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HJ 1153-2020: (Stationary pollution source waste gas Determination of aldehydes and ketones solution absorption-high performance liquid chromatography)
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(Stationary pollution source waste gas Determination of aldehydes and ketones solution absorption-high performance liquid chromatography)
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HJ 1153-2020
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Basic data | Standard ID | HJ 1153-2020 (HJ1153-2020) | | Description (Translated English) | (Stationary pollution source waste gas Determination of aldehydes and ketones solution absorption-high performance liquid chromatography) | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z25 | | Word Count Estimation | 16,161 | | Date of Issue | 2020-12-14 | | Date of Implementation | 2021-03-15 | | Regulation (derived from) | Ministry of Ecology and Environment Announcement No. 63 (2020) | | Issuing agency(ies) | Ministry of Ecology and Environment | HJ 1153-2020: (Stationary pollution source waste gas Determination of aldehydes and ketones solution absorption-high performance liquid chromatography)
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(Stationary pollution source waste gas Determination of aldehydes and ketones solution absorption-high performance liquid chromatography)
National Environmental Protection Standards of the People's Republic of China
Fixed pollution source waste gas aldehyde and ketone compounds
Determination of Solution Absorption-High Performance Liquid Chromatography
Stationary source emission-Determination of aldehyde and ketone
compounds -Solution absorption- High performance liquid
chromatography
2020-12-14 release
2021-03-15 implementation
Issued by the Ministry of Ecology and Environment
Table of contents
Foreword...ii
1 Scope of application...1
2 Normative references...1
3 Principles of the method...1
4 Interference and cancellation...1
5 Reagents and materials...1
6 Instruments and equipment...3
7 Sample...3
8 Analysis steps...5
9 Calculation and presentation of results...6
10 Precision and accuracy...7
11 Quality Assurance and Quality Control...7
12 Waste disposal...8
Appendix A (Normative Appendix) Method detection limit and lower limit of determination...9
Appendix B (informative appendix) Method precision and accuracy...10
Appendix C (informative appendix) Reference chromatogram of acetonitrile-water system separation of aldehydes and ketones-DNPH derivatives...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 China", and protect the ecology
The environment, to protect human health, to standardize the determination methods of aldehydes and ketones in waste gas from stationary sources, and to formulate this standard.
This standard specifies the high performance liquid chromatography method for the determination of aldehydes and ketones in waste gas from stationary sources.
Appendix A of this standard is a normative appendix, and Appendix B and Appendix C 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. Shenyang Ecological Environment Monitoring Center of Liaoning Province.
Verification units of this standard. Liaoning Province Ecological Environment Monitoring Center, Tianjin Ecological Environment Monitoring Center, Dalian Health
Environmental Monitoring Center, Anshan Ecological Environmental Monitoring Center of Liaoning Province, Fushun Ecological Environmental Monitoring Center of Liaoning Province, Shenyang City Health
Environmental Affairs Service and Administrative Law Enforcement Center.
This standard was approved by the Ministry of Ecology and Environment on December 14, 2020.
This standard will come into effect on March 15, 2021.
This standard is interpreted by the Ministry of Ecology and Environment.
Determination of aldehydes and ketones in waste gas from stationary sources
Solution absorption-high performance liquid chromatography
Warning. The acid and organic reagents used in the experiment are strongly corrosive, irritating and toxic. The reagent preparation process
The pre-treatment process of samples and samples should be carried out in a fume hood; protective equipment should be worn as required during operation to avoid breathing in the respiratory tract and
Touch skin and clothing.
1 Scope of application
This standard specifies the high performance liquid chromatography method for the determination of aldehydes and ketones in waste gas from stationary sources.
This standard applies to the organized emission of formaldehyde, acetaldehyde, acrolein, acetone, propionaldehyde, crotonaldehyde,
Determination of 12 aldehydes and ketones including 2-butanone, n-butyraldehyde, benzaldehyde, isovaleraldehyde, n-valeraldehyde and n-hexanal.
