Specifications for carbon analysis of atmospheric aerosol by filter sampling
other information
drafter:Bai Zhipeng, Liu Aixia, Yang Wen, Wang Jing, Geng Chunmei, Han Bin, Zhao Xueyan, Wu Jianhui, Gao Lingyun, Sun Feng, Zhang Changchun, Li Weifang, Huo Jing, Zhang Can, Wu Can, Wang Wan
Drafting unit:Nankai University, Tianjin Meteorological Science Institute, Chinese Academy of Environmental Sciences
Focal point unit:National Technical Committee for Climate and Climate Change Standardization Technical Committee on Atmospheric Composition Observation, Forecast and Warning Services (SAC/TC 540/SC 1)
Proposing unit:National Technical Committee for Climate and Climate Change Standardization Technical Committee on Atmospheric Composition Observation, Forecast and Warning Services (SAC/TC 540/SC 1)
Publishing department:China Meteorological Administration
competent authority:National Technical Committee for Climate and Climate Change Standardization Technical Committee on Atmospheric Composition Observation, Forecast and Warning Services (SAC/TC 540/SC 1)
Introduction to standards:
Standard number: QX/T 508-2019
Standard name: Specifications
for carbon analysis of atmospheric aerosol by filter sampling
English name: Specifications for carbon analysis of atmospheric aerosol by filter sampling
Standard format: PDF
Release time: 2019-09-30
Implementation time: 2020-01-01
Standard size: 1767K
Standard introduction: This standard was drafted in accordance with the rules given in GB/T1.1-2009
This standard was drafted by the Sub-Technical Committee on Atmospheric Composition Observation, Forecast and Warning Services of the National Technical Committee for Climate and Climate Change Standardization (SAC
TC540/SC1) proposed and coordinated
Drafting units of this standard: Nankai University, Tianjin Meteorological Science Institute, Chinese Research Academy of Environmental Sciences Main drafters of this standard: Zi Zhipeng, Liu Aixia, Yang Wen, Wang Jing, Geng Chunmei, Han Bin, Zhao Xueyan, Wu Jianhui, Gao Lingyun, Sun Feng, Zhang Changchong, Li Weifang, Huo Jing, Zhang Can, Wu Can, Wang Wan
Accurate determination of carbon components in atmospheric aerosols is of great significance for understanding the physical and chemical properties and formation mechanism of atmospheric aerosol particles, evaluating the radiative forcing effect of atmospheric aerosols, assessing the degree of atmospheric aerosol pollution and tracing the source of atmospheric aerosol pollution. This standard is specially formulated to improve the accuracy and comparability of the monitoring results of atmospheric aerosol carbon components and to standardize the film sampling and analysis methods of atmospheric aerosol carbon components. This standard specifies the reagents and gases, instruments and materials, sampling, analysis, instrument calibration, result
calculation, data quality control and precautions
for film sampling and analysis of atmospheric aerosol carbon components. This standard applies to film sampling and analysis of atmospheric aerosol carbon components using thermo-optical analysis .
2 Normative referenced documents
The following documents are indispensable for the application of this document. For any dated referenced document, only the dated version applies to this document. For any undated referenced document, the latest version (including all amendments) applies to this document.
H93-2013 Technical requirements and detection methods for ambient air particulate matter (PM1o and PM25) samplers H656-2013 Technical specifications for manual monitoring method (weight method) of ambient air particulate matter (PM23) QX/T118-2010 Quality control of ground meteorological observation data
QX/T305-2015 Technical specifications for weighing atmospheric aerosol filters with a diameter of 47 mm 3 Terms and definitions
The following terms and definitions apply to this document
Atmospheric aerosol particlesatmospheric aerosol part icle
Atmospheric particulate matter
Solid and liquid particles suspended in the atmosphere
LGB/T31159-2014 Definition 2.2]
This standard specifies the reagents, instruments and materials, sampling, analysis, instrument calibration, result calculation, data quality control and precautions for sampling and analysis of atmospheric aerosol carbon components. This standard applies to film sampling and analysis of atmospheric aerosol carbon components using thermo-optical analysis.
