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HJ 783-2016 English PDF

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HJ 783-2016: Soil and sediment. Extraction of organic compounds. Pressurized fluid extraction (PFE)
Status: Valid
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HJ 783-2016299 Add to Cart 3 days Soil and sediment. Extraction of organic compounds. Pressurized fluid extraction (PFE) Valid

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Basic data

Standard ID: HJ 783-2016 (HJ783-2016)
Description (Translated English): Soil and sediment. Extraction of organic compounds. Pressurized fluid extraction (PFE)
Sector / Industry: Environmental Protection Industry Standard
Classification of Chinese Standard: Z13
Word Count Estimation: 12,120
Date of Issue: 2016-02-01
Date of Implementation: 2016-03-01
Quoted Standard: GB 17378.3; GB 17378.5; HJ 613; HJ/T 166
Regulation (derived from): ?Ministry of Environment Protection Bulletin 2016 No.10
Issuing agency(ies): Ministry of Ecology and Environment
Summary: This standard specifies the extraction of organic matter in soil and sediment pressurized fluid extraction. This standard is applicable to the extraction of organophosphorous pesticides, organochlorine pesticides, chlorinated herbicides, polycyclic aromatic hydrocarbons, phthalates, polychlorinated biphenyls and other semi-volatile organic compounds and non-volatile organic compounds in soil and sediments, See Appendix A for details. If verified, this standard can also be applied to soil and sediment in the extraction of other organic matter.

HJ 783-2016: Soil and sediment. Extraction of organic compounds. Pressurized fluid extraction (PFE)


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Soil and sediment.Extraction of organic compounds.Pressurized fluid extraction (PFE) National Environmental Protection Standard of the People 's Republic of China Soil and sediment organic matter extraction Pressurized fluid extraction Soil and sediment-extraction of organic compounds- Pressurized fluid extraction (PFE) 2016-02-01 release 2016-03-01 implementation Ministry of Environmental Protection I directory Preface .ii

1 Scope of application

2 normative reference documents

3 Principle of the method

4 reagents and materials 1 5 instruments and equipment 2 6 Sample 2 Extraction of sample 3 8 Precautions .4 Disposal of waste Appendix A (informative) Reference list for the extraction of compounds by pressurized fluid extraction

Foreword

For the implementation of the "People's Republic of China Environmental Protection Law" to protect the environment, protect human health, regulate soil and sediment Organic matter extraction method, the development of this standard. This standard specifies the pressurized fluid extraction of organic matter in soil and sediments. This standard is the first release. Appendix A to this standard is an informative appendix. This standard is organized by the Ministry of Environmental Protection Science and Technology Standards Division. The main drafting unit of this standard. Henan Province Environmental Monitoring Center. This standard is approved by the Ministry of Environmental Protection on February 1,.2016. This standard has been implemented since March 1,.2016. This standard is explained by the Ministry of Environmental Protection. Extraction of organic matter from soil and sediment. Pressurized fluid extraction WARNING. The organic solvents and standard substances used in the experiments contain toxic compounds. The procedure should be used in the fume hood. Line, the operation should be required to wear protective equipment, to avoid contact with skin and clothing.

1 Scope of application

This standard specifies the extraction of soil and sediment organic matter in the pressurized fluid extraction method. This standard applies to soil and sediment organophosphorus pesticides, organochlorine pesticides, chlorinated herbicides, polycyclic aromatic hydrocarbons, o-benzene Dicarboxylic acid esters, polychlorinated biphenyls and other semi-volatile organic compounds and non-volatile organic compounds extraction, see Appendix A. If verified, This standard is also applicable to the extraction of soil and other organic matter in sediments.

2 normative reference documents

The contents of this standard refer to the following documents or their terms. Those who do not specify the date of the reference file, the effective version of the appropriate For this standard. Specification for ocean monitoring - Part 3. Sample collection, storage and transport Specification for marine monitoring - Part 5. Sediment analysis Determination of Dry Matter and Moisture in Soil Technical specification for soil environmental monitoring

3 Principle of the method

The treated soil or sediment sample is added to a closed container, and a suitable organic solvent is selected. , In the liquid organic solvent and soil or sediment samples in full contact with the soil or sediment in the organic matter extraction To the organic solvent.

