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HJ 950-2018 English PDF

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HJ 950-2018: Solid waste - Determination of polycyclic aromatic hydrocarbon - Gas chromatography mass spectrometry
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Basic data

Standard ID HJ 950-2018 (HJ950-2018)
Description (Translated English) Solid waste - Determination of polycyclic aromatic hydrocarbon - Gas chromatography mass spectrometry
Sector / Industry Environmental Protection Industry Standard
Classification of Chinese Standard Z13
Word Count Estimation 24,278
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 950-2018: Solid waste - Determination of polycyclic aromatic hydrocarbon - Gas chromatography mass spectrometry


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Solid waste - Determination of polycyclic aromatic hydrocarbon - Gas chromatography mass spectrometry National Environmental Protection Standard of the People's Republic Determination of polycyclic aromatic hydrocarbons in solid waste Gas chromatography-mass spectrometry Solid waste-determination of polycyclic aromatic hydrocarbon - Gas chromatography mass spectrometry Published on.2018-07-29 2018-12-01 Implementation Ministry of Ecology and Environment released i directory Foreword.ii 1 Scope 1 2 Normative references 1 3 Principle of the method 1 4 reagents and materials..1 5 instruments and equipment..3 6 samples..4 7 Analysis step 7 8 Results calculation and representation 9 9 Precision and accuracy.11 10 Quality Assurance and Quality Control 12 11 Notes. 13 12 Waste Treatment..13 Appendix A (Normative Appendix) Method Detection Limit and Lower Limit of Measurement 14 Appendix B (informative) Reference parameters for the determination of target compounds 15 Appendix C (informative) The precision and accuracy of the method..16

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 This standard is formulated to protect the environment, protect human health, and regulate the determination of polycyclic aromatic hydrocarbons in solid waste and its leachate. This standard specifies gas chromatography-mass spectrometry for the determination of 16 polycyclic aromatic hydrocarbons in solid waste and its leachate. Appendix A of this standard is a normative appendix, and Appendix B to Appendix C are informative appendices. 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, Institute of Hydrogeology and Environmental Geology, Chinese Academy of Geological Sciences, Environmental Monitoring Station of Kaifeng City 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 polycyclic aromatic hydrocarbons in solid waste - Gas chromatography - mass spectrometry Warning. The organic solvents and reference materials used in the experiment are toxic substances, standard solution preparation and sample preparation process. It should be carried out in a fume hood; wear protective equipment 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 polycyclic aromatic hydrocarbons in solid waste and its leachate. This standard applies to solid waste and its leachate in naphthalene, terpenes, anthracene, anthracene, phenanthrene, anthracene, fluoranthene, anthracene, benzo[a] 蒽, 䓛, benzo[b]fluoranthene, benzo[k]fluoranthene, benzo[a]pyrene,dibenzo[a,h]pyrene,benzo[g,h,i] Determination of 16 polycyclic aromatic hydrocarbons such as 苝 and 茚[1,2,3,-cd]芘. When the solid waste (ash) sample is 10 g and the volume is 1.0 ml, 16 PAHs are detected. The limit is 0.05~0.3 mg/kg, and the lower limit of determination is 0.20~1.2 mg/kg. When the solid waste (biochemical sludge) is sampled at 2 g, When the volume is 1.0 ml, the detection limit of 16 polycyclic aromatic hydrocarbons is 0.3~1 mg/kg, and the lower limit is 1.2~4 mg/kg. When the solid waste leaching solution has a sampling volume of 100 ml and a constant volume of 1.0 ml, 16 polycyclic aromatic hydrocarbons are detected. The limit is 0.01~0.03 mg/L, and the lower limit of determination is 0.04~0.12 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. GB 5085.3 Identification criteria for hazardous wastes HJ 765 solid waste organic matter extraction microwave extraction HJ 782 solid waste organic matter extraction pressurized fluid extraction HJ 892 Determination of Polycyclic Aromatic Hydrocarbons in Solid Wastes by High Performance Liquid Chromatography 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

