Device and method for preparing oxygen-free ultrapure water standard substance
Through the preparation device of standard substances for oxygen-free ultrapure water, the EDI pure water module and the A-EDI deoxygenation module remove dissolved oxygen and sodium sulfite from the water, solving the problem of long time and low accuracy of the traditional dissolved oxygen table zero-point calibration method. , achieving faster and more accurate zero point calibration.
Patent Information
- Application Number
- CN202411781200.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-05
- Publication Date
- 2025-02-14
AI Technical Summary
The traditional zero-point calibration method of dissolved oxygen meters has problems such as long calibration time, significant differences in the salt content of the calibration process and the actual working medium, and offline calibration is greatly affected by air oxygen, resulting in high zero points and reducing the accuracy of the instrument.
A standard preparation device for oxygen-free ultrapure water substances is designed, including a first EDI pure water assembly, a trace sodium sulfite dosing assembly, an A-EDI deoxygenation assembly and a second EDI pure water assembly. Through the continuous operation of these components, the removal of Dissolved oxygen and sodium sulfite in water form standard substances of oxygen-free ultrapure water, which are used for zero-point calibration of dissolved oxygen instruments.
It significantly reduces calibration time, improves the accuracy of zero-point calibration, makes the measured value closer to the actual water sample, and reduces the impact of impurities ions in the water on the measurement results.
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Figure CN119430559A_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to the field of standard substance preparation, and relates to a device and method for preparing an oxygen-free ultrapure water standard substance. Background Art
[0002] Monitoring dissolved oxygen in water vapor plays an important role in the corrosion of thermal systems in power plants. Accurately measuring the concentration of dissolved oxygen in water vapor systems is of great significance to the safe operation of generator sets. The working error of online dissolved oxygen meters in power plants must comply with the provisions of the power industry standard DL / T 677-2018 "Testing Procedures for Online Chemical Instruments in Power Plants", and the accuracy of its zero point has a great influence on the working error.
[0003] The traditional zero-point calibration method of dissolved oxygen meters uses a supersaturated sodium sulfite solution as the zero oxygen standard solution for calibration. This method has the following problems: the calibration time is long, the salt content of the calibration process is significantly different from that of the actual working medium, and the offline calibration is greatly affected by air oxygen. This method can easily cause the zero point to be too high, reduce the accuracy of the instrument's zero point, and cause the measured value to be too low. Summary of the invention
[0004] The purpose of the present invention is to overcome the shortcomings of the above-mentioned prior art and provide a device and method for preparing an oxygen-free ultrapure water standard substance, which can avoid the problem of the difference between the salt content of the existing supersaturated sodium sulfite solution and the actual measured object, as well as the problems of long calibration time and low zero point accuracy.
[0005] To achieve the above-mentioned purpose, the anaerobic ultrapure water standard substance preparation device described in the present invention includes a first EDI pure water component, a trace sodium sulfite dosing component, an A-EDI deoxygenation component and a second EDI pure water component, wherein the inlet of the first EDI pure water component is connected to the water inlet pipe, the outlet of the first EDI pure water component is connected to the inlet of the trace sodium sulfite dosing component, the outlet of the trace sodium sulfite dosing component is connected to the inlet of the A-EDI deoxygenation component, and the outlet of the A-EDI deoxygenation component is connected to the inlet of the second EDI pure water component.
[0006] The device for preparing standard substance of oxygen-free ultrapure water of the present invention is further improved in that:
[0007] Furthermore, the A-EDI deoxygenation component includes a constant current power supply, an anode, a cathode and an anion exchange membrane, wherein the anode, the anion exchange membrane and the cathode are distributed in sequence, and the constant current power supply is connected to the anode and the cathode, wherein the anion exchange membrane and the cathode are filled with reducing ion exchange resin.
[0008] Furthermore, the reducing ion exchange resin is R-SO3 resin.
[0009] Furthermore, it also includes a dissolved oxygen meter, which is connected to the outlet of the second EDI pure water component.
