Device for continuous gas extraction volatile component

 

(57) Abstract:

Use: analytical chemistry, analysis solutions. The device consists of a reaction bubbler for the reaction of formation of volatile component and connected to the absorption bubbler to absorb the volatile component. The reaction bubbler is made in the form of a cylinder having the same diameter in height. The diameter and height of the cylinder is selected from the condition of the volume of the gas space above the reaction solution is much less than the volume of the solution. Inside the cylinder is placed a device for input of gas-extractant, which is made in the form of two concentrically arranged tubes: external and internal. The outer tube has a fitting for gas-extractant in the annular gap between the tubes, the lower end of the inner tube is closed. Absorption bubbler is made U-shaped, one knee it is a tube and serves as a connecting link with the reaction bubbler, and the other knee is a few consistently rigidly connected balls. The invention allows better extraction of the volatile component. 2 C.p. f-crystals, 1 tab., 2 Il.

The invention relates to an issue is in the solutions.

There are many reactions in solution with the formation of gaseous reaction products. In emerging heterogeneous system is installed between phase equilibrium. Due to the relationship between the concentration of a component in different equilibrium phases (Henry's law), it is possible to analyze the liquid phase to gaseous composition. This is one of the tasks of methods of analysis of the equilibrium pair.

When using continuous gas extraction in the gas stream of the extractant [1] the procedure of analysis essentially boils down to the following.

Carry out the reaction of education defined volatile component. From the gas phase above the reaction solution otdovat his gas flow of the extractant in a suitable absorbing solution. Then one or another method is measured in the absorption solution of the analytical signal.

For analysis it is necessary arrangement, consisting mainly of the reaction bubbler (the reaction vessel, the reaction or distillation flask, etc.,) and the absorption bubbler (receiver, trap, etc.,) connected in such a way that the gas-extractant is included in the reaction bubbler, propulsive through the reaction mixture, is mixed with the formed in the ez absorbing solution, where defined volatile component is delayed, and free gas-extractant being released into the atmosphere.

A device for gas extraction, used for radiochemical determination of Halogens and separate them from many of the elements [2]. The device consists of four series-connected reaction of bubblers in the form of three conical flasks in which the gas-extractant propulsive in the reaction mixture through the capillaries, and two series-connected adsorption of bubblers in the form of a cylinder in which the gas-extractant propulsive in the absorption solution through tubes of small diameter.

A device for gas extraction, used for the determination of chlorine and bromine and separate them from other elements in volcanic rocks [3]. The device consists of one reaction bubbler in the form of a spherical flask in which a gas-extractant propulsive in the reaction mixture through a tube of small diameter, and two series-connected adsorption of bubblers, as in the device [2].

A device for gas extraction, used for determination of bromine and separate it from chlorine and iodine [4]. Stoboy tube of small diameter, and another few balls, rigidly connected with each other. The diameter of the ball about 3 times the diameter of the tube. The first of the bubblers are used as reaction, it make the original reagents, and forms a volatile component. Subsequent bubblers are used as adsorption, put them absorbing solutions. The volume of solution placed in a bubbler is 1/3-1/2 of the total volume of the bubbler.

The disadvantages of the known devices is the complexity of the reaction of bubblers, and a bulky design as a whole, the ineffectiveness of individual bubblers, leading to the necessity of incorporating into the device a few of the reaction and adsorption of bubblers to obtain a quantitative yield of volatile component.

The closest in technical essence and the achieved result to the present invention is a device for continuous gas extraction volatile component, comprising the reaction of a bubbler for the reaction of formation of volatile component and connected to the absorption bubbler to absorb volatile component [5]. Both bubblers are cylindrical in shape, the input gas extractant in them is che the EPA has a different diameter in height. In the upper part, where is the gas space, the diameter of 1.5-2 times higher than in the lower part, where the reaction mixture. The volume of the gas space above the reaction mixture is approximately equal to the volume of the mixture.

The disadvantages of this device are:

- broadening the reaction bubbler in the upper part leads to the creation of "dead zones" from which is difficult otbw formed volatile component;

because of the fragmentation of gas-extractant into many small bubbles in the reaction bubbler may back the dissolution of the volatile component in the reaction liquid;

- cylindrical absorption bubbler creates a short path gas-extractant through the absorbing solution.

Thus, the device is characterized by the lack of completeness of Ottawa and absorption of volatile component. The device may be used only for such ultra-sensitive methods of analysis, fluorescent.

The objective of the invention is to increase the efficiency of gas extraction, which will allow the use of continuous gas extraction in any sensitivity analysis methods.

Put Eeactions bubbler for the reaction of formation of volatile component and connected to the absorption bubbler to absorb volatile component, the reaction bubbler is made in the form of a cylinder having the same diameter in height, placed in the cylinder device to enter a gas-extracting agent, executed in the form of two concentrically arranged tubes, absorption bubbler is made U-shaped: one knee it is a tube and serves as a connecting link with the reaction bubbler, and the other knee is a few rigidly connected with each other balls.

The diameter and height of the cylinder reaction bubbler selected from the condition: the volume of the gas space above the reaction solution is much less than the volume of the solution. This results in significantly reduced amount of "dead zones".

