Method for biological material analysis for tetramethylthiuramsulphide

FIELD: medicine.

SUBSTANCE: biological tissue is crushed, processed twice for 30 minutes with portions of ethyl acetate, weight of each twice exceeding weight of a biological object; prepared extractions are combined, filtered through anhydrous sodium sulphate; a solvent is evaporated from the filtrate; the residue is dissolved in acetonitrile; the prepared solution is watered down in the volume ratio 1:4, extracted twice in portions of chloroform, volume of each being equal to volume of a hydrophilic layer; the chloroform extracts are combined, steamed to a dry residue; the residue is dissolved in mixed solvents hexane-dioxane-propanol-2, cleaned in a silica gel column L 40/100µ with using a mobile phase hexane-dioxane-propanol-2; eluate fractions containing an analysed substance are combined; the eluent is evaporated; the residue is dissolved in mixed solvents hexane-dioxane-propanol-2 and analysed by a HELC method in a column of dimensions 64×2 mm filled with the sorbent Silasorb 600 with using a mobile phase hexane-dioxane-propanol-2 and a UV detector.

EFFECT: invention allows higher selectivity, sensitivity and accuracy of biological material analysis for tetramethylthiuramdisulfide.

4 ex, 5 tbl

 

The invention relates to the biology, ecology, sanitary and Toxicological chemistry, and in particular to methods of determining tetramethylthiuramdisuphide in biological material, and can be used in the practice of epidemiological stations, chemical-Toxicological, clinical, veterinary and environmental laboratories. The method refers to the mass number.

There is a method of determining derivatives dithiocarbamates acid, including tetramethylthiuramdisuphide, in biological material of plant origin, based on the grinding biological samples, treated with a solution of tin dichloride and the solution chloroethanol acid at 30°C in a sealed vial for one hour, the selection of the vial vapor-gas phase above the biological material, the introduction of samples into the evaporator gas-liquid chromatograph equipped with a detector constant recombination velocity, with subsequent chromatographytandem column length of 2 m and an internal diameter of 3.5 mm, filled with chromatone-N-cynep with 5% QF-1, with using nitrogen as the carrier gas at a feed rate of the mobile phase of 20 ml/min, column temperature, evaporator and detector, respectively, 60, 100 and 140°C (Methods for the determination of trace pesticides in food, feed and the environment. Vol. 1. - M.: Kolos, 1992. - S-377).

The method is characterized by low selectivity and low accuracy.

There is a method of determining tetramethylthiuramdisuphide in biological material (tissues, organs), which consists in grinding a biological sample, process it within 30 minutes portion of ethanol, one and a half times by weight greater than the number of the biological object, the separation of extract obtained from particles of biomaterial filtering processing of the filtrate ethanolic solution of copper sulfate (II) under conditions of heating at 50-60°C., cooling the resulting colored solution followed by measuring its optical density in the region of 440 nm (Kramarenko V.F., turkevych BM Analysis of pesticides. - M.: Chemistry, 1978. - P.222-223).

The method is characterized by low selectivity, high enough sensitivity and accuracy.

The closest is the way to determine tetramethylthiuramdisuphide in biological material, which consists in grinding the sample, processing approximately equal to the mass amount of the mixture of n-hexane and chloroform, taken in a volume ratio of 6:4, for two hours, separating the resulting extract, chromatographicaliy column filled with anhydrous sodium sulfate and silica gel using the mobile phase hexane-chloro who Orme (6:4 by volume), the evaporation of all the collected eluate to the solids handling balance in sulfuric acid medium with a solution of hydroquinone, and then a solution of copper acetate (II), followed by measuring the optical density of the resulting colored solution in the region of wavelengths 400-420 nm (Mazanowski AB, Fartusi A.F., Sedov, A.I., BACS have Viznachennya the teturama i turama influence materal // Farmaceutyczny magazine. - 1979. No. 2. - P.54-57).

The method is characterized insufficiently high sensitivity, low selectivity, relatively low accuracy.

The present invention is to improve the sensitivity, selectivity and accuracy of definition.

