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HJ 912-2017 English PDF

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HJ 912-2017: Solid waste--Determination of organochlorine pesticides--Gas chromatography mass spectrometry
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HJ 912-2017659 Add to Cart 5 days Solid waste--Determination of organochlorine pesticides--Gas chromatography mass spectrometry Valid

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Basic data

Standard ID: HJ 912-2017 (HJ912-2017)
Description (Translated English): Solid waste--Determination of organochlorine pesticides--Gas chromatography mass spectrometry
Sector / Industry: Environmental Protection Industry Standard
Classification of Chinese Standard: Z13
Word Count Estimation: 27,237
Date of Issue: 2017-12-29
Date of Implementation: 2018-04-01
Regulation (derived from): Ministry of Environmental Protection Bulletin 2017 No. 86
Issuing agency(ies): Ministry of Ecology and Environment

HJ 912-2017: Solid waste--Determination of organochlorine pesticides--Gas chromatography 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.
People's Republic of China national environmental protection standards Solid waste-Determination of organochlorine pesticides -Gas chromatography mass spectrometry 2017-12-29 Posted 2018-04-01 implementation Directory Foreword .ii 1 scope of application .1 2 Normative references .1 3 method principle .1 4 Reagents and materials .1 5 instruments and equipment .3 6 samples .4 7 Analysis steps .8 8 Results Calculation and Presentation 10 9 Precision and accuracy 11 10 Quality Assurance and Quality Control ..12 11 Waste treatment .13 12 Precautions .13 Appendix A (Normative) Method detection limit and lower limit of determination Appendix B (Informative) Determination of the target compound reference parameter 16 Appendix C (informative) precision and accuracy of the method

Foreword

In order to carry out "Law of the People's Republic of China on Environmental Protection" and "Law of the People's Republic of China on Prevention and Control of Environmental Pollution by Solid Wastes" Protect the environment, protect human health, standardize the determination of organochlorine pesticides in solid waste and leachate, and develop this standard. This standard specifies the determination of solid waste and its leachate 23 kinds of organochlorine pesticides by gas chromatography - mass spectrometry. Appendix A of this standard is a normative appendix, Appendix B and Appendix C are informative appendices. This standard is released for the first time. This standard by the Environmental Protection Department of Environmental Monitoring Division and Science and Technology Standards Division to develop. This standard was drafted. Henan Environmental Monitoring Center. This standard verification unit. Xinxiang City Environmental Monitoring Station, Henan Province Environmental Science Research Institute, Zhengzhou City Environmental Protection Supervisor Center Station, Kaifeng City Environmental Monitoring Station, Institute of Hydrogeology and Environmental Geology, Chinese Academy of Geological Sciences and Henan Province Environmental Monitoring Center. This standard MEP approved on December 29,.2017. This standard since April 1,.2018 come into operation. This standard is interpreted by the MEP. Solid waste - Determination of organochlorine pesticides - Gas chromatography - mass spectrometry Warning. The organic solvents and reference materials used in the experiment are toxic substances, standard solution preparation and sample preparation Should be carried out in a fume hood; operation should be worn protective clothing as required to avoid direct contact with the skin and clothing.

1 scope of application

This standard specifies the determination of solid waste and its leachate organochlorine pesticides by gas chromatography - mass spectrometry. This standard applies to solid waste and leaching solution of α-BHC, HCB, β-BHC, γ-BHC, δ-BHC Hexachlorocyclohexane, Aldrin, Ephedrine B, α-Chlordane, Endosulfan I, γ-Chlordane, Dieldrin, p, p'- Endosulfan II, p, p'-Drip, o, p'-DDT, Endrin aldehyde, Endosulfan sulfate, p, p'-DDT, Endrin, Methoxy DDT, mirex and other 23 kinds of organochlorine pesticides determination. If other organochlorine pesticides through the verification, can also use this Standard determination. When the amount of ash solid waste sample was 10 g and the volume of constant volume was 1.0 ml, the detection limits of 23 organochlorine pesticides 0.02 ~ 0.09 mg/kg, the lower limit of determination was 0.08 ~ 0.36 mg/kg. When the sludge solid waste sampling volume of 2 g, the volume of the body The product detection limit of 23 organochlorine pesticides was 0.2-0.8 mg/kg when the product was 1.0 ml. The lower limit of determination was 0.8-3.2 mg/kg. When the sample volume of the leachate is 100 ml and the volume of constant volume is 10 ml, the detection limits of the 23 organochlorine pesticides are 0.04 ~ 0.1 mg/L, the lower limit of determination is 0.16 ~ 0.4 mg/L. Methods for detection of solid waste and leachate detection limits and lower limit see Appendix A.

