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HJ 1224-2021 English PDF

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HJ 1224-2021: Ambient air-Determination of organochlorine pesticides-High resolution gas chromatography/high resolution mass spectrometry
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HJ 1224-2021English739 Add to Cart 6 days [Need to translate] Ambient air-Determination of organochlorine pesticides-High resolution gas chromatography/high resolution mass spectrometry Valid HJ 1224-2021

Standard similar to HJ 1224-2021

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Basic data

Standard ID HJ 1224-2021 (HJ1224-2021)
Description (Translated English) Ambient air-Determination of organochlorine pesticides-High resolution gas chromatography/high resolution mass spectrometry
Sector / Industry Environmental Protection Industry Standard
Word Count Estimation 32,369
Issuing agency(ies) Ministry of Ecology and Environment

HJ 1224-2021: Ambient air-Determination of organochlorine pesticides-High resolution gas chromatography/high resolution mass spectrometry


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(Ambient air - Determination of organochlorine pesticides - High resolution gas chromatography-high resolution mass spectrometry) National Ecological Environment Standard of the People's Republic of China Determination of Organochlorine Pesticides in Ambient Air High Resolution Gas Chromatography-High Resolution Mass Spectrometry Ambient air—Determination of organochlorine pesticides—High resolution gas chromatography/high resolution mass spectrometry This electronic version is the official standard text, which is reviewed and typeset by the Environmental Standards Institute of the Ministry of Ecology and Environment. Published on 2021-12-16 2022-03-01 Implementation Released by the Ministry of Ecology and Environment directory Foreword...ii 1 Scope...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...2 7 Samples...4 8 Analysis steps...6 9 Result calculation and representation...9 10 Accuracy...10 11 Quality Assurance and Quality Control...10 12 Waste Disposal...11 Appendix A (Informative Appendix) List of Organochlorine Pesticides...12 Appendix B (normative appendix) Method detection limit and lower limit of determination...13 Appendix C (Informative Appendix) Examples of Organochlorine Pesticide Standard Substance Use...14 Appendix D (informative appendix) Examples of high-resolution gas chromatography-high-resolution mass spectrometry parameters...17 Appendix E (informative) Accuracy of the method...20 Determination of Organochlorine Pesticides in Ambient Air by High Resolution Gas Chromatography-High Resolution Mass Spectrometry Warning. The solvents and standard samples used in the experiment are toxic, and the preparation of reagents and sample pretreatment should be carried out in a fume hood; When operating, wear protective equipment as required to avoid inhalation into the respiratory tract or contact with skin and clothing.

1 Scope of application

This standard specifies the high-resolution gas chromatography-high-resolution mass spectrometry method for the determination of organochlorine pesticides in ambient air. This standard is applicable to hexachlorobenzene, α-hexahexahexanone, γ-hexahexahexanone, β-hexahexahexanol, δ-hexachlorobenzene, heptachlor, Aldrin, chlordane oxide, cis-epoxyheptachlor, trans-epoxyheptachlor, trans-chlordane, 2,4'-DDE, trans-nonachlor, cis-chlordane, Endosulfan-Ⅰ, 4,4'-DDE, dieldrin, 2,4'-DDD, endrin, 2,4'-DDT, cis-nonachloro, 4,4'-DDD, endosulfan -Ⅱ, 4,4'-DDT Determination of 25 organochlorine pesticides, including mirex. See Appendix A. When the sampling volume is 30 m3 (standard state) and the concentration volume is 20 μl, the detection limit of HCB is 0.9 pg/m3. The limit is 3.6 pg/m3; when the sampling volume is 1200 m3 (standard state) and the concentration volume is 20 μl, other organochlorines except hexachlorobenzene The detection limit of pesticides is 0.006 pg/m3～0.03 pg/m3, and the lower limit of determination is 0.024 pg/m3～0.12 pg/m3.See Appendix B for details.

