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HJ 782-2016: Waste solid. Extraction of organic compounds. Pressurized fluid extraction (PFE)
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Waste solid. Extraction of organic compounds. Pressurized fluid extraction (PFE)
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Basic data | Standard ID | HJ 782-2016 (HJ782-2016) | | Description (Translated English) | Waste solid. Extraction of organic compounds. Pressurized fluid extraction (PFE) | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z13 | | Word Count Estimation | 13,128 | | Date of Issue | 2016-02-01 | | Date of Implementation | 2016-03-01 | | Quoted Standard | HJ/T 20 | | 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 solid waste in the pressurized fluid extraction method. This standard is applicable to the extraction of semi-volatile organic compounds and non-volatile organic compounds such as organophosphorus pesticides, organochlorine pesticides, chlorinated herbicides, polycyclic aromatic hydrocarbons, phthalic acid esters, polychlorinated biphenyls and other solid solid wastes, See Appendix A for details. If verified, this standard can also be applied to solid organic waste in the extraction of other organic matter. | HJ 782-2016: Waste solid. Extraction of organic compounds. Pressurized fluid extraction (PFE)---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.
Waste solid.Extraction of organic compounds.Pressurized fluid extraction (PFE)
National Environmental Protection Standard of the People 's Republic of China
Extraction of organic matter from solid waste
Pressurized fluid extraction
Waste solid - Extraction of organic compounds -
Pressurized fluid extraction (PFE)
2016-02-01 release
2016-03-01 implementation
Ministry of Environmental Protection released
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
9 Waste disposal
Appendix A (informative) Reference list for extraction of organic compounds by pressurized fluid extraction
Foreword
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 the Prevention and Control of Environmental Pollution by Solid Wastes,
Protect the environment, protect human health, regulate the extraction of organic matter in solid waste, the development of this standard.
This standard specifies the pressurized fluid extraction of organic matter in solid waste.
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 Solid Waste Organic Compounds 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 organic solids in solid solid waste fluid extraction method.
This standard applies to solid solid waste organic phosphorus 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 other organic substances in solid solid waste.
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.
Technical specification for SJ sample preparation for industrial solid waste
3 Principle of the method
The treated solid waste sample is added to a closed container, and a suitable organic solvent is selected, and the mixture is pressurized and heated
, In the liquid organic solvent and the sample in full contact, the solid waste of organic matter extracted into 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.
4.9 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.
24.10 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 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 solid waste samples are carried out in accordance with the relevant provisions of HJ/T 20.
Place the solid waste sample in a clean, non-intrusive plug with a brown glass bottle, stamped and sealed. Transport should be dark,
Frozen 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 frozen below 4 ℃, dark and sealed, the determination of semi-volatile organic matter sample retention time of 10 days, non-volatile
Sexual organic matter is 14 days, perishable samples should be analyzed as soon as possible.
6.2 Preparation of the sample
The samples should be dried, crushed, homogenized and sieved into fine particles before extraction. For dry solid waste such as ash,
Can be directly grinding homogenization (6.2.2). Large volumes of dry solid waste should be pulverized, ground and homogenized, and sieved (6.2.2).
Other solid solid wastes are prepared according to the procedure of 6.2.1, 6.2.2.
6.2.1 Drying and dehydration
Place the sample on an enamel plate or stainless steel plate, mix, remove the sticks, leaves, stones, glass, scrap metal and other foreign matter.
The drying of the sample can be selected according to the nature of the target in the following different ways.
Method 1. Fresh samples of non-volatile organic compounds (such as polychlorinated biphenyls) are dark and dry at room temperature.
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 amount of particles containing a small amount of water
Granular solid waste samples, add a certain amount of diatomaceous earth (4.9) to mix well, dehydrate, repeatedly ground in the mortar (5.4)
(About 1 mm), all transferred into the extraction tank (5.2) for extraction.
Note 1. All samples can not be dried using oven drying.
Note 2. If there is a clear aqueous phase in the solid waste sample, the aqueous phase should be centrifuged first and then dried in the appropriate manner
Reason. The results of this method are only the content of solid phase, the pollutants in the water phase are not included.
6.2.2 homogenization screening
3 Samples of the air-dried (Method 1) or freeze-dried (Method 2) were fractionated, ground and sieved in accordance with HJ/T 20 (5.3)
Homogenized into about 1 mm of fine particles.
Note 3. For sticky samples or greasy samples can be used to dry three methods of dehydration, grinding. Fibrous solid waste samples should be chopped,
The crushed material was as small as possible and a certain amount of sample was weighed into diatomaceous earth (4.9) or quartz sand (4.10) to ground into about 1 mm.
6.3 Determination of water content
The dried dish is washed with a washing solution, tap water, acetone (4.3) and experimental water, and dried at 105 ° C ± 2 ° C
Dry to constant weight, cool in the dryer to room temperature (at least 45 min), immediately after taking out (0m, accurate to 0.01 g).
Weigh about 10 g of solid waste sample in a dry dish weighing (1 m, accurate to 0.01 g). Will contain solid waste samples dry
Dry the oven at 105 ° C ± 2 ° C to constant weight, place it in a desiccator and cool to room temperature (at least 45 min). Immediately after removal,
(2m, accurate to 0.01 g). Calculate the moisture content according to formula (1).
21
Mm
Mmw (1)
Where.
W - sample moisture content,%;
0m - the quality of the dried dish after drying, g;
1m - the quality of the dry dish containing the solid waste sample before drying, g;
2m - mass of dry dish containing solid waste samples after drying, g.
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). Extraction pool should be selected
Consider weighing the weight of the solid waste sample, the volume and the amount of desiccant to be incorporated.
Note 4. The amount of sample to be weighed depends on the nature of the sample and the sensitivity of the analytical method used, the purpose of the analysis and the degree of contamination of the sample,
Multi-solid waste should be appropriate to reduce the amount of sampling; for example, sewage treatment sludge, should be controlled in the range of 2 g ~ 5 g.
7.2 Loading of sample
Tighten the bottom of the wash pool (5.2) 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.
4 Note 5. After loading the sample, the upper end of the extraction tank 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).
7.3.6 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.
High concentration of solid waste samples (high organic matter content) at least 2 times to be static extraction.
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.).
58.3 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.
6 Appendix A
(Informative)
Extraction of Organic Compounds by Pressurized Fluid Extraction
Table A gives a reference list of the extraction of some organic compounds from solid waste by pressurized fluid extraction.
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
7 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
8 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 86-74-8 ////
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