2 Normative references

This standard references the following documents or the terms. For undated references, the effective version applies to this book standard. HJ 765 solid waste organic matter extraction microwave extraction method HJ 782 Solid waste - Extraction of organic matter - Pressurized fluid extraction HJ/T 20 Industrial solid waste sampling Sampling specifications HJ/T 298 Hazardous Waste Identification Technical Specifications Industrial solid waste - Extraction toxicity Toxicity - Sulfuric acid nitrate method Industrial solid waste - Extraction toxicity Toxicity - Acetic acid buffer solution method

3 method principle

Organochlorine pesticides in solid wastes and leachate were extracted, purified, concentrated, and fixed, then separated by gas chromatography Spectrum detection. According to mass spectrometry, retention time, fragment ion mass ratio and its abundance qualitative, internal standard method.

4 Reagents and materials

Unless otherwise stated, analytical grade reagents that meet national standards are used. Experimental water for the newly prepared pure water or Distilled water. 4.1 acetone (C3H6O). pesticide grade. 4.2 n-hexane (C6H14). pesticide grade. 4.3 Dichloromethane (CH2Cl2). pesticide residues. Ethyl acetate (C4H8O2). pesticide residues. 4.5 cyclohexane (C6H12). pesticide grade. 4.6 ether (C4H10O). pesticide residues. 4.7 n-hexane - acetone mixed solvent I. 1 1. Mix with n-hexane (4.2) and acetone (4.1) at 1.1 volume ratio. 4.8 n-hexane - acetone mixed solvent II. 9 1. Mix with 9.1 volumes by volume with n-hexane (4.2) and acetone (4.1). 4.9 Dichloromethane - acetone mixed solvent. 1 1. Mix with methylene chloride (4.3) and acetone (4.1) at 1.1 volume ratio. 4.10 n-hexane - ether mixed solvent I. 94 6. Mix with n-hexane (4.2) and diethyl ether (4.6) at a 94.6 volume ratio. 4.11 n-hexane - ether mixed solvent II. 85 15. Mix with 85.15 by volume with n-hexane (4.2) and ether (4.6). 4.12 n-hexane - ether mixed solvent III. 1 1. Mix with n-hexane (4.2) and diethyl ether (4.6) at a 1.1 volume ratio. 4.13 n-hexane - dichloromethane mixed solvent I. 1 1. Mix with n-hexane (4.2) and methylene chloride (4.3) at 1.1 volume ratio. 4.14 n-hexane - dichloromethane mixed solvent II. 74 26. Mix with n-hexane (4.2) and methylene chloride (4.3) in a volume ratio of 74.26. 4.15 gel permeation chromatography mobile phase. Mix with ethyl acetate (4.4) and cyclohexane (4.5) at a volume ratio of 1.1, or prepare other solvents according to the instruction manual system. 4.16 nitric acid. ρ (HNO3) = 1.42 g/ml, excellent grade pure. 4.17 nitric acid solution. 1 1. Mix with nitric acid (4.16) and water at a volume ratio of 1.1. 4.18 Organochlorine pesticide standard stock solution. ρ = 1000 ~ 5000 mg/L. Can be purchased directly from the market certified standard solution. 4.19 Organochlorine pesticides standard solution. ρ =.200 ~ 500 mg/L. Dilute and prepare the standard organochlorine pesticide stock solution (4.18) with n-hexane-acetone mixed solvent I (4.7). 4.20 Internal standard stock solution. ρ = 5 000 mg/L. Pentachloronitrobenzene is used as internal standard. Can be purchased directly from the market certified standard solution. You can also use the Philippines-d10 and 䓛-d12 do Internal standard. 