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HJ 1243-2022 English PDF

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HJ 1243-2022: Soil and sediment - Determination of 20 polybrominated biphenyls - Gas chromatography-high resolution mass spectrometry
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HJ 1243-2022719 Add to Cart 6 days Soil and sediment - Determination of 20 polybrominated biphenyls - Gas chromatography-high resolution mass spectrometry Valid

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Basic data

Standard ID: HJ 1243-2022 (HJ1243-2022)
Description (Translated English): Soil and sediment - Determination of 20 polybrominated biphenyls - Gas chromatography-high resolution mass spectrometry
Sector / Industry: Environmental Protection Industry Standard
Word Count Estimation: 31,355
Issuing agency(ies): Ministry of Ecology and Environment

HJ 1243-2022: Soil and sediment - Determination of 20 polybrominated biphenyls - Gas chromatography-high resolution mass spectrometry


---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.
Soil and sediment - Determination of 20 polybrominated biphenyls - Gas chromatography-high resolution mass spectrometry National Ecological Environment Standard of the People's Republic of China Determination of 20 kinds of polybrominated biphenyls in soil and sediment gas chromatography-high resolution mass spectrometry Soil and sediment-Determination of 20 polybrominated Posted on 2022-04-15 2022-11-01 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 Reagents and materials...1 5 Instruments and equipment...3 6 Samples...3 7 Analysis steps...5 8 Result calculation and representation...8 9 Accuracy...9 10 Quality Assurance and Quality Control...10 11 Waste Disposal...11 Appendix A (normative) Method detection limit and lower limit of determination...12 Appendix B (informative appendix) PBB standard stock solution and series reference concentration...13 Appendix C (Informative Appendix) Gel Permeation Chromatography Calibration Standard Solution Chromatogram...15 Appendix D (informative) Quantitative ions, auxiliary ions and their ion abundance ratios...16 Appendix E (Informative Appendix) Method Precision...17 Appendix F (informative appendix) Method correctness...23 Determination of 20 Polybrominated Biphenyls in Soil and Sediments by Gas Chromatography-High Resolution Mass Spectrometry Warning. The organic solvents and standard substances used in the experiment are toxic and harmful substances. The solution preparation and sample pretreatment process should be ventilated. It should be carried out in a cabinet; during operation, protective equipment should be worn as required to avoid direct contact with skin and clothing.

1 Scope of application

This standard specifies the gas chromatography-high resolution mass spectrometry method for the determination of polybrominated biphenyls in soil and sediment. This standard applies to 2-monobromobiphenyl, 3-monobromobiphenyl, 2,5-dibromobiphenyl, 2,6-dibromobiphenyl, 4,4'-dibromobiphenyl in soil and sediment Benzene, 2,4,6-Tribromobiphenyl, 2,2',4,5'-Tetrabromobiphenyl, 2,2',5,5'-Tetrabromobiphenyl, 3,3',4, 4'-tetrabromobiphenyl, 2,2',4,5,5'-pentabromobiphenyl, 2,2',4,5',6-Pentabromobiphenyl, 2,2',4,4',5,5'-hexabromobiphenyl, 2,2',4,4',5,6 '-Hexabromobiphenyl, 2,3,3',4,4',5-hexabromobiphenyl, 3,3',4,4',5,5'- Hexabromobiphenyl, 2,2',3,4,4',5,5'-heptabromobiphenyl, 2,2',3,3',4,4',5,5'-octabromobiphenyl Benzene, 2,3,3',4,4',5,5',6-octabromobiphenyl, 2,2',3,3',4,4',5,5',6-Nonabromobiphenyl, 2,2',3,3',4,4',5,5',6,6 Determination of 20 kinds of polybrominated biphenyls such as '-decabromobiphenyl. When the sampling amount is 10.0 g and the constant volume is 50 μl, the detection limit of the method for the determination of mono- to deca-bromobiphenyls in this standard is 0.01 μg/kg～ 0.1 μg/kg, the lower limit of determination is 0.04 μg/kg～0.4 μg/kg. See Appendix A 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. GB 17378.3 Marine Monitoring Specification Part 3.Sample Collection, Storage and Transportation GB 17378.5 Marine Monitoring Specification Part 5.Sediment Analysis HJ/T 91 Technical Specification for Surface Water and Sewage Monitoring HJ/T 166 Technical Specification for Soil Environment Monitoring HJ 442.4 Technical Specifications for Environmental Monitoring in Offshore Seas Part 4 Monitoring of Sediments in Offshore Seas HJ 494 Water Quality Sampling Technical Guide HJ 613 Gravimetric Method for Determination of Soil Dry Matter and Moisture

