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HJ 650-2013 English PDF

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HJ 650-2013: Soil and sediment Determination of polychlorinated dibenzo-p-dioxins (PCDDs) and polychlorinated dibenzofurans (PCDFs) Isotope dilution HRGC-LRMS
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Standard IDUSDBUY PDFLead-DaysStandard Title (Description)Status
HJ 650-2013599 Add to Cart 4 days Soil and sediment Determination of polychlorinated dibenzo-p-dioxins (PCDDs) and polychlorinated dibenzofurans (PCDFs) Isotope dilution HRGC-LRMS Valid

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Basic data

Standard ID: HJ 650-2013 (HJ650-2013)
Description (Translated English): Soil and sediment Determination of polychlorinated dibenzo-p-dioxins (PCDDs) and polychlorinated dibenzofurans (PCDFs) Isotope dilution HRGC-LRMS
Sector / Industry: Environmental Protection Industry Standard
Word Count Estimation: 23,218
Quoted Standard: GB/T 8170; GB 17378.3; HJ 77.4; HJ/T 166; HJ 613
Regulation (derived from): Department of Environmental Protection Notice No. 33 of 2013
Issuing agency(ies): Ministry of Ecology and Environment
Summary: This standard specifies: Determination of soil and sediment polychlorinated dibenzo-p-dioxins and polychlorinated dibenzofurans isotope dilution/high resolution gas chromatography low resolution mass spectrometry. This standard applies to: soils and sedim

HJ 650-2013: Soil and sediment Determination of polychlorinated dibenzo-p-dioxins (PCDDs) and polychlorinated dibenzofurans (PCDFs) Isotope dilution HRGC-LRMS


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Soil and sediment Determination of polychlorinated dibenzo-p-dioxins (PCDDs) and polychlorinated dibenzofurans (PCDFs) Isotope dilution HRGC-LRMS National Environmental Protection Standard of the People's Republic Determination of soil and sediment dioxin Isotope dilution/high resolution gas chromatography - low Resolution mass spectrometry Soil and sediment Determination of polychlorinated dibenzo-p-dioxins (PCDDs) and polychlorinated dibenzofurans (PCDFs) Isotope dilution HRGC-LRMS Published on.2013-06-03 2013-09-01 implementation Ministry of Environmental Protection released

Content

Foreword.I 1 Scope..1 2 Normative references..1 3 Terms and definitions, symbols and abbreviations 1 4 principle of the method..3 5 Reagents and materials.4 6 instruments and equipment.5 7 samples.6 8 Analysis steps..8 9 Calculation and representation of results 10 10 Precision and Accuracy 12 11 Quality Assurance and Quality Control.12 12 Test report 13 13 Waste treatment 13 Appendix A (Normative Appendix) Flow chart for dioxin analysis. 155 Appendix B (informative) Examples of dioxin-type calibration substances used..16 Appendix C (informative) Sample preparation and analysis flow chart..17 Appendix D (informative) Method Precision and Accuracy.18 Appendix E (informative) Record of measurement results..19

Foreword

To protect the environment and protect the human body in order to implement the Environmental Protection Law of the People's Republic of China and the Law of the People's Republic of China on Water Pollution Prevention and Control This standard is developed for high-resolution gas chromatography-low resolution mass spectrometry monitoring of dioxin-like contaminants in soils and sediments. This standard specifies high resolution gas chromatography-low resolution mass spectrometry for dioxins in soils and sediments. This standard is the first release. Appendix A of this standard is a normative appendix, and Appendix B to Appendix E are informative appendices. This standard was formulated by the Science and Technology Standards Department of the Ministry of Environmental Protection. This standard is mainly drafted by. Zhejiang Environmental Monitoring Center, Environmental Protection Standards Institute of the Ministry of Environmental Protection. This standard is verified by. National Environmental Analysis and Testing Center, Liaoning Provincial Environmental Monitoring Center, Hubei Environmental Monitoring Center, Ningbo City Ring Environmental monitoring center This standard was approved by the Ministry of Environmental Protection on June 3,.2013. This standard has been implemented since September 1,.2013. This standard is explained by the Ministry of Environmental Protection. Determination of soil, sediment dioxin class isotope dilution / High resolution gas chromatography-low resolution mass spectrometry Warning. The standard and organic reagents used in the experiment are all toxic compounds, and their solution preparation, pretreatment, etc. It should be carried out in a fume hood, and protective equipment should be worn as required to avoid contact with skin and clothing.

