CN106053153B - Short chain chlorinated paraffin passive sampling material and preparation method thereof in a kind of air - Google Patents
Short chain chlorinated paraffin passive sampling material and preparation method thereof in a kind of air Download PDFInfo
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- CN106053153B CN106053153B CN201610346179.5A CN201610346179A CN106053153B CN 106053153 B CN106053153 B CN 106053153B CN 201610346179 A CN201610346179 A CN 201610346179A CN 106053153 B CN106053153 B CN 106053153B
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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
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
- G01N1/2273—Atmospheric sampling
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/025—Gas chromatography
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Abstract
The present invention relates to short chain chlorinated paraffin passive sampling materials and preparation method thereof in a kind of air, belong to ambient air and waste gas monitoring technical field.The passive sampling material is the polyurethane foam that load has carbowax-20M.The sampling quantity of passive sampling material of the present invention is 1.2 times of blank polyurethane foam disk, acquires C12、C13The relative abundance of short chain chlorinated paraffin is 1.1 times of blank polyurethane foam disk, 1.4 times respectively.
Description
Technical field
The present invention relates to short chain chlorinated paraffin passive sampling materials and preparation method thereof in a kind of air, belong to ambient air
And waste gas monitoring technical field.
Background technology
Persistence organic pollutant (POPs) cause global concern be because it has the environmental persistence that is difficult to degrade, it is long away from
From global transporting, bioconcentration and toxicity are (as having carcinogenicity, development toxicity, teratogenesis to have immune and reproduction poison
Property, male may be caused to feminize as incretion interferent).POPs is often through empty gas and water and migrates species and crosses over
The migration of international boundary is simultaneously deposited on the area far from its discharge sites, then terrestrial ecosystems there and ecology of water
Accumulation is got up in system.Although certain persistence organic pollutants have been forbidden producing, it still has in the environment, in water
There is detection in body, air, soil, and it carries out Transport And Transformation between environment hydrosphere, atmospheric thermodynamics and pedosphere.Combine within 2001
United Nations Environment Programme (UNEP) of state issues《Convention of Stockholm about persistence organic pollutant》.According to this pact, respectively conclude a treaty
State will take harmonious action, 12 class persistence organic pollutants be controlled first, respectively in organo-chlorine pesticide (OCPs)
DDT, hexachloro-benzene, Niran, mirex, poisoning phenol, Chinese mugwort reagent, dieldrite, endrin and heptachlor；Polychlorinated biphenyls
(PCBs)；More chloro dibenzo Dui bioxin and polychlorinated dibenzofurans (PCDD/Fs).2009 and 2011, " Si Dege
You rub pact " increase the toxic novel of 9 kinds and a kind serious harm human healths and natural environment in controlled list newly respectively
POPs, i.e.,：Perfluoro capryl carboxylic acid (PFOA), perfluoro octyl sulfonic acid and its salt (PFOS) and full-fluorine octyl sulfuryl fluoride (PFOS-F),
Pentabromo- Biphenyl Ether and octa-BDE (PBDEs), kepone, hexabromobiphenyl, lindane, pentachlorobenzene, α-hexachlorocyclohexanes, β-chlordene ring
Hexane and 5a,6,9,9a-hexahydro-6,9-methano-2,4, and carry out abatement and control in the world.2013 hexabromocyclododecane (HBCDs) also climb up《It closes
In the Convention of Stockholm of persistence organic pollutant》Disable the blacklist of chemicals.
