CN111044589A - Preparation method of zero-point correction oxygen-free water for electrodes of online dissolved oxygen meter in thermal power plant - Google Patents
Preparation method of zero-point correction oxygen-free water for electrodes of online dissolved oxygen meter in thermal power plant Download PDFInfo
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- CN111044589A CN111044589A CN201911211261.7A CN201911211261A CN111044589A CN 111044589 A CN111044589 A CN 111044589A CN 201911211261 A CN201911211261 A CN 201911211261A CN 111044589 A CN111044589 A CN 111044589A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/14—Production of inert gas mixtures; Use of inert gases in general
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
- B01J8/10—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles moved by stirrers or by rotary drums or rotary receptacles or endless belts
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/70—Treatment of water, waste water, or sewage by reduction
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/02—Non-contaminated water, e.g. for industrial water supply
Abstract
The invention discloses a preparation method of zero-point correction oxygen-free water for an electrode of an online dissolved oxygen meter in a thermal power plant. The method prepares the oxygen-free water in the flask, avoids oxygen in air from permeating into the solution in the atmospheric environment, realizes a real zero dissolved oxygen medium, improves the measurement accuracy of a dissolved oxygen meter in a trace range, further enhances the supervision level of a water vapor system, reduces the corrosion risk of a thermodynamic system of a generator set, and reduces the maintenance cost.
Description
Technical Field
The invention relates to the technical field of oxygen measurement equipment, in particular to a preparation method of zero-point correction oxygen-free water for an online dissolved oxygen meter electrode of a thermal power plant.
Background
The dissolved oxygen refers to molecular oxygen dissolved in water or liquid phase, and the index is an important factor influencing the corrosion degree of metal materials of a water vapor system of a thermal power plant and is also an index of key monitoring in water vapor quality supervision of normal operation of a unit. An outlet of a condensate pump of a common generator set, an inlet of a deaerator, an outlet of the deaerator and an inlet of an economizer are all provided with online dissolved oxygen meter monitoring measuring points, and the system corrosion preventive monitoring is enhanced. The key issue for dissolved oxygen determination is the choice and application of the sensor, the most common of which is the membrane electrode method of the electrochemical sensor method.
In daily application and maintenance of the dissolved oxygen meter, the electrode is generally subjected to air correction only, namely the electrode is placed in an atmospheric environment to be subjected to air correction, but zero point correction is not performed, so that when the online dissolved oxygen meter is used for measuring the trace dissolved oxygen content, the indicating value is inaccurate, and a blind zone is generated in monitoring the dissolved oxygen content of a water vapor system. Because the problem that the zero point correction of the online dissolved oxygen meter is difficult to realize in an anaerobic environment cannot reach the anaerobic environment in the true sense, the zero point correction of the online dissolved oxygen meter is inaccurate or cannot be implemented, and the like, the accuracy of the online dissolved oxygen meter is directly reduced, and the dissolved oxygen index cannot be accurately monitored. According to EPRI statistics, the cost of maintenance and the like is increased by 30 billion dollars due to power station corrosion problems in one year in the United states power generation enterprises, and it is very important to implement zero point correction on an online dissolved oxygen meter to improve the accuracy of the dissolved oxygen meter.
The method implements zero correction on an online dissolved oxygen meter, and the key technology is to realize a real zero dissolved oxygen medium, namely an oxygen-free water medium. At present, the problem that oxygen in air permeates into a solution in an atmospheric environment still exists by adopting a method of adding a sodium bisulfite solution, and the problem is difficult to solve. The invention aims to provide a novel preparation method of oxygen-free water for an online dissolved oxygen meter electrode in a thermal power plant, which can realize real zero oxygen correction of the online dissolved oxygen meter and greatly improve the accuracy of the dissolved oxygen meter.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a preparation method of zero-point correction oxygen-free water for electrodes of an online dissolved oxygen meter in a thermal power plant, which aims to solve the problem that the oxygen-free water prepared by adding sodium sulfite into distilled water cannot be truly oxygen-free when air permeates into the solution in an atmospheric environment, and further improve the accuracy of the correction of the dissolved oxygen meter.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows.
