阅读说明：本技术 一种臭氧分析仪的校准方法及装置 (Method and device for calibrating ozone analyzer ) 是由 李学辉 唐巍飚 陈希尧 钟义林 郑波 于 2020-08-06 设计创作，主要内容包括：本发明属于仪器校准领域,公开了一种臭氧分析仪的校准方法,实施步骤为：首先将臭氧通入水中得到初始臭氧水,接着将初始臭氧水静置预定静置时间后得到校准臭氧水,然后再获取校准臭氧水的标准浓度值,然后用臭氧分析仪读取校准臭氧水的实测浓度值,最终根据实测浓度值和标准浓度值校准臭氧分析仪,通过实施本方法,能够彻底消除校准臭氧水中气泡,从而对臭氧分析仪进行准确的校准,本发明还公开了一种臭氧分析仪校准装置,用于配合实施本发明的臭氧分析仪的校准方法,使得本发明的臭氧分析仪的校准方法具有很好的可操作性。(The invention belongs to the field of instrument calibration, and discloses a calibration method of an ozone analyzer, which comprises the following implementation steps: the method comprises the steps of firstly introducing ozone into water to obtain initial ozone water, then standing the initial ozone water for a preset standing time to obtain calibration ozone water, then obtaining a standard concentration value of the calibration ozone water, then reading an actual measurement concentration value of the calibration ozone water by using an ozone analyzer, and finally calibrating the ozone analyzer according to the actual measurement concentration value and the standard concentration value.)

1. A calibration method of an ozone analyzer, characterized by comprising the steps of:

step S1: introducing ozone into water to obtain initial ozone water with initial concentration;

step S2: standing the initial ozone water for a preset standing time to obtain calibrated ozone water, wherein the preset standing time is a time from '0' of the concentration of the ozone in the attenuation characteristic curve of the water to the starting point of an ozone concentration stable section;

step S3: acquiring a standard concentration value of the calibration ozone water;

step S4: reading the actually measured concentration value of the calibration ozone water by using an ozone analyzer;

step S5: calibrating the ozone analyzer according to the measured concentration value and the standard concentration value.

2. The calibration method for an ozone analyzer according to claim 1, characterized in that:

wherein the standard concentration value is 75% to 90% of the initial concentration value.

3. The calibration method for an ozone analyzer according to claim 1, characterized in that:

in step S1, the method includes the following substeps:

step S1-1: obtaining ozone by drying the treated gas source;

step S1-2: introducing the ozone into water;

step S1-3: and stirring the ozone and the water for a preset stirring time to obtain the initial ozone water.

4. The calibration method for an ozone analyzer according to claim 3, wherein:

wherein the predetermined standing time is 30 minutes.

5. The calibration method for an ozone analyzer according to claim 1, characterized in that:

wherein, in step S2, the ambient temperature of the initial ozonated water when it is left to stand is a predetermined rest temperature.

6. The calibration method for an ozone analyzer according to claim 5, wherein:

wherein the predetermined rest temperature range is 0 ℃ to 50 ℃.

7. The calibration method for an ozone analyzer according to claim 1, characterized in that:

wherein the ozone in a free state generated in the steps S1 and S2 is subjected to a drying process, thereby adsorbing and decomposing the ozone.

8. An ozone analyzer calibration device for performing the method for calibrating an ozone analyzer according to any one of claims 1 to 7, comprising:

an ozone generator for generating ozone; and

a liquid storage chamber with water inside for forming and containing the calibration ozone water, the liquid storage chamber is provided with an air inlet channel and a liquid outlet channel, the air inlet channel is communicated with the ozone generator, the liquid outlet channel is provided with a first liquid outlet and at least one second liquid outlet, the second liquid outlet is used for being communicated with the ozone analyzer,

a standard concentration reading part connected with the first liquid outlet and used for reading the standard concentration value,

wherein, a drying medium is arranged in the ozone generator and is used for drying the gas source of the ozone,

the liquid storage chamber comprises a stirring piece for stirring the ozone and the water,

the surface of the liquid storage chamber is provided with a waste gas outlet and a thermostatic bath,

the waste gas outlet is communicated with an external drying device and is used for drying the ozone in a free state,

the constant temperature groove is used for enabling the temperature of the liquid storage chamber to be the preset standing temperature.

