Alcohol thermal dehydration chamber, apparatus and method of determining isotopic composition of non-exchangeable hydrogen and deuterium atoms in ethanol samples

FIELD: chemistry.

SUBSTANCE: described is an alcohol thermal hydration chamber and an apparatus for real-time determination of isotopic composition of non-exchangeable hydrogen and deuterium atoms in ethanol samples, comprising: A) an alcohol thermal dehydration chamber, B) an indicating device which has a pyrolysis reactor (26) and a continuous flow isotope spectrometer and is connected to the alcohol thermal dehydration chamber by C) a system of valves, connectors and capillary tubes which are used to transfer the analysed sample and clean the alcohol thermal dehydration chamber; the procedure for real-time determination of isotopic composition of non-exchangeable hydrogen and deuterium atoms in ethanol samples and the procedure for off-line preparation of ethene (ethylene) gas by means of the alcohol thermal dehydration chamber and for the identity and geographical origin of wines, alcoholic beverages, fruit juices, honey and etc.

EFFECT: high accuracy of determination.

9 cl, 3 dwg

 

The technical field

The present invention relates to a camera thermal dehydration of the alcohol, the apparatus and method for determining in real-time isotopic composition of non-hydrogen atoms and deuterium in ethanol sample and preparation method offline atenololo (ethylene) gas through thermal cameras dehydration, to determine the identity and geographical source of wines and grape must, beer, alcohol, fruit juices, honey and all other products that contain alcohol (ethanol) and/or formatiruem sugar.

Background of the invention

Isotopic methods have shown that they can be very powerful analytical tool for determining the authenticity and geographical sources of wines and spirits. Measuring the content of stable isotopes in these products, you can provide suitable information to detect many fakes in the production of wine and spirits. Instrumental techniques that are suitable for isotopic measurements are based on measuring the respective ratios of stable isotopes by mass spectrometry isotope ratios.

Systems containing pyrolysis chamber and isotope spectrometer in continuous flow CF-TC/EA-IRMS (instantaneous high temperature in a continuous flow - temperature p is the education/elemental analyzer - mass spectrometry isotope ratios from Thermo Electron Corporation), commercially available for the analysis of stable hydrogen solid and liquid samples.

In the analysis of ethanol samples by CF-TC/EA-IRMS (continuous flow - thermal conversion/elemental analyzer - mass spectrometry isotope ratios), because of the hydroxyl group of ethanol, which contains easily exchanged hydrogen, the resulting values of ∆ d for ethanol the same Botanical and geographical origin can vary, and for this reason unable to perform the qualitative and quantitative identification of the origin of the ethanol sample.

One of the problems that can occur, for example, in the manufacture of alcoholic beverages, is in the final stages of production. The distillate is diluted with water to determine the strength of spirit that is needed to alcoholic drink can be used. When adding water, which has a different isotopic content, dynamic isotopic equilibrium is disturbed, and the hydrogen or deuterium, which is linked to the oxygen atom of the hydroxyl group is exchanged. This is one of the reasons for determining error values ∆ d and erroneous information about the origin of ethanol.

Because of the problems noted above, instrumental technique CF-TC/EA-IRMS cannot be PTS is ery successful in detecting forgeries in the production of wine and alcoholic beverages and especially for the detection of ethanol, which is produced from sugar beet, barley, wheat, etc. in wine and alcoholic drinks.

According to the first aspect of the present invention Luggage thermal dehydration of the alcohol, the apparatus and method of determining the isotopic composition in real-time non-hydrogen atoms and deuterium in ethanol samples and the preparation method offline eterovich (ethylene) samples by means of the camera of thermal dehydration of alcohol, gives the opportunity to degidrirovanii ethanol and remove metabolic atom of hydrogen (or deuterium) hydroxyl group without loss or isotopic fractionation. This results in the stabilization and constant values of ∆ d, and this is due to the other atoms of hydrogen and deuterium, which are strongly linked to the carbon atoms in Tenenbaum (ethylene) gas, which is prepared from ethanol sample specific Botanical origin.

The disclosure of this invention

Measuring the relative proportions of deuterium and hydrogen for the purpose of determining the authenticity and origin of wines and alcoholic drinks, beer, fruit juices and honey currently performed by SNIF-NMR (specific natural isotope fractionation - nuclear magnetic resonance), which is based on intermolecular scan measured ethanol sample is the determination of the isotopic composition of hydrogen atoms and deuterium, located on the first and second carbon atom in the ethanol molecule. The results obtained by the method SNIF-NMR, provide information about the presence of ethanol, which comes from sugar beet or other industrial plants, and which belong to the group of C3 plants.

This instrumental technique is very accurate, but has some drawbacks.

Some of these disadvantages:

- first, SNIF-NMR is a very expensive device and method and requires a lot of financial capital (high consumption of helium and liquid nitrogen, and electric energy),

the time required for analysis, it is quite long (a small number of samples can be analyzed),

- occupies a large part of the workplace because of its size and because of the very strong magnetic field that it creates (it requires protection zone),

standards, which are used in the analysis, dear.

The disclosure of this invention

The main purpose of this invention is to overcome barriers and shortcomings of the presently known devices and methods of isotopic composition of non-hydrogen atoms and deuterium in ethanol samples.

The above and additional goals are achieved with the camera thermal dehydration of the alcohol according to claim 1, the apparatus for determining in real-time isotopic composition is obmennik atoms of hydrogen and deuterium in ethanol samples according to claim 2, camera thermal dehydration of the alcohol according to claim 1 and option 1 for the preparation of offline eterovich (ethylene) samples according to claim 3, procedures for determining in real-time isotopic composition of non-hydrogen atoms and deuterium in ethanol samples according to claim 4, procedures for making offline eterovich (ethylene) samples, using the camera, thermal dehydration of alcohol, according to claim 5 and procedures and the principle of determining the authenticity and geographical origin of the wine, alcoholic beverages, fruit juices and honey 6.