Chlorinated paraffin (Chlorinated Paraffins, CPs) is that the n-alkane chloro of lineup's work synthesis derives
Object, formula CnH2n+2-mClm, chlorination degree usually between 30-70% (in mass).Not according to carbon chain lengths
Together, CPs can be divided into short chain chlorinated paraffin (Short-chain CPs, SCCPs, C10–13), middle chain chlorinated paraffin (Medium-
chain CPs,MCCPs,C14–17) and long-chain chlorinated paraffin (long-chain CPs, LCCPs, C>17).CPs has high stability
And the features such as low volatility, it is therefore widely used in fire retardant, the leather of metal working fluid, sealant, rubber and textile
In processing and coating.There is no the source of naturally-produced CPs in nature, CPs is mainly derived from related industries in surrounding medium
The production and use of product.CPs mass production and use since the nineteen thirties, by 1985, global yield was
Reach 300,000 tons, the annual output to the last century 90's Mo, SCCPs is about 50,000 tons.China is maximum CPs lifes in the world
It produces state and uses state, reach 410,000 tons to China's CPs productions in 2011.It is calculated according to the output of CPs, the environment of CPs
Storage is far above other POPs substances.For example, the global annual output of Polychlorinated biphenyls (PCBs) reached highest in 1970, it is 7.55
Ten thousand tons；2001 polybrominated diphenyl ethers (PBDEs) global annual output be about 6.7 ten thousand tons, and the annual output of current CPs both is total
6 times or more of sum.China's CPs products are defined with chlorinity, and the content of SCCPs is mainly by raw material and production technology shadow in product
It rings.Studies have reported that estimation China's SCCPs total emission volumns in 2011, close to 1800 tons, average speedup reaches 10% or more, to big
Gas discharge capacity is close to 500 tons.SCCPs is also referred to as short chain chlorination n-alkane, is that carbon chain lengths are 10 to 13 in chlorinated paraffin product
The product of a carbon atom.It contains 1 to 13 chlorine atom, and (about 16-78% is counted weight, molecular formula：CxH (2x-y+2) Cly, wherein x
=10-13, y=l-13).SCCPs be mainly used as metal working lubricant, paint, sealant, adhesive, plastic additive or
Person's fire retardant etc..From the last century 30's, chlorinated paraffin is just used as industrial products to produce, the toxicity research table of chlorinated paraffin
Its bright target organ includes liver, kidney and thyroid gland etc., and poisonous effect is related to chain length, and chain length is shorter, and toxicity is bigger.In recent years,
SCCPs is classified as the chemical products that limitation uses or forbids production by the U.S., Canada, European Union and Japan successively.SCCPs due to
With persistence, bioaccumulation, long-distance migration ability and toxicity, quilt《Si Degeer about persistence organic pollutant
It rubs pact》It adds as POPs candidate substances.Currently, related field expert carrying out short chain chlorinated paraffin (SCCPs) assessment with
Determine whether it discusses in next meeting and eventually enter into controlled list.Novel POPs, SCCPs are that current international environmental science is ground
The hot fields studied carefully, while the problem of environmental pollution caused by it is also a key factor for influencing China's Environmental security.It is empty
Gas is a kind of important surrounding medium, and SCCPs is to evaluation atmosphere quality, assessment SCCPs long range environment in monitoring air
The ecological risks of migration and evaluation SCCPs all have significance.Have to the monitoring of Atmospheric Organic Pollutants and actively samples
Technology and passive sampling technology.Active sampling instrument-volumes of air sampling instrument (High-volume air sampler) is for supervising
Survey the existing history for many years of POPs in air.These systems bypass air through filter membrane by sampling pump and collect particulate matter, pass through suction
It receives agent trap and collects gaseous substance.The problems of include that volatile materials surface particles volatilization collected by the filter membrane is received
Collecting object passes through absorbent trap, gas phase species to be adsorbed in filter membrane.In addition, actively sampled using the air that big flow sampler carries out
It is of high cost, it needs to guard at the time of power supply (power) and scientific research personnel, is not suitable for field and samples on a large scale.
Passively the sampling technique of POPs pollutants is paid high attention in the world in acquisition air in recent years.Air
Passive sampling technology can make up the defect of traditional actively sampling.Passive sampling technology is simple with sampler structure, price is low
It is honest and clean, easy to carry, do not need the features such as power supply, be very suitable for the multi-point acquisition of POPs air samples, therefore the technology was both fitted
The POPs Detection of Air Quality applied to small scale is closed, and is suitble to large scale, air POPs researchs.Passive sampler is situated between with environment
Fugacity difference between matter is driving force, and by spreading suction-operated, object is adsorbed by the material with high absorption capacity, is realized big
The acquisition of gas sample product.Difference based on sorbing material, Passive sampler are broadly divided into polyurethane foam (PUF) sampler, semi-transparent
Film (SPMD) sampler, XAD resin sampler further include with the plate of oil covering and diffuser absorption pollutant and plant
Monitoring.The major defect of diffuser and plate is their sampling quantities deficiency, is difficult to detect to low concentration compound in air, and
Food tray also acquires wet deposition.Many researchers are sampled using plant as Passive sampler, e.g., bark, moss or pine needle, in order to
Monitor large-scale organic pollution concentration in surrounding air, it is assumed that it is distributed and the close phase of concentration in air in plant
It closes.However, plant tissue sample size and sample rate change with floristics, age, position and season.Therefore, these
Be uncertain with the data that plant samples, and make to become complicated to the explanation of data, to limit using plant as
The potentiality of monitoring instrument.Absorption techniques can acquire larger volume air and concentrate target compound, therefore detectable Trace Species.
