CN205562482U - Device of phthalate content among tracer gas - Google Patents
Device of phthalate content among tracer gas Download PDFInfo
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- CN205562482U CN205562482U CN201620113706.3U CN201620113706U CN205562482U CN 205562482 U CN205562482 U CN 205562482U CN 201620113706 U CN201620113706 U CN 201620113706U CN 205562482 U CN205562482 U CN 205562482U
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- Prior art keywords
- adsorption tower
- acid ester
- phthalic acid
- particulate filter
- porous barrier
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- XNGIFLGASWRNHJ-UHFFFAOYSA-L phthalate(2-) Chemical compound [O-]C(=O)C1=CC=CC=C1C([O-])=O XNGIFLGASWRNHJ-UHFFFAOYSA-L 0.000 title abstract 2
- 239000000700 radioactive tracer Substances 0.000 title abstract 2
- 238000001179 sorption measurement Methods 0.000 claims abstract description 54
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- 230000004888 barrier function Effects 0.000 claims abstract description 16
- 239000003463 adsorbent Substances 0.000 claims abstract description 12
- 230000004913 activation Effects 0.000 claims abstract description 5
- XNGIFLGASWRNHJ-UHFFFAOYSA-N o-dicarboxybenzene Natural products OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 claims description 53
- -1 phthalic acid ester Chemical class 0.000 claims description 53
- 239000011347 resin Substances 0.000 claims description 26
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- 229910000831 Steel Inorganic materials 0.000 claims description 6
- 239000010959 steel Substances 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims 1
- 239000010931 gold Substances 0.000 claims 1
- 229910052737 gold Inorganic materials 0.000 claims 1
- 238000001514 detection method Methods 0.000 abstract description 27
- 239000003960 organic solvent Substances 0.000 abstract description 12
- 238000012360 testing method Methods 0.000 abstract description 12
- 239000003344 environmental pollutant Substances 0.000 abstract description 6
- 231100000719 pollutant Toxicity 0.000 abstract description 6
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- 239000012071 phase Substances 0.000 description 18
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- 229910052740 iodine Inorganic materials 0.000 description 10
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 235000010233 benzoic acid Nutrition 0.000 description 5
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
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- SESFRYSPDFLNCH-UHFFFAOYSA-N benzyl benzoate Chemical compound C=1C=CC=CC=1C(=O)OCC1=CC=CC=C1 SESFRYSPDFLNCH-UHFFFAOYSA-N 0.000 description 1
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Landscapes
- Sampling And Sample Adjustment (AREA)
Abstract
The utility model relates to a check out test set, especially a device of phthalate content among tracer gas. The device includes: the vacuum pump, the exhaust tube, the buffer tank, particulate filter assembly and adsorption tower, particulate filter assembly is connected with the adsorption tower, the adsorption tower is connected with the buffer tank, the vacuum pump is connected with the buffer tank through the exhaust tube, horizontal among the particulate filter assembly have a porous barrier, a porous barrier goes up the tiling has the glass fiber filter membrane after the activation, the adsorption tower is one at least, equal horizontal the 2nd porous barrier that has in every adsorption tower, be provided with stainless steel meshwork on the 2nd porous barrier, the last polymeric adsorbent that has born of stainless steel meshwork. It can make the detectable concentration be close to true concentration in the at utmost, and the detection ring border of adaptable difference can make into that kind gas flow rate, flow remain stable, simple structure, and easily installation operation, the difficult xenobiotic pollutants that introduces can not pollute the sample yet, unnecessaryly consumes a large amount of organic solvent, environmental protection more.
Description
Technical field
This utility model relates to a kind of detection equipment, phthalic acid ester content in a kind of detected gas
Device.
