CN106124255A - The method of phthalic acid ester in a kind of Graphene/ionic liquid composite material enriched air - Google Patents
The method of phthalic acid ester in a kind of Graphene/ionic liquid composite material enriched air Download PDFInfo
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- CN106124255A CN106124255A CN201610431477.4A CN201610431477A CN106124255A CN 106124255 A CN106124255 A CN 106124255A CN 201610431477 A CN201610431477 A CN 201610431477A CN 106124255 A CN106124255 A CN 106124255A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
- G01N1/2202—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/025—Gas chromatography
Abstract
The invention discloses the method for phthalic acid ester in a kind of Graphene/ionic liquid composite material enriched air, Graphene and poly-1 pi-allyl 3 ethyl benzo imidazole hexafluorophosphoric acid ionic liquid is utilized to be combined the material obtained as adsorbent, detection means in conjunction with thermal desorption-gas chromatography-mass spectrum analyzes phthalic acid ester in air, utilizes graphene oxide prepared by ball-milling method through CO2After activation, obtain the material with carbon element of high-ratio surface and multi-pore channel, improve bioaccumulation efficiency；Need not to use a large amount of organic solvent, it is to avoid the problems such as solvent volatilization, cross-contamination, operating procedure is simple, good, highly sensitive to the selectivity of phthalic acid ester, adsorbent recoverable, and can Sync enrichment gaseous state and graininess phthalic acid ester.
Description
Technical field
The present invention relates to a kind of enrichment and the method for detection phthalic acid ester, more particularly to one utilizes stone
Ink alkene/ionic liquid composite material is divided as adsorbing material, the detection means in conjunction with thermal desorption-gas chromatography-mass spectrography
The method of phthalic acid ester in analysis air.
Background technology
Indoor organic pollutant can be divided into volatility and half volatile, and half volatile organic contaminant refers to saturated vapor
Pressure and the class organic pollution materials that volatility is relatively low, adsorptivity is stronger, mainly include pesticide, plasticizer, fire retardant etc..Adjacent benzene
Dicarboxylic acid esters can and the secondary molecules of polymeric chain between produce and interact, and then improve the elasticity of polymeric material, and increase poly-
The ductility of laminate material and pliability, be a kind of more satisfactory plasticizer, but phthalic acid ester shadow can ring the mankind
Hormonal system, causes reproduction, growth and dystropy, the most in the world to the disabling cry of phthalic acid ester the most increasingly
High.Phthalic acid ester belongs to semi-volatile organic matter pollutant, exists with Gas and particles in atmosphere, and majority is in
Trace ultra trace level.Therefore, the phthalic acid ester in enriched air is an important step of environmental analysis.Traditional adopts
Quadrat method needs to use in a large number organic solvent, often along with problems such as solvent volatilization, cross-contaminations, in long pre-treatment
Journey is also easy to introduce the impurity in solvent and surrounding, sample is polluted, affect the accuracy of quantitative result, and not
Can Sync enrichment gas phase and granule.
Ionic liquid is as a kind of novel green solvent, and steam forces down, the most volatile；Good stability, nonflammable；Dissolve energy
Power is strong；Designability is strong, recoverable.Inorganic, organic substance and polymer all had good dissolubility.Use ion
Liquid, as enrichment material, can gather the phthalic acid ester of gaseous state and particulate form simultaneously, the structure designability of ionic liquid
Also considerably increasing the selectivity to pollutant, the application of ionic liquid also simplify the pretreatment process of complexity.
The two-dimensional material of the monolayer atomic thickness that Graphene is made up of with sp2 hydridization carbon atom, thickness is only
0.335nm, has long-range π key conjugated structure, and theoretical specific surface area is up to 2600m2/ g, hexagonal array array structure enables it to and it
Its molecule generation strong interaction, this makes it have stronger absorbability, is comparatively ideal enrichment material.Graphite is dilute to be recognized
For being a kind of nonpolar, hydrophobic, the ring of carbon matrix is had to the structure of the strongest affinity, can use in analytical chemistry field
In reverse phase solid phase extraction, it is possible to as the adsorbing material of SPE and SPME, Graphene can also provide a lot of can decorating site,
Providing possibility for selective enrichment analyte, the preparation of graphene composite material and application have become as the heat of scientific circles' research
Point problem.
