Device for preparation of calibration gas mixtures

 

(57) Abstract:

The invention relates to the field of analytical instrumentation and can be used in the calibration and verification of gas analyzers. The device includes a housing, a vessel for gas saturation pairs of substances, mounted in the housing, a gas line for supplying gas into the vessel, a gas line for output of gas-steam mixture from the vessel, a device for diluting the gas mixture further gas flow, gas line for supplying an additional gas flow in a device for dilution. Gas line for supplying an additional gas flow in a device for dilution is made separately from the gas line for supplying gas into the vessel to saturate. When this vessel to saturate made in the form of a cylindrical Cup mounted inside the case on a mobile platform, equipped with a mechanism for reciprocating movement in the vertical direction. In the upper part of the body motionless cover will be fitted to the vessel, provided with a sealing ring, which tightly contact the edge of the vessel at the extreme upper position of the platform, and in the side wall of the housing is a window to extract the vessel from car C.p. f-crystals, 1 Il.

The invention relates to the field of analytical instrumentation and can be used in the calibration of gas analyzers.

A device for preparation of calibration gas mixtures containing vessel to saturate filled with particles of a fluorinated carbon between the layers of which is placed a starting material, a gas line for supplying gas into the vessel, a gas line for output of gas-steam mixture from the vessel, a device for heating the vessel and the pump gas flow (see C-ku CIS countries 0500938 A1, G 01 T 30/04, 1992).

A disadvantage of the known device is its limited functionality. This is because the known device allows you to change the concentration of the original substance in the gas in a very narrow limits, as the change in concentration is provided only by the temperature change of the vessel to saturate. Moreover, the range of initial substances, are suitable for the preparation of gas-steam mixture, is also very limited.

The closest to the technical nature of the present device is a device for preparation of calibration gas mixtures, comprising a housing, a vessel for saturation ustanovlen absorber preventing mechanical impurities and impurity substances, gas line for output of gas-steam mixture from the vessel, a device for dilution of the gas mixture that is installed in the gas line for output of gas-steam mixture from the vessel to saturation, gas line for supplying a flow of dilution gas in a device for dilution, in which there is a constant pneumatic resistance, tee, connecting a gas line for supplying gas into the vessel for saturation and gas line for supplying a dilution gas, and determining the degree of dilution of the gas mixture in the device for dilution, and the booster gas flow (see the generators of the gauge of concentration of vapours in the air of the firm Cavkit Ltd (England), 1997).

A disadvantage of the known device, taken as a prototype, is its limited capacity. This is due to the fact that in the known device a gas line for supplying gas into the vessel and a gas line for supplying a dilution gas in the United tee, which sets tight relationship threads in the device for diluting and determines the concentration of vapor in the gas at the outlet of the device. The transition to the new concentration at a given temperature can only be done step by replacing the tee with pneumatic resistance, the th accession to the gas lines and other All this greatly complicates the operation of the device. Limited functionality of the device caused by the fact that as starting substances for the preparation of calibration gas mixtures in the device can be used in a very limited range of substances for which a known exact values of the elasticity of steam at different operating temperatures of the device, as the calculation of the concentration of vapor in the gas at the outlet of the device is performed on the basis of these data and taking into account the division factor of the gas stream at the tee.

A disadvantage of the known device is also insufficient accuracy of the determination of the concentration of the calibration gas mixture. The reason for this is the lack of accurate dependency of the saturated vapor pressure on temperature. The speed dependence in the interval between the known values of pressure is unknown and is set using interpolation.

The objective of the invention was to expand the functionality of the device for preparation of calibration gas mixtures and increased precision cooking vapor mixtures.

This task is solved in that the device for cooking gas the gas line for supplying gas into the vessel to saturate, in which you installed the absorber preventing mechanical impurities and impurity substances, gas line for output of gas-steam mixture from the vessel, a device for dilution of the gas mixture that is installed in the gas line for output of gas-steam mixture from the vessel to saturation, gas line for supplying a flow of dilution gas in a device for diluting and booster gas flow, which according to the invention a gas line for supplying a flow of dilution gas in a device for diluting the gas mixture is made separately from the gas line for supplying gas into the vessel to saturate, moreover, in the device there is an additional absorber preventing mechanical impurities and impurity substances and the gas flow regulator installed in the gas line for supplying a flow of dilution gas in a device for dilution.

