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HJ 891-2017 English PDF

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HJ 891-2017: Solid waste. Determination of polychlorinated biphenyls. Gas chromatography/mass spectrometry method
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HJ 891-2017529 Add to Cart 4 days Solid waste. Determination of polychlorinated biphenyls. Gas chromatography/mass spectrometry method Valid

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Basic data

Standard ID: HJ 891-2017 (HJ891-2017)
Description (Translated English): Solid waste. Determination of polychlorinated biphenyls. Gas chromatography/mass spectrometry method
Sector / Industry: Environmental Protection Industry Standard
Classification of Chinese Standard: Z13
Classification of International Standard: 13.030.10
Word Count Estimation: 23,285
Date of Issue: 2017-12-17
Date of Implementation: 2018-02-01
Quoted Standard: HJ 77.3; HJ 782; HJ/T 20; HJ/T 298; HJ/T 299; HJ/T 300
Regulation (derived from): Ministry of Environmental Protection Bulletin 2017 No. 73
Issuing agency(ies): Ministry of Ecology and Environment
Summary: This standard specifies gas chromatography-mass spectrometry for the determination of polychlorinated biphenyls in solid wastes and their leachate. This standard applies to the determination of 18 polychlorinated biphenyls in solid wastes and leachates. If verified, this standard also applies to the determination of other PCB congeners. When the solid waste sample volume is 20 g and the volume constant volume is 1.0 ml, the detection limit of 18 polychlorinated biphenyls is 2 to 3 ��g/kg, the lower limit of determination is 8 to 12 ��g/kg, and the solid waste leachate volume is 300 ml. When the constant volume was 1.0 ml, the method detection limit was 0.08-0.2 ��g/L and the lower limit of determination was 0.32-0.8 ��g/L. See Appendix A for details.

HJ 891-2017: Solid waste. Determination of polychlorinated biphenyls. Gas chromatography/mass spectrometry method


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(Solid waste - Determination of PCBs - Gas chromatography - mass spectrometry) People's Republic of China national environmental protection standards Solid waste - Determination of PCBs Gas chromatography - mass spectrometry Solid waste-Determination of polychlorinated biphenyls -Gas chromatography mass spectrometry 2017-12-17 Published 2018-02-01 implementation Ministry of Environmental Protection released i 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 .4 6 samples .4 7 Analysis steps .7 8 Results Calculation and Presentation 10 9 Precision and accuracy 11 10 Quality Assurance and Quality Control ..12 11 Waste treatment .12 Appendix A (Normative) Method detection limit and lower limit of determination Appendix B (informative) Gel permeation chromatography calibration standard solution peak .14 Appendix C (Informative) Quantitative ions, auxiliary ions and their ion abundance ratio .15 Appendix D (informative) method of precision 16 Appendix E (Informative) Method Accuracy 19

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 solid waste and leaching solution of PCBs, the development of this standard. This standard specifies the determination of solid waste and leachate 18 kinds of PCBs by gas chromatography - mass spectrometry. This standard Appendix A normative appendix, Appendix B ~ Appendix E is informative appendix. 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. Zhejiang Provincial Environmental Monitoring Center. This standard verification unit. Jiangsu Provincial Environmental Monitoring Center, Hubei Provincial Environmental Monitoring Center, Hangzhou Environmental Monitoring Center, Ningbo Environmental Monitoring Center, Shaoxing Environmental Monitoring Center Station and Jiaxing Environmental Monitoring Station. This standard MEP approved on December 17,.2017. This standard since February 1,.2018 implementation. This standard is interpreted by the MEP. Solid waste - Determination of PCBs - Gas chromatography - mass spectrometry Warning. The standard substances and solvents used in the experiment are all toxic substances. The preparation process should be carried out in a fume hood. And pay attention to wear protective equipment, avoid contact with skin and clothing.

1 scope of application

This standard specifies the determination of solid waste and its leachate PCBs by gas chromatography - mass spectrometry. This standard applies to the determination of 18 kinds of PCBs in solid waste and leachate. If verified, this standard is also suitable For other polychlorinated biphenyls congeners determination. When the solid waste sample volume is 20 g and the constant volume is 1.0 ml, the detection limits of the 18 PCBs are 2 to 3 g/kg, the lower limit of determination is 8 ~ 12 g/kg; solid waste leachate volume of 300 ml, volume of 1.0 ml, the side The detection limit was 0.08 ~ 0.2 g/L, and the lower limit of determination was 0.32 ~ 0.8 g/L. See Appendix A for details.