[0010] The method for preparing an oxygen-free ultrapure water standard substance of the present invention comprises the following steps:
[0011] The main steam sampling water passes through the first EDI pure water component, the trace sodium sulfite dosing component, the A-EDI deoxygenation component and the second EDI pure water component in sequence, and then enters the dissolved oxygen meter for zero point calibration of the dissolved oxygen meter.
[0012] The method for preparing the oxygen-free ultrapure water standard substance of the present invention is further improved in that:
[0013] Furthermore, the A-EDI deoxygenation component includes a constant current power supply, an anode, a cathode and an anion exchange membrane, wherein the anode, the anion exchange membrane and the cathode are distributed in sequence, and the constant current power supply is connected to the anode and the cathode, wherein the anion exchange membrane and the cathode are filled with reducing ion exchange resin.
[0014] Furthermore, it also includes a dissolved oxygen meter, which is connected to the outlet of the second EDI pure water component.
[0015] Furthermore, the reducing ion exchange resin is R-SO3 resin.
[0016] Further, the method specifically includes the following steps:
[0017] The main steam sampling water enters the first EDI pure water component to remove impurity ions in the water. The purified main steam sampling water output by the first EDI pure water component enters the trace sodium sulfite dosing component, and is mixed with the sodium sulfite solution output by the trace sodium sulfite metering pump in the trace sodium sulfite dosing component, so that the dissolved oxygen in the main steam sampling water reacts with the sodium sulfite and is removed for the first time. Then, the main steam sampling water enters the A-EDI deoxidation component. In the A-EDI deoxidation component, the main steam sampling water flows through the R-SO3 resin filled in the A-EDI deoxidation component. During this process, the sodium sulfite in the main steam sampling water reacts with the dissolved oxygen in the water, and the R-SO3 resin reacts with the dissolved oxygen in the water, and keeps exchanging with the R-SO3 resin and is continuously regenerated. At the same time, the dissolved oxygen absorbs oxygen under the action of the cathode to generate OH- ions, further removing the dissolved oxygen in the water; the main steam sampling water output by the A-EDI deoxygenation component enters the second EDI pure water component to remove the sodium sulfite in the water to form an oxygen-free ultrapure water standard substance, and then enters the dissolved oxygen meter for zero point calibration of the dissolved oxygen meter.
[0018] Furthermore, the impurity ions include trace amounts of sodium ions, chloride ions and chromate ions.
[0019] The present invention has the following beneficial effects:
[0020] The oxygen-free ultrapure water standard substance preparation device and method described in the present invention, during specific operation, removes impurity ions in water through the first EDI pure water component, allows the dissolved oxygen in the main steam sampling water to react with sodium sulfite and be removed for the first time through the first EDI pure water component, further removes the dissolved oxygen in the water through the A-EDI deoxygenation component, and removes the sodium sulfite in the water through the second EDI pure water component to form an oxygen-free ultrapure water standard substance, thereby avoiding the problem of the difference between the salt content of the existing supersaturated sodium sulfite solution and the actual measured object, the long calibration time and the low accuracy of the zero point, significantly reducing the calibration time, being close to the actual measured water quality salt content of the measured water sample, and reducing the influence of impurity ions in the water on the measurement result; when calibrating the dissolved oxygen meter, the three-way valve is switched to avoid the dissolved oxygen sensor from contacting with the air, thereby improving the accuracy of the zero point calibration. BRIEF DESCRIPTION OF THE DRAWINGS
[0021] The accompanying drawings constituting a part of the present invention are used to provide a further understanding of the present invention. The exemplary embodiments of the present invention and their descriptions are used to explain the present invention and do not constitute an improper limitation of the present invention. In the accompanying drawings:
[0022] Figure 1 It is a structural diagram of the present invention;
[0023] Figure 2 This is a structural diagram of the A-EDI deoxidation component.