9. The ozone analyzer calibration device according to claim 8, wherein:

wherein the ozone analyzer comprises an online ozone analyzer,

the online ozone analyzer comprises a flow cell,

and the inlet of the flow cell is communicated with the second liquid outlet and is used for accommodating the calibration ozone water.

10. The ozone analyzer calibration device according to claim 8, wherein:

wherein, the liquid storage chamber also comprises an aeration disc which is communicated with the ozone generator through the air inlet channel, and the aeration disc is used for introducing the ozone into the water in the liquid storage chamber.

Technical Field

The invention belongs to the field of instrument calibration, and particularly relates to a calibration method and a calibration device for an ozone analyzer.

Background

Ozone itself has a strong oxidizing property, and therefore has a strong sterilizing power. And ozone is unstable in water, a large amount of ozone is quite easy to be digested automatically to form ozone water, and the ozone water sterilization is a safe and reliable method and is widely applied to the fields of medical treatment, pharmacy, food processing industry, aquaculture, cosmetics, daily life and the like. However, the trace ozone residue in water is closely related to the safety of medicines and food. If the water sterilized by ozone is regulated, the concentration value of the water must be reduced to be below 0.50mg/L for use. The food and drug industry is more severe, the value of the product is required to be below 0.01mg/L, and the product can be packaged and delivered. Organic by-products generated by trace ozone in water are represented by aldehydes (formaldehyde is the most common), inorganic by-products are represented by bromate, and the two substances are classified as possible carcinogens by the international cancer research organization (IRAC). Therefore, related industries make different regulations and strictly control the residual quantity of ozone in water. Along with ozone disinfection application field is more and more extensive, the amount of residual of aquatic ozone has also been formulated in each trade simultaneously, various aquatic ozone analysis appearance on the market is used by a large amount, for making online ozone analysis appearance and portable ozone analysis appearance survey data accurate reliable, the measurement calibration work of these ozone analysis appearance equipment is imperative, and in order to guarantee the authority of calibration, ozone analysis appearance equipment should regularly be sent to specially to its calibration institution department that carries out the accurate calibration.

At present, the method for calibrating ozone analyzer equipment by a calibration mechanism is as follows: firstly, mixing an ozone generator and externally introduced water through a gas-liquid mixing pump to obtain standard ozone water, then continuously inputting the standard ozone water into a calibration system containing ozone analyzer equipment from the gas-liquid mixing pump, and finally calibrating the ozone analyzer equipment through the standard ozone water.

However, after the calibration mechanism uses the method to accurately calibrate the ozone analyzer device, the ozone analyzer device always has inevitable errors when in use, and the reasons for the errors and how to solve the problems bothering the numerous calibration mechanisms up to now are still in an unimportant state.

Disclosure of Invention

Aiming at the defects of the prior art, the following researches are found out: the existing calibration method can cause the standard ozone water to generate a large amount of bubbles in a certain time along with the mixing process when gas and liquid are mixed,

for enterprise application, the pipeline for disinfecting by using the ozone water is longer or the ozone water storage tank is larger, and the ozone generator and the gas-liquid mixing pump are far away from the point position for monitoring the concentration of the ozone water by an enterprise, so that no bubble exists in the ozone water at the sampling point position or the monitoring point position of the portable ozone analyzer or the online ozone analyzer, and the ozone water has no influence on the test or monitoring result.

For the calibration mechanism, the gas-liquid mixing pump is very close to the calibration system, so that the standard ozone water can be input into the calibration system only in a very short time, and therefore, a large amount of bubbles are continuously generated in the standard ozone water at the moment, and the generated bubbles can be attached to the surface of a probe of the ozone analyzer device, so that the accuracy of the calibration of the ozone analyzer device, particularly an online ozone analyzer, is seriously affected, and the condition has not been noticed in the past.

The invention provides a calibration method and a calibration device for an ozone analyzer, which can thoroughly eliminate the influence of bubbles in calibration ozone water on the calibration accuracy of the ozone analyzer, thereby improving the calibration accuracy of the ozone analyzer.

