CN105510484B - The device and method of phthalic acid ester content in a kind of detection gas - Google Patents
The device and method of phthalic acid ester content in a kind of detection gas Download PDFInfo
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- CN105510484B CN105510484B CN201610078992.9A CN201610078992A CN105510484B CN 105510484 B CN105510484 B CN 105510484B CN 201610078992 A CN201610078992 A CN 201610078992A CN 105510484 B CN105510484 B CN 105510484B
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- -1 phthalic acid ester Chemical class 0.000 title claims abstract description 63
- XNGIFLGASWRNHJ-UHFFFAOYSA-N o-dicarboxybenzene Natural products OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 238000000034 method Methods 0.000 title claims abstract description 22
- 238000001514 detection method Methods 0.000 title abstract description 33
- 238000001179 sorption measurement Methods 0.000 claims abstract description 54
- 239000003365 glass fiber Substances 0.000 claims abstract description 26
- 238000012360 testing method Methods 0.000 claims abstract description 18
- 239000003463 adsorbent Substances 0.000 claims abstract description 15
- 230000004888 barrier function Effects 0.000 claims abstract description 14
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 8
- 239000010959 steel Substances 0.000 claims abstract description 8
- 230000004913 activation Effects 0.000 claims abstract description 5
- 239000007789 gas Substances 0.000 claims description 58
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 46
- 238000005070 sampling Methods 0.000 claims description 38
- 239000012071 phase Substances 0.000 claims description 23
- 150000002148 esters Chemical class 0.000 claims description 22
- 238000011084 recovery Methods 0.000 claims description 19
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- 239000010410 layer Substances 0.000 claims description 16
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims description 15
- 229910052740 iodine Inorganic materials 0.000 claims description 15
- 239000011630 iodine Substances 0.000 claims description 15
- 239000000243 solution Substances 0.000 claims description 14
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 claims description 13
- 238000000605 extraction Methods 0.000 claims description 11
- 239000000126 substance Substances 0.000 claims description 11
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- 241000220324 Pyrus Species 0.000 claims description 3
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- 238000002604 ultrasonography Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 2
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- 229960004365 benzoic acid Drugs 0.000 claims 2
- 150000001335 aliphatic alkanes Chemical class 0.000 claims 1
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- 230000002034 xenobiotic effect Effects 0.000 abstract description 4
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 12
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 12
- 239000003570 air Substances 0.000 description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 8
- UHOVQNZJYSORNB-UHFFFAOYSA-N monobenzene Natural products C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 6
- 230000002000 scavenging effect Effects 0.000 description 5
- 239000002250 absorbent Substances 0.000 description 4
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
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- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 3
- 229920002554 vinyl polymer Polymers 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 241001465754 Metazoa Species 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 2
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- KBPLFHHGFOOTCA-UHFFFAOYSA-N caprylic alcohol Natural products CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 2
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- 235000013305 food Nutrition 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 206010062333 Congenital genital malformation Diseases 0.000 description 1
- 206010011498 Cryptorchism Diseases 0.000 description 1
- BDAGIHXWWSANSR-UHFFFAOYSA-N Formic acid Chemical class OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 1
- 208000031320 Teratogenesis Diseases 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000000443 aerosol Substances 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000002280 anti-androgenic effect Effects 0.000 description 1
- 239000000051 antiandrogen Substances 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
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- 239000013256 coordination polymer Substances 0.000 description 1
- 201000000160 cryptorchidism Diseases 0.000 description 1
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- 231100000025 genetic toxicology Toxicity 0.000 description 1
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- 239000008266 hair spray Substances 0.000 description 1
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- 206010021093 hypospadias Diseases 0.000 description 1
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- 231100000350 mutagenesis Toxicity 0.000 description 1
- 238000002703 mutagenesis Methods 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N n-Octanol Natural products CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 210000002307 prostate Anatomy 0.000 description 1
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Classifications
-
- 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
-
- 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some components
-
- 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
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The present invention relates to a kind of testing equipment and detection method, especially a kind of device and method for detecting phthalic acid ester content in gas.Device includes：Vavuum pump, exhaust tube, surge tank, particulate filter arrangement and adsorption tower, particulate filter arrangement is connected with adsorption tower, adsorption tower is connected with surge tank, vavuum pump is connected by exhaust tube with surge tank, horizontal in particulate filter arrangement to have the first porous barrier, and tiling has the glass fiber filter after activation on the first porous barrier, adsorption tower is at least one, it is horizontal in each adsorption tower to have the second porous barrier, stainless (steel) wire is provided with the second porous barrier, polymeric adsorbent is carried on stainless (steel) wire.It can make detectable concentration to the full extent close to actual concentration, be suitable for different detection environment, and sample introduction gas flow rate, flow can be made to keep stabilization, simple structure, it is easy to installation operation, is not easily introduced xenobiotic pollutants, also will not contaminated samples, it is not necessary to consume substantial amounts of organic solvent, it is more environmentally-friendly.
Description
Technical field
The present invention relates to phthalic acid ester content in a kind of testing equipment and detection method, especially a kind of detection gas
Device and method.
