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HJ 835-2017 English PDF

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HJ 835-2017: Soil and sediment. Determination of organochlorine pesticides. Gas chromatography/Mass spectrometry
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HJ 835-2017English489 Add to Cart 5 days [Need to translate] Soil and sediment. Determination of organochlorine pesticides. Gas chromatography/Mass spectrometry Valid HJ 835-2017

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Basic data

Standard ID HJ 835-2017 (HJ835-2017)
Description (Translated English) Soil and sediment. Determination of organochlorine pesticides. Gas chromatography/Mass spectrometry
Sector / Industry Environmental Protection Industry Standard
Classification of Chinese Standard Z18
Classification of International Standard 13.080
Word Count Estimation 21,23
Date of Issue 2017-07-18
Date of Implementation 2017-09-01
Quoted Standard GB 17378.3; GB 17378.5; HJ 613; HJ 783; HJ/T 166
Regulation (derived from) MEP Announcement 2017 No. 31
Issuing agency(ies) Ministry of Ecology and Environment
Summary This standard specifies the determination of organochlorine pesticides in soil and sediment by gas chromatography - mass spectrometry. This standard is applicable to the determination of 23 organochlorine pesticides in soils and sediments. The targets include: ��-BHC, ��-BHC, ��-BHC, ��-BHC, Chloride, Aldrin, Epichlorohydrin, ��-Endosulfan, ��-Chlordane, Dieldrin, p, p "" - DDE, Endrin, ��-Endosulfan, p, DDD, endosulfan sulfate, endrin aldehyde, 0, p "" - DDT, endrin, p, p "" - DDT, methionine, mirex. Through verification, other organochlorine pesticides can also apply this standard. When the sample volume is 20.0 g, the volume of volume after concentration is 1.0 ml, the total scanning method

HJ 835-2017: Soil and sediment. Determination of organochlorine pesticides. Gas chromatography/Mass spectrometry


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(Soil and sediment - Determination of organochlorine pesticides - Gas chromatography - mass spectrometry) National Environmental Protection Standard of the People 's Republic of China Soil and sediments - Determination of organochlorine pesticides Gas chromatography - mass spectrometry Soil and sediment - Determination of organochlorine pesticides - Gas chromatography/Mass spectrometry 2017-07-18 released 2017-09-01 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 3 6 Sample 3

7 Analysis steps

8 Calculation and representation of results

9 precision and accuracy ..10 Quality Assurance and Quality Control 11 Waste disposal 12 12 Note ..12 Appendix A (normative appendix) method detection limit and lower limit of determination Appendix B (informative) Determination of the target compound Reference parameter 14 Appendix C (informative) method of precision and accuracy

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 In the determination of organochlorine pesticides, the development of this standard. This standard specifies the determination of 23 organochlorine pesticides in soil and sediments by gas chromatography-mass spectrometry. This standard is the first release. Appendix A to this standard is a normative appendix, Appendix B and Appendix C are informative appendices. This standard is organized by the Environmental Monitoring Department of the Ministry of Environmental Protection, the Secretary for Science and Technology Standards. The main drafting of this standard. Henan Province Environmental Monitoring Center. The standard verification unit. Xinxiang City Environmental Monitoring Station, Henan Province Environmental Science Research Institute, Zhengzhou City, environmental protection monitoring Heart station, Kaifeng City Environmental Monitoring Station, Institute of Hydrogeology and Geology, Chinese Academy of Geological Sciences, Henan Province Environmental Monitoring Center. The Environmental Protection Department of this standard approved on July 18,.2017. This standard has been implemented since September 1,.2017. This standard is explained by the Ministry of Environmental Protection. Determination of organochlorine pesticides in soil and sediments - Gas chromatography - mass spectrometry Warning. The organic solvents and reference materials used in the test are toxic and hazardous substances, standard solution preparation and sample pretreatment Should be carried out in the fume hood; operation should be required to wear protective equipment, to avoid direct contact with skin and clothing.

1 Scope of application

This standard specifies the determination of organochlorine pesticides in soil and sediments by gas chromatography-mass spectrometry. This standard is applicable to the determination of 23 organochlorine pesticides in soil and sediments. Targets include. α- 6606, hexachlor Benzene, beta-hexachloride, γ-six six six, δ-six six six, heptachlor, aldrin, epoxidized heptachlor, α-chlordane, α-endosulfan, γ- Dibenzo, p, p'-DDE, endrin, β-endosulfan, p, p'-DDD, endosulfan sulfate, aldrin aldehyde, o, p'-DDT, Endrin ketone, p, p'-DDT, methotrexate, mirex. This organism is also applicable to other organochlorine pesticides. When the sampling volume is 20.0 g and the volume of the volume after concentration is 1.0 ml, the detection limit is 0.02 mg/kg to 0.09 mg/kg, with a lower limit of 0.08 mg/kg to 0.36 mg/kg. See Appendix A.

