CN110763639A - Calibration method of ozone analyzer in water - Google Patents

Calibration method of ozone analyzer in water Download PDF

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Publication number
CN110763639A
CN110763639A CN201911108547.2A CN201911108547A CN110763639A CN 110763639 A CN110763639 A CN 110763639A CN 201911108547 A CN201911108547 A CN 201911108547A CN 110763639 A CN110763639 A CN 110763639A
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ozone
water
analyzer
gas
calibrating
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李学辉
陈希尧
唐巍飚
钟义林
刘悦
丁臻敏
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Shanghai Institute of Measurement and Testing Technology
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Shanghai Institute of Measurement and Testing Technology
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/01Arrangements or apparatus for facilitating the optical investigation
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/01Arrangements or apparatus for facilitating the optical investigation
    • G01N2021/0106General arrangement of respective parts
    • G01N2021/0112Apparatus in one mechanical, optical or electronic block

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
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  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
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  • Spectroscopy & Molecular Physics (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)

Abstract

The invention provides a calibration method of an ozone analyzer in water, which comprises the following steps: the gas-liquid mixing pump mixes the stable ozone gas emitted by the ozone generator with water to form stable ozone water, and the stable ozone water enters the liquid storage chamber from the water inlet pipeline; the water outlet pipeline is connected with a gas-liquid mixing pump to form a stable ozone water circulating system; the water inlet pipeline of the liquid storage chamber is connected with an ultraviolet spectrophotometer which is used for measuring the concentration of the ozone water in real time to be an ozone water standard value, and the water inlet pipeline of the liquid storage chamber is connected with an ozone analyzer to be calibrated to measure the concentration value of the ozone water; and comparing the ozone water concentration value with the ozone water standard value, and calibrating the ozone analyzer to be calibrated. The method has the advantages that the concentration of the ozone in the water is accurate and stable, the concentration of the ozone in the water can be monitored in real time, the ozone loss in the process from the time when the water outlet pipe is taken out to the time when the water outlet pipe starts to be detected is prevented, the concentration deviation of the ozone is prevented, and all the ozone analyzers in the water on the market can be effectively calibrated.

