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HJ 1132-2020 English PDF

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HJ 1132-2020: Stationary source emission - Determination of nitrogen oxides - Portable ultraviolet absorption method
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Basic data

Standard ID: HJ 1132-2020 (HJ1132-2020)
Description (Translated English): Stationary source emission - Determination of nitrogen oxides - Portable ultraviolet absorption method
Sector / Industry: Environmental Protection Industry Standard
Classification of Chinese Standard: Z25
Word Count Estimation: 12,196
Date of Issue: 2020-05-15
Date of Implementation: 2020-08-15
Regulation (derived from): Ministry of Ecology and Environment Announcement No. 29, 2020
Issuing agency(ies): Ministry of Ecology and Environment

HJ 1132-2020: Stationary source emission - Determination of nitrogen oxides - Portable ultraviolet absorption method

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Stationary source emission - Determination of nitrogen oxides - Portable ultraviolet absorption method National Environmental Protection Standards of the People's Republic of China Determination of nitrogen oxides in waste gas from stationary sources Portable UV Absorption Method 2020-05-15 release 2020-08-15 Implementation Issued by the Ministry of Ecology and Environment

Foreword...ii 1 Scope of application...1 2 Normative references...1 3 Terms and definitions...1 4 Principle of the method...2 5 Interference and cancellation...2 6 Reagents and materials...2 7 Instruments and equipment...2 8 Sample...3 9 Analysis steps...3 10 Calculation and presentation of results...4 11 Precision and accuracy...6 12 Quality Assurance and Quality Control...7 13 Precautions...7 Appendix A (informative appendix) Table of results of instrument performance audit before and after monitoring...8

Foreword

To 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 This standard is formulated to ensure the environment, protect human health, standardize portable measurement methods of nitrogen oxides in exhaust gas from fixed sources. This standard specifies a portable ultraviolet absorption method for the determination of nitrogen oxides in exhaust gas from stationary sources. Appendix A of this standard is an informative appendix. 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 organizations of this standard. China Environmental Monitoring Center, Shandong Ecological Environment Monitoring Center. Verification units of this standard. Tianjin Ecological Environment Monitoring Center, Hubei Province Ecological Environment Monitoring Center Station, Qinhuangdao City Environmental Environmental Monitoring Center, Shenyang Ecological Environment Monitoring Center of Liaoning Province, Binzhou Ecological Environmental Monitoring Center of Shandong Province, and Guiyang Environmental Monitoring Center Test center station. This standard was approved by the Ministry of Ecology and Environment on May 15, 2020. This standard will be implemented on August 15, 2020. This standard is interpreted by the Ministry of Ecology and Environment.

1 Determination of nitrogen oxides in exhaust gas from stationary sources of portable ultraviolet absorption method

1 Scope of application

This standard specifies a portable ultraviolet absorption method for the determination of nitrogen oxides in exhaust gas from stationary sources. This standard applies to the determination of nitrogen oxides in exhaust gas from stationary sources. The detection limit of nitric oxide method is 1 mg/m3, and the lower limit of determination is 4 mg/m3; the method detection limit of nitrogen dioxide is 2 mg/m3, the lower limit of determination is 8 mg/m3.

2 Normative references

This standard quotes the following documents or their clauses. For undated reference documents, their valid versions are applicable to this standard. GB/T 16157 Determination of particulate matter in exhaust from stationary sources and sampling method for gaseous pollutants HJ 75 Technical specification for continuous monitoring of emission of stationary pollution source flue gas (SO2, NOX, particulate matter) HJ/T 373 Fixed pollution source monitoring quality assurance and quality control technical specifications HJ/T 397 Fixed source exhaust gas monitoring technical specification HJ 1045 Fixed pollution source flue gas (sulfur dioxide and nitrogen oxide) portable ultraviolet absorption method technical requirements Seeking and testing methods

3 Terms and definitions

The following terms and definitions apply to this standard. 3.1 Nitrogen oxides Refers to the oxides of nitrogen in the form of nitrogen monoxide (NO) and nitrogen dioxide (NO2) in the exhaust gas from stationary sources. 3.2 Calibration span The concentration value of the standard gas used for calibration (when performing multi-point calibration, it is the highest concentration value of the standard gas used for calibration), The calibration range (indicated by CS below) should be less than or equal to the full range of the instrument. 3.3 Error of indication The absolute or relative error between the measurement result of the standard gas directly imported into the analyzer and the concentration value of the standard gas. 3.4 Zero drift Before and after the measurement, the absolute error of the measurement result of the same zero gas or the absolute error and the percentage of the calibration range ratio. 23.5 Span drift Before and after the measurement, the absolute error or absolute error of the measurement result of the instrument on the same calibration range point standard gas is compared with the calibration Percentage of range. 3.6 Systematic error The standard gas is directly introduced into the air inlet of the main body of the instrument (direct measurement mode). The absolute error between the measurement results obtained by the instrument (system measurement mode) or the absolute error and the percentage of the calibration range ratio.