[0024] Among them, 1 is the first EDI pure water component, 2 is the trace sodium sulfite dosing component, 3 is the A-EDI deoxygenation component, 4 is the second EDI pure water component, 41 is the anode, 42 is the cathode, 43 is the anion exchange membrane, and 44 is the reducing ion exchange resin. DETAILED DESCRIPTION
[0025] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
[0026] In the description of the present invention, it should be understood that the terms “include” and “comprises” indicate the presence of described features, wholes, steps, operations, elements and / or components, but do not exclude the presence or addition of one or more other features, wholes, steps, operations, elements, components and / or collections thereof.
[0027] It should also be understood that the terms used in the present specification are only for the purpose of describing specific embodiments and are not intended to limit the present invention. As used in the present specification and the appended claims, unless the context clearly indicates otherwise, the singular forms "a", "an" and "the" are intended to include plural forms.
[0028] It should be further understood that the term "and / or" used in the present specification and the appended claims refers to any combination of one or more of the associated listed items and all possible combinations, and includes these combinations. For example, A and / or B can represent: A exists alone, A and B exist at the same time, and B exists alone. In addition, the character " / " in the present invention generally indicates that the associated objects are in an "or" relationship.
[0029] It should be understood that, although the terms first, second, third, etc. may be used to describe preset ranges, etc. in the embodiments of the present invention, these preset ranges should not be limited to these terms. These terms are only used to distinguish preset ranges from each other. For example, without departing from the scope of the embodiments of the present invention, the first preset range may also be referred to as the second preset range, and similarly, the second preset range may also be referred to as the first preset range.
[0030] The word "if" as used herein may be interpreted as "at the time of" or "when" or "in response to determining" or "in response to detecting", depending on the context. Similarly, the phrases "if it is determined" or "if (stated condition or event) is detected" may be interpreted as "when it is determined" or "in response to determining" or "when detecting (stated condition or event)" or "in response to detecting (stated condition or event)", depending on the context.
[0031] In order to make the purpose, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are part of the embodiments of the present invention, rather than all of the embodiments. The components of the embodiments of the present invention described and shown in the drawings here can usually be arranged and designed in various different configurations. Therefore, the following detailed description of the embodiments of the present invention provided in the drawings is not intended to limit the scope of the claimed invention, but merely represents selected embodiments of the present invention. Based on the embodiments in the present invention, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the present invention.
[0032] Various structural schematic diagrams of the embodiments disclosed in the present invention are shown in the accompanying drawings. These figures are not drawn to scale, and some details are magnified and some details may be omitted for the purpose of clear expression. The shapes of various regions and layers shown in the figures and the relative sizes and positional relationships therebetween are only exemplary, and may deviate in practice due to manufacturing tolerances or technical limitations, and those skilled in the art may additionally design regions / layers with different shapes, sizes, and relative positions according to actual needs.
[0033] As is known, the working principle of EDI water treatment is mainly based on electrodialysis and ion exchange technology, which realizes deep purification of water through the action of electric field and the selective permeability of ion exchange membrane. Electrodialysis process: Under the action of DC electric field, cations and anions in water pass through cation exchange membrane and anion exchange membrane respectively, thereby realizing selective migration of ions. This process helps to remove soluble salts in water. Ion exchange process: In the EDI unit, ion exchange resins are filled, which can exchange with ions in water, further remove impurity ions in water and improve the purity of water. Electrochemical regeneration process: Under the action of electric field, water molecules are electrolyzed to produce hydrogen ions and hydroxide ions, which regenerate the resin so that the resin can be used continuously without the use of chemical agents. The whole process is a continuous automated operation, which does not require shutdown for chemical regeneration, thereby improving efficiency and reducing environmental pollution. EDI technology is widely used in many fields such as electronics, medicine, and chemical industry to provide high-quality ultrapure water.
[0034] Embodiment 1
[0035] refer to Figure 1 The anaerobic ultrapure water standard substance preparation device described in the present invention includes a first EDI pure water component 1, a trace sodium sulfite dosing component 2, an A-EDI deoxygenation component 3 and a second EDI pure water component 4, wherein the inlet of the first EDI pure water component 1 is connected to the water inlet pipe, the outlet of the first EDI pure water component 1 is connected to the inlet of the trace sodium sulfite dosing component 2, the outlet of the trace sodium sulfite dosing component 2 is connected to the inlet of the A-EDI deoxygenation component 3, and the outlet of the A-EDI deoxygenation component 3 is connected to the inlet of the second EDI pure water component 4.