1 Scope of application

This standard specifies the determination of polychlorinated dibenzodioxins and polychlorinated dibenzofurans in soils and sediments. Resolution gas chromatography-low resolution mass spectrometry. This standard applies to the preliminary screening of dioxins in soils and sediments, mainly including polychlorinated from tetrachloro to octachlor. Determination of dibenzodioxin and dibenzofuran by high resolution gas chromatography/low resolution mass spectrometry. Accident arbitration, construction Project evaluation and acceptance are recommended using high resolution mass spectrometry methods such as HJ 77.4. The detection limits of this standard method vary with the sensitivity of the instrument, the concentration of dioxin in the sample, and the level of interference. Earth When the soil sample volume is 20g, the detection limit for 2,3,7,8-T4CDD should be less than 1.0 ng/kg, see Table 1.

2 Normative references

The contents of this standard refer to the following documents or their terms. For undated references, the valid version is appropriate. Used in this standard. GB/T 8170 Numerical Rounding Rules and Representation and Determination of Limit Values GB 17378.3 Marine monitoring specification Part 3. Sample collection, storage and transport HJ 77.4 Determination of Dioxins in Soils and Sediments Isotope Dilution High Resolution Gas Chromatography-High Resolution Mass Spectrometry HJ/T 166 Technical Specifications for Soil Environmental Monitoring HJ 613 Determination of dry matter and moisture in soils - Gravimetric method 3 Terms and definitions, symbols and abbreviations The following terms and definitions apply to this standard. 3.1 Terms and definitions 3.1.1 Dichlorinated dibenzodioxins (PCDDs) and Polychlorinated dibenzofurans (PCDFs) A collective term for polychlorinated dibenzo-p-dioxins (PCDDs) and polychlorinated dibenzofurans (PCDFs). 3.1.2 Congener Congener All compounds of dioxins are similar to each other. There are 210 congeners in the dioxin class. 3.1.3 2,3,7,8-chlorinated dioxins PCDDs/PCDFs isomer substituted at 2,3,7,8-positions Refers to dioxin-like congeners with chlorine atoms at the 2, 3, 7, and 8 positions. Among them, there are 7 kinds of polychlorinated dibenzo-p-dioxins. There are 10 kinds of chlorodibenzofurans, and there are 17 kinds, see Table 1. 3.1.4 Dioxin internal standard Internal standard for PCDDs/PCDFs analysis See Table 2 for the dioxin-like standard substances labeled with known concentrations of isotope (13C or 37Cl). Including sample preparation process Added purified internal standard and injection internal standard. 3.1.5 Toxicity equivalency factor, referred to as TEF Refers to the ratio of dioxin-like congeners to 2,3,7,8-tetrachlorodibenzo-p-dioxin to aromatic hydrocarbon (Ah) receptor affinity. 3.1.6 Toxic equivalent quantity, referred to as TEQ The mass fraction of each dioxin-like congener is converted to the equivalent mass of 2,3,7,8-tetrachlorodibenzo-p-dioxin Fraction, toxic equivalent mass fraction is the product of the measured mass fraction and the toxic equivalent factor of the isomer. Table 1 Detection limits of 2,3,7,8-chlorodioxins and methods Serial number isomer name short name detection limit (ng/kg) 1 2,3,7,8-tetrachlorodibenzo-p-dioxin 2,3,7,8-T4CDD 0.3 2 1,2,3,7,8-pentachlorodibenzo-p-dioxin class 1,2,3,7,8-P5CDD 0.5 3 1,2,3,4,7,8-hexachlorodibenzo-p-dioxin class 1,2,3,4,7,8-H6CDD 0.6 4 1,2,3,6,7,8-hexachlorodibenzo-p-dioxin class 1,2,3,6,7,8-H6CDD 0.6 5 