Background technology
Phthalic acid ester (Phthalate Esters is called for short PAEs), also known as phthalate ester, has aromatic odor, logical
It is often water white oily thick liquid, is insoluble in water, is soluble in the organic solvent such as methanol, ether, boiling point
Higher, the most volatile under room temperature.Phthalic acid ester is the plasticizer that currently used amount is maximum, in plasticising process
In, between phthalic acid ester and TPO plastic molecules, the main physics by hydrogen bond with Van der Waals force merges
Rather than chemical bond, thus maintain independent chemical property each other, As time goes on, work as plastic
Easily dissolution and volatilization after touching the organic solvents such as oils and fats or being heated, hence in surrounding air.Additionally,
Phthalic acid ester is a lipophilic organic pollution of class, and its character is relevant with the length of side chain.Along with side chain
The increase of length, the elevation of boiling point of phthalic acid ester, n-Octanol/Water Partition (Kow) reduces, saturated steaming
Vapour pressure reduces, and the phthalic acid ester that molecular weight is bigger has stronger absorption affinity, is easily adsorbed on granule
Thing and material surface.Phthalic acid ester has carcinogenic, teratogenesis, mutagenic action, has androgen antagonist effect,
Male rodent is had stronger genotoxicity, the male filial generation genital malformation in utero exposed can be caused,
Mainly show as prostate deformity, hypospadias, cryptorchidism etc., also can disturb humans and animals under extremely low concentration
Hormonal system, cause Reproductive Performance not normal.
From the thirties in 20th century, phthalic acid ester is commonly used for the increasing of plastics particularly polrvinyl chloride (PVC)
Mould agent, add pliability and draftability with reinforcing material in polymer to.Phthalic acid ester is to produce and disappear
The plasticizer that the amount of expense is maximum, accounts for the 88% of plasticizer total output, has the O-phthalic of millions of tons the most every year
Acid esters is added in vinyl floors, wallpaper, toy, packaging material for food, medical blood bag and sebific duct, cleaning
Agent, personal-care supplies etc., in hundreds of products such as nial polish, hair spray, shampoo and bath foam.
Phthalic acid ester content in plastic is typically in the range of 10～60%.Owing to phthalic acid ester makes
With extensively, the most measured in water, soil, air, food and human body, it means that it has become general
Time environmental contaminants.Due to the phthalic acid ester impact on health and the destruction of ecological environment, investigation
Just it is particularly important with analyzing phthalic ester concentration in various media.The most both at home and abroad to benzene adjacent in air
The sampling of diformic ester relates generally to the collection of gas phase, is not all enriched with by Gas and particles PAEs,
Cause indoor phthalic acid ester level of pollution is underestimated.The detection method of phthalic acid ester content in gas
Foundation and the research and development of device allow us to it is detected, can accurately measure adjacent benzene two in air
The concentration level of formic acid esters, lays a good foundation in source and transportion and transformation for research pollutant.
In liquid, the detection of PAEs concentration mainly uses ionic liquid dispersion liquid-liquid microextraction method to be enriched with, then
Use the PAEs that HS GC-mass spectrum is used in conjunction in method detection pregnant solution.The detection side of PAEs concentration in solid
Method is usually in the mixed liquor putting into hexane and acetone after solid sample is processed into little granule and carries out microwave extracting,
Solution after extraction carries out GC-MS analysis again.In conventional gas the detection method of PAEs concentration mainly have with
Under several: micro-porous filter is usually used in atmospheric environment or the collection of large space endoparticle thing, is not particularly suited for concentration
Relatively low, that the sampling time is longer room air sample；Solvent absorption is usually used in gathering the gaseous state in air or steaming
Gaseous material, it is possible to the aerosol that collecting part coexists with it；In activated carbon tube method is applicable to little scope, air is adjusted
Look into sampling.Pretreatment link frequently with soxhlet's extraction or ultrasonic extraction mode, extractant mainly have methanol, two
Chloromethanes/acetone (1:1, v:v) and dichloromethane, analysis method generally capillary column carries out chromatography.
Existing detection equipment is the highest with the accumulation rate of solid phase phthalic acid ester to gas phase in gas, causes sampling
Inefficient, it is easily generated error, affects testing result.Utilize organic solvent to soak microporous filter membrane and collect solid phase neighbour
During phthalic acid ester, organic solvent volatilization makes sampling efficiency reduce, and the method is usually used in atmospheric environment or bigger sky
In interior gas, the collection of solid-state phthalic acid ester, is not particularly suited for phthalic ester concentration relatively low, sampling
The room air sample that time is longer.When utilizing solvent rich gas phase phthalic acid ester, solvent is the most organic
Solvent, has bigger volatility, is easily generated low precision, problem that sample rate is low, and data show, with 1L/min
Traffic sampling 1h, sampling efficiency is about 50%-60%, and detection is limited to 1.32ug/m3.Utilize activated carbon
When collection and centrifugation, due to reasons such as little granular active carbon losses, easily cause phthalic acid ester
Loss, sampling rate is 1L/min, and the sampling time is about 3d, and the sampling time is longer, and sample recovery rate is not
High.
