HJ 1154-2020 English PDF

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HJ 1154-2020: (Ambient air Determination of aldehydes and ketones solution absorption-high performance liquid chromatography)
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HJ 1154-2020	369	Add to Cart	4 days	(Ambient air Determination of aldehydes and ketones solution absorption-high performance liquid chromatography)	Valid

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HJ 870   GB/T 15516   GB/T 14675   HJ 1271   HJ 1270   HJ 1155   

Basic data

Standard ID: HJ 1154-2020 (HJ1154-2020)
Description (Translated English): (Ambient air Determination of aldehydes and ketones solution absorption-high performance liquid chromatography)
Sector / Industry: Environmental Protection Industry Standard
Classification of Chinese Standard: Z15
Word Count Estimation: 16,153
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 1154-2020: (Ambient air Determination of aldehydes and ketones solution absorption-high performance liquid chromatography)

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(Ambient air Determination of aldehydes and ketones solution absorption-high performance liquid chromatography) National Environmental Protection Standards of the People's Republic of China Determination of aldehydes and ketones in ambient air Solution absorption-high performance liquid chromatography Ambient air-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...2 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...13

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 To protect human health, regulate the determination method of aldehydes and ketones in ambient air, and formulate this standard. This standard specifies high performance liquid chromatography for the determination of aldehydes and ketones in ambient air and unorganized emission monitoring points. law. 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 ambient air 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 high performance liquid chromatography for the determination of aldehydes and ketones in ambient air and unorganized emission monitoring points. law. This standard is applicable to formaldehyde, acetaldehyde, acrolein, acetone, propionaldehyde, Ccrotonaldehyde, 2-butanone, n-butyraldehyde, benzaldehyde, isovaleraldehyde, n-valeraldehyde, n-hexanal, o-methylbenzaldehyde, m-tolualdehyde Determination of 16 aldehydes and ketones including aldehyde, p-methylbenzaldehyde and 2,5-dimethylbenzaldehyde. When the sample volume is 2.0 ml and the injection volume is 10 μl, the minimum detectable amount of aldehydes and ketones is 0.024 μg～0.060 μg, When the sampling volume is 20 L (under standard conditions), the detection limit of the method is 0.002 mg/m3～0.003 mg/m3, the lower limit of determination It is 0.008 mg/m3～0.012 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. HJ/T 55 Technical Guidelines for Monitoring Unorganized Emissions of Air Pollutants HJ 194 Technical specification for manual monitoring of ambient air quality

3 Principles of the method

Ambient air and fugitive emission monitoring points The aldehydes and ketones in the air in the acid medium and the 2,4-in the absorption liquid Dinitrophenylhydrazine (DNPH) undergoes a derivatization reaction to generate 2,4-dinitrophenylhydrazone compounds, using dichloromethane-n-hexane After the mixed solution or dichloromethane is extracted and concentrated, the solvent is changed to acetonitrile, separated by high performance liquid chromatography, ultraviolet or diode Array 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). Bake at 450°C for 4 h, cool, and store in a ground glass bottle sealed. 5.10 Standard stock solution of 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 aldehyde, Based on ketone compounds. Refer to the certificate of the standard solution for storage. After opening, it should be airtight and refrigerated below 4°C and protected from light. It can be stored 2 Months. 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, dilute with acetonitrile (5.1) Relieve 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 of water. Ultrasound for 30 min. A saturated solution is formed and filtered. Transfer the filtered saturated solution of DNPH to a 2 L separatory funnel, add 60 ml of dichloromethane (5.2), Extract for 3 min (pay attention to gassing), let it stand, after stratification, discard the lower organic phase, repeat the above operation, and extract once. Finally, it was extracted with 60 ml n-hexane (5.3). After the organic phase was separated from the DNPH solution, the DNPH solution in the lower layer was transferred to Transfer to a brown reagent bottle rinsed with acetonitrile and dried, sealed, and stored in a desiccator 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 Double-end-capped reversed-phase chromatography column with bonded silica gel (ODS) or other columns with similar performance. 6.3 Air sampler. sampling flow rate 0.1 L/min～1.0 L/min. 6.4 Brown porous glass plate absorption bottle. 25 ml. 6.5 Brown bubble absorption bottle. 25 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 125 ml, PTFE piston. 6.8 Brown reagent bottle. 1 L. 6.9 Ultrasonic cleaner. 6.10 Instruments and equipment commonly used in general laboratories.

