RU2210069C1 - Sampler for drawing samples of liquid and gas at increased temperatures and pressures - Google Patents

Abstract

FIELD: study of physico-chemical properties of multi-component solutions containing one or several gaseous components in liquid-gas equilibrium state or in vertically stratified state. SUBSTANCE: proposed device includes autoclave, valve with stem coaxially running through obturator and sampler. Stem is revolving. Sampler is made in form of inserts calibrated in volume and turned over with bottom upwards. Said inserts are provided with screw covers and perforated neck and are mounted in perforated holder which is coaxially secured on obturator by means of bayonet lock. Several inserts with partially screwed covers are engageable with each other, with revolving stem of valve and with bottom of perforated holder by means of splined joints, thus making it possible to screw down all covers simultaneously during rotation of valve stem; covers are sealed up by means of knife seal over gasket ring made from inert metal. Proposed device makes it possible to draw sample duplicates without disturbance of thermodynamic and chemical equilibrium and to determined pH and chemical composition. EFFECT: enhanced efficiency. 7 dwg

Description

 The invention relates to techniques for physico-chemical studies of the properties of substances and can be used for simultaneous sampling of liquid and gas with dissolved non-volatile and gaseous components in equilibrium at elevated temperatures and pressures, to study their density, pH, chemical composition, and also for sampling from stratified gas and liquid solutions at elevated temperatures and pressures to study their chemical and physical properties.

 A known sampler for sampling liquid samples in the study of solubility of solids in hydrothermal solutions (Geletiy VF Equilibrium sulfides of lead, cadmium, manganese, zinc in hydrothermal conditions. The dissertation for the degree of candidate of geological and mineralogical sciences. Irkutsk, 1982).

 Sampling is carried out in a cylindrical sampler, hermetically and coaxially fixed to the obturator and occupying the upper third of the autoclave. The bottom of the sampler has a through hole with a ground saddle, through which during the experiment the capacity of the sampler communicates with the capacity of the autoclave. In the experiment, after equilibrium in the solution is established, the hole is closed by a valve stem coaxially passing through the obturator and the sampler itself, after which the experiment is terminated. The sampler thus closed with the sample is removed from the autoclave after it has cooled. The sample extracted from the sampler is sent for analysis.

 The disadvantage of this device in the study of liquid-gas systems, firstly, is the inability to take a sample of the liquid located in the lower part of the autoclave, because when it cools, it is mixed with condensate from the steam remaining outside the sampler. Secondly, the design of the sampler does not allow duplicate samples to be taken in one experiment. Thirdly, the sampler does not allow to obtain data on the density of the vapor-gas phase, and the lack of tap to the manometer does not allow to measure the pressure in the autoclave.

 There is also known a device for sampling liquid and steam (Patent 2004904 for the invention of a "Device for sampling liquid and steam", Zhatnuev N. S.), in which sampling is carried out in a row of coaxially mounted and turned upside down glasses, some of which are in liquid zone, and the other in the vapor zone and locked by squeezing the curved gaskets.

 The disadvantage of this device is that it is designed for systems that do not contain gas components, since locking the glasses by squeezing the gaskets with the rod does not allow the gas to be kept under pressure in the glasses and bursting immediately after removing the load from the valve stem.

 The technical result of the invention is the simultaneous selection of duplicate samples of a known volume of liquid and gas (vapor) in equilibrium, as well as layered solutions in multicomponent systems at elevated temperatures and pressures, in contrast to the prototype, which allows to study systems containing gaseous components.

 The technical result of the invention is achieved by the fact that in a device consisting of an autoclave, a valve with a stem coaxially passing through the obturator, and a sampler, according to the invention, the rod is rotated and the sampler is made in the form of inserts turned upside down with volume perforated, equipped with perforated screw caps a neck, sequentially installed in a perforated holder, which is coaxially fixed with a bayonet lock on the shutter, and a number of inserts with half-screwed caps mate between each other by the rotating valve stem and the bottom of the perforated holder by means of splined joints, which allows for rotation of the valve stem to simultaneously wrap all covers sealed with a knife seal on an inert metal gasket ring and seal all inserts.

 In FIG. 1 shows a general diagram of an apparatus for sampling liquid and gas; figure 2 - the position of the vacuum three-way valve 7a and 7b in the process of evacuation of the autoclave and valve 7a when discharging excess gas from the system after it is filled; figure 3 - the position of the vacuum three-way valve 7A in the process of filling the autoclave with the test solution and valve 7b when discharging excess gas into the atmosphere after filling the system; figure 4 - the position of the vacuum three-way valve 7b during the inlet of the atmosphere into the forballon and the inlet of the solution into the system; figure 3 - autoclave with a valve and a sampling system, fixed on the shutter; figure 6 - perforated holder with inserts having screw caps, and a circuit for connecting the rod with the head and inserts; Fig.7 - sampler insert with a lid.

