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HJ 951-2018 English PDF

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HJ 951-2018: Solid waste - Determination of semivolatile organic compounds - Gas chromatography mass spectrometry
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Basic data

Standard ID HJ 951-2018 (HJ951-2018)
Description (Translated English) Solid waste - Determination of semivolatile organic compounds - Gas chromatography mass spectrometry
Sector / Industry Environmental Protection Industry Standard
Classification of Chinese Standard Z13
Word Count Estimation 38,363
Date of Issue 2018-07-29
Date of Implementation 2018-12-01
Regulation (derived from) Ministry of Ecology and Environment Announcement No. 21 of 2018
Issuing agency(ies) Ministry of Ecology and Environment

HJ 951-2018: Solid waste - Determination of semivolatile organic compounds - Gas chromatography mass spectrometry


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Solid waste - Determination of semivolatile organic compounds - Gas chromatography mass spectrometry National Environmental Protection Standard of the People's Republic Determination of semi-volatile organic matter in solid waste Gas chromatography-mass spectrometry Solid waste-determination of semivolatile organic compounds - Gas chromatography mass spectrometry Published on.2018-07-29 2018-12-01 Implementation Ministry of Ecology and Environment Ministry of the Environment release i directory Foreword.ii 1 Scope..1 2 Normative references..1 3 method principle..1 4 Reagents and materials.1 5 instruments and equipment.3 6 samples.3 7 Analysis steps..6 8 Results calculation and representation 10 9 Precision and accuracy 12 10 Quality Assurance and Quality Control..12 11 Precautions.13 12 Waste treatment.14 Appendix A (Normative) Method Detection Limit and Lower Limit of Measurement 15 Appendix B (informative) Reference parameters for the determination of target compounds 18 Appendix C (informative) Precision and accuracy of the method 21

Foreword

To implement the Environmental Protection Law of the People's Republic of China and the Law of the People's Republic of China on the Prevention and Control of Environmental Pollution by Solid Waste To protect the environment, protect human health, and regulate the determination of semi-volatile organic compounds in solid waste and its leachate. standard. This standard specifies gas chromatography-mass spectrometry for the determination of semi-volatile organic compounds in solid waste and its leachate. Appendix A of this standard is a normative appendix, and Appendix B~Appendix C is an informative appendix. This standard is the first release. This standard is formulated by the Environmental Monitoring Department and the Science and Technology Standards Department. This standard was drafted. Henan Environmental Monitoring Center. This standard is verified by. Xinxiang City Environmental Protection Monitoring Station, Henan Environmental Science Research Institute, Henan Entry-Exit Inspection Technical Center of the Epidemic Bureau, Environmental Monitoring Station of Kaifeng City, Institute of Hydrogeology and Environmental Geology of Chinese Academy of Geological Sciences and Environment of Henan Province Monitoring center. This standard is approved by the Ministry of Ecology and Environment on July 29,.2018. This standard has been implemented since December 1,.2018. This standard is explained by the Ministry of Ecology and Environment. 1 Determination of semi-volatile organic matter in solid waste - Gas chromatography - mass spectrometry Warning. The organic solvents and reference materials used in the experiment are toxic and hazardous substances, standard solution preparation and sample preparation. The process should be carried out in a fume hood; protective equipment should be worn as required to avoid direct contact with skin and clothing.

1 Scope of application

This standard specifies gas chromatography-mass spectrometry for the determination of semi-volatile organic compounds in solid waste and its leachate. This standard applies to chlorinated hydrocarbons, phthalates, nitrosamines, ethers, halogens in solid waste and its leachate. Ethers, ketones, anilines, pyridines, quinolines, nitroaromatics, phenols including nitrophenols, organochlorine pesticides, Screening and quantitative analysis of 64 semi-volatile organic compounds such as polycyclic aromatic hydrocarbons. When the solid waste (ash) sample is 10 g and the volume is 1.0 ml, 64 kinds of semi-volatile organic compounds The detection limit was 0.04~0.4 mg/kg, and the lower limit of determination was 0.16~1.6 mg/kg. When solid waste (biochemical sludge) is sampled When the volume is 2 g and the volume is 1.0 ml, the detection limit of 64 semi-volatile organic compounds is 0.3~1 mg/kg. The limit is 1.2~4 mg/kg. When the solid waste leachate has a sample volume of 100 ml and a constant volume of 10.0 ml, 64 semi-volatile organic compounds The detection limit of the method was 0.1~0.8 mg/L, and the lower limit of determination was 0.4~3.2 mg/L. The detection limits and lower limit of determination of solid waste and its leachate are detailed in Appendix A.