3 Principles of the method

The target compounds such as 2-bromobiphenyl in soil or sediment samples were extracted, concentrated, purified and fixed with organic solvents, and then analyzed by gas chromatography. Spectroscopic-high-resolution mass spectrometer separation and detection, qualitative determination based on retention time, characteristic ion abundance ratio, and quantification by isotope dilution internal standard method.

4 Reagents and Materials

Unless otherwise specified, analytical reagents that meet national standards are used in the analysis, and the experimental water is freshly prepared without target compounds. Distilled water or water prepared by pure water equipment. 4.1 Acetone (C3H6O). pesticide residue grade. 4.2 Toluene (C7H8). pesticide residue grade. 4.3 n-hexane (C6H14). pesticide residue grade. 4.4 Methanol (CH3OH). pesticide residue grade. 4.5 Dichloromethane (CH2Cl2). pesticide residue grade. 4.6 Nonane (C9H20). pesticide residue grade. 4.7 Hydrochloric acid (HCl). excellent grade, =1.18 g/ml. 4.8 Sulfuric acid (H2SO4). excellent grade pure, =1.84 g/ml. 4.9 Sodium hydroxide (NaOH). excellent grade pure. 4.10 Potassium hydroxide (KOH). excellent grade pure. 4.11 Anhydrous sodium sulfate (Na2SO4). excellent grade. Ignited at 450 °C for 4 h, cooled to 150 °C and transferred to a desiccator. After cooling to room temperature, it was put into a glass reagent bottle and kept in a desiccator. live. 4.12 Acetone-n-hexane mixed solvent. Acetone (4.1) and n-hexane (4.3) were mixed in a volume ratio of 1.9. 4.13 Hydrochloric acid solution. Hydrochloric acid (4.7) and water were mixed in a volume ratio of 1.5. 4.14 Sodium hydroxide solution. (NaOH)=40 g/L. Weigh 4 g of sodium hydroxide (4.9), dissolve it in a small amount of water, and dilute to 100 ml. 4.15 Potassium hydroxide solution. (KOH)=112 g/L. Weigh 11.2 g of potassium hydroxide (4.10), dissolve it in a small amount of water, and dilute to 100 ml. 4.16 Standard stock solution of polybrominated biphenyls. =50 μg/ml. For the standard solution of polybrominated biphenyls prepared with nonane (4.6) or other solvents, see Table B.1 in Appendix B. Available for direct purchase Standard solution, refrigerated, sealed, and protected from light below 4 °C, or stored in accordance with the requirements of the standard solution certificate. 4.17 Standard solution for polybrominated biphenyls. =1.0 μg/ml. Dilute the standard stock solution of polybrominated biphenyls (4.16) with toluene (4.2) or nonane (4.6), refrigerate, seal, and protect from light for 1 a at below 4 °C. 4.18 Extract internal standard stock solution. =50 μg/ml. Select isotope-labeled compounds as internal standards for extraction, see Table B.1 in Appendix B for details. Commercially available certified standard solutions can be purchased directly, 4 ℃ The following refrigerated, sealed, protected from light, or stored in accordance with the requirements of the standard solution certificate. 4.19 Internal standard extraction solution. =100 ng/ml. Dilute the extraction internal standard stock solution (4.18) with toluene (4.2) or nonane (4.6), refrigerate it below 4 °C, seal it, and store it in the dark for 1 a. 4.20 Internal standard stock solution for injection. =2000 μg/ml. Select isotope-labeled compounds as the injection internal standard, see Table B.1 in Appendix B. Commercially available certified standard solutions can be purchased directly, 4 ℃ The following refrigerated, sealed, protected from light, or stored in accordance with the requirements of the standard solution certificate. 4.21 Internal standard solution for injection. =100 ng/ml. Dilute the injection internal standard stock solution (4.20) with toluene (4.2) or nonane (4.6), refrigerate it below 4 °C, seal it, and store it in the dark for 1 a. 4.22 Calibration and tuning standard solution. high boiling point perfluoro kerosene (PFK-High), 98% purity. Commercially available certified standard solutions, refrigerated, sealed, and protected from light below 4 ℃, or stored in accordance with the requirements of the standard solution certificate. 4.23 Gel permeation chromatography calibration standard stock solution. corn oil (ρ=300 mg/ml), bis(2-ethylhexyl) phthalate (ρ=15 mg/ml), pentachlorophenol (ρ=1.4 mg/ml), pyrene (ρ=0.1 mg/ml), elemental sulfur (ρ=0.5 mg/ml), the solvent is dichloromethane alkane (4.5). Commercially available certified standard solutions, refrigerated, sealed, and protected from light below 4 ℃, or stored in accordance with the requirements of the standard solution certificate. 4.24 Copper powder (beads). Store in a desiccator, rinse with hydrochloric acid solution (4.13) and methanol (4.4) before use, and prepare for immediate use. 4.25 Silica gel. particle size of 75 µm to 230 µm (200 mesh to 100 mesh). Wash with dichloromethane (4.5), and after the dichloromethane is completely evaporated, spread it in an evaporating dish or beaker, the thickness is less than 10 mm, and the temperature is 130 °C. Activated under conditions for 18 h, and cooled in a desiccator for 30 min. Fill into glass reagent bottles and store in a desiccator. 4.26 Basic silica gel. Take 67 g of activated silica gel (4.25), add 33 g of sodium hydroxide solution (4.14) or potassium hydroxide solution (4.15), stir well, Make it a fluid powder. After the preparation is completed, put it into a glass reagent bottle, seal it, and store it in a desiccator. 4.27 Sulfuric acid silica gel. Take 100 g of activated silica gel (4.25), add 78.6 g of sulfuric acid (4.8), and stir well to make it a fluid powder. After preparation Pack into glass reagent bottles, seal and store in a desiccator. 4.28 Quartz sand. Burn at 450 °C for 4 h, cool to room temperature in a desiccator, transfer to a glass reagent bottle, and store in a desiccator. 4.29 Quartz wool. Before use, it was extracted with dichloromethane (4.5) under reflux for 24 h, dried and stored in an airtight glass container. 4.30 Nitrogen. purity ≥99.999%. 4.31 Helium. purity ≥99.999%.