According to the first aspect of the present invention Luggage thermal dehydration of alcohol contains: a reaction chamber that contains the top hole with cap and septa, which is used for introduction of the ethanol sample syringe, and the left side hole with a valve whose purpose is to clean the chamber with an inert gas helium. One part of the reaction vessel has the form of termokozhuhi that contains two electric heater. Also, alternatively, thermohousing is possible to apply an open flame to heat the reaction vessel. The second part of the reaction vessel, this part has a tubular shape, rotated to the right, contains a dehydration catalyst, and for this purpose it is possible to use aluminum oxide (Al2O3), with whom liegel, the zeolite or a mixture of these substances or similar materials. The right end of the reaction vessel is connected to the tube with a gas-tight stopper. Inside this tube with a gas-tight tube, you can put a small amount of silica gel or similar inert gigroskopichnomu material. The right end of the tube with a gas-tight tube contains two valves, which are used for cleaning camera thermal dehydration of alcohol helium gas. Luggage thermal dehydration of the alcohol is located on the cradle.

Camera thermal dehydration of the alcohol can be used as part of an apparatus for determining in real-time isotopic composition of non-hydrogen atoms and deuterium in ethanol samples and as an alternative solution for making offline eterovich (ethylene) samples. If it is used as an alternative solution for making offline eterovich (ethylene) samples, camera thermal dehydration of the alcohol added to the pre-vakuumirovannoi vessel, in which is collected atanomy gas. Prepared atanomy gas is then injected gas-tight syringe into existing instrumental techniques CF-TC/EA-IRMS or GC/TC-IRMS (gas chromatography/thermal conversion - mass spectrometer isotope balance of the clusters).

According to an additional aspect of this invention, the apparatus for determining in real-time isotopic composition of non-hydrogen atoms and deuterium in ethanol samples contains: A) the camera thermal dehydration of alcohol, In) display device that contains the pyrolysis reactor and isotope spectrometer in continuous flow, and it is attached to the camera thermal dehydration of alcohol through With a system of valves, connectors, and capillary tubes, which are used to move the analyzed sample for cleaning camera thermal dehydration of the alcohol.

It will be clear that the device will in General contain additional features, known in the prior art, for example, the control modules and the processor interacting with the functional components of the apparatus (automatic control). Can be provided by the implementation or appropriate modifications of the available laboratory equipment for control and interaction with the apparatus of this invention.

According to an additional aspect of this invention, the procedure and the principle of determining in real-time isotopic composition of non-hydrogen atoms and deuterium in ethanol samples is a pre-cleaning chamber thermal dehydration of alcohol in the Oka inert gas helium, introduction ethanol sample into a reaction chamber (introduction can be done manually or by autosampler), heating the alcohol and the production of superheated vapors of alcohol, and the passage of these ethanol vapor over a dehydration catalyst (alumina - Al2O3, silica gel, zeolite, or a mixture of these substances or similar materials) in the flow of carrier gas helium to the pyrolysis reactor. Elementary gases obtained by the pyrolysis prepared Athena (H2and WITH), pass through the column gas chromatography, where separated, and through an interface with an open flow divider comes in IRMS, where found.

According to an additional aspect of this invention, the procedure and the principle of making offline eterovich samples using thermal cameras dehydration of alcohol is a pre-cleaning chamber thermal dehydration of alcohol in a stream of inert gas helium through the left side hole opening of the valve for helium gas. Before you begin cleaning, you want to open the valves on the right side of the camera. After cleaning needs to close the right valve and then the valve for helium gas. After cleaning the metal needle with right side attached to pre-vakuumirovannoi the vessel and then driveout valve on the right side of the camera. Additionally, when heated reaction vessel through termokozhuhi or alternative open flame and the introduction of an ethanol sample in the reaction container is a dehydration reaction, and the generated gas Aten is collected in the vessel. After this, the vessel is removed from the camera and eaten then manually enter gas-tight syringe into existing instrumental techniques CF-TC/EA-IRMS or GC/TC-IRMS.

A brief description of graphic materials

The above and other features and objectives of this invention and the manner of achieving them will become more apparent, and the invention will be better understood with reference to the following description of various embodiments of the present invention in conjunction with accompanying graphics.

Figure 1 - camera view of thermal dehydration of the alcohol.

Figure 2 - view of the device determine in real-time isotopic composition of non-hydrogen atoms and deuterium in ethanol samples.

Figure 3 - view of option 1 camera thermal dehydration of the alcohol to cook offline eterovich samples and existing instrumental techniques CF-TC/EA-IRMS or GC/TC-IRMS.

The best embodiments of the present invention

In accordance with the idea of the invention of figures 1, 2 and 3 are illustrative of the camera image is ergicheskoi dehydration of alcohol, apparatus determining in real-time isotopic composition of non-hydrogen atoms and deuterium in ethanol samples and alternative camera thermal dehydration of the alcohol to cook offline for eterovich (ethylene) samples for existing instrumental techniques CF-TC/EA-IRMS or GC/TC-IRMS.

According to the idea of this invention figure 1 shows the camera thermal dehydration of alcohol. Figure 1 shows all the important parts of the camera thermal dehydration of alcohol. Luggage thermal dehydration of alcohol contains: a reaction chamber (1), which contains the top hole with cap and septa (2), which is used for introduction of the ethanol sample (6) syringe, and the left side hole (3) from valve (4), the purpose of which is to purify the inert gas helium. One part of the reaction vessel is a thermojacket (5), which contains two electric heater. Also alternatively, thermojacket (5) you can apply an open flame to heat the reaction vessel. The second part of the reaction vessel, this part has a tubular shape, turned to the right, figure 1, contains a dehydration catalyst (7), and for this purpose it is possible to use aluminum oxide (Al2O3), silica gel, zeolite, or a mixture of these substances or similar materials. With the rights of the th side of a reaction chamber connected to the tube with a gas-tight tube (8). Inside this tube with a gas-tight tube (8), a small amount of silica gel or similar inert giroskopicheskogo material can be placed (9). The right end of the tube with a gas-tight tube (8) contains two valves (10) and (11), which are used for cleaning camera thermal dehydration of alcohol helium gas. Luggage thermal dehydration of alcohol is on the cradle (15).

