simultaneously with the starting mixture for the joint analysis. In this case, provided the reduction of labor costs and time when the appreciation is giving relates to gas chromatography and can be used for quantitative determination (certification) of the individual components of multicomponent mixtures of arbitrary composition.

Known chromatograph containing connected in series to the source of carrier gas, the first and second dispensers, the separation column, a detector, a third dispenser connected to a source of carrier gas, switch gas streams and several on the number of defined components of the cumulative columns, provided with a device for maintaining the temperature of desorption, are parallel to each other and connected by inputs and outputs through the switch of gas flows from the metering volume of the second dispenser. Chromatograph provides the selection of the individual components of the analyzed mixture and putting one of them in mixture with the gas propellant is used in the separation column together with the analyzed source mix for re-analysis. The concentration of the component is determined using the additive according to the results of three chromatographic analyses.

However, the known chromatograph, working only with the concentration detector has limited analytical capabilities and requires considerable time and increased labor costs to determine the concentrations of the individual components of the analyzed mixture (three analysis to determine the content of each component, not counting the pre-anal is ograph has a relatively low accuracy of determination of the concentrations of the components of the mixture by increasing the random components of error when changing the parameters of the chromatographic process in time in a period of three cycles of analysis.

Closest to the invention by the technical nature of a chromatograph, containing connected in series to the source of carrier gas, the first and second dispensers are connected to the line of the original mixture, the third dispenser, the first separation column with a flow divider, a differential detector, which can be applied not only concentration, but also streaming destructive detectors. The output of the separation column via switch gas flows simultaneously connected with the corresponding defined component of the cumulative column and the second and third dispensers. Cumulative speakers have a device for maintaining a predetermined temperature desorption and filled with sorbent. The entrance to the third dispenser is connected to the source line of the analyzed mixture, and exit through the second separation column and the flow divider with a concentration detector. The concentration of the analyzed component in the original mixture is determined using the additive according to the results of three chromatographic analyses: analysis of the initial mixture, the analysis of the initial mixture with the additive binary mixtures-defined component carrier gas, the analysis of the initial mixture with the additive binary mixtures opredelyayutsya increase in time and labor required for the determination of concentrations of components of the analyzed mixture, the decrease in accuracy by increasing the random component of the error when changing the parameters of the chromatographic process in a period of three cycles of analyses, and that the chromatograph is not possible to fully realize the information potential of the chromatographic analysis, such as those associated with the use of interpolation methods for quantitative analysis when determining components suiryudan respectively before and after the two components known content.

The objective of the invention is to improve the accuracy of determining the concentration of components in the application of interpolation methods for quantitative analysis, as well as reducing labor costs and time to quantify the individual components of multicomponent mixtures of arbitrary composition.

This is solved due to the fact that in the chromatograph containing a source of carrier gas, the first and second dispensers are connected to the line of the original mixture, the third dispenser, the first separation column with a flow divider mounted on its output, which is connected simultaneously with the first detector with the comparative and the measuring chamber, and through switch gas flow temperature desorption and connected via switch gas flows from the metering volumes of the second and third dispensers, the second separation column with a concentration detector having comparative and measuring chamber at its outlet, and the second dispenser at its input, according to the invention introduced a fourth dispenser installed in series with the first and third dispensers and dosing volumes of the second and fourth dispensers are connected in series, and the output switch gas flows connected with dosing volumes respectively of the third and second or the fourth and second dispensers are introduced through the gas valve, and the line original mix connected via a flow divider with comparative camera concentration detector.

This allows you to determine concentrations of components with greater accuracy interpolation using the dual additive (similar to the dual internal standard). When this occurs, the cross-correlation between the errors of the measured chromatographic values of the analyzed components that are shared during one cycle analysis. It is known that errors are not correlated, if measurements are performed as a result of several cycles of analysis, for example, as known in the chromatograph, the method of single supplements consistently for two separate compo the house.

The invention is illustrated in the drawing.

Chromatograph contains source 1 carrier gas, the first dispenser with 2 dosing volume V1the second dispenser with 3 dosing volume V2the third dispenser with 4 dosing volume V3, the separation column 5, an adjustable throttle 6, the divider 7 flow, differential detector 8, which can be used destructively or selective detectors, fourth dispenser 9 dosing volume V4the switch 10 gas flows, the cumulative column 11, the device 12 to maintain a predetermined temperature desorption, separation column 13, the divider 14 flow, concentration differential detector 15, an adjustable throttle 16 and the additional gas valve 17.

The divider 7 flow divider 14 flow consist of two permanent chokes different resistance. Chokes a large resistance connected respectively through adjustable throttles 6 and 16 with source 1 carrier gas and the source line of the analyzed mixture for alignment of gas consumption in both cells of the detectors 8 and 15.