When the sample volume is 10.0 ml and the injection volume is 10 μl, the minimum detectable amount of aldehyde and ketone compounds is 0.13 μg～0.29 μg,
When collecting 20 L of organized exhaust gas (dry flue gas under standard conditions), the detection limit of the method is 0.01 mg/m3～
0.02 mg/m3, the lower limit of determination is 0.04 mg/m3～0.08 mg/m3.See Appendix A for details.
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/T 373 Fixed pollution source monitoring quality assurance and quality control technical specifications (trial implementation)
HJ/T 397 Fixed source exhaust gas monitoring technical specification
3 Principles of the method
Organized emission of fixed pollution sources of aldehydes and ketones in exhaust gas in acidic medium and 2,4-dinitro in the absorption liquid
Phenylhydrazine (DNPH) undergoes a derivatization reaction to generate 2,4-dinitrophenylhydrazone compounds, which are dissolved in a mixture of dichloromethane and n-hexane
After extraction and concentration of liquid or dichloromethane, change the solvent to acetonitrile, separate by high performance liquid chromatography, UV or diode array detection
Detector detection. Qualitatively based on retention time and quantified by external standard method.
4 Interference and elimination
Other organic compounds with the same retention time and absorption at 360 nm can interfere with the determination. You can change
The mobile phase composition and other methods improve the separation conditions and avoid interference.
5 Reagents and materials
Unless otherwise specified, analytical reagents conforming to national standards are used for analysis, and the experimental water is newly prepared ultrapure water.
5.1 Acetonitrile (CH3CN). pure by high performance liquid chromatography.
5.2 Dichloromethane (CH2Cl2). pure by high performance liquid chromatography.
5.3 n-hexane (C6H14). pure by high performance liquid chromatography.
5.4 Hydrochloric acid (HCl). ρ=1.19 g/ml, excellent grade pure.
5.5 2,4-Dinitrophenylhydrazine (DNPH). w ≥98.0%.
5.6 Acrolein (C3H4O). w ≥98.0%.
5.7 Ccrotonaldehyde (C4H6O). w ≥98.0%.
5.8 Dichloromethane-n-hexane mixed solution. 37, ready for use.
5.9 Anhydrous sodium sulfate (Na2SO4). Burn at 450°C for 4 h, cool, and store in a ground glass bottle sealed.
5.10 Standard stock solutions of 12 aldehydes and ketones-DNPH derivatives. ρ=100 µg/ml (calculated as aldehydes and ketones).
Directly purchase commercially available certified standard solutions of aldehydes and ketones-DNPH derivatives, the solvent is acetonitrile, and the mass concentration is based on aldehydes and ketones.
Class compound meter. Refer to the certificate of the standard solution for storage. After opening the package, keep it airtight below 4°C and keep it away from light. 2 can be stored
month.
5.11 Aldehydes and ketones-DNPH derivatives standard liquid. ρ=10.0 μg/ml (calculated as aldehydes and ketones).
Pipette 1.00 ml aldehyde and ketone-DNPH derivative standard stock solution (5.10) into a 10 ml volumetric flask, use acetonitrile (5.1)
Dilute and dilute to the mark and mix well. It can be stored for 2 months in airtight, dark and cold storage below 4℃.
5.12 Standard stock solution of aldehydes and ketones. ρ=1000 μg/ml.
Directly purchase commercially available standard solutions of aldehydes and ketones with acetonitrile as the solvent. Refer to the standard solution certificate for guarantee
Store, after opening, airtight and refrigerate below 4℃, avoid light, and can be stored for two weeks.
5.13 Standard liquid for aldehydes and ketones. ρ=100 μg/ml.
Pipette 1.00 ml aldehyde and ketone standard stock solution (5.12) into a 10 ml volumetric flask and dilute with acetonitrile (5.1)
And dilute to the marking line and mix well. Store in airtight, dark and cold storage below 4°C for two weeks.
5.14 Acrolein standard stock solution. ρ≈1000 μg/ml.
Weigh 0.100 g of acrolein (5.6), dissolve it with acetonitrile (5.1) in a 100 ml volumetric flask, and dilute to the mark.
uniform. It can be stored for 1 month in airtight, dark and cold storage below 4℃.