Additionally in gas, the detection method of phthalic acid ester content often uses additional traffic sampling device to collect gas-solid
Biphase sample, but same equipment can not carry out specific qualitative and quantitative detection for different detection environment, causes
The detection of sample does not have universality, need to constantly change the sampler of different model, and therefore the sampling such as sampler sets
Standby too much, sampling process is the most loaded down with trivial details, and sampling efficiency is low, complex operation step, wastes time and energy Detection results not
Good, testing cost is high, additionally, the turnover flow velocity of sample, flow, pressure are non-constant, easily by temperature, humidity,
The external environment impacts such as wind direction, testing result poor reproducibility, sensitivity is the highest, and sample range is limited to.
Existing detection equipment typically utilizes organic solvent to be enriched with phthalic acid ester, meeting in sample pretreatment process
Consuming a large amount of organic solvent, organic solvent volatilization and toxicity are relatively big, cause waste of solvent, also make environment simultaneously
Become to pollute.
When utilizing pipeline air-inlet or utilize gas sampling box etc. to collect sample, equipment is plastic, may contain
Phthalic ester plasticizer, sample collection process can be brought new pollutant into, become polluter, cause sample
The secondary pollution of product, the accuracy of impact detection data.
Utility model content
This utility model aims to solve the problem that the problems referred to above, it is provided that the detection of phthalic acid ester content in a kind of gas
Device, on the one hand adsorption rate is up to more than 95% for it, and accuracy is high, and detectable concentration can be made to connect to the full extent
Nearly actual concentration, is on the one hand suitable for different detection environment, and sample introduction gas flow rate, flow can be made to keep stable,
Device structure is simple, it is easy to installing operation, testing cost is low, and scavenging period is short, and practicality and versatility are relatively strong,
Another further aspect is not easily introduced xenobiotic pollutants, also will not contaminated samples, use Resin Absorbent gas phase PAEs, it is not necessary to
Consuming substantial amounts of organic solvent, more environmentally-friendly, cost performance is higher, and its technical scheme used is as follows:
The device of phthalic acid ester content in a kind of detected gas, it is characterised in that including: vacuum pump, take out
Trachea, surge tank, particulate filter arrangement and adsorption tower, described adsorption tower is at least one, for time multiple then by
Removably connect successively under up to；Bottom described particulate filter arrangement, the top with the adsorption tower being positioned at the top can
Dismounting connects, and the bottom of the adsorption tower being positioned at bottom is connected with surge tank, and described vacuum pump passes through exhaust tube
Being connected with surge tank, horizontal in described particulate filter arrangement have the first porous barrier, described first porous barrier
Upper tiling has the glass fiber filter after activation, and the most horizontal in each adsorption tower have the second porous barrier, and described
It is provided with stainless (steel) wire on two porous barriers, described stainless (steel) wire carries adsorbent resin.
On the basis of technique scheme, also include effusion meter and escape pipe, described effusion meter by escape pipe with
Vacuum pump is connected.
On the basis of technique scheme, described particulate filter arrangement and adsorption tower are made by metal material.
On the basis of technique scheme, described adsorption tower totally three, passes through screwed connection between upper and lower adsorption tower.
A kind of utilize the method for phthalic acid ester content in said apparatus detected gas, it is characterised in that include
Following steps:
A) sample collection and keeping: the glass fiber filter having weighed quality in advance is put in particulate filter arrangement,
The adsorbent resin after purification having weighed quality in advance is put in adsorption tower, opens vacuum pump, adopt with default
Sample flow, sampling time, height of sampling are sampled, and record the ginsengs such as temperature, humidity, flow while sampling
Number, after sampling terminates, seals glass fiber filter and adsorbent resin with aluminium foil at once, takes back laboratory
Processing, if having little time to process, being stored in-4 DEG C of refrigerators, the resting period is less than 7 days；
B) sample pretreatment: use supersound extract method to extract the solid phase in glass fiber filter and adsorbent resin
Gentle phase phthalic acid ester；
C) Concentration Testing: measure by GC method and analyze phthalic acid ester content in sample.