This object is achieved by using the proposed method, which consists in the fact that biological tissue is crushed, twice for 30 minutes, treated with portions of ethyl acetate, the mass of each of which exceeds 2 times the mass of a biological object. The obtained extract combine, filtered through anhydrous sodium sulfate, the solvent of the filtrate is evaporated, the residue is dissolved in acetonitrile, the resulting solution is diluted with water in a volume ratio of 1:4, extracted twice with portions of chloroform, each volume of which is equal to the volume of the hydrophilic layer, the chloroform extracts are combined evaporated to a dry residue, the residue rest the accelerate in a solvent mixture of hexane - dioxane - propanol-2 (15:5:1 by volume), purified in a column of silica gel L 40/100µ using the mobile phase hexane - dioxane - propanol-2 (15:5:1 by volume), fractions of the eluate containing an analyte, unite, eluent is evaporated, the residue is dissolved in a solvent mixture of hexane - dioxane - propanol-2 (15:5:1 by volume) and carry out the determination by HPLC in a column of size 64×2 mm, filled with sorbent Silsor 600" by using the mobile phase hexane - dioxane-propanol-2 (15:5:1 by volume) and UV-detector.

The method is as follows: biological tissue containing tetramethylthiuramdisulphide, crushed, twice for 30 minutes, treated with portions of ethyl acetate, the mass of each of which is twice the mass of a biological object, resulting extract is separated from the solid particles of the biomaterial, combine, combined extract was filtered through anhydrous sodium sulfate, the solvent is evaporated from the filtrate, the residue is dissolved in acetonitrile, the resulting solution is diluted with water in a volume ratio of 1:4, extracted twice with portions of chloroform, each volume of which is equal to the volume of the hydrophilic layer, the chloroform extracts are combined evaporated to a dry residue, the residue is dissolved in a mixture of solvents hexane - dioxane - propanol-2 (15:5:1 by volume), making a column of silica gel L 40/10µ, chromatographic, using the mobile phase hexane - dioxane - propanol-2 (15:5:1 by volume), fractions of the eluate containing an analyte, unite, eluent is evaporated, the residue is dissolved in a solvent mixture of hexane - dioxane - propanol-2 (15:5:1 by volume) and carry out the determination by HPLC in the column with sorbent Silsor 600" using the mobile phase hexane - dioxane - propanol-2 (15:5:1 by volume) and UV-detector.

Example 1

The definition of tetramethylthiuramdisuphide in liver tissue

To 10 g of finely ground liver tissue was added 5 mg of tetramethylthiuramdisuphide, thoroughly mixed biological tissue with a substance and leave for half an hour at a temperature of 18-20°C. after this time the biological object containing an analyte, pour 20 g of ethyl acetate and incubated for 30 minutes with occasional stirring. The extract is separated from the solid particles of the biomaterial, the operation processing is repeated in these conditions. Separate hoods combine, filtered through a glass filter with a diameter of 4 cm with a layer of anhydrous sodium sulfate height of 1-1,5 cm Filter additionally washed with 10 g of ethyl acetate. The filtrate and wash liquid are combined, the solvent evaporated under conditions of heating in a water bath at 50-60°C. the Residue is dissolved in 10 ml of acetonitrile, to the floor of the obtained solution was added 40 ml of water and extracted twice with portions of chloroform, 50 ml each. Separate extracts are combined into varicellae Cup, combined extract evaporated to a dry residue under conditions of heating in a water bath at 50-60°C. the Residue is dissolved in 2-3 ml of the solvent system hexane-dioxane-propanol-2 (15:5:1 by volume). The resulting solution contribute to column dimensions 490×11 mm, filled with 10 g of silica gel L 40/100µ. After full entry of the solution into the layer of sorbent in the column add eluent - solvent system hexane-dioxane-propanol-2 (15:5:1 by volume). Emerging from the column eluate is collected in separate fractions of 2 ml each. Fractions 4 and 5 are combined into varicellae Cup, eluent evaporated under conditions of heating at 50-60°C in a water bath. The residue is dissolved in a mixture of 10 ml of dioxane and 2 ml of propanol-2, quantitatively transferred into a volumetric flask with a capacity of 25 ml and bring the contents of the flask to the mark with hexane. 8 μl of the obtained solution are injected type "milikhrom".