Another distinctive feature of the proposed device is that the vessel to saturate the gas pairs substances made in the form of easily removable element with the possibility of removal from the chassis.

In a preferred embodiment of the device the vessel to saturate made in the form of a cylindrical Cup mounted inside the case on padenie, and in the upper part of the body still set cover for the vessel, equipped with a ring of flexible inert material which tightly contact the edge of the vessel at the extreme upper position of the platform, and in the side wall of the housing is a window to extract the vessel from the body.

Another distinctive feature of the proposed device is that the lid of the vessel is equipped with nozzles that are connected to gas lines for gas supply and withdrawal of gas-steam mixture.

Among the differences, it should be noted that the platform, which is a vessel for saturation, equipped with a thermoelectric Converter to set the target temperature of the vessel.

Thanks to the above features of the proposed device are expanding the functionality of the device, because the device allows you to smoothly change the concentration of vapor in the gas at the outlet of the device within wide limits and can be used to prepare a gas mixture of a wide range of substances. The calculation of the concentration of vapor in the gas is carried out on the basis of periodic weighing of the vessel to be extracted from the body, which increases the accuracy of determining the concentration.

Crete and the scheme of its gas lines.

The device includes a housing 1 in which is placed a vessel 2 for saturation of gas pairs substances. The vessel 2 is made in the form of a cylindrical Cup of inert material (stainless steel), partially filled with the liquid substance 3 mounted on a movable platform 4, equipped with a mechanism 5 for reciprocating movement in the vertical direction. In the upper part of the housing 1 still set cover 6 of the vessel 2, provided with a ring 7 of flexible inert material, such as silicone rubber, which serves for hermetic sealing end surface of the vessel 2 at the extreme upper position of the platform 4. The cover 6 is also equipped with nozzles 8 and 9 for the supply and withdrawal of gas from the vessel 2. The pipe 8 is connected with a gas line 10 for supplying air, which includes an absorber 11 to prevent trapping of mechanical impurities and impurity substances from the air. The absorber 11 is a tube filled with particles of a sorbent to absorb moisture (silica gel) and impurities of organic substances (activated charcoal). Inlet tube absorber 11 is placed mesh for trapping particles such as dust and smoke. The pipe 9 is connected with a gas line 12 to wyborowa mixture, the other input of which is connected with a gas line 14 for supplying dilution air. As a device 13 for dilution can be used tee. In the gas line 14 for supplying a dilution gas has been consistently found to absorber 15 preventing mechanical impurities and impurity substances and the controller 16 of the gas flow. The absorber 15 is identical to the absorber 11. Gas line 14 for supplying a flow of dilution gas in the device 13 to dilute the gas mixture is made separately from the gas line 10 for supplying a gas into the vessel 2 to saturation so that the gas inlet 17 of the gas line 14 is not connected to the gas inlet 18 gas line 10. The output of the device 13 to dilute the gas mixture connected with calibrated the detector 19, the output of which is connected to the booster 20 gas flow. As the pump 20 of the gas flow can be used in the pump of diaphragm type, which is commonly used in the calibrated detector 19.

In the side wall of the housing 1 has a window 21 for extraction vessel 2 with a view to its periodic weighing. Platform 4 on which is mounted a receptacle 2 for saturation, equipped with a thermoelectric Converter 22, to set the mechanism 5 for moving the platform 4 is provided with a handle 23 for imparting rotational motion, which is converted into the reciprocating movement of the platform 4. On the upper horizontal surface of the platform 4 is made a circular depression in the shape of the bottom of the vessel 2, is designed to center the vessel 2 with respect to an axis of the cylindrical casing 1 and the sealing ring 7 in the cover 6.

