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HJ 1043-2019Ambient air - Automatic determination of nitrogen oxides - Chemiluminescence method (English PDF)

环境空气 氮氧化物的自动测定 化学发光法

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Issued by

Ministry of Ecology and Environment

Level / Type

National · Mandatory

Issue date

January 1, 1970

Implementation date

April 24, 2020

Scope

HJ 1043-2019 is the English-translated version of 环境空气 氮氧化物的自动测定 化学发光法.

HJ 1043-2019 — This standard specifies the chemiluminescence method for automatic determination of nitrogen oxides in ambient air. This standard applies to the automatic determination of nitric oxide, nitrogen dioxide and nitrogen oxides in ambient air.

When the measuring range of the instrument is (0 ~ 500) nmol/mol, the nitrogen oxide, nitrogen dioxide and the NOx detection limits are 1 µg/m3, 3 µg/m3, and 2 µg/m3, and the lower detection limits are 4 µg/m3, 12 µg/m3, and 8 µg/m 3; Under standard conditions, the detection limits of nitrogen oxide, nitrogen dioxide and nitrogen oxide are 2 µg/m3, 3 µg/m3 and 2 µg/m 3. The lower detection limits are 8 µg/m3, 12 µg/m3 and 8 µg/m3, respectively.

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Document preview — HJ 1043-2019

National Standard of the People's Republic of China

ICS
13.040.20
Classification
Z 15

Issued by: Ministry of Ecology and Environment

Contents

  • Foreword
  • 1 Scope
  • 2 Normative references
  • 3 Methodology
  • 4 Interference and cancellation
  • 5 Reagents and materials
  • 6 Instruments and equipment
  • 7 Analysis steps
  • 8 Results calculation and representation
  • 9 Precision and accuracy
  • 10 Quality Assurance and Quality Control
  • 11 Notes

Foreword

In order to implement the "Environmental Protection Law of the People's Republic of China" Environment, protect human health, standardize automatic determination methods of nitrogen oxides in ambient air, and formulate this standard.

This standard specifies the chemiluminescence method for automatic determination of nitrogen oxides in ambient air.

This standard is issued for the first time.

This standard is formulated by the Department of Eco-Environmental Monitoring, Laws and Standards Department of the Ministry of Ecology and Environment.

This standard was drafted. Dalian Ecological Environment Monitoring Center, Liaoning Province.

Verification units of this standard. Harbin Environmental Monitoring Center Station, Hangzhou Environmental Monitoring Center Station, Anshan Ecology, Liaoning Province Environmental Monitoring Center, Guangzhou Environmental Monitoring Center Station, Shenyang Ecological Environment Monitoring Center in Liaoning Province and Qingdao Ecological Environment Center in Shandong Province Environmental Monitoring Center.

This standard was approved by the Ministry of Ecology and Environment on October 24, 2019.

This standard will be implemented from April 24, 2020.

This standard is explained by the Ministry of Ecology and Environment.

Chemiluminescence method for automatic determination of nitrogen oxides in ambient air Warning. Nitric oxide is a toxic gas. Prevent leakage during operation, and perform protective work as required.

1 Scope

This standard specifies the chemiluminescence method for automatic determination of nitrogen oxides in ambient air.

This standard applies to the automatic determination of nitric oxide, nitrogen dioxide and nitrogen oxides in ambient air.

When the measuring range of the instrument is (0 ~ 500) nmol/mol, the nitrogen oxide, nitrogen dioxide and the NOx detection limits are 1 µg/m3, 3 µg/m3, and 2 µg/m3, and the lower detection limits are 4 µg/m3, 12 µg/m3, and 8 µg/m 3; Under standard conditions, the detection limits of nitrogen oxide, nitrogen dioxide and nitrogen oxide are 2 µg/m3, 3 µg/m3 and 2 µg/m 3. The lower detection limits are 8 µg/m3, 12 µg/m3 and 8 µg/m3, respectively.

2 Normative references

This standard refers to the following documents or clauses therein. For undated references, the valid version applies to this standard.

HJ 193 Ambient air gaseous pollutants (SO2, NO2, O3, CO) continuous automatic monitoring system installation and acceptance technology specification HJ 654 Ambient air gaseous pollutants (SO2, NO2, O3, CO) continuous automatic monitoring system technical requirements and inspection Test method HJ 663 Technical Specification for Ambient Air Quality Evaluation (Trial) HJ 818 Ambient air gaseous pollutants (SO2, NO2, O3, CO) continuous automatic monitoring system operation and quality control technology Technical specifications

3 Method principle

The sample air is divided into two channels, one of which directly enters the reaction chamber to measure nitric oxide; the other channel converts Nitrogen was converted into nitric oxide and entered the reaction chamber to measure nitrogen oxides. Nitric oxide in the reaction chamber is oxidized by excess ozone the excited state of nitrogen dioxide molecules emit light during the return to the ground state, and the concentration of nitric oxide in the sample air within a certain concentration range the intensity is directly proportional to the light intensity. The concentration of nitrogen dioxide is calculated from the difference between the concentration of nitrogen oxides and nitric oxide.

