CN102937589A - Measuring device and measuring method of oxygen solubility under high-pressure conditions - Google Patents
Measuring device and measuring method of oxygen solubility under high-pressure conditions Download PDFInfo
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- CN102937589A CN102937589A CN2012104453213A CN201210445321A CN102937589A CN 102937589 A CN102937589 A CN 102937589A CN 2012104453213 A CN2012104453213 A CN 2012104453213A CN 201210445321 A CN201210445321 A CN 201210445321A CN 102937589 A CN102937589 A CN 102937589A
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Abstract
The invention relates to a measuring device and a measuring method of oxygen solubility under high-pressure conditions. A sampling kettle is connected with the bottom of a high-pressure reaction kettle through a second air inlet pipe and a water inlet pipe. A stirrer is arranged outside the top of the high-pressure reaction kettle, and a transmission shaft of the stirrer penetrates through the top of the high-pressure reaction kettle to be inserted at the central position of the high-pressure reaction kettle. A heating sleeve is wrapped in the middle of the high-pressure reaction kettle and connected with one end of a temperature control instrument, and the other end of the temperature control instrument is connected with a temperature measuring instrument. A pressure gauge is arranged at the top of the high-pressure reaction kettle, and a high-pressure oxygen cylinder is connected to the top of the high-pressure reaction kettle through a first control valve and a first air inlet pipe. By means of the measuring device and the measuring method, accurate solubility of oxygen in the water under the high-pressure conditions can be measured, and theoretical direction and technical support can be provided for scientific research, industry, agriculture, aquaculture, waste water biochemical treatment, self-purification of water and reduction of influences of dissolved oxygen oversaturation on fishes.
Description
Technical field
The present invention relates to a kind of measuring technique of gas solubility, particularly a kind of measuring method and measurement mechanism thereof for concentration of oxygen gas under the condition of high voltage and pressure relation belong to hydraulic engineering dissolved gas supersaturation technical field.
Background technology
In the many large hydraulic engineerings of China, according to its water regulation demand, hydraulic engineering need to be passed through the outlet structure escape works such as spillway, flood discharging tunnel and sluice in the river course downstream.Because current pressure is higher than atmospheric pressure far away in cushion pool or the river course, reach several even ten above atmospheric pressure, simultaneously current can be followed a large amount of aerations during water discharge, therefore the dissolved oxygen DO supersaturation can occur in this large flow, strong aerated flow under the hyperbaric environment of dam cushion pool, and this supersaturation dissolved oxygen DO can be present in the tens of kms in downstream even the hundreds of km water body, cause the hydrobiont trouble bubble illness such as fish, thereby to river aquatic ecosystem harm.
Generation and the release of dam downstream supersaturation dissolved oxygen DO, mainly with air entrainment and mix gas in water body the pressure-bearing size and under time, dam the factors such as the depth of water in cushion pool and river course and flow velocity relevant, therefore the dissolved oxygen DO supersaturation problem under the condition of high voltage belongs to complicated aqueous vapor two-phase flow problem, it relates to many fields such as water conservancy project hydraulics, environmental hydraulics, liquid-gas interface mass transfer, and its research difficulty is very big.Therefore, comparatively deficient about concentration of oxygen gas research under the condition of high voltage at present, the experimental provision that is used for research also lacks.
In present stage, the means that in the hydraulic engineering dissolved oxygen DO Study on Problems under the condition of high voltage adopted usually are prototype measurements, but there are many restrictive factors in it: (1) observer must arrive the dam field observation that is sluicing, very inconvenience; (2) many physical factors such as water flow, flow velocity, air entrainment, downstream pressure, depth of water and physical condition all exist uncontrollability and nonrepeatability in the high dam flood discharge; (3) the current pressure measurement work in the sluicing process middle and lower reaches water body is difficulty comparatively, often adopts experimental formula or semiempirical half theoretical formula, thereby causes larger error; (4) for guaranteeing the comprehensive benefits such as hydraulic engineering generating, irrigation, high dam sluicing frequency is lower, and lasts short.Therefore it is far from being enough the research of dissolved oxygen DO problem under the condition of high voltage of dam downstream only being relied on prototype measurement.
