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HJ 1079-2019: Stationary source emission--Determination of chlorobenzenes--Gas chromatography
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Stationary source emission--Determination of chlorobenzenes--Gas chromatography
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HJ 1079-2019
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Basic data | Standard ID | HJ 1079-2019 (HJ1079-2019) | | Description (Translated English) | Stationary source emission--Determination of chlorobenzenes--Gas chromatography | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z25 | | Classification of International Standard | 13.040.40 | | Word Count Estimation | 17,113 | | Date of Issue | 2019 | | Date of Implementation | 2020-06-30 | | Issuing agency(ies) | Ministry of Ecology and Environment | HJ 1079-2019: Stationary source emission--Determination of chlorobenzenes--Gas chromatography---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.
Stationary source emission--Determination of chlorobenzenes--Gas chromatography
National Environmental Protection Standard of the People's Republic of China
Replacing HJ/T 39-1999, HJ/T 66-2001
Exhaust gas from stationary sources
Determination of chlorobenzene compounds by gas chromatography
Stationary source emission-Determination of chlorobenzenes
-Gas chromatography
2019-12-31 release
2020-06-30 Implementation
Published by the Ministry of Ecology and Environment
i directory
Foreword ... ii
1 Scope ... 1
2 Normative references ... 1
3 Method principle ... 1
4 Reagents and materials ... 1
5 Instruments and equipment ... 2
6 Sample ... 3
7 Analysis steps ... 5
8 Calculation and presentation of results ... 6
9 Precision and accuracy ... 7
10 Quality Assurance and Quality Control ... 7
11 Waste disposal ... 8
Appendix A (Normative Appendix) The detection limit and lower limit of determination of the method ... 9
Appendix B (informative appendix) Precision and accuracy of the method ... 10
Appendix C (Informative) Chromatographic column selection ... 12
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
Environment, protect human health, regulate the measurement of chlorobenzene compounds in the air of fixed pollution sources and fugitive emission monitoring points
Determine the method and formulate this standard.
This standard stipulates the determination of chlorobenzene, 2-chlorotoluene and 3-chloromethyl in the air of stationary pollution sources and fugitive emission monitoring points
Benzene, 4-chlorotoluene, 1,3-dichlorobenzene, 1,4-dichlorobenzene, 1,2-dichlorobenzene, 1,3,5-trichlorobenzene, 1,2,4-trichlorobenzene , 1, 2, 3-
Gas chromatographic method of 10 kinds of chlorobenzene compounds such as chlorobenzene.
This standard refers to the "Gas Chromatography Method for the Determination of Chlorobenzenes in the Exhaust of Stationary Pollution Sources" (HJ/T 39-1999) and the "Atmosphere
Amendment to the determination of chlorobenzene compounds from stationary sources by gas chromatography (HJ/T 66-2001).
"Determination of Chlorobenzenes in Exhaust Gas from Stationary Sources of Gas Chromatography" (HJ/T 39-1999) was published in.1999, the original
The standard was drafted by the Shanghai Institute of Organic Chemistry, Chinese Academy of Sciences;
Gas Chromatography (HJ/T 66-2001) was released in.2001. The original standard drafting unit was Shenyang Environmental Monitoring Center Station.
This standard is the first revision of the above two standards. The main contents of the revision are as follows.
-The standard name was revised to "Determination of Chlorinated Benzene Compounds from Stationary Pollution Source Gas Chromatography"
-Added target compounds, chlorobenzene compounds increased from 3 to 10;
-Revised the detection limit of the method;
-Added activated carbon adsorption sampling method;
-Added the installation diagram of waste gas sampling system of fixed pollution source;
-Added quality assurance and quality control requirements.
Since the implementation of this standard, "Determination of Chlorobenzenes in Exhaust Gas from Stationary Pollution Sources by Gas Chromatography" (HJ/T 39-1999)
At the same time as the "Gas Chromatography Method for the Determination of Chlorobenzenes from Stationary Air Pollution Sources" (HJ/T 66-2001).
Appendix A of this standard is a normative appendix, and Appendix B and Appendix C are informative appendices.
This standard is organized and revised by the Eco-Environmental Monitoring Department and the Regulations and Standards Department of the Ministry of Ecology and Environment.