Background technology
Phthalic acid ester (Phthalate Esters, abbreviation PAEs), also known as phthalate ester, with aromatic odor, generally
It is the oily thick liquid of water white transparency, is insoluble in water, be soluble in the organic solvents such as methyl alcohol, ether, boiling point is higher, under normal temperature not
It is volatile.Phthalic acid ester is the maximum plasticizer of current usage amount, during plasticising, phthalic acid ester and polyolefin
Mainly merged with the physics of Van der Waals force rather than chemical bond by hydrogen bond, thus maintain independence each other between class plastic molecules
Chemical property, over time, easily dissolution and waved after plastic products touch the organic solvents such as grease or are heated
Hair, hence into surrounding air.Additionally, phthalic acid ester is the lipophilic organic pollution of a class, its property and side chain
Length it is relevant.With the increase of side chain lengths, the elevation of boiling point of phthalic acid ester, n-Octanol/Water Partition (Kow) subtracts
Small, saturated vapor pressure reduction, the larger phthalic acid ester of molecular weight has stronger absorption affinity, is easily adsorbed on particle
Thing and material surface.Phthalic acid ester has carcinogenic, teratogenesis, mutagenesis, with antiandrogen effect, to male grinding tooth
Animal has stronger genotoxicity, can cause in utero exposed male filial generation genital malformation, is mainly shown as that prostate is abnormal
Shape, hypospadia, cryptorchidism etc., can also disturb the internal system of humans and animals under extremely low concentration, cause Reproductive Performance to lose
Often.
Since the thirties in 20th century, phthalic acid ester is commonly used for the plasticizer of plastics particularly polyvinyl chloride (PVC),
It is added in polymer with the pliability and draftability of reinforcing material.Phthalic acid ester is the maximum plasticising of production and consumption amount
Agent, accounts for the 88% of plasticizer total output, have every year in the world millions of tons of phthalic acid ester be added in vinyl floors,
Wallpaper, toy, packaging material for food, medical blood bag and sebific duct, cleaning agent, personal-care supplies etc., such as nail polish, hair sprays
In hundreds of products such as agent, shampoo and bath foam.Content of the phthalic acid ester in plastic products is general 10~60%
In the range of.Because phthalic acid ester is using extensive, also often it is measured in water, soil, air, food and human body, this meaning
Taste it has turned into universal environmental contaminants.Influence and ecological environment due to phthalic acid ester to health it is broken
Bad, phthalic ester concentration is just particularly important in investigating and analyzing various media.At present both at home and abroad to adjacent benzene in air
The sampling of diformic ester relates generally to the collection of gas phase, is not enriched with Gas and particles PAEs all, causes to interior
Phthalic acid ester level of pollution is underestimated.The foundation of the detection method of phthalic acid ester content and the research and development of device in gas
Allow us to detect it, can accurately determine the concentration level of phthalic acid ester in air, for research is dirty
The source and transportion and transformation for contaminating thing are laid a good foundation.
The detection of PAEs concentration is mainly enriched with using ionic liquid dispersion liquid-liquid microextraction method in liquid, then is used
HS GC-mass spectrum is used in conjunction the PAEs in method detection pregnant solution.The detection method of PAEs concentration is usually to consolidate in solid
Body sample treatment carries out microwave abstracting into being put into after little particle in mixed liquor of the hexane with acetone, and the solution after extraction is carried out again
GC-MS is analyzed.The detection method of PAEs concentration mainly has following several in conventional gas：Micro-porous filter is usually used in big compression ring
Border or the collection of large space endoparticle thing, are not particularly suited for that concentration is relatively low, sampling time room air sample more long；Solvent is inhaled
Receipts method is usually used in gathering the gaseous state or vaporous material in air, also can the aerosol that is coexisted with it of collecting part；Activated carbon tube
Method is applied to a small range air and investigates sampling.Pretreatment link is frequently with soxhlet's extraction or ultrasonic extraction mode, extractant
Mainly there are methyl alcohol, dichloromethane/acetone (1:1, v:V) and dichloromethane, analysis method is generally capillary column and carries out chromatogram point
Analysis.
Existing testing equipment is not high with the accumulation rate of solid phase phthalic acid ester to gas phase in gas, causes sampling efficiency
It is relatively low, error is also easy to produce, influence testing result.When collecting solid phase phthalic acid ester using organic solvent immersion miillpore filter,
Organic solvent volatilization reduces sampling efficiency, and the method is usually used in atmospheric environment or larger space solid-state O-phthalic in gas
The collection of acid esters, is not particularly suited for that phthalic ester concentration is relatively low, sampling time room air sample more long.Using solvent
During enriched gas phase phthalic acid ester, solvent is generally organic solvent, with larger volatility, is also easy to produce low precision, sampling
The low problem of rate, as shown by data, with the traffic sampling 1h of 1L/min, sampling efficiency is about 50%-60%, and detection is limited to
1.32ug/m3.During using activated carbon collection and centrifugation, due to reasons such as little particle activated carbon losses, neighbour is easily caused
The loss of phthalic acid ester, sampling rate is 1L/min, and the sampling time is about 3d, and the sampling time is more long, and sample recovery rate is not high.