Some standard content:
ICS07.060
Meteorological Industry Standard of the People's Republic of China
QX/T508—2019
Specifications for carbon analysis of atmospheric aerosol by filter samplingIndustry Standard Information Service Platform
Published on September 30, 2019
China Meteorological Administration
Implementation on January 1, 2020
Industry Standard Information Service Platform
Normative Reference Documents
3 Terms and Definitions
4 Reagents and Gases
4.1 Reagents
4.2 Gases
5 Instruments and Materials
Sampling Instruments
Analyzers tt||Other instruments, equipment and materials
6 Sampling
Pretreatment, weighing and storage of filter membrane
On-site sampling
Pre-analysis check
Instrument stability check
Instrument blank analysis
Sample analysis
Analysis result check
8 Instrument calibration
Sampling instrument calibration
8.2 Analytical instrument calibration
General requirements
Drawing standard curve
Result calculation
Instrument analysis results
Mass concentration under standard conditions
Data summary
Data quality control
Notes
Appendix A (Informative Appendix)
Appendix B (Informative Appendix)
Appendix C (Informative Appendix)
Appendix D (Informative Appendix)
Appendix E (Informative Appendix)
Appendix F (Informative Appendix)||tt| |Filter membrane tracking form
Carbon analysis sample delivery form and data analysis record formSample collection record form
Calculation method of sampling area
Preparation method of standard solution
Sample data analysis summary table
QX/T508—2019
QX/T508—2019
References
Industry standard information service platform
This standard is drafted in accordance with the rules given in GB/T1.1—2009. QX/T508-2019
This standard is proposed and managed by the Sub-Technical Committee on Atmospheric Composition Observation, Forecast and Warning Services of the National Technical Committee for Climate and Climate Change Standardization (SAC) TC540/SC1).
The drafting units of this standard: Nankai University, Tianjin Meteorological Science Institute, Chinese Academy of Environmental Sciences The main drafters of this standard: Bai Zhipeng, Liu Aixia, Yang Wen, Wang Jing, Geng Chunmei, Han Bin, Zhao Xueyan, Wu Jianhui, Gao Lingyun, Sun Feng, Zhang Changchun, Li Weifang, Huo Jing, Zhang Can, Wu Can, Wang Wan. Industry Standard Information Service Platform
Industry Standard Information Service Platform
QX/T508—2019
Accurate determination of carbon components in atmospheric aerosols is of great significance for understanding the physical and chemical properties and formation mechanism of atmospheric aerosol particles, evaluating the radiative forcing effect of atmospheric aerosols, evaluating the degree of atmospheric aerosol pollution, and tracing the source of atmospheric aerosol pollution. This standard is specially formulated to improve the accuracy and comparability of the monitoring results of weather aerosol carbon components and standardize the membrane sampling and analysis method of atmospheric aerosol carbon components. Industry Standard Information Service Platform
Industry Standard Information Service Platform
1 Scope
Specification for Film Sampling and Analysis of Carbon Components in Atmospheric Aerosols QX/T508—2019
This standard specifies the reagents and gases, instruments and materials, sampling, analysis, instrument calibration, result calculation, data quality control and precautions for film sampling and analysis of carbon components in atmospheric aerosols. This standard applies to film sampling and analysis of carbon components in atmospheric aerosols using thermo-optical analysis. 2 Normative Reference Documents
The following documents are indispensable for the application of this document. For any dated referenced document, only the dated version applies to this document. For any undated referenced document, its latest version (including all amendments) applies to this document. HJ93-2013 Technical requirements and detection methods for ambient air particulate matter (PMi, and PM2.5) samplers HJ656-2013 Technical specifications for manual monitoring methods (weight method) for ambient air particulate matter (PM2.) QX/T118-2010 Quality control of ground meteorological observation data QX/T305-2015 Technical specifications for weighing atmospheric aerosol filters with a diameter of 47 mm 3 Terms and definitions
The following terms and definitions apply to this document. 3.1
atmospheric aerosol particle
Atmospheric particulate matter
Solid and liquid particles suspended in the atmosphere. [GB/T31159—2014, definition 22]
Carbon organic carbon; OC
Organic carbon
Ya Information Service
Carbon components in organic matter such as hydrocarbons, hydrocarbon derivatives, multi-energy solid derivatives and polymer compounds in aerosol particles. [GB/T31159—2014, definition 5.2]
Elemental carbon elemental carbon; EC
Service Platform
Highly polymerized, black, difficult to be oxidized below 400°C, and showing chemical, water-loving, and insoluble in any solvent atmospheric carbon components at room temperature.