Chromatographic by HPLC. The process of chromatography was carried out is carried out in a column of size 64×2 mm, filled normalnotorowym sorbent "Selasar 600" using the mobile phase hexane-dioxane-propanol-2 (15:5:1 by volume) and UV-detector.

The feed rate of eluent is 100 ál/min Scale registration of 0.8 eop, the measurement time of 0.6 sec. The optical density recorded at a wavelength of 276 nm./p>

The peak on the chromatogram with time holding 4,15 min (retention 415 μl) corresponds to tetramethylthiuramdisuphide.

The quantitative content of tetramethylthiuramdisuphide determine, based on the chromatographic peak area, the equation of the calibration graph and count on a portion of the substance made in the liver tissue.

Preparation of calibration graph.

In a series of volumetric flasks with a capacity of 10 ml make 0,25; 0,5; 1,0; 2,0; 4,0; 5,0 ml of 0.01% solution of tetramethylthiuramdisuphide in a solvent mixture of hexane-dioxan-propanol-2 (15:5:1 by volume) and bring to the mark with a mixture solvent of hexane-dioxane-propanol-2 (15:5:1 by volume). 8 μl of each of the obtained solutions are injected. The chromatography was carried out is carried out in a column of size 64×2 ml, filled with sorbent Silsor 600"using the mobile phase hexane-dioxane-propanol-2 (15:5:1 by volume) and a UV detector. The feed rate of eluent is 100 ál/min

The scale registration of 0.8 eop, the measurement time of 0.6 sec. The optical density recorded at a wavelength of 276 nm.

According to the results of measurements on the chromatograph build a graph of the dependence of chromatographic peak area against the concentration of the detected substance. Linear within the concentration range of 0.02 to 0.4 mcg.

By the method of least squares to calculate the calibration equation graphy is a, which in this case is:

S=10,94309·C+0,156341,

where S is the area of the chromatographic peak With the concentration of analyte in khromatograficheskoi sample, ág.

The results of quantitative determination of tetramethylthiuramdisuphide presented in table 1.

Example 2

The definition of tetramethylthiuramdisuphide in the tissue of the stomach

To 10 g of finely ground tissue of the stomach is added 5 mg of tetramethylthiuramdisuphide, thoroughly mixed biological tissue with a substance and leave for 1.5 hours at a temperature of 18-20°C. after this time the biological object containing an analyte, pour 20 g of ethyl acetate and incubated for 30 minutes with occasional stirring. The extract is separated from the solid particles of the biomaterial, the operation processing is repeated in these conditions. Separate hoods combine, filtered through a glass filter with a diameter of 4 cm with a layer of anhydrous sodium sulfate height of 1-1,5 cm Filter additionally washed with 10 g of ethyl acetate. The filtrate and wash liquid are combined, the solvent evaporated under conditions of heating in a water bath at 50-60°C. the Residue is dissolved in 10 ml of acetonitrile, the resulting solution was added 40 ml of water and extracted twice with portions of chloroform, 50 ml each. Separate extracts are combined into varicellae cha is ke, combined extract evaporated to a dry residue under conditions of heating in a water bath at 50-60°C. the Residue is dissolved in 2-3 ml of the solvent system hexane-dioxane-propanol-2 (15:5:1 by volume). The resulting solution contribute to column dimensions 490×11 mm, filled with 10 g of silica gel L 40/100µ. After full entry of the solution into the layer of sorbent in the column add eluent - solvent system hexane-dioxane-propanol-2 (15:5:1 by volume). Emerging from the column eluate is collected in separate fractions of 2 ml each. Fractions 4 and 5 are combined into varicellae Cup, eluent evaporated under conditions of heating at 50-60°C in a water bath. The residue is dissolved in a mixture of 10 ml of dioxane and 2 ml of propanol-2, quantitatively transferred into a volumetric flask with a capacity of 25 ml and bring the contents of the flask to the mark with hexane. 8 μl of the obtained solution are injected type "milikhrom".

Chromatographic by HPLC. The process of chromatography was carried out is carried out in a column of size 64×2 mm, filled normalnotorowym sorbent "Selasar 600" using the mobile phase hexane-dioxane-propanol-2 (15:5:1 by volume) and UV-detector.