2 Normative references

This standard references the following documents or the terms. For undated references, the effective version applies to this book standard. HJ 77.3 Solid waste Dioxins Determination Isotope dilution High-resolution gas chromatography-high resolution mass spectrometry 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 Solid waste extraction toxicity Toxicity method HNO3 method HJ/T 300 solid waste leaching toxic leaching method acetic acid buffer solution method

3 method principle

PCBs in solid wastes are extracted by Soxhlet or pressurized fluid extraction. PCBs in leachate Using liquid-liquid extraction, the extraction liquid selected appropriate methods of purification, concentration and separation by gas chromatography - mass spectrometry, detection, according to Retention time and characteristic ion abundance ratio qualitative, internal standard method.

4 Reagents and materials

Unless otherwise specified, the analysis of the use of analytical reagents in line with national standards, the experimental water for the newly prepared non-containing head Standard water, subject to a blank test before use. 4.1 acetone (C3H6O). pesticide grade. 4.2 Toluene (C7H8). pesticide residues. 4.3 n-hexane (C6H14). pesticide grade. 4.4 methanol (CH3OH). pesticide grade. 24.5 Dichloromethane (CH 2 Cl 2). Pesticide grade. 4.6 Dimethyl sulfoxide (C2H6OS). Saturated with n-hexane (4.3) before use. 4.7 Hydrochloric acid.  (HCl) = 1.18 g/ml, excellent grade pure. 4.8 Sulfuric acid.  (H2SO4) = 1.84 g/ml, excellent grade pure. 4.9 Sodium hydroxide (NaOH). excellent grade pure. 4.10 Potassium hydroxide (KOH). excellent pure grade. 4.11 Sodium chloride (NaCl). Heat at 450 ° C for 4 h, cool to room temperature in a desiccator and store in a clean reagent bottle. 4.12 anhydrous sodium sulfate (Na2SO4). excellent grade pure. 660 ℃ calcined 6 h, cooled to 150 ℃ after the transfer to the dryer, after cooling into the reagent bottle, stored in a desiccator. 4.13 Dichloromethane - n-hexane mixed solvent. 3 7. Dichloromethane (4.5) and n-hexane (4.3) were mixed at a volume ratio of 3.7. 4.14 n-hexane - acetone mixed solvent. 1 1. Hexane (4.3) and acetone (4.1) were mixed in a volume ratio of 1.1. 4.15 hydrochloric acid solution. 1 1. Hydrochloric acid (4.7) and water were mixed in a volume ratio of 1.1. 4.16 Sodium hydroxide solution.  (NaOH) = 40 mg/L. Weigh 4 g of sodium hydroxide (4.9) and dilute to 100 ml with water. 4.17 Potassium hydroxide solution.  (KOH) = 112 mg/L. Weigh 11.2 g of potassium hydroxide (4.10) and dilute to 100 ml with water. 4.18 Sodium chloride solution.  (NaCl) = 50 mg/L. Weigh 5 g of sodium chloride (4.11) and dilute to 100 ml with water. 4.19 PCB stock standard solution.  = 100 mg/L. Buy a certified standard solution (polychlorinated biphenyls standard solution or single component polychlorinated biphenyl standard solution), - below 20 ℃ Protect from light, or refer to the standard solution certificate for instructions. 4.20 Polychlorinated biphenyls standard solution.  = 10.0 mg/L (reference concentration). Dilute PCB stock standard solution (4.19) with n-hexane (4.3) or methanol (4.4). The solution is below -20 ℃ avoidance Light preservation, can be stored for two months. 4.21 Internal standard stock solution.  = 100 mg/L. Buy a certified standard solution. Choosing tetrachloro-m-xylene (TCMX) as an internal standard can also use deca-biphenyl and deuterium Substitute polychlorinated biphenyls or isotope standards as internal standard, below -20 ℃ dark preservation, or reference to the standard solution certificate that Save it. 4.22 Internal standard solution.  = 10.0 mg/L (reference concentration). The internal standard stock solution (4.21) is diluted with n-hexane (4.3) or methanol (4.4). The solution at -20 ℃ below light preservation, Can be kept for two months. 