[GB/T31159—2014, definition 5.3]
Total carbon total carbon; TC
The sum of organic carbon (3.2) and elemental carbon (3.3) in aerosol particles. [GB/T31159—2014, definition 5.4]
QX/T508—2019
Optical pyrolyzed carbon opticalpyrolyzedcarbon;OPC Organic carbon converted into elemental carbon by pyrolysis at high temperature measured by optical methods. 3.6
carbonatecarbon;ccbzxZ.net
Carbonate carbon
Carbon in the form of carbonate or bicarbonate in atmospheric aerosol particles. 3.7
thermalopticalmethod
Thermo-optical analysis method
A method for measuring the organic carbon and elemental carbon content in filter membrane samples by combining heating pyrolysis and optical segmentation based on the differences in the physicochemical properties of carbon components in atmospheric aerosol particles and the changes in optical properties during pyrolysis. Note: Optical segmentation includes reflection method and transmission method, and thermo-optical analysis method is divided into thermal reflection method and thermal transmission method. 4 Reagents and gases
4.1 Reagents
Reagents that meet the following requirements should be used:
Potassium hydrogen phthalate (CH(COOK) (COOH)): analytical grade or above; Sucrose (Ci2H22Ou): analytical grade or above; Hydrochloric acid (HCl, 0.4mol/L): analytical grade or above; Ultrapure water: The resistivity at 25°C is greater than or equal to 18.2M2·cm. 4.2 Gases
Gases that meet the following requirements should be used:
Ammonia (He): purity greater than or equal to 99.999%; Hydrogen (H2): purity greater than or equal to 99.999%; Ammonia-oxygen mixed gas (He): made of ammonia and oxygen with purity greater than or equal to 99.999% in a ratio of 9:1; Ammonia-methane mixed standard gas (HeCH): made of ammonia and methane with purity greater than or equal to 99.999% in a ratio of 19:1. Made of:
Quasi-information service platform
Dry clean air: a mixed gas in the atmosphere except water vapor, liquid, solid particles and organic matter 5 Instruments and materials
5.1 Sampling instrument
Sampling instruments that meet the requirements of Chapter 5 of HJ93-2013 should be used 5.2 Analytical instruments
5.2.1 Working principle
Thermo-optical carbon analyzer is used to analyze the concentration of atmospheric carbon aerosol: thermal light reflection method and thermal light transmission method are used. The main principle of this method is: organic carbon (OCHe) released in pure ammonia environment and elemental carbon (ECo,+He) is oxidized to CO under the action of a catalyst, which can be directly detected by a non-dispersive infrared detector (NDIR), or CO is reduced to CH and detected by a flame ionization detector (FID) in a hydrogen environment. During the analysis process, the sample is irradiated with a reflected laser or a transmitted laser throughout the entire process, and the initial light intensity signal is used as a reference. When organic carbon begins to crack, the light intensity signal decreases. As oxygen continues to flow in, the light intensity signal will rise again. The point at which the initial light intensity signal returns to the initial light intensity signal is set as the OC and EC split point to obtain optical cracking carbon (OPC). 5.2.2 Instrument composition, technical requirements and performance indicators The thermal optical carbon analyzer consists of a host, an oxidation furnace, a detector and a laser detector. Depending on the detector, a reduction furnace can be optionally equipped.
TC measurement range: 0.05uμg/cm~750μg/cm; detection limit: 0.93μg/cm; precision: about 10%; accuracy: 2%~6%.
5.3 Other instruments, equipment and materials
5.3.1 Sampler
Should be made of alloy steel. It is advisable to use a circular sampler with a diameter of 10mm and 5mm or a rectangular sampler with a side length of 1cm×1cm and 1.5cm×1cm. Different sizes can be customized according to actual needs. 5.3.2 Syringe
Should be equipped with one 10μL and one 25μL syringe. 5.3.3 Balance
Should meet the requirements of Chapter 4 of QX/T305-2015 5.3.4 Filter membrane
Quartz fiber filter membrane should be used.
