CN113310770A - Preservation method for monitoring and analyzing persistent organic pollutant sample in environment - Google Patents
Preservation method for monitoring and analyzing persistent organic pollutant sample in environment Download PDFInfo
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- CN113310770A CN113310770A CN202110698556.2A CN202110698556A CN113310770A CN 113310770 A CN113310770 A CN 113310770A CN 202110698556 A CN202110698556 A CN 202110698556A CN 113310770 A CN113310770 A CN 113310770A
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- 238000000034 method Methods 0.000 title claims abstract description 33
- 239000002957 persistent organic pollutant Substances 0.000 title claims abstract description 33
- 238000012544 monitoring process Methods 0.000 title claims abstract description 19
- 238000004321 preservation Methods 0.000 title claims description 14
- 238000009461 vacuum packaging Methods 0.000 claims abstract description 25
- 230000000694 effects Effects 0.000 claims abstract description 7
- 238000004458 analytical method Methods 0.000 claims abstract description 6
- 239000000523 sample Substances 0.000 claims description 64
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 45
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 33
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 239000011347 resin Substances 0.000 claims description 17
- 229920005989 resin Polymers 0.000 claims description 17
- 238000005406 washing Methods 0.000 claims description 11
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 238000004806 packaging method and process Methods 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 7
- 238000000944 Soxhlet extraction Methods 0.000 claims description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 6
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- 239000011521 glass Substances 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- 230000007613 environmental effect Effects 0.000 claims description 5
- 239000000447 pesticide residue Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- 238000005070 sampling Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 238000007781 pre-processing Methods 0.000 claims description 3
- 238000005086 pumping Methods 0.000 claims description 3
- 239000012521 purified sample Substances 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 239000000356 contaminant Substances 0.000 claims 1
- 230000002085 persistent effect Effects 0.000 claims 1
- 150000003071 polychlorinated biphenyls Chemical class 0.000 abstract description 6
- 125000005575 polycyclic aromatic hydrocarbon group Chemical group 0.000 abstract description 6
- 238000007789 sealing Methods 0.000 abstract description 6
- USIUVYZYUHIAEV-UHFFFAOYSA-N diphenyl ether Chemical class C=1C=CC=CC=1OC1=CC=CC=C1 USIUVYZYUHIAEV-UHFFFAOYSA-N 0.000 abstract description 4
- 150000002790 naphthalenes Chemical class 0.000 abstract description 4
- 239000003463 adsorbent Substances 0.000 description 11
- 239000003570 air Substances 0.000 description 5
- 239000012080 ambient air Substances 0.000 description 5
- 239000003960 organic solvent Substances 0.000 description 5
- 230000009286 beneficial effect Effects 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000004896 high resolution mass spectrometry Methods 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65B—MACHINES, APPARATUS OR DEVICES FOR, OR METHODS OF, PACKAGING ARTICLES OR MATERIALS; UNPACKING
- B65B31/00—Packaging articles or materials under special atmospheric or gaseous conditions; Adding propellants to aerosol containers
- B65B31/04—Evacuating, pressurising or gasifying filled containers or wrappers by means of nozzles through which air or other gas, e.g. an inert gas, is withdrawn or supplied
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65B—MACHINES, APPARATUS OR DEVICES FOR, OR METHODS OF, PACKAGING ARTICLES OR MATERIALS; UNPACKING
- B65B5/00—Packaging individual articles in containers or receptacles, e.g. bags, sacks, boxes, cartons, cans, jars
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
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- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- Mechanical Engineering (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Dispersion Chemistry (AREA)
- Biomedical Technology (AREA)
- Molecular Biology (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
A method for preserving samples of persistent organic pollutants in environment monitoring and analysis comprises vacuumizing a vacuum packaging bag by a vacuum packaging machine to make the vacuum degree in the container about-70 KPa, and sealing the opening of the bag; storing the vacuum packaging bag filled with the sample into a sample box with a light-proof effect, wherein the storage temperature is lower than 30 ℃; the method is used for monitoring Persistent Organic Pollutants (POPs) such as Polycyclic Aromatic Hydrocarbons (PAHs), polychlorinated biphenyls (PCBs), polybrominated diphenyl ethers (PBDEs), polychlorinated naphthalenes (PCNs) and the like in the environment.