1,2,3,7,8,9-hexachlorodibenzo-p-dioxin class 1,2,3,7,8,9-H6CDD 0.6 6 1,2,3,4,6,7,8-heptachlorodibenzo-p-dioxin class 1,2,3,4,6,7,8-H7CDD 1.2 7 octachlorodibenzo-p-dioxin OCDD 1.7 8 2,3,7,8-tetrachlorodibenzofuran 2,3,7,8-T4CDF 0.2 9 1,2,3,7,8-pentachlorodibenzofuran 1,2,3,7,8-P5CDF 0.3 10 2,3,4,7,8-pentachlorodibenzofuran 2,3,4,7,8-P5CDF 0.3 11 1,2,3,4,7,8-hexachlorodibenzofuran 1,2,3,4,7,8-H6CDF 0.4 12 1,2,3,6,7,8-hexachlorodibenzofuran 1,2,3,6,7,8-H6CDF 0.4 13 1,2,3,7,8,9-hexachlorodibenzofuran 1,2,3,7,8,9-H6CDF 0.4 14 2,3,4,6,7,8-hexachlorodibenzofuran 2,3,4,6,7,8-H6CDF 0.4 15 1,2,3,4,6,7,8-heptachlorodibenzofuran 1,2,3,4,6,7,8-H7CDF 1.4 16 1,2,3,4,7,8,9-heptachlorodibenzofuran 1,2,3,4,7,8,9-H7CDF 1.4 17 octachlorodibenzofuran OCDF 1.4 Table 2 Available Dioxin Internal Standards Replace the number of chlorine atoms PCDDs PCDFs Tetrachloro 37Cl4-2,3,7,8-T4CDD 13C12-2,3,7,8-T4CDD 13C12-1, 2, 3, 4-T4CDD 13C12-1, 2, 7, 8-T4CDF 13C12-2,3,7,8-T4CDF Pentachloro 13C12-1,2,3,7,8-P5CDD 13C12-2,3,4,7,8-P5CDF 13C12-1,2,3,7,8-P5CDF Hexachloro 13C12-1, 2, 3, 7, 8, 9-H6CDD 13C12-1, 2, 3, 4, 7, 8-H6CDD 13C12-1,2,3,6,7,8-H6CDD 13C12-2,3,4,6,7,8-H6CDF 13C12-1,2,3,6,7,8-H6CDF 13C12-1,2,3,4,7,8-H6CDF 13C12-1,2,3,7,8,9-H6CDF Heptachlor 13C12-1,2,3,4,6,7,8-H7CDD 13C12-1,2,3,4,7,8,9-H7CDF Octachloro 13C12-OCDD 13C12-OCDF 3.2 Symbols and abbreviations 3.2.1 PCDDs Polychlorinated dibenzo-p-dioxins Polychlorinated dibenzo-p-dioxin. There are 75 similar species. 3.2.2 PCDFs Polychlorinated dibenzofurans Polychlorinated dibenzofuran. There are 135 similar species. 3.2.3 T4CDDs Tetrachlorodibenzo-p-dioxins Tetrachlorodibenzo-p-dioxin. There are 22 isomers. 3.2.4 P5CDDs Pentachlorodibenzo-p-dioxins Pentachlorodibenzo-p-dioxin. There are 14 isomers. 3.2.5 H6CDDs Hexachlorodibenzo-p-dioxins Hexachlorodibenzo-p-dioxin. There are 10 isomers. 3.2.6 H7CDDs Heptachlorodibenzo-p-dioxins Heptachlorodibenzo-p-dioxin. There are 2 isomers. 3.2.7 OCDD Octachlorodibenzo-p-dioxin Octachlorodibenzo-p-dioxin. There is 1 isomer. 3.2.8 T4CDFs Tetrachlorodibenzofurans Tetrachlorodibenzofuran. There are 38 isomers. 3.2.9 P5CDFs Pentachlorodibenzofurans Pentachlorodibenzofuran. There are 28 isomers. 3.2.10 H6CDFs Hexachlorodibenzofurans Hexachlorodibenzofuran. There are 16 isomers. 3.2.11 H7CDFs Heptachlorodibenzofurans Heptachlorodibenzofuran. There are 4 isomers. 3.2.12 OCDF Octachlorodibenzofuran Octachlorodibenzofuran. There is 1 isomer. 3.2.13 RRF Relative response factor Relative response factor. 3.2.14 HRGC High-resolution gas chromatography High resolution gas chromatography. 3.2.15 LRMS Low-resolution mass spectrometry Low resolution mass spectrometer. 3.2.16 SIM selective ion monitoring Select ion detection. 3.2.17 EI electron impact ionization Electron bombardment ionization 3.2.18 S/N signal/noise ratio Signal to noise ratio 3.2.19 PCBs polychlorinated biphenyls Polychlorinated biphenyl

4 Principle of the method

Samples are taken and dried according to the appropriate sampling specifications, using Soxhlet extraction, accelerated solvent extraction or other equivalent and verified The method is carried out, and the extract is purified by a sulfuric acid/silica gel column or a multi-layer silica gel column and an alumina column or an activated carbon dispersed silica gel column. Separate, concentrate and add the internal standard, and use high resolution gas chromatography-low resolution mass spectrometry (HRGC-LRMS) for qualitative and Quantitative analysis. See Appendix A, Flow Chart for Dioxin Analysis.