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 Extraction of pressurized fluid from soil and sediment organic matter Technical specification for soil environmental monitoring

3 Principle of the method

The organochlorine pesticides in soil or sediments are extracted using a suitable extraction method (Soxhlet extraction, pressurized fluid extraction, etc.) According to the sample matrix interference to choose the appropriate purification method (copper powder desulfurization, magnesium silicate column or gel permeation chromatography), to mention Take liquid purification, and then concentrated, constant volume, by gas chromatography separation, mass spectrometry. According to the standard substance mass spectrometry, retention time, Debris ion mass ratio and its abundance characterization. Internal standard method.

4 reagents and materials

Unless otherwise stated, analytical reagents conforming to national standards are used for analysis. Experimental water for the new preparation of ultra-pure water Or distilled water. 4.1 acetone (C3H6O). pesticide residues. 4.2 n-hexane (C6H14). pesticide residues. 4.3 dichloromethane (CH2Cl2). pesticide residues. 4.4 ethyl acetate (C4H8O2). pesticide residues. 4.5 Cyclohexane (C6H12). Pesticide level. 4.6 ether (C4H10O). pesticide residues 24.7 N-Hexane - Acetone Mixed Solvent I. 1 1 Mix with 1. 1 by volume using n-hexane (4.2) and acetone (4.1). 4.8 N-Hexane-Acetone Mixed Solvent II. 9 1 Mixed with n-hexane (4.2) and acetone (4.1) at a volume ratio of 9. 1 4.9 Dichloromethane - acetone mixed solvent. 1 1 Mix with methylene chloride (4.3) and acetone (4.1) at a 1. 1 volume ratio. 4.10 N-Hexane-Ethyl Ether Mixed Solvent I. 94 6 Mix with 94. 6 volume with n-hexane (4.2) and diethyl ether (4.6). 4.11 n-Hexane-Ether Mixed Solvent II. 85 15 Using n-hexane (4.2) and diethyl ether (4.6) at a volume of 85.15. 4.12 N-Hexane-Ether Mixed Solvent III. 1 1 Mix with 1. 1 volume with n-hexane (4.2) and diethyl ether (4.6). 4.13 n-hexane-dichloromethane mixed solvent I. 1 1 Mix with 1. 1 volume with n-hexane (4.2) and dichloromethane (4.3). 4.14 n-hexane-dichloromethane mixed solvent II. 74 26 Mixed with hexanes (4.2) and dichloromethane (4.3) at a volume of 74.26. 4.15 Gel Permeation Chromatography Mobile phase. mixed with ethyl acetate (4.4) and cyclohexane (4.5) at 1 1 volume ratio, or by instrument The preparation of other solvent system. 4.16 nitric acid. ρ (HNO3) = 1.42 g/ml, excellent grade pure. 4.17 Nitric acid solution. 1 1. With excellent grade nitric acid (4.16) and experimental water by 1. 1 volume ratio mixed configuration. 4.18 organic chlorine pesticide standard stock solution. ρ = 1000 mg/L ~ 5000 mg/L, commercially available standard solution. 4.19 Organochlorine pesticide standard intermediate liquid. ρ =.200 mg/L ~ 500 mg/L. The organochlorine pesticide standard stock solution (4.18) was diluted with n-hexane-acetone mixed solvent I (4.7) and mixed. 4.20 Internal standard stock solution. ρ = 5000 mg/L Selection of pentachloronitrobenzene or phenanthrene-d10 or 䓛-d12 as internal standard. A commercially available standard solution. Other compounds can also be used to do Internal standard. 