2 Normative references

This standard refers to the following documents or their terms. For undated references, the valid version applies to this standard. HJ 765 solid waste organic matter extraction microwave extraction HJ 782 solid waste organic matter extraction pressurized fluid extraction HJ 834 Determination of semi-volatile organic matter in soils and sediments - Gas chromatography - mass spectrometry HJ/T 20 Technical Specifications for Sampling and Sample Preparation of Industrial Solid Waste HJ/T 298 Hazardous Waste Identification Technical Specification HJ/T 299 solid waste leaching toxicity leaching method sulfuric acid nitric acid method HJ/T 300 solid waste leaching toxicity leaching method acetic acid buffer solution method

3 Principle of the method

The semi-volatile organic compounds in the solid waste and the leachate are separated, purified, concentrated, and made up to a volume by gas chromatography. Mass spectrometry detection. According to the mass spectrum, retention time, fragment ion mass-to-charge ratio and its abundance qualitative, the internal standard method is used for quantification.

4 reagents and materials

Unless otherwise stated, analytically pure reagents that meet national standards were used for the analysis. The experimental water is freshly prepared pure water or 2 distilled water. 4.1 Acetone (C3H6O). pesticide residue level. 4.2 Dichloromethane (CH2Cl2). pesticide residue grade. 4.3 Ethyl acetate (C4H8O2). pesticide residue grade. 4.4 Cyclohexane (C6H12). pesticide residue grade. 4.5 Dichloromethane-acetone mixed solvent. 1 1. Mix with dichloromethane (4.2) and acetone (4.1) in a 1.1 volume ratio. 4.6 Gel Permeation Chromatography Mobile Phase. Mix with 1.1 volume ratio with ethyl acetate (4.3) and cyclohexane (4.4), or prepare other solvents according to the instrument manual. system. 4.7 Nitric acid. ρ (HNO3) = 1.42 g/ml, excellent grade pure. 4.8 Nitric acid solution. 1 1. It was prepared by mixing nitric acid (4.7) and water in a 1.1 volume ratio. 4.9 Sodium chloride (NaCl). excellent grade. It was placed in a muffle furnace and baked at 400 ° C for 4 h. After cooling, it was sealed in a glass bottle with a stopper and placed in a desiccator for storage. 4.10 Standard stock solution of semi-volatile organic compounds. ρ=1000～5000 mg/L. Commercially available certified standard solutions can be purchased directly. 4.11 Standard use solution for semi-volatile organic compounds. ρ=200～500 mg/L. Dilute the semi-volatile organic standard stock solution (4.10) with a dichloromethane-acetone mixed solvent (4.5), and Mix well. 4.12 Internal standard stock solution. ρ=5000 mg/L. 1,4-Dichlorobenzene-d4, naphthalene-d8, 苊-d10, phenanthrene-d10, 䓛-d12 and 苝-d12 were selected as internal standards. Can be purchased directly for sale Certified standard solution. Other semi-volatile organic compounds with similar properties may also be used as internal standards. 4.13 Internal standard use solution. ρ=200～500 mg/L. The internal standard stock solution (4.12) was diluted with a dichloromethane-acetone mixed solvent (4.5) and mixed. 4.14 Standard stock solution for substitutes. ρ=1000～5000 mg/L. Phenol-d6, 2-fluorophenol, 2,4,6-tribromophenol, nitrobenzene-d5, 2-fluorobiphenyl, 4,4'-terphenyl-d14 were used as the substitute Substance. Commercially available certified standard solutions can be purchased directly. 4.15 Standard use solution for alternatives. ρ=200～500 mg/L. The substitute standard stock solution (4.14) was diluted with a dichloromethane-acetone mixed solvent (4.5) and mixed. 4.16 Decafluorotriphenylphosphine (DFTPP) standard solution. ρ = 50 mg/L. Commercially available certified standard solutions can be purchased directly. Other concentrations were diluted to a concentration of 50 mg/L with dichloromethane (4.2). 4.17 Gel Permeation Chromatography Calibration Standard Solution. Containing corn oil (25 mg/ml), di(2-ethylhexyl) phthalate (1 mg/ml), methoxychlor (200 mg/L), A mixed solution of hydrazine (20 mg/L) and sulphur (80 mg/L). Commercially available certified standard solutions can be purchased directly. 4.18 Desiccant. superior grade anhydrous sodium sulfate (Na2SO4) or granular diatomaceous earth 150-250 μm (100-60 mesh). Bake in a muffle furnace at 400 ° C for 4 h, cool and place in a glass jar with a stoppered glass and seal in a desiccator. 4.19 Column. 20 mm inner diameter, 10-20 cm long, with Teflon piston, made of glass or other equivalent Energy materials. 34.20 Quartz sand. 150~830 μm (100~20 mesh). It was baked in a muffle furnace at 400 ° C for 4 h, cooled and placed in a glass jar with a stopper to seal and stored. 4.21 Glass wool or glass fiber filter. Dip with dichloromethane (4.2) before use, wait until the methylene chloride is volatilized, store in a glass jar with a stopper and store it in a sealed container. 4.22 Sleeve of glass fiber or natural fiber. The glass fiber sleeve was placed in a muffle furnace at 400 ° C for 4 h before use, and the natural fiber sleeve was the same as the sample extraction. The solvent is treated by ultrasound or Soxhlet extraction. 4.23 High purity nitrogen. purity ≥ 99.999%. 4.24 High purity helium. purity ≥ 99.999%.