2 Normative references

This standard refers to the following documents or clauses thereof. For dated references, only the dated version applies to this standard. For undated references, the latest edition (including all amendments) applies to this standard. HJ 194 Technical Specification for Manual Monitoring of Ambient Air Quality HJ 691 Technical Guidelines for Sampling of Semi-volatile Organic Compounds in Ambient Air HJ 900 Determination of Organochlorine Pesticides in Ambient Air Gas Chromatography-Mass Spectrometry

3 Principles of the method

This method uses an active sampler to collect ambient air particulate matter and organochlorine pesticides in the gas phase to filter membranes and polyurethane foam (PUF) Add isotope-labeled extraction internal standard to the sampled filter membrane and PUF, extract with n-hexane-dichloromethane mixed solvent, and extract the solution. After concentration, purification and other operations, an isotope-labeled injection internal standard was added to it, and high-resolution gas chromatography-high-resolution mass spectrometry was used for separation and detection. According to the retention time and the monitoring ion abundance ratio, the isotope dilution method was used for quantification.

4 Interference and cancellation

Other organic substances in the sample may interfere with the determination. Select a purification column such as Florisil, graphitized carbon black, etc. to remove the interference, see 7.3.4 for details.

5 Reagents and Materials

Unless otherwise stated, superior-grade pure reagents meeting national standards were used in the analysis, and the experimental water was newly prepared pure water. 5.1 Acetone (C3H6O). pesticide residue grade. 5.2 n-hexane (C6H14). pesticide residue grade. 5.3 Dichloromethane (CH2Cl2). pesticide residue grade. 5.4 Nonane (C9H20). pesticide residue grade. 5.5 Toluene (C7H8). pesticide residue grade. 5.6 n-hexane-dichloromethane mixed solvent. n-Hexane (5.2) and dichloromethane (5.3) were mixed in a 1.1 volume ratio. 5.7 Anhydrous sodium sulfate (Na2SO4). bake in a muffle furnace at 400 °C for 4 h, cool and seal it in a ground glass bottle with a stopper, and dry it. saved in the device. 5.8 Internal standard extraction. select isotope-labeled compounds as the internal standard for extraction, see Appendix C.1.Commercially available certified reference materials can be purchased directly (solution). 5.9 Internal standard for injection. Select the isotope-labeled compound as the internal standard for injection, see Appendix C.1.Commercially available certified standards can be purchased directly quality (solution). 5.10 Organochlorine pesticide standard solution series. refers to the mixture of the organochlorine pesticide standard substance and the corresponding internal standard substance prepared with nonane or other solvents. mixture. The mass concentration of the standard solution is accurately known, and the mass concentration series should cover the quantification of high-resolution gas chromatography-high-resolution mass spectrometry Linear range, including 5 or more mass concentration gradients, see Appendix C.2.Commercially available certified reference materials (solutions) can be purchased directly. 5.11 Florisil solid phase extraction column. 1 g, 74 μm~150 μm (200 mesh~100 mesh), the column volume is 6 ml~10 ml. 5.12 Graphitized carbon black solid phase extraction column. 500 mg, 38 μm ~ 125 μm (400 mesh ~ 120 mesh), the column volume is 6 ml ~ 10 ml. 5.13 Quartz/glass fiber membrane. the retention efficiency of 0.3 μm standard particles is not less than 99%. Bake in a muffle furnace at 400 ℃ before use Bake for 5 h, cool to room temperature, and store in a vacuum drying oven. 5.14 Polyurethane Foam (PUF). Commonly used density is 0.022 g/cm3.Wash it with boiling water before use, then put it in warm water Repeatedly scrub for more than 2 times, drain the water, put it in the oven to remove the water, and then use the following method to extract and clean the PUF (you can also use the processed by other equivalent methods). Soxhlet extraction and cleaning. The extraction solvent is n-hexane-dichloromethane mixed solvent (5.6). For other extraction conditions, please refer to the relevant information in HJ 900. content. The cleaned PUF was heated in a vacuum drying oven at 50 °C until the solvent was completely evaporated, and then placed in a vacuum drying oven for vacuum storage. Pressurized fluid extraction and cleaning. the extraction solvent is n-hexane-dichloromethane mixed solvent (5.6); the extraction temperature is 100 °C; the heating time is 5 min; The static extraction time was 8 min; the number of cycles was 3; the purge time was 180 s; the rinsing volume was 60%. The cleaned PUF is placed in a vacuum drying oven It was heated under vacuum at 50 °C until the solvent was completely evaporated, and then placed in a vacuum drying oven for vacuum storage. 5.15 Nitrogen. purity ≥99.999%. 5.16 Helium. purity ≥99.999%.