5.3.5 Auxiliary instruments and materials
Some elements
Filter membrane box, aluminum foil, sealing bag, tweezers, glass plate, dust-free paper, volumetric flask, beaker, glass rod, muffle furnace, indoor ventilation equipment, etc. 6 Sampling
6.1 Pretreatment, weighing and storage of filter membrane
6.1.1 Pretreatment
Before sampling, the quartz fiber filter membrane should be placed in a 550℃ muffle furnace for measurement, and the TC should be less than 1ug/cm
6.1.2 Weighing
Your service platform
The operation should be carried out in accordance with the requirements of Chapter 5 of QX/T305-2015. 6.1.3 Storage requirements are as follows: After weighing and sampling, the filter membrane should be placed in a filter membrane box, wrapped with aluminum foil, and then sealed in a sealing bag for storage; during transportation, it should be stored in a 0℃~4℃ constant temperature box to prevent falling and shock; before analysis, the sample filter membrane should be sealed and refrigerated at 0℃~4℃ for no longer than 30 days; 3
QX/T5082019
Each filter membrane should be accompanied by a full tracking table. The table style is shown in Appendix A. The filter membrane used for carbon analysis should fill in the carbon analysis sample submission form, see Table B.1 and Table B.2 in Appendix B. 6.2 On-site sampling
On-site sampling should comply with Chapter 6 and the following requirements of HJ656-2013: The filter membrane after sampling should be photographed and preserved, and the photos should be numbered and recorded by date and type. The form style is shown in Table B.2 in Appendix B;
- Fill in the sample collection record form. The form style is shown in Appendix C7 Analysis
7.1 Pre-analysis inspection
Perform a pre-analysis inspection according to the instrument operating instructions. The items are as follows: Check the gas cylinder pressure;
Check the airtightness of the instrument;
- Check the furnace temperature;
- Check the gas flow.
7.2 Instrument stability check
Three peak detection or single point detection can be used to check the instrument stability. The inspection requirements are as follows: Three peak detection: get three peak areas in the anaerobic stage, aerobic stage and internal standard peak stage respectively. The relative standard deviation of the peak area should be less than 5%. Otherwise, check the cylinder pressure, air tightness, carrier gas flow, replacement of oxidation tube or methane conversion tube, etc.; Single point detection: on the blank quartz fiber filter membrane with TC less than 0.5μg/cm2 measured after baking. Use a syringe to drop 10uL potassium hydrogen phthalate or sucrose standard solution for three repeated analyses. The relative standard deviation of TC should be less than 5%. Otherwise, check the cylinder pressure, gas flow, air tightness, replacement of oxidation tube or methane conversion tube, etc. After meeting the requirements, the average value of TC mass calculated from the three repeated analyses and the relative error of the mass of carbon in the standard solution should be within ±5% (TC mass is TC measured value multiplied by 1cm), otherwise the instrument should be recalibrated; Stability check should be done before each analysis and after 24b of continuous operation. 7.3 Instrument blank analysis
Before starting the analysis of the membrane sample, the membrane holder or blank quartz fiber filter should be analyzed. The TC measurement value should be less than 0.5ug/cm. Otherwise, the instrument blank analysis should be repeated, or the air tightness of the analytical instrument and the degree of cleanliness of the holder should be checked. 7.4 Sample analysis
7.4.1 Place the filter on a clean glass plate and use a sampler to intercept the filter sample in the effective sampling area of the filter. Multiple filter samples can be intercepted as needed, and the remaining filter membranes are returned to the filter box for standby use. Each time a filter sample is intercepted, the plate probe and sampler should be cleaned with dust-free paper.
7.4.2 Record the filter number, analysis procedure, sampler area (see Appendix D for calculation method), filter effective deposition area and other information, and start the analysis.
7.4.3After each sample is analyzed, the instrument will automatically inject a quantitative amount of ammonia-methane standard gas for analysis to obtain the corrected peak area, which will be used in the calculation of organic carbon and elemental carbon.