5 Instruments and equipment

5.1 Gas Chromatography-Mass Spectrometer. has an electron bombardment source (EI source). 5.2 Column. quartz capillary column, 30 m × 0.25 mm × 0.25  m, stationary phase is 5% phenyl-95% methyl silicone Alkane, or other equivalent capillary column. 5.3 Extraction device. A comparable device such as a Soxhlet extractor or a pressurized fluid extractor. 5.4 Gel Permeation Chromatograph. A 254 nm fixed-wavelength UV detector filled with a gel packing purification column. 5.5 Concentrator. Nitrogen blow concentrator, rotary evaporator or other concentrating device. 5.6 Vacuum freeze dryer. The vacuum of no-load is less than 13 Pa. 5.7 Solid phase extraction unit. 5.8 Flip-type oscillator. 5.9 Common instruments and equipment used in general laboratories.

6 samples

6.1 Sample collection and preservation Collection and storage of solid waste samples were carried out in accordance with the relevant regulations of HJ/T 20 and HJ/T 298. The sample should be clean Store in a brown glass jar with a stopper. It should be sealed, protected from light and refrigerated below 4 °C during transportation. After being shipped to the laboratory, if Can not be analyzed in time, should be refrigerated, protected from light, sealed and stored below 4 °C, the storage time does not exceed 10 d. 6.2 Preparation of samples 6.2.1 Preparation of solid waste leachate The preparation of solid waste leachate is carried out in accordance with the relevant regulations of HJ/T 299 or HJ/T 300. 6.2.2 Preparation of solid waste samples The preparation of solid waste samples is carried out in accordance with the relevant regulations of HJ 782 or HJ 765. 46.3 Preparation of samples 6.3.1 Preparation of samples of solid waste leachate 6.3.1.1 Extraction Transfer 100 ml of solid waste leachate (6.2.1) to a suitable volume of separatory funnel and add 8-20 μl of substitute Standard use solution (4.15) and appropriate amount of sodium chloride (4.9), add 20 ml of dichloromethane (4.2), shake well, stand still After the layer, the organic phase is dehydrated through a funnel containing an appropriate amount of anhydrous sodium sulfate (4.18), and the organic phase is collected in a concentrated bottle. The extraction was repeated once, the organic phase was combined, and the funnel and sodium sulfate layer were repeatedly washed with a small amount of dichloromethane (4.2) for 2 to 3 times. And the organic phase is to be concentrated. Note 1. If the concentration of the leachate is high, the sampling amount can be appropriately reduced. Note 2. If the emulsification occurs during the extraction process, it can be broken by freezing and stirring. 6.3.1.2 Concentration When using a nitrogen blow concentrator, the nitrogen gas should be turned on at room temperature to have a gas flow fluctuation on the surface of the solvent (to avoid the formation of a gas vortex). The concentrator wall exposed during the nitrogen blowing process was washed several times with dichloromethane (4.2), and the extract was concentrated to about 5 ml, no When purifying, all transfer, add appropriate amount of internal standard solution (4.13) (addition amount should be such that the internal standard concentration and calibration after constant volume The concentration of the internal standard in the line is the same), make up to 10.0 ml, mix and test. For purification, continue to concentrate to 1 ml for purification. Other equalization methods can also be used. Note. When purifying by gel permeation chromatography, when concentrating to about 1ml, add about 5 ml of gel permeation chromatography mobile phase (4.6). Solvent conversion was carried out and concentrated to about 1 ml for purification. 