Summary of the invention
The deficiency existed for prior art, it is an object of the invention to provide phthalic acid ester in a kind of enriched air
Method, it is not necessary to using a large amount of organic solvent, it is to avoid the problems such as solvent volatilization, cross-contamination, operating procedure is simple, to neighbour
The selectivity of phthalic acid ester is good, highly sensitive, the repeatable utilization of adsorbent, and can Sync enrichment gaseous state and graininess neighbour's benzene two
Formic acid esters.
For achieving the above object, the technical scheme is that a kind of Graphene/ionic liquid composite material is rich
The method of phthalic acid ester in collection air, it is characterised in that: comprise the steps:
1) preparation of graphene oxide: weigh graphite oxide in ball grinder, add DMF, add ammonium hydrogen carbonate, ball milling
10-15h, in product joins ethanol in ball grinder, at 20-30 DEG C, carries out ultrasonic 24-36h, obtains the glue of graphene oxide
Liquid solution, centrifugal, clean successively with deionized water and ethanol, centrifugal, it is dried；Graphite oxide is dilute is the precursor that synthetic graphite is dilute,
It has the group being very easy to be modified by sulphation so that Graphene can be combined with multiple material.
2) activation of graphene oxide: weigh dried graphene oxide and be placed in tube furnace, be passed through 60-80mL
min-1N230-60min；By stove with 5-20 DEG C of min-1Heating rate be raised to 750-950 DEG C；Then gas is changed into CO2,
Flow 10-60mL min-1, it is incubated 2-5h；Change gas into N2, flow 60-80mL min-1, tube furnace is cooled to room temperature,
To activation Graphene；Pass through CO2The grapheme material that activation obtains, it is possible to introduce micropore in the material, make Graphene have many
The pore passage structure of level, it is possible to decrease the reunion of Graphene, keeps high specific surface area, it is ensured that Graphene is abundant with material upon adsorption
Contact, improves its accumulation ability to a lot of chemical substances.
3) preparation of Graphene/ionic liquid composite material sampling tube: weigh activation Graphene and poly-1-pi-allyl-3-
Ethyl benzo imidazole hexafluorophosphoric acid ionic liquid, adds DMF, makes it be distributed to solution uniformly at 30-60 DEG C of sonic oscillation
In, obtain Graphene and the mixture of poly-1-pi-allyl-3-ethyl benzo imidazole hexafluorophosphoric acid ionic liquid；It is coated in white
The surface of color carrier, the white carrier infrared baking lamp being coated with Graphene/ionic liquid composite material is dried；It is dried rearmounted
In baking oven, dry 2-5h in 110-120 DEG C, after being down to room temperature, insert in glass tubing；Activation, two beyond the Great Wall, put under room temperature
In exsiccator standby.Ionic liquid is combined with Graphene, hydrophilic and the dispersibility of Graphene can be increased, obtain stability
Higher complex, is avoided that the phenomenon that Graphene is reunited, energy due to π-pi-electron sedimentation and van der Waals interaction simultaneously
Obtain bioaccumulation efficiency more higher than single graphene oxide.
4) sampling: utilize double gas circuit constant current atmosphere sampling instrument to sample, sampling flow: 500-1000mL/min, sampling
Time: 90min, after sampling, seals immediately.
5) thermal desorption-gas chromatography-mass spectrometry analysis: utilize automatic heating desorption instrument-gas chromatograph-mass spectrometer (GC-MS) to examine
Cls analysis, the condition of thermal desorption is: desorption gas: helium；First stage sample cell is desorbed, desorption temperature 220-280 DEG C, desorption
Time 10-15min, is desorbed flow velocity 50mL/min；Cold trap trapping temperature 0 DEG C, second stage cold-trap is desorbed, desorption temperature 260-
280 DEG C, desorption time 5-15min, heating rate 30-40 DEG C/s, all without shunting after trap before trap；Six-way valve temperature 230 DEG C, transmission
Line temperature 240-280 DEG C；GC conditions: chromatographic column: use DB-5MS chromatographic column；Specification: 30m × 0.25mm × 0.25 μ
m；Carrier gas: high-pure helium, purity >=99.999%；Injector temperature: 250 DEG C；Sample size: 1 μ L；Split sampling, split ratio: 20:
1；Constant current mode, flow velocity: 1.0mL/min；Mass Spectrometry Conditions: ionization mode: electron bombardment ionization source (FI)；Ionizing energy: 70eV；Transmission
Line temperature: 280 DEG C；Ion source temperature: 230 DEG C；Quadrupole rod temperature: 150 DEG C；Grab type: select ion scan+full scan
(SIM+Scan)；Solvent delay: 10min；Heating schedule: initial temperature 80 DEG C, keeps 0.5min, with the speed of 30 DEG C/min extremely