[0036] Embodiment 2
[0037] refer to Figure 1 and Figure 2The anaerobic ultrapure water standard substance preparation device described in the present invention includes a first EDI pure water component 1, a trace sodium sulfite dosing component 2, an A-EDI deoxygenation component 3 and a second EDI pure water component 4, wherein the inlet of the first EDI pure water component 1 is connected to the water inlet pipe, the outlet of the first EDI pure water component 1 is connected to the inlet of the trace sodium sulfite dosing component 2, the outlet of the trace sodium sulfite dosing component 2 is connected to the inlet of the A-EDI deoxygenation component 3, and the outlet of the A-EDI deoxygenation component 3 is connected to the inlet of the second EDI pure water component 4.
[0038] As an embodiment of the present invention, the A-EDI deoxygenation component 3 includes a constant current power supply, an anode 41, a cathode 42 and an anion exchange membrane 43, wherein the anode 41, the anion exchange membrane 43 and the cathode 42 are distributed in sequence, and the constant current power supply is connected to the anode 41 and the cathode 42, wherein a reducing ion exchange resin 44 is filled between the anion exchange membrane 43 and the cathode 42.
[0039] As an embodiment of the present invention, the reducing ion exchange resin 44 is R-SO3 resin.
[0040] Embodiment 3
[0041] refer to Figure 1 The present embodiment discloses a method for preparing an anaerobic ultrapure water standard substance, which is implemented based on the anaerobic ultrapure water standard substance preparation device, which includes a first EDI pure water component 1, a trace sodium sulfite dosing component 2, an A-EDI deoxygenation component 3 and a second EDI pure water component 4, wherein the inlet of the first EDI pure water component 1 is connected to the water inlet pipe, the outlet of the first EDI pure water component 1 is connected to the inlet of the trace sodium sulfite dosing component 2, the outlet of the trace sodium sulfite dosing component 2 is connected to the inlet of the A-EDI deoxygenation component 3, and the outlet of the A-EDI deoxygenation component 3 is connected to the inlet of the second EDI pure water component 4.
[0042] Specifically, the method for preparing the oxygen-free ultrapure water standard substance comprises the following steps:
[0043] The main steam sampling water passes through the first EDI pure water component 1, the trace sodium sulfite dosing component 2, the A-EDI deoxygenation component 3 and the second EDI pure water component 4 in sequence, and then enters the dissolved oxygen meter for zero point calibration of the dissolved oxygen meter.
[0044] Embodiment 4
[0045] refer to Figure 1 and Figure 2The present embodiment discloses a method for preparing an anaerobic ultrapure water standard substance, which is implemented based on the anaerobic ultrapure water standard substance preparation device, which includes a first EDI pure water component 1, a trace sodium sulfite dosing component 2, an A-EDI deoxygenation component 3 and a second EDI pure water component 4, wherein the inlet of the first EDI pure water component 1 is connected to the water inlet pipe, the outlet of the first EDI pure water component 1 is connected to the inlet of the trace sodium sulfite dosing component 2, and the outlet of the trace sodium sulfite dosing component 2 is connected to the inlet of the trace sodium sulfite dosing component 2. It is connected to the inlet of the A-EDI deoxygenation component 3, and the outlet of the A-EDI deoxygenation component 3 is connected to the inlet of the second EDI pure water component 4. Specifically, the A-EDI deoxygenation component 3 includes a constant current power supply, an anode 41, a cathode 42 and an anion exchange membrane 43, wherein the anode 41, the anion exchange membrane 43 and the cathode 42 are distributed in sequence, and the constant current power supply is connected to the anode 41 and the cathode 42, wherein a reducing ion exchange resin 44 is filled between the anion exchange membrane 43 and the cathode 42; the reducing ion exchange resin 44 is R-SO3 resin.
