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Basic dataStandard ID: HJ 1099-2020 (HJ1099-2020)Description (Translated English): Technical specifications for level 1 calibration of ambient air ozone monitoring Sector / Industry: Environmental Protection Industry Standard Word Count Estimation: 20,236 Date of Issue: 2020 Date of Implementation: 2020-04-12 Issuing agency(ies): Ministry of Ecology and Environment HJ 1099-2020: Technical specifications for level 1 calibration of ambient air ozone monitoring---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.Technical specifications for level 1 calibration of ambient air ozone monitoring National Environmental Protection Standards of the People's Republic of China Technical specification for primary calibration of ambient air ozone monitoring 2020-02-12 release 2020-04-12 Implementation Issued by the Ministry of Ecology and Environment Table of contentsForeword...ii 1 Scope of application...1 2 Normative references...1 3 Terms and definitions...1 4 Composition and requirements of primary calibration facilities for ozone monitoring...2 5 Primary calibration method for ozone monitoring...4 6 Result calculation and evaluation...6 7 Recalibration interval...7 8 Quality Assurance and Quality Control...8 Appendix A (informative appendix) Performance indicators of ozone transmission standards/ozone control standards...9 Appendix B (informative appendix) Ozone monitoring primary calibration report template...10 Appendix C (Informative Appendix) Performance Verification Method of Ozone Standard Reference Photometer...12 Appendix D (informative appendix) Ozone Standard Reference Photometer Performance Verification Record Form...15ForewordTo implement the "Environmental Protection Law of the People's Republic of China" and "The Air Pollution Prevention and Control Law of the People's Republic of China" to protect the ecological environment To ensure human health, standardize the first-level calibration operation of ambient air ozone monitoring, and formulate this standard. This standard specifies the requirements for the primary calibration of ambient air ozone monitoring and the method for calibration of the primary ozone standard for ozone transmission standards. Law and its quality assurance and quality control. Appendix A to Appendix D of this standard are informative appendices. This standard is issued for the first time. This standard was formulated by the Department of Ecological Environment Monitoring and the Department of Regulations and Standards of the Ministry of Ecology and Environment. Drafting organization of this standard. Standard Sample Research Institute of Ministry of Ecology and Environment. Verification units of this standard. China Environmental Monitoring Center, Shanghai Environmental Monitoring Center, Jiangsu Environmental Monitoring Center. This standard was approved by the Ministry of Ecology and Environment on February 12, 2020. This standard will be implemented on April 12, 2020. This standard is interpreted by the Ministry of Ecology and Environment. Technical specification for primary calibration of ambient air ozone monitoring1 Scope of applicationThis standard specifies the requirements for the primary calibration of ambient air ozone monitoring and the method for calibration of the primary ozone standard for ozone transmission standards. Law and its quality assurance and quality control. This standard applies to the transfer of the value of the ozone level 1 standard to the ozone transmission standard, the level 1 calibration of ozone monitoring and its quality assurance Certification and quality control. Other ozone standard reference photometers can refer to this standard to calibrate the ozone transmission standard.2 Normative referencesThis standard quotes the following documents or their clauses. For undated reference documents, their valid versions are applicable to this standard. HJ 590 Determination of Ozone in Ambient Air Ultraviolet Photometric Method3 Terms and definitionsThe following terms and definitions apply to this standard. 3.1 Calibration For a set of operations under specified conditions, the first step is to determine the relationship between the value provided by the measurement standard and the corresponding display value. The second step is to use this information to determine the relationship between the measurement results obtained from the displayed value, where the measurement standard provided by the measurement standard and the corresponding The displayed value has measurement uncertainty. 3.2 Ozone standard reference photometer (SRP) Based on the principle that ozone has a significant absorption of ultraviolet light of a specific wavelength (253.7 nm), the ultraviolet double-path detection technology is adopted Technology, an ozone standard measuring instrument recognized by an international authoritative organization. 