CN112858613B - Device for calibrating trace dissolved oxygen monitor on line and operation method thereof - Google Patents
Device for calibrating trace dissolved oxygen monitor on line and operation method thereof Download PDFInfo
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- CN112858613B CN112858613B CN202110075000.8A CN202110075000A CN112858613B CN 112858613 B CN112858613 B CN 112858613B CN 202110075000 A CN202110075000 A CN 202110075000A CN 112858613 B CN112858613 B CN 112858613B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/18—Water
Abstract
The invention relates to a device for calibrating a trace dissolved oxygen monitor on line and an operation method thereof, wherein the device comprises a sample water supply mechanism, a pure water purification system, a mixing chamber connected with the pure water purification system, a standard solution supply mechanism connected with the mixing chamber, and a sample water supply mechanism connected with the mixing chamber through a circulating check assembly, wherein the sample water supply mechanism comprises an intermediate water tank, a reflux valve connected with the intermediate water tank and a circulating pump, and the sample water is stored in the intermediate water tank; the pure water purification system comprises an deoxidization resin column connected with the output end of the circulating pump and a mixed bed resin column unit connected with the deoxidization resin column, and the output end of the mixed bed resin column unit is connected with the mixing chamber; the circulation checking assembly comprises a circulation pipe connected with the mixing chamber and the middle water tank, an electric conductivity meter and a dissolved oxygen meter to be tested, wherein the electric conductivity meter and the dissolved oxygen meter are arranged on the circulation pipe. The invention carries out ultrapure water treatment on sample water, adopts barium chloride standard solution as chemical reagent, and has low input cost and high detection precision.
Description
Technical Field
The invention relates to the technical field of instrument calibration, in particular to a device for calibrating a trace dissolved oxygen monitor on line and an operation method thereof.
Background
The dissolved oxygen monitor is specially designed for measuring the ppb level of boiler feed water, condensed water and the like, ensures the stability and the accuracy of (ultra) low concentration, and greatly improves the measurement performance, the use environment and the like. The dissolved oxygen monitor is mainly used for continuously monitoring the dissolved oxygen value in chemical fertilizers, metallurgy, environmental protection, pharmacy, biochemistry, food, tap water and other solutions.
The existence of trace oxygen in water can greatly affect the production process, so that the accurate measurement of the trace oxygen in water is significant. The trace dissolved oxygen tester is used for measuring the content of trace dissolved oxygen in water, and is widely applied to industries such as electric power, electronics, chemical industry and the like. The conventional detection method of trace oxygen in water is a trace dissolved oxygen meter method, which can realize rapid measurement, but the trace dissolved oxygen meter needs to be calibrated before measurement, because the accuracy of measurement data is critical to the accuracy of the trace dissolved oxygen meter.
At present, the calibration device of the trace dissolved oxygen meter is mainly two types, one type is manufactured based on a Faraday electrolysis method, the other type is a standard gas method, wherein the technical principle manufactured based on the Faraday electrolysis method is that water flows through a background oxygen water treatment system, oxygen in the water is treated, then flows through a Faraday electrolytic cell (namely a standard oxygen generating device), quantitative oxygen is generated by controlling electric quantity to dissolve into the water, reaches a built-in dissolved oxygen electrode, is connected in series to the measured dissolved oxygen meter, and the outflow water is recycled to the closed system; standard gas methods such as DL/T1002-2006 "method of calibrating a micro dissolved oxygen meter" and standard gas methods of ASTM in the united states, etc. The two methods are different in that the standard oxygen generating device generates oxygen through electrolysis, and the second method is to introduce gaseous oxygen; the pretreatment of both devices is basically the same, and the treated background oxygen water is introduced.