4 reagents and materials

Unless otherwise stated, the analytical grade is used in accordance with national standards. Experimental water is not prepared for new preparation Ultrasonic water or distilled water. 4.1 dichloromethane (CH2Cl2). pesticide residues. 4.2 n-hexane (C6H14). pesticide residues. 4.3 Acetone (C3H6O). pesticide residues. 4.4 Acetone-dichloromethane mixed solution. 1 1. Mix with acetone (4.3) and dichloromethane (4.1) in a 1. 1 by volume ratio. 4.5 Acetone-n-hexane mixed solution. 1 1. Mix with acetone (4.3) and n-hexane (4.2) in a 1. 1 by volume ratio 4.6 phosphoric acid. ρ (H3PO4) = 1.69 g/ml, excellent grade pure. 4.7 Phosphoric acid solution. 1 1. Mixed with phosphoric acid (4.6) and experimental water at a volume ratio of 1. 1. 4.8 Mixed solution of acetone-dichloromethane-phosphoric acid solution. 250 125 15 Mixed with acetone (4.3), dichloromethane (4.1) and phosphoric acid solution (4.7) at a volume ratio of 250. 125. 15. 24.9 Desiccant. Granular diatomaceous earth or other equivalent desiccant, 20 mesh to 100 mesh. Before use should be desiccant purification treatment, the specific method. 400 ℃ baking 4 h, or with organic solvents (4.1 or 4.2 Or 4.3) to remove the interference. 4.10 quartz sand. 20 mesh ~ 30 mesh. Before use to be purified, the specific method with the desiccant purification treatment (4.9). 4.11 Nitrogen. Purity ≥99.999%.

5 instruments and equipment

5.1 pressurized fluid extraction device. heating temperature range of 100 ℃ ~ 180 ℃; pressure up to.2000 psi (about 13.8 MPa). Equipped with 40 ml, 60 ml or other specifications of the glass receiving bottle (threaded cap, coated with silicone PTFE gasket); metal Material for funnel; dedicated glass fiber filter and so on. 5.2 Extraction cell. 11 ml, 22 ml, 34 ml, 66 ml or other specifications. Stainless steel, or resistant to.2000 psi (approx 13.8 MPa) pressure of the other materials, the extraction tank through a special polishing inside; the upper and lower ends are equipped with a spiral seal Cover and stainless steel sand core. 5.3 soil sieve. 1 mm diameter, metal mesh. 5.4 mortar. agate, glass or ceramic and other materials made. 5.5 General laboratory equipment and equipment.

6 samples

6.1 Collection and storage The collection and storage of soil samples were carried out in accordance with the relevant provisions of HJ/T 166. In accordance with the relevant provisions of GB 17378.3 Collection and storage of sediment samples. The soil and sediment samples are packed in a clean, non-intrusive stoppered brown glass bottle, stamped, sealed. transport process Should be protected from light, cold storage, as soon as possible back to the laboratory for analysis, on the way to avoid the introduction of interference or damage to the sample. If not Timely analysis, should be below 4 ℃ cold storage, dark and sealed preservation, determination of semi-volatile organic matter sample retention time of 10 Day, non-volatile organic matter for 14 days. 6.2 Preparation of the sample 6.2.1 Drying and dehydration The sample on the enamel plate or stainless steel plate, mix, remove branches sticks, leaves, stones, glass, scrap metal and other foreign matter, According to HJ/T 166 for the four points split. The drying of the sample can be selected according to the nature of the target in the following different ways. Method 1. Determination of PCBs and other non-volatile organic compounds and non-polar organic samples should be at room temperature to avoid Light, dry. Method 2. the need to determine the fresh sample, the use of freeze-drying method for drying dehydration. Method 3. the need to determine the fresh sample, you can also use desiccant dehydration method. Weigh the right amount of fresh sample and add A certain amount of diatomaceous earth (4.9) was thoroughly mixed and dehydrated and ground repeatedly into fine particles (about 1 mm) in a mortar (5.4) Fully mix until it is scattered, all transferred into the extraction tank (5.2) for extraction. Note 1. All samples can not be dried using oven. Note 2. If there is a significant aqueous phase in soil or sediment samples, the aqueous phase should be centrifuged first and then dried in the appropriate manner 3 dry treatment. 6.2.2 homogenization screening Samples of the air-dried (method 1) or freeze-dried (method 2) were ground and sieved (5.3) and homogenized About 1 mm fine particles. 6.3 Determination of water content Soil samples were measured in accordance with HJ 613, and the moisture content of the sediment samples was measured in accordance with GB 17378.5.