This standard was drafted by. Zhejiang Environmental Monitoring Center.
Verification unit of this standard. Hangzhou Environmental Monitoring Center Station, Ningbo Environmental Monitoring Center, Shaoxing Environmental Monitoring Center
Station, Huzhou Environmental Protection Monitoring Center Station, Jiaxing Environmental Protection Monitoring Station and Hangzhou Xiaoshan District Environmental Monitoring Station.
This standard was approved by the Ministry of Ecology and Environment on December 31,.2019.
This standard will be implemented from June 30, 2020.
This standard is interpreted by the Ministry of Ecology and Environment.
1 Determination of chlorobenzene compounds in waste gas from stationary pollution sources by gas chromatography
Warning. The chlorobenzene compounds and carbon disulfide used in the experiment have certain toxicity. Sample preparation and dissolution
Liquid preparation should be carried out in a fume hood, and protective equipment should be worn as required to avoid direct contact with skin and clothing. Gas phase
The exhaust gas from the combustion of the chromatographic hydrogen flame ionization detector should be discharged to the outside through the exhaust hood.
1 Scope of application
This standard stipulates the determination of the gas phase color of chlorobenzene compounds in the air of stationary pollution sources and fugitive emission monitoring points
Notation.
This standard is applicable to chlorobenzene, 2-chlorotoluene, 3-chlorotoluene,
4-chlorotoluene, 1,3-dichlorobenzene, 1,4-dichlorobenzene, 1,2-dichlorobenzene, 1,3,5-trichlorobenzene, 1,2,4-trichlorobenzene, 1 , 2,3-Trichlorobenzene
Determination of 10 kinds of chlorobenzene compounds.
When the sampling volume of waste gas from a fixed pollution source is 10 L (standard state) and the volume of desorption liquid is 2.00 ml, the detection limit of the method
0.02 mg/m3 ～ 0.04 mg/m3, the lower limit of determination is 0.08 mg/m3 ～ 0.16 mg/m3;
When the gas sampling volume is 30 L (standard state) and the desorption solution volume is 1.00 ml, the method detection limit is 0.007 mg/m3 ～
0.01 mg/m3, the lower limit of determination is 0.028 mg/m3 ～ 0.04 mg/m3; see Appendix A for details.
2 Normative references
This standard refers to the following documents or their clauses. For the cited documents without date, the valid version applies to this
standard.
GB/T 16157 Determination of particulate matter in exhaust gas from stationary sources and sampling method of gaseous pollutants
Technical conditions of HJ/T 47 flue gas sampler
HJ/T 55 Technical Guidelines for the Monitoring of Unorganized Emissions of Air Pollutants
HJ/T 373 Technical Specifications for Quality Assurance and Quality Control of Fixed Pollution Source Monitoring (Trial)
Technical requirements and testing methods of HJ/T 375 ambient air sampler
HJ/T 397 Fixed source exhaust gas monitoring technical specification
3 Method principle
Chlorobenzene compounds in the air from stationary pollution sources and fugitive emission monitoring points are passed through GDX-103 adsorbent (styrene-
Divinylbenzene polymer) or activated carbon adsorbent, after desorption with carbon disulfide, the desorption liquid is separated by capillary gas chromatography
It is detected by hydrogen flame ionization detector, qualitative according to retention time, and quantified by external standard method.
4 Reagents and materials
Unless otherwise specified, analytically pure reagents that meet national standards are used in the analysis, and the experimental water is newly prepared without a target
Pure water of the compound.
24.1 Carbon disulfide (CS2). chromatographically pure, tested without interference peaks under the reference analysis conditions of gas chromatography (7.1)
The target compound concentration in the medium is below the detection limit of the method.
4.2 Dichloromethane (CH2Cl2). chromatographically pure.
4.3 Acetone (C3H6O). chromatographically pure.
4.4 Acetone-dichloromethane mixed solution. 19, ready for use immediately.
4.5 Standard stock solution. ρ = 1000 μg/ml.
Direct purchase of commercially available certified chlorobenzene standard solutions (carbon disulfide media), in accordance with the standard solution certificate requirements
It can also be prepared by using chlorobenzene standard compounds. After the standard stock solution is opened, the
The screwed brown compact bottle (5.5) is cryopreserved and stored for 3 months.