On the basis of technique scheme, described step b) sample pretreatment includes:
The pretreatment of glass fiber filter:
With sharp shears, glass fiber filter is cut into the length of side square less than 2mm, accurate on analytical balance
Really weigh quality, transfer to clean in the iodine flask dried.The analytically pure normal hexane that rotation is steamed is measured with graduated cylinder
20ml, joins in iodine flask, then is added thereto to 1ml benzoic acid Bian ester standard solution and adds as calculating
The standard substance of the mark response rate, builds bottle stopper, shakes up；
Being placed on ultrasonic cleaner by iodine flask, ultrasonic cleaning 30min takes out, temperature during in order to reduce extraction
The interference that degree difference causes, during extraction, temperature is set as a definite value, after ultrasonic end, the extracting solution that will take out
Filter in the triangular flask being transferred to correspondence, then carry the most again three times with same normal hexane, add 10mL every time,
Rinsing completely, extracting solution is transferred in triangular flask；
By sample extracting solution sucking filtration in defecator, and rinse with a small amount of normal hexane, filtrate is transferred to pyriform
In flask, and clean more than 3 times with normal hexane, rear solution will be washed and integrate with in pear-shaped flask, at 35 DEG C
Rotation is steamed to less than 1ml, stops rotation and steams, finally transfers in chromatogram bottle with special microsyringe, and with few
Amount chromatographically pure normal hexane cleans pear-shaped flask, and the normal hexane after washing with microsyringe is extracted out and is transferred to chromatogram bottle
In, repeat aforesaid operations more than 3 times, be finally settled to 1.5mL, label after adding a cover and put into freezer storage；
The pretreatment of adsorbent resin:
The resin precise 0.2000g on analytical balance that will reclaim, is accurate to 0.0001g, transfers to clean
In the iodine flask dried, measure, with graduated cylinder, the analytically pure normal hexane 20ml that rotation is steamed, join in iodine flask,
It is added thereto to the 1ml benzoic acid Bian ester standard solution standard substance as calculating recovery of standard addition again, builds
Bottle stopper, shakes up；
Subsequent operations is identical with the pretreatment of glass fiber filter.
On the basis of technique scheme, after described step c) Concentration Testing is for placing one day, take from refrigerator
Going out sample, sufficient standing makes impurity precipitate completely, injects all-glass syringe with microsyringe extraction supernatant,
Filter to another corresponding chromatogram bottle with disposable aspiration needle filter, add a cover and place into refrigerator, finally survey by GC method
Setting analysis phthalic acid ester content.
On the basis of technique scheme, described chromatogram bottle soaks a period of time by washing liquid before using, and cleans and dries,
4h is activated at 450 DEG C in Muffle furnace.
The beneficial effects of the utility model are as follows: one, the PAEs in gaseous sample under the effect of three grades of adsorption towers
Can be adsorbed completely, adsorption rate reaches more than 95%, reduces the error of detection data, improves accuracy, makes
Detectable concentration is to the full extent close to actual concentration.
Two, surge tank can make this device adapt to different detection environment with the installation of effusion meter, makes sample introduction gas stream
Speed, flow keep stable, it is possible to shorten scavenging period, improve cleaning efficiency, improve detection data accuracy,
Assay device structures is simple, it is easy to install operation, reduces testing cost, shortens scavenging period, and practicality is with logical
Stronger by property.
Three, particulate filter arrangement and adsorption tower are welded by stainless steel tube, are not easily introduced xenobiotic pollutants,
Also will not contaminated samples, use Resin Absorbent gas phase PAEs, it is not necessary to consuming substantial amounts of organic solvent, this device is more
Adding environmental protection, cost performance is higher.
Accompanying drawing explanation
In order to be illustrated more clearly that this utility model embodiment or technical scheme of the prior art, below will be to reality
Execute the required accompanying drawing used in example or description of the prior art to be briefly described.It should be evident that describe below
In accompanying drawing be only a kind of embodiment of the present utility model, for those of ordinary skill in the art, not
On the premise of paying creative work, it is also possible to extend according to the accompanying drawing provided and obtain other enforcement accompanying drawing.
