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HJ 911-2017: Soil and sediment--Extraction of organic compounds--Ultrasonic extraction
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Soil and sediment--Extraction of organic compounds--Ultrasonic extraction
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HJ 911-2017
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Basic data | Standard ID | HJ 911-2017 (HJ911-2017) | | Description (Translated English) | Soil and sediment--Extraction of organic compounds--Ultrasonic extraction | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z18 | | Word Count Estimation | 13,196 | | Date of Issue | 2017-12-29 | | Date of Implementation | 2018-04-01 | | Regulation (derived from) | Ministry of Environmental Protection Bulletin 2017 No. 86 | | Issuing agency(ies) | Ministry of Ecology and Environment | HJ 911-2017: Soil and sediment--Extraction of organic compounds--Ultrasonic extraction---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.
People's Republic of China national environmental protection standards
Soil and sediment-Extraction of organic compounds
-Ultrasonic extraction
2017-12-29 Posted
2018-04-01 implementation
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 .2
6 samples .2
7 Extraction steps .2
8 Quality Assurance and Quality Control 3
9 Waste treatment .3
10 Notes 3
Appendix A (informative) Available organic extraction of ultrasonic extraction reference list.4
Appendix B (informative) Extraction efficiency of different extractants .7
Foreword
In order to carry out "Environmental Protection Law of the People's Republic of China", protect the environment, protect human health, regulate soil and sediment
In the extraction of organic matter, the development of this standard.
This standard specifies the extraction of organic matter in soil and sediment by ultrasonic extraction.
This standard Appendix A and Appendix B is an informative annex.
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. Shanghai Environmental Monitoring Center.
This standard MEP approved on December 29,.2017.
This standard since April 1,.2018 come into operation.
This standard is interpreted by the MEP.
Soil and sediment extraction of organic matter by ultrasonic extraction
Warning. The organic solvents and standard solutions used in the experiment are toxic and hazardous substances, should be operated in a fume hood, and press
Provisions on wearing protective equipment, to avoid contact with skin and clothing.
1 scope of application
This standard specifies the extraction of organic matter in soil and sediment by ultrasonic extraction.
This standard applies to soil and sediment polycyclic aromatic hydrocarbons, phenols, phthalates and organochlorine pesticides and other semi-volatile
For the extraction of sexual organics, the reference list of organics that can be extracted by this method is shown in Appendix A. If verified, other organic matter also
This method can be used to extract.
This standard does not apply to the extraction of volatile organic substances (such as organophosphorus pesticides, etc.) extraction conditions.
2 Normative references
This standard references the following documents or the terms. For undated references, the effective version applies to this book
standard.
GB 17378.3 Marine monitoring code - Part 3. Sample collection, storage and transport
GB 17378.5 Marine monitoring code - Part 5. Sediment analysis
HJ 613 Determination of soil dry matter and moisture Gravimetric method
HJ/T 166 Soil Environmental Monitoring Technical Specifications
3 method principle
Utilizing the mechanical vibration effect, cavitation effect and perturbation effect caused by ultrasonic radiation,
Adsorption on the surface of sediments increases the frequency and speed of movement of matter molecules, increases the penetration of solvents, and accelerates organic matter
Dissolution in the organic phase.
4 Reagents and materials
Unless otherwise stated, analytical grade reagents that meet national standards are used.
4.1 extractant.
4.1.1 Dichloromethane (CH2Cl2).
4.1.2 n-Hexane (C6H14).
4.1.3 Acetone (C3H6O).
4.1.4 Dichloromethane - acetone mixed solvent. 1 1.
Mix with dichloromethane (4.1.1) and acetone (4.1.3) at a volume ratio of 1.1.
4.1.5 n-hexane - acetone mixed solvent. 1 1.
Mix with n-hexane (4.1.2) and acetone (4.1.3) at a volume ratio of 1.1.
Note. According to the determination of the target compound extractant can use dichloromethane (4.1.1), n-hexane (4.1.2), dichloromethane - acetone mixed solvent
(4.1.4) or n-hexane-acetone mixed solvent (4.1.5) (see Appendix B). If verified, other solvents are acceptable
As the method of extracting agent.