The detection method of phthalic acid ester content often collects gas-particle two-phase using additional traffic sampling device in other gas
Sample, but same equipment can not carry out specific qualitative and quantitative detection for different detection environment, cause the detection of sample not
With generality, the sampler of different model need to be constantly changed, therefore the sample devices such as sampler is excessive, sampling process is excessively numerous
Trivial, sampling efficiency is low, complex operation step, and Detection results of wasting time and energy are bad, and testing cost is high, additionally, the flow velocity of turnover sample,
Flow, pressure are non-constant, are easily influenceed by external environments such as temperature, humidity, wind directions, and testing result poor reproducibility, sensitivity is not high,
Sample range is limited to.
Existing testing equipment is typically enriched with phthalic acid ester using organic solvent, can be consumed in sample pretreatment process
A large amount of organic solvents, organic solvent volatilizees and toxicity is larger, waste of solvent is caused, while also being polluted to environment.
When using pipeline air-inlet or collecting sample using gas sampling box etc., equipment is plastic products, may contain adjacent benzene
Diformic ester plasticizer, sample collection process can bring new pollutant into, as pollution sources, cause the secondary pollution of sample,
Influence the accuracy of detection data.
The content of the invention
Present invention seek to address that above mentioned problem, there is provided the detection means of phthalic acid ester content and side in a kind of gas
Method, its one side adsorption rate is up to more than 95%, and accuracy is high, can make detectable concentration to the full extent close to actual concentration,
On the one hand different detection environment are suitable for, sample introduction gas flow rate, flow can be made to keep stabilization, device structure is simple, it is easy to pacify
Dress operation, testing cost is low, and scavenging period is short, and practicality and versatility are stronger, and another further aspect is not easily introduced xenobiotic pollutants,
Will not contaminated samples, using Resin Absorbent gas phase PAEs, it is not necessary to consume substantial amounts of organic solvent, more environmentally-friendly, cost performance is higher,
The technical scheme that it is used is as follows：
The device of phthalic acid ester content in a kind of detection gas, it is characterised in that including：It is vavuum pump, exhaust tube, slow
Tank, particulate filter arrangement and adsorption tower are rushed, the adsorption tower is at least one, then from top to bottom detachably connects successively when being multiple
Connect；The particulate filter arrangement bottom is connected with the top side detachable of the adsorption tower positioned at the top, positioned at the absorption of bottom
The bottom of tower is connected with surge tank, and the vavuum pump is connected by exhaust tube with surge tank, in the particulate filter arrangement
Horizontal to have the first porous barrier, tiling has the glass fiber filter after activation on first porous barrier, in each adsorption tower
It is horizontal to have the second porous barrier, stainless (steel) wire is provided with second porous barrier, suction is carried on the stainless (steel) wire
Attached resin.
On the basis of above-mentioned technical proposal, also including flowmeter and escaping pipe, the flowmeter passes through escaping pipe and vacuum
Pump is connected.
On the basis of above-mentioned technical proposal, the particulate filter arrangement and adsorption tower are made by metal material.
On the basis of above-mentioned technical proposal, the adsorption tower totally three passes through screwed connection between upper and lower adsorption tower.
A kind of method of phthalic acid ester content in utilization said apparatus detection gas, it is characterised in that including as follows
Step：
A) sample collection and keeping:The glass fiber filter for having weighed quality in advance is put into particulate filter arrangement, will
The polymeric adsorbent after purification for having weighed quality in advance is put into adsorption tower, vavuum pump is opened, with default sampling flow, sampling
Time, height of sampling are sampled, and the parameters such as temperature, humidity, flow are recorded while sampling, after sampling terminates, aluminium are used at once
Paper tinsel is sealed glass fiber filter and polymeric adsorbent, takes back laboratory treatment, and -4 DEG C of refrigerators are stored in if treatment is had little time
In, the resting period is no more than 7 days；
B) sample pretreatment:The solid phase extracted using sonic oscillation extraction method in glass fiber filter and polymeric adsorbent is gentle
Phase phthalic acid ester；
C) Concentration Testing:Determined with GC methods and analyze phthalic acid ester content in sample.
