FIELD: chemistry.
SUBSTANCE: invention relates to sampling in chemistry, as well as to analytical chemistry equipment, and can be used for the rapid detection of components, as well as for the quantitative and qualitative determination of the content of individual organochlorine compounds, sulfur-containing compounds, formaldehyde in oil, naphtha, kerosene, gas oil, diesel fuel, naphtha fraction, fuel oil, gasoline, complex hydrocarbon mixtures, chemical reagents using a laboratory or industrial chromatograph analyzer by the method of equilibrium vapor analysis in cyclic and continuous modes. The proposed method for detecting the content of individual organochlorine and sulfur-containing components of a hydrocarbon mixture by chromatographic analysis of steam includes taking a sample of equilibrium steam and supplying steam through a pipeline or a nebulizer to a continuous or cyclic sampling device with a compressor in the form of a finely dispersed gas-liquid fraction at a rate of not more than 1000 ml / min, heating the sampling device to 20-150°С for no more than 60 min, ensuring the transition of the analyzed components to the vapor phase accumulating in the upper part of the sampler, while for more efficient extraction of the determined components into the vapor phase, bubbling is carried out with a heated inert gas, and after reaching the phase equilibrium, the transfer of equilibrium steam from the sampler is provided by opening the valve from the sampler into the dosing loop of the analyzer / chromatograph dosing valve through the supply line (with or without heating), and the loop is made with a volume from 10 μl to 5 ml, then dosing is carried out into the chromatographic guard column to separate interfering components-impurities, and the target components are sent to the next main analytical chromatographic column, where they are separated at a temperature of 50-350 ° C and registered with a detector, and the liquid part of the oil products is discharged through the drain located in the lower part of the sampling device, while the filling level of the sampling device is ensured using a level gauge or by the pressure value. Also proposed is a sampling device for extracting equilibrium vapor of continuous and cyclic type.
EFFECT: technical result of the claimed invention consists in the possibility of increasing the degree of extraction of components into the vapor phase with obtaining high sensitivity and precision of the method, reducing the analysis time, achieving a high degree of automation of the analysis, the possibility of using digital technologies, a wide range of analyzed components, simplifying the process of calibrating the chromatograph.
7 cl, 2 dwg, 1 tbl
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Authors
Dates
2021-03-31—Published
2020-04-30—Filed