5 Instruments and equipment

5.1 Brown screw-top glass bottle. 50 ml ~ 500 ml. 5.2 Gas chromatography-high resolution mass spectrometer. equipped with a splitless injection port, the maximum operating temperature is not lower than 280 °C, and on-column injection or Programmable temperature large volume injection method; programmable temperature column oven that can be adjusted in the temperature range of 50 ℃ to 350 ℃; with electron bombardment Shock ion source, the electron energy can be adjusted in the range of 25 eV to 70 eV; it has the function of selective ion monitoring, and uses the locked mass mode (Lock mass) for mass correction; dynamic resolution ≥5000 (10% peak-valley definition, the same below) and stable for at least 24 h. 5.3 Chromatographic column. 30 m (column length) × 0.25 mm (inner diameter) × 0.10 μm (film thickness), the stationary phase is 5% phenyl-95% methyl polysiloxane alkane, the maximum operating temperature is not lower than 350 ℃, or use other chromatographic columns with the same effect. 5.4 Soxhlet extractor or equivalent device. 5.5 Pressurized fluid extraction instrument. the extraction pressure is above 10.3 MPa, and the extraction temperature is above 100 ℃. 5.6 Multilayer silica gel column. glass column with an inner diameter of 8 mm to 15 mm and a length of.200 mm to 300 mm. Add some quartz wool to the bottom of the glass column (4.29), add 3 g silica gel (4.25), 5 g basic silica gel (4.26), 2 g silica gel (4.25), 10 g sulfuric acid silica gel (4.27), 2 g silica gel (4.25), 5 g anhydrous sodium sulfate (4.11). After packing, the multi-layer silica gel column was rinsed with 100 ml of n-hexane (4.3), and the liquid level was kept at Anhydrous sodium sulfate layer. Commercially available multi-layer silica columns can also be purchased for sample cleanup if blank validation is passed. 5.7 Automatic gel permeation chromatograph. equipped with UV detector (wavelength 254 nm) and gel column, packed with about 70 g of porous polystyrene diethyl ether Alkenylbenzene bioactive microsphere packing, 5 ml ~ 10 ml sample loop. 5.8 Concentration device. rotary evaporation concentrator, nitrogen blower or other concentration device with equivalent performance. 5.9 Freeze dryer. 5.10 General laboratory instruments and equipment.