160 DEG C, keep 3min, then with the speed of 5 DEG C/min to 300 DEG C, keep 5min.
As a further improvement on the present invention, in described step 1, the mass ratio of graphite oxide: DMF: ammonium hydrogen carbonate is 10: 1
∶6。
As a further improvement on the present invention, selecting planetary ball mill in described step 1, ball mill rotational velocity is
1200r/min, revolution speed is 600r/min.
As a further improvement on the present invention, Graphene in described step 3: the mass ratio of ionic liquid: DMF is 1: 2: 6.
As a further improvement on the present invention, described step 3 activates and makees carrier gas with helium, at the flow velocity of 60mL/min
Under, 250-280 DEG C of activation 30-60min, is down to less than 30 DEG C in the case of uninterrupted helium stream.
As a further improvement on the present invention, the standard substance of selection include phthalic acid two (2-ethyl hexyl ester)
(DEHP), dibutyl phthalate (DBP), O-phthalic acid butyl benzyl group ester (BBP), dimethyl phthalate (DMP),
Diethyl phthalate (DEP) and diisooctyl phthalate (DIDP), select following qualitative ion and quota ion
As follows:
The present invention utilize Graphene/ionic liquid composite material as adsorbent, in conjunction with thermal desorption-gas chromatography-mass spectrum
Associated with detection means analyze phthalic acid ester in air, utilize graphene oxide prepared by ball-milling method through CO2Activation
After, obtain specific surface and pore volume has been respectively 1047m2g-1And 3.8cm3g-1Material with carbon element, improve bioaccumulation efficiency；Need not
Using a large amount of organic solvent, it is to avoid the problems such as solvent volatilization, cross-contamination, operating procedure is simple, to phthalic acid ester
Selectivity is good, highly sensitive, adsorbent recoverable, and can Sync enrichment gaseous state and graininess phthalic acid ester.
Accompanying drawing explanation
Fig. 1 is Graphene Raman of the present invention figure；
Fig. 2 is Graphene SEM of the present invention figure；
Fig. 3 is Graphene of the present invention/ionic liquid TEM figure.
Detailed description of the invention
Following example are given below the present invention is described in further detail
1) thermal desorption-gas chromatography-mass spectrometry analysis: the condition of thermal desorption is: desorption gas: helium；First stage sample
Pipe is desorbed, desorption temperature 220-280 DEG C, desorption time 10-15min, is desorbed flow velocity 50mL/min；Cold trap trapping temperature 0 DEG C, the
Two-stage cold-trap is desorbed, desorption temperature 260-280 DEG C, desorption time 5-15min, heating rate 30-40 DEG C/s, before trap after trap all
Without shunting；Six-way valve temperature 230 DEG C, transmission line temperature 240-280 DEG C；GC conditions: chromatographic column: use DB-5MS chromatograph
Post；Specification: 30m × 0.25mm × 0.25 μm；Carrier gas: high-pure helium, purity >=99.999%；Injector temperature: 250 DEG C；Sample introduction
Amount: 1 μ L；Split sampling, split ratio: 20: 1；Constant current mode, flow velocity: 1.0mL/min；Mass Spectrometry Conditions: ionization mode: electronics bangs
Hit source (EI)；Ionizing energy: 70eV；Transmission line temperature: 280 DEG C；Ion source temperature: 230 DEG C；Quadrupole rod temperature: 150 DEG C；Adopt
Collection type: select ion scan+full scan (SIM+Scan)；Solvent delay: 10min；Heating schedule: initial temperature 80 DEG C, protects
Hold 0.5min, with the speed of 30 DEG C/min to 160 DEG C, keep 3min, then with the speed of 5 DEG C/min to 300 DEG C, keep 5min；
The qualitative ion of table 1 mass spectral analysis selection and quota ion
2) preparation of standard solution: the most accurately weigh six kinds of phthalic acid ester standard substance: phthalic acid two (2-second
Base hexyl ester) (DEHP), dibutyl phthalate (DBP), O-phthalic acid butyl benzyl group ester (BBP), phthalic acid two
Methyl ester (DMP), diethyl phthalate (DEP), diisooctyl phthalate (DIDP) 500mg, uses methanol dilution constant volume
In 100ml volumetric flask, it is made into the mixed standard solution of 5mg/ml；By the mixed standard solution of 5mg/ml methanol stepwise dilution
Constant volume, obtains 0.1 μ g/mL, 0.5 μ g/mL, 2 μ g/mL, 5 μ g/mL, 10 μ g/mL, 30 μ g/mL, the mark of 50 μ g/mL Concentraton gradient
Quasi-solution.