4.21 Internal standard broth. ρ = 500 mg/L Measure the amount of 1.0ml internal standard stock (4.20) in 10 ml volumetric flask, with n-hexane - acetone mixed solvent I (4.7) dilute Release to the marking, mixing. 4.22 Substitute stock solution. ρ =.2000 mg/L to 4000 mg/L, commercially available standard solution. Decachlorobenzene or 2,4,5,6-tetrachloro-xylene and dibutyl fumarate should be used. 4.23 Substitutes Intermediate. ρ =.200 mg/L to 400 mg/L The mixture was diluted with n-hexane-acetone mixed solvent I (4.7) on the standard stock solution (4.22) and mixed. 4.24 decafluorotriphenylphosphine (DFTPP) solution. ρ = 50 mg/L, commercially available standard solution. The other concentrations were diluted with dichloromethane (4.3) to a concentration of 50 mg/L. 4.25 Gel Permeation Chromatography Calibration solution. containing corn oil (25 mg/ml), di (2-diethylhexyl) phthalate (1 mg/ml), methotrexate (200 mg/L), perylene (20 mg/L) and sulfur (80 mg/L). Commercially available. 3 Note. All standard stock solutions from 4.18 to 4.25 should be stored in the manufacturer's product description. -10 ℃ below the dark preservation. Before use should check the changes, once the evaporation or degradation should be re-preparation, should be used before the room temperature, mixing. 4.26 desiccant. excellent pure anhydrous sodium sulfate (Na2SO4) or granular diatomaceous earth 250 μm ~ 150 μm (60 mesh ~ 100 Head). Placed in muffle furnace 400 ℃ baking 4 h, after cooling into the grinding glass bottle sealed in the dryer to save. 4.27 Copper powder (Cu). purity 99.5% Use the nitric acid solution (4.17) to remove the oxide on the surface of the copper powder before use, rinse off the acid with laboratory water, (4.1) cleaning, and then use high-purity nitrogen (4.34) dry standby, each temporary treatment, keep the copper powder surface bright. 4.28 Magnesium silicate adsorbent. 75 μm ~ 150 μm (200 mesh -100 mesh). Placed in the surface dish, with aluminum foil or tin paper light cover, 130 ℃ activated 12 h or so, remove the dryer into the cooling, stand-by. Proactively activated before use. 4.29 glass column. about 20 mm in diameter, 10 cm ~ 20 cm long, with PTFE piston. 4.30 Magnesium silicate purification column. filler for the magnesium silicate, 1000 mg, column volume of 6 -10 ml. 4.31 quartz sand. 150 μm ~ 830 μm (100 mesh to 20 mesh) Placed in the muffle furnace 400 ℃ bake 4 h, after cooling into a plugged glass bottle sealed in the preservation. 4.32 glass wool or glass fiber filter. before use with dichloromethane - acetone mixed solvent (4.9) dip, until the solvent volatile dry , Stored in a sealed mouth glass bottle sealed to save. 4.33 Soxhlet extraction sleeve. glass fiber or natural fiber material sleeve, glass fiber sleeve placed in muffle furnace 400 ℃ bake Bake 4 h, natural fiber material sleeve before use and sample extraction the same solvent cleaning purification. 4.34 High purity nitrogen. purity 99.999%. 4.35 Carrier gas. high purity helium, purity 99.999%.