A preparation method of zero-point correction oxygen-free water for an on-line dissolved oxygen meter electrode in a thermal power plant comprises the following specific preparation steps:
s1: filling desalted water or a water sample at an outlet of a deaerator into a double-neck flask with a certain capacity, and adding a deaerator and a catalyst, wherein the mass ratio of the water sample to the deaerator to the catalyst is 100: 5: 0 to 1;
s2: inserting a dissolved oxygen electrode into the solution at the bottle mouth right above the two-neck flask, inserting a nitrogen channel into the solution at the other bottle mouth of the two-neck flask, and ensuring the sealing performance of the two-neck flask mouth to be complete; the V-shaped exhaust pipe of the double-neck flask is blocked by cotton which prevents outside air from flowing back to the double-neck flask;
s3: introducing high-purity nitrogen to the bottom of the solution through a nitrogen channel at a flow rate of 1-3L/h, continuously shaking the double-neck flask or stirring by adopting a magnetic stirrer for 1-2 hours, and discharging air from the V-shaped exhaust pipe under the action of the nitrogen;
s4: when the online data measured by using the dissolved oxygen electrode stably reach 0ug/L, the preparation of the oxygen-free water is finished.
In a further optimized technical scheme, the deoxidant in the step S1 is a mixture of 5.0% sodium hydrosulfite and sodium ascorbate, and the mass ratio of the sodium hydrosulfite to the sodium ascorbate in the mixture is 1: 1.
Further optimizing the technical scheme, the catalyst in the step S1 is cobalt chloride.
Further optimizing the technical scheme, the side wall of the bottom of the double-neck flask is provided with a sampling water outlet for taking out the oxygen-free water.
Due to the adoption of the technical scheme, the technical progress of the invention is as follows.
The preparation method of the zero-point correction oxygen-free water for the electrodes of the on-line dissolved oxygen meter in the thermal power plant can realize a real zero dissolved oxygen medium, namely the oxygen-free water medium, can avoid the problem that air permeates into the solution in the atmospheric environment in the existing sodium bisulfite solution method, and can realize real zero oxygen correction, thereby greatly improving the measurement accuracy of the instrument in the range of trace dissolved oxygen content, improving the qualification rate of the instrument, enhancing the chemical supervision level of a water vapor system and reducing the risk of corrosion of a thermodynamic system of a generating set.
Drawings
FIG. 1 is a schematic structural diagram of an application apparatus of the present invention;
wherein: 1. an electrode, 2, a nitrogen channel, 3, a magnetic stirrer, 4, a sampling water outlet, 5, a V-shaped exhaust pipe and 6, a double-neck flask.
Detailed Description
A preparation method of zero-point correction oxygen-free water for an on-line dissolved oxygen meter electrode in a thermal power plant comprises the following specific preparation steps:
s1: filling a demineralized water sample into a double-neck flask 6, adding 5.0% of a mixture of sodium hydrosulfite and sodium ascorbate in a mass ratio of 1:1, and adding cobalt chloride for catalysis, wherein the mass ratio of the water sample, a deoxidant and a catalyst is 100: 5: 0 ~ 1, start magnetic stirrer 3 and carry out magnetic stirring, perhaps constantly rock double-necked flask 6, the stirring of magnetic stirrer 3 is more even, speed is more stable.
S2: inserting a dissolved oxygen electrode 1 into the solution at the bottle mouth right above the two-neck flask 6, inserting a nitrogen channel into the solution at the other bottle mouth of the two-neck flask 6, sealing the two-neck flask 6 completely, plugging cotton with a V-shaped exhaust pipe 5, and preventing outside air from flowing back into the two-neck flask 6.