3.3 Ozone level 1 standard Refers to the ozone standard reference photometer recognized by the ecological environment monitoring department, which is the highest meter in the national ecological environment system Measuring appliances. The primary ozone standard is mainly used for comparison with the value of the national measurement base (standard) and the SRP in the ecological environment system. The quantity value comparison and the quantity value transmission to the ozone transmission standard. 3.4 Ozone transfer standard Refers to the ability to accurately reproduce or accurately analyze the ozone concentration, traceable to a higher level or higher authority in accordance with relevant operating procedures Granville standard transportable equipment. The ozone transmission standard is used to transmit the authority of the ozone level 1 standard or to calibrate the monitoring station Point ozone calibration instrument or ozone analysis instrument. 3.5 Ozone control standard The ozone transfer standard calibrated by the ozone standard reference photometer is the quality assurance and quality control instrument of SRP. Often placed in the laboratory. Mainly used as a backup standard when the ozone standard reference photometer fails or for the first level of ozone monitoring The reference standard when calibration is in doubt. 3.6 Ozone monitoring level 1 calibration Refers to the operation of a photometer with ozone primary standards calibrated to ozone transfer standards or ozone control standards to establish ozone transfer The quantitative relationship between ozone concentration standards or ozone control standards and ozone level 1 standards. 3.7 Zero air Refers to do not contain ozone, sulfur dioxide, nitrogen oxides, hydrocarbons and any ozone photometer that can produce ultraviolet absorption Air of other substances. 3.8 Traceability Refers to the measurement results being traced back to the national measurement standard or the national measurement standard through the intermediate comparison link with appropriate accuracy. The process of measuring standards.4 Composition and requirements of primary calibration facilities for ozone monitoring4.1 Composition of primary calibration facility for ozone monitoring The first-level calibration facility for ozone monitoring consists of an ozone standard reference photometer, a zero gas generator, auxiliary equipment, and an ozone transmission standard. Standard and data acquisition and transmission equipment composition, as shown in Figure 1. Figure 1 Composition of primary calibration facilities for ozone monitoring 4.2 Requirements for primary calibration environmental facilities for ozone monitoring 4.2.1 Environmental conditions The temperature is maintained between (15~30)℃, and the temperature fluctuation should not exceed ±1℃/h. Choosing an appropriate air conditioning system can Automatically control the temperature in the laboratory and maintain sufficient air circulation to balance the temperature distribution. Do not blow the air conditioner directly against the instrument. The relative humidity is kept between (10~50)%. When the humidity cannot meet the requirements, a dehumidifier or humidifier is required. Avoid dehumidifier or humidifier directly facing the instrument when using. The laboratory should be equipped with good ventilation equipment and exhaust outlets. The working table of the ozone standard reference photometer should be set to pump The wind system removes the excess ozone generated during the calibration process. The exhaust gas outlet should be equipped with activated carbon cleaning and absorption devices to avoid create pollution. The power supply system should be equipped with power supply overvoltage, overload and leakage protection devices, and the power supply voltage should be maintained at. 220×(1±10%)V, (50±1) Hz. The laboratory should have a good grounding circuit, and the grounding resistance should be less than 4 Ω. Such as the supply of ozone standard reference photometer The electrical voltage is required to be 110×(1±10%) V, a voltage-stabilizing transformer is required, and an uninterruptible power supply is required if conditions permit. 4.2.2 Equipment requirements 4.2.2.1 Zero gas generator The zero-gas generator is mainly composed of an air compressor and a zero-gas generator, which provides a stable zero for the primary calibration of ozone monitoring. Gas source. The zero gas generator needs to be equipped with a particulate removal device, ozone and other interference removal device and a gas drying device, and can The output pressure is at least 172 kPa zero gas. The zero gas index shall meet the relevant requirements of HJ 590. 