4.6 Standard use solution. ρ = 100 μg/ml.
Pipette the standard stock solution (4.5) of chlorobenzene compounds, dilute with carbon disulfide (4.1), and mix to a constant volume. Standard use
The solution is cryogenically stored in a brown tight bottle (5.5) with a Teflon liner screw cap, and the storage period is 1 month.
4.7 Adsorption sampling tube.
4.7.1 GDX-103 adsorption sampling tube.
The sampling tube is made of glass, the specification is Φ6 × (80 ～ 120) mm, and the two-stage particle size is 250 µm ～ 380 µm (60
Mesh ~ 40 mesh) GDX-103 adsorbent (styrene-divinylbenzene polymer), of which 100 mg in section A (sampling section),
Section B (indication section) 50 mg, see Figure 1 for details. Commercially available sampling tubes can be purchased.
The GDX-103 adsorbent was extracted with dichloromethane (4.2) under reflux for 16 h before use, and then mixed with acetone-dichloromethane
(4.4) Continue reflux extraction for 16 h, then place in a fume hood to evaporate the solvent to dryness (or use vacuum drying at 50 ℃ for 8 h),
Store in a sealed glass jar.
4.7.2 Activated carbon adsorption sampling tube.
The sampling tube is made of glass, the specification is Φ6 × (80 ～ 120) mm, and the two-stage particle size is 380 µm ～ 830 µm (40
Mesh ~ 20 mesh) Coconut shell activated carbon, of which 100 mg in section A (sampling section) and 50 mg in section B (indicating section), see Figure 1 for details.
Commercially available sampling tubes can be purchased.
1-glass wool; 2-GDX-103 or activated carbon;
A-100 mg GDX-103 or activated carbon; B-50 mg GDX-103 or activated carbon.
Figure 1 GDX-103 or activated carbon adsorption sampling tube
4.8 High purity nitrogen. purity ≥99.999%.
4.9 Hydrogen. purity ≥99.99%.
5 Instruments and equipment
5.1 Air sampler. sampling flow range 0.1 L/min ～ 1.0 L/min, accuracy ± 5%, other performance and technical indicators
Meet the requirements of HJ/T 375.
35.2 Sampling system for exhaust gas from stationary pollution sources. including sampling gun, refrigeration and dehumidification device, adsorption (absorption) sampling tube, flow
Controller and suction pump etc. Sampling flow range 0.1 L/min ～ 1.0 L/min, accuracy ± 5%, sampling gun should have heating and
Insulation function, heating temperature is not less than 120 ℃; other performance and technical indicators should comply with GB/T 16157, HJ/T 47, HJ/T
397 related requirements.
5.3 Gas chromatograph. with split/splitless inlet, programmed temperature function and hydrogen flame ionization detector
5.4 Chromatography column. Quartz capillary chromatography column, the stationary phase is 14% cyanopropylphenyl-86% dimethyl polysiloxane, 30 m ×
0.25 mm × 0.25 µm; or other equivalent chromatographic column.
5.5 Brown compact bottle. 2 ml, 4 ml, with PTFE liner and solid screw cap.
5.6 Ultrasonic cleaner. power.200W.
5.7 Commonly used instruments and equipment in general laboratories.
6 samples
6.1 Sample collection
6.1.1 Sampling of waste gas from stationary pollution sources
Determination of sampling location and sampling point, sampling frequency and sampling time of exhaust gas from fixed pollution sources, measurement and sampling of exhaust parameters
This kind of operation implements the relevant regulations of GB/T 16157, HJ/T 373 and HJ/T 397.
Figure 2 shows the exhaust gas sampling system for stationary pollution sources.
1- Exhaust flue; 2- Sampling gun; 3- Refrigeration and dehumidification device; 4- Three-way valve; 5- Adsorption sampling tube; 6- Bypass adsorption tube;
7- dryer; 8- thermometer; 9- pressure gauge; 10- flow controller; 11- air pump.