6.3.1.3 Purification The extract is darker in color and needs to be purified. When the purpose of the analysis is to screen all semi-volatile organic compounds, gel permeation chromatography or other equivalents should be used. Purification method. The gel permeation chromatography purification method is carried out according to a) gel permeation chromatography purification in 6.3.2.3.3. When analyzing specific semi-volatile organic compounds such as polycyclic aromatic hydrocarbons and organochlorine pesticides, chromatography with different adsorbents may be used. The column (4.19) is purified. The detailed procedure is carried out according to b) column purification in 6.3.2.3.3. 6.3.2 Preparation of solid waste samples 6.3.2.1 Aqueous liquid solid waste Weigh 10.0 g (accurate to 0.01 g) of the sample, add 90 ml of water, mix and transfer to the separatory funnel, the rest The steps are carried out in accordance with the procedures of 6.3.1.1 to 6.3.1.3. 6.3.2.2 Oily liquid solid waste Weigh an appropriate amount or 10.0 g (accurate to 0.01 g) of the sample, add appropriate amount of dichloromethane (4.2) until the sample is completely dissolved, After mixing, transfer all the ingredients into the separatory funnel, add 100 ml of water, and the rest of the steps are carried out according to the procedures of 6.3.1.1 to 6.3.1.3. 6.3.2.3 Solid and semi-solid solid waste 56.3.2.3.1 Extraction The extraction method may be selected from Soxhlet extraction, pressurized fluid extraction, microwave extraction or other equivalent extraction methods. Extraction solvent is Dichloromethane-acetone mixed solvent (4.5). a) Soxhlet extraction. transfer all the dehydrated solid waste samples (6.2.2) into glass fiber or natural fiber material In the cartridge (4.22), add the standard use solution (4.15) for the concentration near the middle point of the curve, and carefully place the sleeve in Soxhlet. In the extractor return tube, add 100 ml of dichloromethane-acetone mixed solvent (4.5) to the round bottom solvent bottle and extract for 16~18 h. The reflow speed is controlled at 4~6 times/h. After the extraction is completed, the round bottom solvent bottle is taken out and concentrated. b) Pressurized fluid extraction. extraction according to HJ 782 procedure. c) Microwave extraction. extraction according to HJ 765 procedure. Note 1. Samples of solid waste with high organic content can be appropriately reduced. Note 2. If there is significant moisture in the extract, further filtration and dehydration are required. a layer of glass wool or fiberglass filter on the glass funnel Membrane (4.21), about 5 g of anhydrous sodium sulfate (4.18) was added and the extract was filtered into a concentrating vessel. Use a small amount of dichloromethane - C The ketone mixed solvent (4.5) is used to wash the extraction container 3 times, the washing liquid is added to the funnel for filtration, and finally mixed with a small amount of dichloromethane-acetone. The solvent was rinsed with the solvent (4.5) and collected into a concentrating vessel for concentration. 6.3.2.3.2 Concentration When concentration is required, the following two concentration methods are recommended. Other methods can be used if they are verified to meet the requirements. a) nitrogen blowing Follow the procedure for nitrogen blown concentration in 6.3.1.2. b) Rotary evaporation The heating temperature was set at 30 to 60 ° C depending on the boiling point of the solvent, and the extract (6.3.2.3.1) was concentrated to 10 ml to stop concentration. Transfer the concentrate to a graduated concentrating vessel using a disposable dropper and mix the solvent with a small amount of dichloromethane-acetone (4.5) Rinse the bottom of the rotary evaporation bottle twice, combine all the concentrated liquids, and concentrate with nitrogen (6.3.1.2), then add the appropriate