On the basis of above-mentioned technical proposal, the step b) sample pretreatments include：
The pretreatment of glass fiber filter：
Glass fiber filter is cut into square of the length of side less than 2mm, the precise on assay balance with sharp scissors
Quality, is transferred in the iodine flask for cleaning drying.The analytically pure n-hexane 20ml for having rotated is measured with graduated cylinder, iodine number is added to
In bottle, then 1ml benzoic acid Bian ester standard solution is added thereto to as the standard substance for calculating recovery of standard addition, cover bottle
Plug, shakes up；
Iodine flask is placed on ultrasonic cleaner, is cleaned by ultrasonic 30min and is taken out, it is different in order to reduce temperature during extraction
The interference for causing, temperature is set as a definite value during extraction, after ultrasound terminates, the extract solution filtering of taking-up is transferred to corresponding
In triangular flask, then so carried again three times with same n-hexane, 10mL is added every time, rinse complete, extract solution is transferred to triangle
In bottle；
By sample extracting solution in filter suction filtration, and with a small amount of n-hexane rinse, filtrate is transferred to pear-shaped flask
In, and cleaned more than 3 times with n-hexane, will wash during rear solution integrates with pear-shaped flask, rotated at 35 DEG C at least in 1ml, stop
Spin-ended steaming, is finally transferred in chromatogram bottle with special microsyringe, and cleans pear-shaped flask with a small amount of chromatographically pure n-hexane,
N-hexane after being washed with microsyringe is extracted out and is transferred in chromatogram bottle, repeats aforesaid operations more than 3 times, is finally settled to
1.5mL, labels after adding a cover and is put into freezer storage；
The pretreatment of polymeric adsorbent：
The resin that will be reclaimed precise 0.2000g on assay balance, is accurate to 0.0001g, is transferred to clean drying
Iodine flask in, the analytically pure n-hexane 20ml for having rotated is measured with graduated cylinder, be added in iodine flask, then be added thereto to
1ml benzoic acid Bian ester standard solution covers bottle stopper as the standard substance for calculating recovery of standard addition, shakes up；
Subsequent operations are identical with the pretreatment of glass fiber filter.
On the basis of above-mentioned technical proposal, after the step c) Concentration Testings are to place one day, sample is taken out from refrigerator,
Sufficient standing makes impurity precipitate completely, extracts supernatant with microsyringe and injects all-glass syringe, is filtered with disposable aspiration needle
Device is filtered into another correspondence chromatogram bottle, is added a cover and is placed into refrigerator, finally determines analysis phthalic acid ester content with GC methods.
On the basis of above-mentioned technical proposal, the chromatogram bottle soaks a period of time before with washing lotion, cleans drying,
In Muffle furnace 4h is activated at 450 DEG C.
Beneficial effects of the present invention are as follows：First, the PAEs in gaseous sample in the presence of three-level adsorption tower can be complete
Full absorption, adsorption rate reduces the error of detection data up to more than 95%, improves accuracy, makes detectable concentration at utmost
On close to actual concentration.
2nd, surge tank can make the different detection environment of device adaptation with the installation of flowmeter, make sample introduction gas flow rate, stream
Amount keeps stabilization, can shorten scavenging period, improves cleaning efficiency, improves detection data accuracy, and assay device structures are simple,
Operation is easily installed, testing cost is reduced, shortens scavenging period, practicality and versatility are stronger.
3rd, particulate filter arrangement and adsorption tower are welded by stainless steel tube, are not easily introduced xenobiotic pollutants, also will not
Contaminated samples, using Resin Absorbent gas phase PAEs, it is not necessary to consume substantial amounts of organic solvent, the device is more environmentally-friendly, and cost performance is more
It is high.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
The accompanying drawing to be used needed for having technology description is briefly described.It should be evident that drawings in the following description are only this
A kind of embodiment of invention, for those of ordinary skill in the art, on the premise of not paying creative work, can be with
Accompanying drawing according to providing is extended and obtains other implementation accompanying drawings.
Fig. 1：The structure of the device of phthalic acid ester content is shown in a kind of detection gas of one embodiment of the present of invention
It is intended to；
Fig. 2：The structural representation of the particulate filter arrangement of one embodiment of the present of invention；
Fig. 3：The structural representation of the adsorption tower of one embodiment of the present of invention；
Specific embodiment
The invention will be further described with example below in conjunction with the accompanying drawings：
Embodiments of the invention are described below in detail, the example of the embodiment is shown in the drawings, wherein from start to finish
Same or similar label represents same or similar element or the element with same or like function.Below with reference to attached
It is exemplary to scheme the embodiment of description, is only used for explaining the present invention, and is not considered as limiting the invention.
In the description of the invention, it is to be understood that term " on ", the orientation of the instruction such as D score be all based on specification
What the orientation shown in accompanying drawing Fig. 1 was defined, it is for only for ease of and describes of the invention and simplify description, rather than instruction or hint
Signified device or element must have specific orientation, with specific azimuth configuration and operation, therefore it is not intended that to this
The limitation of invention.
In the description of the invention, it is necessary to illustrate, unless otherwise clearly defined and limited, term " installation ", " phase
Company ", " connection " should be interpreted broadly, for example, it may be being fixedly connected, or being detachably connected, or be integrally connected；Can
Being to be joined directly together, it is also possible to be indirectly connected to by intermediary.For the ordinary skill in the art, can be specific
Situation understands above-mentioned term concrete meaning in the present invention.