The two devices need treated background oxygen water, namely, the original oxygen in the water is completely removed, and a strict closed environment is needed for removing the original oxygen in the water; in addition, the flow rate of the sample flowing through the electrode is strictly limited, if the flow rate is generally required to be set at (15-20) mL/min, and the balance time is also required to be determined empirically, so that the system of the verification and calibration device of the conventional trace dissolved oxygen meter is complex, the manufacturing cost is high, the balance time is required to be manually mastered during the calibration, and the calibration precision is low.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a device for calibrating a trace dissolved oxygen monitor on line and an operation method thereof.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the device for calibrating the trace dissolved oxygen monitor on line comprises a sample water supply mechanism, a pure water purification system connected with the sample water supply mechanism, a mixing chamber connected with the pure water purification system, and a standard solution supply mechanism connected with the mixing chamber, wherein the mixing chamber is connected with the sample water supply mechanism through a circulating check assembly, the sample water supply mechanism comprises an intermediate water tank, a reflux valve and a circulating pump connected with the intermediate water tank, and sample water is stored in the intermediate water tank;
the pure water purification system comprises an deoxidization resin column connected with the output end of the circulating pump and a mixed bed resin column unit connected with the deoxidization resin column, and the output end of the mixed bed resin column unit is connected with the mixing chamber;
the circulation verification assembly comprises a circulation pipe connected with the mixing chamber and the middle water tank, and an electric conductivity meter and a dissolved oxygen meter to be tested which are arranged on the circulation pipe.
Further, the standard solution supply mechanism comprises a standard solution bottle, an air pump connected with the standard solution bottle, the standard solution bottle is connected with the mixing chamber through a standard solution peristaltic pump, standard solution containing barium chloride and saturated solution oxygen is stored in the standard solution bottle, and an air sand head connected with the air pump is arranged in the standard solution bottle.
Further, a flowmeter for monitoring the flow rate of the circulating sample water in the system is arranged on the circulating pipe.
Further, the mixed bed resin column unit comprises a first mixed bed resin column and a second mixed bed resin column, and is used for removing anions and cations (except hydroxide ions and hydrogen ions) in the system sample water.
Further, the deoxidizing resin column is used for removing the dissolved oxygen in the system sample water, so that the content of the dissolved oxygen in the system sample water is removed to be approximately 0.
An operation method for calibrating a trace dissolved oxygen monitor on line comprises the following steps:
s1, high-purity water is used as sample water to be stored in an intermediate water tank, the whole circulating water system is closed, air in the system is replaced by pure nitrogen, then the nitrogen is replaced by the high-purity water, and finally the whole system is guaranteed to be full of water;
s2, adjusting the opening of a reflux valve to enable the flow rate of circulating sample water of the system to reach L1;
s3, absorbing dissolved oxygen contained in the sample water when the sample water passes through the deoxidizing resin column, wherein the content of the dissolved oxygen approaches to 0;
s4, injecting a proper amount of hydrazine solution into the system through a standard liquid peristaltic pump, wherein the hydrazine solution can further eliminate the dissolved oxygen content in sample water, and the dissolved oxygen content in the sample is further reduced by observing the indication value of a dissolved oxygen meter to be detected;
s5, removing anions and cations in the sample water when the sample water passes through the mixed bed resin column unit;
s6, filling a barium chloride standard solution with the concentration of C1 into the standard solution bottle, and fully blowing air into the standard solution bottle through an air pump to enable the dissolved oxygen content of the barium chloride standard solution in the standard solution bottle to be in a saturated state, wherein the concentration of the dissolved oxygen is C2;
s7, injecting the barium chloride standard solution in the standard solution bottle into the mixing chamber through the standard solution peristaltic pump at a certain rotating speed, wherein the injection flow rate is L2;
s8, injecting a barium chloride standard solution into a circulating sample water system, mixing the sample water in a mixing chamber, diluting the sample water, diluting the barium chloride standard solution with saturated solution oxygen in equal proportion, and enabling the ratio of the barium chloride to the dissolved oxygen content in the sample to be the same as the ratio of the barium chloride to the dissolved oxygen content in the standard solution;
s9, the sample water in the mixing chamber flows through an electric conductivity meter, the electric conductivity meter measures the electric conductivity value of the sample water, the electric conductivity value is closely related to the concentration of barium chloride in the sample water, the concentration C3=f (Con) of the barium chloride in the sample water in the mixing chamber can be calculated, f (Con) is a mathematical model of conversion relation between electric conductivity and the concentration of the barium chloride, and the concentration of the barium chloride in the sample water in the mixing chamber and the concentration C4 of the dissolved oxygen in the sample can be calculated because the concentration of the barium chloride in the standard solution and the saturated dissolved oxygen are diluted in equal proportion synchronously;
s10, taking the dissolved oxygen concentration C4 of the sample in the mixing chamber as a standard value, and checking and calibrating the dissolved oxygen meter to be tested when the sample water in the mixing chamber flows through the dissolved oxygen meter.