5 instruments and equipment

5.1 Gas Chromatography/Mass Spectrometer. Electron Impact (EI) Ionization Source. 5.2 Column. quartz capillary column, length 30 m, inner diameter 0.25 mm, film thickness 0.25 m, stationary phase 5% - phenyl - Methylpolysiloxane, or other equivalent capillary column. 5.3 Extraction device. Soxhlet extraction and other equivalent equipment. 5.4 Gel Permeation Chromatography (GPC). a 254 nm fixed wavelength UV detector, filled with gel packing column. 5.5 Concentration device. rotary evaporator, nitrogen blowing instrument or other equivalent equipment. 5.6 Vacuum Freeze Dryer. No load vacuum below 13 Pa. 5.7 solid phase extraction device. 5.8 General laboratory equipment and equipment commonly used.

6 samples

6.1 Collection and storage of samples Soil samples were collected and preserved according to the relevant requirements of HJ/T 166, and the samples of sediment were in accordance with GB 17378.3 Seeking collection and preservation. Samples should be stored in a clean, flat-edged brown glass bottle. Transport should be sealed, dark, 4 ℃ The following refrigerated. Transported to the laboratory, if not timely analysis, should be below 4 ℃ cold storage, dark, sealed preservation, preservation Time no more than 10 days. 6.2 Determination of moisture 4 Determination of dry matter and moisture of soil samples According to HJ 613, the moisture content of sediment samples is measured according to GB 17378.5 implementation. 6.3 Preparation of the sample 6.3.1 Sample preparation The sample on the enamel plate or stainless steel plate, mix, remove branches sticks, leaves, stones and other foreign bodies, according to HJ/T 166 Quadrilateral Under normal circumstances should deal with fresh samples. Natural drying does not affect the purpose of analysis, can also be The sample is naturally dry. Fresh soil or sediment samples can be dried by freeze-drying and desiccant drying. If soil or deposited The moisture content of the sample is higher (greater than 30%). The aqueous phase should be centrifuged before drying. Method 1. freeze-drying method. Take appropriate sample after mixing, into the vacuum freeze dryer (5.6) dry and dehydrated. dry After the sample to be ground, over 250 μm (60 mesh) pore size of the sieve, homogenized into 250 μm (60 mesh) around the stars grain. Then take 20 g (accurate to 0.01 g) sample for extraction. Method 2. desiccant method. Weigh 20 g (accurate to 0.01 g) fresh sample, add a certain amount of desiccant (4.26) Mix, dehydrate and grind into fine particles, mix well until it is scattered, all transferred to the extraction container. 6.3.2 Extraction Extraction method can choose Soxhlet extraction, pressurized fluid extraction and other equivalent extraction method. a) Soxhlet extraction. Transfer the prepared soil or sediment samples to the Soxhlet extraction sleeve (4.33) and add Curve intermediate point above the concentration of the substitute intermediate (4.23), carefully placed in the Soxhlet extractor tube, in the round bottom solvent 100 ml of n-hexane-acetone mixed solvent I (4.7) was added to the bottle for 16 h to 18 h, and the reflux rate was controlled at 4-6 times/h. Then stop heating the reflux, remove the round bottom solvent bottle, to be concentrated. b) Pressurized fluid extraction is performed according to HJ 783. Note. If the above extract has significant moisture, further filtration and dehydration are required. Place a layer of glass wool or glass fiber on the glass funnel Filter (4.32), add about 5 g of anhydrous sodium sulfate (4.26), and extract the extract into a concentrated vessel. And then a small amount of n-hexane - acetone mixed solvent I (4.7) Wash the container 3 times, the washing liquid into the funnel to filter, and finally a small amount of n-hexane - acetone mixed solvent I (4.7) Bucket, all collected to the concentration of utensils, to be concentrated. 6.3.3 Concentration Concentration method is recommended in the following two ways. Other methods can also be used when proven to be superior or equivalent. a) Nitrogen blowing At room temperature, open the nitrogen to the solvent surface with airflow fluctuations (to avoid the formation of gas vortex), with n-hexane - acetone mixture Solvent I (4.7) Wash the wall of the concentrator that has been exposed during the nitrogen blowing process and concentrate to about 1 ml to be purified. When purified by gel permeation chromatography, when concentrated to about 2 ml, add about 5 ml gel permeation chromatography (4.15) for solvent conversion, and then concentrated to about 1 ml, to be purified. b) Rotate Evaporation Concentration The heating temperature was set at about 40 ° C, and the extract (6.3.2) was concentrated to about 2 ml to stop the concentration. With disposable drops The tube was transferred to a graduated concentrator and the rotary vial was washed with a small amount of n-hexane-acetone mixed solvent I (4.7) Wash the bottom 2 times, merge all the concentrate, and then boil with nitrogen to about 1 ml, to be purified. When purifying by gel permeation chromatography, when the above concentrated solution was concentrated to about 2 ml, about 5 ml of gel The permeate chromatographic mobile phase (4.15) was subjected to solvent conversion and then concentrated to about 1 ml with nitrogen to be purified. 6.3.4 Purification 5 Purification is recommended using the following methods. Other methods can also be used when proven to be superior or equivalent. 