Description
Technical Field
The invention relates to the technical field of sample preservation, in particular to a preservation method for a persistent organic pollutant sample monitored and analyzed in an environment.
Background
The method for preserving the adsorbent of some domestic environment detection units has obvious and insufficient effect for users, most ecological environment monitoring laboratories have the phenomenon that samples and transportation blanks for manually monitoring persistent organic pollutants such as polycyclic aromatic hydrocarbon, polychlorinated biphenyl, polybrominated diphenyl ether, polychlorinated naphthalene and the like in ambient air are easy to be polluted, so that the blank background concentration of the adsorbent is higher than the standard requirement, the concentration of the persistent organic pollutants in the ambient air in China is low, and the difficulties that the actual concentration in the ambient air cannot be accurately measured, the quality of the ambient air cannot be evaluated and the like can occur. HJ646-3. The ministry of ecology environment releases the survey of the standard of PBDEs high-resolution gas chromatography-high-resolution mass spectrometry in the ambient air in 2020, and the lower limit of the survey is 0.04-36 pg/m3. Therefore, the background value of the sampling consumables is highly required, and in view of this, it is crucial to ensure that the adsorbent is not contaminated during storage and transportation.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for preserving a persistent organic pollutant sample for monitoring and analyzing in an environment, which can effectively solve the problems in the background technology.
In order to solve the problems, the technical scheme adopted by the invention is as follows: a method for preserving samples of persistent organic pollutants for environmental monitoring and analysis, comprising the steps of:
s1, sampling: selecting a sample to be stored, wherein the sample is PUF or XAD-2 resin;
s2, preprocessing: in a clean laboratory, the sample is started to be processed; when the sample is the PUF, scalding the PUF by using boiled deionized water, then putting the PUF into warm water for repeatedly rubbing and washing, and draining the water in the PUF; when the sample is XAD-2 resin, directly washing with deionized water, and then pumping water in XAD-2; this step was repeated twice;
s3, secondary treatment: pre-washing the pretreated sample by using methanol, removing water, performing Soxhlet extraction on XAD2 resin for 48 hours by using dichloromethane, and performing Soxhlet extraction on the PUF by using a mixed solution prepared from methanol and toluene for 48 hours; placing the extracted and purified sample into a vacuum drier for 8 hours;
s4, sample containing: taking out the sample in the vacuum drier, and placing the sample in a special vessel;
s5, packaging vessel: putting the vessel with the sample into a vacuum packaging bag, and manufacturing a vacuum environment for the vacuum packaging bag by using a vacuum packaging machine;
s6, storing samples: and (4) storing the vacuum packaging bag filled with the sample into a sample box with a light-proof effect.
As a further preferable embodiment of the present invention, the mixing ratio of the mixed solution is methanol: toluene =1:1 (volume ratio).
As a further preferable embodiment of the present invention, the temperature in the vacuum dryer in S3 is lower than 50 ℃.
In a further preferred embodiment of the present invention, the vacuum degree in the vacuum environment in S5 is-70 Kpa.
As a further preferred version of the invention, the temperature inside the sample chamber is below 30 ℃.
As a further preferred aspect of the present invention, the vessel is an aluminum can or a brown glass bottle.
As a further preferable scheme of the invention, the methanol, the toluene and the dichloromethane are pesticide residue grade solvents.
As a further preferred aspect of the present invention, the vacuum packaging bag is a food grade packaging bag combining PE and PA.
As a further preferable scheme of the invention, the transportation method of the sample of the persistent organic pollutant monitored and analyzed in the environment comprises the preservation method of the sample of the persistent organic pollutant monitored and analyzed in the environment.
