HJ 911-2017Soil and sediment--Extraction of organic compounds--Ultrasonic extraction (English PDF)

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 °C 4 h above, cooled and transferred to glass bottles, sealed and stored in a dry dish.

4.3 quartz glass wool.

Ignition at 400 °C 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) °C.

5.4 Sampling bottles. brown capping large mouth glass bottles, PTFE cap with a pad.

5.5 General laboratory equipment and equipment.

6 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 (%)