As shown in Figure 1 to Figure 3, in a kind of detection gas of the present embodiment phthalic acid ester content device, its feature
It is, including：Vavuum pump 1, exhaust tube 2, surge tank 3, particulate filter arrangement 4 and adsorption tower 5, the adsorption tower 5 are at least one
It is individual, then from top to bottom it is detachably connected successively when being multiple；The bottom of the particulate filter arrangement 4 and the adsorption tower for being located at the top
5 top side detachable connection, the bottom positioned at the adsorption tower 5 of bottom is connected with surge tank 3, preferably selects, on surge tank 3
A connecting tube communicated with the inner chamber of surge tank 3 is welded with, the bottom positioned at the adsorption tower 5 of bottom is connected with connecting tube by screw thread
Connect, the vavuum pump 1 is connected by exhaust tube 2 with surge tank 3, in the particulate filter arrangement 4 it is horizontal have first it is porous every
Plate 40, tiling has the glass fiber filter after activation on first porous barrier 40, horizontal in each adsorption tower 5 to have second
Porous barrier 50, is provided with stainless (steel) wire on second porous barrier 50, polymeric adsorbent is carried on the stainless (steel) wire (such as
XAD -2 resin).
The particulate filter arrangement 4 is preferably designed as infundibulate.
Preferably, also including flowmeter 6 and escaping pipe 7, the flowmeter 6 is connected by escaping pipe 7 with vavuum pump 1.
Surge tank can make the different detection environment of device adaptation with the installation of flowmeter, sample introduction gas flow rate, flow is kept stabilization,
Influence of the environmental change to sampling is reduced, scavenging period can be shortened, improve cleaning efficiency, improve detection data accuracy, inspection
Measurement equipment simple structure, it is easy to installation operation, reduces testing cost, shortens scavenging period, practical.
Preferably, the particulate filter arrangement 4 and adsorption tower 5 are made by metal material.It is preferred that be made of stainless steel,
But this is not limited only to, xenobiotic pollutants is not easily introduced so, also will not contaminated samples.
Preferably, the adsorption tower 5 totally three, they are that primary adsorption tower 5-1, secondary absorption tower 5-2 and three-level are adsorbed
Tower 5-3, by screwed connection between upper and lower adsorption tower, on the one hand the mode of screwed connection can ensure the compactness of connection, another
Aspect is easy to dismounting and polymeric adsorbent and is taken out with facilitating to be placed in adsorption tower.
A kind of method of phthalic acid ester content in utilization said apparatus detection gas, it is characterised in that including as follows
Step：
A) sample collection and keeping:The glass fiber filter (diameter 37mm, 0.45 μm of aperture) of quality will in advance have been weighed
It is put into particulate filter arrangement 4,2.0g polymeric adsorbents after purification is put into adsorption tower 5, opens vavuum pump 1, sampling flow
1.0L/min, sampling time 3-5h, height of sampling 0.5m, record the parameters such as temperature, humidity, flow, sampling knot while sampling
Shu Hou, is at once sealed glass fiber filter and polymeric adsorbent with aluminium foil, takes back laboratory treatment, if treatment is had little time
It is stored in -4 DEG C of refrigerators, the resting period is no more than 7 days；
B) sample pretreatment:
The pretreatment of glass fiber filter：
Glass fiber filter is cut into square of the length of side less than 2mm, the precise on assay balance with sharp scissors
Quality, is transferred in the 150ml iodine flasks for cleaning drying.The analytically pure n-hexane 20ml for having rotated is measured with graduated cylinder, is added
To in iodine flask, then 1ml benzoic acid Bian ester standard solution is added thereto to as the standard substance for calculating recovery of standard addition, lid
Good bottle stopper, shakes up；
Iodine flask is placed on ultrasonic cleaner, is cleaned by ultrasonic 30min and is taken out, it is different in order to reduce temperature during extraction
The interference for causing, temperature is set as 25 degree, after ultrasound terminates during extraction, and the extract solution filtering of taking-up is transferred into corresponding triangle
In bottle, then so carried again three times with same n-hexane, 10mL is added every time, rinse complete, extract solution is transferred in triangular flask；
By sample extracting solution in filter suction filtration, and with a small amount of n-hexane rinse, filtrate is transferred to the pears of 150mL
In shape flask, and cleaned more than 3 times with n-hexane, will washed during rear solution integrates with pear-shaped flask, rotated at 35 DEG C at least in
1ml, stops revolving, is finally transferred in chromatogram bottle with special microsyringe, and clean pears with a small amount of chromatographically pure n-hexane
Shape flask, the n-hexane after being washed with microsyringe is extracted out and is transferred in chromatogram bottle, repeats aforesaid operations more than 3 times, finally
1.5mL is settled to, is labelled after adding a cover and is put into freezer storage；
The pretreatment of polymeric adsorbent：
The resin that will be reclaimed precise 0.2000g on assay balance, is accurate to 0.0001g, is transferred to clean drying
150ml iodine flasks in, the analytically pure n-hexane 20ml for having rotated is measured with graduated cylinder, be added in iodine flask, then thereto
Add 1ml benzoic acid Bian ester standard solution as the standard substance for calculating recovery of standard addition, cover bottle stopper, shake up；
Subsequent operations are identical with the pretreatment of glass fiber filter；
C) Concentration Testing:After placing one day, sample is taken out from refrigerator, sufficient standing makes impurity precipitate completely, with micro
Injector extracts supernatant injection all-glass syringe, is filtered into another correspondence chromatogram bottle with disposable aspiration needle filter, adds a cover
Refrigerator is placed into, finally analysis phthalic acid ester content is determined with GC methods.Further, the chromatogram bottle uses washing lotion before
Immersion a period of time, drying is cleaned, activate 4h at 450 DEG C in the Muffle furnace.