As a further preferred embodiment of the invention, the method for detecting the organic pollutant sample comprises the preservation method for monitoring and analyzing the persistent organic pollutant sample in the environment.
Compared with the prior art, the invention provides a method for preserving a sample for monitoring and analyzing persistent organic pollutants in an environment, which has the following beneficial effects:
the method comprises the steps of performing purification treatment on an adsorbent before preservation, wherein the type and volume of an organic solvent are less than those specified by a standard and are more beneficial to the environment, performing primary sealing storage on a sample by using a special vessel, performing secondary sealing storage on the sample by using a packaging bag and a vacuum machine, and performing tertiary sealing storage on the sample by using a light shielding box, so that the preservation time of the adsorbent is greatly prolonged and can be as long as 8 days; the method is used for monitoring Persistent Organic Pollutants (POPs) such as Polycyclic Aromatic Hydrocarbons (PAHs), polychlorinated biphenyls (PCBs), polybrominated diphenyl ethers (PBDEs), polychlorinated naphthalenes (PCNs) and the like in the environment.
Drawings
FIG. 1 is a schematic flow chart of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
The invention provides a method for preserving a sample for monitoring and analyzing persistent organic pollutants in an environment, which comprises the following steps:
s1, sampling: selecting a sample to be stored, wherein the sample is PUF or XAD-2 resin;
s2, preprocessing: in a clean laboratory, the sample is started to be processed; when the sample is the PUF, scalding the PUF by using boiled deionized water, then putting the PUF into warm water for repeatedly rubbing and washing, and draining the water in the PUF; when the sample is XAD-2 resin, directly washing with deionized water, and then pumping water in XAD-2; this step was repeated twice;
s3, secondary treatment: pre-washing the pretreated sample by using methanol, removing water, performing Soxhlet extraction on XAD2 resin for 48 hours by using dichloromethane, and performing Soxhlet extraction on the PUF by using a mixed solution prepared by using methanol and toluene in a one-to-one volume manner for 48 hours; placing the extracted and purified sample into a vacuum drier for 8 hours;
s4, sample containing: taking out the sample in the vacuum drier, and placing the sample in a special vessel;
s5, packaging vessel: putting the vessel with the sample into a vacuum packaging bag, and manufacturing a vacuum environment for the vacuum packaging bag by using a vacuum packaging machine;
s6, storing samples: and (4) storing the vacuum packaging bag filled with the sample into a sample box with a light-proof effect.
As a further preferable scheme of the invention, the volume of the used organic solvent is less than that specified in HJ646-2013 and HJ647-2013, the variety of the organic solvent is less, and the organic solvent is more beneficial to the environment, and the organic solution is a mixed solution prepared by deionized water, dichloromethane, methanol and toluene; the mixing proportion of the mixed solution is methanol: toluene =1:1 (volume ratio).
As a further preferable embodiment of the present invention, the temperature in the vacuum dryer in S3 is lower than 50 ℃.
In a further preferred embodiment of the present invention, the vacuum degree in the vacuum environment in S5 is-70 Kpa.
As a further preferred version of the invention, the temperature inside the sample chamber is below 30 ℃.
As a further preferred aspect of the present invention, the vessel is an aluminum can or a brown glass bottle.
As a further preferable scheme of the invention, the methanol, the toluene and the dichloromethane are pesticide residue grade solvents.
As a further preferred aspect of the present invention, the vacuum packaging bag is a food grade packaging bag combining PE and PA.
As a further preferable scheme of the invention, the transportation method of the sample of the persistent organic pollutant monitored and analyzed in the environment comprises the preservation method of the sample of the persistent organic pollutant monitored and analyzed in the environment.
As a further preferred embodiment of the invention, the method for detecting the organic pollutant sample comprises the preservation method for monitoring and analyzing the persistent organic pollutant sample in the environment.