7 sample extraction

7.1 Extraction pool selection Under normal circumstances, 11 ml of the extraction tank (5.2) can hold 10 g sample, 22 ml extraction tank (5.2) can hold 20 g sample, 34 ml extraction tank (5.2) can be installed 30 g sample (extraction tank specific specifications see the instrument manual). Note 3. The sample weighed depends on the sensitivity of the analytical method used for subsequent use, the purpose of the analysis and the degree of contamination of the sample, the soil or sediment sample should Control in the range of 10 g ~ 30 g. 7.2 Loading of sample Take a clean extraction cell (5.2) to tighten the bottom cover and place it vertically on the horizontal table. Place a dedicated glass fiber filter on the filter Its bottom, the top placed a special funnel. Appropriate amount of sample (6.2) with a small beaker, if you want to add a substitute or isotope internal standard, Should be added to the sample, slightly shaking the small beaker to mix it into the sample. According to the number of samples in turn through the special funnel carefully turn Move to the extraction tank (5.2), remove the funnel, tighten the top cover (avoid sticking the sample to the extraction tank thread or spill). Vertical and smooth Pick up the extraction tank (5.2), tighten the lid at both ends and place it vertically and smoothly into the pressurized fluid extraction unit (5.1) in. Place a clean receiving bottle at the corresponding position of each extraction cell, record the corresponding extraction pool (5.2) for each sample and receive The number of the bottle. Corresponding to the receiving bottle volume, usually the extraction pool volume of 0.5 times to 1.4 times, different instruments will be different. Note 4. The upper end of the extraction cell after loading the sample should be kept at a height of 0.5 cm to 1.0 cm. If the upper space of the extraction cell is larger than 1.0 cm, Add appropriate amount of quartz sand (4.10). 7.3 Selection of solvents The following solvents or mixed solvents are recommended depending on the target. 7.3.1 Organophosphorus pesticides Dichloromethane (4.1); or acetone-dichloromethane mixed solution (4.4). 7.3.2 Organochlorine pesticides Acetone-dichloromethane mixed solution (4.4); or acetone-n-hexane mixed solution (4.5). 7.3.3 Chlorinated Herbicides Acetone - dichloromethane - phosphoric acid solution (4.8). 7.3.4 Polycyclic aromatic hydrocarbons Acetone-n-hexane mixed solution (4.5). 7.3.5 Polychlorinated biphenyls N-hexane (4.2); or acetone-dichloromethane mixed solution (4.4); or acetone-n-hexane mixed solution (4.5). 47.3.6 Other semi-volatile organic compounds Acetone-dichloromethane mixed solution (4.4); or acetone-n-hexane mixed solution (4.5). 7.4 Extraction conditions Carrier pressure. 0.8 MPa; Heating temperature. 100 ℃ (organic phosphorus pesticide can also choose 80 ℃, PCBs can choose 120 ℃); Extraction tank pressure. 1200 psi ~.2000 psi (about 8.3 MPa ~ 13.8 MPa); Preheat balance. 5 min; Static extraction time. 5 min; Solvent elution volume. 60% pool volume; Nitrogen (4.11) Purge time. 60 s (according to the extraction tank volume to increase the purge time in order to thoroughly rinse the sample); Static extraction times. 1 ~ 2 times. The above parameters are optimized for this method, and other reference conditions can also be selected according to the target compound or different instruments. 7.5 Automatic extraction of samples Conditions set, start the program, the instrument automatically complete the extraction. After the extraction is finished, the receiving vials are removed in turn, and the extract is concentrated and purified according to the analytical method. Analysis. 7.6 blank test Take the same mass of quartz sand (4.10) instead of the sample and follow the same procedure as the sample extraction (7.1 to 7.5).

8 Precautions

8.1 The extraction process should be carried out under ventilation conditions. 8.2 Extraction solvents can not be used in the self-ignition point in the range of 40 ℃ ~.200 ℃ extraction solvent (such as carbon disulfide, ether and 1,4- Dioxane, etc.). 8.3 The organic solvent should be degassed before use. The error indication of the organic solvent sensor is subject to troubleshooting, generally As a result of solvent leakage, should be carefully checked whether the sealing pool, or whether the gasket failure. Sometimes due to exposure to The light near the receiving bottle is too strong and the alarm. 8.4 When removing the sample from the extraction cell or cleaning the extraction tank, avoid the scratches on the inner wall of the extraction tank to affect the extraction effect. 8.5 A mixed solution of acetone-dichloromethane-phosphoric acid solution (4.8) was used in the extraction of chlorinated herbicides, using acetone (4.3) Rinse the piping used in the instrument. 8.6 The used extraction tank should be thoroughly cleaned to avoid contamination of the sample and residual sample clogging the extraction tank Stainless steel Sand filter mat. Specific cleaning methods. the extraction pool all open, with hot water, organic solvents (4.1 or 4.2 or 4.3) and the experiment Wash the water in turn with an ultrasonic cleaner. 8.7 All glassware application of washing liquid, tap water followed by washing, with chromic acid lotion soak overnight, and then tap water, the experiment Wash the water in turn, dry, spare, to prevent organic residues. 8.8 When the extraction conditions such as solvent, temperature and pressure are changed, the recovery rate should be re-verified.