The feed rate of eluent is 100 ál/min Scale registration of 0.8 eop, the measurement time of 0.6 sec. The optical density recorded at a wavelength of 276 nm.

The peak on the chromatogram with time holding 4.15 m is n (volume retention 415 μl) corresponds to tetramethylthiuramdisuphide.

The quantitative content of tetramethylthiuramdisuphide determine, based on the chromatographic peak area, the equation of the calibration graph and count on a portion of the substance introduced into the tissue of the stomach.

Preparation of calibration graph and its equation is given above in example 1.

Example 3

The definition of tetramethylthiuramdisuphide in wheat

To 10 g of finely ground tissue of wheat grains add 5 ml of tetramethylthiuramdisuphide, thoroughly mixed biological tissue with a substance and leave for 1.5 hours at a temperature of 18-20°C.

After this time the biological object containing an analyte, pour 20 g of ethyl acetate and incubated for 30 minutes with occasional stirring. The extract is separated from the solid particles of the biomaterial, the operation processing is repeated in these conditions. Separate hoods combine, filtered through a glass filter with a diameter of 4 cm with a layer of anhydrous sodium sulfate height of 1-1,5 cm Filter additionally washed with 10 g of ethyl acetate. The filtrate and wash liquid are combined, the solvent evaporated under conditions of heating in a water bath at 50-60°C. the Residue is dissolved in 10 ml of acetonitrile, the resulting solution was added 40 ml of water and extracted twice with portions of chloroform, 50 ml each. Separate xtracta unite in varicellae Cup, combined extract evaporated to a dry residue under conditions of heating in a water bath at 50-60°C. the Residue is dissolved in 2-3 ml of the solvent system hexane-dioxane-propanol-2 (15:5:1 by volume). The resulting solution contribute to column dimensions 490×11 mm, filled with 10 g of silica gel L 40/100µ. After full entry of the solution into the layer of sorbent in the column add eluent - solvent system hexane-dioxane-propanol-2 (15:5:1 by volume). Emerging from the column eluate is collected in separate fractions of 2 ml each. Fractions 4 and 5 are combined into varicellae Cup, eluent evaporated under conditions of heating at 50-60°C in a water bath. The residue is dissolved in a mixture of 10 ml of dioxane and 2 ml of propanol-2, quantitatively transferred into a volumetric flask with a capacity of 25 ml and bring the contents of the flask to the mark with hexane. 8 μl of the obtained solution are injected type "milikhrom".

Chromatographic by HPLC. The process of chromatography was carried out is carried out in a column of size 64×2 mm, filled normalnotorowym sorbent "Selasar 600" using the mobile phase hexane-dioxane-propanol-2 (15:5:1 by volume) and UV-detector.

The feed rate of eluent is 100 ál / min Scale registration of 0.8 eop, the measurement time of 0.6 sec. The optical density recorded at a wavelength of 276 nm.

The peak on the chromatogram with time holding 4,15 is Jn (volume retention 415 μl) corresponds to tetramethylthiuramdisuphide.

The quantitative content of tetramethylthiuramdisuphide determine, based on the chromatographic peak area, the equation of the calibration graph and count on a portion of the substance introduced into the tissue of wheat.

Preparation of calibration graph and its equation is given above in example 1.