4.23 Replacement standard stock solution.  = 500 mg/L. Buy a certified standard solution. 2,2 ', 4,4', 5,5'-hexabromobiphenyl (PBB-153) was chosen as the standard stock solution of substitutes, 3 It is also possible to use deca-biphenyl, deuterium-substituted PCBs or isotope standards as a substitute for the standard, keep it in the dark at -20 ° C, Or refer to the standard solution certificate instructions for preservation. 4.24 Alternatives Standard solution.  = 40.0 mg/L (reference concentration). Dilute the replacement standard stock (4.23) with n-hexane (4.3) or methanol (4.4). The solution below -20 ℃ dark Save, can be saved for two months. 4.25 decafluorotriphenylphosphine (DFTPP) stock solution.  = 1000 mg/L, the solvent is methanol. Buy a certified standard solution, stored below 4 ℃ dark, or refer to the standard solution certificate to save the relevant instructions. 4.26 Dodecafluorotriphenylphosphine (DFTPP) Solution.  = 50.0 mg/L. Dilutetriphenylphosphine (DFTPP) stock solution (4.25) was diluted with methanol (4.4). Use liquid below -20 ℃ to avoid light Save. 4.27 gel permeation chromatography calibration standard stock solution. corn oil ( = 300 mg/ml), diethylhexyl phthalate ( Pentahydrate ( = 1.4 mg/ml), pyrene ( = 0.1 mg/ml), elemental sulfur ( = 0.5 mg/ml) Methylene chloride. Buy a certified standard solution, 4 ℃ below the dark preservation, or refer to the standard solution certificate instructions for preservation. 4.28 gel permeation chromatography calibration standard solution. corn oil ( = 30.0 mg/ml), diethylhexyl phthalate ( = 1.5 mg/ml), pentachlorophenol ( = 0.14 mg/ml), pyrene ( = 0.01 mg/ml) and elemental sulfur ( = 0.05 mg/ml). Dilute gel permeation chromatography calibration stock (4.27) with dichloromethane (4.5). 4 ℃ below dark preservation, can be guaranteed Save six months. 4.29 Copper beads (powder). 1.5 mm in diameter (250 μm, 60 mesh). Before using hydrochloric acid solution (4.15), toluene (4.2) were rinsed, placed in a desiccator to save. 4.30 Silicone. 75 ~ 150 μm (200 ~ 100 mesh). Wash with dichloromethane (4.5) until all the methylene chloride volatilized, spread in the evaporating dish or beaker, the thickness is less than 10 mm, activated at 130 ℃ for 18 h and placed in a desiccator for 30 min. Into a closed container into the dryer In save. 4.31 sodium hydroxide alkaline silica gel. Take activated silica gel (4.30) 67 g, sodium hydroxide solution (4.16) 33 g, stir, make it a fluid powder Last shape. After the preparation is completed, the glass bottle is sealed and stored in a desiccator. 4.32 Silica gel. Take activated silica (4.30) 100 g, add 78.6 g sulfuric acid (4.8), stir, make it into a fluid powder. After the preparation is completed, it is sealed in a reagent bottle and stored in a desiccator. 4.33 10% Silver Nitrate Silicone. Commercial, protected from light. 4.34 Magnesium silicate. 150 ~ 250 μm (100 ~ 60 mesh). Activate at 130 ° C for 18 h before use. Placed in a desiccator cooled to room temperature, sealed and stored in a clean reagent bottle in. Preparation before use. 4.35 Diatomaceous earth. 38 ~ 150 μm (400 ~ 100 mesh). Baking at 450 ℃ for 4 h, placed in a desiccator cooled to room temperature, transferred to a ground glass jar, stored in a desiccator. 4.36 quartz sand. 297 ~ 840 μm (50 ~ 20 mesh). Baking at 450 ℃ for 4 h, placed in a desiccator cooled to room temperature, transferred to a ground glass jar, stored in a desiccator. 44.37 glass wool. Before use, with dichloromethane (4.5) reflux extraction 24 h, dried and stored in airtight glass containers. 4.38 high purity nitrogen. purity ≥ 99.999%. 4.39 high purity helium. purity ≥ 99.999%.