The measuring method of dissolved oxygen DO commonly used has chemical iodimetric titration and the membrane electrode method of use in dissolved oxygen meter etc. at present.The principle of chemistry iodimetric titration is: when adding manganese sulfate and alkaline potassium iodide solution in the water sample, can generate immediately the manganous hydroxide precipitation, manganous hydroxide is extremely unstable, easily be oxidized to mangaic acid manganese by the dissolved oxygen DO in the water, after adding sulfuric acid acidation again, the dissolved oxygen DO of chemical combination is with the potassium iodide oxidation and discharge the free state iodine suitable with dissolved oxygen content, and then the standard solution with sodium thiosulfate carries out titration.According to the consumption of sodium thiosulfate, calculate the content of oxygen in water.Use its principle of electrode method to be: oxygen permeation membrane makes the dissolved oxygen DO in the water produce the electric signal that is directly proportional with oxygen concentration at electrode by having optionally, again this signal is outputed in the dissolved oxygen meter after amplification, conversion and temperature compensation, thereby directly measure the dissolving oxygen concentration.Above two kinds of methods all are the dissolved oxygen sensing methods under the condition of normal pressure, can not finish the measurement of concentration of oxygen gas under the condition of high voltage.This is to adopt the membrane electrode method of chemical iodimetric titration or dissolved oxygen meter to measure concentration of oxygen gas because if the water body that condition of high voltage is issued to dissolution equilibrium is down to normal pressure again, the meeting appearance reduces suddenly to cause the problem of dissolved oxygen DO release owing to pressure, have a strong impact on measuring accuracy.Therefore in order to guarantee measuring accuracy, need under the condition of high voltage of autoclave, to finish the measurement to concentration of oxygen gas, but because the limited space of reactor, dissolved oxygen meter is put into reactor, might collide with stirrer, thereby dissolved oxygen meter is damaged, and dissolved oxygen meter is the instrument that uses under the condition of normal pressure in addition, is placed in the reactor to be damaged because of High Pressure.
This seminar improves traditional iodimetric titration through exploration, research and analysis, proposes the high pressure chemistry iodimetric titration, and concentration of oxygen gas measurement mechanism under the design condition of high voltage, to realize the accurate measurement to concentration of oxygen gas under the condition of high voltage.
Summary of the invention
Purpose of the present invention in order to overcome existing shortcomings and deficiencies in the traditional measurement method, provides a kind of measurement mechanism for concentration of oxygen gas under the condition of high voltage just; And provide this measurement mechanism of a kind of usefulness to be used for the measuring method of concentration of oxygen gas under the condition of high voltage.By this measurement mechanism and measuring method, can measure the precise solubility of oxygen in water under condition of high voltage, thereby for scientific research, industry, aquaculture, agricultural, wastewater biochemical processing, the self-purification of water and how to slow down the dissolved oxygen DO supersaturation and provide theoretical direction and technical support to the impacts of fish.
The objective of the invention is to realize by the technical scheme that following technical measures consist of.
The measurement mechanism of concentration of oxygen gas under the condition of high voltage of the present invention is characterized in that comprising high-pressure oxygen cylinder, the first by-pass valve control, temperature controller, temperature measurer, the first draft tube, autoclave, stirrer, tensimeter, heating jacket, the second by-pass valve control, the second draft tube, sampling still, water inlet pipe and the 3rd by-pass valve control; Described sampling still is connected with the autoclave bottom by the second draft tube that the second by-pass valve control is installed and the water inlet pipe that the 3rd by-pass valve control is installed; Stirrer is installed in the autoclave top outer, and the stirrer transmission shaft passes the autoclave top and inserts its center; Heating jacket is wrapped in the autoclave middle part and links to each other with temperature controller one end, and the temperature controller other end links to each other with temperature measurer; Tensimeter is installed on the autoclave top, and high-pressure oxygen cylinder is connected to the autoclave top by the first draft tube that the first by-pass valve control is installed.
In the technique scheme, described stirrer is that a motor consists of by two blades that transmission shaft connects.
In the technique scheme, the outlet elevation of described the first draft tube should near the autoclave bottom position, fully dissolve with the oxygen that accelerates the high-pressure oxygen cylinder supply.
In the technique scheme, the distance of described the first draft tube outlet distance high-voltage reactor bottom is no more than 10cm.
In the technique scheme, the installation of described the second draft tube should be higher than the position of water inlet pipe, also should be higher than the water surface in the autoclave.