The proposed device operates as follows. The vessel 2 is partially filled with liquid the starting material 3, for example hexane, and produce weighing on an analytical balance (not shown) to determine the initial amount of source liquid substance in the vessel 2. Then the vessel 2 through the window 21 in the housing 1 mounted on the platform 4 in a circular depression, and by the rotation mechanism 5 by means of arms 23 carry out lifting platform 4 to the extreme upper position in which the end surface of the vessel 2 is tightly in contact with the sealing ring 7, thereby making the sealing of the internal volume of the vessel 2. Then, using a controller (not shown) and a thermoelectric Converter 22 is set at the correct operating temperature in the vessel 2 and include booster 20 gas flow and calibrated the detector 19. The booster 20 flow gazabo through a gas inputs 17 and 18 of the gas lines 14 and 10 respectively from the ambient air. Gas flowing through the gas line 10, purified particles from mechanical impurities, impurities, moisture and organic substances contained in the air in the absorber 11 and through the pipe 8 enters the internal volume of the vessel 2, where it is saturated vapors of the original substance and through the pipe 9 and the gas line 12 to the output of gas-steam mixture enters the device 13 for dilution. To the second input device 13 for the dilution gas flows through line 14, the flow of dilution air is sucked in through the gas inlet 17, which is mixed with the stream of gas-steam mixture flowing through the gas line 12, and a dilute stream of gas-steam mixture enters the calibrated detector 19. The detector 19 in the process, produces an electrical signal proportional to the concentration of vapor of the substance in the gas at the output device 13 for dilution. The vapor concentration of a substance in a gas output device 13 for dilution calculated based on volumetric flow rates of gas in the gas lines 10 and 14, and data about the change quantity of the substance in the vessel 2 for a certain period of time. Measurement of gas flow in the gas lines 10 and 14 is carried out by incorporating in at (not shown). Measuring the amount of substance transferred in the form of steam from the vessel 2 into the gas stream passing through the vessel 2 and the output from the gas line 12, is carried out by periodic extraction vessel 2 from the housing 1 and weighing it on an analytical balance (not shown). The extraction vessel 2 from the housing 1 is made by lowering the platform 4 to the level at which the vessel 2 is placed in front of the window 21, and removing the vessel 2 through the window 21.

The transition to the new value of the concentration of vapor in the diluted stream of the gas mixture fed to the detector 19, is carried out by the fine adjustment of the resistance to the gas flow in the gas line 14 through the controller 16 of the gas flow. It may also be done by changing the temperature of the vessel 2 using thermoelectric Converter 22.

1. Device for preparation of gas mixtures, comprising a housing, a vessel for gas saturation pairs of substances, mounted in the housing, a gas line for supplying gas into the vessel to saturate, which includes an absorber preventing mechanical impurities and impurity substances, gas line for output of gas-steam mixture from the vessel, a device for dilution of the ha line for supplying a flow of dilution gas in a device for diluting and booster gas flow, characterized in that the gas line for supplying a flow of dilution gas in a device for diluting the gas mixture is made separately from the gas line for supplying gas into the vessel to saturate, and the device introduced an additional absorber preventing mechanical impurities and impurity substances and the gas flow regulator installed in the gas line for supplying a flow of dilution gas in a device for dilution.

2. The device under item 1, characterized in that the receptacle for the gas saturation pairs of substances made in the form of easily removable element with the possibility of removal from the chassis without disconnecting the gas lines.

3. The device according to p. 2, characterized in that the vessel to saturate made in the form of a cylindrical Cup mounted inside the case on a mobile platform, equipped with a mechanism for reciprocating movement in a vertical direction, and in the upper part of the body still set cover for the vessel, equipped with a ring of flexible inert material which tightly contact the edge of the vessel at the extreme upper position of the platform, and in the side wall of the housing is a window to extract the vessel from CDF and gas lines for gas supply and withdrawal of gas-steam mixture.

5. The device under item 3 or 4, characterized in that the platform on which is mounted a receptacle for saturation, equipped with a thermoelectric Converter to maintain a constant temperature vessel.

 

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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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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.

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11 cl, 2 dwg

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1 ex, 3 tbl

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15 cl, 19 dwg

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