Description

Calibration method of ozone analyzer in water
Technical Field
The invention belongs to the field of instrument calibration, and particularly relates to a calibration method of an in-water ozone analyzer.
Background
Because of the strong oxidizing property of ozone, the ozone has strong sterilization capability. Meanwhile, ozone is unstable in water, and a large amount of ozone is quite easy to be automatically digested, so that ozone sterilization is a safe and reliable method and is widely applied. At present, the method is mainly 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 the increasingly wide application field of ozone disinfection, the residual quantity of ozone in water is formulated in various industries, various ozone analyzers in water are used in large quantities in the market, and the metering calibration of the ozone analyzer equipment is urgent for the accuracy and reliability of data measured by portable ozone analyzers.
Therefore, in order to overcome the defect that the ozone in water does not have standard substances, and the ozone analyzer in water needs to be measured and calibrated in the market, the invention provides the method suitable for calibrating the ozone analyzer in water.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a calibration method of an in-water ozone analyzer, the concentration of ozone in water prepared by the method is accurate and stable, the concentration of ozone in water can be monitored in real time, and ozone loss and ozone water concentration deviation caused in the chemical method detection process in national relevant standards are prevented. The method can effectively calibrate all the ozone analyzers in water on the market.
The invention is realized by the following technical scheme:
a calibration method for an in-water ozone analyzer, comprising the steps of:
(1) the gas-liquid mixing pump mixes the stable ozone gas emitted by the ozone generator with water to form stable ozone water, and the stable ozone water enters the liquid storage chamber from the water inlet pipeline; the water outlet pipeline of the liquid storage chamber is connected with a gas-liquid mixing pump to form a stable ozone water circulating system;
(2) the water inlet pipeline of the liquid storage chamber is connected with an ultraviolet spectrophotometer provided with a flow cell, the ultraviolet spectrophotometer is used for measuring the concentration of the ozone water in real time to be an ozone water standard value, and the water inlet pipeline of the liquid storage chamber is connected with an ozone analyzer to be calibrated to measure the concentration value of the ozone water;
(3) and comparing the ozone water concentration value with the ozone water standard value, and calibrating the ozone analyzer to be calibrated.
Preferably, the ozone analyzer to be calibrated is a portable in-water ozone analyzer and/or an online ozone analyzer.
Preferably, the portable in-water ozone analyzer obtains the ozone water concentration value by detecting an ozone water sample taken out from a liquid outlet provided on the water inlet pipeline of the liquid storage chamber.
Preferably, the online ozone analyzer is provided with a flow cell, and a probe instrument is connected behind the flow cell to detect the concentration value of the ozone water in real time.
Preferably, the water outlet pipeline of the liquid storage chamber is arranged at the diagonal of the water inlet pipeline, so that ozone water can be well mixed in the liquid storage chamber.
Preferably, the ozone generator is adjustable in power and connected with a gas-liquid mixing pump to stabilize the mixing of ozone gas and water in the gas-liquid mixing pump.
Preferably, a thermostatic bath is arranged outside the liquid storage chamber, and the temperature is adjusted to be 5-50 ℃.
Preferably, the gas source for generating ozone gas in the ozone generator is dried with activated carbon, which improves the efficiency of generating ozone gas.
Preferably, the gas source for generating ozone gas is air.
Preferably, the liquid storage chamber is provided with a waste gas outlet, and gas discharged from the waste gas outlet is dried and then discharged, so that the pollution to the environment is reduced.
Preferably, after the ozone generator emits the stable ozone gas, the ozone generated by the ozone generator is tested by a traceable ozone gas analyzer to confirm the stability of the emitted ozone gas.
Compared with the prior art, the invention has the advantages that:
1. the calibration method for the ozone analyzer in water adopts the ozone water circulating system, the concentration of ozone water in the system is accurate and stable in the whole calibration process, the concentration of ozone in water can be monitored in real time, and the measured ozone water standard value is more accurate, so that the ozone analyzer is accurately calibrated.
2. The invention adopts the ultraviolet spectrophotometer to monitor the ozone water concentration in real time, is accurate and rapid, and avoids the ozone loss caused by the processes of sampling, reagent adding and the like in the domestic related detection standards to cause the deviation of the ozone concentration in the measured water.
3. The invention adopts the thermostatic bath outside the liquid storage chamber, can control the water temperature, and because the solubility of ozone in water is related to the temperature, the stability of ozone water can be controlled by controlling the water temperature.
4. The liquid storage chamber of the invention adopts the water inlet and the water outlet on the diagonal line, and the ozone water can be well mixed in the liquid storage chamber.
5. The invention is connected with the online ozone analyzer on the pipeline entering the liquid storage chamber, can calibrate the online ozone analyzer in water, and can take out a water sample from the water inlet to calibrate the portable ozone analyzer in water.
6. The invention adopts the active carbon to dry the gas source (air) generating the ozone gas, thereby improving the efficiency of generating the ozone gas.
7. The invention adopts the waste gas outlet to connect with the drying agent, so as to adsorb and decompose ozone gas and reduce the pollution to the environment.
Drawings
FIG. 1 is a schematic flow chart of a calibration method for an in-water ozone analyzer.
Fig. 2 is a schematic structural view of an ozone water circulation system.
Detailed Description
A calibration method for an in-water ozone analyzer, comprising the steps of:
(1) the gas-liquid mixing pump mixes the stable ozone gas emitted by the ozone generator with water to form stable ozone water, and the stable ozone water enters the liquid storage chamber from the water inlet pipeline; the water outlet pipeline is connected with a gas-liquid mixing pump to form a stable ozone water circulating system;
(2) the water inlet pipeline of the liquid storage chamber is connected with an ultraviolet spectrophotometer DR6000(254nm) provided with a flow cell, the ultraviolet spectrophotometer is used for measuring the concentration of the ozone water in real time to be an ozone water standard value, and the water inlet pipeline of the liquid storage chamber is connected with an ozone analyzer to be calibrated to measure the concentration value of the ozone water;
(3) and comparing the ozone water concentration value with the ozone water standard value, correcting the ozone analyzer to be calibrated according to the standard value on the basis of the ozone water standard value measured by the ultraviolet spectrophotometer, and calibrating the ozone analyzer to be calibrated.
The ozone analyzer to be calibrated is a portable in-water ozone analyzer and/or an online ozone analyzer.
The portable aquatic ozone analyzer obtains the ozone water concentration value by detecting the ozone water sample taken out from the liquid outlet arranged on the water inlet pipeline of the liquid storage chamber.
The online ozone analyzer is provided with a flow cell, and a probe instrument is connected behind the flow cell to detect the concentration value of ozone water in real time.
The liquid storage chamber water outlet pipeline is arranged on the diagonal line of the water inlet pipeline.
The ozone generator is adjustable in power and connected with the gas-liquid mixing pump, and ozone gas and water are stably mixed in the gas-liquid mixing pump.
The liquid storage chamber is provided with a thermostatic bath outside, and the temperature is adjusted at 5-50 ℃.
The gas source used for generating ozone gas in the ozone generator is dried by active carbon, so that the ozone gas generation efficiency is improved.
The gas source for generating ozone gas is air.
The liquid storage chamber is provided with a waste gas outlet, gas discharged from the waste gas outlet is dried and then discharged, ozone gas is adsorbed and decomposed in the drying process, and the pollution to the environment is reduced.
After the ozone generator emits stable ozone gas, the ozone generated by the ozone generator is tested by a traced ozone gas analyzer to confirm the stability of the emitted ozone gas.
In the whole calibration process, the concentration of ozone water in the ozone water circulating system is balanced, the decomposition time of the ozone in the water is 10min-15min, a stable ozone generator in the ozone water circulating system is continuously filled with the ozone, the concentration of the ozone is not increased after the ozone is filled into the water for a period of time, and the concentration of the ozone in the water is not reduced because the ozone gas is continuously filled. After reaching the stable value, the concentration of the ozone water in the ozone water circulating system is stable.
The above description is only an embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that are not thought of through the inventive work should be included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope defined by the claims.