Fig. 1: the device of phthalic acid ester content in a kind of detected gas of an embodiment of the present utility model
Structural representation；
Fig. 2: the structural representation of the particulate filter arrangement of an embodiment of the present utility model；
Fig. 3: the structural representation of the adsorption tower of an embodiment of the present utility model；
Detailed description of the invention
The utility model is described in further detail with example below in conjunction with the accompanying drawings:
Of the present utility model embodiment is described below in detail, and the example of described embodiment is shown in the drawings, wherein
The most same or similar label represents same or similar element or has the unit of same or like function
Part.The embodiment described below with reference to accompanying drawing is exemplary, is not only used for explaining this utility model, and not
It is understood that as to restriction of the present utility model.
In description of the present utility model, it is to be understood that term " on ", the orientation of the instruction such as D score equal
To be defined based on the orientation shown in Figure of description Fig. 1, be for only for ease of description this utility model and
Simplify and describe rather than indicate or imply that the device of indication or element must have specific orientation, with specifically
Azimuth configuration and operation, therefore it is not intended that to restriction of the present utility model.
In description of the present utility model, it should be noted that unless otherwise clearly defined and limited, term
" install ", " being connected ", " connection " should be interpreted broadly, and connect for example, it may be fixing, it is also possible to be can
Dismounting connects, or is integrally connected；Can be to be joined directly together, it is also possible to be indirectly connected to by intermediary.Right
For those of ordinary skill in the art, above-mentioned term tool in this utility model can be understood with concrete condition
Body implication.
As shown in Figure 1 to Figure 3, the device of phthalic acid ester content in a kind of detected gas of the present embodiment,
It is characterized in that, including: vacuum pump 1, exhaust tube 2, surge tank 3, particulate filter arrangement 4 and adsorption tower 5,
Described adsorption tower 5 at least one, for removably connecting the most successively time multiple；Described particle filtering
Bottom device 4, the top side detachable with the adsorption tower 5 being positioned at the top is connected, and is positioned at the adsorption tower 5 of bottom
Bottom be connected with surge tank 3, preferably select, surge tank 3 be welded with one and communicate with surge tank 3 inner chamber
Connecting tube, be positioned at bottom and the connecting tube of adsorption tower 5 of bottom by screwed connection, described vacuum pump 1
Being connected with surge tank 3 by exhaust tube 2, horizontal in described particulate filter arrangement 4 have the first porous barrier 40,
Glass fiber filter after tiling has activation on described first porous barrier 40, the most horizontal in each adsorption tower 5
There is the second porous barrier 50, described second porous barrier 50 is provided with stainless (steel) wire, on described stainless (steel) wire
Carry adsorbent resin (such as XAD-2 resin).
Described particulate filter arrangement 4 is preferably designed as infundibulate.
Preferably, also including effusion meter 6 and escape pipe 7, described effusion meter 6 is by escape pipe 7 and vacuum pump
1 is connected.Surge tank can make this device adapt to different detection environment with the installation of effusion meter, makes sample introduction gas
Flow velocity, flow keep stable, reduce the environmental change impact on sampling, it is possible to shorten scavenging period, improve clear
Washing efficiency, improve detection data accuracy, assay device structures is simple, it is easy to install operation, reduces and detects into
This, shorten scavenging period, practical.
Preferably, described particulate filter arrangement 4 and adsorption tower 5 are made by metal material.Preferably employ stainless
Steel is made, but is not limited only to this, is not the most easily introduced xenobiotic pollutants, also will not contaminated samples.
Preferably, described adsorption tower 5 totally three, they are primary adsorption tower 5-1, secondary absorption tower 5-2 and
Three grades of adsorption 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 connected, is on the other hand easy to dismount and places adsorbent resin in adsorption tower to facilitate and be taken out.