9 Waste disposal

The organic waste generated in the experiment and other hazardous waste should be classified and stored, centralized custody, sent to the qualified unit processing.

5 Appendix A

(Informative) Extraction of Compounds by Pressurized Fluid Extraction Table A gives a reference list of pressurized fluid extraction methods for the extraction of soil organic compounds from soils or sediments. A list of organic compounds extracted by pressurized fluid extraction No. Name English Name CAS No. No. Name English Name CAS No. Organochlorine pesticides Organochlorine pesticides 1 α-hexahydrate α-BHC 319-84-6 17 endosulfan sulfate 1031-07-8 2 γ-hexahydrate γ-BHC 58-89-9 18 4,4'-DDT 4,4'-DDT 50-29-3 3 β-hexahydrate β-BHC 319-85-7 19 Endrin ketone Endrin ketone 53494-70-5 4 δ-6,6 6 δ-BHC 319-86-8 20 Methoxychlorine Methoxychlor 72-43-5 5 Hexachlor Heptachlor 76-44-8 21 Mirex Mirex 2385-85-5 6 Aldrin Aldrin 309-00-2 Organophosphorus pesticides 7 Heptachlor epoxide 1024-57-3 22 Dimethoate 60-51-5 8 γ-chlordane Gamma chlordane 5103-74-2 23 Phorbolidum Disulfoton 298-04-4 9 α-endosulfan α-Endosulfan Ⅰ 1031-07-8 24 Phytophosphate Mevinphos 7786-34-7 10 α-chitosan α-Chlordane 5103-71-9 25 Diazinon 333-41-5 11 Dieldrin Dieldrin 60-57-1 26 Phthalidide Tokuthion 34643-46-4 12 4,4'-drops of iso 4,4'-DDE 72-55-9 27 thiophosphate Bolstar 35400-43-2 13 Endrin Endrin 72-20-8 28 Flies Phosphorus Ronnel 299-84-3 14 beta-endosulfan II 33213-65-9 29 Phytophosphate Famphur 52-85-7 15 4,4'-drop 4,4'-DDD 72-54-8 30 methyl parathion Methyl parathion 298-00-0 16 Endrin aldehyde. Endrin aldehyde 7421-93-4 31 Phorate Phorate 298-02-2 6 No. Name English Name CAS No. No. Name English Name CAS No. Organophosphorus pesticide 53 Indene (1, 2, 3-cd) pyrene Indeno (1,2,3-cd) pyrene 193-39-5 32 Trees Bosphate Sulfotep 3689-24-5 54 Dibenzo (a, h) Anthracene Dibenzo (a, h) anthracene 53-70-3 33 Treated Phosphor Thionazin 297-97-2 55 Benzene perylene Benzo (ghi) perylene 191-24-2 34 Chlorpyrifos Thlorpyrifos 2921-88-2 Polychlorinated Biphenyls Chlorinated Herbicide 56 2,4,4'-Trichlorobiphenyl PCB28 7012-37-5 35 2,4-D 2,4-Dichlorophenoxyacetic acid 94-75-7 57 2,2 ', 5,5'-tetrachlorobiphenyl PCB52 35693-99-3 36 2,4-Dibutyrate methyl ester 2,4 DB-2-ethylhexyl ester 18625-12-2 58 2,2 ', 3,4,4', 5'-hexachlorobenzene PCB138 35065-28-2 37 2,4,5-chlorobenzoic acid (2, 4,5-richlorophenoxy) acetic acid 93-76-5 59 2,2 ', 4,5,5'-pentachlorobenzene PCB101 37680-73- 2 38 2,4,5-propionic acid methyl ester 2,4,5-TP methyl ester 4841-20-7 60 2,2 ', 4,4', 5,5'-hexachlorobenzene PCB153 35065-27 -1 Polycyclic aromatic hydrocarbons 61 2,2 ', 3,4,4', 5,5'-heptachlorobenzene PCB180 35065-29-3 39 Naphthalene Naphthalene 91-20-3 62 2,3 ', 4,4,5'-Pentachlorobiphenyl PCB118 31508-00-6 40 2-Methylnaphthalene 2-Methylnaphthalene 91-57-6 Other