The outer tube of the device to enter a gas-extractant is in the upper part of the socket for receipt of a gas-extractant in the annular gap between the tubes, and the lower end of the inner tube is closed. This leads to the fact that the gas-extractant does not split large bubbles propulsive through the reaction solution and makes the resulting volatile component from the liquid phase. In such bubbles the desorption of the component in the gas phase dominate the sorption processes it in the liquid phase. In the mind the gas phase, than in the prototype.

In absorbing the bubbler is U-shaped with the same volume of absorbing solution path of a gas-extractant longer than in the prototype. Different design of the knee leads to a drastic and abrupt change of diameter, which contributes to more intense fragmentation of the gas flow of the extractant into small bubbles and a more efficient absorption of the component than in the prototype.

Device for continuous gas extraction volatile component is illustrated in the drawing, where Fig.1 shows a schematic diagram of the device, and Fig. 2 - diagram of the device for input of gas-extractive solvent in the reaction bubbler.

The reaction bubbler And made in the form of a cylinder 1 having the same diameter in height. In the upper part of the cylinder perpendicular to its axis is outlet fitting 2. Inside the cylinder is placed a device In the input gas extractant, made in the form of two concentrically arranged tubes: an outer tube 3 and inner tube 4. The outer tube device has a socket 5 for receiving a gas-extractant in the annular gap 6 between the tubes. The lower end 7 of the inner tube is closed. Absorption bubbler B is made of a U-shaped fo the natives knee 9 is a somewhat rigidly connected with each other balls. The connecting element 10 can be selected of any shape and made from any inert material.

The device operates as follows.

In absorption bubbler filled accurately measured volume of the corresponding absorption solution. From the reaction bubbler remove the device to enter a gas-extractant and make the analyzed sample in the reaction vessel. Connect the reaction bubbler with absorption. Add in the reaction vessel reagents that cause the formation of volatile component, quickly closed his device to enter a gas-extractant and let the current of gas with a certain constant speed. If necessary, the reaction mixture is heated. After extraction rassadina bubblers, turn off the current of gas. Next, analyze the adsorption solution that go by another method.

The effectiveness of the described device is evaluated by ionometric determination of bromide-ion in natural waters.

In the reaction bubbler height of 200 mm and a diameter of 30 mm was placed 50 ml of a standard solution containing from 0.1 to 1000 mg/l bromide ion. Was added potassium permanganate solution and the mixture was heated to 90oC. Formed in achiev the fit of sodium absorption in the bubbler, having a tube diameter equal to 6 mm, and the diameter of the ball - 24 mm solution of sodium sulfite bromine was restored again to the bromide ion. The concentration of bromide-ion in the absorbing solution was determined using a chloride - selective electrode.

For comparison, similar definitions were made in the devices of other designs.

Tested the following construction:

1 - reaction bubbler in the form of a three-neck conical flask with gas inlet of the extractant into the reaction solution through the capillary absorption bubbler - of the proposed device;

2 - device according to the prototype;

3 - the proposed device,

4 - the proposed device with two U-shaped absorptive bubblers.

For definitions of all devices in the reaction bubbler was placed 50 ml of a standard solution of bromide-ion in the absorption bubbler 15 ml of a solution of sodium sulfite. The extraction was carried out with gaseous nitrogen for 30 min at 50 ml/min. and the Comparative data presented in the table (see the end of the description).

The table shows that the found concentrations of bromide-ion in the most high and constant over the entire range of concentrations when using h is s definition.

Obtained data indicate the effectiveness of the proposed device in comparison with the prototype and other known devices.

Thus, the combination of the reaction bubbler cylindrical shape having an annular gap for receiving a gas-extractant with absorption bubbler U-shaped, having a different design of the knees, allows the most complete extraction of this volatile component.

The proposed device is successfully used for indirect determination of nitrite ion in waters, based on the oxidation of nitrite-ion iodide ion with formation of gaseous iodine.

Sources of information:

1. Vitenberg A. G., Joffe B. C. Gas extraction in chromatographic analysis. L.: Chemistry, 1982, S. 16, 40.

2. Polanski N. G. Analytical chemistry of bromine. M., Nauka, 1980, S. 54, the reference 909.

3. Polanski N. G. Analytical chemistry of bromine. M., Nauka, 1980, S. 54, the link a.

4. Polanski N. G. Analytical chemistry of bromine. M., Nauka, 1980, S. 58, reference 586.

5. Pilipenko A. G., Duy, O. C. Chemistry and water technology, 1991, T. 13, N 3, p. 230.

1. Device for continuous gas extraction volatile component, consisting of the reaction barbeau is to absorb the volatile component, characterized in that the reaction bubbler is made in the form of a cylinder having the same diameter in height, placed in the cylinder device to enter a gas-extracting agent, executed in the form of two concentrically arranged tubes, absorption bubbler is made U-shaped, one knee it is a tube and serves as a connecting link with the reaction bubbler, and the other knee is a few rigidly connected with each other balls.

2. The device under item 1, characterized in that the diameter and height of the cylinder is selected from the condition: the volume of the gas space above the reaction solution is much less than the volume of the solution.

3. The device under item 1, characterized in that the outer tube of the device to enter a gas-extractant is in the upper part of the socket for receipt of a gas-extractant in the annular gap between the tubes, and the lower end of the inner tube is closed.

 

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