7.4.4After the analysis of the previous sample is completed, wait for the furnace temperature to drop below 50°C, take out the analyzed filter membrane sample and paste it on the data analysis record.2 Instrument stability check
Three peak detection or single point detection can be used to check the instrument stability. The inspection requirements are as follows: Three peak detection: get three peak areas in the anaerobic stage, aerobic stage and internal standard peak stage respectively. The relative standard deviation of the peak area should be less than 5%, otherwise the cylinder pressure, air tightness, carrier gas flow rate, replacement of oxidation tube or methane conversion tube, etc. should be checked; Single point detection: on the blank quartz fiber filter membrane with TC less than 0.5μg/cm2 measured after baking. Use a syringe to drop 10uL of potassium hydrogen phthalate or sucrose standard solution for three repeated analyses. The relative standard deviation of TC should be less than 5%, otherwise the cylinder pressure, gas flow rate, air tightness, replacement of oxidation tube or methane conversion tube, etc. should be checked. After meeting the requirements, the average value of TC mass calculated from three repeated analyses and the relative error of the mass of carbon in the standard solution should be within ±5% (TC mass is TC measurement value multiplied by 1cm), otherwise the instrument should be recalibrated; Stability check should be done before each analysis and after 24b of continuous operation. 7.3 Instrument blank analysis
Before starting the analysis of the membrane sample, the membrane holder or blank quartz fiber filter should be analyzed. The TC measurement value should be less than 0.5ug/cm. Otherwise, the instrument blank analysis should be repeated, or the air tightness of the analytical instrument and the degree of cleanliness of the holder should be checked. 7.4 Sample analysis
7.4.1 Place the filter on a clean glass plate and use a sampler to intercept the filter sample in the effective sampling area of the filter. Multiple filter samples can be intercepted as needed, and the remaining filter membranes are returned to the filter box for standby use. Each time a filter sample is intercepted, the plate probe and sampler should be cleaned with dust-free paper.
7.4.2 Record the filter number, analysis procedure, sampler area (see Appendix D for calculation method), filter effective deposition area and other information, and start the analysis.
7.4.3After each sample is analyzed, the instrument will automatically inject a quantitative amount of ammonia-methane standard gas for analysis to obtain the corrected peak area, which will be used in the calculation of organic carbon and elemental carbon.
7.4.4After the analysis of the previous sample is completed, wait for the furnace temperature to drop below 50°C, take out the analyzed filter membrane sample and stick it on the data analysis record.2 Instrument stability check
Three peak detection or single point detection can be used to check the instrument stability. The inspection requirements are as follows: Three peak detection: get three peak areas in the anaerobic stage, aerobic stage and internal standard peak stage respectively. The relative standard deviation of the peak area should be less than 5%, otherwise the cylinder pressure, air tightness, carrier gas flow rate, replacement of oxidation tube or methane conversion tube, etc. should be checked; Single point detection: on the blank quartz fiber filter membrane with TC less than 0.5μg/cm2 measured after baking. Use a syringe to drop 10uL of potassium hydrogen phthalate or sucrose standard solution for three repeated analyses. The relative standard deviation of TC should be less than 5%, otherwise the cylinder pressure, gas flow rate, air tightness, replacement of oxidation tube or methane conversion tube, etc. should be checked. After meeting the requirements, the average value of TC mass calculated from three repeated analyses and the relative error of the mass of carbon in the standard solution should be within ±5% (TC mass is TC measurement value multiplied by 1cm), otherwise the instrument should be recalibrated; Stability check should be done before each analysis and after 24b of continuous operation. 7.3 Instrument blank analysis
Before starting the analysis of the membrane sample, the membrane holder or blank quartz fiber filter should be analyzed. The TC measurement value should be less than 0.5ug/cm. Otherwise, the instrument blank analysis should be repeated, or the air tightness of the analytical instrument and the degree of cleanliness of the holder should be checked. 7.4 Sample analysis
7.4.1 Place the filter on a clean glass plate and use a sampler to intercept the filter sample in the effective sampling area of the filter. Multiple filter samples can be intercepted as needed, and the remaining filter membranes are returned to the filter box for standby use. Each time a filter sample is intercepted, the plate probe and sampler should be cleaned with dust-free paper.
7.4.2 Record the filter number, analysis procedure, sampler area (see Appendix D for calculation method), filter effective deposition area and other information, and start the analysis.
7.4.3After each sample is analyzed, the instrument will automatically inject a quantitative amount of ammonia-methane standard gas for analysis to obtain the corrected peak area, which will be used in the calculation of organic carbon and elemental carbon.
7.4.4After the analysis of the previous sample is completed, wait for the furnace temperature to drop below 50°C, take out the analyzed filter membrane sample and stick it on the data analysis record.
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