Further, in step S9, f (Con) = 0.743 ×con, where Con is a sample water conductivity value measured by the conductivity meter.
In addition, it should be expanded that the similar method of the invention can be used for measuring trace sodium, potassium, calcium, magnesium, iron, copper and other ions.
The beneficial effects of the invention are as follows: the invention adopts an deoxidization resin column and a mixed bed resin column unit to remove dissolved oxygen and anions and cations from sample water, so that the sample water is close to theoretical pure water, a barium chloride standard solution is injected into a circulating sample water system and is mixed with the sample water in a mixing chamber for dilution, as the barium chloride standard solution is diluted with saturated solution oxygen in equal proportion, the ratio of the content of barium chloride to the content of dissolved oxygen in the sample is the same as the ratio of the content of barium chloride to the content of dissolved oxygen in the standard solution, the conductivity value of the sample water is measured through a conductivity meter, the concentration of barium chloride in the sample water in the mixing chamber can be calculated, and as the barium chloride concentration of the barium chloride standard solution is diluted with saturated dissolved oxygen in equal proportion synchronously, the concentration of dissolved oxygen in the sample water in the mixing chamber can be calculated, the sample dissolved oxygen concentration in the mixing chamber is taken as a standard value, and the sample water in the mixing chamber can be checked and calibrated when flowing through a dissolved oxygen meter to be tested;
the invention carries out ultrapure water treatment on sample water, adopts the barium chloride standard solution as a chemical reagent, has convenient and stable operation, and has low input cost and high detection precision.
Drawings
FIG. 1 is a schematic diagram of the structure of the present invention;
Detailed Description
As shown in fig. 1, the device for calibrating the trace dissolved oxygen monitor on line comprises a sample water supply mechanism, a pure water purification system connected with the sample water supply mechanism, a mixing chamber 5 connected with the pure water purification system, a standard solution supply mechanism connected with the mixing chamber 5, wherein the mixing chamber 5 is connected with the sample water supply mechanism through a circulation verification assembly, the sample water supply mechanism comprises an intermediate water tank 13, a reflux valve 12 connected with the intermediate water tank 13 and a circulating pump 1, and the sample water is stored in the intermediate water tank 13;
the pure water purification system comprises an deoxidization resin column 2 connected with the output end of the circulating pump 1 and a mixed bed resin column unit connected with the deoxidization resin column 2, wherein the output end of the mixed bed resin column unit is connected with a mixing chamber 5;
the circulation checking assembly comprises a circulation pipe connected with the mixing chamber 5 and the intermediate water tank 13, an electric conductivity meter 9 arranged on the circulation pipe and a dissolved oxygen meter 10 to be tested. The circulation pipe is provided with a flowmeter 11 for monitoring the flow rate of the circulating sample water in the system.
The standard solution supply mechanism comprises a standard solution bottle 7, an air pump 8 connected with the standard solution bottle 7, the standard solution bottle 7 is connected with the mixing chamber 5 through a standard solution peristaltic pump 6, standard solution containing barium chloride and saturated solution oxygen is stored in the standard solution bottle 7, and an air sand head connected with the air pump 8 is arranged in the standard solution bottle.
Further, the mixed bed resin column unit includes a first mixed bed resin column 3 and a second mixed bed resin column 4, and is used for removing anions and cations (excluding hydroxide ions and hydrogen ions) in the system sample water.
In this embodiment:
circulation pump 1: the device is used for circulating the sample water of the whole system.