semi-volatile organic compounds 41 acenaphthylene 83-32-9 63 N-nitrosodimethylamine N-nitrosodimethylamine 621-64-7 42 acenaphthylene enhenaphthene 208-96-8 64 N-nitrosodi-n-propylamine 621-64-7 43 fluorene Fuorene 86-73-7 65 phenol Phenol 108-95-2 44 phenanthrene Phenanthrene 85-01-8 66 2-Chlorophenol 2-Chlorophenol 95-57-8 45 anthracene 120-12-7 67 2-methylphenol 2-Methyl-Phenol 95-48-7 46 Fluoranthene Fluoranthene 206-44-0 68 4-Methylphenol 4-Methylphenol 106-44-5 47 pyrene Pyrene 129-00-0 69 2-nitrophenol 2-Nitrophenol 88-75-5 48 Benzo (b) fluoranthene Benzo (b) fluoranthene 205-99-2 70 2, 4-xylenol 2,4-Dimethylphenol 105-67-9 49 䓛 Chrysene 218-01-9 71 2, 4-dichlorophenol 2,4-Dichloro-phenol 120-83-2 50 benzo (k) fluoranthene Benzo (k) fluoranthene 207-08-9 72 4-Chloro-3-methylphenol 4-Chloro-3-methyl-phenol 59-50-7 51 benzo (a) pyrene Benzo (a) pyrene 50-32-873 2,4,6-trichlorophenol 2,4,6-Trichloro-phenol 1988-6-2 52 benzo (a) anthracene Benzo (a) anthracene 56-55-3 74 4-nitrophenol 4-Nitrophenol 100-02-7 7 No. Name English Name CAS No. No. Name English name CAS No. 75 hexachlorocyclopentadiene 1,3-Cyclopentadiene, 1,2,3,4,5,5-Hexachloro- 77-47-4 93 Hexachlorobutadiene 1,3-Butadiene, 1,1,2,3,4,4-hexachloro- 87-68-3 76 2,4,5-Trichlorophenol 2,4,5-Trochlorophenol 95-95-4 94 Hexachloroethane 118-74-1 77 Pentachlorophenol 87-86-5 95 bis (2-chloroethoxy) methane Methane, bis (2-chloroethoxy) - 111-91-1 78 4,6-Dinitro-2-cresol 4,6-Dinitro-2-methylphenol 534-52-1 96 Azobenzene Azobenzene 103-33-3 79 2, 4-dinitrophenol 2,4-Dinitrophenol 51-28-5 97 4-bromodiphenyl ether 4-Bromophenyl phenyl ether 101-55-3 80 2, 4-dinitrotoluene 2,4-Dinitrotoluene 121-14-2 98 bis (2-chloroethyl) ether Bis (2-chloroethyl) ether 111-44-4 81 nitrobenzene Benzene, nitro-98-95-3 99 4-chlorophenyl phenyl ether 4-Chlorophenyl phenyl ether 7005-72-3 82 2, 6-dinitrotoluene 2,6-Dinitrotoluene 606-20-2 100 bis (2-chloroisopropyl) ether Bis (2-chloroisopropyl) ther 108-60-1 83 2-nitroaniline 2-Nitroaniline 88-74-4 101 Isophorone Isophorone 78-59-1 84 3-nitroaniline 3-Nitroaniline 99-09-2 102 Dibenzofuran Dibenzofuran 132-64-9 85 4-nitroaniline 4-Nitroaniline 100-01-6 103 Di-n-butyl phthalate Dibutyl phthalate 84-74-2 86 4-chloroaniline 4-Chloroaniline 106-47-8 104 bis (2-ethylhexyl) phthalate Bis (2-ethylhexyl) phthalate 117-81-7 87 1,3-dichloro Benzene, 1,3-dichloro- 541-73-1 105 Dimethyl phthalate 131-11-3 88 1,4-dichlorobenzene Benzene, 1,4-dichloro- 106-46-7 106 Diethyl phthalate 84-66-2 Benzene 1,2-dichloro- 95-50-1 107 Benzyl butyl phthalate 85-68-7 90 1,2,4-Trichlorobenzene Benzene, 1,2,4-trichloro- 120-82-1 108 Di-n-octyl phthalate phthalate 117-84-0 91 Hexachlorobenzene 118-74-1 109 2-Chloronaphthalene Naphthalene, 2-chloro-91-58-7 92 carbazole Carbazole 86-74-8
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