Assay method Recovery test
Agents useful for same medicine：
N-hexane：Analyze pure (AR), content >=98.0%, after purification is rotated on Rotary Evaporators 80 DEG C, pour into dry
It is stand-by in net brown reagent bottle.
N-hexane：Chromatographically pure (HPLC), content >=99.5%.
Benzoic acid Bian ester：Chemical pure (CP), density 1.116-1.120, content >=99.0%.
AmberiiteXAD-2 macroreticular resins：Acetone soak, successively with dichloromethane, methyl alcohol on apparatus,Soxhlet's constant temperature
More than refluxing extraction 24h, dries removal organic solvent, sealing preserve.
Glass fiber filter：Diameter 37mm, 0.45 μm of aperture, the preceding 450 DEG C of activation 4h in Muffle furnace of sampling, aluminium-foil paper is close
Envelope is preserved.
Methyl alcohol：Analyze pure (AR), content >=99.5%.
Dichloromethane：Analyze pure (AR), content >=99.5%.
Acetone：Analyze pure (AR), content >=99.5%.
16 kinds of mixed mark 1000mg/L of phthalic acid ester, are shown in Table 1
Table 1 determines 16 kinds of mixed mark species and purity of phthalate compound
GC conditions：
Carrier gas (nitrogen), air generator, hydrogen generator, gas chromatograph are opened in sequence, and are connected with computer
Success, gas chromatograph qualitative method is set by following condition, is determined.
Agilent 7820A GC, DB-5 fused-silica capillary column (30m × 0.32mm × 0.25 μm, U.S. J＆W
Scientific), flame photometric detector (FID).
Temperature programming：140 DEG C of initial temperature, retention time 1min, the first stage is with 20 DEG C of min-1Rise to 235 DEG C and protect
0.5min is held, second stage is with 2 DEG C of min-1Rise to 240 DEG C and keep 0.5min, the phase III is with 5 DEG C of min-1Rise to 280
DEG C and keep 2.5min.
260 DEG C of injector temperature, 300 DEG C of detector temperature；
Highest post case temperature：325℃；
Detector：Flame photometric detector (FID)；
Chromatographic column：DB-5 fused-silica capillary columns (30m × 0.32mm × 0.25 μm), J＆W Co, USA.
Carrier gas：High Purity Nitrogen (purity N2>=99.999%)
Sample size：1 μ L, Splitless injecting samples, column flow 1mLmin-1。
It is qualitative：It is defined by the relative retention time of standard substance, the plastic sample time is 25min
The measure of phthalic acid ester：With in the quantitative sample of the ratio of peak area in external standard method and standard external standard peak area
The content of each object.
Rate of recovery indicator：100mg·L-1Ergol.
After the completion of sample pre-treatments, the chromatogram bottle that will be equipped with sample is placed in specified location, waits to be determined.After the completion of measure,
Bring into graticule to measure the content and total content of each esters by the integration to collection of illustrative plates peak area.
The method rate of recovery
0.5mL concentration is separately added on blank AmberiiteXAD-2 macroporous absorbent resins and glass fiber filter is
The mixed marks of the PAEs of 4mg/L with n-hexane as extractant, 30min are extracted using excusing from death extraction mode using liquid (16 kinds of mixed marks), are put down
Row five times, does rate of recovery experiment.Every time using blank experiment, the rate of recovery of every kind of object under the conditions of this is determined, and count
Relative standard deviation is calculated, be the results are shown in Table shown in 2, table 3.
The rate of recovery (%) of the gas phase PAEs of table 2
The rate of recovery (%) of the particle phase PAEs of table 3
From table 1 it follows that 6 kinds of gas phase PAEs rate of recovery be respectively 89.12 ± 6.41%, 87.08 ± 2.82%,
85.18 ± 4.47%, 82.80 ± 7.56%, 82.00 ± 6.25%, 93.70 ± 8.75%, the average recovery rate of 16 kinds of esters is
88.06±2.62；From Table 2, it can be seen that the rate of recovery of 6 kinds of particle phase PAEs be respectively 87.22 ± 7.47%, 86.80 ±
4.08%th, 82.90 ± 4.84%, 82.80 ± 9.56%, 85.93 ± 6.12%, 85.30 ± 9.3%, 16 kinds of esters it is average
The rate of recovery is 85.30 ± 5.54%.Precision RSD<10.0%, illustrate that this analysis method is feasible.
Adsorption tower penetrability is tested
Respectively in the morning, afternoon, three period samplings of night same vinyl house, using three layers of absorption during sampling
Gas phase phthalic acid ester in tower absorption air, during three layers of adsorption tower are detected respectively resin to the adsorbance of phthalic acid ester,
Compare PAEs contents in three layers of adsorption tower resin and its account for the ratio of total adsorbance, the results are shown in Table shown in 4.