Chromatograph operates as follows.

The initial mixture with a sample volume of V1the dosing device 2 enters p is between the corresponding cumulative column 11 through the switch 10, the gas flows through the divider 7 flow in both cell differential detector 8. Measured by the detector difference signal S proportional to the difference of the concentrations of the component to be determined in the cells of the detector and its quantity in the original mixture, which excludes the impact of systematic error due to the presence of the initial factor in the equation of the calibration characteristics of the chromatograph.

After several tests the initial mixture adsorbed in the cumulative columns 11 components alternately desorbers for the joint analysis with the original mixture. This enables the device 12 to maintain the temperature of desorption. One of the defined components desorbed from the corresponding cumulative column in a mixture with a carrier gas, is fed through an optional gas valve 17 in the dosing volume V2and V4the second and fourth dispensers. The binary mixture of the first component to be determined (volume dose V4) dosed in second separation column 13, purged of the original mixture. The detector 15 registers the change in the concentration of the carrier gas method acanthamoebae. After this additional gas valve 17 switches and the second detectable component desorbed from the appropriate macheteros dispensers. Then at the entrance of the separating column 5 are dosed simultaneously the initial mixture volume V1and a binary mixture of two defined components with the carrier gas V2and V3. In addition, the binary mixture of the second component to be determined by the volume V4dosed in second column 13.

The concentration of the two components in the original mixture is determined by the results of three chromatographic analyses using the dual additive.

The analysis of the original mixture. Dose V1the initial mixture. Dose V2V3and V4pure carrier gas.

Analysis of binary mixture of the first component to be determined with the carrier gas. Dose V4.

Analysis of the initial mixture with the additive binary mixtures of the first and second defined components. Dose V1the initial mixture. Dose V2the binary mixture of the first component to be determined. Dose V3and V4the binary mixture of the second component to be determined.

The normalized system of equations for calculation of the concentrations of the designated components in the original mixture is

C -1 + 1, where C1=

C -1 + 1, where C12=

C1i= S1iV1< / BR>
or

S12/nS22/nand S32/nchromatographic signals (vacancy) carrier gas in the first, second and third tests (dose V4detector 15); Si1, S11, S21,S13S23chromatographic signals of the i-th component and two components in the first and third tests (dose V1V2and V3detector 8).

The use of the invention can significantly reduce the time and effort required to conduct quantitative determination (certification) of the individual components of multicomponent mixtures of arbitrary composition, as through the application of the fourth dosing with dosing volume V4and more of the gas valve at the output of the switch gas flows is provided by the determination of the concentrations of the analyzed components of the original mixture interpolation using the dual additive, it reduces the total number of tests for the quantitative determination of three components enough to hold all three analysis; to improve the accuracy of quantitative determination is elizerbeth components, shared during one cycle analysis when the interpolation method dual additive; to determine the retention time of rezorbiruetsa component when working with a flame ionization detector, which is one of the dosing volume (V2or V3) fills this component for the joint analysis with the original mixture (dose V1).

CHROMATOGRAPH containing a source of carrier gas, the first and second dispensers are connected to the line of the original mixture, the third dispenser, the first separation column with a flow divider mounted on its output, which is connected simultaneously with the first detector with the comparative and the measuring chamber, and through switch gas flows from the cumulative columns defined components, provided with a device for maintaining a predetermined temperature desorption and connected via switch gas flows from the metering volumes of the second and third dispensers, the second separation column with a concentration detector, having comparative and measuring chamber on its output and the second dispenser at its input, characterized in that it has a fourth dispenser installed in series with the first and third Donatos gas flows connected with dosing volumes respectively of the third and second or the fourth and second dispensers are additionally introduced through the gas valve, and the line original mix connected via a flow divider with comparative Luggage concentration detector.

 

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FIELD: chemical technology.

SUBSTANCE: invention relates to a method for synthesis of ester perfluorinated derivative by using a chemical reaction. This reaction represents the fluorination reaction of the parent compound as a raw, the reaction of chemical conversion of fragment of ester perfluorinated derivative to yield another ester perfluorinated derivative or the interaction reaction of carboxylic acid with alcohol under condition that at least one or reagent, i. e. carboxylic acid or alcohol, represents a perfluorinated compound wherein indicated perfluorinated derivative of ester represents a compound comprising a fragment of the formula (1):

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8 cl, 1 dwg, 2 ex

FIELD: instrument engineering.