[0046] Specifically, the method for preparing the oxygen-free ultrapure water standard substance comprises the following steps:
[0047] The main steam sampling water enters the first EDI pure water component 1 to remove impurity ions in the water. The purified main steam sampling water output by the first EDI pure water component 1 enters the trace sodium sulfite dosing component 2, and in the trace sodium sulfite dosing component 2, it is mixed with the sodium sulfite solution output by the trace sodium sulfite metering pump, so that the dissolved oxygen in the main steam sampling water reacts with the sodium sulfite and is removed for the first time, and then enters the A-EDI deoxidation component 3. In the A-EDI deoxidation component 3, the main steam sampling water flows through the device The R-SO3 resin is filled in the A-EDI deoxygenation component 3. During this process, the sodium sulfite in the main steam sampling water reacts with the dissolved oxygen in the water, and the R-SO3 resin reacts with the dissolved oxygen in the water, and keeps exchanging with the R-SO3 resin and is continuously regenerated. At the same time, the dissolved oxygen reacts with the remaining dissolved oxygen in the water under the action of the cathode 42 to generate OH- ions, further removing the dissolved oxygen in the water; the main steam sampling water output by the A-EDI deoxygenation component 3 enters the second EDI pure water component 4.
[0048] Embodiment 5
[0049] Taking a thermal power plant as an example, the apparatus and method for preparing an oxygen-free ultrapure water standard substance of the present invention are explained.
[0050] The oxygen-free ultrapure water standard substance preparation device is installed on the instrument panel of the thermal power plant. The main steam sampling water enters the first EDI pure water component 1 to remove impurity ions in the water. The impurity ions include trace amounts of sodium ions, chloride ions and chromate ions, thereby reducing the influence of impurity ions on the dissolved oxygen measurement result; the purified main steam sampling water output by the first EDI pure water component 1 enters the trace sodium sulfite dosing component 2, and is mixed with the sodium sulfite solution output by the trace sodium sulfite metering pump in the trace sodium sulfite dosing component 2, so that the dissolved oxygen in the main steam sampling water reacts with the sodium sulfite and is removed for the first time, and then enters the A-EDI deoxygenation component 3, and then in the A-EDI In the deoxygenation component 3, the main steam sampling water flows through the R-SO3 resin loaded in the A-EDI deoxygenation component 3. During this process, the sodium sulfite in the main steam sampling water reacts with the dissolved oxygen in the water. At the same time, the R-SO3 resin reacts with the dissolved oxygen in the water and keeps exchanging with the R-SO3 resin to be continuously regenerated. At the same time, the dissolved oxygen reacts with the remaining dissolved oxygen in the water under the action of the cathode 42 to generate OH- ions, thereby further removing the dissolved oxygen in the water. The main steam sampling water output by the A-EDI deoxygenation component 3 enters the second EDI pure water component 4 to remove impurity ions such as sodium sulfite in the water to form an oxygen-free ultrapure water standard substance for zero point calibration of the dissolved oxygen meter.
[0051] Those skilled in the art will readily appreciate other embodiments of the present invention after considering the specification and disclosure of the invention. This application is intended to cover any variations, uses or adaptations of the present invention that follow the general principles of the present invention and include common knowledge or customary techniques in the art that are not disclosed by the present invention. The specification and examples are to be considered exemplary only, and the true scope and spirit of the present invention are indicated by the following claims.
[0052] It should be understood that the present invention is not limited to the exact construction that has been described above and shown in the drawings and that various modifications and changes may be made without departing from the scope thereof. The scope of the present invention is limited only by the appended claims.
[0053] The above description is only a preferred embodiment of the present invention and does not limit the present invention in any way. Any simple modification, change and equivalent structural change made to the above embodiment based on the technical essence of the present invention still falls within the protection scope of the technical solution of the present invention.