Need to be placed it in when SPMD sampler samples completely without reduced in any chemically treated wooden Stevenson casees temperature,
The influence of the environmental changes such as wind, frost, rain, snow, operation sequence are complicated.XAD resin sampler be it is a kind of utilize stryrene divinyl
Passive air sampling device of the base benzene copolymer XAD-2 powder as adsorbent, the disadvantage is that it is complicated, make with transport at
This costliness, cumbersome, sample rate is slow, limits its universal and application.When actively and passively sampling method acquires ring using PUF
In the air of border when CPs, because most PUF are in production added with not same amount, different types of CPs fire retardants, the pretreatment of PUF is outstanding
Its is important, and treatment effect quality influences the subsequent quantitative analysis of sample notable.The pretreated methods of PUF are mainly normal at present
Have with n-hexane/dichloromethane (1：1, v：V), multiple, large dosage, for a long time pretreatment of (e.g., 48,72h) Soxhlet extraction；
Or methanol (48h), acetone (for 24 hours) and the pretreatment of dichloromethane (for 24 hours) Soxhlet extraction；Or toluene (for 24 hours), acetone (8h) and toluene
(8h) Soxhlet extraction pre-processes；Soxhlet extraction waste of solvent amount is big, and time-consuming, and generates a large amount of toxic extraction waste liquid in ring
Border.Also have with accelerated solvent extraction, be the method that extractant carries out purified treatment to PUF with dichloromethane, acetone etc., add
Although quick-dissolving agent extraction Extraction solvent usage amount can reduce, because extraction pool volume it is small, PUF filling with take out when be easy by
It destroys, so that it cannot for sampling in next step.And leads to common simple PUF at present and sample disk, there are its samplings to hold
Measure it is small, some POPs be not achieved instrument detection limit, cannot detect；It is easy to reach saturation absorption, is unable to long-term linearity sampling etc.
Disadvantage.
The physicochemical property of SCCPs and poisonous effect be initially included in《Pact》12 class classics POPs and 2009,2011 Hes
2013, the novel POPs increased newly in " Convention of Stockholm " controlled list had larger difference, and there is presently no for this
The proprietary passive sampling material development report of substance.
Invention content
The present invention solves the above problem by the way that carbowax-20M to be supported in polyurethane foam.
The present invention provides short chain chlorinated paraffin passive sampling material in a kind of air, the passive sampling material is load
There is the polyurethane foam of carbowax-20M.
The weight of carbowax-20M of the present invention is preferably the 1-8% of polyurethane foam weight.
Another object of the present invention is to provide a kind of preparation method of above-mentioned passive sampling material, the preparation method is that will gather
Urethane foam impregnation is in carbowax-20M solution, and after solvent volatilization, aging obtains passive sampling material.
Carbowax-20M solution concentration of the present invention is preferably 0.1429-1.143g/L.
Aging temperature of the present invention is preferably 50 DEG C.
Ageing time of the present invention is preferably 30min.
Preparation method of the present invention further includes preferably polyurethane foam pre-treatment step；The polyurethane foam is located in advance
Managing step is：It is 1 that polyurethane foam, which is immersed in volume ratio,：In 1 n-hexane and dichloromethane mixed liquor, ultrasonic wave extraction,
Extracting solution is removed, the above-mentioned mixed liquor in polyurethane foam is volatilized, pretreated polyurethane foam is obtained.
Another object of the present invention is to provide a kind of above-mentioned passive sampling material short chain chlorinated paraffin in passive sampling air
In application.
Passive sampling material after present invention sampling preferably uses n-hexane Soxhlet extraction.
The present invention has the beneficial effect that：
1. the sampling quantity of passive sampling material of the present invention is 1.2 times of blank polyurethane foam disk.
2. passive sampling C acquired for materials of the present invention12、C13The relative abundance of short chain chlorinated paraffin is that blank is poly- respectively
1.1 times, 1.4 times of urethane foam disk.
Description of the drawings
4 width of attached drawing of the present invention,
Fig. 1 is the scanning electron microscope (SEM) photograph of passive sampling material prepared by embodiment 1；
Fig. 2 is the scanning electron microscope (SEM) photograph of blank polyurethane foam disk in application examples 1；
Fig. 3 is that measure within 1 month different carbon contents short for passive sampling material passive sampling that in application examples 1 prepared by embodiment 1
Chain chlorinated paraffin figure；
Fig. 4 is that blank polyurethane foam disk passive sampling measures different carbon content short chain chlorination stones for 1 month in application examples 1
Wax figure.