5 reagents and materials

Unless otherwise stated, pesticide-level reagents that meet the relevant standards were used for the analysis and a blank test was performed. Organic solvents Dioxins should not be detected at a concentration of 10,000 times. 5.1 Acetone ((CH3)2CO) 5.2 Toluene (C7H8) 5.3 n-hexane (n-C6H14) 5.4 Methanol (CH3OH) 5.5 dichloromethane (CH2Cl2) 5.6 anhydrous sodium sulfate (NaSO4). excellent grade pure, calcined at 660 ° C for 6 h in muffle furnace before use, after cooling to 150 ° C, turn Move to a desiccator, cool it, put it into a reagent bottle, and store it dry. 5.7 Hydrochloric acid solution. excellent grade, 1 1. 5.8 Sulfuric acid. excellent grade, ρ (H2SO4) = 1.84g/ml. 5.9 sodium hydroxide solution. c (NaOH) = 1 mol/L. 5.10 10% silver nitrate silica gel. commercially available, stored in a desiccator. 5.11 Reduction of copper Rinse with hydrochloric acid (5.7), distilled water, acetone (5.1), and toluene (5.2) before use, and store in a desiccator. 5.12 Silicone The chromatographic silica gel (100 ∼.200 mesh) was placed in a beaker and washed with dichloromethane (5.5) until the dichloromethane was completely After the hair is spread, placed in an evaporating dish or beaker, the thickness is less than 10mm, heated at 130 ° C for 18h, placed in a desiccator Cool for 30 min. Put it in a closed container and store it in a desiccator. 5.13 sodium hydroxide alkaline silica gel. ω = 33% Take 67g of silica gel (5.12), add 33g of sodium hydroxide solution (5.9) at a concentration of 1mol/l, stir well to make it The fluid is in the form of a powder. After the preparation is completed, it is sealed in a reagent bottle and stored in a desiccator. 5.14 Silicate Sulfuric Acid. ω=44% 100 g of silica gel (5.12) was taken, and 78.6 g of sulfuric acid (5.8) was added thereto, and after fully shaking, it became a powder. After the preparation is completed Seal into the reagent bottle and store in the desiccator. 5.15 Alumina Alumina for chromatography (basic activity I). Activated alumina can be used directly during the analysis. If necessary The activation method is as follows. the alumina is placed in a beaker and the thickness is less than 10 mm, and heated at 130 ° C for 18 hours. Or spread in a Petri dish to a thickness of 5 mm, heat at 500 ° C for 8 h, and cool in a desiccator for 30 min. Load The container is sealed and placed in a desiccator for storage. It should be used as soon as possible after activation. 5.16 Activated carbon dispersing silica gel. commercially available and stored in a desiccator. 5.17 Nitrogen. High purity nitrogen, 99.999%. 5.18 Water. Distilled water thoroughly washed with n-hexane (5.3). Unless otherwise stated, the water referred to in this standard refers to the above Treated distilled water. 5.19 dichloromethane-n-hexane solution. 3% (v/v) Methylene chloride and n-hexane were mixed in a volume ratio of 3.97. 5.20 dichloromethane-n-hexane solution. 50% (v/v) Methylene chloride and n-hexane were mixed in a volume ratio of 1.1. 5.21 dichloromethane-n-hexane solution. 25% (v/v) Methylene chloride and n-hexane were mixed in a volume ratio of 1.3. 5.22 Sodium chloride solution. ρ (NaCl) = 0.15 g/ml. 150 g of sodium chloride was dissolved in water and diluted to 1 L. 5.23 Alkaline detergent. commercially available. 5.24 Calibration Standards. Commercially available dioxin calibration standards, covering 17 different chlorine-substituted dioxins and furans, see attached Record B. 5.25 Purification of internal standard. Commercially available dioxins to purify internal standard substances, generally 8-17 kinds of 13C labeled compounds are selected as purification internal standards. See Appendix B. 5.26 Injecting internal standard. Commercially available dioxin-like injection internal standard substance, generally choose 1 2 kinds of 13C labeled compounds as injection internal standard. See Appendix B. 5.27 Perfluorotributylamine (PFTBA) calibration tuning standard solution, commercially available.