Polycyclic aromatic hydrocarbons in solid waste and leachate are extracted, purified, concentrated, and made up to a volume by gas chromatography 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 Hexane (C6H14). pesticide residue grade. 4.3 Dichloromethane (CH2Cl2). pesticide residue grade. 4.4 Ethyl acetate (C4H8O2). pesticide residue grade. 4.5 Pentane (C5H12). pesticide residue grade. 4.6 Cyclohexane (C6H12). pesticide residue grade. 4.7 n-hexane-acetone mixed solvent. 1 1. Mix with n-hexane (4.2) and acetone (4.1) in a 1.1 volume ratio. 4.8 Dichloromethane-pentane mixed solvent. 2 3. Mix with dichloromethane (4.3) and pentane (4.5) in a 2.3 volume ratio. 4.9 Dichloromethane-n-hexane mixed solvent I. 19. Mix with dichloromethane (4.3) and n-hexane (4.2) in a volume ratio of 1.9. 4.10 Dichloromethane-n-hexane mixed solvent II. 1 1. Mix with dichloromethane (4.3) and n-hexane (4.2) in a 1.1 volume ratio. 4.11 Gel Permeation Chromatography Mobile Phase. Mix with 1.1 volume ratio with ethyl acetate (4.4) and cyclohexane (4.6), or prepare other solvents according to the instrument manual. system. 4.12 Nitric acid. ρ (HNO3) = 1.42 g/ml, excellent grade pure. 4.13 Nitric acid solution. 1 1. It was prepared by mixing nitric acid (4.12) and water in a 1.1 volume ratio. 4.14 Standard stock solution of polycyclic aromatic hydrocarbons. ρ=1000～5000 mg/L. Commercially available certified standard solutions can be purchased directly. 4.15 Polycyclic aromatic hydrocarbon standard use solution. ρ=200～500 mg/L. The polycyclic aromatic hydrocarbon standard stock solution (4.14) was diluted with a n-hexane-acetone mixed solvent (4.7) and mixed. 4.16 Internal standard stock solution. ρ=5000 mg/L. Naphthalene-d8, 苊-d10, phenanthrene-d10, 䓛-d12 and 苝-d12 were selected as internal standards. Commercially available certified standard solutions can be purchased directly. Other compounds can also be used as internal standards. 4.17 Internal standard use solution. ρ=200～400 mg/L. The internal standard stock solution (4.16) was diluted with a n-hexane-acetone mixed solvent (4.7) and mixed. 4.18 Standard stock solution for substitutes. ρ=1000～5000 mg/L. 2-fluorobiphenyl and 4,4'-terphenyl-d14 were used as substitutes. Commercially available certified standard solutions can be purchased directly. Also available Deuterated markers of polycyclic aromatic hydrocarbons are used as substitutes. 4.19 Alternative standard use solution. ρ = 500 mg/L. The substitute standard stock solution (4.18) was diluted with a n-hexane-acetone mixed solvent (4.7) and mixed. 4.20 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 (4.3). 4.21 Gel Permeation Chromatography Calibration Standard Solution. Contains corn oil (25 mg/ml), di(2-ethylhexyl) phthalate (1 mg/ml), and methoxychlor (200 mg) A mixed solution of 3 mg/L), hydrazine (20 mg/L) and sulfur (80 mg/L). Commercially available certified standard solutions can be purchased directly. 4.22 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. 4.23 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. 4.24 Copper (powder). purity ≥ 99.5%. Before use, remove the oxide on the surface of the copper powder with a nitric acid solution (4.13), rinse off with water, and then clear with acetone (4.1). Wash, then use high-purity nitrogen (4.31) to dry and use, and treat the surface of the copper powder brightly before each use. 4.25 Silica gel. 75~150 μm (200~100 mesh). The silica gel is heated at 150-160 ° C for several hours for activation treatment, and then water is added to make it contain 10% to 20%. Water, sealed for use. The silica gel needs to be reactivated before use, activated at 130 ° C for at least 16 h, and taken out into a desiccator for cold. But, staying. 4.26 Column. 20 mm inner diameter, 10-20 cm long, with Teflon piston, made of glass or other equivalent Energy materials. 4.27 Magnesium silicate cartridge. 1 g/6 ml. 4.28 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. 4.29 Glass wool or glass fiber filter. Dip with dichloromethane (4.3) before use, wait until the methylene chloride is volatilized, store in a glass jar with a stopper and store it in a sealed container. 4.30 Sleeve of glass fiber or natural fiber. Before use, place the fiberglass sleeve in a muffle furnace at 400 ° C for 4 h, natural fiber sleeve and sample extraction. The same solvent is treated by sonication or Soxhlet extraction. 4.31 High purity nitrogen. purity ≥ 99.999%. 4.32 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. Rotary evaporator, nitrogen blower or other concentrating unit. 5.6 Vacuum freeze dryer. The vacuum of no-load is less than 13 Pa. 5.7 Flip-type oscillator. 5.8 Solid phase extraction unit. 5.9 Common instruments and equipment used in general laboratories. 46 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. 