In order to achieve the purpose, the invention provides the following technical scheme:

a calibration method of an ozone analyzer, characterized by comprising the steps of:

step S1: introducing ozone into water to obtain initial ozone water with initial concentration;

step S2: standing the initial ozone water for a preset standing time to obtain calibrated ozone water, wherein the preset standing time is a time from '0' of the concentration of ozone in the attenuation characteristic curve of water to the starting point of the stable ozone concentration section;

step S3: acquiring a standard concentration value of the calibrated ozone water;

step S4: reading an actually measured concentration value of the calibrated ozone water by using an ozone analyzer;

step S5: calibrating the ozone analyzer according to the measured concentration value and the standard concentration value.

Preferably, the standard concentration value is 75% to 90% of the initial concentration value.

Preferably, in step S1, the following sub-steps are included:

step S1-1: obtaining ozone by drying the treated gas source;

step S1-2: introducing ozone into water;

step S1-3: stirring the ozone and the water for a preset stirring time to obtain initial ozone water.

Preferably, the predetermined rest time is 30 minutes.

Preferably, in step S2, the ambient temperature at which the initial ozonated water is left to stand is a predetermined rest temperature.

Preferably, the predetermined rest temperature range is 0 ℃ to 50 ℃.

Preferably, the ozone in a free state generated in the steps S1 and S2 is subjected to a drying process, thereby adsorbing and decomposing the ozone.

An ozone analyzer calibration device, comprising: an ozone generator for generating ozone; and a liquid storage chamber with water inside, which is used for forming and containing the calibrated ozone water, the liquid storage chamber is provided with an air inlet channel and a liquid outlet channel, the air inlet channel is communicated with an ozone generator, the liquid outlet channel is provided with a first liquid outlet and at least one second liquid outlet, the second liquid outlet is used for being communicated with an ozone analyzer, a standard concentration reading part is connected with the first liquid outlet and used for reading a standard concentration value, wherein a drying medium is placed in the ozone generator and used for drying ozone, the liquid storage chamber comprises a stirring part and used for stirring the drying ozone and water, the surface of the liquid storage chamber is provided with a waste gas outlet and a constant temperature tank, the waste gas outlet is communicated with an external drying device and used for drying ozone in a free state, and the constant temperature tank is used for enabling the temperature of the liquid storage chamber to.

Preferably, the ozone analyzer includes online ozone analyzer, and online ozone analyzer contains the flowcell, and the import and the second liquid outlet intercommunication of flowcell for hold calibration ozone water.

Preferably, the liquid storage chamber further comprises an aeration disc, the aeration disc is communicated with the ozone generator through an air inlet channel, and the aeration disc is used for introducing ozone into the water in the liquid storage chamber.

Compared with the prior art, the invention has the beneficial effects that:

1. since the calibration ozone water of the calibration method of an ozone analyzer of the present invention is obtained after the initial ozone water is left to stand for a predetermined standing time, the calibration method of an ozone analyzer of the present invention can completely eliminate bubbles in the calibration ozone water, and thus can be used for accurately calibrating the ozone analyzer.

2. Since the standard concentration value of the calibration method of an ozone analyzer of the present invention is 75% to 90% of the initial concentration value, the calibrated ozone water of the standard concentration value can be conveniently and rapidly prepared according to such a relationship.

3. Because the gas source of ozone is dried in the calibration method of the ozone analyzer of the present invention, the efficiency of ozone generation can be improved.

4. Since the predetermined rest time of the calibration method of the ozone analyzer of the present invention is 30 minutes, and the predetermined rest time is determined based on a period of time in which the ozone water concentration derived from the ozone water decay characteristic is relatively stable, it is possible to allow bubbles in the calibration ozone water to be completely eliminated.

5. Since the ambient temperature at which the initial ozone water is left standing of the calibration method of the ozone analyzer of the present invention is the predetermined rest temperature, the relatively stable ambient temperature makes the standard concentration value relatively stable.

6. Since the calibration method of the ozone analyzer of the present invention performs the drying process on the ozone in a free state generated in steps S1 and S2 to adsorb and decompose the ozone, the present invention can perform the timely sterilization process on the ozone in a free state generating environmental pollution.

7. The calibration device for an ozone analyzer of the present invention can well perform the calibration method for an ozone analyzer of the present invention, so that the calibration method for an ozone analyzer of the present invention has good operability.