S3: starting the magnetic stirring bar 3 for stirring, introducing high-purity nitrogen from the nitrogen channel 2, and controlling the flow rate of the nitrogen to be 1-3L/h and introducing the nitrogen for 1-2 h. In the nitrogen introducing process, the original air in the two-neck flask 6 is expelled out of the two-neck flask 6, the oxygen in the water sample is gradually reacted, or the oxygen is expelled out of the two-neck flask 6 along with the nitrogen in the nitrogen bubbling process.
S4: open dissolved oxygen electrode 1, survey on-line data can stably reach when 0ug/L, no oxygen water preparation is accomplished, can carry out the zero point correction of online dissolved oxygen meter, open the stagnant water valve of the sampling delivery port 4 that 6 bottom lateral walls in two neck flasks set up, can take out no oxygen water.
The invention will be described in further detail below with reference to the figures and specific examples.
Example 1:
s1: 700mL of a demineralized water sample is put into a 1L double-neck flask 6, 35g of a 5.0% mixture of sodium hydrosulfite and sodium ascorbate in a mass ratio of 1:1 is added, 0.7g of cobalt chloride is added for catalysis, and a magnetic stirrer 3 is started for stirring.
S2: inserting a dissolved oxygen electrode 1 into the solution at the bottle mouth right above the two-neck flask 6, inserting a nitrogen channel into the solution at the other bottle mouth of the two-neck flask 6, sealing the two-neck flask 6 completely, plugging cotton with a V-shaped exhaust pipe 5, and preventing outside air from flowing back into the two-neck flask 6.
S3: and starting the magnetic stirrer 3 for stirring, introducing high-purity nitrogen from the nitrogen channel 2, controlling the flow rate of the nitrogen to be 2L/h, and introducing the nitrogen for 2 h. In the nitrogen introducing process, the original air in the two-neck flask 6 is expelled out of the two-neck flask 6, the oxygen in the water sample is gradually reacted, or the oxygen is expelled out of the two-neck flask 6 along with the nitrogen in the nitrogen bubbling process.
S4: and (3) opening the dissolved oxygen electrode 1, measuring the online data to be 0ug/L stably, completing the preparation of the oxygen-free water, and performing zero correction of the online dissolved oxygen meter.
Example 2:
s1: 600mL of a demineralized water sample is put into a 1L double-neck flask 6, 30g of a 5.0% mixture of sodium hydrosulfite and sodium ascorbate in a mass ratio of 1:1 is added, 0.6g of cobalt chloride is added for catalysis, and a magnetic stirrer 3 is started for stirring.
S2: inserting a dissolved oxygen electrode 1 into the solution at the bottle mouth right above the two-neck flask 6, inserting a nitrogen channel into the solution at the other bottle mouth of the two-neck flask 6, sealing the two-neck flask 6 completely, plugging cotton with a V-shaped exhaust pipe 5, and preventing outside air from flowing back into the two-neck flask 6.
S3: starting the magnetic stirring bar 3 for stirring, introducing high-purity nitrogen from the nitrogen channel 2, controlling the flow rate of the nitrogen to be 2L/h, and introducing the nitrogen for 1.5 h. In the nitrogen introducing process, the original air in the two-neck flask 6 is expelled out of the two-neck flask 6, the oxygen in the water sample is gradually reacted, or the oxygen is expelled out of the two-neck flask 6 along with the nitrogen in the nitrogen bubbling process.
S4: and (3) opening the dissolved oxygen electrode 1, measuring the online data to be 0ug/L stably, completing the preparation of the oxygen-free water, and performing zero correction of the online dissolved oxygen meter.
Example 3:
s1: 800mL of a demineralized water sample is put into a 1L double-neck flask 6, 40g of a 5.0% mixture of sodium hydrosulfite and sodium ascorbate in a mass ratio of 1:1 is added, 0.8g of cobalt chloride is added for catalysis, and a magnetic stirrer 3 is started for stirring.