A kind of utilize the method for phthalic acid ester content in said apparatus detected gas, it is characterised in that include
Following steps:
A) sample collection and keeping: glass fiber filter (diameter 37mm, the aperture of quality will have been weighed in advance
0.45 μm) put in particulate filter arrangement 4,2.0g adsorbent resin after purification is put in adsorption tower 5,
Open vacuum pump 1, sampling flow 1.0L/min, sampling time 3-5h, height of sampling 0.5m, sampling same
The parameters such as Shi Jilu temperature, humidity, flow, after sampling terminates, at once with aluminium foil by glass fiber filter and suction
Attached resin seals, and takes back laboratory treatment, if having little time to process, is stored in-4 DEG C of refrigerators, the resting period
Less than 7 days；
B) sample pretreatment:
The pretreatment of glass fiber filter:
With sharp shears, glass fiber filter is cut into the length of side square less than 2mm, accurate on analytical balance
Really weigh quality, transfer to clean in the 150ml iodine flask dried.Rotation is measured steamed analytically pure with graduated cylinder
Normal hexane 20ml, joins in iodine flask, then is added thereto to 1ml benzoic acid Bian ester standard solution conduct
Calculate the standard substance of recovery of standard addition, build bottle stopper, shake up；
Being placed on ultrasonic cleaner by iodine flask, ultrasonic cleaning 30min takes out, temperature during in order to reduce extraction
The interference that degree difference causes, during extraction, temperature is set as 25 degree, after ultrasonic end, the extracting solution mistake that will take out
Filter is transferred in the triangular flask of correspondence, then carries the most again three times with same normal hexane, adds 10mL every time,
Rinsing completely, extracting solution is transferred in triangular flask；
By sample extracting solution sucking filtration in defecator, and rinse with a small amount of normal hexane, filtrate is transferred to 150
In the pear-shaped flask of mL, and clean more than 3 times with normal hexane, rear solution will be washed and integrate with in pear-shaped flask,
Steam to less than 1ml at 35 DEG C of backspins, stop rotation and steam, finally transfer to chromatogram bottle with special microsyringe
In, and cleaning pear-shaped flask with a small amount of chromatographically pure normal hexane, the normal hexane after washing with microsyringe is extracted out and is turned
Move in chromatogram bottle, repeat aforesaid operations more than 3 times, be finally settled to 1.5mL, label after adding a cover and put into
Freezer storage；
The pretreatment of adsorbent resin:
The resin precise 0.2000g on analytical balance that will reclaim, is accurate to 0.0001g, transfers to clean
In the 150ml iodine flask dried, measure, with graduated cylinder, the analytically pure normal hexane 20ml that rotation is steamed, join iodine
In measuring bottle, then it is added thereto to 1ml benzoic acid Bian ester standard solution as the reference material calculating recovery of standard addition
Matter, builds bottle stopper, shakes up；
Subsequent operations is identical with the pretreatment of glass fiber filter；
C) Concentration Testing: after placing a day, takes out sample from refrigerator, and sufficient standing makes impurity precipitate completely, with micro-
Amount injector extraction supernatant injects all-glass syringe, filters to another corresponding chromatograph with disposable aspiration needle filter
In Ping, add a cover and place into refrigerator, finally measure by GC method and analyze phthalic acid ester content.Further, institute
State before chromatogram bottle uses and soak a period of time by washing liquid, clean and dry, Muffle furnace activates at 450 DEG C 4h.
Assay method Recovery test
Agents useful for same medicine:
Normal hexane: analytical pure (AR), content >=98.0%, after on Rotary Evaporators, 80 DEG C of backspins steam and purify,
Pour in clean brown reagent bottle stand-by.
Normal hexane: chromatographically pure (HPLC), content >=99.5%.
Benzoic acid Bian ester: chemical pure (CP), density 1.116-1.120, content >=99.0%.
AmberiiteXAD-2 macroporous resin: acetone soak, successively with dichloromethane, methanol at apparatus,Soxhlet's
More than upper constant temperature reflux, extract, 24h, it is dried and removes organic solvent, seal and preserve.
Glass fiber filter: diameter 37mm, aperture 0.45 μm, 450 DEG C of activation 4 in Muffle furnace before sampling
H, aluminium-foil paper seals and preserves.
Methanol: analytical pure (AR), content >=99.5%.
Dichloromethane: analytical pure (AR), content >=99.5%.
Acetone: analytical pure (AR), content >=99.5%.
16 kinds of phthalic acid ester mixed mark 1000mg/L, are shown in Table 1
Table 1 measures 16 kinds of mixed mark kinds and the purity of phthalate compound
GC conditions:
Open carrier gas (nitrogen) in order, air generator, hydrogen generator, gas chromatograph, and with
Computer successful connection, sets gas chromatograph qualitative method by following condition, measures.
Agilent 7820A GC, DB-5 fused-silica capillary column (30m × 0.32mm × 0.25 μm, the U.S.