In accordance with the idea of the present invention Luggage thermal dehydration of the alcohol gives the opportunity to degidrirovanii ethanol and remove metabolic atom of hydrogen (or deuterium) hydroxyl group without loss or isotopic fractionation. Thus stabilization and constant values of ∆ d can be achieved, and it depends on other atoms of hydrogen and deuterium, which are strongly linked to the carbon atoms in atenolol (ethylene) gas, which is prepared from ethanol sample specific Botanical origin.

In accordance with the idea of the present invention figure 2 shows in detail the apparatus for determining in real-time isotopic composition of non-hydrogen atoms and deuterium in ethanol samples. Figure 2 shows all the important parts of apparatus for determining in real-time isotopic composition of non-hydrogen atoms and deuterium in ethanol samples it contains.

p> In accordance with the idea of the present invention apparatus for determining in real-time isotopic composition of non-hydrogen atoms and deuterium in ethanol samples contains: A) the camera thermal dehydration of alcohol, In) display device that contains the pyrolysis reactor and isotope spectrometer in continuous flow, and it is connected with camera thermal dehydration of alcohol through With a system of valves, connectors, and capillary tubes, which are used to move the analyzed sample for cleaning camera thermal dehydration of alcohol. Luggage thermal dehydration of alcohol, which is part of the apparatus for determining in real-time isotopic composition of non-hydrogen atoms and deuterium in ethanol samples, includes: a reaction chamber (1), which contains the top hole with cap and septa (2), which is used for introduction of the ethanol sample (6) syringe, and the left side opening (3) with "switching" valve to the "source" and "carrier" of helium gas (4). One part of the reaction vessel is a thermojacket (5), which contains two electric heater. The second part of the reaction vessel, this part has a tubular shape, turned to the right, figure 2, contains a dehydration catalyst (7), and for this purpose which you can use aluminum oxide (Al 2O3), silica gel, zeolite, or a mixture of these substances or similar materials. From the right end of a reaction chamber connected to the tube with a gas-tight tube (8). Inside this tube with a gas-tight tube (8) a certain amount of silica gel or similar inert gigroskopichnomu material can be placed (9). The right end of the tube with a gas-tight tube (8) contains two valves (10) and (11). The tube with a gas-tight tube (8) on one end connected by means of a connector introduction (12) directly to the pyrolysis reactor (26), which is connected by means of GC columns (22) and interface with the open flow divider (23), which has a capillary for helium dilution (24), with isotope ratio mass spectrometer IRMS (25). Luggage thermal dehydration of alcohol is on the stand (17), fixed to the body of the external equipment (16), which contains the pyrolysis reactor (26), screws (18). Capillary tube (21) with one end connected to the output of the helium source gas (15), which is used for cleaning the chamber, and with its other end connected with the "switching" valve (4). Capillary tube (20) through the "T" connector (13) with one end connected to the outlet of the main flow of the helium carrier gas" (14), and with its other end connected with the "switching" to what Apana (4). The output of the main stream of helium gas"media" (14) is connected through a "T" connector (13) and capillary tubes with protective valve (19) and connector introduction (12) on the pyrolysis reactor (26).

In accordance with the idea of the present invention the procedure and principle of operation with the apparatus for determining in real-time isotopic composition of non-hydrogen atoms and deuterium in ethanol samples contains the following steps.

The first phase relates to the cleaning chamber of thermal dehydration of alcohol, which is a part of the apparatus for determining in real-time isotopic composition of non-hydrogen atoms and deuterium in ethanol samples of the inert gas is helium. Before you begin cleaning, you must close the valve (11) and open valve (10), and then, through a side opening (3) and move the "switching" of the valve (4) into position for the "source" of helium gas (21), to start the cleaning chamber of thermal dehydration of alcohol. The flow of the "source" of helium gas should be in the range of 20 ml/min to 200 ml/minute. After the cleaning is made, it should last a maximum of 15 minutes, close the valve (10) and then open the valve (11) and move the "switching" valve (4) into position for the main gas flow of the"carrier" of helium (20). The flow of carrier gas helium must be in d is apatone from 70 ml/min to 170 ml/minute. After cleaning chamber thermal dehydration of the alcohol is made, the heating of the reaction vessel (1) through termokozhuhi (5) can be started up until the temperature reaches a range from 250°C to 500°C. Once this is done, enter a maximum of 1 ml of pre-distilled and selected alcohol (ethanol) sample of the analyzed wine, beer or alcoholic beverages or the like. When entering into a reaction chamber, the sample instantly evaporates into the superheated vapor of alcohol, in which the gas flow passes over the catalyst dehydration (7). When dehydration and water separation and absorption of the catalyst in excess prepared atanomy (ethylene) gas through a capillary tube with a gas-tight tube (8) and open valve (11) is included in the pyrolysis reactor (26) and then through the column for gas chromatography (22) and interface with the open flow divider (23) is detected isotope ratio mass spectrometer IRMS (25). The generated gas Aten (ethylene), prepared by thermal dehydration of alcohol, decomposed by pyrolysis to elemental gases (H2and CO), which then pass through the column for gas chromatography, where separated, and then through the interface with the open flow divider included in the IRMS where it is finally detected.

In accordance with and is EA of the present invention, figure 3 shows an alternative for camera thermal dehydration of the alcohol to cook offline eterovich (ethylene) samples for existing instrumental techniques CF-TC/EA-IRMS or GC/TC-IRMS. Figure 3 shows all important part of alternative camera thermal dehydration of the alcohol to cook offline eterovich (ethylene) samples for existing instrumental techniques CF-TC/EA-IRMS or GC/TC-IRMS. An alternative option for camera thermal dehydration of alcohol contains: a reaction chamber (1), which contains the top hole with cap and septa (2), which is used for the introduction of the ethanol sample (6) syringe and the left side hole (3) from valve (4), the purpose of which is to purify the inert gas helium. One part of the reaction vessel is a thermojacket (5), which contains two electric heater. Also alternatively, thermojacket (5) you can apply an open flame to heat the reaction vessel. The second part of the reaction vessel, this part has a tubular shape, turned to the right, figure 1, contains a dehydration catalyst (7), and for this purpose it is possible to use aluminum oxide (Al2O3), silica gel, zeolite, or a mixture of these substances or similar materials. From the right end of a reaction chamber connected to the tube with a gas-tight tube (8). Inside this tube with a gas-tight tube (8), a small amount of silica gel or similar inert gigroskopichnomu material can what about the place (9). The right end of the tube with a gas-tight tube (8) contains two valves (10) and (11), which are used for cleaning camera thermal dehydration of alcohol helium gas. From the right end of the tube with a gas-tight tube (8) connected with a metal needle (12) and through a tube (13) with the receptacle (14). Luggage thermal dehydration of alcohol is on the cradle (15).