The present invention adopts designed measurement mechanism to be used for measuring the measuring method of concentration of oxygen gas under the condition of high voltage, it is characterized in that comprising following processing step:
(1) in sampling still (9), puts into the manganese sulfate of 6g, the potassium iodide of 13g and the NaOH of 4g; The clear water that in autoclave (6), adds 3L;
(2) temperature that by temperature controller (13) water body in the autoclave is set is 20 ℃-100 ℃, opens stirrer (3), opens the first by-pass valve control (1) and the second by-pass valve control (7); Tensimeter (4) reading is set as predetermined value pressure, closes the first by-pass valve control again, when treating that pressure gauge reading is stablized, open the 3rd by-pass valve control (11), the sampling still is then taken a sample, and closes the second by-pass valve control and the 3rd by-pass valve control after sampling is finished;
(3) rock gently the sampling still, after chemical substance in it is fully reacted, the still of will taking a sample takes off, and get the solution of 100ML the still from sampling, and place beaker, adding 20mL concentration is the sulfuric acid solution of 3mol/L, hypo solution with 0.5moL/L carries out titration again, behind the micro-Huang of hypo solution, add again starch, continue to be titrated to the blue disappearance of this solution, the consumption of record hypo solution this moment;
(4) according to the solubleness of the sodium byposulfite consumption that records according to following formula calculating oxygen under different pressure:
Wherein, C
1Be the amount of substance concentration of hypo solution, V
1Be the volume of hypo solution, V
2For from the sampling still, obtaining the volume of solution.
In the measuring process of the present invention, open the first by-pass valve control by high-pressure oxygen cylinder toward autoclave when filling oxygen, control oxygen and slowly enter autoclave, observe simultaneously manometric reading, the pressure counting is near predetermined pressure in tensimeter, then turn the aperture of the first by-pass valve control down, make in the tensimeter pressure counting accurately reach predetermined pressure value.
In the measuring process of the present invention, how much not limitting of its sampling still sampling all can as long as be no more than the volume of the solution in the sampling still.
The principle of water temperature is in the temperature controller control autoclave of the present invention: temperature measurer records the water temperature in the autoclave, temperature controller is regulated and control the heating power of heating jacket according to the difference of the temperature of the temperature that records and setting, thus the water temperature in the control autoclave.
The consumption of each chemical substance in the measuring process of the present invention: manganese sulfate is got 6g, potassium iodide is got 13g, when NaOH is got the sulfuric acid solution 20ml of 4g, 3mol/L, can be measured the concentration of oxygen gas of 3L clear water under 0.1MPa-1.2 MPa pressure conditions.
The characteristics that the present invention compared with prior art has and useful technique effect:
Suddenly reduce to cause the difficult problem of measuring error when 1, measurement mechanism of the present invention has solved traditional iodimetric titration to the oxygen measurement that dissolves under the condition of high voltage because of its pressure, this measurement mechanism can be measured the concentration of oxygen gas under the different condition of high voltage accurately and fast.
2, measurement mechanism of the present invention has overcome because dam or high dam sluicing frequency is few, the time is short, uncontrollability and the nonrepeatability of many physical factors and physical condition have limited the difficulty to dissolved oxygen sensing under dam or the high dam sluicing downstream condition of high voltage simultaneously.
3, the Installation and Measurement of measurement mechanism of the present invention is all very convenient; Material requested and equipment investment are little, and cost is low.
Description of drawings
Concentration of oxygen gas measurement mechanism structural representation under Fig. 1 condition of high voltage of the present invention;
The relation curve of concentration of oxygen gas and pressure when temperature is 20 ℃ under Fig. 2 condition of high voltage of the present invention.
Among the figure, 1 first by-pass valve control, 2 first draft tube, 3 stirrers, 4 tensimeters, 5 heating jackets, 6 autoclaves, 7 second by-pass valve controls, 8 second draft tube, 9 sampling stills, 10 water inlet pipes, 11 the 3rd by-pass valve controls, 12 temperature measurers, 13 temperature controllers, 14 high-pressure oxygen cylinders.
Embodiment
Below in conjunction with accompanying drawing, and by specific embodiment the present invention is described in further detail, but do not mean that any restriction of the present invention.
The structure of the measurement mechanism of concentration of oxygen gas comprises high-pressure oxygen cylinder 14, the first by-pass valve control 1, the second by-pass valve control 7, the 3rd by-pass valve control 11, the first draft tube 2, the second draft tube 8, water inlet pipe 10, tensimeter 4, autoclave 6, heating jacket 5, sampling still 9, stirrer 3 and temperature measurer 12 and temperature controller 13 as shown in Figure 1 under the condition of high voltage of the present invention.Described high-pressure oxygen cylinder 14 links to each other with autoclave 6 with the first by-pass valve control 1 by the first draft tube 2; Tensimeter 4 is directly installed on autoclave 6 tops; Stirrer 4 is installed in autoclave 6 top outer, and the transmission shaft of stirrer 3 passes autoclave 6 tops and inserts its center; Heating jacket 5 is wrapped in autoclave 6 middle parts; Sampling still 9 is connected with autoclave 6 bottoms by the second draft tube 9 that the second by-pass valve control 7 is installed and the water inlet pipe 10 that the 3rd by-pass valve control 11 is installed.