5 instruments and equipment

5.1 Gas Chromatography-Mass Spectrometer (GC-MS). Equipped with capillary split/splitless inlet, with constant flow or constant pressure Can; oven temperature programmable; with electron bombardment source (EI source). 5.2 Column. Low loss quartz capillary column. Column I. 30 m (length) 0.25 mm (ID) × 0.25 μm (film Thick), the stationary phase is 5% phenyl 95% methylpolysiloxane. Column II. 60 m (length) 0.25 mm (ID), fixed Phase modified 5% phenyl 95% methylpolysiloxane. Other equivalent low-loss columns are also available. NOTE. In order to ensure that the chlorine-substituted PCBs of interest are well separated, capillaries of different properties may be selected in case of interference Column check. 5.3 freeze-drying equipment. 5.4 Extraction device 5.4.1 Soxhlet extractor or equipment with considerable functionality. 5.4.2 Pressurized fluid extractor. with about 40 ml extraction cell, the extraction pressure of more than 1 500 psi, the extraction temperature needs Greater than 120 ° C. 5.5 Purification device 5.5.1 Column. Glass column with inner diameter of 8 ~ 15 mm and length of.200 ~ 300 mm. 5.5.2 Automatic Gel Permeation Chromatography. with UV detector (254 nm wavelength) and length 600 mm, diameter 25 mm Gel column packed with about 70 g of porous polystyrene divinylbenzene bioactive microspheres filler, 5 ~ 10 ml sample quantitative ring. 5.6 Concentration device. rotary evaporation concentrator, nitrogen blowing instrument or other functionally equivalent enrichment device. 5.7 Metal sieve. 840 μm (20 mesh). 5.8 General laboratory equipment and equipment.