Figure 2 Schematic diagram of the exhaust gas sampling system of fixed pollution sources
At the sampling site, remove the seals at both ends of the adsorption sampling tube, and follow the Figure 2 with the fixed pollution source waste gas sampling system (5.2)
Connect, check the air tightness of the sampling system, adjust the flow rate of the sampling device, this sampling tube is only used to adjust the flow rate.
When sampling, remove the GDX-103 adsorption sampling tube (4.7.1) or the activated carbon adsorption sampling tube (4.7.2) at both ends,
Connect the B end of the adsorption sampling tube to the dryer with a silicone rubber tube, and the A end of the adsorption sampling tube to the refrigeration dehumidification device
After the sampling gun is heated to 120 ° C, insert it near the center of the exhaust pipe of the pollution source to maintain the temperature of the sampling gun at 120 ° C (with
4 Except for explosion-proof safety requirements, collect exhaust gas samples at a flow rate of 0.5 L/min for at least 10 minutes (according to the concentration of exhaust gas may be appropriate
Adjust the sampling time), and simultaneously record the sampling flow rate, sampling time, temperature and pressure of the gas in the sampling system, and production
Operating conditions and other information. Immediately after sampling, seal the ends of the sampling tube with a rubber cap to protect from light.
6.1.2 Air sampling at unorganized emission monitoring points
Arrangement of unorganized emission monitoring points, number of monitoring points, sampling frequency, sampling time, and sampling operation execution HJ/T 55
Relevant regulations.
When sampling, remove the GDX-103 adsorption sampling tube (4.7.1) or the activated carbon adsorption sampling tube (4.7.2) at both ends,
Connect the B end of the adsorption sampling tube to the air sampler (5.1) with a silicone rubber tube. The adsorption sampling tube is placed vertically and fixed on the
Sample position, collect air samples at a flow rate of 0.5 L/min ～ 1.0 L/min, and record the sampling flow rate, sampling time and sampling at the same time
Ambient temperature and atmospheric pressure. Immediately after sampling, seal the ends of the sampling tube with a rubber cap to protect from light.
6.1.3 Blank sample of the whole program
At least one GDX-103 adsorption sampling tube (4.7.1) or activated carbon adsorption sampling of the same batch should be taken with each sampling
The tube (4.7.2) is used as a blank sample of the whole program. After removing the seals on both ends of the adsorption sampling tube at the sampling site, it is connected to the sampler.
Do not start the sampler. After the sampling is finished, remove the adsorption sampling tube and immediately seal it with a rubber cap to protect it from light. Return with sample
laboratory.
6.2 Storage of samples
The samples should be stored away from light, and can be stored at 4 ℃ for 7 days. The refrigerated samples should be returned to room temperature before pretreatment.
6.3 Preparation of samples
6.3.1 Exhaust gas samples from stationary sources
Remove the GDX-103 adsorption sampling tube or activated carbon adsorption sampling tube that collects waste gas samples from fixed pollution sources.
Sealing caps, the adsorbents of section A and section B are transferred to 5 ml glass test tubes with stoppers, add 2.00 ml to each
Carbon disulfide (4.1), sealed, ultrasonically desorbed in an ultrasonic cleaner (5.6) for 1 min, and left to stand for about 30 min, to be tested.
6.3.2 Air samples from unorganized emission monitoring points
Remove the GDX-103 adsorption sampling tube or activated carbon adsorption sampling tube that collects air samples from the fugitive emission monitoring point
Sealing rubber caps at both ends, and the adsorbent of segment A and segment B were transferred to 5 ml glass test tubes with plugs, and added to each test tube
1.00 ml of carbon disulfide (4.1), sealed, ultrasonically desorbed in an ultrasonic cleaner (5.6) for 1 min, let stand for about 30 min, wait
Measurement.
6.3.3 Blank sample of the whole program
Prepare the whole procedure blank sample (6.1.3) according to the same procedure as the sample preparation (6.3.1) or (6.3.2)
Blank sample.
6.4 Preparation of blank samples
Take the same batch of GDX-103 adsorption sampling tube (4.7.1) or activated carbon adsorption sampling tube (4.7.2), according to the sample preparation
5 Prepare the blank sample in the same steps as (6.3.1) or (6.3.2).
7 Analysis steps
7.1 Reference analysis conditions of gas chromatography
Injection port. 260 ℃; splitless injection, split flow is started at 0.75 min, flow rate is 45 ml/min; injection volume is 1.0 µl.