The temperature measurer 12 that the present invention uses is used for measuring the water temperature in the autoclave 6, Temperature numerical is sent to temperature controller 13, temperature controller 13 is according to the temperature of passing back and the height of preset temperature, thus the heating power of control heating jacket 5, and then the temperature of water body in the control autoclave 6.
Embodiment
This example instrument equipment is as follows:
1, employed high-pressure oxygen cylinder is the WGA-229-20-63-20 model;
2, employed tensimeter is the YO-60 model tensimeter that river, Shanghai cloud instrucment and meter plant produces;
3, employed temperature controller is the XMT 122PT100 CU50 temperature indicating regulator of the Kunlun, Beijing permanent industry electronics technology company limited;
4, employed stirrer is the automatic stirrer of designed, designed, and its structure is that a motor consists of by two blades that transmission shaft connects.
Adopt its concrete operation step of measurement mechanism measurement concentration of oxygen gas of concentration of oxygen gas under the condition of high voltage of the present invention as follows:
(1) sampling put in the still 9 6g manganese sulfate, the potassium iodide of 13g and the NaOH of 4g, and in autoclave 6, add the clear water of 3L;
(2) temperature that sets autoclave is 20 ℃, open stirrer 3, open again the first by-pass valve control 1 and the second by-pass valve control 7, open the first by-pass valve control by high-pressure oxygen cylinder toward autoclave when filling oxygen, control oxygen and slowly enter autoclave, observe simultaneously manometric reading, when pressure readings in the tensimeter reaches setting value 0.1MPa, close the first by-pass valve control 1, when treating rain glass 4 stable reading, open the 3rd by-pass valve control 11, intake gauge 10 is connected with sampling still 9, sampling still 9 is taken a sample, and closes the second by-pass valve control 7 and the 3rd by-pass valve control 11 after sampling is finished;
(3) gently rock the sampling still 9, after its chemical substance is fully reacted, the still 9 of will taking a sample takes off, from sampling still 9, get the solution of 100ml, place beaker, adding 20ml concentration is the sulfuric acid solution of 3mol/L, carries out titration with the hypo solution of 0.5moL/L, add afterwards 1% starch solution 2ml until the micro-Huang of solution, then carry out titration with hypo solution; Continue to be titrated to blue the disappearance, the consumption of record hypo solution this moment; Calculate the solubleness of oxygen under the pressure at this moment according to the consumption of sodium thiosulfate of record;
(4) repeat above-mentioned three steps, when manometric reading is set to respectively 0.4MPa, 0.6MPa, 0.9MPa, 1.1MPa, calculate respectively 20 ℃ the time solubleness of oxygen under the different pressure conditions according to the consumption of sodium thiosulfate of record;
Calculate the solubleness of oxygen according to following formula according to sodium byposulfite consumption:
Wherein, C
1Be the amount of substance concentration of hypo solution, V
1Be the volume of hypo solution, V
2For from the sampling still, obtaining the volume of solution.
The chemical equation of whole process is as follows:
MnSO
4+ 2NaOH=Mn (OH)
2(white)+NaSO
4
2Mn (OH)
2+ O
2=2MnO (OH)
2(brown);
MnO(OH)
2+2H
2SO
4=Mn(SO
4)
2+H
2O；
Mn(SO
4)
2+KI=MnSO
4+I
2+K
2SO
4；
I
2+Na
2S
2O
3=2NaI+Na
2S
4O
6。
The present invention is according to above-mentioned measuring method and operation steps, and the temperature of setting is 20 ℃ to be measured, and the control gas pressure intensity is respectively 0.1 Mpa, 0.4 Mpa, 0.6 Mpa, 0.9 Mpa, 1.1 MPa measure, and the record measurement result is as shown in the table.
| Atmospheric pressure (Mpa) | 0.1 | 0.4 | 0.6 | 0.9 | 1.1 |
| Solubleness (mg/l) | 8.56 | 27.9 | 52.6 | 74.4 | 134.9 |
When water temperature is set to 20 ℃, when pressure was 0.1MPa-1.2MPa, concentration of oxygen gas with the change curve of its pressure as shown in Figure 2.