Example 4

The definition of tetramethylthiuramdisuphide in the seeds of sugar beet

To 10 g of finely ground tissue of sugar beet seeds added 5 mg. of tetramethylthiuramdisuphide, thoroughly mixed biological tissue with a substance and leave for 1.5 hours at a temperature of 18-20°C. after this time the biological object containing an analyte, pour 20 g of ethyl acetate and incubated for 30 minutes with occasional stirring. The extract is separated from the solid particles of the biomaterial, the operation processing is repeated in these conditions. Separate hoods combine, filtered through a glass filter with a diameter of 4 cm with a layer of anhydrous sodium sulfate height of 1-1,5 cm Filter additionally washed with 10 g of ethyl acetate. The filtrate and wash liquid are combined, the solvent evaporated under conditions of heating in a water bath at 50-60°C. the Residue is dissolved in 10 ml of acetonitrile, the resulting solution was added 40 ml of water and extracted twice with portions of chloroform at 50 is l each. Separate extracts are combined into varicellae Cup, combined extract evaporated to a dry residue under conditions of heating in a water bath at 50-60°C. the Residue is dissolved in 2-3 ml of the solvent system hexane-dioxane-propanol-2 (15:5:1 by volume). The resulting solution contribute to column dimensions 490×11 mm, filled with 10 g of silica gel L 40/100µ. After full entry of the solution into the layer of sorbent in the column add eluent - solvent system hexane-dioxane-propanol-2 (15:5:1 by volume). Emerging from the column eluate is collected in separate fractions of 2 ml each. Fractions 4 and 5 are combined into varicellae Cup, eluent evaporated under conditions of heating at 50-60°C in a water bath. The residue is dissolved in a mixture of 10 ml of dioxane and 2 ml of propanol-2, quantitatively transferred into a volumetric flask with a capacity of 25 ml and bring the contents of the flask to the mark with hexane. 8 μl of the obtained solution are injected type "milikhrom".

Chromatographic by HPLC. The process of chromatography was carried out is carried out in a column of size 64×2 mm, filled normalnotorowym sorbent "Selasar 600" using the mobile phase hexane-dioxane-propanol-2 (15:5:1 by volume) and UV-detector.

The feed rate of eluent is 100 ál/min Scale registration of 0.8 eop, the measurement time of 0.6 sec. The optical density recorded at a wavelength of 276 nm./p>

The peak on the chromatogram with time holding 4,15 min (retention 415 μl) corresponds to tetramethylthiuramdisuphide.

The quantitative content of tetramethylthiuramdisuphide determine, based on the chromatographic peak area, the equation of the calibration graph and count on a portion of the substance introduced into the tissue of sugar beet seeds.

Preparation of calibration graph and its equation is given above in example 1.

The proposed method is compared with the prototype 3 times increases the detection sensitivity (open at least reduced from 1 mg to 0.3 mg per 100 g liver tissue), characterized by a higher selectivity (in contrast to the known method, it allows the determination of artemetherlumefantrine in the presence of a number of closely related structure compounds: tetraethylthiuramdisulphide, diethyldithiocarbamate sodium, tetramethylrhodamine, tetradecylthioacetic, carbon disulfide), increases the accuracy (relative error of the mean of the reduced 1.5 times). Comparative characteristics of the proposed and known methods are presented in table 5.

Table 1
The results of determining tetramethylthiuramdisulphide is in the liver tissue
No.Made of tetramethylthiuramdisuphide, mg in 10 g liverFoundMetrological characteristics
mg%
1.5,002,98259,64
2.5,003,15363,06S=2,34
3.5,003,24264,84
4.5,003,30666,12
5.5,003,06361,26

Table 2
The results of determination of tetramethylthiuramdisuphide in the tissue of the stomach
No.Made of tetramethylthiuramdisuphide, mg in 10 g of tissue of the stomachFoundMetrological characteristics
mg%
1.5,004,02080,39
2.5,003,81776,34S=2,18
3.5,003,96379,26
4.5,003,93478,67
5.5,004,15183,02

Table 3
The results of determination of tetramethylthiuramdisuphide in wheat
No.Made of tetramethylthiuramdisuphide, mg in 10 g of wheatFoundMetrological characteristics
mg%
1.5,004,22684,51
2.5,004,12282,44S=2,04
3.5,004,26885,35
4.5,004,02980,58
5.5,004,31086,19ε=3,03

Table 4
The results of determination of tetramethylthiuramdisuphide in the seeds of sugar beet
No.Made of tetramethylthiuramdisuphide, mg in 10 g of sugar beet seedsFoundMetrological characteristics
mg%
1.5,004,49986,82
2.5,004,50490,07S=1,75
3.5,004,41688,31
4.5,004,26585,29
5.5,004,47489,48 ε=2,48