4.2 anhydrous sodium sulfate (Na2SO4). granular.
Burning at 400 ℃ 4 h above, cooled and transferred to glass bottles, sealed and stored in a dry dish.
4.3 quartz glass wool.
Ignition at 400 ℃ 1 h above, cooled and placed in a sealed glass jar sealed.
5 instruments and equipment
5.1 Sample ultrasonic extraction instrument. probe type, the power is not less than 500 W, the ultrasonic output power can be adjusted.
5.2 Centrifuge. 2 000 r/min or above.
5.3 oven. temperature can be controlled at (105 ± 5) ℃.
5.4 Sampling bottles. brown capping large mouth glass bottles, PTFE cap with a pad.
5.5 General laboratory equipment and equipment.
6 samples
6.1 Sample Collection and Storage
Soil samples were collected and stored according to HJ/T 166. In accordance with the relevant provisions of GB 17378.3 into
Sediment sample collection and preservation.
6.2 Sample Preparation
6.2.1 Place the soil sample on a stainless steel plate, remove the sticks, leaves, stones, glass, scrap metal and other foreign matter, mix well
Samples; sediment samples to remove the surface of the water sample layer, and then remove sticks, leaves, stones, glass, scrap metal and other foreign matter,
Mix samples. Then follow the HJ/T 166 requirements for sample fractionation.
If the analytical method is otherwise specified, it shall be implemented according to the provisions.
6.2.2 When extracting fresh samples, weigh approximately 20 g (to 0.01 g) of the sample in a 250 ml glass beaker and add a
Quantitative anhydrous sodium sulfate (4.2) (anhydrous sodium sulfate added depending on the amount of moisture content of the sample, but to ensure that the total is not super
Half the capacity of the beaker), stir with a stainless steel spoon, so that the sample after stirring flow sand, to be extracted.
Note 1. Freeze-drying method can also be used.
Note 2. All samples should not be oven dried.
6.3 Determination of moisture content
The moisture content was measured at the same time as the samples were taken. Soil samples were dried according to HJ 613
Determination, in accordance with the requirements of GB 17378.5 Determination of moisture content of sediment samples.
7 extraction steps
7.1 Add about 50 ml of extractant (4.1) to the beaker containing the sample (6.2.2) to ensure that the level of extractant added is high
The surface of the solid sample is about 2 cm, and the ultrasonic probe is inserted 1 cm below the liquid surface. However,
Surface (according to the sample volume, increase or decrease the appropriate amount of extractant).
7.2 Adjust the ultrasonic power and probe depth probe to ensure that the sample can be completely extracted in the extraction, ultrasonic extraction 3 min.
7.3 Put a small amount of quartz glass wool in the neck of the funnel (4.3), then add the appropriate amount of anhydrous sodium sulfate (4.2), the extract through the funnel
Dry filter.
Note. After ultrasonic extraction, such as extract suspended in solid particles, to be centrifuged. Pour the extract into the centrifuge tube and centrifuge at low speed
In addition to the solid particles, the subsequent steps with 7.3.
7.4 Repeat extraction twice, the combined extract three times until further processing.
8 Quality Assurance and Quality Control
Quality assurance and quality control requirements, reference to specific compounds corresponding analytical method standards.
9 Waste treatment
Solid waste generated by the laboratory should be kept in a centralized manner and sent to a qualified unit for unified treatment.
10 Matters needing attention
10.1 Avoid contact with plastic products during both sampling and ultrasonic extraction.
10.2 After the sample is extracted, the ultrasonic extraction probe is washed with extractant and the washing solution is incorporated into the extract.
Appendix B
(Informative)
Extraction efficiency of different extractants
Standard soil samples (semi-volatile organic standard soil concentration of about 1 mg/kg, organochlorine pesticide standard soil concentration
About 5 μg/kg), each sample was extracted three times with different extractants, extracted for 3 min each time,
Concentration, semi-volatile organic compounds were analyzed by gas chromatography-mass spectrometry, organochlorine pesticides analysis by gas chromatography-
Electronic capture detection method, the results shown in Table B.1 and Table B.2.
Table B.1 different solvents on the semi-volatile organic compounds extraction efficiency (%)
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