6 samples

6.1 Sample Collection and Storage Soil samples were collected in accordance with the relevant requirements of HJ/T 166, and water sediment samples were collected in accordance with the relevant requirements of HJ/T 91 and HJ 494. Marine sediment samples were collected in accordance with the relevant requirements of GB 17378.3 and HJ 442.4. After the sample is collected, it should be stored in a brown screw-top glass bottle (5.1), and it should be refrigerated, protected from light and sealed during transportation. If not in time For analysis, it can be frozen, protected from light, and sealed for 1 year. 6.2 Preparation of samples Remove foreign matter (sticks, leaves, stones, etc.) in the sample, and mix the sample thoroughly. Samples can be dried using a freeze dryer (5.9). After drying, weigh two samples, each weighing approximately 10 g (to the nearest 0.01 g). Prepare air-dried soil and sediment samples according to the relevant requirements of HJ/T 166 and GB 17378.3 respectively. One soil sample for determination Dry matter content, another for extraction. One sediment sample was used for moisture determination and the other for extraction. 6.3 Determination of moisture The determination of the dry matter content of soil samples is performed in accordance with HJ 613, and the determination of moisture content of sediment samples is performed in accordance with GB 17378.5. 6.4 Preparation of test specimens 6.4.1 Extraction 6.4.1.1 Soxhlet extraction Weigh 10 g of sample (6.2) into the extraction cup of the Soxhlet extractor (5.4), add 10.0 μl of internal standard extraction solution (4.19), Extract with.200 ml ~ 300 ml acetone-n-hexane mixed solvent (4.12) and other solvents for more than 16 hours, and reflux 3 to 4 times per hour. the extract Concentrated to 1 ml ~ 2 ml, to be purified. Note. The extraction solvent acetone-n-hexane mixed solvent (4.12) can also be replaced by toluene (4.2) or n-hexane (4.3). 6.4.1.2 Pressurized fluid extraction Weigh 10 g of the sample (6.2) and transfer it to the extraction cell of the pressurized fluid extraction device (5.5), add 10.0 μl of the internal standard extraction solution (4.19). Set the extraction conditions, the pressure is 10.3 MPa, the temperature is 100 °C, and the extraction solvent is n-hexane-acetone mixed solvent (4.12), 100% Fill the extraction tank mode, static extraction time of 5 min, cycle 3 times, and collect the extract. The extract was concentrated to 1 ml ~ 2 ml, to be purified. Note. If the sample concentrate cannot be analyzed as soon as possible, it should be frozen below -10 °C and stored in the dark, and the analysis should be completed within 1 year. 6.4.2 Purification 6.4.2.1 Sulfur removal When the sample contains sulfur, the sulfur removal should be carried out first. Add 50 ml of n-hexane (4.3) to the concentrated extract (6.4.1), then add an appropriate amount of copper powder (beads) (4.24), shake well, Until the copper powder (beads) does not change color, let stand for 30 min, filter with a triangular funnel filled with anhydrous sodium sulfate (4.11), collect the filtrate, and concentrate to 1 ml to 2 ml. 6.4.2.2 Multilayer silica column purification Transfer the concentrated extract (6.4.1), or the concentrated solution (6.4.2.1) after desulfurization and purification to the multi-layer silica gel column (5.6), use 1 ml~ Rinse the container wall with 2 ml of n-hexane (4.3), repeat 2 to 3 times. with 120 ml n-hexane (4.3) at 2.5 ml/min (1 drop per second) Elution was carried out at a flow rate of 1 to 1, and the eluate was collected, and the eluate was concentrated to 1 ml to 2 ml. Concentrate the eluate further using the concentrator (5.8) When it is nearly dry, add 10.0 μl injection internal standard solution (4.21), and 40 μl nonane (4.6) or toluene (4.2), and mix well for measurement. 