In accordance with the idea of the present invention the procedure for making offline eterovich (ethylene) samples by means of the camera of thermal dehydration of alcohol is as follows.

The first phase is associated with the purification chamber thermal dehydration of the alcohol with an inert gas helium through a side opening (3) by opening valve for helium gas (4). Before the release of the helium flow is necessary to open the valves (10) and (11). After cleaning the chamber dehydration valves (10) and (11) must be closed and then the valve of helium gas (4) is also closed. Once this is done, pre-vakuumirovaniya vessel (14) put on a metal needle (13) and then the valve (11) opens. After cleaning chamber thermal dehydration of alcohol has completed, heating of the reaction vessel (1) through termokozhuhi (5) can be started until the temperature reaches a range from 250°C to 500°C. Alternative for heating the reaction vessel can emanate an open flame. Once this is done, previously distilled and selected alcohol (ethanol) sample of the analyzed wine, beer or alcoholic beverages or the like is injected, and after a reaction time than 5 minutes, the valve (11) is closed and the vessel (14) disconnect from the camera dehydration. The prepared gas Aten (ethylene), caught in the vessel (14), used for manual injection through a gas-tight syringe injection in the instrumental system CF-TC/EA-IRMS or GC/TC-IRMS.

In accordance with the idea of the present invention, apparatus for thermal dehydration of alcohol and procedures for determining the relative isotopic composition of all non-hydrogen atoms and deuterium in ethanol samples, and for the purpose of determining the authenticity and geographical origin of the wine and grape must, beer, alcoholic beverages, fruit juices, honey and all other food products that contain alcohol and/or formatiruem sugar, the method has the advantages of:

- first, it gives very good accuracy and reproducibility values for ∆ d analyzed ethanol samples, regardless of whether the ethanol sample is diluted with water before distillation, and gives a noticeable permanent difference and relationship between ethanol samples with the Botanical origin of C3 plant group;

the time the analysis is rather shorter in comparison with the SNIF-NMR;

- does not require a large financial capital and special conditions to maintain, as in the case of instrumental techniques SNIF-NMR,

- not required protective area,

- provides the ability to detect the presence of ethanol, which comes from sugar beet, wheat, barley and other industrial plants that belong to the C3 group of plants, the ethanol samples, which are extracted from the analyzed wines and alcoholic beverages or fermented juices and fermented honey.

It should be noted that modifications of the embodiments described above are of course possible. Therefore, the present innovation is not limited to variants of implementation described above.

Industrial applicability

Luggage thermal dehydration of the alcohol, the apparatus and procedure for determining in real-time isotopic composition of non-hydrogen atoms and deuterium in ethanol samples and procedure for making offline eterovich (ethylene) samples by means of the camera of thermal dehydration of alcohol fit in instrumental analytical chemistry and applied for determining the authenticity and geographical origin of wines and grape must, alcoholic drinks, beer, fruit juices, honey and other foods that contain ethanol and/or farm the sugar together.

1. The method of measuring the relative ratios of isotopes in the alcohol-containing composition material containing phases, which are:
clean the capacity for thermal dehydration of the alcohol by means of inert gas helium;
heat capacity for dehydration;
previously administered distilled and selected alcoholic sample;
evaporate the sample to a state of superheated alcohol vapor, which passes through a dehydration catalyst, thus prepared Allenby gas enters the pyrolysis reactor, and then through the column for gas chromatography and interface with the open flow divider is detected isotope ratio mass spectrometer (IRMS, and then measure the relative ratio of hydrogen and deuterium in alkenovich molecules.

2. The method according to claim 1, additionally containing phase, which compare the measured relative ratio of hydrogen and deuterium with a relative ratio of hydrogen and deuterium in alkenovich molecules derived from the alcohol-containing composition of the material of known origin.

3. The method according to claim 1, where the alcohol-containing composition of a material selected from the following group consisting of: wine, alcoholic beverages, fermented fruit juices, diluted and fermented honey, food products containing ethanol, foods containing Fe is entirelyi sugar and any combination thereof.

4. The method according to claim 1, which additionally emit hydrogen gas separation hydrogen atoms from alkenovich molecules.

5. The method according to claim 4, in which the separation of hydrogen atoms from alkenovich molecules includes pyrolysis alkenovich molecules in the gas mixture and separating the hydrogen gas from the gas mixture.

6. Apparatus for determining the origin of the alcohol-containing composition material containing:
capacity for dehydration of alcohol containing a dehydration catalyst to obtain alcohol sample of alcohol-containing food product and conversion of the alcohol sample in Allenby gas;
a heater for heating capacity for alcohol dehydration;
pyrolysis reactor for lowering alkinoos gas to a gaseous mixture containing gases of hydrogen and carbon monoxide;
column for gas chromatography for the separation of gaseous hydrogen from the gaseous mixture;
interface with open flow divider; and isotope ratio mass spectrometer (IRMS to measure the isotopic composition, i.e. the relative isotopic ratios of hydrogen and deuterium in Allenova gas, and calculate the value D for the measured isotopic composition and comparing the calculated values D value D related to alcohol-containing composition of the material of known origin.

7. The apparatus according to claim 6, where sleep is esterase composition of a material selected from the following group, contains: wine, spirits, fermented fruit juices, diluted and fermented honey, food products containing ethanol, foods containing formatiruem sugar and any combination thereof.