Claims
1. An oxygen-free ultrapure water standard substance preparation device, characterized in that: The invention comprises a first EDI pure water component (1), a trace sodium sulfite dosing component (2), an A-EDI deoxygenation component (3) and a second EDI pure water component (4), wherein the inlet of the first EDI pure water component (1) is connected to a water inlet pipe, the outlet of the first EDI pure water component (1) is connected to the inlet of the trace sodium sulfite dosing component (2), the outlet of the trace sodium sulfite dosing component (2) is connected to the inlet of the A-EDI deoxygenation component (3), and the outlet of the A-EDI deoxygenation component (3) is connected to the inlet of the second EDI pure water component (4).
2. The oxygen-free ultrapure water standard substance preparation device according to claim 1, characterized in that: The A-EDI deoxidation component (3) comprises a constant current power supply, an anode (41), a cathode (42) and an anion exchange membrane (43), wherein the anode (41), the anion exchange membrane (43) and the cathode (42) are arranged in sequence, and the constant current power supply is connected to the anode (41) and the cathode (42), wherein a reducing ion exchange resin (44) is filled between the anion exchange membrane (43) and the cathode (42).
3. The oxygen-free ultrapure water standard substance preparation device according to claim 1, characterized in that: The reducing ion exchange resin (44) is R-SO3 resin.
4. The oxygen-free ultrapure water standard substance preparation device according to claim 1, characterized in that: It also includes a dissolved oxygen meter, which is connected to the outlet of the second EDI pure water component (4).
5. A method for preparing an oxygen-free ultrapure water standard substance, characterized in that: The device for preparing an oxygen-free ultrapure water standard substance according to claim 1 comprises the following steps: The main steam sampling water passes through the first EDI pure water component (1), the trace sodium sulfite dosing component (2), the A-EDI deoxygenation component (3) and the second EDI pure water component (4) in sequence, and then enters the dissolved oxygen meter for zero point calibration of the dissolved oxygen meter.
6. The method for preparing an oxygen-free ultrapure water standard substance according to claim 5, characterized in that: The A-EDI deoxidation component (3) comprises a constant current power supply, an anode (41), a cathode (42) and an anion exchange membrane (43), wherein the anode (41), the anion exchange membrane (43) and the cathode (42) are arranged in sequence, and the constant current power supply is connected to the anode (41) and the cathode (42), wherein a reducing ion exchange resin (44) is filled between the anion exchange membrane (43) and the cathode (42).
7. The method for preparing an oxygen-free ultrapure water standard substance according to claim 6, characterized in that: It also includes a dissolved oxygen meter, which is connected to the outlet of the second EDI pure water component (4).
8. The oxygen-free ultrapure water standard substance preparation device according to claim 7, characterized in that: The reducing ion exchange resin (44) is R-SO3 resin.
9. The method for preparing an oxygen-free ultrapure water standard substance according to claim 8, characterized in that: The specific steps include: The main steam sampling water enters the first EDI pure water component (1) to remove impurity ions in the water. The purified main steam sampling water outputted from the first EDI pure water component (1) enters the trace sodium sulfite dosing component (2) and is mixed with the sodium sulfite solution outputted from the trace sodium sulfite metering pump in the trace sodium sulfite dosing component (2) so that the dissolved oxygen in the main steam sampling water reacts with the sodium sulfite and is removed for the first time. The main steam sampling water then enters the A-EDI deoxidation component (3). In the A-EDI deoxidation component (3), the main steam sampling water flows through the R- SO3 resin, during this process, the sodium sulfite in the main steam sampling water reacts with the dissolved oxygen in the water, and at the same time, the R-SO3 resin reacts with the dissolved oxygen in the water, and keeps exchanging with the R-SO3 resin and is continuously regenerated. At the same time, the dissolved oxygen undergoes an oxygen absorption reaction under the action of the cathode (42) to generate OH- ions, further removing the dissolved oxygen in the water; the main steam sampling water output by the A-EDI deoxygenation component (3) enters the second EDI pure water component (4), removes the sodium sulfite in the water, and forms an oxygen-free ultrapure water standard substance, and then enters the dissolved oxygen meter for zero point calibration of the dissolved oxygen meter.
10. The method for preparing an oxygen-free ultrapure water standard substance according to claim 9, characterized in that: The impurity ions include trace amounts of sodium ions, chloride ions and chromate ions.
Citation Information
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