4.21 Internal standard solution. ρ = 500 mg/L. Measure 1.0 ml internal standard stock solution (4.20) in a 10 ml volumetric flask with n-hexane - acetone mixed solvent I (4.7) Release to the mark, mix well. 4.22 Replacement standard stock solution. ρ = 1000 to 5000 mg/L. Use decalin or 2,4,5,6-tetrachloro-m-xylene and dibutyl chloroformate as alternatives. Can be purchased directly from the market Standard solution. 4.23 Alternatives Standard solution. ρ =.200 ~ 400 mg/L. Dilute the standard stock solution (4.22) with n-hexane-acetone mixed solvent I (4.7) and mix well. 4.24 Tenodiphenylphosphine (DFTPP) standard solution. ρ = 50 mg/L. Can be purchased directly from the market certified standard solution. Other concentrations were diluted with dichloromethane (4.3) to a concentration of 50 mg/L. 4.25 gel permeation chromatography calibration standard solution. Corn oil (25 mg/ml), Di (2-diethylhexyl) phthalate (1 mg/ml), Methoxy DDT mg/L), perylene (20 mg/L) and sulfur (80 mg/L). Can be purchased directly from the market certified standard solution. 4.26 desiccant. superior grade pure anhydrous sodium sulfate (Na2SO4) or granular diatomite 150 ~ 250 μm (100 ~ 60 mesh). Bake in a muffle furnace at 400 ° C for 4 h, cool and put it into a stoppered glass jar and seal in a desiccator. 4.27 Sodium Chloride (NaCl). Placed in a muffle furnace at 400 ℃ for 4 h, cooled and filled into a sealed glass jar sealed, placed in a desiccator to save. 4.28 copper powder. purity ≥ 99.5%. Before use with nitric acid solution (4.17) to remove the copper oxide surface, rinse with acid, then acetone (4.1) Wash, and then use high purity nitrogen (4.35) to dry stand-by, before each use of pre-treatment, to keep the copper surface light. 4.29 Magnesium silicate. 75-150 μm (200-100 mesh). Placed in a watch glass, lightly covered with aluminum foil, baked in an oven at 130 ° C. for 12 h, taken out into a desiccator, cooled, stand-by. Pro use before treatment. 4.30 Column. 20 mm in inside diameter and 10 to 20 cm in length with Teflon piston made of glass or other equivalent Can material. 4.31 Magnesium silicate solid phase extraction column. 1 000 mg/6 ml, or other equivalent specifications. 4.32 quartz sand. 150 ~ 830 μm (100 ~ 20 mesh) Placed in a muffle furnace 400 ℃ baking 4 h, cooled and filled into the stopper sealed glass jar sealed. 4.33 glass wool or glass fiber filter. Before use with dichloromethane - acetone mixed solvent (4.9) dipping, until the solvent is evaporated, stored in a stopper glass mouth Sealed and saved 4.34 Fiberglass or natural fiber sleeve. Before use, the glass fiber sleeve is placed in a muffle furnace for baking at 400 ° C. for 4 h, and the natural fiber sleeve and the sample are taken The same solvent treatment. 4.35 high purity nitrogen. purity ≥ 99.999%. 4.36 high purity helium. purity ≥ 99.999%.

5 instruments and equipment

5.1 Gas Chromatography - Mass Spectrometer. Electron bombardment source (EI source). 5.2 Column. quartz capillary column, 30 m × 0.25 mm × 0.25 m, the stationary phase of 5% phenyl -95% methyl silicone Alkane, or other equivalent capillary column. 5.3 Extraction device. Soxhlet extractor or pressurized fluid extractor and other equipment of considerable performance. 5.4 Gel Permeation Chromatograph. a 254 nm fixed wavelength UV detector packed with gel packing column. 5.5 Concentration device. Nitrogen concentration concentrator, rotary evaporator or other concentration device. 5.6 vacuum freeze dryer. no-load vacuum of 13 Pa or less. 5.7 flip oscillator. 5.8 solid phase extraction device. 5.9 General laboratory equipment and equipment.