8. The apparatus according to claim 6, further containing a hygroscopic material for the removal of water molecules formed by conversion of the alcohol sample Allenby gas in the tank for the dehydration of alcohol.

9. The apparatus according to claim 6 where the catalyst dehydration receives a portion of thermal energy generated by the heater.



 

Same patents:

FIELD: food industry.

SUBSTANCE: method includes detection of diacetyl concentration by comparison of optical densities of beer solution with addition of standardised solution of diacetyl and solution of beer, besides, concentration of diacetyl is determined by comparison of optical density growth in beer with diacetyl added to growth of beer solution optical density. Besides, growth of optical density of solutions is measured relative to arbitrary solution of comparison from the moment of reagents addition until maximum value of optical density is achieved.

EFFECT: simplified and improved accuracy of analysis.

1 dwg

FIELD: food industry.

SUBSTANCE: proposed is a device containing the first and the second sensor elements accordingly represented by a hollow metal waveguide and a coaxial line section. Inside each of the said sensor elements, on a section along its length, a measurement cell is installed having coordinating dielectric windows on both sides and filled with controllable fluid. The input and output of each sensor element are accordingly connected to the output of the corresponding microwave generator of fixed frequency electromagnetic oscillations (via excitation and oscillation takeoff elements) and one of the inputs of the corresponding power transmission coefficient recording unit the second input whereof is connected to the output of the corresponding microwave generator. The outputs of the power transmission coefficient recording units are accordingly connected to the first and the second inputs of the calculation unit he output whereof is connected to the indicator. The hollow metal waveguide and the coaxial line section are positioned coaxially, the outside surface of the hollow metal waveguide serving as the coaxial line section internal conductor.

EFFECT: increased accuracy of alcohol content determination.

2 cl, 2 dwg

FIELD: food industry.

SUBSTANCE: device contains a support element and a stabilised oxidation element for contact with the wine fabricated of an alloy containing copper (60 - 99.9%), silver (0.05 - 20%) and gold (0.05-20%). The oxidation element contact surface and oxidation-reduction capacity enable a second of this element maintenance in wine to correspond to a year of aging. The oxidation element may be made of an alloy containing copper (95%), silver (2%) and gold (3%). Copper may be forged while the device shape may be adapted to a bottleneck or to a hole arranged in the wine barrel.

EFFECT: device enables wine testing at a specific ageing stage and possibility to accelerate the process of determining wine ageing capabilities.

4 cl, 3 dwg

FIELD: chemistry.

SUBSTANCE: 25 cm3 of wine or wine material is put into a 50 cm3 flask and the distillate is distilled. 1.5-2.0 cm3 of the distillate is collected. 0.1 N HCl is added to the remaining wet extract until attaining pH equal to 5 and then dried. A portion of this residue in amount of 5-10 mg is used for isotope analysis. The remaining portion is dissolved in 5 cm3 distilled water and 1 cm3 of 1M NaOH and 5 cm3 of 0.5M BaCl2 is added. The insoluble salts formed are precipitated by centrifuging and the supernatant liquid is separately collected. The precipitate which contains acid salts is washed with distilled water to pH of approximately 7 and dried. The supernatant liquid is titrated with 0.1M HCl to pH equal to 7 and dried. Samples of insoluble salts of organic acids and organic substances from the supernatant liquid are used to determine isotope characteristics. 0.1 mg of dry precipitate, 0.1 mg of barium salts of organic acids and 0.1 mg of organic substances which have not reacted with barium are separately put into ampoules made from refractory pyrex glass and sealed at one end, into which 0.5 g of oxidised copper oxide is put. The ampoules are evacuated to pressure 2·10-2 mmHg and sealed, put into a metallic container and held in a muffle furnace. After cooling down, the ampoules are broken open in a vacuum installation and the carbon dioxide obtained after combustion is quantitatively collected in hermetic containers for subsequent isotope analysis. The containers are opened in the discharge system of a mass-spectrometer and the analysed carbon dioxide is added in batched manner. During isotope mass-spectrometric analysis, currents arising from the number of ions with m/z 44(12C16O2+), m/z 45(13C16O2+) and m/z 46(12C16O18O) are alternately recorded in mass-spectra of the carbon dioxide sample and the laboratory standard. Characteristics of the isotope composition of carbon dioxide relative the international carbon standard V-PDB is determined in relative units δ13C (‰) using formula (1), included in the software for mass-spectrometer Delta V plus Thermo Finnigan, of the following type: δ13C=(Robr/Rst-1)1000(‰), where Robr=([13C16O2]/[l2O16O2])obr Rst=([l3C16O2]/[12016O2])st, Robr and Rst are ratios of abundance of stable isotopes 13C and 12C in the analysed carbon dioxide, obtained when burning the residue, and the international carbon standard V-PDB, respectively. The obtained ratios of abundance of stable isotopes 13C and 12C of control mixtures consisting of water and sugar of different origins are compared with results of the analysed grape wine or wine material and the origin of sugar therein is determined from the degree of coincidence or deviation.

EFFECT: proposed method increases accuracy and reliability by 90%.

2 tbl, 4 ex

FIELD: chemistry.