6 samples

6.1 Sample Collection and Storage Solid waste samples were collected and prepared according to HJ/T 20 and HJ/T 298 requirements. After sample collection 4 ℃ under dark storage, 14 days to complete the extraction, within 40 d to complete the analysis of the extract. 6.2 Sample Preparation 6.2.1 Solid waste Weigh 20.0 g sample, add an appropriate amount of anhydrous sodium sulfate (4.12), the sample was dried and mixed sand-like flow, spare. If using pressurized fluid extraction, dehydrate with diatomaceous earth (4.35). Or directly selected after grinding sieved sample extraction. 5 Note 1. For large particles or hard solid waste samples that can not be agitated and can only be treated by crushing or other suitable air-dried or Lyophilized samples may be dewatered using freeze-drying equipment (5.3) or other means and ground through a metal sieve (5.7), but should be considered To low chlorinated PCBs loss. Note 2. Sampling capacity can be adjusted according to sample type, degree of interference, pollutant content and extraction method. For organic pollutants with high content Of the sample, may be appropriate to reduce the sample size, or take part of the extract for purification analysis. 6.2.2 solid waste leachate Prepare solid waste leachate according to HJ/T 299 or HJ/T 300. 6.3 Sample Preparation 6.3.1 Extraction 6.3.1.1 Solid waste 6.3.1.1.1 Water-soluble and oily liquid solid waste Weigh 20.0 g sample, add 80 ml of water and 50  l replacement of the standard solution (4.24), after mixing all transferred to the points Liquid funnel, extracted with 100 ml of dichloromethane (4.5) three times, and the extract was dehydrated with anhydrous sodium sulfate (4.12) Collected in a concentrate bottle. Note. If the extract contains a lot of oil, you can refer to HJ 77.3 using dimethyl sulfoxide extraction method to remove hydrocarbons such as low polarity After organic matter, and then 6.3.3 purification. Specific measures are as follows. The extract solvent was converted to n-hexane, concentrated to 3 ml left Right, added to 25 ml of dimethylsulfoxide saturated with n-hexane (4.6), and the concentrate was washed three times with n-hexane (4.3) Transferred to a solution of dimethyl sulfoxide, with a separatory funnel shaking extraction four times to collect about 100 ml of dimethylsulfoxide solution; collected 100 ml dimethyl sulfoxide solution was added 40 ml of n-hexane (4.3) shaken extraction, n-hexane was discarded; further dimethyl sulfoxide solution 75 ml of n-hexane (4.3) and 100 ml of water were added and the mixture was extracted by shaking. After standing, the n-hexane layer was collected and the operation was repeated three times. And n-hexane was collected; to a hexane solution was added potassium hydroxide solution (4.17) 10 ml, shaking wash, discard the water layer and then After adding 25 ml of water to wash and standing, the n-hexane extracts were dehydrated in anhydrous sodium sulfate (4.12) and collected in a concentrating flask. 6.3.1.1.2 Solid and semi-solid waste a) Soxhlet extraction Dehydrated sample (6.2.1) all transferred to the Soxhlet extractor (5.4.1) extraction cup, in each sample plus Into 50  l replacement standard solution (4.24). With.200 ~ 300 ml n-hexane - acetone mixed solvent (4.14) or toluene (4.2) solvent extraction more than 8 h, reflux rate control in 4 to 6 times/h, collecting the extract. b) Pressurized fluid extraction With reference to HJ 782 will dehydrated samples (6.2.1) all transferred to a suitable extraction tank, while adding 50 替 l instead Standard standard solution (4.24). Set the extraction conditions, the pressure of 1 500 psi, a temperature of 120 ℃, the extraction solvent for n-hexane - acetone mixed solvent (4.14) or toluene (4.2) solution, 100% full extraction cell mode, high temperature and pressure stand 5 min, Loop three times and collect the extract. Note. In the premise of meeting the quality control requirements of this method, other extraction solvents may be used after verification. 6.3.1.2 solid waste leachate 6 take solid waste leachate (6.2.2) 300 ml in a separatory funnel, add 40  l replacement standard solution (4.24), Extract according to 6.3.1.1.1 Procedure and collect the extract. 6.3.2 extract (extract) concentration The sample extract or extract (6.3.1) was transferred to the concentration device, concentrated to 1 ~ 2 ml, to be purified. Such as extraction The solution is dichloromethane, concentrated to about 10 ml added 3 ml n-hexane (4.3) conversion solvent, continue to concentrate to 1 ~ 2 ml, To be purified analysis. 6.3.3 Purification and separation 6.3.3.1 sulfur purification Such as samples containing large amounts of sulfur, you need to first desulfurization purification. In the concentrated extract (6.3.2) add about 50 ml of n-hexane (4.3), then add 15 g of copper beads after treatment (Powder) (4.29), the full oscillation, filtration, the filtrate was concentrated to 1 ~ 2 ml, according to 6.3.3.3 method of purification. 6.3.3.2 sulfuric acid purification If the extract color darker, you can use sulfuric acid purification method for the initial purification treatment. The concentrated extract or extract (6.3.2) was transferred to a 125 ml separatory funnel, 75 ml of n-hexane (4.3). Shake with 5-10 ml of sulfuric acid (4.8) for about 1 min. Discard the aqueous phase after standing and repeat until the sulfuric acid layer is clear color. To the separatory funnel was added 30 ml of sodium chloride solution (4.18) to wash the organic phase, put it aside after stratification, the organic phase Phase anhydrous sodium sulfate (4.12) after drying dehydration, concentrated to 1 ~ 2 ml, and then 6.3.3.3 or 6.3.3.4 purification method. 6.3.3.3 Multi-layer silica gel column purification Add some glass wool (4.37) to the bottom of the glass column (inner diameter 12 ~ 15 mm) and add 3 g Silica gel (4.30), 5 g basic sodium hydroxide (4.31), 2 g silica gel (4.30), 10 g silica gel (4.32), 2 g Silica gel (4.30), 5 g of 10% silver nitrate silica gel (4.33, optional with minor sulfur interference) and 5 g of anhydrous sodium sulfate (4.12). After filling, the multi-layer silica gel column was rinsed with 100 ml of n-hexane (4.3), keeping the liquid level in the anhydrous sodium sulfate layer. Transfer concentrated extract or extract (6.3.2), or 6.3.3.1,6.3.3.2 purified concentrate to the purification column Wash the wall of the extract with 1 to 2 ml of n-hexane (4.3) and repeat ......
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