 The device contains a pressure vessel (autoclave) 1 (Fig. 1) with standard locking parts 1.11-1.14 (Fig. 5), placed in a gradientless furnace, which is connected to the medium separator 2 by means of the high-pressure capillary pipe 1.10 (Fig. 3) and manometer 3 (figure 1). Then, using a pipeline, the autoclave-manometer system is connected to the autoclave evacuation and filling system. These systems are cut off from each other by a high pressure valve 4a (Fig. 1). The autoclave evacuation and filling system consists of 4b-4g high-pressure valves; gas cylinders with gears 5, 6; burettes with test solution 9; vacuum three-way cranes 7a and 7b, as well as a pre-ballon 10; a vacuum gauge 11 and a vacuum pump 12 (figure 1). The pressure vessel is a standard laboratory autoclave 1 (Fig. 1), consisting of a housing 1.15 and a shutter 1.11-1.14, on which a valve developed by the author is installed, consisting of a stem 1.1, a support nut 1.2, a support bearing 1.3, a water-cooled nut 1.4 with a valve for its retention during rotation of the valve 1.5-1.6, a water jacket cooling 1.9, as well as an elongated obturator 1.16 (figure 5). A sampling device is installed on the obturator using a bayonet lock, consisting of a perforated holder 1.17, a head for transmitting rotation from the stem to the insert 1.18 and a number of sampling inserts, the number of which can be different (from 3 or more) depending on the size of the autoclave, sizes the insert itself and the problem to be solved. The insert consists of a housing having slotted slots 1.19, a screw cap with a perforated neck and a slotted protrusion 1.20 and a disposable inert metal ring 1.21 (Fig. 5). All parts are made of heat-resistant stainless steel and can be lined with the same inert metal from which O-rings 1.21 are made.

 The device operates as follows.

 First, the autoclave closed with an obturator is filled with the test solution to the required volume. The amount of solution is selected experimentally in such a way that, under the experimental parameters, the interface between the liquid and gas is at the level of the middle liner. In this case, gas will be in the upper glasses during sampling, liquid in the lower glasses, and, on average, a mixture of these two phases. Before filling the autoclave, air is evacuated from it with a vacuum pump 12 with open valves 4a, 4g, closed valves 4b, 4c and the position of the vacuum valves 7a and 7b shown in Fig.2.

 After evacuating the air, the valve 7a switches to the position shown in FIG. 3, the crane 7b is in the position shown in figure 4. At the same time, a solution is sucked into the autoclave from the burette 9, the amount of which is controlled by the divisions on the burette. After filling the autoclave with a solution, the 4g valve is shut off, cutting off the burette and the vacuum system from the autoclave-manometer system. To fill the test system with a mixture of gases, they open and, to prevent gas flows between the cylinders, valves 4b and 4c are closed alternately. The amount of gas is calculated according to the pressure gauge 3. After filling the system with gases, valve 4a closes. To discharge gases from the filling system, the valve 7a is placed in the position shown in figure 2, and the valve 7b is shown in figure 3, then the valve 4g slowly opens. After that, the autoclave is placed in a vertical position in a gradientless furnace and displayed on the desired temperature. After putting into operation and reaching equilibrium, the semi-screwed sample inserts are closed by rotation of the rod 1.1, which transfers the movement of the 1.18 head freely sliding on the rod, which has a spline protrusion and which, in turn, rotates all the inserts and their covers in turn. In this case, the lids are completely wrapped in the liners, blocking the perforation on their necks, providing free access to the solution and gases. The cover of the last lower liner with its spline protrusion, sitting in the slot of the cage, provides immobility of the last link of the chain, which is necessary for reliable sealing of the liners. After closing the liners, the experiment is terminated by turning off the furnace. In this case, the upper liners contain gas (steam), the lower - liquid. After the autoclave has cooled, pipeline 1.10 is disconnected, with the help of nuts 1.11 and 1.13, the autoclave is opened and the obturator is pulled out together with the yoke 1.17 and the overlapped liners, after which the yoke is removed from the obturator. First, the head 1.18 is removed from it, and then the liners are first pushed out first with gas (steam condensate), a mixture of condensate and liquid, and a breakdown of the liquid.

 The proposed device allows, without disturbing the thermodynamic and chemical equilibrium, to take several duplicate samples of liquid and gas at elevated temperatures and pressures in volume-calibrated inserts to determine the densities of the phases under study by weighing the selected samples, as well as to determine the pH and chemical composition.

Claims (1)

 A device for sampling liquid and gas at elevated temperatures and pressures, consisting of an autoclave, a valve with a stem coaxially passing through the obturator, and a sampler, characterized in that the rod is made rotating, and the sampler is in the form of inserts turned upside down, calibrated over the volume of inserts, equipped with screw caps with a perforated neck, sequentially installed in a perforated holder, which is coaxially fixed with a bayonet lock on the shutter, and a number of inserts with half-screwed caps mate They are interconnected by the rotating valve stem and the bottom of the perforated holder by means of splined joints, which allows rotation of the valve stem to simultaneously wrap all the covers sealed with a knife seal on an inert metal spacer ring and seal all the inserts.

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