SUBSTANCE: 25 cm3 of wine or wine material is put into a 50 cm3 flask and the distillate is distilled off. 1.5-2.0 cm3 of the distillate is collected. A first portion is thrown away in amount of 0.2 cm3. The wet residue remaining after distilling off the distillate is dried until complete removal of water. An aliquot of the obtained dry residue in amount of 5-10 mg and an aliquot of the distilled off distillate (about 5 mcl) are separately put into ampoules made from refractory pyrex glass and sealed at one end, into which 0.5 g of oxidised copper oxide is put. The copper oxide is pre-annealed in a muffle furnace. The distillate in the ampoule is frozen at liquid nitrogen temperature (-196°C). The ampoules are evacuated to pressure 2·10-2 mm Hg and sealed. The ampoules are then put into metal containers and held in the muffle furnace at temperature 560°C for 24 hours. After cooling down, the ampoules are broken open in a vacuum installation and the carbon dioxide obtained after ethanol oxidation is quantitatively collected in a hermetic container for subsequent isotope analysis. Containers with carbon dioxide gas are opened in the discharge system of a mass-spectrometer and the analysed carbon dioxide is added in a batched manner. During isotope mass-spectrometric analysis, currents arising from the number of ions with m/z 44(12C16O2+), m/z 45(13C16O2+) and m/z 46(12C16O18O) are alternately recorded in mass-spectra of the carbon dioxide sample and the laboratory standard. The working gas used is gaseous carbon dioxide. Characteristics of the isotope composition of the carbon of the carbon dioxide, obtained during combustion of the distillate and dried residue relative the international carbon standard V-PDB is determined in relative units δ13C (‰) using formula (1), included in the software for mass-spectrometer Delta V plus Thermo Finnigan, of the following type: δ13C=(Robr/Rst-1)1000(‰), where Robr=([13C16O2]/[l2O16O2])obr Rst=([l3C16O2]st, Robr and Rst are ratios of abundance of stable isotopes 13C and 12C in the analysed carbon dioxide, obtained from combustion of the distillate or dry residue, and the standard. Isotope characteristics of carbon (δ13C,‰) of all control samples of ethanol of different origins must be predefined. The obtained ratios of abundance of stable isotopes 13C and 12C of control mixtures consisting of water and ethyl alcohol of different origins are compared with results of the analysed grape wine and the origin of ethanol and naturalness of the wine or wine material is determined from the degree of coincidence or deviation. The difference in values of quantitative carbon isotope characteristics of ethanol and dry residue of over 0.5‰, as well as that between the control and analysed sample of over 1‰, indicates that the ethanol does not originate from grape.

EFFECT: disclosed method increases accuracy and reliability by 90%.

2 tbl, 6 ex

FIELD: food industry.

SUBSTANCE: sample is distilled at the temperature of 50, 78 and 90°C. Aliquots of distilled fractions of distillate are placed into ampoules, where oxidised copper oxide is previously placed, frozen, ampoules are vacuumised and sealed. Aliquot of each fraction is burnt to produce carbon dioxide, which is quantitatively collected and exposed to isotopic mass spectrometric analysis. In process of analysis, currents provided by quantity of ions with m/z 44(12C16O2+), m/z 45(13C16O2+) and m/z 46(12C16O18O) are alternately registered in mass spectra of carbon dioxide sample and laboratory standard. Characteristics of isotopic composition of carbon dioxide produced when each fraction of distillate is burnt, relative to international carbon standard V-PDB, are defined in relative units δ16C (‰), using formula, included into software for mass-spectrometer Delta V plus Thermo Finnigan, of the following type: δ13C=(Rs/Rst-1)·1000(‰), where Rs=([13C16O2]/[12C16O2])s, Rst=([13C16O2]/[12C16O2])st, Rs and Rst - ratios of abundances of stable isotopes 13C and 12C in analysed carbon dioxide, produced when fraction of distillate and standard are burnt. Isotopic characteristics of carbon composition are defined in reference samples produced using available samples of ethanol. Produced ratios of abundances of stable isotopes 13C and 12C are compared to each other and to characteristics of reference sample, and extent of match or deviation is used to justify origin of ethanol. Difference in values of quantitative isotopic characteristics of carbon in all fractions of distillate that exceeds 0.5‰ is used to detect availability of ethanol of non-grape origin in sample.

EFFECT: increased accuracy and validity of method.

2 tbl, 6 ex

FIELD: chemistry.

SUBSTANCE: coulometric titration of 0.5-1.5 cm3 of wine in 50 cm3 of sodium chloride is carried out with generated OHˉ ions. A titration curve is plotted from the titration results and pH at the initial titration point is determined and the number of equivalents of H+ ions is calculated. pH discontinuity (equivalence point) is determined and the number of equivalents of H+ ions is calculated. The numerical value of the ratio of calculated number of equivalents found and if the numerical value lies in the 0.5±0.1 range, the wine is natural. The number of equivalents of H+ ions at the initial titration point and at the equivalence point is calculated using the following formulae: C=10-pH·Vsol/Vv and C'= I·τ·1000/F·Vv, where Vsol is volume of the analysed solution in cm3; Vv is the volume of the wine sample in cm3; I is current in A; τ is time passed from the beginning of electrolysis to the equivalence point in s; F is the Faraday constant.

EFFECT: invention provides reliability of the method owing to the reduced effect of impurities and atmospheric carbon dioxide on the process of determining the number of equivalents of H+ ions in wine, and simplification of the process of authenticating wine owing to non-use of complex mathematical calculations.

5 dwg, 2 tbl, 3 ex

FIELD: measurement equipment.

SUBSTANCE: there prepared is biological test system by mixing 0.1% water solution of mixture of the following amino acids: valine, lysine, asparagine, glutaminic acid, tyrosine, tryptophane and serine, which are taken in equal proportions, 0.5% water solution of dopamine neuromediator, 1 mM of water concentration of nucleotide DNA bases - guanine, cytosine, thymine, adenine, which are taken in equal proportions, and 25% water solution of magnesium sulphate. Components of the test system are used at the following ratio, wt %: mixture of amino acids - 38-42, dopamine neuromediator - 8-12, nucleotide DNA bases - 8-12, magnesium sulphate - 38-42. On microscope glass there put is 0.02-0.03 ml of biological test system in the form of a track which is enveloped along the periphery with a strap of the tested product, exposed, dried and the obtained specimen is tested in polarisation light with quartz compensator, and as per oriented sub-parallel aggregates and structural elements available in biological test system there estimated is naturality of the tested specimen.

EFFECT: invention increases fidelity of information and reduces the time required for analysis.

8 dwg, 4 ex

FIELD: physics, measurement.