PAEs contents (μ g/m in the resin of table 43)
As can be seen from the table, the morning, afternoon and the total concentration of gas phase phthalic acid ester is respectively in night gas
204.72、235.40、148.50μg/m3, it is seen that rate of release influence of the temperature on phthalic acid ester in vinyl house canopy film
Significantly.For three layers of adsorption tower, when gas is gathered by ground floor resin, the PAEs for having more than 90% is adsorbed, the morning,
The PAEs accountings example of ground floor adsorption tower retention is respectively in three treatment of afternoon and night：91.01%th, 90.70%,
99.19%.When gas is gathered by first and second layer of resin, the PAEs for having more than 96% is adsorbed, the morning, afternoon and night
The PAEs accountings example sum of first and second layer of adsorption tower retention is respectively in three treatment：97.26%th, 96.90%, 100.00%.
And with the increase of phthalic ester concentration in gas, ground floor ratio of adsorption reduces, the increase of third layer ratio of adsorption, therefore
When in gas gas phase phthalic ester concentration it is higher (concentration be more than 250 μ g/m3) when use three layers of adsorption tower, when gas in gas
Phase phthalic ester concentration is relatively low, and (concentration is less than 150 μ g/m3) when using one layer or two-layer adsorption tower just enough.
Phthalic ester concentration detection in gas under varying environment
Using the detection means of the application respectively in campus, No. 1 canopy, three sampling point samplings of No. 2 canopies, wherein No. 1 canopy is
Old canopy film, No. 2 canopies change canopy film for new, and detection means is using particulate filter arrangement and glass fiber filter filtering solid phase particles shape
Phthalic acid ester, using gas phase phthalic acid ester in three layers of adsorption tower and Resin Absorbent air, detects glass fibre respectively
The content of the phthalic acid ester in filter membrane and three layers of adsorption tower in resin, calculates the ratio that each several part is accounted for, and the results are shown in Table 5 institutes
Show.
The different sample point testing results of table 5
From the testing result of table 5, phthalic acid ester is made up of solid phase (graininess) and gas phase two parts in air, Gu
Phase phthalic acid ester can be filtered by glass fiber filter, and its content accounts for the 5-10% of total content in gas.Gas phase neighbour's benzene two
Formic acid esters can be by resin adsorption, and its content accounts for the 90-95% of total content in gas, wherein ground floor can be inhaled in three layers of adsorption tower
More than the 85% of phthalic acid ester total amount in attached gas, the 1-5% of phthalic acid ester total amount in the adsorbable gas of the second layer,
1% of third layer adsorbance less than phthalic acid ester total amount in gas.In campus, No. 1 canopy, three sampled point gases of No. 2 canopies
Phthalic ester concentration is respectively 16.30,37.68,215.03 μ g/m3, analyzed more than, when O-phthalic in gas
Acid esters concentration is less than 200 μ g/m3, the invention device and method can be used.
The present invention is described by way of example above, but the invention is not restricted to above-mentioned specific embodiment, it is all to be based on
Any change or modification that the present invention is done belong to the scope of protection of present invention.
Claims (7)
1. it is a kind of detect gas in phthalic acid ester content device, it is characterised in that including：Vavuum pump (1), exhaust tube
(2), surge tank (3), particulate filter arrangement (4) and adsorption tower (5), the adsorption tower (5) are at least one, when being multiple then by
It is detachably connected successively under up to；Particulate filter arrangement (4) bottom is removable with the top of the adsorption tower (5) positioned at the top
Connection is unloaded, the bottom positioned at the adsorption tower (5) of bottom is connected with surge tank (3), the vavuum pump (1) is by exhaust tube
(2) it is connected with surge tank (3), horizontal in the particulate filter arrangement (4) to have the first porous barrier (40), described first is porous
Tiling has the glass fiber filter after activation on dividing plate (40), horizontal in each adsorption tower (5) to have the second porous barrier (50),
Stainless (steel) wire is provided with second porous barrier (50), polymeric adsorbent, the particle mistake are carried on the stainless (steel) wire
Filter device (4) and adsorption tower (5) are made by metal material, when gas phase phthalic ester concentration is less than 150 μ g/m in gas3
Mono- layer of Shi Caiyong or two-layer adsorption tower.
2. it is according to claim 1 it is a kind of detect gas in phthalic acid ester content device, it is characterised in that：Also wrap
Flowmeter (6) and escaping pipe (7) are included, the flowmeter (6) is connected by escaping pipe (7) with vavuum pump (1).
3. it is according to claim 2 it is a kind of detect gas in phthalic acid ester content device, it is characterised in that：It is described
Adsorption tower (5) totally three, passes through screwed connection between upper and lower adsorption tower.