Oxygen-scavenging resin column 2: is used for removing the dissolved oxygen in the circulating sample water in the system, so that the dissolved oxygen content of the circulating sample water in the system approaches to 0.
A first mixed bed resin column 3 and a second mixed bed resin column 4: the anion and cation (excluding hydroxide ion and hydrogen ion) in the sample water of the system are removed to make the ion content in the sample water approach 0, and the sample water is close to theoretical pure water.
Mixing chamber 5: for injecting an external barium chloride standard solution into the circulating sample water. The standard solution contains saturated dissolved oxygen and barium chloride, and after the saturated dissolved oxygen and the barium chloride are injected into the circulating sample water, the standard solution is diluted in equal proportion, so that the content of the dissolved oxygen in the sample water can be converted by monitoring the concentration of the barium chloride in the sample water.
Label peristaltic pump 6: for injection of standard solutions. The standard solution in the standard solution bottle can be quantitatively extracted and injected into the circulating sample water system, and the amount of the standard solution injected into the circulating sample water system can be regulated by regulating the diameter and the rotating speed of a pump pipe of a peristaltic pump, so that the concentration of barium chloride and the concentration of dissolved oxygen in the system are regulated.
Label liquid bottle 7: standard solutions for storing barium chloride and saturated solution oxygen. The concentration of the barium chloride standard solution is C1. The bottle is provided with an air sand head, and after full air blowing, the content of dissolved oxygen in the barium chloride standard solution can reach a saturated state, and the concentration is C2.
Air pump 8: the method is used for fully blowing air into the barium chloride standard solution in the standard solution bottle to enable the oxygen content of the solution to reach a saturated state.
Conductivity table 9: for detecting conductivity values in the sample solution.
Dissolved oxygen meter 10 to be measured: the meter is a meter to be measured, when the barium chloride standard solution is injected into sample water, the content of dissolved oxygen in the standard solution is in a saturated state, the concentration of saturated oxygen can be calculated according to the temperature and the atmospheric pressure of the current environment, and then the standard solution of the barium chloride is injected into circulating sample water through a peristaltic pump of the standard solution and is fully mixed. The barium chloride and the saturated dissolved oxygen in the standard solution can be diluted in equal proportion, so that the concentration of the barium chloride can be calculated by measuring the conductivity, the content of the dissolved oxygen in the sample water can be obtained, the concentration C4 of the dissolved oxygen in the mixed indoor sample is taken as a standard value, and the mixed indoor sample water can be checked and calibrated when flowing through the dissolved oxygen meter 10 to be tested.
11 flowmeter: the flow rate of the circulating sample water in the monitoring system is matched with the flow rate of the peristaltic pump, so that the concentration of dissolved oxygen in the sample can be verified.
Further, an operation method for calibrating the trace dissolved oxygen monitor on line comprises the following steps:
s1, high-purity water is used as sample water to be stored in an intermediate water tank 13, the whole circulating water system is closed, air in the system is replaced by pure nitrogen, then the nitrogen is replaced by the high-purity water, and finally the whole system is guaranteed to be full of water;
s2, adjusting the opening of the reflux valve 12 to enable the flow rate of circulating sample water of the system to reach L1;
s3, absorbing dissolved oxygen contained in the sample water when the sample water passes through the deoxidizing resin column 2, wherein the content of the dissolved oxygen approaches to 0;