4.2.2.2 Auxiliary equipment Auxiliary equipment is used to measure or adjust the temperature, humidity, pressure, voltage, etc. of the environment, mainly by thermometers and hygrometers, atmospheric It is composed of pressure gauge, voltmeter, voltage regulator transformer, etc. 4.2.2.3 Ozone transmission standard/ozone control standard The ozone transmission standard/ozone control standard instrument should have a product nameplate, and the nameplate should be marked with the name, model, and production of the instrument Unit, factory number, manufacturing date and other information. The surface of the instrument should be intact, without obvious defects, and the parts should be connected reliably. The operation keys and buttons are flexible and effective. The main panel of the instrument is clearly displayed, and characters and logos are easy to identify. The ozone transmission standard/ozone control standard should be able to accurately generate and analyze ozone concentration, with digital signal or analog signal output The output function can be used for feedback adjustment of the ozone generator. Refer to Appendix A for the performance indicators of the ozone transmission standard/ozone control standard. 4.2.2.4 Data acquisition and transmission equipment Mainly used to collect, process and store data.5 Primary calibration method for ozone monitoring5.1 Warm up the instrument After the ozone standard reference photometer is turned on, the warm-up stability should be no less than 48 hours, and the ozone transmission standard/ozone control standard should be sufficient The warm-up is stable, so that the instrument reaches the best working condition. 5.2 Piping and signal connection 5.2.1 Pipeline connection The ozone generator of the ozone standard reference photometer should be used for the primary calibration of ozone monitoring. Connect the air pressure as shown in Figure 2 The pipes between the compressor, zero gas generator, ozone standard reference photometer, and ozone transmission standard should be tightly connected. Avoid air leakage and falling off. Note 1.The material of the pipeline should be made of inert materials that do not chemically react with ozone, such as borosilicate glass, polytetrafluoroethylene, etc. Connect to multiple The pipelines of the pipes should be of equal length and no more than 1 meter. Note 2.Zero gas from different sources may contain different interfering substances and produce different UV absorption. Therefore, to provide ozone delivery standards The zero gas must be the same source as the zero gas used by the ozone standard reference photometer ozone generator. 5.2.2 Signal connection Serial interface connection mode. use a data cable to connect the serial interface port of the ozone transmission standard instrument and the computer port. according to Ozone transfer standard communication protocol for parameter setting. Analog signal connection mode. use a signal cable to connect the analog signal port of the ozone transmission standard instrument and the ozone standard reference light Meter signal converter port. Set the parameters according to the voltage and range of the standard analog signal transmitted by ozone. Figure 2 Ozone monitoring primary calibration pipeline and signal connection diagram 5.3 Parameter setting Set the relevant parameters of the ozone standard reference photometer to calibrate the ozone transmission standard, in which the stability factor (Instrument Stability Factor and Data Quality Factor are usually set to 0.7, and the maximum cannot exceed 2.0. For other parameter settings, refer to the manual of the ozone delivery standard instrument. Note. When the ozone standard reference photometer is calibrated with multiple ozone transmission standards, by adjusting the built-in flow controller of the ozone standard reference photometer, Control the gas flow into the manifold to ensure that the exhaust port margin of the manifold is at least 1 L/min. 5.5 Multi-point calibration Within the full scale range of the ozone transmission standard, set the concentration points to no less than 7 (including a zero point and 6 different gradients) Concentration point). The reading of each concentration point is set to the average of 10 repeated readings, and the standard deviation of the 10 repeated readings should be small At 2 nmol/mol. Run the calibration program, first run a multi-point calibration, and calculate the slope m of the calibration curve according to step 6.1 And intercept I. According to the following indicators, determine whether the ozone transmission standard needs to be adjusted for zero and span points. When | m-1| >0.03 or | I | >3 nmol/mol, you need to find the possible cause and adjust the zero point and span point; When 0.015≤ | m-1| ≤0.03 or 1.5≤ | I | ≤3 (nmol/mol), zero point and span point adjustment is required; When | m-1| < 0.015 and | I | < 1.5 nmol/mol, zero and span point adjustments are not necessary. After completing the above operations, run a multi-point calibration. The primary calibration of ozone monitoring needs to be carried out within 3 days or more for at least 6 After the multi-point calibration is completed every day, zero gas should be used to purge for at least 10 minutes after the end of the calibration to eliminate the residual ozone gas in the pipeline system. 