Claims (6)
1. the measurement mechanism of concentration of oxygen gas under the condition of high voltage is characterized in that comprising high-pressure oxygen cylinder (14), the first by-pass valve control (1), temperature controller (13), temperature measurer (12), the first draft tube (2), autoclave (6), stirrer (3), tensimeter (4), heating jacket (5), the second by-pass valve control (7), the second draft tube (8), sampling still (9), water inlet pipe (10) and the 3rd by-pass valve control (11); Described sampling still (9) is connected with autoclave (6) bottom with the water inlet pipe that the 3rd by-pass valve control (11) are installed (10) by the second draft tube (8) that the second by-pass valve control (7) is installed; Stirrer (3) is installed in autoclave (6) top outer, and stirrer (3) transmission shaft passes autoclave (6) top and inserts its center; Heating jacket (5) is wrapped in the autoclave middle part and links to each other with temperature controller (13) one ends, and the temperature controller other end links to each other with temperature measurer (12); Tensimeter (4) is installed on autoclave (6) top, and high-pressure oxygen cylinder (14) is connected to autoclave (6) top by the first draft tube (2) that the first by-pass valve control (1) is installed.
2. the measurement mechanism of concentration of oxygen gas under the described condition of high voltage according to claim 1 is characterized in that described stirrer (3) is that a motor consists of by two blades that transmission shaft connects.
3. the measurement mechanism of concentration of oxygen gas under the described condition of high voltage according to claim 1 is characterized in that the outlet elevation of described the first draft tube (2) should be near autoclave (6) bottom position.
4. the measurement mechanism of concentration of oxygen gas according to claim 1 or under the 3 described condition of high voltage is characterized in that the distance of described the first draft tube (2) outlet distance high-voltage reactor bottom is no more than 10cm.
5. the measurement mechanism of concentration of oxygen gas under the described condition of high voltage according to claim 1 is characterized in that the installation of described the second draft tube (8) should be higher than the position of water inlet pipe (10), also should be higher than the water surface in the autoclave (6).
6. a measurement mechanism that adopts claim 1-5 is characterized in that comprising following processing step for the measuring method of measuring concentration of oxygen gas under the condition of high voltage:
(1) in sampling still (9), puts into the manganese sulfate of 6g, the potassium iodide of 13g and the NaOH of 4g; The clear water that in autoclave (6), adds 3L;
(2) temperature that by temperature controller (13) water body in the autoclave is set is 20 ℃-100 ℃, opens stirrer (3), opens the first by-pass valve control (1) and the second by-pass valve control (7); Tensimeter (4) reading is set as predetermined value pressure, closes the first by-pass valve control again, when treating that pressure gauge reading is stablized, open the 3rd by-pass valve control (11), the sampling still is then taken a sample, and closes the second by-pass valve control and the 3rd by-pass valve control after sampling is finished;
(3) rock gently the sampling still, after chemical substance in it is fully reacted, the still of will taking a sample takes off, and get the solution of 100ML the still from sampling, and place beaker, adding 20mL concentration is the sulfuric acid solution of 3mol/L, hypo solution with 0.5moL/L carries out titration again, behind the micro-Huang of hypo solution, add again starch, continue to be titrated to the blue disappearance of this solution, the consumption of record hypo solution this moment;
(4) according to the solubleness of the sodium byposulfite consumption that records according to following formula calculating oxygen under different pressure:
Wherein, C
1Be the amount of substance concentration of hypo solution, V
1Be the volume of hypo solution, V
2For from the sampling still, obtaining the volume of solution.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106568770A (en) * | 2016-11-11 | 2017-04-19 | 上海利康消毒高科技有限公司 | Preparation method of rapid test card for rapidly testing peroxyacetic acid concentration |
| CN109323953A (en) * | 2017-08-01 | 2019-02-12 | 中国石油天然气股份有限公司 | The measuring method of element sulfur solubility in sulfurous gas |
| US11255832B2 (en) | 2017-07-06 | 2022-02-22 | Petrochina Company Limited | Device and method for determining solubility of elemental sulfur in sulfur-containing gas |
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| JPH02306141A (en) * | 1989-05-19 | 1990-12-19 | Toshiba Corp | Automatic measuring apparatus of hydrogen and oxygen concentration |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106568770A (en) * | 2016-11-11 | 2017-04-19 | 上海利康消毒高科技有限公司 | Preparation method of rapid test card for rapidly testing peroxyacetic acid concentration |
| US11255832B2 (en) | 2017-07-06 | 2022-02-22 | Petrochina Company Limited | Device and method for determining solubility of elemental sulfur in sulfur-containing gas |
| CN109323953A (en) * | 2017-08-01 | 2019-02-12 | 中国石油天然气股份有限公司 | The measuring method of element sulfur solubility in sulfurous gas |
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Application publication date: 20130220 |