Column temperature. hold at 40 ℃ for 4 min, increase to 80 ℃ at 4 ℃/min, then increase to 240 ℃ at 8 ℃/min for 1 min;
Gas. high purity nitrogen (4.8), column flow rate 1.8 ml/min.
Detector. hydrogen flame ionization detector (FID), 300 ℃; combustion gas. hydrogen (4.9), flow rate 40 ml/min;
Combustion gas. air, flow rate 350 ml/min; makeup gas. high-purity nitrogen (4.8), flow rate 25 ml/min.
7.2 Establishment of standard curve
Pipette the standard use solution (4.6) of chlorobenzene compounds, and prepare the mass concentration with carbon disulfide (4.1) as
Standard series solutions of 1.00 μg/ml, 2.00 μg/ml, 5.00 μg/ml, 10.0 μg/ml, 20.0 μg/ml (this is the reference concentration
degree). According to the gas chromatography reference analysis conditions (7.1), the standard series of solutions were sampled in order from low concentration to high concentration,
Taking the mass concentration of the target compound as the abscissa and the corresponding peak area (or peak height) as the ordinate, establish the chlorobenzene type
Standard curve of the compound.
Under the reference analysis conditions (7.1) recommended by this standard for gas chromatography, the gas chromatograms of 10 chlorobenzene compounds are shown in the figure
3 shown.
min5 7.5 10 12.5 15 17.5 20 22.5
pA
FID2 B, rear signal (2019E3 \\ E20190718000024.D)
1-chlorobenzene; 2-2-chlorotoluene; 3-3-chlorotoluene; 4-4-chlorotoluene; 5-1,3-dichlorobenzene;
6-1,4-dichlorobenzene; 7-1,2-dichlorobenzene; 8-1,3,5-trichlorobenzene; 9-1,2,4-trichlorobenzene; 10-1,2, 3-Trichlorobenzene.
Figure 3 Standard chromatogram of chlorobenzene compounds (ρ = 10.0 μg/ml)
7.3 Determination of samples
According to the same conditions as the standard curve establishment (7.2), the waste gas samples from fixed pollution sources (6.3.1) and unorganized emissions
6 Monitor the air sample (6.3.2) and the whole program blank sample (6.3.3) for measurement. When the concentration of chlorobenzene compounds in the sample
When the degree exceeds the upper limit of the standard curve, the sample should be diluted before measurement.
7.4 Blank test
Carry out the measurement of the blank sample (6.4) according to the same analysis conditions as the measurement of the sample (7.3).
8 Calculation and presentation of results
8.1 Qualitative analysis
Qualitative based on the retention time of the target compound. If necessary, another capillary of different polarity can be used in Appendix C
The chromatographic column is qualitatively assisted or confirmed using gas chromatography/mass spectrometry.
8.2 Calculation of results
8.2.1 Exhaust gas from stationary sources
The mass concentration (ρi) of the target chlorobenzene compounds in the waste gas sample from the stationary pollution source is calculated according to formula (1).
nd
BA
V ) ( (1)
In the formula. ρi--the mass concentration of the target compound in the exhaust gas sample of the fixed pollution source, mg/m3;
ρA, ρB—the mass concentration of the target compound in the sample A and B of the sampling tube obtained from the standard curve, μg/ml
V--volume of desorption solvent, ml;
Vnd-the volume of dry gas sampling in the standard state (273.15 K, 1013.25 hPa) of the fixed source exhaust gas, L.
8.2.2 Air at unorganized emission monitoring points
The mass concentration (ρj) of chlorobenzene target compounds in the air samples of the fugitive emission monitoring point is calculated according to formula (2).
BA
V ) ( (2)
In the formula. ρj--mass concentration of the target compound in the air sample of the fugitive emission monitoring point, mg/m3;
ρA, ρB—the mass concentration of the target compound in the sample A and B of the sampling tube obtained from the standard curve, μg/ml
V--volume of desorption solvent, ml;
Vr--Unorganized emission monitoring point sampling volume in air standard (273.15 K, 1013.25 hPa), L.