Specific implementation mode
Following non-limiting embodiments can make those skilled in the art be more fully understood the present invention, but not with
Any mode limits the present invention.
Following carbowax-20Ms are GC stationary liquid, and chromatographically pure grade is purchased from one factory of Shanghai reagent；
Following polyurethane foam disks are purchased from Beijing Sai Fulaibo Science and Technology Ltd.s, the polyurethane foam disc diameter
For 14.05cm, a height of 1.25cm, density 0.02437g/cm3。
Embodiment 1
The preparation method of short chain chlorinated paraffin passive sampling material in a kind of air, the preparation method include following step
Suddenly：
1. it is 1 that polyurethane foam disk, which is immersed in volume ratio,：1 n-hexane and 12h in dichloromethane mixed liquor, ultrasound
Wave extracts 1h, removes extracting solution, adds above-mentioned mixed liquor ultrasonic wave extraction 1h, removes extracting solution, is repeated 2 times, by polyurethane
Mixed liquor volatilization in foam disk, obtains pretreated polyurethane foam disk.
2. pretreated polyurethane foam disk to be immersed in the dichloromethane of the carbowax-20M of a concentration of 1.143g/L
In solution, after dichloromethane volatilization, 50 DEG C of aging 30min obtain short chain chlorinated paraffin passive sampling material in air, described poly-
The weight of ethylene glycol 20M is the 8% of polyurethane foam weight.
Application examples 1
The passive sampling material and quilt in blank polyurethane foam disk Mr. Yu research institute laboratory prepared using embodiment 1
Dynamic sampling 1 month, the passive sampling material after sampling is carried with 250mL n-hexane Soxhlets respectively with blank polyurethane foam disk
It takes for 24 hours, gas chromatography-mass spectrometry analysis will be used after extracting solution evaporation, concentration, purification, constant volume, it is acquired for materials to measure passive sampling
Short chain chlorinated paraffin total amount is 3810.0ng, and it is 3188.0ng that blank polyurethane foam disk, which acquires short chain chlorinated paraffin total amount,
Then the sampling quantity of passive sampling material is 1.2 times of blank polyurethane foam disk, is obtained by Fig. 3 and Fig. 4, passive sampling material is adopted
Collect C12、C13The relative abundance of short chain chlorinated paraffin is 1.1 times of blank polyurethane foam disk, 1.4 times respectively.
Claims (8)
1. short chain chlorinated paraffin passive sampling material in a kind of air, it is characterised in that：The passive sampling material is by poly- ammonia
Ester foam impregnation is in carbowax-20M solution, after solvent volatilization, aging；
The carbowax-20M solution concentration is 0.1429-1.143g/L；
The weight of the carbowax-20M is the 1-8% of polyurethane foam weight.
2. the preparation method of passive sampling material described in claim 1, it is characterised in that：The preparation method is that by polyurethane foam
Foam is immersed in carbowax-20M solution, and after solvent volatilization, aging obtains passive sampling material.
3. preparation method according to claim 2, it is characterised in that：The carbowax-20M solution concentration is 0.1429-
1.143g/L。
4. preparation method according to claim 2, it is characterised in that：The aging temperature is 50 DEG C.
5. preparation method according to claim 2, it is characterised in that：The ageing time is 30min.
6. preparation method according to claim 2, it is characterised in that：The preparation method further includes that polyurethane foam is located in advance
Manage step；The polyurethane foam pre-treatment step is：It is 1 that polyurethane foam, which is immersed in volume ratio,：1 n-hexane and dichloro
In methane blended liquid, ultrasonic wave extraction removes extracting solution, and the above-mentioned mixed liquor in polyurethane foam is volatilized, is pre-processed
Polyurethane foam.
7. application of the passive sampling material in passive sampling air in short chain chlorinated paraffin described in claim 1.
8. application according to claim 7, it is characterised in that：Passive sampling material after sampling is extracted using n-hexane.
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Citations (2)
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|---|---|---|---|---|
| CN102680284A (en) * | 2012-05-29 | 2012-09-19 | 大连交通大学 | Passive sampling device for persistent organic pollutants (POPs) in air |
| 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 |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN102680284A (en) * | 2012-05-29 | 2012-09-19 | 大连交通大学 | Passive sampling device for persistent organic pollutants (POPs) in air |
Non-Patent Citations (6)
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| 大气中持久性有机污染物的采样技术进展;朱青青等;《生态毒理学报》;20160415;第11卷(第2期);50-60 * |
| 持久性有机污染物的环境大气被动采样技术;朱秀华等;《环境化学》;20131031;第32卷(第10期);1957-1969 * |
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