6 Instruments and equipment

6.1 Sampling device 6.1.1 Sampling tool. It should meet the requirements of HJ/T 166 and GB 17378.3, and use stainless steel which has no adsorption to dioxin. Steel or aluminum alloy appliances. 6.1.2 Sample container. It should meet the requirements of HJ/T 166 and GB 17378.3, and use stainless steel which has no adsorption to dioxin. Steel or glass sealables. 6.2 pre-processing device The sample pretreatment device should be thoroughly washed with alkaline detergent (5.23) and water, and acetone (5.1) and positively used before use. Rinse with a solvent such as alkane (5.3) or toluene (5.2) and perform a blank test periodically. Grease is strictly prohibited at all interfaces. 6.2.1 Soxhlet extractor or equivalent device 6.2.2 Concentration device. rotary evaporation concentrator, nitrogen blowing instrument and equivalent concentrating device. 6.2.2 Rapid extraction device. with 34ml and 66ml extraction tank, the extraction pressure is not less than 1500psi, the extraction temperature needs to be large At 120 ° C. 6.2.3 Chromatography column. inner diameter 8∼15mm, length.200∼300mm glass column. 6.3 Analytical instrument Dioxins were analyzed using high resolution gas chromatography-low resolution mass spectrometry (HRGC-LRMS). 6.3.1 High-resolution gas chromatography. The injection part adopts on-column injection or splitless injection, the maximum use temperature of the inlet 250 ∼ 280 ° C. 6.3.1.1 Quartz capillary column. length 25∼60m, inner diameter 0.1∼0.32mm, film thickness 0.1∼0.25μm quartz hair Thin tube column for good separation of 2,3,7,8-position chloro-substituted isomers and identification of chromatographic peaks of these compounds Out order. In order to ensure good separation of all 2,3,7,8-position chloro-substituted isomers, it is advisable to choose 2 different polarities. Capillary columns were measured separately. 6.3.1.2 Oven temperature. The temperature control range is 50∼350°C, which can be programmed. 6.3.2 Low Resolution Mass Spectrometry Ion source temperature, 250 ° C; electron bombardment (EI) mode; electron bombardment energy, 70 eV; selective ion detection method (SIM law). 6.3.3 Carrier gas. high purity helium (purity of 99.999% or more).

7 samples

7.1 Acquisition and preservation 7.1.1 Sampling in accordance with HJ/T 166 and GB 17378.3. After the sample is collected, save it in the dark and send it to the laboratory as soon as possible. Sample preparation and sample analysis. Instruments, materials, etc. used for sample collection should be kept clean and water and organic should be used before sampling. Solvent cleaning. 7.1.2 According to the requirements of HJ/T 166 and GB 17378.3, the collected samples are air-dried, crushed and sieved in the laboratory. save In a brown glass bottle. 7.1.3 Determination of moisture content The soil moisture content was determined by reference to HJ 613. 7.2 Preparation of samples The preparation of the sample mainly includes the addition of the purification internal standard, the extraction of the sample, the various purification of the extraction liquid, the concentration of the purification liquid, For the addition of the internal standard of injection, the flow chart of the pretreatment process is shown in Appendix C. 7.2.1 Sample extraction 7.2.1.1 Soxhlet extraction Weigh about 20g of air-dried sieved sample into the extraction cup of the Soxhlet extractor, and add 1ng of 13C12-standard to each sample. Remember to purify the internal standard. Extract with about.200 ∼ 300 ml of toluene (5.2) for more than 16 hours. Concentrate the extract to 1∼2ml, set Allow 5ml to be purified. 7.2.1.2 Rapid extraction method Weigh about 20g of air-dried sieved sample in a small beaker, add a certain amount of anhydrous sodium sulfate (5.6), and transfer the sample to A certain amount of 13C12-labeled purification internal standard was added to the extraction cell of the rapid extraction apparatus. The set extraction conditions are. pressure The pressure is 1500 psi, the temperature is 120 ° C, the solvent toluene (5.2) is extracted, the 100% is filled in the extraction cell mode, and the high temperature and high pressure are allowed to stand for 5 min. Cycle three times. The extracted sample is concentrated to volume according to the method of 7.2.1.1 and to be purified. 7.2.1.3 If the sediment sample contains a large amount of sulfide, desulfurization purification is required. The desulfurization method is as follows. the sample extract is concentrated Reduce to about 50ml, add the treated reduced copper, shake well, filter, collect the filtrate, and concentrate according to 7.2.1.1 Rong. 7.2.2 Purification of samples 7.2.2.1 Sulfuric acid-silica column purification. When the sample color is darker and the interference is large, the sulfuric acid-silica gel column purification method is adopted. 7.2.2.1.1 Place the 7.2.1 concentrated sample into a 250 ml separatory funnel, add 75 ml of n-hexane (5.3), and use 30 ml. ......
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