6 Instruments and equipment

6.1 Sampling device 6.1.1 Sampler Meet the relevant requirements of HJ 691 for the sampler, with automatic cumulative sampling volume, and can automatically convert the cumulative standard according to air temperature and air pressure The function of sampling volume under condition should have automatic timing, restart after power failure, and automatic compensation for flow changes caused by voltage fluctuations and resistance changes. Features. 6.1.2 Sampling head Meet the relevant requirements of HJ 691 for sampling heads. The sampling head is mainly composed of the filter membrane and the support part of the filter membrane, the sampling cylinder filled with the adsorbent, the sampling The sample tube holder and the silicone rubber sealing ring, etc., are shown in Figure 1.The material of the sampling head should be stainless steel or polytetrafluoroethylene that does not adsorb organic substances or An inert material that does not chemically react with the contaminants being tested. The filter membrane and the filter membrane support part include the upper pressure ring of the filter membrane, the sealing gasket, the filter membrane, the filter Membrane support mesh and filter membrane support frame. There is a glass sampling cylinder inside the sampling cylinder holder, and the bottom of the glass sampling cylinder is provided with an adsorbent fixing net, and the adsorbent material is PUF. There are silicone rubber sealing gaskets between the sampling cylinder and the filter membrane support frame and the bottom of the glass sampling cylinder for sealing. 6.2 Analytical instruments 6.2.1 High-resolution gas chromatograph 6.2.1.1 Injection port. with split/splitless injection function, the maximum operating temperature is not lower than 280 ℃. 6.2.1.2 Column oven. It has the function of temperature program and can be adjusted in the range of 50 °C to 350 °C. 6.2.1.3 Chromatographic column. 30 m × 0.25 mm × 0.2 μm, a special chromatographic column for the analysis of medium-polarity organochlorine pesticides or other equivalent capillary color column. 6.2.1.4 Carrier gas. Helium (5.16). 6.2.2 High-resolution mass spectrometer 6.2.2.1 It has a gas connection interface. 6.2.2.2 With electron bombardment ion source, the electron energy can be adjusted in the range of 25 eV ~ 70 eV. 6.2.2.3 It has the function of selected ion monitoring, and uses the locked mass mode (Lock mass) for mass calibration. 6.2.2.4 The static resolution is greater than 8000 (10% peak-valley definition, the same below) and can be stable for at least 24 hours. 6.2.2.5 Data processing system. capable of collecting, recording and storing mass spectrometry data in real time. 6.3 Pretreatment device 6.3.1 Sample extraction device. Soxhlet extractor, pressurized fluid extraction device or other extraction device with equivalent performance. 6.3.2 Vacuum drying oven with heating function. the heating temperature should not be lower than 50 ℃. 6.3.3 Concentrating device. rotary evaporator, nitrogen blowing concentrator or other concentrating device with equivalent performance. 6.3.4 Solid phase extraction device. with flow control function. 6.3.5 Common laboratory instruments and equipment.