6.3 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 μl of replacement standard Use liquid (4.19) and appropriate amount of sodium chloride (4.23), then add 20 ml of dichloromethane (4.3), shake well and let stand. After the layer, the organic phase is dehydrated through a funnel containing an appropriate amount of anhydrous sodium sulfate (4.22), 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 washed repeatedly with a small amount of dichloromethane (4.3) 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 Samples with lower concentrations need to be concentrated. When using a nitrogen blow concentrator, the nitrogen should be turned on at the room temperature to the solvent surface. Fluctuating the gas flow (avoiding the formation of a gas vortex), washing the exposed concentrator wall during the nitrogen blowing process several times with dichloromethane (4.3). Concentrate the extract to about 1 ml. When it is not necessary to purify, transfer it all. Add the appropriate amount of internal standard solution (4.17). The internal standard concentration after constant volume should be kept consistent with the internal standard concentration in the calibration curve. Make up to 1.0 ml, mix and test. Elected When using a silica gel column purification method (6.3.2.3.3), concentrate to about 2 ml, add 5 ml of cyclohexane (4.6) and concentrate. To about 1 ml, the concentration process was repeated twice and the solvent was completely converted to cyclohexane for purification. Other equalization methods can also be used. 6.3.1.3 Purification The magnesium silicate cartridge (4.27) was fixed on a solid phase extraction unit (5.8) and rinsed with 4 ml of n-hexane (4.2). Add about 5 ml of n-hexane (4.2), close the control valve, infiltrate for 5 min, then slowly open the control valve. Continue to add 5 ml 5 N-hexane (4.2) is rinsed, and the control valve is closed and the effluent is discarded before the column packing is exposed to air. Concentrated extract The liquid (6.3.1.2) was transferred to a small column, and the concentrated bottle was washed in 2 ml of n-hexane (4.2), and the washing liquid was transferred to the small column. in. Slowly open the control valve, release some of the liquid, and close the control valve before the column packing is exposed to air. Slowly open the control The valve was eluted with 10 ml of dichloromethane-n-hexane mixed solvent I (4.9) at a rate of 1 ml/min. After liquid, reconcentrate (6.3.1.2), add appropriate amount of internal standard solution (4.17) (addition amount should be such that the internal standard concentration and calibration after constant volume The internal standard concentration in the quasi-curve remains the same), make up to 1.0 ml, mix and test. Other equivalent purification methods can also be used. 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 (4.3) 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 6.3.2.3.1 Extraction The extraction method may be selected from Soxhlet extraction, pressurized fluid extraction, microwave extraction or other equivalent extraction methods. a) Soxhlet extraction. transfer all the dehydrated solid waste samples (6.2.2) into glass fiber or natural fiber material In the cylinder (4.30), add the standard use solution (4.19) of the concentration near the middle point of the curve, and carefully place the sleeve on the cable. In the extractor of the extractor, add 100 ml of n-hexane-acetone mixed solvent (4.7) to the round bottom solvent bottle, and extract 16~ At 18 h, the reflux rate was controlled at 4 to 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 (4.29), about 5 g of anhydrous sodium sulfate (4.22) was added and the extract was filtered into a concentrating vessel. Use a small amount of n-hexane-prop The ketone mixed solvent (4.7) was used to wash the extraction container 3 times, the washing liquid was added to the funnel for filtration, and finally mixed with a small amount of n-hexane-acetone. The solvent (4.7) was rinsed through the funnel and all collected into a concentrating vessel to be concentrated. 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 is set at 30~60 °C according to the boiling point of the solvent, and the extract (6.3.2.3.1) is concentrated to about 10 ml, and the concentration is stopped. 6 shrink. Transfer the concentrate to a graduated concentrating vessel using a disposable dropper and mix the solvent with a small amount of n-hexane-acetone (4.7) Rinse the bottom of the rotary evaporation flask twice and combine all the concentrates. After concentrating with nitrogen (6.3.1.2), add appropriate amount of internal standard. Use liquid (4.17) (add the amount so 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 the liquid is to be purified, concentrate it with nitrogen (6.3.1.2) to 1-2 ml; when using silica gel column purification method, Add about 5 ml of cyclohexane (4.6) to concentrate to about 1 ml, repeat the concentration process twice, and completely convert the solvent into a cyclohexane. The alkane was concentrated to about 1 ml and to be purified. Note. When the subsequent purification step is purified by gel permeation chromatography, concentrate the extract to less than 5 ml and add about 10 ml of gel permeate. Chromatographic mobile phase (4.11), concentrated to 1~2 ml, to be purified. 