The preparation of activation Graphene A
1) preparation of graphene oxide A: weigh 10g graphite oxide in ball grinder, add 1gDMF, add 6g bicarbonate
Ammonium, ball milling 13h, in product joins ethanol in ball grinder, at 20 DEG C, carry out ultrasonic 28h, obtain the glue of graphene oxide A
Liquid solution, centrifugal, clean successively with deionized water and ethanol, centrifugal, it is dried；
2) activation of graphene oxide A: weigh dried graphene oxide A and be placed in tube furnace, be passed through 65mL min-1
N240min；By stove with 10 DEG C of min-1Heating rate be raised to 800 DEG C；Then gas is changed into CO2, flow 20mL min-1, it is incubated 3h；Change gas into N2, flow 60mL min-1, tube furnace is cooled to room temperature, obtains activating Graphene A；
The preparation of activation Graphene B
1) preparation of graphene oxide B: weigh 10g graphite oxide B in ball grinder, add 1gDMF, add 6g bicarbonate
Ammonium, ball milling 14h, in product joins ethanol in ball grinder, at 25 DEG C, carry out ultrasonic 30h, obtain the glue of graphene oxide B
Liquid solution, centrifugal, clean successively with deionized water and ethanol, centrifugal, it is dried；
2) activation of graphene oxide B: weigh dried graphene oxide B and be placed in tube furnace, be passed through 70mL min-1
N250min；By stove with 15 DEG C of min-1Heating rate be raised to 850 DEG C；Then gas is changed into CO2, flow 40mL min-1, it is incubated 4h；Change gas into N2, flow 70mL min-1, tube furnace is cooled to room temperature, obtains activating Graphene B；
The preparation of Graphene/ionic liquid composite material A sampling tube
Weigh 1g and activate Graphene A and 2g poly-1-pi-allyl-3-ethyl benzo imidazole hexafluorophosphoric acid ionic liquid, add
Enter 6gDMF, make it disperse uniformly at 40 DEG C of sonic oscillations, obtain Graphene and poly-1-pi-allyl-3-ethyl benzo imidazole six
The mixture of fluorophosphate ionic liquid；Weigh 45g white carrier and be added to Graphene A and poly-1-pi-allyl-3-ethyl benzo miaow
In the mixture of azoles hexafluorophosphoric acid ionic liquid, it is coated with the white carrier of Graphene/ionic liquid composite material A with red
Outer heat lamp is dried；It is placed in after drying in baking oven and dries 3h in 115 DEG C, after being down to 25 DEG C, insert in glass tubing；Activation, two beyond the Great Wall,
Put in the exsiccator under room temperature standby.
The preparation of Graphene/ionic liquid composite material B sampling tube
Weigh 2g and activate Graphene B and 4g poly-1-pi-allyl-3-ethyl benzo imidazole hexafluorophosphoric acid ionic liquid, add
Enter 12gDMF, make it be distributed to uniformly in solution at 30-60 DEG C of sonic oscillation, obtain Graphene B solution and ionic liquid
Mixture；Weigh 90g white carrier be added to Graphene B solution and poly-1-pi-allyl-3-ethyl benzo imidazole hexafluorophosphate from
In the mixture of sub-liquid, the white carrier infrared baking lamp being coated with Graphene/ionic liquid composite material B is dried；Will
Dried ionic liquid/graphene composite material is placed in baking oven and dries 4h in 120 DEG C, is down to 25 DEG C, inserts in glass tubing；Live
Change, two beyond the Great Wall, put in the exsiccator under room temperature standby.
Embodiment 1
The 0.1 μ g/mL of 1uL, 0.5 μ g/mL, 2 μ g/mL, 5 μ g/mL, 10 μ g/mL, 30 μ are drawn respectively with microsyringe
G/mL, the standard solution of 50 μ g/mL concentration, inject in sampling tube A, carry out under the conditions of thermal desorption-gas chromatography-mass spectrometry analysis
Measuring, with peak area as vertical coordinate, concentration is abscissa drawing curve.