4 Principle of the method

Nitric oxide has a characteristic wavelength of.200 nm～235 nm in the ultraviolet range, and nitrogen dioxide has a characteristic wavelength of 220 nm～ 250 nm or 350 nm～500 nm characteristic wavelength light has selective absorption, quantitative determination of exhaust gas according to Lambert-Beer law The concentration of nitrogen monoxide and nitrogen dioxide.

5 Interference and elimination

5.1 The particulate matter in the exhaust gas is easy to pollute the absorption pool. The particulate matter in the exhaust gas should be eliminated or reduced by means of high-efficiency filter dust removal. For the contamination of the instrument by particles, the material of the filter material should avoid physical adsorption or chemical reaction with nitrogen oxides. 5.2 The water vapor in the exhaust gas will absorb the nitrogen dioxide in the sample when it is cold and produce condensed water during the sampling process, resulting in the test result. If the result is too low, it should be eliminated by heating sampling pipes and air ducts, cooling devices for rapid dehumidification or measuring hot and humid exhaust gas samples, etc. Or reduce the pollution of the instrument caused by the condensation of water vapor in the exhaust gas and the loss of nitrogen oxide adsorption and dissolution.

6 Reagents and materials

6.1 Standard gas of nitric oxide and nitrogen dioxide. commercially available certified standard gas, expanded uncertainty ≤ 2%; or use 6.2 The gas distribution device used to dilute high-concentration commercially available certified standard gas with suitable concentration gas with nitrogen. 6.2 Gas distribution device. a commercially available dilution gas distribution device, the maximum output flow is not less than 5 L/min, all input and output flow The maximum allowable error of the meter flow should meet. when the flow is less than 50% of the full range, the maximum allowable error of the flow does not exceed the full range When the flow is not less than 50% of the full scale, the maximum allowable error of the flow does not exceed ±1.0% of the set flow. The material of the gas system of the gas distribution device should avoid physical adsorption or chemical reaction with nitrogen oxides. 6.3 Zero gas. nitrogen or air with purity ≥99.99% that does not interfere with the measurement.

7 Apparatus and equipment

7.1 Nitrogen Oxide Analyzer by UV Absorption Method 7.1.1 Composition Ultraviolet absorption method nitrogen oxide analyzer (abbreviation. instrument) composition. analyzer (including light source, detector, absorption cell, 3 Control unit, etc.), gas flow meter, air pump, sampling pipe, air duct, dehumidification and dust removal device, printer, etc. The instrument for measuring exhaust gas samples using the thermal and humidity method should be equipped with a detector for measuring the moisture content in the exhaust gas, and no dehumidification device is required. However, the moisture content in the exhaust gas should be measured simultaneously. Note. Thermal moisture method refers to the method of directly measuring the concentration of high-temperature wet exhaust gas without condensation and removal of water. 7.1.2 Performance requirements a) Indication error. when the calibration range ＞100 μmol/mol, the relative error does not exceed ±3%; the calibration range ≤ When 100 μmol/mol, the absolute error does not exceed ±3.0 μmol/mol; b) System error. when the calibration range >60 μmol/mol, the relative error does not exceed ±5%; the calibration range≤ When 60 μmol/mol, the absolute error does not exceed ±3.0 μmol/mol; c) Zero drift. when the calibration range >100 μmol/mol, the relative error does not exceed ±3%; the calibration range≤ When 100 μmol/mol, the absolute error does not exceed ±3.0 μmol/mol; d) Range drift. when the calibration range >100 μmol/mol, the relative error does not exceed ±3%; the calibration range≤ When 100 μmol/mol, the absolute error does not exceed ±3.0 μmol/mol; e) With sampling flow display function; f) Sampling tube heating and heat preservation temperature. can be set and adjusted within 120℃～160℃; g) Other properties should meet the requirements of HJ 1045. 7.2 Standard gas cylinder. equipped with adjustable pressure reducing valve, flow controller and gas pipe. Pressure reducing valve, flow controller and pilot The air tube material should avoid physical adsorption or chemical reaction with nitrogen oxides. 7.3 Air collecting bag. used to calibrate the instrument by air bag method. The lining material should be polyfluoroethylene film, polyperfluoroethylene propylene film, etc. Inert material that affects the measured component or has little effect on the measured component.