5.15 Standard stock solution of crotonaldehyde. ρ≈1000 μg/ml.
Weigh 0.100 g of crotonaldehyde (5.7), dissolve it with acetonitrile (5.1) in a 100 ml volumetric flask, and dilute to the mark.
uniform. It can be stored for 1 month in airtight, dark and cold storage below 4℃.
5.16 Standard liquid for acrolein and crotonaldehyde. ρ≈100 μg/ml.
Pipette 1.00 ml acrolein standard stock solution (5.14) and crotonaldehyde standard stock solution (5.15) into a 10 ml volumetric flask,
Dilute with acetonitrile (5.1) and make up to the mark, and mix well. It can be stored for 1 month in airtight, dark and cold storage below 4℃.
5.17 DNPH saturated absorbent
Weigh 4.0 g of DNPH (5.5) into a brown reagent bottle, add 180 ml of hydrochloric acid (5.4), and then add 820 ml
Water, ultrasound for 30 min. A saturated solution is formed and filtered.
Transfer the filtered saturated DNPH solution to a 2 L separatory funnel, add 60 ml of dichloromethane (5.2), and extract
Take 3 minutes (pay attention to venting), let it stand, after stratification, discard the lower organic phase, repeat the above operation, and extract once. most
Then extract with 60 ml n-hexane (5.3). When the organic phase is separated from the DNPH solution, transfer the lower DNPH solution
Into a brown reagent bottle rinsed and dried with acetonitrile, sealed, and stored in a desiccator filled with activated carbon.
Note. Each batch of DNPH saturated solution should be prepared and purified within 48 hours before sampling. The blank after purification should meet the requirements of 11.1.
5.18 High purity nitrogen. purity ≥99.999%.
5.19 Filter membrane. 0.45 μm polytetrafluoroethylene membrane.
6 Apparatus and equipment
6.1 High performance liquid chromatograph. with ultraviolet or diode array detector and gradient elution function.
6.2 Chromatographic column. C18 column, 4.60 mm×250 mm×5.0 μm, pH range. 2～11, packing is octadecylsilane bond
Double-end-capped reversed-phase column with silica gel (ODS) or other columns with similar performance.
6.3 Flue gas sampler. with anti-negative pressure function. The sampling flow rate is 0.2 L/min～1.5 L/min, and the sampling tube is made of hard glass or
Fluorine resin material should have heating and heat preservation function, heating temperature ≥120℃.
6.4 Connecting pipe. PTFE hose or silicone rubber pipe lined with PTFE film.
6.5 Brown bubble absorption bottle. 75 ml.
6.6 Concentration device. equipment with equivalent performance such as rotary evaporation device or nitrogen blowing concentrator.
6.7 Separation funnel. 2 L and 250 ml, PTFE piston.
6.8 Brown reagent bottle. 1 L and 4 L.
6.9 Ultrasonic cleaner.
6.10 Instruments and equipment commonly used in general laboratories.
7 samples
7.1 Sample collection
7.1.1 Fixed pollution source waste gas samples
The location, sampling and parameter determination of waste gas from stationary sources shall comply with relevant regulations in GB/T 16157 and HJ/T 397.
The sampling device is shown in Figure 1.
Connect three brown bubble absorption bottles (6.5) each containing 50 ml DNPH saturated absorption liquid (5.17) in series, and
The sampler (6.3) is connected, according to the gaseous pollutant collection method, with a flow rate of 0.2 L/min～0.5 L/min, continuous sampling 1
h, or collect 3 to 4 samples at equal time intervals within 1 h, and the flow fluctuation during sampling should be ≤±10%. According to the sample
Prolong or shorten the sampling time appropriately. During the sampling process, the temperature of the insulation jacket of the sampling pipe should be kept not lower than 120℃.
To avoid condensation of water vapor in the collected gas before the absorption bottle.
After sampling, cut off the gas path between the sampling pump and the absorption bottle, take out the sampling tube, remove the absorption bottle, and seal it with a sealing cap.
Seal and store away from light.
7.1.2 Transporting blank samples
Bring three brown bubble absorption bottles (6.5) with 50 ml DNPH saturated absorption solution (5.17) from the same batch
Go to the sampling site but do not collect samples, and transport them back to the laboratory together with the samples as blank samples for transportation.