6.3.2.3.3 Purification When purification is required, the concentrated extract (6.3.2.3.2) may be a silica gel column, a magnesium silicate cartridge or a gel penetrating color. The spectrum is purified in three ways. Other methods can be used if they are verified to meet the requirements. a) Silica gel column purification 1) Preparation of silica gel column Fill the bottom of the column (4.26) with glass wool (4.29) and add 1 to 2 cm thick anhydrous sodium sulfate (4.22). And 10~20 g silica gel (4.25), tap the column wall to fill the silica gel. Fill the upper part with 1~2 cm thick anhydrous sodium sulfate (4.22), if desulphurization is required, add about 2 g of copper powder (4.24) to the top of the column. Use 30~60 ml of dichloromethane (4.3) Wash and tap the column wall to avoid visible air in the packing. Close the piston when the solvent begins to flow out through the column, dip Foam the packing for at least 10 minutes, then open the column valve to release the dichloromethane, continue to add 30 ~ 60 ml of n-hexane (4.2), when Before the upper anhydrous sodium sulfate layer is exposed to air, the piston is closed and ready for use. 2) Purification The silica gel column prepared by rinsing with 40 ml of pentane (4.5) is controlled at 2 ml/min, in the eluent. When flowing through the anhydrous sodium sulfate (4.22) layer and remaining unexposed in the air, close the piston, discard the pentane eluent, and turn The extract (6.4.2.3.2), which was replaced with cyclohexane, was transferred to a silica gel column and washed with 2 ml of cyclohexane (4.6). Wall, all moved into the column, open the piston, slowly add 25 ml of pentyl before the anhydrous sodium sulfate layer is exposed to the air The alkane (4.5) was eluted and the pentane eluent was again discarded. Then elute with 25 ml of dichloromethane-pentane mixed solvent (4.8), and Collect all eluents. After concentration (6.3.2.3.2), add appropriate amount of internal standard solution (4.17) (the amount should be added to make the volume The concentration of the internal standard and the internal standard concentration in the calibration curve are the same. Mix well and dilute to 1.0 ml (can also be made up to 10.0 ml). To be tested. b) Magnesium silicate column purification Follow the steps for purifying the magnesium silicate cartridge in 6.3.1.3. c) gel permeation chromatography purification 1) Calibration of gel permeation chromatography column Calibrate the gel permeation column using the gel permeation chromatography calibration standard solution (4.21) according to the instrument instructions. The obtained chromatographic peak should satisfy the following conditions. all peak shapes are uniformly symmetrical; corn oil and di(2-ethylhexyl) phthalate The resolution between the chromatographic peaks of the ester is greater than 85%; the chromatographic peak of di(2-ethylhexyl) phthalate and methoxychlor The resolution is greater than 85%; the resolution between the peaks of methoxychlor and hydrazine is greater than 85%; the peaks of bismuth and sulphur cannot 7 overlap, baseline separation greater than 90%. 2) Determine the collection time The initial collection time of polycyclic aromatic hydrocarbons is limited to the peak after the peak of corn oil and before the peak of sulfur. set. Then use the polycyclic aromatic hydrocarbon standard solution (4.15) to directly inject the standard spectrum, and determine the starting point according to the standard spectrum. The collection time was stopped and the recovery rate was determined. 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 and concentration again (6.3.2.3.2), add appropriate amount of internal standard solution (4.17) (the amount should be added to make the internal standard thick after constant volume). The concentration of the internal standard in the calibration curve is the same), and the volume is adjusted to 1.0 ml (can also be adjusted to 10.0 ml) for testing. 6.4 Preparation of blank samples 6.4.1 Solid waste leachate blank sample Replace the actual sample with quartz sand (4.28), 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 (4.28) 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, or split injection. Injection volume. 1 μl. Column flow. 1.0 ml/min (constant current). Column temperature. 80 ° C for 2 min, at 20 ° C/min rate to 180 ° C, for 5 min; then at 10 ° C/min rate Rise to 290 ° C for 5 min. 7.1.2 Mass Spectrometry Reference Conditions Electr...

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