8. Because the second liquid outlet of the ozone analyzer calibration device of the invention is communicated with the inlet of the flow cell, bubble-free calibration ozone water can directly flow into the flow cell, so that the online ozone analyzer can be accurately calibrated.

Drawings

Fig. 1 is a schematic view of the steps of a calibration method of an ozone analyzer according to an embodiment of the present invention; and

fig. 2 is a schematic structural view of an ozone analyzer calibration device according to an embodiment of the present invention.

In the figure: 100. ozone analyzer calibrating device, A, deionized water injection device, B, drying device, C, waste liquid case, D, portable ozone analyzer, E, online ozone analyzer, E1, flow-through cell, E2, detection electrode, 10, ozone generator, 11, drying medium, 20, liquid storage chamber, 21, inlet channel, 22, aeration disc, 23, stirring piece, 24, liquid outlet channel, 25, thermostatic bath, 30, standard concentration reading piece.

Detailed Description

In order to make the technical means, the creation features, the achievement objects and the efficacy of the present invention easy to understand, the following examples are specifically set forth in the calibration method and the device of the ozone analyzer of the present invention with reference to the accompanying drawings, and it is to be noted that the description of the embodiments is provided to help understanding of the present invention, but not to limit the present invention.

As shown in fig. 1, the calibration method S100 of the ozone analyzer in the present embodiment includes the steps of:

step S1: and introducing ozone into water to obtain initial ozone water with initial concentration. In this example, the initial concentration ranges from 0.6mg/L to 1.8 mg/L.

The method comprises the following substeps:

step S1-1: and drying the treated gas source to obtain ozone. In this embodiment, the air source of the ozone is air, and the drying process is performed by passing the air through activated carbon.

Step S1-2: ozone is introduced into the water. In this embodiment, the water is deionized water.

Step S1-3: stirring the ozone and the water for a preset stirring time to obtain initial ozone water. In the present embodiment, the stirring is synchronized with the ozone introduction, the stirring is performed by a stirring member, and the predetermined stirring time is the same as the ozone introduction time.

The initial ozonated water obtained through step S1 is ozonated water having a stable concentration in which ozone is completely dissolved in water, and bubbles are present in the initial ozonated water.

Step S2: and standing the initial ozone water for a preset standing time to obtain the calibrated ozone water, wherein the preset standing time is a time from '0' of the concentration of the ozone in the attenuation characteristic curve of the water to the starting point of the stable ozone concentration section.

The predetermined standing time range is 30min, the environment temperature when the initial ozone water is standing is the predetermined standing temperature, and the predetermined standing temperature range is 0 ℃ to 50 ℃. In the present embodiment, the predetermined standing time range is a difference between a time point 0 and a range from a starting point to an end point of a relatively stable section of the ozone concentration in the initial ozone water, that is, a time period of a process in which the ozone concentration in the initial ozone water is from an unstable state immediately after ozone is introduced to a stable state, the unstable state means that the solubility of ozone in the initial ozone water is constantly reduced and bubbles are constantly generated, and the stable state means that the solubility of ozone in the initial ozone water is constantly unchanged and bubbles are not generated any more, and therefore, the predetermined standing temperature is preferably 20 ℃.

The ozone in a free state generated in steps S1 and S2 is subjected to a drying process, so that the ozone is adsorbed and decomposed, thereby preventing the environmental pollution by the ozone.

Step S3: and acquiring a standard concentration value of the calibrated ozone water. In the present embodiment, a standard concentration value of the calibration ozone water was obtained using an ultraviolet spectrophotometer (detection wavelength: 258 nm).

The standard concentration values are 75% to 90% initial concentration values.

Step S4: and reading the actually measured concentration value of the calibrated ozone water by using an ozone analyzer. In this embodiment, the ozone analyzer includes online ozone analyzer and portable ozone analyzer, and online ozone analyzer's theory of operation does: the detection electrode is used to detect its measured concentration value in the calibration ozone water.

Step S5: calibrating the ozone analyzer according to the measured concentration value and the standard concentration value. In this embodiment, the ozone analyzer is calibrated after the standard concentration value and the measured concentration value are displayed by the connection display instrument.