7 samples

7.1 Collection of samples 7.1.1 Ambient air samples Sampling as required by HJ 194 and HJ 691.Meteorological parameters such as air temperature, air pressure, wind speed, and wind direction at the sampling site should be measured, and the sampling should be recorded. technical parameters of the process. Before sampling, confirm that the quartz/glass fiber filter (5.13) is not damaged, then gently clamp the edge of the filter with tweezers and place it On the filter membrane support net, install the glass sampling cylinder with PUF (5.14) on the sampling cylinder holder, assemble the sampling head in sequence as shown in Figure 1, and then place the The sampling head is mounted on the sampler and ensures that the instrument is stable. The air tightness of the sampling system and the stability of instrument operation should be checked before each sampling. Check to ensure that the instrument meets the requirements before sampling. After sampling, turn off the power, remove the sampling head, and put it in a clean, non-polluting and dark place. Take out the filter membrane from the sampling head, fold the dust side inwards, take out the glass sampling cylinder from the sampling head, wrap it with aluminum foil, and put it in the storage box Store tightly sealed. The filtered membrane and PUF after sampling are ambient air samples. Note. There should be no creases on the filter membrane before sampling; when PUF is loaded into the glass sampling tube, make sure that there is no gap between the PUFs and between the PUF and the inner wall of the glass sampling tube. 7.1.2 Full program blank sample Bring the sealed blank quartz/glass fiber filter membrane (5.13) and the glass sampling cartridge filled with blank PUF (5.14) to the sampling site, It is installed on the sampling head without sampling, then the filter membrane and glass sampling cylinder are taken out, stored in the same way as the sample, and shipped together with the sample. Back to the lab. 7.2 Storage of samples After the samples were collected, they were placed in airtight bags, stored in the dark and refrigerated, and the extraction was completed within 60 days. The sample extract should be kept refrigerated and protected from light below 4 °C. stored, and the analysis was completed within 40 days. 7.3 Preparation of test specimens 7.3.1 Extraction of samples 7.3.1.1 Addition of Extraction Internal Standard The extraction internal standard (5.8) should be added prior to sample extraction. Pipette a certain volume of the extracted internal standard and add it to the sample evenly, and place it in the dark for 1 h. Then proceed to the next step. The addition amount of the extraction internal standard can be appropriately increased or decreased according to the division ratio of the sample solution, so that the extracted internal standard in the sample on the machine can be increased or decreased appropriately. It is the same as the mass concentration of the extracted internal standard when making the relative response factor. 7.3.1.2 Extraction and water removal 7.3.1.2.1 Extract the sample (7.1) by the Soxhlet extraction method. take the PUF out of the glass sampling cylinder and put it into the Soxhlet together with the filter membrane. In the extractor (6.3.1), use a small amount of acetone (5.1) to clean the glass sampling cylinder, and the cleaning solvent is combined into the sample, according to the method of 7.3.1.1. method to add extraction internal standard. Use n-hexane-dichloromethane mixed solvent (5.6) as the extraction solvent, other conditions refer to the relevant Soxhlet extraction in HJ 900. Extract the content. After the extraction is completed, add anhydrous sodium sulfate (5.7) to the receiving bottle until the sodium sulfate particles can flow freely. 30 min to fully remove water. 7.3.1.2.2 Extract the sample (7.1) by means of pressurized fluid extraction. remove the PUF from the glass sampling cylinder and place it with the filter membrane. into the pressurized fluid extraction device (6.3.1), rinse the glass sampling cylinder with a small amount of acetone (5.1), and combine the cleaning solvent into the sample. The method of 7.3.1.1 was performed after adding the extraction internal standard. Extraction conditions. the extraction solvent is n-hexane-dichloromethane mixed solvent (5.6); The temperature was 100 °C; the heating time was 5 min; the static extraction time was 8 min; the number of cycles was 3 times; the purging time was 180 s; the rinsing volume was 60%. After the extraction, add anhydrous sodium sulfate (5.7) to the receiving bottle until the sodium sulfate particles can flow freely, and leave it for 30 minutes to fully remove water. Note. Other equivalent extraction methods can also be used if verified. 7.3.2 Concentration of samples Transfer the sample extract (7.3.1.2) to a concentration bottle, select a rotary evaporator (6.3.3) or other concentration device, and concentrate to 1 ml~ 2 ml. NOTE. Avoid evaporation or blow-drying of the sample solution. 