5.6 Zero point adjustment Adjust the ozone generator of the ozone standard reference photometer so that the ozone concentration produced is 0 nmol/mol. Wait for the ozone standard After the indication values of the reference photometer and the ozone transfer standard are stable (at least stable for 10 min), adjust the calibration parameters of the ozone transfer standard, Keep its response value consistent with the output value of the ozone standard reference photometer. 5.7 Span point adjustment Adjust the ozone generator of the ozone standard reference photometer to produce an ozone concentration of 80% of the ozone transfer standard full scale. After the indications of the ozone standard reference photometer and the ozone transfer standard are stable (at least stable for 10 min), adjust the ozone transfer standard The response value is consistent with the output value of the ozone standard reference photometer.6 Result calculation and evaluation6.1 Drawing of calibration curve Take the measured value of the ozone standard reference photometer as the abscissa, and the response value of the ozone transmission standard as the ordinate, using the least square Multiply to establish a calibration curve, and record the slope and intercept of the calibration curve. 6.2 Result calculation The average slope and average intercept of multi-point calibration are calculated according to formula (1) and formula (2) respectively; multi-point calibration slope The relative standard deviation and the standard deviation of the intercept are calculated according to formula (3) and formula (4) respectively. 6.3 Evaluation Index Each slope of multiple multi-point calibration should be between 0.97~1.03, and each intercept should be between (0±3) nmol/mol The relative standard deviation of the multi-point calibration slope should be ≤ 3.7%, and the standard deviation of the intercept should be ≤ 1.5 nmol/mol. Otherwise, the original Because of this, re-calibrate after repairing the ozone transmission standard. Refer to Appendix B for the primary calibration report of ozone monitoring.7 Recheck intervalThe recalibration interval of primary ozone monitoring calibration is generally not more than one year. During the validity period of the certificate, the ozone transmission standard needs to be calibrated again if the following situations occur. a) The calibration parameters have been adjusted; b) Relevant maintenance affecting ozone concentration measurement has been carried out; c) Obvious deviation of the instrument value.8 Quality Assurance and Quality Control8.1 Operation day/operation week verification 8.1.1 Operation day verification During the operation of the ozone standard reference photometer, the temperature, humidity and pressure of the laboratory environment should be checked daily. 8.1.2 Operation Weekly Check During the operation of the ozone standard reference photometer, run once a week or run a performance check before and after calibration to confirm The ozone standard reference photometer has stable performance. Performance verification includes pressure test, temperature test, UV lamp source background temperature test, UV lamp source intensity test, photometric blank value, stability test, etc. Refer to the attachment for the performance verification method of the ozone standard reference photometer Record C. Refer to Appendix D for the Ozone Standard Reference Photometer Performance Verification Record Sheet. Note. The performance verification of the ozone standard reference photometer must be carried out with the zero gas generating device not opened. 8.2 Semi-annual verification 8.2.1 Ozone control standards The ozone control standard should be checked by the ozone standard reference photometer every 6 months, the operation steps are shown in 5, evaluation guidelines See 6.3. The ozone standard reference photometer should be compared with the ozone control standard before and after leaving the laboratory. The comparison result deviates from the ozone monitoring When measuring the first-level calibration index, a comparison with another ozone standard reference photometer should be carried out. 8.2.2 Zero gas generator In order to ensure zero gas quality, it should be replaced every 6 months in accordance with the relevant requirements of HJ 590 to remove various interfering substances. Supplies. 8.3 Instrument verification Atmospheric pressure gauges and voltage measuring meters used to monitor the laboratory environment and the working status of instruments and equipment shall be The regulations require periodic verification. 8.4 Traceability The primary ozone standard should be traced back to the social public measurement standards of the Chinese Academy of Metrology or the ecological environment department. 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