8.3 Results
The number of digits after the decimal point of the measurement result is consistent with the detection limit of the method, and at most three significant digits are retained. To calculate chlorobenzene
The total amount of compounds should be added according to the components specified in the relevant environmental quality standards and pollutant discharge (control) standards.
The detected components are not counted in the total amount.
79 Precision and accuracy
9.1 Precision
Six laboratories respectively spiked 6 groups of GDX-103 with chlorobenzene compounds spiked at 0.100 mg/m3 and 2.50 mg/m3
Adsorption sampling tube, simulated after sampling the air at the fugitive emission monitoring point, the relative standard deviation in the laboratory is 0.5% ~
7.4%, 1.3% ～ 5.9%, relative standard deviations between laboratories are 2.0% ～ 12%, 2.5% ～ 4.8%, repeatability limit points
It is 0.01 mg/m3, 0.26 mg/m3 ～ 0.31 mg/m3, and the reproducibility limits are 0.01 mg/m3 ～ 0.04 mg/m3,
0.31 mg/m3 ～ 0.41 mg/m3. See attached table B.1 for details.
Six laboratories respectively spiked 6 groups of activated carbon with chlorobenzene compounds with spiked concentrations of 0.100 mg/m3 and 5.00 mg/m3.
A sampling tube is attached to simulate the air sampling at the fugitive emission monitoring point. The relative standard deviation in the laboratory is 2.0% ~
8.7%, 0.42% ～ 4.7%, relative standard deviations between laboratories are 4.9% ～ 10%, 1.6% ～ 9.7%, repeatability limit points
They are 0.01 mg/m3 ～ 0.02 mg/m3, 0.21 mg/m3 ～ 0.31 mg/m3, and the reproducibility limits are 0.02 mg/m3 ～ 0.03 respectively.
mg/m3, 0.35 mg/m3 ～ 1.3 mg/m3. See attached table B.2.
9.2 Accuracy
Six laboratories respectively spiked 6 groups of GDX-103 with chlorobenzene compounds spiked at 0.100 mg/m3 and 2.50 mg/m3
Adsorption sampling tube, simulated after sampling air at the fugitive emission monitoring point, the average recovery rate of each component is respectively
97.8% ～ 107%, 95.3% ～ 98.3%, see attached table B.1 for details.
Six laboratories respectively spiked 6 groups of activated carbon with chlorobenzene compounds with spiked concentrations of 0.100 mg/m3 and 5.00 mg/m3.
With a sampling tube, it is measured after simulating the air sampling at the fugitive emission monitoring point, and the average recovery rate of each component is respectively
89.0% ～ 106%, 82.0% ～ 99.4%, see attached table B.2.
10 Quality assurance and quality control
10.1 Calibration of sampling instruments
Atmospheric samplers and other instruments should be calibrated for flow in accordance with GB/T 16157, and HJ/T 375 and HJ/T 47 before sampling.
Requirements to check the air tightness of the sampling system.
10.2 Blank
Every 20 samples or each batch (less than 20 samples/batch) should be measured with a full program blank and a laboratory
For blank samples, the target compound concentration in the blank samples should be below the detection limit of the method.
10.3 Calibration
A standard curve should be established for each batch of samples, and the linear correlation coefficient of the standard curve should be ≥0.995.
Every 20 samples or each batch (less than 20 samples/batch) should be analyzed once the intermediate concentration point of the standard curve
For the quasi solution, the relative error between the measurement result and the standard value should be within ± 10%, otherwise, the standard curve should be re-established.
810.4 Blank spike test
Each batch of samples shall be subjected to at least one blank spike recovery test, and the spike recovery rate of each component shall be between 70% and 120%.
10.5 Penetration test
If the GDX-103 adsorption sampling tube or activated carbon adsorption sampling tube has a B-stage analyte greater than or equal to the A-stage analyte
The amount of 25% indicates that the adsorbent penetrates, and the sampling volume should be appropriately reduced to resample.
11 Waste disposal
The waste liquid generated during the experiment and the samples after analysis should be collected separately, and they should be safely disposed of as required or commissioned by a qualified company.
Bit disposal.
9 Appendix A
...
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