SUBSTANCE: invention is related to alcoholic beverage industry. Product samples are selected, there physical and chemical parameters Pij are defined, where k-number of analysed parameters; n - number of analysed samples. Organoleptic assessment of samples is carried out, parameters of "ideal" sample Pij are selected according to obtained data, physical and chemical parameters are ranged, and organoleptic assessment is carried out according to extent of significance, and significance coefficients Kpij are assigned to selected parameters, provided that their sum is equal to 1. Value of every sample parameter ratio to parameters of "ideal" sample is determined according to formula Nij=pij/Pij, (when Pij≥pij); or Nij= Pij /pij, (when Pij≤pij), product of Nij and Kpij is found, products of selected Kpij are summed for every parameter and found Nij, and generalised criterion of drinks quality assessment is calculated according to the following formula, comparing to value of generalised criterion for ideal sample equal to 1: for n samples, it makes it possible to more accurately define compliance of studied samples with required organoleptic and physical and chemical parameters.

EFFECT: higher validity of drinks quality analysis.

2 dwg, 2 tbl, 2 ex

FIELD: food products; chemistry.

SUBSTANCE: in the wine sample under study by the method of current ultramicroscopy the initial concentration of colloidal particles is measured, and in 10-12 minutes after electrolyte introduction their final concentration is measured, at which coagulation process activation starts. After that they determine the rate of the relative decrease of the initial particle concentration after electrolyte introduction according to the specified experimentally received formula the respective wine resistance is calculated in months. As an electrolyte salt solutions of different concentrations are used. The final concentration in the wine sample is chosen in accordance with the metal ion valence in its salt, and namely: 0.02-0.03 M; or 0.002-0.003 M; or 0.0002-0.0003 M.

EFFECT: increase of accuracy of the resistance value of wine to colloidal haze with simultaneous simplification of the measurement techniques and reduction of investigation terms.

3 ex, 1 tbl

FIELD: chemistry.

SUBSTANCE: invention can be used for simultaneous determination of content of ions of transition metals Fe(III), Fe(II), Cu, Pb, Zn, Ni, Co, Cd, Mn in natural, surface, waste, underground water and water extracts of saline soil. High-performance liquid chromatography is used for simultaneous determination of content of ions with separation of the ions in a chromatographic column in eluent flow. The eluent consists of a solution of sodium octane sulphonate, sodium hydrotartrate and acetonitrile in dionised water. Mixing is then carried out in a post-column reaction module with a reagent which is a solution of PAR ([4-(2-pyridylazo) resorcinol], glacial acetic acid and aqueous ammonia in deionised water. Further, the difference in optical absorption of the eluent and complexes of the determined ions with the added reagent is detected using spectrophotometric detector in the visible spectrum at 520 nm.

EFFECT: increased accuracy, faster simultaneous determination of content of transition metal ions in natural, surface, waste, underground water and water extracts of saline soil.

2 tbl

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):

with a boiling point 400°C, not above. The reaction time for carrying out abovementioned chemical reaction is sufficient to provide the required yield of ester perfluorinated derivative and wherein this yield of ester perfluorinated compound is determined by the gas chromatography method by using a nonpolar column. Also, invention relates to a method for pyrolysis of ester perfluorinated derivative with a boiling point 400°C, not above, to yield the dissociation product wherein this product represents a derivative of acyl fluoride or ketone and wherein pyrolysis time is sufficient to provide the required degree of conversion of ester perfluorinated derivative and wherein the indicated conversion degree of ester perfluorinated derivative is determined by gas chromatography method by using a nonpolar column. Also, invention relates to a method for analysis of ester perfluorinated derivative with a boiling point 400°C, not above, that involves analysis of ester perfluorinated derivative in a sample containing ester perfluorinated derivative by gas chromatography method by using a nonpolar column wherein ester perfluorinated derivative represents compound comprising a fragment of above given formula (1).

EFFECT: improved method of synthesis.

8 cl, 1 dwg, 2 ex

Gas analyzer // 2141656
The invention relates to devices for analytical instrumentation and can be used as a chromatographic device in the refining, petrochemical and other fields to measure the microtraces

FIELD: chemistry.

SUBSTANCE: invention relates to a method of producing styrene and/or substituted styrene from material containing 1-phenylethanol and 2-phenylethanol and/or substituted 1-phenylethanol and substituted 2-phenylethanol. The method involves dehydration of material in gaseous phase at high temperature in the presence of a catalyst containing aluminium oxide particles, having multimodal pore size distribution.

EFFECT: use of the present method enables to obtain styrene with sufficient activity for a long period of time.

25 cl, 2 tbl, 5 dwg

FIELD: chemistry.

SUBSTANCE: one of the versions involves reaction of ketone and hydrogen at reaction temperature ranging from 150°C to 250°C in the presence of a Cu-containing hydrogenation catalyst and a metal oxide type solid acid, where the Cu-containing hydrogenation catalyst additionally contains at least one element from group IIIA, group IIB and group VIB of the periodic table of elements, and where the metal oxide type solid acid is β-zeolite.

EFFECT: use of the present invention enables to obtain olefins with high selectivity.

5 cl, 8 ex, 4 tbl

FIELD: chemistry.

SUBSTANCE: invention relates to a method of producing ethylene through vapour-phase chemical decomposition of material containing ethanol, water and ethoxyethane in a reactor at high temperature and pressure in the presence of a catalyst layer containing supported heteropolytungstic acid. The method is characterised by that the reactor is adjusted and operates in conditions corresponding to the following parameters: 0.05<(Pwater/(Pethanol+Pethoxyethane))/(8×10-5HBSG+0.75) (1) and - 20<Treaction-Tdew point, - 40×Ptotal.material+40×Pinert.<+80 (2). Pwater, Pethanol and Pethoxyethane denote partial pressure of water, ethanol and ethoxyethane, respectively, with thermodynamic equilibrium composition of the material at operating temperature and pressure of the process in MPa. HBSG is hourly bulk speed of the gaseous material passing over the catalyst in h-1. Treaction is reaction temperature in °C, Tdew point is dew point of the material at its thermodynamic equilibrium composition in °C. Ptotal.material is total pressure of material in MPa, and Pinert. is partial pressure of inert substances in the composition of the material in MPa.

EFFECT: use of the present method enables to maintain moisture of the catalyst at an optimum level.

13 cl, 137 ex, 1 dwg

FIELD: chemistry.