amount. Standard use liquid (4.13) (addition amount should be such that the internal standard concentration after constant volume is consistent with the internal standard concentration in the calibration curve) To 1.0 ml (can also be made up to 10.0 ml), to be tested. If purification is required, continue to concentrate to 1~2 ml for purification. Note. When the subsequent purification step is selected by gel permeation chromatography, the extract is concentrated to less than 5 ml with nitrogen blowing, and about 10 ml of gel permeate is added. The chromatographic mobile phase (4.6) was passed through and concentrated to 1 to 2 ml for purification. 6.3.2.3.3 Purification When purification is required, when the purpose of the analysis is to screen all semi-volatile organic compounds, gel permeation chromatography should be used. Law or other equivalent purification method. a) gel permeation chromatography purification 1) Calibration of gel permeation chromatography column Calibrate the gel permeation column according to the instrument instructions, and the resulting peak should meet the following conditions. all peak shapes Uniform symmetry; the resolution between the peaks of corn oil and di(2-ethylhexyl) phthalate is greater than 85%; phthalic acid The resolution between the chromatographic peaks of di(2-ethylhexyl)carboxylate and methoxydiazine is greater than 85%; the color of methoxychlor and hydrazine The resolution between peaks is greater than 85%; the peaks of bismuth and sulphur cannot overlap, and the baseline separation is greater than 90%. 2) Determine the collection time 6 The initial collection time of semi-volatile organic compounds is limited to the peak after the peak of corn oil to the peak of sulfur, and immediately after elution Stop collecting. Then use the semi-volatile organic standard solution (4.11) to directly inject the standard spectrum, according to the standard spectrum. The graph determines the start and stop collection times and determines the recovery. The determined collection time should ensure that the target recovery rate is ≥90%. 3) Cleaning on the machine According to the determined collection time, the concentrated extract is placed in turn, and the instrument is automatically cleaned and collected after programming. After liquid discharge, concentrate again (6.3.2.3.2), add appropriate amount of internal standard use solution (4.13) (addition amount should be such that the internal standard concentration after constant volume Keep the same concentration as the internal standard in the calibration curve. Make up to 1.0 ml (can also be made up to 10.0 ml), mix and test. b) column purification When analyzing specific semi-volatile organic compounds, such as polycyclic aromatic hydrocarbons, organochlorine pesticides, etc., it is possible to use different adsorbents. The column (4.19) is cleaned and the specific steps are performed in accordance with Appendix B of HJ 834. Collect the eluent and wait again After concentration (6.3.2.3.2), add appropriate amount of internal standard solution (4.13) (addition amount should be such that the internal standard concentration and calibration curve after constant volume The concentration of the internal standard is kept consistent. Adjust the volume to 1.0 ml (also to 10.0 ml), mix and test. 6.4 Preparation of blank samples 6.4.1 Solid waste leachate blank sample Replace the actual sample with quartz sand (4.20), prepare according to the solid waste leachate sample (6.2.1) and solid waste. A blank sample was prepared by the same procedure as in the preparation of the leachate sample (6.3.1). 6.4.2 Blank sample of solid waste Replace the actual sample with quartz sand (4.20) and prepare for the same procedure as the solid waste sample preparation (6.3.2). White sample.