6.4.2.3 Automated gel permeation chromatography (GPC) cleanup When there is macromolecular interference in the sample, an automatic gel permeation chromatograph (5.7) can be selected to purify the concentrated extract (6.4.1). Then use the method in 6.4.2.1 or 6.4.2.2 for further purification and separation, or direct concentration and constant volume analysis. Rinse the automated gel permeation chromatograph with dichloromethane (4.5) and discard the eluent. Inject 5.00 ml GPC calibration standard The stock solution (4.23) is placed in the sample loop, and the calibration standard solution is automatically eluted with dichloromethane (4.5), and the response signal of the UV detector is recorded. No. The normal chromatographic elution peak sequence is corn oil, bis(2-ethylhexyl) phthalate, pentachlorophenol, pyrene and sulfur, gel permeation See Appendix C for the chromatogram of the chromatographic calibration standard solution. Set the polybrominated biphenyl collection time period, the peak of corn oil is more than 85% and the peak of corn oil is more than 85%, and bis(2-ethylhexyl) phthalate The time point when the ester can be collected is the time when the sample starts to collect, and the time point when the lowest signal peak between the pyrene and sulfur signals is the time when the sample ends. Dilute the concentrated extract (6.4.1) to 10.0 ml with dichloromethane (4.5), and accurately pipette 5.00 ml into the loop to make Elute with dichloromethane (4.5) and collect the eluent over a period of PBBs. Concentrate the eluent to 10 ml, add 3 ml of n-hexane (4.3), Continue to concentrate to 1 ml ~ 2 ml, and then further separate and purify according to the method in 6.4.2.1 or 6.4.2.2 to prepare samples for testing. Note 1.During the automatic gel permeation chromatography purification process, the gel permeation chromatography calibration standard stock solution (4.23) should be confirmed after every 20 samples. If the recovery rate of chlorophenol is higher than 85%, it is considered that the purification is effective; otherwise, it is necessary to re-extract and purify the samples of the previous treatment batch. Note 2.On the premise of meeting the quality control requirements of this method, other automatic or manual extraction and purification methods can be used after verification. 6.5 Preparation of blank samples Substitute quartz sand (4.28) for the actual sample, and carry out the preparation of the blank sample in the same manner as in the sample preparation (6.4).

7 Analysis steps

7.1 Instrument reference conditions 7.1.1 Gas chromatograph reference conditions The temperature program of the column oven. hold at 100 °C for 5 min, increase to 325 °C at 10 °C/min, and hold for 10 min. Carrier gas. Helium (4.31), Flow. 1.2 ml/min. Injection method. splitless injection. Injection volume. 1.0 μl, injection port temperature. 280 °C, transfer line temperature. 280 °C. 7.1.2 High-resolution mass spectrometer reference conditions Ion source temperature. 280 ℃; electron energy. 35 eV; data acquisition method. selective ion scanning detection; dynamic resolution R≥5000. See Appendix D for the selection of quantitative ions and qualifier ions for each target compound. 7.2 Calibration Tuning the mass spectrometer system before sample analysis, import the c......
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