4. a kind of method that device using as described in any one of claims 1 to 3 detects phthalic acid ester content in gas,
It is characterised in that it includes following steps：
A) sample collection and keeping:The glass fiber filter for having weighed quality in advance is put into particulate filter arrangement (4), will be pre-
The polymeric adsorbent after purification for first having weighed quality is put into adsorption tower (5), vavuum pump (1) is opened, with sampling flow 1.0L/
Min, sampling time 3-5h, height of sampling 0.5m are sampled, and temperature, humidity, flow parameter, sampling knot are recorded while sampling
Shu Hou, is at once sealed glass fiber filter and polymeric adsorbent with aluminium foil, takes back laboratory treatment, if treatment is had little time
It is stored in -4 DEG C of refrigerators, the resting period is no more than 7 days；
B) sample pretreatment:The solid phase extracted using sonic oscillation extraction method in glass fiber filter and polymeric adsorbent is gentle adjacent
Phthalic acid ester；
C) Concentration Testing:Determined with GC methods and analyze phthalic acid ester content, GC conditions in sample：Open in sequence
Carrier gas, air generator, hydrogen generator, gas chromatograph, and be connected with computer, after success, set by following condition：Program
Heat up：140 DEG C of initial temperature, retention time 1min, the first stage is with 20 DEG C of min-1Rise to 235 DEG C and keep 0.5min, the
Two-stage is with 2 DEG C of min-1Rise to 240 DEG C and keep 0.5min, the phase III is with 5 DEG C of min-1Rise to 280 DEG C and keep
2.5min；Injector temperature：260 DEG C, detector temperature：300℃；Highest post case temperature：325℃；
Detector：Flame photometric detector；Chromatographic column：DB-5 fused-silica capillary columns, size is 30m × 0.32mm × 0.25
μm；Carrier gas：High Purity Nitrogen, purity N2>=99.999%；Sample size：1 μ L, Splitless injecting samples, column flow 1mLmin-1；It is qualitative：
It is defined by the relative retention time of standard substance, the plastic sample time is 25min；The measure of phthalic acid ester：With external standard method
Middle peak area quantifies the content of each object in sample with the ratio of standard external standard peak area；Rate of recovery indicator：100mg·
L-1Ergol.
5. it is according to claim 4 it is a kind of detect gas in phthalic acid ester content method, it is characterised in that：It is described
Step b) sample pretreatments include：
The pretreatment of glass fiber filter：Glass fiber filter is cut into square of the length of side less than 2mm with sharp scissors, is being divided
Precise quality on analysis balance, is transferred in the iodine flask for cleaning drying；Measured with graduated cylinder rotated it is analytically pure just oneself
Alkane 20ml, is added in iodine flask, then is added thereto to 1ml benzoic acid Bian ester standard solution as calculating recovery of standard addition
Standard substance, covers bottle stopper, shakes up；Iodine flask is placed on ultrasonic cleaner, is cleaned by ultrasonic 30min and is taken out, in order to subtract
The interference that temperature difference is caused when extracting less, temperature is set as a definite value during extraction, after ultrasound terminates, the extract solution that will be taken out
Filtering is transferred in corresponding triangular flask, then is so carried again three times with same n-hexane, and 10mL is added every time, rinses complete,
Extract solution is transferred in triangular flask；By sample extracting solution in filter suction filtration, and with a small amount of n-hexane rinse, by filtrate turn
In moving to pear-shaped flask, and cleaned more than 3 times with n-hexane, will washed during rear solution integrates with pear-shaped flask, rotated at 35 DEG C
To 1ml is less than, stop revolving, be finally transferred in chromatogram bottle with microsyringe, and pears are cleaned with a small amount of chromatographically pure n-hexane
Shape flask, the n-hexane after being washed with microsyringe is extracted out and is transferred in chromatogram bottle, repeats aforesaid operations more than 3 times, finally
1.5mL is settled to, is labelled after adding a cover and is put into freezer storage；
The pretreatment of polymeric adsorbent：
The resin that will be reclaimed precise 0.2000g on assay balance, is accurate to 0.0001g, is transferred to the iodine for cleaning drying
In measuring bottle, the analytically pure n-hexane 20ml for having rotated is measured with graduated cylinder, be added in iodine flask, then be added thereto to 1ml benzene
Formic acid Bian ester standard solution covers bottle stopper as the standard substance for calculating recovery of standard addition, shakes up；Subsequent operations and glass fibers
The pretreatment for tieing up filter membrane is identical.
6. it is according to claim 5 it is a kind of detect gas in phthalic acid ester content method, it is characterised in that：It is described
After step c) Concentration Testings are to place one day, sample is taken out from refrigerator, sufficient standing makes impurity precipitate completely, uses micro-sampling
Device extracts supernatant injection all-glass syringe, is filtered into another correspondence chromatogram bottle with disposable aspiration needle filter, adds a cover and puts again
Enter refrigerator, finally determine analysis phthalic acid ester content with GC methods.
7. it is according to claim 6 it is a kind of detect gas in phthalic acid ester content method, it is characterised in that：It is described
Chromatogram bottle soaks a period of time before with washing lotion, cleans drying, activates 4h at 450 DEG C in the Muffle furnace.
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| CN110274991B (en) * | 2019-03-15 | 2022-02-22 | 暨南大学 | Evaluation method for phthalate absorption of greenhouse vegetables and application of evaluation method in human health risk prediction |
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