7 Analysis steps

7.1 Instrument Reference Conditions 7.1.1 Gas Chromatography Reference Conditions Inlet. Temperature 280 ° C, no split. Injection volume. 1.0 μl. Column flow. 1.0 ml/min (constant current). Column temperature. 35 ° C for 2 min; 15 ° C/min to 150 ° C for 5 min; 3 ° C/min Hold at 290 ° C for 2 min. 7.1.2 Mass Spectrometry Reference Conditions Electron bombardment source. EI; Ion source temperature. 230 ° C; Ionization energy. 70 eV; Interface temperature. 280 ° C; Quadrupole temperature. 150 ° C 7 mass scanning range. 35 ~ 450 amu; Solvent delay time. 5 min. Data acquisition method. full scan mode (SCAN) or select ion scan mode (SIM). 7.2 Calibration 7.2.1 Mass spectrometry performance check Before each analysis, mass spectrometry should be performed automatically, and the gas chromatograph and mass spectrometer should be set to the instruments required by the analytical method. Conditions, and in standby mode, directly inject 1.0 μl of decafluorotriphenylphosphine (DFTPP) standard through the GC inlet Solution (4.16), to obtain the spectrum of decafluorotriphenylphosphine, the ion abundance of the mass fragments should meet the requirements in Table 1, Otherwise, the mass spectrometer ion source needs to be cleaned. Table 1 Evaluation of key ions and ion abundance of decafluorotriphenylphosphine (DFTPP) Mass-to-charge ratio (m/z) relative abundance specification mass-to-charge ratio (m/z) relative abundance specification 30%-60% of 51 198 peak (base peak) 5%-9% of.199 198 peak 68 less than 69 peaks 2% 275 base peaks 10%-30% 70% less than 69 peaks 365 is greater than 1% of the base peak 127 base peak 40%-60% 441 exists and less than 443 peak 197 1% 442 base peak less than 198 peak or 40% larger than 198 peak 198 base peak, abundance 100% 443 442 peak 17%-23% 7.2.2 Establishment of calibration curve Take 5 5 ml volumetric flasks and pre-add 2 ml of dichloromethane (4.2) to measure the appropriate amount of semi-volatile organic compounds. Standard use solution (4.11), substitute standard use solution (4.15) and internal standard use solution (4.13), with dichloromethane (4.2) After constant volume, mix and prepare into a standard series of 5 mass concentration points. The mass concentration of the target and the substitute is in turn 5.0 μg/ml, 10.0 μg/ml, 20.0 μg/ml, 40.0 μg/ml, 50.0 μg/ml, and the internal standard mass concentration was 40.0 μg/ml. According to the instrument reference conditions (7.1), the samples were injected sequentially from low to high concentrations. Sit with the target compound mass concentration The product of the ratio of the ratio of the target compound to the internal standard compound quantitative ion response and the internal standard compound mass concentration Mark, establish a calibration curve. The total ion chromatogram of the target is shown in Figure 1 under the instrument reference conditions recommended in this standard. 81. N-nitrosodimethylamine; 2.2-fluorophenol (alternative); 3. phenol-d6 (alternative); 4. phenol; 5. bis(2-chloroethyl)ether; 6.2-chlorophenol ; 7.1,3-dichlorobenzene; 8.1,4-dichlorobenzene-d4 (internal standard 1); 9.1,4-dichlorobenzene; 10.1,2-dichloro Benzene; 11.2-methylphenol; 12. bis(2-chloroisopropyl)ether; 13. hexachloroethane; 14. N-nitroso-di-n-propylamine; 15.4-methylphenol; 16. nitrobenzene -d5 (alternative); 17. nitrobenzene; 18. isophorone; 19.2-nitrophenol; 20.2, 4- Dimethylphenol; 21. bis(2-chloroethoxy)methane; 22.2,4-dichlorophenol; 23.1,2,4-trichlorobenzene; 24.naphthalene-d8 (internal standard 2); 25. naphthalene ; 26.4-chloroaniline; 27. hexachloro-1,3-butadiene; 28.4-chloro-3-methylphenol; 29.2-methyl Naphthalene; 30. Hexachlorocyclopentadiene; 31.2,4,6-trichlorophenol...

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