J&W scientific), flame photometric detector (FID).
Temperature programming: initial temperature 140 DEG C, retention time 1min, the first stage is with 20 DEG C of min-1Rise
To 235 DEG C and keep 0.5min, second stage is with 2 DEG C of min-1Rise to 240 DEG C and keep 0.5min,
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 DEG C；
The highest post case temperature: 325 DEG C；
Detector: flame photometric detector (FID)；
Chromatographic column: DB-5 fused-silica capillary column (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, post flow 1mL min-1。
Qualitative: to be as the criterion with the relative retention time of standard substance, the plastic sample time is 25min
The mensuration of phthalic acid ester: with the quantitative sample of ratio of peak area in external standard method Yu standard external standard peak area
In the content of each object.
Response rate indicator: 100mg L-1Benzyl benzoate.
After sample pre-treatments completes, the chromatogram bottle that will be equipped with sample is placed in appointment position, waits to be determined.Measure
Cheng Hou, by bringing content and the total content recording each esters in graticule into the integration of collection of illustrative plates peak area.
The method response rate
Blank AmberiiteXAD-2 macroporous adsorbent resin and glass fiber filter are separately added into 0.5mL concentration
The mixed mark of PAEs for 4mg/L uses liquid (16 kinds of mixed marks), with normal hexane as extractant, uses excusing from death extraction
Mode extracts 30min, parallel five times, does response rate experiment.Use blank experiment every time, measure this
The response rate of every kind of object under part, and calculate relative standard deviation, the results are shown in Table 2, shown in table 3.
The response rate (%) of table 2 gas phase PAEs
The response rate (%) of table 3 granule phase PAEs
From table 1 it follows that 6 kinds of gas phase PAEs response rate are 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 response rate of 6 kinds of granule phases PAEs is respectively 87.22 ± 7.47%,
86.80 ± 4.08%, 82.90 ± 4.84%, 82.80 ± 9.56%, 85.93 ± 6.12%, 85.30 ± 9.3%, 16 kinds of esters
Average recovery rate be 85.30 ± 5.54%.Precision RSD < 10.0%, illustrate that this analysis method is feasible.
Adsorption tower penetrance is tested
Respectively in the morning, afternoon, three period samplings at night same hot house, during sampling, use three
Layer adsorption tower absorbs gas phase phthalic acid ester in air, respectively in three layers of adsorption tower of detection resin to O-phthalic
The adsorbance of acid esters, compares PAEs content in three layers of adsorption tower resin and accounts for the ratio of total adsorbance, result
It is shown in Table 4.
PAEs content (μ g/m in table 4 resin3)
As can be seen from the table, in the morning, afternoon and night gas, the total concentration of gas phase phthalic acid ester is respectively
It is 204.72,235.40,148.50 μ g/m3, it is seen that temperature is to phthalic acid ester in Plastic Greenhouse film
Rate of release impact is notable.For three layers of adsorption tower, when gathering gas by ground floor resin, have 90%
Above PAEs is adsorbed, and the PAEs that in processing at the morning, afternoon and night three, ground floor adsorption tower retains accounts for
Ratio is respectively as follows: 91.01%, 90.70%, 99.19%.When gathering gas by first and second layer of resin, have
The PAEs of more than 96% is adsorbed, and in processing at the morning, afternoon and night three, first and second layer of adsorption tower retains
PAEs accounting example sum is respectively as follows: 97.26%, 96.90%, 100.00%.And along with phthalic acid in gas
The increase of ester concentration, ground floor ratio of adsorption reduces, and third layer ratio of adsorption increases, therefore when gas phase in gas
Phthalic ester concentration is higher, and (concentration is more than 250 μ g/m3) time 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) time just use one layer or two-layer adsorption tower
Enough.
Phthalic ester concentration detection in gas under varying environment
Use the detection device of the application respectively in campus, No. 1 canopy, three the sampled points samplings of No. 2 canopies, wherein 1
Number canopy is old canopy film, and No. 2 canopies are new canopy film of changing, and detection device uses particulate filter arrangement and glass fibre filter
Membrane filtration solid phase particles shape phthalic acid ester, uses gas phase neighbour's benzene two in three layers of adsorption tower and Resin Absorbent air
Formic acid esters, the content of the phthalic acid ester detected in glass fiber filter and three layers of adsorption tower in resin respectively,
Calculate the ratio that each several part accounts for, the results are shown in Table shown in 5.