4 Interference and cancellation

In the process of determination, in addition to the conversion of nitrogen dioxide to nitric oxide, the molybdenum catalytic converter also contains gaseous compounds such as ammonia.

Nitrogen compounds are partially or completely converted to nitric oxide, which positively interferes with the measurement results.

5 Reagents and materials

5.1 Zero gas. Zero gas is generated by a zero gas generating device, and can also be provided by a zero gas cylinder. The performance index of zero gas should meet HJ 654 Requirements. If synthetic air is used, the oxygen concentration shall be (20.9 ± 2.0)% of the synthetic air.

5.2 Standard gas. Certified reference material for nitric oxide, the unit is µmol/mol.

5.3 Filter membrane. The material is polytetrafluoroethylene, and the pore size is <=5 µm.

6 Instruments and equipment

6.1 Sample injection pipeline. should be polytetrafluoroethylene, fluorinated polyethylene propylene, stainless steel that does not react with nitrogen oxides or borosilicate glass.

6.2 Particulate matter filter. installed between the sampling manifold and the instrument inlet. Particle filter other than the filter membrane it should be polytetrafluoroethylene, fluorinated polyethylene propylene, stainless steel or borosilicate glass that does not react with nitrogen oxides.

And other materials. The instrument does not require an external particulate filter if it has a built-in particulate filter.

6.3 Nitrogen oxide analyzer. Divided into dual reaction chamber dual detector type, dual reaction chamber single detector type and single reaction chamber single detection Device, the system components are shown in Figure 1, Figure 2 and Figure 3 respectively. Performance indicators should meet the requirements of HJ 654.

1-air inlet; 2-roof; 3-fan; 4-dehumidifying device; 5-injection pipeline; 6-way valve; 7-zero gas; 8-standard gas; 9- particulate filter;

10-dryer; 11-nitrogen oxide analyzer; 12-nitrogen dioxide converter (molybdenum catalysis); 13-ozone generator; 14-flow controller; 15-reaction Chamber 16-signal output; 17-data output; 18-ozone remover; 19-pump; 20-evacuation port.

Figure 1 Schematic diagram of a dual-reactor dual-detector NOx measurement system

1-air inlet; 2-roof; 3-fan; 4-dehumidifying device; 5-injection pipeline; 6-way valve; 7-zero gas; 8-standard gas; 9- particulate filter;

10-dryer; 11-nitrogen oxide analyzer; 12-nitrogen dioxide converter (molybdenum catalyst); 13-ozone generator; 14-flow controller; 15-reverse Application room 16-signal output; 17-data output; 18-ozone remover; 19-pump; 20- emptying port.

Figure 2 Schematic diagram of a dual-reactor single-detector NOx measurement system

1-air inlet; 2-roof; 3-fan; 4-dehumidifying device; 5-injection pipeline; 6-way valve; 7-zero gas; 8-standard gas; 9- particulate filter;

10-dryer; 11- nitrogen oxide analyzer; 12- sequence controller; 13- nitrogen dioxide converter (molybdenum catalysis); 14- ozone generator; 15- flow Controller; 16-reaction chamber; 17-signal output; 18-data output; 19-ozone remover; 20-pump; 21- emptying port.

Figure 3 Schematic diagram of single-reactor single-detector NOx measurement system

7 Analysis steps

7.1 Installation and commissioning of the instrument

After the newly purchased instrument is installed, various parameters should be set and debugged according to the operation manual. Debugging indicators include zero noise, Minimum detection limit, range noise, indication error, range accuracy, 24 h zero point drift and 24 h range drift.

The detection methods and indicators are implemented in accordance with HJ 193.

7.2 Inspection

During the operation of the instrument, zero point check, range check, linearity check, and converter conversion efficiency check are required.

The method was performed according to Appendix B in HJ 818. If the inspection results are unsatisfactory, the instrument needs to be calibrated, if necessary, the instrument Make repairs.

After the instrument is repaired, perform a linear check and recalibrate the instrument.