As shown in fig. 2, the ozone analyzer calibration apparatus 100 in the present embodiment is used to implement the calibration method S100 of the ozone analyzer in the present embodiment, so that the calibration method S100 of the ozone analyzer in the present embodiment has good operability, including: ozone generator 10, reservoir 20 and standard concentration reading 30.

The ozone generator 10 is used to generate ozone. The air source used by the ozone is external air. The ozone generator is internally provided with a drying medium 11.

The drying medium 11 is used for drying the ozone gas source and is activated carbon.

The liquid storage chamber 20, which has deionized water inside for forming and containing calibration ozone water, has an air inlet channel 21, an aeration plate 22, a stirring member 23, a liquid outlet channel 24 and a constant temperature tank 25, and in this embodiment, the liquid storage chamber 20 is communicated with an external deionized water injection device a for injecting deionized water into the liquid storage chamber 20.

The surface of the liquid storage chamber 20 is provided with a waste gas outlet (not shown in the drawings) and a thermostatic bath 25, and in the embodiment, the thermostatic bath 25 is sleeved on the liquid storage chamber 20.

The waste gas outlet is communicated with an external drying device B and is used for drying the ozone in a free state generated in the liquid storage chamber 20.

The constant temperature bath 25 is used to make the temperature of the liquid storage chamber 20 be a predetermined standing temperature, and the temperature control range of the constant temperature bath 25 is 0 ℃ to 50 ℃, and in the embodiment, the temperature control of the constant temperature bath 25 is preferably 20 ℃.

The air inlet channel 21 is communicated with the ozone generator 10, and the ozone generated by the ozone generator 10 enters the liquid storage chamber 20 through the air inlet channel 21. In the present embodiment, the air inlet passage 21 is a PE pipe having a specification of 6 mm.

In the present embodiment, the aeration disc 22 is installed on the air inlet channel 21, and is communicated with the ozone generator 10 through the air inlet channel 21 for introducing the ozone in the air inlet channel 21 into the deionized water in the liquid storage chamber 20.

In this embodiment, the stirring member 23 is installed at the bottom of the liquid storage chamber 20, and is used for continuously stirring the ozone and the water after the ozone is aerated into the deionized water, the stirring time is a predetermined stirring time, the predetermined stirring time is the same as the ozone introducing time, and the stirred ozone water is the initial ozone water.

After obtaining the initial ozone water, the initial ozone water is left to stand for a predetermined standing time, which is preferably 30min in this embodiment, to obtain the calibration ozone water.

Liquid outlet channel 24 has a first liquid outlet (not marked in the drawing) and at least one second liquid outlet (not marked in the drawing), the second liquid outlet is used for intercommunication ozone analyzer, ozone analyzer is used for reading the actual measurement concentration value of calibration ozone water, in this embodiment, liquid outlet channel 24 is the cross valve, the quantity of second liquid outlet is 2, ozone analyzer includes online ozone analyzer E and portable ozone analyzer D, liquid outlet channel 24 communicates stock solution room 20, standard concentration reading piece 30, online ozone analyzer E and portable ozone analyzer D each other, and let in standard ozone water standard concentration reading piece 30, online ozone analyzer E and portable ozone analyzer D respectively from stock solution room 20.

The online ozone analyzer E comprises a flow cell E1 and a detection electrode E2.

The inlet of the flow cell E1 is in communication with the second outlet for receiving calibrated ozonated water from the reservoir 20.

The detection electrode E2 is inserted into the flow cell E1 and is partially immersed in the calibration ozone water for detecting and reading a measured concentration value of the calibration ozone water.

The standard concentration reading unit 30 is used for reading a standard concentration value of the introduced calibration ozone water, and the standard concentration reading unit is an ultraviolet spectrophotometer (detection wavelength: 258 nm).

In this embodiment, a waste liquid tank C communicated with the flow cell E1 is further provided, and after calibration is completed, the calibrated ozone water introduced into the flow cell E1 flows into the waste liquid tank C, so that a complete calibration process is completed.

The above-described embodiments are preferred embodiments of the present invention, and are not intended to limit the scope of the present invention, and various modifications and changes can be made by those skilled in the art without inventive work within the scope of the appended claims.