s4, injecting a proper amount of hydrazine solution into the system through a standard solution peristaltic pump 6, wherein the hydrazine solution can further eliminate the dissolved oxygen content in sample water, and the dissolved oxygen content in the sample is further reduced by observing the indication value of a to-be-detected dissolved oxygen meter;
s5, removing anions and cations in the sample water when the sample water passes through the mixed bed resin column unit;
s6, filling a barium chloride standard solution with the concentration of C1 in the standard solution bottle 7, and fully blowing air into the standard solution bottle 7 through an air pump 8 to enable the dissolved oxygen content of the barium chloride standard solution in the standard solution bottle 7 to be in a saturated state, wherein the concentration of the dissolved oxygen is C2;
s7, injecting the barium chloride standard solution in the standard solution bottle 7 into the mixing chamber 5 through the standard solution peristaltic pump 6 at a certain rotating speed, wherein the injection flow rate is L2;
s8, injecting a barium chloride standard solution into a circulating sample water system, mixing the sample water in the mixing chamber 5, diluting the sample water, diluting the barium chloride standard solution with saturated solution oxygen in equal proportion, and enabling the ratio of the barium chloride to the dissolved oxygen content in the sample to be the same as the ratio of the barium chloride to the dissolved oxygen content in the standard solution;
s9, the sample water in the mixing chamber flows through an electric conductivity meter 9, the electric conductivity meter 9 measures an electric conductivity value of the sample water, the electric conductivity value is closely related to the concentration of barium chloride in the sample water, the concentration C3=f (Con) of the barium chloride in the sample water in the mixing chamber can be calculated, f (Con) is a mathematical model of conversion relation between electric conductivity and the concentration of the barium chloride, and the concentration of the barium chloride in the sample water in the mixing chamber 5 and the concentration C4 of the dissolved oxygen in the sample water can be calculated because the concentration of the barium chloride in the standard solution and the saturated dissolved oxygen are diluted in equal proportion synchronously;
s10, taking the dissolved oxygen concentration C4 of the sample in the mixing chamber as a standard value, and checking and calibrating the dissolved oxygen meter 10 to be tested when the sample water in the mixing chamber flows through the dissolved oxygen meter.
In step S9, f (Con) = 0.743 ×con, where Con is a sample water conductivity value measured by the conductivity meter.
In addition, it should be expanded that the similar method of the invention can be used for measuring trace sodium, potassium, calcium, magnesium, iron, copper and other ions.
The invention adopts an deoxidization resin column and a mixed bed resin column unit to remove dissolved oxygen and anions and cations from sample water, so that the sample water is close to theoretical pure water, a barium chloride standard solution is injected into a circulating sample water system and is mixed with the sample water in a mixing chamber for dilution, as the barium chloride standard solution is diluted with saturated solution oxygen in equal proportion, the ratio of the content of barium chloride to the content of dissolved oxygen in the sample is the same as the ratio of the content of barium chloride to the content of dissolved oxygen in the standard solution, the conductivity value of the sample water is measured through a conductivity meter, the concentration of barium chloride in the sample water in the mixing chamber can be calculated, and as the barium chloride concentration of the barium chloride standard solution is diluted with saturated dissolved oxygen in equal proportion synchronously, the concentration of dissolved oxygen in the sample water in the mixing chamber can be calculated, the sample dissolved oxygen concentration in the mixing chamber is taken as a standard value, and the sample water in the mixing chamber can be checked and calibrated when flowing through a dissolved oxygen meter to be tested;
the invention carries out ultrapure water treatment on sample water, adopts the barium chloride standard solution as a chemical reagent, has convenient and stable operation, and has low input cost and high detection precision.