6.3.4.1 Magnesium silicate column purification method a) Preparation of magnesium silicate column Fill glass wool (4.32) at the bottom of the glass column (4.29), add about 1.5 cm thick anhydrous sodium sulfate (4.26) And 20 g of magnesium silicate adsorbent (4.28). The column walls were tapped and the magnesium silicate adsorbent (4.28) was filled evenly. Add again About 1.5 cm thick anhydrous sodium sulfate (4.26). Add 60 ml of n-hexane (4.2) to leach, and tap the column wall, The bubbles are filled with magnesium silicate adsorbent (4.28), keeping the filler filled with n-hexane (4.2), closing the piston, soaking the filler At least 10 min, at which time about 2 g of copper powder (4.27) is added to the top of the column to remove sulfur from the extract. Open the piston At the same time, continue to add n-hexane 60 ml leaching, when the top of the anhydrous sodium sulfate layer is exposed to the air just before the closure of the piston stand-by. If the filler is dry, it needs to be reprocessed. b) purification The concentrated extract was transferred to a magnesium silicate column and the concentrated tube was washed twice with 2 ml of n-hexane (4.2) All moved to the column, the solution should be immersed in copper powder (4.27) for about 5 min. 1) When it is not necessary to separate PCBs and organochlorine pesticides from samples, use.200 ml of n-hexane-dichloromethane Mix the solvent I (4.13) to elute the chromatographic column and collect the entire eluent. After re-concentration (6.3.5) after the determination. 2) When separating the PCB and organochlorine pesticides from the sample, place a round bottom flask under the magnesium silicate column and open Piston so that the concentrate (6.3.3) to the liquid level just off the sodium sulfate layer, close the piston. With.200 ml of n-hexane-ether mixture I (4.10) elution chromatography column, the eluent speed remained at 5 ml/min, collecting all eluent. The eluent contains polychloride Benzene and six six six, chlordane and other organochlorine pesticides (see Table 1). The solvent II was then mixed with.200 ml of n-hexane-diethyl ether (4.11) The elution solution was again eluted with beta-endosulfan, endosulfan sulfate, aldrin aldehydes and piecitrin Organochlorine pesticides. The column was washed again with.200 ml of n-hexane-diethyl ether mixed solvent III (4.12), and the eluent was left I-beta-endosulfan, endosulfan, phyto-phthalate, and endrin ketone are completely eluted and do not require independent testing When the polychlorinated biphenyls are combined with all the eluent, the independent test of PCBs should not be combined with the first part of the leaching. After re-concentration (6.3.5) after the determination. Note 1. Other rinsing systems are also available when they are verified to have a better purifying effect on the target. Table 1 Calcium silicate column at different stages of elution components No. Compound name Eluent 1 Eluent 2 Effluent 3 1 α 666 95.2% 2 hexachlorobenzene 107.3% 3 β-six six six 111.3% 4 γ-666 105.5% 5 δ-666 122.6% 6 Heptachlor 107.9% 7 aldrin 109.5% 8 epoxidized heptachlor 105.6% 9 α-Chloranal 113.8% 10 α-endosulfan 114.5% 11 γ-chlordane 108.4% 12 dieldrin 118.3% 13 p, p'-DDE 104.4% 14 endrin 123.8% 15 β-endosulfan 7.4% 60.9% 7.2% 616 p, p'-DDD 120.5% 17 Sulfate Sulfate 5.8% 33.6% 40.0% 18 Alder Aldehyde Aldehyde 2.0% 31.2% 78.4% 19 o, p'-DDT 111.8% 20 endrin ketone 11.0% 79.1% 7.1% 21 p, p'-DDT 117.4% 22 Methanol DDT 121.8% 23 Mirex 99.8% Note 2. The eluent component Eluent 1..200 ml ether. n-hexane mixture (volume ratio 6.94) Eluent 2..200 ml ether. n-hexane mixture (volume ratio 15.85) Eluent 3..200 ml ether. n-hexane mixture (1. 1 by volume) 6.3.4.2 Magnesium silicate purification column After the concentrated extract (6.3.3) is lighter in color, it can be purified by a magnesium silicate purification column (4.30). Steps as follows. The magnesium silicate purification column (4.30) was fixed on a solid phase extraction apparatus (5.7) and rinsed with 4 ml of n-hexane (4.2) Purify the column, then add 5 ml of n-hexane (4.2), after the column is filled to close the flow control valve infiltration 5 min, slow open control Valve, at this time in the top of the column by adding about 2 g copper powder (4.27) for the removal of sulfur in the extract. Continue to join 5 ml positive Hexane (4.2), before the copper powder (4.27) is exposed to air, close the control valve and discard the effluent. The concentrate (6.3.3) Transferred to the column, with 2 ml of n-hexane (4.2) fractional washing concentrated containers, lotion all into the column (if desulfurization, The solution should be immersed in copper powder for about 5 min). Slowly open the control valve and close it before the copper powder (4.27) is exposed to air Control valve. When the need for separation of PCBs and organochlorine pesticides in the sample, open the control valve and mix with 9 ml of n-hexane-acetone Agent II (4.8) elution, slowly open the control valve, so that the eluent immersed in the filler layer, close the control valve for about 1 min, The whole eluate was collected and allowed to concentrate again after adding the internal standard (6.3.5). 6.3.4.3 Gel Chromatography Purification a) Gel permeation column calibration The gel permeation column was calibrated according to the instrument manual, and the gel permeation chromatographic calibration solution (4.25) The peaks shall meet the following conditions. all peaks are symmetrically symmetrical; the color of corn oil and bis (2-diethylhexyl) phthalate The resolution between the peaks is greater than 85%; between the peaks of the bis (2-diethylhexyl) phthalate and the droplets of methotrexate Resolution is greater than 85%; the resolution between methoxazole and perylene peaks is greater than 85%; the peaks of perylene and sulfur can not overlap, Baseline separation is greater than 90%. b) Determine ...

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