S2: inserting a dissolved oxygen electrode 1 into the solution at the bottle mouth right above the two-neck flask 6, inserting a nitrogen channel into the solution at the other bottle mouth of the two-neck flask 6, sealing the two-neck flask 6 completely, plugging cotton with a V-shaped exhaust pipe 5, and preventing outside air from flowing back into the two-neck flask 6.
S3: and starting the magnetic stirrer 3 for stirring, introducing high-purity nitrogen from the nitrogen channel 2, controlling the flow rate of the nitrogen to be 2L/h, and introducing the nitrogen for h. In the nitrogen introducing process, the original air in the two-neck flask 6 is expelled out of the two-neck flask 6, the oxygen in the water sample is gradually reacted, or the oxygen is expelled out of the two-neck flask 6 along with the nitrogen in the nitrogen bubbling process.
S4: and (3) opening the dissolved oxygen electrode 1, measuring the online data to be 0ug/L stably, completing the preparation of the oxygen-free water, and performing zero correction of the online dissolved oxygen meter.
Claims (4)
1. A preparation method of zero-point correction oxygen-free water for an electrode of an online dissolved oxygen meter in a thermal power plant is characterized by comprising the following specific preparation steps:
s1: filling desalted water or a water sample at an outlet of a deaerator into a double-neck flask (6) with a certain capacity, and adding a deaerator and a catalyst, wherein the mass ratio of the water sample to the deaerator to the catalyst is 100: 5: 0 to 1;
s2: inserting a dissolved oxygen electrode (1) into the solution from the bottle mouth right above the two-neck flask (6), inserting a nitrogen channel into the solution from the other bottle mouth of the two-neck flask (6), and ensuring the sealing performance of the two-neck flask mouth to be intact; the V-shaped exhaust pipe (5) of the double-neck flask (6) is blocked by cotton which prevents outside air from flowing back to the double-neck flask (6);
s3: introducing high-purity nitrogen to the bottom of the solution through a nitrogen channel (2) at a flow rate of 1-3L/h, continuously shaking the double-neck flask (6) or stirring for 1-2 hours by adopting a magnetic stirrer (3), and discharging air from a V-shaped exhaust pipe (5) under the action of the nitrogen;
s4: when the online data measured by using the dissolved oxygen electrode (1) stably reaches 0ug/L, the preparation of the oxygen-free water is finished.
2. The method for preparing the zero-point correction oxygen-free water for the electrodes of the on-line dissolved oxygen meter in the thermal power plant according to claim 1, characterized by comprising the following steps: the oxygen scavenger in step S1 is a mixture of 5.0% sodium dithionite and sodium ascorbate, and the mass ratio of sodium dithionite to sodium ascorbate in the mixture is 1: 1.
3. The method for preparing the zero-point correction oxygen-free water for the electrodes of the on-line dissolved oxygen meter in the thermal power plant according to claim 1, characterized by comprising the following steps: the catalyst in step S1 is cobalt chloride.
4. The method for preparing the zero-point correction oxygen-free water for the electrodes of the on-line dissolved oxygen meter in the thermal power plant according to claim 1, characterized by comprising the following steps: and a sampling water outlet (4) for taking out the oxygen-free water is formed in the side wall of the bottom of the double-neck flask (6).
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CN113466423A (en) * | 2021-07-28 | 2021-10-01 | 西安热工研究院有限公司 | Dissolved oxygen meter calibration test system and method |
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Address after: 050000 2nd floor, Yingpan commercial and residential building, 129 Nanxiao street, Qiaoxi District, Shijiazhuang City, Hebei Province Applicant after: Hebei Jiantou energy science and Technology Research Institute Co.,Ltd. Address before: 050000 2nd floor, Yingpan commercial and residential building, 129 Nanxiao street, Qiaoxi District, Shijiazhuang City, Hebei Province Applicant before: HEBEI JI-YAN ENERGY SCIENCE AND TECHNOLOGY RESEARCH INSTITUTE Co.,Ltd. |
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Application publication date: 20200421 |