Table 5
Comparative characteristics of the proposed and known methods (for example, the study of the liver tissue)
IndexThe proposed methodThe known method
1. Sensitivity (open minimum) in 100 g of a biomaterial0.3 mg1.0 mg
2. SelectivityAllows you to selectively define tetramethylthiuramdisulphide in the presence of closely related structure compounds (tetraethylthiuramdisulphide, diethyldithiocarbamate sodium, tetramethylrhodamine, tetradecylthioacetic, carbon disulfide)Does not allow you to selectively define tetramethylthiuramdisulphide in the presence of closely related structure compounds (tetraethylthiuramdisulphide, diethyldithiocarbamate sodium, tetramethylrhodamine, tetradecylthioacetic, carbon disulfide)
3. The relative error of the mean results (n=5; P=0,95) (provided content 50 mg analyte per 100 g of biomaterial)About 7%

Method of determining tetramethylthiuramdisuphide in biological material, which consists in the fact that the analyzed sample is crushed, treated with an organic extractant, the organic extract dehydrated, passing through a layer of anhydrous sodium sulfate, purified by column chromatography was carried out gidrauxilirovannogo sorbent, using as mobile phase a mixture of organic solvents, emerging from the column eluate is collected, evaporated to a dry residue with subsequent determination of the analyte chemical method, wherein as the organic extractant used ethyl acetate, the processing of the sample carried out twice for 30 min portions of ethyl acetate, the mass of each of which is twice the weight biomaterial, after dehydration of an ethyl acetate extract, the ethyl acetate is evaporated, the residue is dissolved in acetonitrile, the resulting solution is diluted with water in a volume ratio of 1:4, extracted twice with portions of chloroform, each volume of which is equal to the volume of the hydrophilic layer, the chloroform extracts are combined evaporated to a dry residue, the chromatographic purification is carried out in a column of silica gel L 40/100µ using the mobile phase hexane-dioxane-propanol-2 (15:5: amount of the residue obtained after evaporation of the fractions of the eluate containing an analyte, dissolved in a solvent mixture of hexane-dioxane-propanol-2 (15:5:1 by volume) and carry out the determination by HPLC in a column of size 64×2 mm, filled with sorbent Silsor 600", using the mobile phase hexane-dioxane-propanol-2 (15:5:1) and UV detector.



 

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9 cl, 1 dwg

FIELD: chemistry.

SUBSTANCE: invention relates to analytical chemistry. The method is realised as follows: a sample of ground up premix is filled with a hydrochloric acid solution and put into an opaque case which is put into an ultrasonic bath. Extraction is carried out for 15-20 minutes at 38-42°C and centrifuging is then carried out for 10 minutes at 8000 rpm. The mixture is then brought up to the mark in a measurement flask. The obtained solution undergoes chromatographic separation on a column with Purospher sorbent. Chromatography conditions: eluent A - 0.005 M lithium perchlorate solution, pH=2.5; eluent B- acetonitrile; elution gradient mode - from 0 to 26% eluent B for 14 minutes.

EFFECT: high efficiency and accuracy and possibility of detecting a wider range of vitamins independent of the premix base.

2 dwg, 5 tbl, 1 ex

FIELD: chemistry.

SUBSTANCE: method for chromatographic analysis of a substance involves exposing the separated mixture of substances carried by a carrier through a chromatographic column to acoustic oscillations. Before chromatographic analysis, a liquid nematic crystal is deposited on the wall of the chromatographic column, where the said crystal is directed across the propagation of sound oscillations.

EFFECT: high efficiency of separating an analysed mixture of substances into components using sound waves.

1 dwg

FIELD: oil and gas industry.

SUBSTANCE: gas chromatograph includes chamber for samples with piston position sensor, which is connected through sample valve to pipeline and through oil pump to reservoir for compensation of hydraulic oil pressure, electrical thermostat with temperature sensor and chromatograph tube located inside thermostat, which is in-series connected on one side through rotating sample injector, zeolite filter, the first return valve and isolating valve of chromatograph with connection line of sample valve and chamber for specimens, in-series connected on the other side to the second return valve, fraction detector, bottle with sample portion and the second pressure sensor. At that, rotating sample injector is in-series connected to pressure reducer, valve for transporting medium, bottle with compressed nitrogen and the first pressure sensor, bypass line with bypass valve is parallel connected to rotating sample injector, chromatograph tube and fraction detector, and circuit of electronic telemetry is connected to output of fraction detector. Method of downhole gas chromatography is proposed as well.

EFFECT: development of device allowing to perform gas chromatography for determining the type of well fluids in well in real time.