7.3.3 Constant volume and division of the sample solution According to the estimated mass concentration of organochlorine pesticides in the sample, the concentrated sample (7.3.2) is accurately adjusted to a certain volume with n-hexane (5.2). Integrate, divide the 10%~100% (integer ratio) sample solution after constant volume as the purified sample solution, and store the remaining sample solution in the dark and refrigerated. live. 7.3.4 Cleanup of samples 7.3.4.1 Florisil SPE column cleanup 7.3.4.1.1 Activation Install the Florisil SPE column (5.11) on the SPE unit (6.3.4), add 5 ml of toluene (5.5), open the valve Open the door to let a few drops of toluene flow out to exhaust the air in the column packing, close the valve and let the toluene soak the column packing for 5 minutes, open the valve to let the toluene flow out, When the liquid level of 1 mm to 2 mm remains above the column packing, close the valve and keep the column packing in a wet state. The toluene effluent was discarded. 7.3.4.1.2 Loading samples Accurately draw a certain volume of sample solution (7.3.3), add it to the activated solid phase extraction column, open the valve, and control the flow rate at each 1 to 2 drops per second, collect all the sample effluent. Close the valve when there is a liquid level of 1 mm to 2 mm above the column packing. Note. The sample loading body should be appropriately increased or decreased according to the situation of organochlorine pesticides and interferences in the sample, as well as the specifications of the Florisil SPE column, the amount of filler and other factors. product. According to the purification method of this standard, the added solution volume (including the sample volume and the solution volume for washing the sample bottle) should be no more than 2 ml. each real The laboratory needs to conduct a conditional test before use. As long as the quality control requirements specified in this standard can be met, other sample volumes can also be used. 7.3.4.1.3 Elution Aspirate 10 ml of toluene (5.5), add it to the solid phase extraction column after loading, open the valve, and control the flow rate at 1 to 2 drops per second. Collect all eluate. The eluate and sample effluent were combined as the cleaned-up sample solution. 7.3.4.1.4 Concentration Concentrate the purified sample solution (7.3.4.1.3) to 1 ml to 2 ml and then purify it with a graphitized carbon black solid phase extraction column. 7.3.4.2 Graphitized carbon black SPE column cleanup 7.3.4.2.1 Activation Install the graphitized carbon black solid phase extraction column (5.12) on the solid phase extraction device (6.3.4) and activate it according to the method in 7.3.4.1.1. 7.3.4.2.2 Loading samples Add the concentrated sample solution of 7.3.4.1.4 to the activated solid phase extraction column, wash the sample vial with n-hexane, and load the sample together. beat Open the valve, control the flow rate at 1 to 2 drops per second, and collect all the sample effluent. Turn off when there is a liquid level of 1 mm to 2 mm above the column packing. Close the valve. Note. The sample should be appropriately increased or decreased according to the situation of organochlorine pesticides and interferences in the sample, as well as the specifications of the graphitized carbon black solid phase extraction column, the amount of packing and other factors. product. According to the purification method of this standard, the added solution volume (including the sample volume and the solution volume for washing the sample bottle) should be no more than 2 ml. each real The laboratory needs to conduct a conditional test before use. As long as the quality control requirements specified in this standard can be met, other sample volumes can also be used. 7.3.4.2.3 Elution Elute the graphitized carbon black solid phase extraction cartridge after loading according to the method in 7.3.4.1.3. 7.3.4.2.4 Concentration Concentrate the sample solution of 7.3.4.2.3 to 1 ml ~ 2 ml. 7.3.5 Preparation of samples on the machine Add 20 μl of nonane (5.4) to the injection vial, transfer the concentrated sample solution (7.3.4.2.4) to the injection vial containing nonane, flush with nitrogen After the gas (5.15) is purged and concentrated to about 20 μl, add the injection internal standard (5.9) to the injection bottle to prepare the sample on the machine, so that the sample is injected into the sample on the machine. The mass concentration of the internal standard in the sample is the same as the mass concentration of the internal standard in the injection when making the relative response factor. Mix well and wait for analysis. 7.4 Preparation of blank samples 7.4.1 Full program blank Full-program blank sample (7.1.2) Prepare the full-program blank sample according to the same operation steps as the sample preparation (7.3). 7.4.2 Laboratory Blanks Quartz/glass fiber filter membrane (5.13) and PUF (5.14) processed in the same batch are directly prepared according to the sample preparation without going through the sampling step. Prepare a laboratory blank sample with the same operation steps as (7.3).