As a specific embodiment of the present invention:
selecting a proper adsorbent in a clean laboratory, and when the selected adsorbent is a PUF (physical unclonable function), scalding the adsorbent by using boiled deionized water, and then repeatedly rubbing and washing the adsorbent in warm water; if the selected adsorbent is XAD-2 resin, washing with deionized water, and draining water in the PUF or XAD-2 resin; the above procedure was repeated twice, then pre-washed with methanol (pesticide residue grade) and water removed, and finally the XAD2 resin was soxhlet extracted with dichloromethane for 48 hours, with methanol: soxhlet extracting PUF with mixed solution of toluene (V: V, pesticide residue grade) =1:1 for 48 hr, and putting the purified PUF or XAD-2 resin in vacuum drier at 50 deg.C or below for 8 hr; after 8 hours, taking out the PUF or XAD-2 resin in the vacuum dryer, recovering the original state of the PUF, placing the PUF or XAD-2 resin in a vessel with a moderate size, wherein the vessel can be an aluminum can or a brown glass bottle, covering the vessel with a cover, and screwing down the vessel; filling the aluminum pot or brown glass bottle filled with the sample into a vacuum packaging bag; vacuumizing the vacuum packaging bag by using a vacuum packaging machine to ensure that the vacuum degree in the container is about-70 KPa, and sealing the opening of the bag; and (3) storing the vacuum packaging bag filled with the sample into a sample box with a light-proof effect, wherein the storage temperature is lower than 30 ℃. The adsorbent for monitoring is purified by using an organic solvent according to a certain proportion, so that the storage time of the sample is greatly prolonged.
The vacuum packaging machine is an existing instrument in the market, the vacuum degree in a container reaches-70 KPa, the working power is 120W, the air suction speed is 12L/min, and the sealing width is at most 30 cm. A PE + PA food-grade vacuum packaging bag is adopted, and the specification is 20 cm multiplied by 25 cm. The specification of the aluminum pot/brown glass bottle is that the height is 9.5cm, and the inner diameter is 8 cm; the PUF is 90 cm × 70mm at most, 9 cm in height and 7cm in inner diameter, the XAD-2 resin is fine particles, and the PUF and the XAD-2 resin can be completely wrapped in a vacuum bag.
Vacuum packaging, also called pressure reduction packaging, is to completely draw out and seal the air in a packaging container, maintain the bag in a highly reduced pressure state, reduce the oxygen content in the package, make the air rare equivalent to a low oxygen effect, make the air quantity low, make the microorganism have no living condition, so as to achieve the purpose that POPs samples can not adsorb air. The vacuum package is used for protecting the product from environmental pollution and prolonging the storage life of the sample, and can improve the value and quality of the product.
The preserver adopted by the invention does not contain persistent organic pollutants such as polycyclic aromatic hydrocarbon, polychlorinated biphenyl, polybrominated diphenyl ether, polychlorinated naphthalene and the like.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. A method for preserving samples of persistent organic pollutants for environmental monitoring and analysis, comprising the steps of:
s1, sampling: selecting a sample to be stored, wherein the sample is PUF or XAD-2 resin;
s2, preprocessing: in a clean laboratory, the sample is started to be processed; when the sample is the PUF, scalding the PUF by using boiled deionized water, then putting the PUF into warm water for repeatedly rubbing and washing, and draining the water in the PUF; when the sample is XAD-2 resin, directly washing with deionized water, and then pumping water in XAD-2; this step was repeated twice;
s3, secondary treatment: pre-washing the pretreated sample by using methanol, removing water, performing Soxhlet extraction on XAD2 resin for 48 hours by using dichloromethane, and performing Soxhlet extraction on the PUF by using a mixed solution prepared from methanol and toluene for 48 hours; placing the extracted and purified sample into a vacuum drier for 8 hours;
s4, sample containing: taking out the sample in the vacuum drier, and placing the sample in a special vessel;
s5, packaging vessel: putting the vessel with the sample into a vacuum packaging bag, and manufacturing a vacuum environment for the vacuum packaging bag by using a vacuum packaging machine;
s6, storing samples: and (4) storing the vacuum packaging bag filled with the sample into a sample box with a light-proof effect.