The foregoing has shown and described the basic principles, principal features and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made therein without departing from the spirit and scope of the invention, which is defined by the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (6)
1. The operation method of the on-line calibration micro dissolved oxygen monitor is based on a device for calibrating the micro dissolved oxygen monitor on line, and is characterized by comprising a sample water supply mechanism, a pure water purification system connected with the sample water supply mechanism, a mixing chamber connected with the pure water purification system, a standard solution supply mechanism connected with the mixing chamber, wherein the mixing chamber is connected with the sample water supply mechanism through a circulating check assembly, the sample water supply mechanism comprises an intermediate water tank, a reflux valve and a circulating pump, and the sample water is stored in the intermediate water tank;
the pure water purification system comprises an deoxidization resin column connected with the output end of the circulating pump and a mixed bed resin column unit connected with the deoxidization resin column, and the output end of the mixed bed resin column unit is connected with the mixing chamber;
the circulating check assembly comprises a circulating pipe connected with the mixing chamber and the middle water tank, and an electric conductivity meter and a dissolved oxygen meter to be tested which are arranged on the circulating pipe;
the operation method comprises the following steps:
s1, high-purity water is used as sample water to be stored in an intermediate water tank, the whole circulating water system is closed, air in the system is replaced by pure nitrogen, then the nitrogen is replaced by the high-purity water, and finally the whole system is guaranteed to be full of water;
s2, adjusting the opening of a reflux valve to enable the flow rate of circulating sample water of the system to reach L1;
s3, absorbing dissolved oxygen contained in the sample water when the sample water passes through the deoxidizing resin column, wherein the content of the dissolved oxygen approaches to 0;
s4, injecting a proper amount of hydrazine solution into the system through a peristaltic pump of the standard solution, wherein the hydrazine solution can further eliminate the dissolved oxygen content in the sample water, and further reduce the dissolved oxygen content in the sample by observing the indication value of a dissolved oxygen meter to be detected;
s5, removing anions and cations in the sample water when the sample water passes through the mixed bed resin column unit;
s6, filling a barium chloride standard solution with the concentration of C1 into the standard solution bottle, and fully blowing air into the standard solution bottle through an air pump to enable the dissolved oxygen content of the barium chloride standard solution in the standard solution bottle to be in a saturated state, wherein the concentration of the dissolved oxygen is C2;
s7, injecting the barium chloride standard solution in the standard solution bottle into the mixing chamber through the standard solution peristaltic pump at a certain rotating speed, wherein the injection flow rate is L2;
s8, after the barium chloride standard solution is injected into a circulating sample water system, mixing the sample water in a mixing chamber, diluting the sample water, diluting the barium chloride standard solution and saturated solution oxygen in equal proportion, wherein the ratio of the barium chloride to the dissolved oxygen content in the sample is the same as the ratio of the barium chloride to the dissolved oxygen content in the standard solution;
s9, the sample water in the mixing chamber flows through an electric conductivity meter, the electric conductivity meter measures the electric conductivity value of the sample water, the electric conductivity value is closely related to the concentration of barium chloride in the sample water, the concentration C3=f (Con) of the barium chloride in the sample water in the mixing chamber can be calculated, f (Con) is a mathematical model of conversion relation between electric conductivity and the concentration of the barium chloride, and the concentration of the barium chloride in the sample water in the mixing chamber and the concentration C4 of the dissolved oxygen in the sample can be calculated because the concentration of the barium chloride in the standard solution of the barium chloride and the saturated dissolved oxygen are diluted in equal proportion synchronously;
s10, taking the dissolved oxygen concentration C4 of the sample in the mixing chamber as a standard value, and checking and calibrating the dissolved oxygen meter to be tested when the sample water in the mixing chamber flows through the dissolved oxygen meter.
2. The method according to claim 1, wherein in step S9, f (Con) = 0.743 ×con, wherein Con is a sample water conductivity value measured by a conductivity meter.
3. The operation method of the on-line calibration micro dissolved oxygen monitor according to claim 1, wherein the standard solution supply mechanism comprises a standard solution bottle, an air pump connected with the standard solution bottle, the standard solution bottle is connected with the mixing chamber through a standard solution peristaltic pump, standard solution containing barium chloride and saturated solution oxygen is stored in the standard solution bottle, and an air sand head connected with the air pump is arranged in the standard solution bottle.
4. An operating method for an on-line calibrated micro dissolved oxygen monitor as claimed in claim 3, wherein the circulation pipe is provided with a flow meter for monitoring the flow rate of the circulating sample water in the system.
5. The method of operating an on-line calibrated micro dissolved oxygen monitor of claim 3, wherein the mixed bed resin column unit comprises a first mixed bed resin column and a second mixed bed resin column, the mixed bed resin column unit being used for removing anions and cations in the system sample water.
6. The method for operating an on-line calibration micro dissolved oxygen monitor according to claim 3, wherein the deoxidizing resin column is used for removing dissolved oxygen in system sample water, so that the content of the dissolved oxygen in the system sample water is approximately 0.
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| CN113567514A (en) * | 2021-07-20 | 2021-10-29 | 国网山东省电力公司电力科学研究院 | Intelligent sodium ion analyzer device with full-automatic online calibration function and online calibration method |
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