3 cl, 5 dwg

FIELD: chemistry.

SUBSTANCE: device for chromatographic separation of substances contains three chromatographic columns connected to each other by crossover channels fitted with switching elements and extra channels fitted with switching elements which are connected to a source of the separated medium, eluent stream and system of receivers for collecting fractions. A controlled flow divider, one or more detectors and an analytical column are fitted at the output of the chromatographic separation system. Also in order to increase output and efficiency of the device for chromatographic separation of substances dissolved in supercritical fluids, the receivers for collecting fractions are fitted with level sensors and their outputs are further fitted with pilot-controlled valves which prevent diffusion of collected substances between receivers. The device also has a collector with a receiver and a flow regulator for the stream of fluids evaporated when pressure falls below the critical value. The device also has a high-pressure pump whose output is also connected to the flow regulator with pressure sensors at the input and output and a flow sensor, which guide part of the stream of formed fluids through the pilot-controlled valve into one or more spherical reactors which have an outer insulating layer and outer and inner heat chambers connected to heat or cold sources, temperature sensors, and the other part of the stream is directed to the analytical column and reactor. The reactor is connected through the pilot-controlled valve to the spherical collector of fluid solutions which is similar to the reactor whose output is connected to liquid batch collection device.

EFFECT: more accurate batching and increased output and efficiency of the disclosed device.

1 dwg

FIELD: chemistry.

SUBSTANCE: method involves taking a sample, concentration of impurities, chromatographic analysis with separation of the concentrate on a capillary column and mass-selective detection while raising temperature from 35°C to 280°C, isolation of tridecane and 1-methylnaphthalene as reference compounds on the chromatogram, calculation of their concentration ratio in the sample and calculation of the time of contact between diesel fuel and water using the formula: x=0.42·y-1.8, where x is the time of contact between diesel fuel and water, h; y=Stridecane/Smethylnaphthalene; Stridecane and Smethylnaphthalene are area of peaks of tridecane and 1-methylnaphthalene on reconstructed chromatograms on selective ions with mass to charge ratio of 85 for tridecane and 145 for 1-methylnaphthalene, which correspond to concentrations of given compounds in the sample.

EFFECT: simple and reliable method with high information content.

1 ex, 1 tbl

FIELD: test equipment.

SUBSTANCE: proposed invention relates to gas chromatographic analysis and can be used in alcohol quality tests. Proposed method consists in that, additionally, water-spirit mix in the ratio of 60/40% by volume is prepared to a series of model samples based thereon to prepared by adding every component of analysed drink separately in said mix. Then model sample are analysed at the inlet assembly temperature of 180°C, 250°C and 310°C. Note that unknown substance detected in model sample is qualified as artifact formed in analysis, while is it is absent from model samples, check sample is prepared by combining the entire series of model samples to be analysed at aforesaid 180°C, 250°C and 310°C. Then mass spectra and chromatograms related therewith are analyzed and, if there is no revealed unknown substance in check sample, it is qualified as marker of nonfoods origin.

EFFECT: unambiguous identification of chemical compounds and fragments thereof as well as their origin, higher accuracy and faster identification.

4 tbl, 3 ex

FIELD: chemistry.

SUBSTANCE: invention relates to chemistry and can be used in coke-chemical production when processing coke gas. The method involves using fractions of heavy crude pyridine bases which form during coal carbonisation as raw material, from which pyridine bases are extracted first and the obtained faction of crude quinoline bases is split into components. The fractions of crude quinoline bases are split into components through supercritical preparative chromatography, where the separated mixture is brought into contact with gas in supercritical state, which is simultaneously the mobile phase and adsorbent.

EFFECT: simpler, faster and more reliable separation.

1 dwg

FIELD: chemical engineering; medical engineering.

SUBSTANCE: method involves plotting two chromatograms one of which is based on radioactivity (No 1) and the other one on ultraviolet absorption (No 2) or on radioactivity (No 1) and on fluorescence (No 2) and chromatogram specific relative to ultraviolet absorption (No 3) or relative to fluorescence (No 3). Material quality is estimated to be the more high the more close studied labeled compound peak shape is to trapezoid shape on the third chromatogram.

EFFECT: high accuracy of the method.

8 dwg

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