7.3 Calibration

7.3.1 Determine instrument range

Instrument range should be determined according to the actual concentration of nitrogen oxides in different seasons. When the NOx concentration is below the range at 20%, a lower range should be selected.

7.3.2 Calibration procedure

7.3.2.1 Pass zero gas into the instrument and adjust the output value of the instrument to zero after the reading is stable.

7.3.2.2 Pass a standard gas with a concentration of 80% of the range into the instrument. After the reading is stable, adjust the output value of the instrument to be equal to the standard.

Gas concentration value.

7.4 Determination of samples

The sample air was passed into the instrument for automatic determination and recording of the volumetric concentrations of nitric oxide and nitrogen oxides.

8 Results calculation and representation

8.1 Calculation of results

When used for ambient air quality monitoring, fugitive emissions monitoring or indoor air quality monitoring, Result calculations are performed for the states required by the emission standards and emission standards.

The mass concentrations of nitric oxide, nitrogen dioxide, and nitrogen oxides (the results are measured in terms of nitrogen dioxide) are based on formula (1), (2), (3) Calculation.

In the formula. rho (NO)-mass concentration of nitric oxide, µg/m 3;

30-Molar mass of nitric oxide, g/mol;

Vm-molar volume of nitric oxide, 22.4 in the standard state and 24.5 in the reference state, L/mol;

NO ()-Volumetric concentration of nitric oxide, nmol/mol.

NONO

Where. rho (NO

)-Mass concentration of nitrogen dioxide, µg/m 3;

46-Molar mass of nitrogen dioxide, g/mol;

Vm-molar volume of nitrogen dioxide, 22.4 in the standard state and 24.5 in the reference state, L/mol;

NO )XNO

-Volumetric concentration of nitrogen oxides, nmol/mol.

NO ()-Volumetric concentration of nitric oxide, nmol/mol.

eta-the conversion efficiency of nitrogen dioxide, when eta>=98%, eta = 1; when 96% <=eta < 98%, eta is true International conversion efficiency.

XX NO

Where. rho (NO

)-Mass concentration of nitrogen oxides, µg/m 3;

46-Molar mass of nitrogen dioxide, g/mol;

Vm-molar volume of nitrogen oxides, 22.4 in the standard state and 24.5 in the reference state, L/mol;

NO )XNO

-Volumetric concentration of nitrogen oxides, nmol/mol.

8.2 Results representation

The measurement results are reserved in whole digits, and the statistical method of monitoring data used for air quality evaluation is implemented in accordance with HJ 663.

9 Precision and accuracy

9.1 Precision

Six laboratories performed 6 nitric oxide standard gases at concentrations of 5 µg/m3, 119 µg/m3, and 549 µg/m3 Repeated determination. The relative standard deviations in the laboratory were 1.8% to 4.1%, 0.1% to 1.9%, and 0.1% to 0.5%, respectively.

The relative standard deviations are 2.8%, 0.9% and 0.4% respectively; the repeatability limits are 1 µg/m3, 4 µg/m3 and 6 µg/m3;

Reproducibility limits are 1 µg/m3, 5 µg/m3, and 9 µg/m3, respectively.

9.2 Accuracy

Six laboratories performed 6 nitric oxide standard gases at concentrations of 5 µg/m3, 119 µg/m3, and 549 µg/m3 Repeated measurement. the relative errors are -0.1% to 3.0%, -1.4% to 0.9%, and -0.7% to 0.8%; the final value of the relative error is They are 1.2% ± 2.8%, -0.4% ± 2.2%, and 0.3% ± 1.4%.

10 Quality Assurance and Quality Control

10.1 Instrument zero check, range check, linearity check, flow rate check, conversion efficiency check, calibration frequency and indicators Follow HJ 818.

10.2 The filter holder of the particulate filter is cleaned at least once every six months; the filter is generally replaced every two weeks, and the particulate matter is concentrated.

In areas with high temperature or high concentration periods, the frequency of replacement should be increased depending on the actual pollution of the filter membrane.

10.3 The sampling pipeline should be checked for air tightness monthly, cleaned every six months, and replaced if necessary.

11 Matters needing attention

11.1 After replacing the sampling system components and membranes, the sample air should be collected at a normal flow rate for at least 10 minutes and saturated for suction.

With processing, the measurement data generated during the period is not regarded as valid data. This process can also be performed in the laboratory.

11.2 Excess ozone shall be removed by activated carbon.

11.3 Sulfide and carbonyl compounds will reduce the conversion efficiency of molybdenum-catalyzed converters.

At 96%, the molybdenum catalyst should be replaced immediately.

......
This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 6 pages — is available in the English PDF.

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