6 samples

6.1 Sample Collection and Storage Solid waste samples were collected and stored in accordance with HJ/T 20 and HJ/T 298 regulations. Samples should be clean Stuffed and sealed in brown glass bottle. During transportation should be sealed, dark, cold storage below 4 ℃. After shipped to the laboratory, if Can not be timely analysis, should be refrigerated at below 4 ℃, dark, sealed, storage time does not exceed 10 d. 6.2 Sample Preparation 6.2.1 Preparation of solid waste leachate Solid waste leachate preparation according to HJ/T 299 or HJ/T 300 of the relevant regulations. 6.2.2 Preparation of solid waste samples Solid waste samples were prepared according to HJ 782 or HJ 765 regulations. 6.3 Sample Preparation 6.3.1 Preparation of solid waste leachate samples 6.3.1.1 Extraction Take 100 ml solid waste leachate (6.2.1) into the appropriate volume separatory funnel, add 10 ~ 20 μl of the alternative The standard use of liquid (4.23) and the amount of sodium chloride (4.27), then add 20 ml of methylene chloride (4.3), full oscillation, static After the layers were separated, the organic phase was dehydrated by a funnel equipped with an appropriate amount of anhydrous sodium sulfate (4.26). The organic phase was collected in a concentration flask, Then repeat the extraction once, the combined organic phase, with a small amount of methylene chloride (4.3) repeatedly washed funnel and sodium sulfate layer 2 to 3 times, The organic phases are combined and concentrated. Note 1. If the leachate concentration may be appropriate to reduce the sample size. Note 2. If the extraction process occurs emulsification, demulsification can be frozen and stirring methods. 6.3.1.2 Concentration Use nitrogen blowing concentrator should be at room temperature, open the nitrogen gas flow to the solvent surface fluctuations (to avoid the formation of gas vortex), The wall of the concentrator, exposed during the nitrogen blowing, was washed several times with dichloromethane (4.3) and the extract was concentrated to about 5 ml. Need to purify, all transferred, add appropriate amount of internal standard solution (4.21), constant volume to 10.0 ml, mix, test. For the net Continue to concentrate to 2 ml, add about 5 ml n-hexane (4.2) and concentrate to about 1 ml, repeat this concentration process twice, Concentrate to 1 ml, to be purified. Other equivalent effects of concentration can also be used. 6.3.1.3 Purification The magnesium silicate solid-phase extraction column (4.31) was fixed on a solid-phase extraction device (5.8) and eluted with 4 ml of n-hexane (4.2) Wash, add 5 ml of n-hexane (4.2), close the control valve, soak for 5 min and then slowly open the control valve. Continue to join 5 ml n-Hexane (4.2). Close the control valve and discard the effluent before the column packing is exposed to the air. The extract will be concentrated Liquid (6.3.1.2) was transferred to a magnesium silicate solid phase extraction column, with 2 ml of n-hexane (4.2) fractional washing concentrated flask, lotion Department transferred to magnesium silicate solid phase extraction column. Slowly open the control valve and close the control valve before the column packing is exposed to the air. slow Open the control valve and elute with 9 ml n-hexane-acetone mixed solvent II (4.8) at a rate of 1 ml/min. Collect the complete elution Liquid, add appropriate amount of internal standard solution (4.21), constant volume to 10.0 ml, mix well, test. Other equivalent decontamination 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) samples, add 90 ml of water, mix thoroughly transferred to a separatory funnel, the rest Follow steps 6.3.1.1 to 6.3.1.3. 6.3.2.2 Oily liquid solid waste Weigh out or 10.0 g (accurate to 0.01 g) sample, add appropriate amount of dichloromethane (4.3) until the sample is completely dissolved, After mixing all transferred to a separatory funnel, add 100 ml of water, the remaining steps in accordance with 6.3.1.1 to 6.3.1.3 steps. 