Claims (10)

1. A calibration method of an ozone analyzer in water is characterized by comprising the following steps:
(1) the gas-liquid mixing pump mixes the stable ozone gas emitted by the ozone generator with water to form stable ozone water, and the stable ozone water enters the liquid storage chamber from the water inlet pipeline; the water outlet pipeline of the liquid storage chamber is connected with a gas-liquid mixing pump to form a stable ozone water circulating system;
(2) the water inlet pipeline of the liquid storage chamber is connected with an ultraviolet spectrophotometer provided with a flow cell, the ultraviolet spectrophotometer is used for measuring the concentration of the ozone water in real time to be an ozone water standard value, and the water inlet pipeline of the liquid storage chamber is connected with an ozone analyzer to be calibrated to measure the concentration value of the ozone water;
(3) and comparing the ozone water concentration value with the ozone water standard value, and calibrating the ozone analyzer to be calibrated.
2. The method of calibrating an ozone analyzer in water according to claim 1, wherein the ozone analyzer to be calibrated is a portable ozone analyzer in water and/or an online ozone analyzer.
3. The method of calibrating an in-water ozone analyzer according to claim 2, wherein the portable in-water ozone analyzer obtains the ozone water concentration value by detecting an ozone water sample taken out from a liquid outflow port provided in the water inlet line of the reservoir.
4. The method of calibrating an in-water ozone analyzer according to claim 2, wherein the on-line ozone analyzer is equipped with a flow cell, and a probe instrument is connected to the rear of the flow cell to detect the ozone water concentration value in real time.
5. The method of calibrating an in-water ozone analyzer of claim 1, wherein the reservoir outlet line is at a diagonal of the inlet line.
6. The method for calibrating an ozone analyzer in water according to claim 1, wherein the liquid storage chamber is externally provided with a constant temperature bath, and the temperature is adjusted at 5 ℃ to 50 ℃.
7. The method of calibrating an in-water ozone analyzer of claim 1, wherein the ozone generator is power-adjustable and is connected to a gas-liquid mixing pump to stabilize the mixing of ozone gas and water in the gas-liquid mixing pump.
8. The method for calibrating an ozone analyzer in water according to claim 1, wherein a gas source for generating ozone gas in the ozone generator is dried with activated carbon.
9. The method for calibrating an in-water ozone analyzer according to claim 1, wherein the reservoir chamber is provided with an exhaust gas outlet port, and the gas discharged from the exhaust gas outlet port is dried and discharged.
10. The method of calibrating an ozone analyzer in water according to claim 1, wherein after the ozone generator emits the stable ozone gas, the ozone generated by the ozone generator is tested by a traceable ozone gas analyzer to confirm the stability of the emitted ozone gas.
CN201911108547.2A 2019-11-13 2019-11-13 Calibration method of ozone analyzer in water Pending CN110763639A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111272750A (en) * 2020-03-23 2020-06-12 华润怡宝饮料(中国)有限公司 Ozone colorimeter calibration method based on potassium iodate and application thereof
CN111812291A (en) * 2020-08-06 2020-10-23 上海市计量测试技术研究院 Method and device for calibrating ozone analyzer
CN112067682A (en) * 2020-09-27 2020-12-11 华能陕西秦岭发电有限公司 Online dissolved oxygen meter zero calibration system and method
CN113702434A (en) * 2021-09-16 2021-11-26 北京软通智慧科技有限公司 Ozone sensor baseline calibration system and calibration method
CN114349136A (en) * 2021-12-06 2022-04-15 上海市计量测试技术研究院 Portable device and method capable of accurately preparing ozone water with different concentrations

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CN104990885A (en) * 2015-07-08 2015-10-21 安徽蓝盾光电子股份有限公司 Portable high-concentration ozone calibration source
CN108828172A (en) * 2018-06-21 2018-11-16 中国计量科学研究院 The calibration method and device of total organic carbon analyzer
CN109374536A (en) * 2018-12-13 2019-02-22 青岛海纳光电环保有限公司 Ozone concentration measurement device and method

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111272750A (en) * 2020-03-23 2020-06-12 华润怡宝饮料(中国)有限公司 Ozone colorimeter calibration method based on potassium iodate and application thereof
CN111812291A (en) * 2020-08-06 2020-10-23 上海市计量测试技术研究院 Method and device for calibrating ozone analyzer
CN112067682A (en) * 2020-09-27 2020-12-11 华能陕西秦岭发电有限公司 Online dissolved oxygen meter zero calibration system and method
CN113702434A (en) * 2021-09-16 2021-11-26 北京软通智慧科技有限公司 Ozone sensor baseline calibration system and calibration method
CN114349136A (en) * 2021-12-06 2022-04-15 上海市计量测试技术研究院 Portable device and method capable of accurately preparing ozone water with different concentrations

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