2. The preservation method for the sample of persistent organic pollutants monitored and analyzed in the environment as claimed in claim 1, wherein the mixing solution is prepared by mixing methanol: toluene ═ 1:1 (volume ratio).
3. The method of claim 1, wherein the temperature in the vacuum dryer of S3 is less than 50 ℃.
4. The preservation method for monitoring and analyzing persistent organic pollutant sample in environment according to claim 1, wherein the vacuum degree in the vacuum environment in the S5 is-70 KPa.
5. The method of claim 1, wherein the temperature inside the sample chamber is lower than 30 ℃.
6. The preservation method for the persistent organic contaminant sample monitored and analyzed in the environment as claimed in claim 1, wherein the vessel is an aluminum can or a brown glass bottle.
7. The preservation method for the persistent organic pollutant sample monitored and analyzed in the environment according to claim 1, wherein the methanol, the toluene and the dichloromethane are pesticide residue grade solvents.
8. The method for storing samples of persistent organic pollutants for environmental monitoring and analysis according to claim 1, wherein the vacuum packaging bag is a food grade packaging bag combining PE and PA.
9. A method for transporting samples of persistent organic pollutants for environmental monitoring and analysis, comprising the method for preserving samples of persistent organic pollutants for environmental monitoring and analysis according to claims 1 to 8.
10. A method for detecting samples of organic pollutants, comprising the method for preserving samples of persistent organic pollutants monitored and analyzed in an environment according to claims 1 to 8.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110698556.2A CN113310770A (en) | 2021-06-23 | 2021-06-23 | Preservation method for monitoring and analyzing persistent organic pollutant sample in environment |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110698556.2A CN113310770A (en) | 2021-06-23 | 2021-06-23 | Preservation method for monitoring and analyzing persistent organic pollutant sample in environment |
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|---|---|---|---|---|
| JP2009168202A (en) * | 2008-01-18 | 2009-07-30 | Panasonic Corp | Vacuum heat insulation box body |
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| CN101961649A (en) * | 2010-10-19 | 2011-02-02 | 同济大学 | Regeneration method of air sampling adsorbing agent |
| CN103418354A (en) * | 2012-05-22 | 2013-12-04 | 中国科学院生态环境研究中心 | Absorbent material used for collection of persistent organic pollutants in the atmosphere |
| CN105170116A (en) * | 2015-09-16 | 2015-12-23 | 中国科学院生态环境研究中心 | Preparation method of polyurethane sampling plate and passive adsorption sampling and detection method of organic phosphorus flame retardant |
| CN105466737A (en) * | 2015-12-29 | 2016-04-06 | 河海大学 | Passive sampler for gaseous polycyclic aromatic hydrocarbon in root box experiment and sample determining method thereof |
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2021
- 2021-06-23 CN CN202110698556.2A patent/CN113310770A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009168202A (en) * | 2008-01-18 | 2009-07-30 | Panasonic Corp | Vacuum heat insulation box body |
| JP2010022982A (en) * | 2008-07-23 | 2010-02-04 | Shinten Kogyo Kk | Method for preserving oil adsorbent |
| CN101961649A (en) * | 2010-10-19 | 2011-02-02 | 同济大学 | Regeneration method of air sampling adsorbing agent |
| CN103418354A (en) * | 2012-05-22 | 2013-12-04 | 中国科学院生态环境研究中心 | Absorbent material used for collection of persistent organic pollutants in the atmosphere |
| CN105170116A (en) * | 2015-09-16 | 2015-12-23 | 中国科学院生态环境研究中心 | Preparation method of polyurethane sampling plate and passive adsorption sampling and detection method of organic phosphorus flame retardant |
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| Title |
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