7 samples

7.1 Sample collection 7.1.1 Ambient air and unorganized emission monitoring point air samples The layout and sampling of ambient air sampling points meet the requirements of HJ 194, and the layout and sampling of unorganized emission monitoring points Comply with relevant regulations in HJ/T 55. According to Figure 1, put the brown porous glass plate absorption bottle (6.4) containing 20 ml DNPH saturated absorption solution (5.17) and separate The brown bubble absorption bottle (6.5) containing 20 ml and 10 ml absorption solution (5.17) is connected in series to the air sampler (6.3). To Flow rate of 0.3 L/min～0.5 L/min, continuous sampling for 1 hour, if the concentration is low, the sampling time can be extended appropriately, but the total sampling The volume does not exceed 80 L. If the temperature is lower than 4℃ during sampling, the absorption bottle should be placed in a thermostat. After sampling, immediately remove the absorption bottle, seal it with a sealing cap, and store it in the dark. 7.1.2 Transporting blank samples Take the three brown multi-well glass plate absorption bottles each containing 20 ml DNPH saturated absorption solution (5.17) from the same batch (6.4) The brown bubble absorption bottle (6.5) of 20 ml and 10 ml absorption solution (5.17) is brought to the sampling site but not sampled The product is collected and shipped back to the laboratory together with the sample as a blank sample for transportation. 7.2 Sample storage The samples should be sealed and kept in cold storage below 4℃ and protected from light. The preparation of the samples should be completed within 3 days after the samples are collected. The sample was analyzed within 3 days. 7.3 Preparation of samples Transfer the sample in the absorption bottle to a 125 ml separatory funnel (6.7), wash the absorption with a small amount of dichloromethane (5.2) Bottle twice, transfer the cleaning solution to the separatory funnel, add 10 ml dichloromethane (5.2) or dichloromethane-n-hexane and mix Solution (5.8), shake for 3 min, stand for layering, collect the organic phase in a 150 ml Erlenmeyer flask. Use 10 ml dichloromethane again (5.2) or dichloromethane-n-hexane mixed solution (5.8), repeat the extraction of the water phase twice, combine the organic phases, and add anhydrous sulfur Sodium (5.9) to 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 2.0 ml with acetonitrile. After mixing thoroughly, filter it through the filter 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). 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. Note. m-methylbenzaldehyde-DNPH and p-methylbenzaldehyde-DNPH are difficult to separate substances. When the chromatographic column cannot separate the two, test The result is the sum of the pairs of difficult-to-separate substances. 10 Precision and accuracy 10.1 Precision The six laboratories added 0.2 μg, 1.0 μg and 4.0 μg (equivalent to blank spikes) for aldehydes and ketones. Gas samples (0.010 mg/m3, 0.050 mg/m3, and 0.200 mg/m3) of the absorption solution were tested for 6 repetitions. The relative standard deviations in the laboratory are. 4.3%～11%, 2.1%～7.9% and 0.9%～4.9%; The relative standard deviations between laboratories are. 2.7%-12%, 3.3%-9.3% and 1.3%-6.6%; Repeatability limits are. 0.001 mg/m3～0.003 mg/m3, 0.005 mg/m3～0.007 mg/m3 and 0.010 mg/m3～ 0.017 mg/m3; The reproducibility limits are. 0.002 mg/m3～0.004 mg/m3, 0.006 mg/m3～0.012 mg/m3 and 0.016 mg/m3～ 0.036 mg/m3. 10.2 Accuracy Six laboratories have performed spiked analysis and determination on ambient air samples, and the spiked amount of aldehydes and ketones is 1.0 µg (Equivalent to 0.050 mg/m3 of air sample), the recovery rate of standard addition is between 62.8% and 110%, and the final recovery rate of standard addition is 65.5%±6.8%～105%±9.4%. 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 50 ml absorption solution. formaldehyde is 0.15 μg; acetaldehyde is 0.10 μg; acetone is 0.30 μg; other substances are 0.10 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 0.15 μg; acetaldehyde is 0.10 μg; acetone is 0.30 μg; all other substances are 0.10 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%. 11.3 Parallel samples Use two instruments to collect the same gas at the same time to obtain parallel samples. Collect at least one parallel sample for each batch of samples. When the result is greater than the lower limit of determination, the relative deviation shall not exceed 30%. 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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