8 samples

According to GB/T 16157, HJ/T 397, HJ/T 373, HJ 75 and relevant regulations, determine the sampling location, sampling point and frequency Next, samples of nitric oxide and nitrogen dioxide were collected for analysis.

9 Analysis steps

9.1 Air tightness check of the instrument According to the instrument manual, connect the analyzer, sampling tube, air duct, etc., turn on the power of the instrument, and stabilize after the instrument is warmed up After that, check the air tightness according to HJ 1045.If the check fails, check for leaks and maintain until the check is qualified. 9.2 Instrument calibration Import the zero point gas and nitric oxide standard gas into the instrument in turn, and calibrate the instrument zero point and calibration volume according to the instrument manual Cheng. The method of introducing zero gas and standard gas is as follows. a) Air bag method. Fill the clean air bag with standard gas and empty it, repeat three times, and use it within 3 hours after refilling. use. The concentration of the standard gas introduced should not exceed 50 μmol/mol. According to the calibration specified in the instrument manual Calibrate according to the exact steps. If this measurement needs to determine the zero point drift and span drift, record the zero point and calibrate the span 4-point instrument display. b) Cylinder method. connect a standard gas cylinder equipped with a flow controller and a gas pipe to the sampling pipe, and open the cylinder gas valve Door, adjust the flow controller to pass the standard gas into the inlet of the instrument at the flow rate specified by the instrument. Pay attention to each No air leaks at the connection. For the built-in suction pump of the analyzer, the cylinder gas supply flow should be appropriately increased, and the The bypass pressure relief method ensures that there is no negative pressure in the gas path and that the air intake of the analyzer will not be too large. According to the instrument manual Perform calibration according to the calibration procedure specified in. If this measurement needs to determine the zero point drift, span drift, record the zero point, Calibrate the range point of the instrument display. 9.3 Sample determination Insert the sampling tube into the sampling point, and continuously and automatically sample at the sampling flow rate specified by the instrument, and wait for the instrument reading to stabilize. Record readings, save an average value every minute, and continuously sample for 5 min～15 min. The average value of measured data can be used as a sample Product measured value. During the measurement, if the concentration of nitrogen dioxide is found to exceed the lower limit of this method, the measurement should be stopped, and the measurement should be stopped according to the requirements of 9.2 After calibrating the instrument with nitrogen dioxide standard gas, perform the measurement again. 9.4 Quality check and shutdown After the determination, proceed as follows. a) Place the sampling tube in the zero point gas and wait for the instrument display to stabilize; b) If you need to perform a zero drift check, record the value of the instrument at this time, and calculate the zero drift, otherwise go directly to the next One step (the monitoring unit arranges according to the requirements of 12.3 of this standard to regularly carry out zero-point drift inspection); c) Pass the standard gas through the inlet of the instrument and the sampling pipe respectively, and calculate the indication error and the system after the instrument display is stable. System error; or directly pass standard gas through the sampling pipe to check the indication error of the whole system; d) To carry out the span drift check, pass the standard gas whose concentration is the calibration span from the sampling tube, and wait for the indicator to stabilize. After setting, record the displayed value of the instrument and calculate the range drift, otherwise go directly to the next step (the monitoring unit is based on this standard 12.3 requires arrangements to regularly carry out range drift inspection); e) If the results of b), c), and d) meet the requirements of 7.1.2, the test result is valid, otherwise the test result is invalid; f) Place the sampling tube in the zero point gas, and after the instrument display is stable, turn off the power of the instrument and the preprocessor, and disconnect the instrument All parts are connected, the instrument is packed and the test is over. 10 Calculation and presentation of results 10.1 Result calculation The concentration of nitrogen oxides is calculated as nitrogen dioxide and calculated by the following formula. Mass concentration of nitrogen oxides. a) The dry basis concentration obtained by the test is converted from the volume concentration of nitrogen monoxide and nitrogen dioxide to the mass concentration of nitrogen oxides Degree, calculated according to formula (1). 