Table 2 standard curve detection limit and quantitative limit
| Sequence number | Title | Regression equation | Correlation coefficient | Detection limit μ g/g | Quantitative limit μ g/g |
| 1 | DBP | Y=2569x+1375.4 | 0.9991 | 0.07 | 0.36 |
| 2 | BBP | Y=2635x+1824.6 | 0.9994 | 0.01 | 0.21 |
| 3 | DEHP | Y=3761x+2015.7 | 0.9993 | 0.04 | 0.19 |
| 4 | DMP | Y=3258x+2038.4 | 0.9992 | 0.02 | 0.27 |
| 5 | DEP | Y=1983x+1164.3 | 0.9993 | 0.03 | 0.32 |
Embodiment 2
The 0.1 μ g/mL of 1uL, 0.5 μ g/mL, 2 μ g/mL, 5 μ g/mL, 10 μ g/mL, 30 μ are drawn respectively with microsyringe
G/mL, the standard solution of 50 μ g/mL concentration, inject in sampling tube B, carry out under the conditions of thermal desorption-gas chromatography-mass spectrometry analysis
Measuring, with peak area as vertical coordinate, concentration is abscissa drawing curve.
Table 3 standard curve detection limit and quantitative limit
| Sequence number | Title | Regression equation | Correlation coefficient | Detection limit μ g/g | Quantitative limit μ g/g |
| 1 | DBP | Y=3148x+2014.5 | 0.9990 | 0.04 | 0.25 |
| 2 | BBP | Y=2874x+2137.5 | 0.9994 | 0.03 | 0.27 |
| 3 | DEHP | Y=3637x+1962.1 | 0.9991 | 0.03 | 0.18 |
| 4 | DMP | Y=1958x+1983.6 | 0.9993 | 0.02 | 0.34 |
| 5 | DEP | Y=2536x+2036.5 | 0.9994 | 0.03 | 0.36 |
Embodiment 3
Take concentration and be respectively 0.1 μ g/mL, 5 μ g/mL, the standard sample of 50 μ g/mL, respectively with sampling tube A and sampling tube B
Do precision and response rate experiment
The response rate of 4 three kinds of mark-on samples of table and RSD
Embodiment 4
Utilize double gas circuit constant current atmosphere sampling instrument, sampling time: 90min, after sampling, seal immediately.
The testing result of the different embodiment of table 5
Claims (6)
1. the method for phthalic acid ester in Graphene/ionic liquid composite material enriched air, it is characterised in that: include
Following steps:
1) preparation of graphene oxide: weigh graphite oxide in ball grinder, add DMF, add ammonium hydrogen carbonate, ball milling 10-
15h, joins in ethanol by ball grinder product, at 20-30 DEG C, carries out ultrasonic 24-36h, and the colloid obtaining graphene oxide is molten
Liquid, centrifugal, clean successively with deionized water and ethanol, centrifugal, it is dried；
2) activation of graphene oxide: weigh dried graphene oxide and be placed in tube furnace, be passed through 60-80mLmin-1's
N230-60min；By stove with 5-20 DEG C of min-1Heating rate be raised to 750-950 DEG C；Then gas is changed into CO2, flow
10-60mL min-1, it is incubated 2-5h；Change gas into N2, flow 60-80mL min-1, tube furnace is cooled to room temperature, is lived
Functionalized graphene；
3) preparation of Graphene/ionic liquid composite material sampling tube: weigh activation Graphene and poly-1-pi-allyl-3-ethyl
Benzimidazole hexafluorophosphoric acid ionic liquid, adds DMF, makes it disperse uniformly at 30-60 DEG C of sonic oscillation, obtain living fossil
Ink alkene and the mixture of poly-1-pi-allyl-3-ethyl benzo imidazole hexafluorophosphoric acid ionic liquid；Mixture is coated in white
The surface of carrier, the white carrier infrared baking lamp being coated with Graphene/ionic liquid composite material is dried；It is placed in after drying
Baking oven dries 2-5h in 110-120 DEG C, after being down to room temperature, inserts in glass tubing；Activation, two beyond the Great Wall, put into doing under room temperature
In dry device standby；
4) sampling: utilize double gas circuit constant current atmosphere sampling instrument to sample, sampling flow: 500-1000mL/min, the sampling time:
90min, after sampling, seals immediately；
5) thermal desorption-gas chromatography-mass spectrometry analysis: utilize automatic heating desorption instrument-gas chromatograph-mass spectrometer (GC-MS) to carry out detection point
Analysis, the condition of thermal desorption is: desorption gas: helium；First stage sample cell is desorbed, desorption temperature 220-280 DEG C, desorption time