Figure 1 Schematic diagram of the composition of a stationary source waste gas sampling system
7.2 Sample storage
The samples should be sealed and stored in cold storage at a temperature below 4℃, and the sample preparation should be completed within 3 days after the sample is collected.
The analysis will be completed within 3 days.
7.3 Preparation of samples
Transfer the sample in the absorption bottle to a 250 ml separatory funnel (6.7), wash the absorption with a small amount of dichloromethane (5.2)
The bottle was washed twice, and then washed with water and dichloromethane. The washing liquid was transferred to the separatory funnel, and 10 ml dichloromethane or
Dichloromethane-n-hexane mixed solution (5.8), shake for 3 min, stand still for layering, collect the organic phase in a 150 ml Erlenmeyer flask
in. Use 10 ml dichloromethane (5.2) or dichloromethane-n-hexane mixed solution (5.8) to extract the water phase twice, and
And organic phase, add anhydrous sodium sulfate (5.9) until the sodium sulfate particles can flow freely. Let it stand for 30 min, dehydrated and dried.
Transfer the sample extract to the concentrating device (6.6), and concentrate to near dryness below 45°C, and change the solvent to acetonitrile
(5.1), and dilute to 10.0 ml with acetonitrile. After mixing thoroughly, filter through membrane (5.19) into a sample bottle for testing. in case
The measured concentration is too high and can be diluted appropriately.
Note. When the sample is placed for a long time after collection or the DNPH has a greater influence on the measurement, the sample is extracted with a dichloromethane-n-hexane mixed solution.
7.4 Preparation of blank samples
7.4.1 Transport blank sample
Transport blank (7.1.2) Prepare a transport blank sample in accordance with sample preparation (7.3).
7.4.2 Laboratory blank sample
Prepare a laboratory blank sample for the absorption solution sampled in the same batch according to the sample preparation (7.3).
8 Analysis steps
8.1 Instrument reference conditions
Column oven temperature. 35°C; injection volume. 10 μl; UV detector wavelength. 360 nm.
The gradient elution program is shown in Table 1, mobile phase A. acetonitrile, mobile phase B. water, and mobile phase C. methanol.
Note. Refer to Appendix C for reference chromatographic conditions and chromatograms of the acetonitrile-water binary system. When using different mobile phase systems, the compound peaks
The order is different. See Figure 2 and Figure C.1 for details.
8.2 Calibration
Take a certain amount of aldehyde and ketone-DNPH derivative standard use solution (5.11) in acetonitrile, dilute with acetonitrile (5.1), and prepare
The system concentrations (calculated as aldehydes and ketones) are 0.10 µg/ml, 0.20 µg/ml, 0.50 µg/ml, 1.00 µg/ml,
Standard series solutions of 2.00 µg/ml and 4.00 µg/ml. Inject into the high performance liquid chromatograph from low concentration to high concentration, press the instrument
Measure with reference condition (8.1) to obtain chromatograms of target compounds at different concentrations, and record retention time and peak area. To
The concentration of aldehydes and ketones is the abscissa, and the peak area of the corresponding compound is the ordinate to establish a standard curve. 12 aldehydes and ketones
The standard chromatogram of -DNPH derivative is shown in Figure 2.
Figure 2 Standard chromatograms of 12 aldehydes and ketones-DNPH derivatives
8.3 Sample measurement
Measure the sample according to the same instrument reference conditions (8.1) as the standard curve establishment, and record the peak of the target compound
Area and retention time.
8.4 Blank test
Transport the blank sample (7.4.1) and laboratory blank sample according to the same instrument conditions as the sample measurement (8.3)
(7.4.2) determination.
9 Calculation and presentation of results
9.1 Qualitative analysis
9.1.1 According to the retention time, sample UV spectrum and standard solution UV spectrum comparison for qualitative.
Note. Acrolein is derivatized in DNPH saturated absorption solution (5.17) to produce acrolein hydrazone and its polymers, and double peaks appear in the chromatogram.
Need to use acrolein standard liquid to prepare acrolein hydrazone and its polymer for qualitative determination. Ccrotonaldehyde saturated absorption liquid in DNPH (5.17)
The derivatization in medium will also generate crotonaldehyde hydrazone and its polymers. Double peaks appear in the chromatogram under the conditions of the acetonitrile-water binary system.