8 Analysis steps

8.1 Instrument Reference Conditions 8.1.1 High-resolution gas chromatography reference conditions Injection port temperature. 250 °C. Injection method. splitless. Injection volume. 1 μl. Transfer line temperature. 280°C. Mass calibration substance. Perfluorokerosene (PFK) or other mass calibration substance. Mass calibration material cell temperature. 130 °C. Heating program. the initial temperature was 110 °C, maintained for 1 min, and then increased to 210 °C at a rate of 20 °C/min, and then increased at a rate of 1.5 °C/min. The temperature was raised to 218 °C, held for 1 min, and then increased to 260 °C at a rate of 2 °C/min and held for 1 min. Carrier gas. Helium (5.16). Column flow (constant flow mode). 1.0 ml/min. 8.1.2 High-resolution mass spectrometry reference conditions Ion source temperature. 280 °C. Electron energy. 35 eV. Capture current. 650 μA. Detector voltage. 350 V. Resolution. Greater than 8000. Set instrument parameters and determine retention time window division using standard solutions (5.10), using Selected Ion Monitoring Mode (SIM) Two monitoring ion peaks (M1, M2) of the target compound were monitored. Quantitative reference material, reference retention time and window division, monitoring The measured ion mass-to-charge ratio, the monitored ion abundance ratio and its variation range are shown in Table D.1. 8.2 Calibration 8.2.1 Instrument tuning Set high-resolution gas chromatography-high-resolution mass spectrometry conditions as required in 8.1.1 and 8.1.2.Introduce mass calibration material for stable response Then, optimize the parameters of the mass spectrometer so that the static resolution of the monitored ions of the mass calibration material is greater than 8000. 8.2.2 Mass Correction Perform mass calibration in locked mass mode after instrument tuning. The resolution of all monitored ions of the mass calibration material should be greater than 6000, And the resolution of monitoring ions near the middle mass number in the same time window should be greater than 8000.Mass calibrators corresponding to each window See Table D.1 for mass-locked ions. 8.2.3 Average relative response factor Draw a certain volume of the standard solution of organochlorine pesticides (5.10), inject it into the set high-resolution gas chromatography-high-resolution mass spectrometry, and separate The target compound, extraction internal standard, and injection internal standard in the standard solution should be determined separately, and at least 5 concentrations should be determined. standard for calculation The relative response factors (RRFes) of each target compound in the solution to the extraction internal standard, the relative response factor of the extraction internal standard to the injection internal standard Subs (RRFrs), see Table D.1 for quantitative relationships. RRF ---- rs--the average relative response factor of the extracted internal standard relative to the injected internal standard. 9.4 Result representation The retention of the number of digits after the decimal point of the determination result is consistent with the detection limit of the method, and a maximum of 3 significant figures are retained. 10 Accuracy 10.1 Precision Six laboratories performed six replicates of blank samples spiked at 100 pg, 400 pg, and 15 ng, and 25 organochlorine pesticides The intra-laboratory relative standard deviations were 1.4%-30%, 0.5%-23%, and 1.1%-19%, respectively; the inter-laboratory relative standard deviations were 4.0%～31%, 2.8%～22% and 1.7%～20%; repeatability limits are 0.013 pg/m3～1.1 pg/m3, 0.028 pg/m3～2.3 pg/m3, respectively and 1.27 pg/m3 to 97.3 pg/m3; reproducibility limit...

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