6.3.2.3 Solid and semi-solid solid waste 6.3.2.3.1 Extraction Extraction method may choose Soxhlet extraction, pressurized fluid extraction, microwave extraction or other equivalent extraction method, the extraction solvent is N-hexane-acetone mixed solvent I (4.7) or methylene chloride-acetone mixed solvent (4.9). a) Soxhlet extraction. The dehydrated solid waste samples (6.2.2) are all transferred to a glass fiber or natural fiber sleeve (4.34), add the standard alternative solution (4.23) at a concentration near the midpoint of the curve and carefully place the sleeve on the Soxhlet In the receiver reflux tube, 100 ml n-hexane-acetone mixed solvent I (4.7) was added to the round bottom solvent bottle and extracted for 16-18 h. Reflux speed control in 4 to 6 times/h. Extraction is completed, remove the bottle, to be concentrated. b) Pressurized fluid extraction. Extract according to HJ 782 procedure. c) Microwave Extraction. Extract according to HJ 765 procedure. Note 1. Solid waste samples with high organic content may be appropriate to reduce the sampling volume. Note 2. If there is significant water extract, need further filtration and dehydration. Place a layer of glass wool or glass fiber filter on the glass funnel Membrane (4.33), add about 5 g of anhydrous sodium sulfate (4.26) and filter the extract into a concentrating vessel. Re-use a small amount of n-hexane - acetone Mixed solvent I (4.7) 3 times the extraction container was washed, the washing liquid was collected in a funnel and filtered, and finally a small amount of n-hexane - acetone mixed solution Agent I (4.7) rinse the funnel, all collected to concentrate containers, to be concentrated. 6.3.2.3.2 Concentration The following two methods of concentration are recommended. Other methods have been verified to meet the requirements can also be used. a) Nitrogen blowing In accordance with the 6.3.1.2 nitrogen blowing concentrated operation steps. b) Rotary evaporation Heating temperature according to the boiling point of the solvent is set at 30 ~ 60 ℃, the extract (6.3.2.3.1) is concentrated to about 10 ml, stop concentrate. Transfer the concentrate to a graduated vessel using a disposable pipette and use a small amount of n-hexane-acetone mixed solvent I (4.7) The bottom of the rotary evaporator rinsed 2 times, the combined liquid concentrate, and then concentrated to 10 ml nitrogen blowing, transfer Completely, add the appropriate amount of internal standard solution (4.21), set at 10.0 ml, mix well and test. For purification, continue to concentrate To 1 ~ 2 ml, to be purified. Note. When gel permeation chromatography is used for subsequent purification steps, the extract is concentrated to less than 5 ml with nitrogen and about 10 ml of gel permeation is added The chromatographic mobile phase (4.15), concentrated to 1 ~ 2 ml, to be purified. 6.3.2.3.3 Purification The concentrated extract (6.3.2.3.2) can be purified using a magnesium silicate column, gel permeation chromatography or a magnesium silicate cartridge. its His method is validated to meet the requirements can also be used. a) Magnesium silicate column purification 1) Magnesium silicate chromatography Glass wool (4.33) was packed in the bottom of the column (4.30), and anhydrous sodium sulfate (4.26) And 20 g of magnesium silicate (4.29), tap the column wall to make the magnesium silicate (4.29) evenly packed. Add about 1.5 cm thick again Anhydrous sodium sulfate (4.26). For desulfurization, add approximately 2 g of copper powder (4.28) to the top of the column. Add 60 ml of n-hexane (4.2) Rinsed, tapped the column wall at the same time, driven out air bubbles, filled the magnesium silicate, kept the packing full of n-hexane (4.2), closed Plug, soak the packing for at least 10 min. While opening the piston, continue adding 60 ml n-hexane (4.2) rinse at the top Before the anhydrous sodium sulfate layer is exposed to the air, close the piston and stand still. 2) purification The concentrated extract (6.3.2.3.2) was transferred to a magnesium silicate column and washed twice with 2 ml of n-hexane (4.2) The vessel was concentrated and all transferred to a prepared magnesium silicate column and the solution immersed in copper powder for about 5 min. A round bottom flask w......
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