SUBSTANCE: invention relates to a method of processing methyldihydropyran and/or by-products of synthesis of isoprene from isobutylene and formaldehyde via thermocatalytic decomposition thereof over an aluminosilicate-containing catalyst with preheating (or without) of the starting material in the presence of water vapour followed by condensation of the obtained contact gas to form aqueous and oil layers. Reaction products - isoprene, isobutylene and formaldehyde - are then extracted from said layers. The method is characterised by that an isoprene fraction containing 3-25 wt % isobutylene dimers is added to the contact gas at temperature 35-90°C, with weight ratio of the isoprene fraction to the contact gas equal to (0.02-0.15):1.

EFFECT: use of the present method enables to considerably improve the quality of waste water from the process and reduce loss of the end products without reducing selectivity of the process and without increasing deposition of coke on the catalyst.

1 cl, 4 ex, 1 tbl

FIELD: chemistry.

SUBSTANCE: invention relates to use of heteropoly acid catalysts for converting oxygenates to alkenes. Described is a method of producing an alkene (alkenes) from an oxygenate starting material through dehydration in a reactor in the presence of a heteropoly acid catalyst deposited on a support, characterised by that the specific pore volume thereof satisfies the following relationship: OP>0.6-0.3 [amount of heteropoly acid catalyst/surface area of dried catalyst], where OP denotes the specific pore volume of the dried heteropoly acid catalyst deposited on the support (given in ml/g catalyst); the amount of the heteropoly acid catalyst is the amount of heteropoly acid contained in the dried heteropoly acid catalyst deposited on the support (given in micromole/g); the surface area of the dried catalyst is the specific surface area of the dried heteropoly acid catalyst deposited on the support (given in m2/g). Described is a method of converting a hydrocarbon to an alkene (alkenes), involving the following successive steps: a) converting hydrocarbon starting material in a synthetic gas reactor into a mixture of carbon oxide (oxides) and hydrogen, b) converting said mixture of carbon oxide (oxides) and hydrogen from step a) in the presence of a powdered catalyst in a reactor at temperature ranging from 200 to 400°C and at pressure ranging from 50 to 200 bars into starting material containing at least one monoatomic aliphatic paraffin alcohol and/or the corresponding ether containing 2-5 carbon atoms, and c) continuing to realise the method as described above to obtain alkenes, owing to which the oxygenate starting material contains at least a portion of alcohol (alcohols) and/or ethers obtained at step b). Described is use of the heteropoly acid catalyst deposited on a support in the method of producing alkene (alkenes) from oxygenate starting material for increasing alkene selectivity and output while simultaneously preventing formation of alkanes, in the presence of the catalyst described above.

EFFECT: high efficiency of producing alkenes and low amount of alkanes formed.

20 cl, 7 tbl, 1 dwg, 19 ex

FIELD: chemistry.

SUBSTANCE: invention refers to the way of production of phenol, acetone and α-methylsterene, and to the installation for its implementation. The way consists in decompounding of cumene hydroperoxide and dimethylphenyl carbinol that are included into the technical cumene hydroperoxide, in the solvent with the presence of heterogeneous catalyst by means of catalytical distillation in the continuous isothermal mode at the boiling point of the solvent and with the latter's recirculation; as a solid heterogeneous catalyst, heteropoly acid H3PW12O40 or caesium-displaced salt of heteropoly acid Cs2.5H0.5PW12O40 is applied on the silicon dioxide, and as a solvent, acetone is employed. As a bearer, mesoporous silicon dioxide of MCM-41 grade is used, and decompounding of the cumene hydroperoxide and dimethylphenyl carbinol is carried out in two stages; the first stage stipulates decompounding of cumene hydroperoxide thus releasing phenol and acetone, and the second one - of dimethylphenyl carbinol thus releasing a-methylsterene; the mesoporous silicon dioxide and heteropoly acid or caesium-displaced salt of the heteropoly acid are used with the following component ratio, weight %: heteropoly acid - 10-50; silicon dioxide - the rest; or caesium-displaced salt of the heteropoly acid - 10-20; silicon dioxide - the rest.

EFFECT: decompounding of the cumene hydroperoxide and dimethylphenyl carbinol with 100 % conversion and 100 % selectance.

8 cl, 1 dwg, 8 ex

FIELD: chemistry.

SUBSTANCE: invention relates to a method of producing ethylene on modified aluminium oxide catalysts during dehydration of ethanol. Described is a catalyst for producing ethylene during dehydration of ethanol, containing aluminium oxide and chlorine in amount of 1.0-4.0 wt %. Described is a method of producing the catalyst by saturating aluminium oxide with hydrochloric acid, followed by drying and calcination, thereby obtaining a catalyst containing aluminium oxide and chlorine in amount of 1.0-4.0 wt % with specific surface of 150-300 m2/g and pore size distribution of 3-30 nm. Described is a method of producing ethylene via dehydration of ethanol using the catalyst described above at 350-400°C and contact time of 0.3-1 s.

EFFECT: high activity and selectivity of producing ethylene from ethanol.

11 cl, 10 ex, 3 tbl

FIELD: chemistry.

SUBSTANCE: invention relates to a method of producing alkene(s) from starting material consisting of monoatomic aliphatic paraffin primary (and/or secondary) alcohol(s), containing ethanol, propanol(s) or mixture thereof, characterised by the following steps: 1) monoatomic aliphatic paraffin primary (or secondary) alcohol(s) in a reaction-fractionation column at high pressure and high temperature in the presence of a catalyst is converted to alkene(s) with the corresponding number of carbon atoms so that stream of overhead distillates tapped from the top part of the said reaction-fractionation column essentially includes said alkene(s), 2) the stream of overhead distillates from step 1 is then cooled to temperature which is sufficient for condensation of at least a portion of alkene(s) with the highest boiling point, 3) further at least a portion of the condensed alkene(s) from step 2 is returned to the said reaction-fractionation column as reflux, 4) the remaining alkene(s) are simultaneously extracted. The invention also relates to a method of converting hydrocarbon to alkene, involving the method given above.

EFFECT: improved method of producing C2+ alkene from alcohols.

11 cl, 1 dwg

Up!