The crotonaldehyde standard solution is used to prepare crotonaldehyde hydrazone and its polymers for qualitative determination.
9.1.2 Qualitative of acrolein and crotonaldehyde
In a 250 ml separatory funnel, add 150 ml DNPH saturated absorption solution (5.17), then add 100 μl acrolein and
For the crotonaldehyde standard use solution (5.16), follow the same steps as the sample preparation (7.3) for sample preparation. By instrument
Analyze with reference condition (8.1), record the retention time of acrolein hydrazone polymer and crotonaldehyde hydrazone polymer for qualitative purposes.
The chromatogram of acrolein hydrazone and its polymer is shown in Figure 3.The chromatogram of crotonaldehyde hydrazone and its polymers is shown in Figure C.2.
9.2 Quantitative analysis
According to the peak area of the compound, the external standard method was used for quantification. In the sample, acrolein and crotonaldehyde are based on their hydrazone and hydrazone polymers.
The sum of peak areas is substituted into the standard curve for quantification.
9.3 Calculation of results
In the formula. --the mass concentration of the target compound in the sample, mg/m3;
i --Get the mass concentration of the target compound in the sample from the standard curve, µg/ml;
0 - Obtain the average mass concentration of the target compound in two laboratory blanks from the standard curve, µg/ml;
V-the concentrated volume of the sample, ml;
D-the dilution factor of the sample;
V1--Sampling volume, L. Sampling in specified conditions shall be adopted in accordance with the requirements of corresponding quality standards or emission standards
volume.
9.4 Presentation of results
The number of digits retained after the decimal point of the determination result is consistent with the detection limit, and up to three significant digits are retained.
10 Precision and accuracy
10.1 Precision
The 6 laboratories added the blank spiked amounts of 2.0 μg, 5.0 μg and 20.0 μg for aldehydes and ketones respectively (equivalent to
The concentration of 0.10 mg/m3, 0.25 mg/m3 and 1.00 mg/m3) of the absorption solution was repeated 6 times.
The relative standard deviations in the laboratory were 3.4%～9.8%, 2.6%～6.7% and 0.8%～3.8%;
The relative standard deviations between laboratories are. 3.4%～9.7%, 2.2%～8.1% and 1.3%～7.7%;
Repeatability limits are. 0.01 mg/m3～0.02 mg/m3, 0.02 mg/m3～0.03 mg/m3 and 0.04 mg/m3～
0.07 mg/m3;
The reproducibility limits are. 0.02 mg/m3～0.03 mg/m3, 0.03 mg/m3～0.05 mg/m3 and 0.06 mg/m3～
0.20 mg/m3.
10.2 Accuracy
Six laboratories have carried out spiked determinations on organized exhaust gas samples. The spiked amount of aldehydes and ketones is
5.0 µg (equivalent to exhaust gas concentration 0.25 mg/m3), the recovery rate of standard addition is between 61.7% and 102%, and the recovery rate of standard addition is final
The value is 70.9%±10.8%～96.8%±9.2%.
See Appendix B for details of precision and accuracy.
11 Quality Assurance and Quality Control
11.1 Blank
Limits for the content of aldehydes and ketones in 150 ml absorption liquid. 0.50 μg for formaldehyde; 0.30 μg for acetaldehyde;
0.90 μg; other substances are 0.30 μg.
At least 2 laboratory blanks and 1 shipping blank are analyzed for each batch of samples. Limits of content of aldehydes and ketones in the blank.
Formaldehyde is 0.50 μg; acetaldehyde is 0.30 μg; acetone is 0.90 μg; other substances are 0.30 μg.
11.2 Calibration
11.2.1 Initial calibration
The correlation coefficient of the standard curve is ≥0.995, otherwise, the standard curve is re-established.
11.2.2 Continuous calibration
During the sample measurement period, measure the standard solution at the midpoint of the curve at least once a day, the measured value of the target compound and the standard
The relative error of the standard value should be within ±20%.
12 Waste treatment
The waste liquid generated in the experiment should be collected in a centralized manner, and the corresponding identification should be made, and a qualified unit should be entrusted for processing according to law.
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