10-15min, is desorbed flow velocity 50mL/min；Cold trap trapping temperature 0 DEG C, second stage cold-trap is desorbed, desorption temperature 260-280 DEG C,
Desorption time 5-15min, heating rate 30-40 DEG C/s, all without shunting after trap before trap；Six-way valve temperature 230 DEG C, transmission line temperature
240-280℃；GC conditions: chromatographic column: use DB-5MS chromatographic column；Specification: 30m × 0.25mm × 0.25 μm；Carrier gas:
High-pure helium, purity >=99.999%；Injector temperature: 250 DEG C；Sample size: 1 μ L；Split sampling, split ratio: 20: 1；Constant current mould
Formula, flow velocity: 1.0mL/min；Mass Spectrometry Conditions: ionization mode: electron bombardment ionization source (FI)；Ionizing energy: 70eV；Transmission line temperature:
280℃；Ion source temperature: 230 DEG C；Quadrupole rod temperature: 150 DEG C；Grab type: select ion scan+full scan (SIM+
Scan)；Solvent delay: 10min；Heating schedule: initial temperature 80 DEG C, keeps 0.5min, with the speed of 30 DEG C/min to 160
DEG C, keep 3min, then with the speed of 5 DEG C/min to 300 DEG C, keep 5min.
Phthalic acid ester in a kind of Graphene/ionic liquid composite material enriched air the most according to claim 1
Method, it is characterised in that: the mass ratio of graphite oxide in described step 1: DMF: ammonium hydrogen carbonate is 10: 1: 6.
Phthalic acid ester in a kind of Graphene/ionic liquid composite material enriched air the most according to claim 2
Method, it is characterised in that: selecting planetary ball mill in described step 1, ball mill rotational velocity is 1200r/min, revolution speed
For 600r/min.
Phthalic acid ester in a kind of Graphene/ionic liquid composite material enriched air the most according to claim 3
Method, it is characterised in that: the mass ratio of Graphene in described step 3: ionic liquid: DMF is 1: 2: 6.
Phthalic acid ester in a kind of Graphene/ionic liquid composite material enriched air the most according to claim 4
Method, it is characterised in that: described step 3 activates and makees carrier gas with helium, under the flow velocity of 60mL/min, 250-280 DEG C of activation
30-60min, is down to less than 30 DEG C in the case of uninterrupted helium stream.
6. according to benzene two adjacent in a kind of Graphene/ionic liquid composite material enriched air described in any one of claim 1-5
The method of formic acid esters, it is characterised in that: the standard substance of selection include phthalic acid two (2-ethyl hexyl ester) (DEHP), adjacent benzene
Dibutyl carboxylic acid (DBP), O-phthalic acid butyl benzyl group ester (BBP), dimethyl phthalate (DMP), phthalic acid
Diethylester (DEP) and diisooctyl phthalate (DIDP), select following qualitative ion and quota ion as follows:
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| CN108387668A (en) * | 2018-05-04 | 2018-08-10 | 清华大学 | A kind of particulate organic matter on-line preconcentration resolver and its application method |
| CN108387668B (en) * | 2018-05-04 | 2023-04-11 | 清华大学 | Particle organic matter online enrichment and analysis device and use method thereof |
| CN109991323A (en) * | 2018-12-29 | 2019-07-09 | 江苏微谱检测技术有限公司 | The detection method of VOCs in ambient air |
| CN109991323B (en) * | 2018-12-29 | 2022-06-28 | 江苏微谱检测技术有限公司 | Method for detecting volatile organic compounds in ambient air |
| CN110333127A (en) * | 2019-06-24 | 2019-10-15 | 北京大学 | A kind of gas phase semi-volatile organic matter on-line measurement system, methods and applications |
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| CN110850007A (en) * | 2019-11-13 | 2020-02-28 | 云南中烟工业有限责任公司 | Method for measuring phthalate component migration in filter stick by simulating real smoking of cigarette |
| CN112285256A (en) * | 2020-11-09 | 2021-01-29 | 上海市质量监督检验技术研究院 | Method for rapidly screening content of phthalic acid ester in textile |
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