The different sample point testing result of table 5
From table 5 testing result, in air, phthalic acid ester is by solid phase (graininess) and gas phase two parts
Composition, solid phase phthalic acid ester can be filtered by glass fiber filter, and its content accounts for total content in gas
5-10%.Gas phase phthalic acid ester can be by resin absorption, and its content accounts for the 90-95% of total content in gas,
Wherein in three layers of adsorption tower in the adsorbable gas of ground floor more than the 85% of phthalic acid ester total amount, the second layer can
The 1-5% of phthalic acid ester total amount in adsorbed gas, third layer adsorbance is total less than phthalic acid ester in gas
The 1% of amount.In campus, No. 1 canopy, three sampled point gases of No. 2 canopies phthalic ester concentration be respectively 16.30,
37.68、215.03μg/m3, above analyze, when in gas, phthalic ester concentration is less than 200
μg/m3, this invention device and method all can use.
The most by way of example this utility model is illustrated, but this utility model is not limited to above-mentioned concrete reality
Executing example, all any changes done based on this utility model or modification belong to the model that this utility model is claimed
Enclose.
Claims (4)
1. the device of phthalic acid ester content in a detected gas, it is characterised in that bag
Include: vacuum pump (1), exhaust tube (2), surge tank (3), particulate filter arrangement (4) and
Adsorption tower (5), described adsorption tower (5) at least, for the most from top to bottom depending on time multiple
Secondary removably connect；Described particulate filter arrangement (4) bottom and the adsorption tower being positioned at the top
(5) top side detachable connects, and is positioned at bottom and the surge tank of the adsorption tower (5) of bottom
(3) being connected, described vacuum pump (1) is connected with surge tank (3) by exhaust tube (2)
Connecing, horizontal in described particulate filter arrangement (4) have the first porous barrier (40), and described first
The upper tiling of porous barrier (40) has the glass fiber filter after activation, each adsorption tower (5)
In the most horizontal have the second porous barrier (50), described second porous barrier (50) is provided with
Stainless (steel) wire, described stainless (steel) wire carries adsorbent resin.
The dress of phthalic acid ester content in a kind of detected gas the most according to claim 1
Put, it is characterised in that: also include effusion meter (6) and escape pipe (7), described effusion meter (6)
It is connected with vacuum pump (1) by escape pipe (7).
Phthalic acid ester content in a kind of detected gas the most according to claim 1 and 2
Device, it is characterised in that: described particulate filter arrangement (4) and adsorption tower (5) are by gold
Belong to material to make.
The dress of phthalic acid ester content in a kind of detected gas the most according to claim 3
Put, it is characterised in that: described adsorption tower (5) totally three, passes through silk between upper and lower adsorption tower
Button connects.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201620113706.3U CN205562482U (en) | 2016-02-04 | 2016-02-04 | Device of phthalate content among tracer gas |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105510484A (en) * | 2016-02-04 | 2016-04-20 | 青岛农业大学 | Device and method for detecting content of phthalate in gas |
| CN110133117A (en) * | 2018-02-02 | 2019-08-16 | 佛山市华祥检测技术服务有限公司 | The detection method of phthalic acid ester in electric wire plastic components |
| LU102450B1 (en) * | 2021-01-27 | 2022-08-09 | Univ Qingdao Agricultural | A device and method for testing the content of phthalic acid esters in gas |
-
2016
- 2016-02-04 CN CN201620113706.3U patent/CN205562482U/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105510484A (en) * | 2016-02-04 | 2016-04-20 | 青岛农业大学 | Device and method for detecting content of phthalate in gas |
| CN105510484B (en) * | 2016-02-04 | 2017-06-30 | 青岛农业大学 | The device and method of phthalic acid ester content in a kind of detection gas |
| CN110133117A (en) * | 2018-02-02 | 2019-08-16 | 佛山市华祥检测技术服务有限公司 | The detection method of phthalic acid ester in electric wire plastic components |
| LU102450B1 (en) * | 2021-01-27 | 2022-08-09 | Univ Qingdao Agricultural | A device and method for testing the content of phthalic acid esters in gas |
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