SUBSTANCE: device for generating flow of vapor-gas mixture with preset concentration of vapor has vessel partially filled with fluid, second vessel provided with branch pipes for supply and removal of gas, and vapors of fluid pipeline-leak. One of vessels is connected with gas discharge forcer; fluid vapors pipeline-leak connects both vessels. Vessel, partially filled with fluid, is mounted inside second vessel. Pipeline-line, connecting both vessels, is totally placed inside second vessel. Device is also provided with additional discharge forcer for adjusting concentration of fluid vapor in second vessel. Granulated filler is introduced into vessel partially filled with fluid. Device is also provided with gas analyzer for providing gas concentration in space of second vessel.

EFFECT: higher precision of keeping of preset concentration of vapor; improved efficiency of vapor concentration control and adjustment.

FIELD: instrument engineering.

SUBSTANCE: invention is designed for calibrating gas analyser detectors, according to which there prepared is calibration substance solution with concentration A=By/k (%) as per Henry constant value k (mg/m %) at calibration temperature and as per the specified value of calibration substance mass concentration in calibration steam/gas mixture By (mg/m). After the solution has been introduced into the vessel in quantity enough for fully saturated equilibrium calibration steam/gas mixture to appear above the solution surface, the sensor calibration is carried out by means of mixture; at that, mixture concentration is changed by means of direct proportional change of solution concentration by diluting concentrated reference solution of calibration substance with analytical accuracy up to the specified concentration value A (%). There also proposed is the device for realising this method, which includes a solution point for preparing calibration solution with analytical accuracy, vessel with thermostatic device for obtaining steam/gas mixture with constant concentration corresponding to Henry law; at that, solution point includes graduated dose metre, graduated diluter, mixer with a reducer, capacity with solvent, and reference container with reference solution, which is stabilised with a gate valve meant for multiple use of container, and vessel with thermostatic device consists of thermometre and heat-insulating cover plate with an inlet branch pipe containing a normally closed return valve and a pusher for valve opening.

EFFECT: decrease of calibration substance losses; accuracy and reproducibility of metrological performance, and meeting requirements of industrial and ecological safety.

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11 cl, 2 dwg

FIELD: chemistry.

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EFFECT: invention allows increasing accuracy of quantitative determination of manganese, lead and nickel in bile.

6 tb

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1 cl, 1 ex, 1 tbl, 1 dwg

FIELD: chemistry.

SUBSTANCE: invention relates to analytical chemistry, particularly to methods of determining benzoic acid, and describes a method for quantitative determination of benzoic acid from a methyl derivative thereof - methyl ether in aqueous matrices with determination sensitivity of 5.010-5 mg/cm3 with determination error of not more than 25%. The method is characterised by that quantitative determination of benzoic acid is carried out using a chromatographic method with flame-ionisation detection and includes the following steps: extraction concentration of an analyte with benzene in water samples acidified with 25% sulphuric acid solution to pH 1-3 while adding sodium chloride until a saturated solution is obtained, conducting a benzoic acid methylation reaction with diazomethane to obtain a derivative - methyl ether of benzoic acid and determining the formed methyl ether of benzoic acid by a chromatographic method with flame-ionisation detection.

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1 ex, 3 tbl

FIELD: instrumentation.

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3 cl, 6 tbl, 1 ex

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1 cl, 6 dwg, 2 tbl, 1 ex

FIELD: physics; measurement.

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8 cl, 5 dwg

FIELD: instrument making.

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EFFECT: abrupt increase of concentration of adsorbed substance by increasing the amount of accumulated substance on maximum large surface with its further desorption to volume of minimum dimensions.

2 dwg

FIELD: chemistry.

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EFFECT: improved reliability of results, reduced power costs and material consumption.

12 cl, 2 dwg

FIELD: investigating or analyzing materials.

SUBSTANCE: method comprises supplying of batched volumes of oil sample, standard material for comparison, and n-heptane by displacing them by the gas flow to the capillary column for chromatography. The pressure in the gas flow is higher than that at the inlet of the column. The device comprises batching cock, check valve in the gas line, and resistance in the line for discharging the gas. The valving members are made of pipes with plugs at the center and are interconnected through a gas cross-piece and vessel for batching the gas.

EFFECT: enhanced accuracy of determining hydrocarbons.

2 cl, 1 dwg, 1 tbl

FIELD: physics.

SUBSTANCE: proposed device comprises unit of carrier gas preparation, sample feed assembly, two chromatographic columns, DC source, detector and results processing system, all said units being connected in series. Note here that one of the columns is connected with sample feed assembly, while the other one is connected with detector. Note also that second column is mounted between two flat parallel electrodes connected to DC source.

EFFECT: higher efficiency and selectivity.

1 tbl, 1 dwg

FIELD: physics.

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2 cl, 1 dwg, 1 tbl

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