10.2 Presentation of results The concentration of nitrogen oxides is calculated as nitrogen dioxide, and the calculation result is reserved to the integer. When the concentration is ≥1.00×103mg/m3, it is reserved Three significant figures. If the measurement result of nitrogen dioxide is less than the lower limit of measurement, the corresponding volume concentration and mass concentration in 10.1 are Zero count. 11 Precision and accuracy 11.1 Precision The six laboratories have carried out the standard gas concentration of 14 mg/m3, 65 mg/m3, and 134 mg/m3. 6 repeated determinations. the relative standard deviations in the laboratory are 0.8%～3.2%, 0.3%～1.1% and 0.5%～1.8% respectively; The relative standard deviations between laboratories were 4.3%, 1.7%, and 3.1%, respectively; the repeatability limits were 0 mg/m3, 0 mg/m3, and 2 mg/m3; The reproducibility limits are 2 mg/m3, 3 mg/m3 and 12 mg/m3. The six laboratories carried out the standard gases of nitrogen dioxide with concentrations of 23 mg/m3, 105 mg/m3, and.200 mg/m3. 6 repeated determinations. the relative standard deviations in the laboratory were 1.3%～4.3%, 0.3%～1.1% and 0.2%～2.9%; The relative standard deviations between laboratories were 6.8%, 2.0%, and 5.6%; the repeatability limits were 1 mg/m3, 1 mg/m3, and 5 mg/m3; The reproducibility limits are 4 mg/m3, 6 mg/m3 and 31 mg/m3. Six laboratories carried out tests on the nitrogen oxide concentration in the exhaust outlet of a sintering machine, the exhaust outlet of a power plant, and the flue gas of a chemical enterprise Simultaneous determination, where the concentration of nitric oxide in the flue gas of the sintering machine is 4 mg/m3～13 mg/m3, and the average value is 8 mg/m3, the concentration of nitrogen dioxide is not detected; the concentration of nitrogen monoxide in the flue gas of the boiler exhaust of the power plant is 13 mg/m3～ 22 mg/m3, the average value is 18 mg/m3, the concentration of nitrogen dioxide is not detected; the concentration of nitrogen monoxide in the flue gas of chemical enterprises is 205 mg/m3～233 mg/m3, the average value is 222 mg/m3, the nitrogen dioxide concentration is 44 mg/m3～74 mg/m3, the average The value is 62 mg/m3.The relative standard deviations in the testing nitric oxide laboratory are. 3.9%～25.0%, 26.4%～41.7% And 28.7%～36.7%; the relative standard deviations between laboratories are 39.7%, 16.7% and 4.6% respectively; the repeatability limit is 1 mg/m3, 2 mg/m3 and 15 mg/m3; reproducibility limits are 9 mg/m3, 9 mg/m3 and 32 mg/m3.Testing nitrogen dioxide in the laboratory The relative standard deviation is 15.8%～22.4%; the relative standard deviation between laboratories is 15.9%; the repeatability limit is 7 mg/m3; The current limit is 29 mg/m3 (not detected at the outlet of sintering machine and power plant boiler). 11.2 Accuracy Six laboratories measure the standard gases of nitric oxide with concentrations of 14 mg/m3, 65 mg/m3, and 134 mg/m3. The relative errors are -5.7%～4.7%, -1.2%～3.7%, and -7.2%～-1.5%; the final values of the relative errors are respectively -0.2%±8.6%, 0.7%±3.5%, -1.2%±6.1%. Six laboratories respectively measured nitrogen dioxide standard gases with concentrations of 23 mg/m3, 105 mg/m3, and.200 mg/m3. The relative errors are -11.8%～6.4%, -4.5%～0.0% and -8.9%～5.6%; the final values of the relative errors are respectively -1.1%±13.4%, -1.9%±3.9%, -1.8%±11.0%. 12 Quality Assurance and Quality Control 12.1 After the sample is measured, measure the zero point gas and nitric oxide standard gas according to 9.4, calculate the measured indication error, and check the instrument The system error of the device should meet the requirements of 7.1.2 a) and b). It can also include sampling pipes, air ducts, dehumidification devices, etc. The inspection of the indication error of the whole system shall be evaluated according to the requirements of 7.1.2 a). When the measurement result of nitrogen dioxide exceeds this method At the lower limit, it should also be checked for indication error, system deviation or the whole system indication error. 12.2 The measurement result of the sample should be between 20% and 100% of the calibration range of the instrument......

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