CN107860853A - A kind of needle type extraction device and its application method for concentrating volatile benzene homologues - Google Patents
A kind of needle type extraction device and its application method for concentrating volatile benzene homologues Download PDFInfo
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- CN107860853A CN107860853A CN201711349709.2A CN201711349709A CN107860853A CN 107860853 A CN107860853 A CN 107860853A CN 201711349709 A CN201711349709 A CN 201711349709A CN 107860853 A CN107860853 A CN 107860853A
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- syringe
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/08—Preparation using an enricher
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
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Abstract
The invention discloses a kind of needle type extraction device and its application method for concentrating volatile benzene homologues, the device is including the stainless steel syringe needle with needle stand, the dilatation syringe being removably tightly connected with needle stand, with dilatation syringe afterbody by being tightly connected the reinforcing gas operated device that base is connected, the air extractor or gas injection device that are removably tightly connected with reinforcing gas operated device afterbody；Solid-phase adsorbent is filled with dilatation syringe, syringe outer wall is provided with heat-transfer device, and heat-transfer device is connected with temperature controller, and dilatation syringe is heat-conducting metal material.The device has the advantages of enrichment time is short, simple to operate, specific selective is high, it can overcome that the permeability occurred in existing pin type abstraction technique is poor, reappearance is low, prepares the shortcomings of difficult, and it can be combined with gas-chromatography, it is easy to use, provide a new abstraction technique for the accurate analysis and detection of trace gas.
Description
Technical field
The present invention relates to technical field of analytical chemistry, for the analysis volatilized with semi-volatile organic compounds, is specially
A kind of needle type extraction device and its application method for concentrating volatile benzene homologues, the present invention is based on molecular imprinting technology
Specific recognition principle and a kind of new abstraction technique to grow up.
Background technology
The phenomenon of China's atmosphere pollution in recent years is increasingly severe, with the continuous progress of industrial development, various organic matters
The pollution brought is also following.The benzene homologues of house decoration volatilization, seriously endanger human body health.But due in air
Benzene homologues are usually trace, it is impossible to reach the detection line of instrument, can not realize quantitative analysis, therefore invent a kind of to benzene homologues sample
The needle type extraction device that product have enrichment function is extremely necessary.Using applying gas phase color after needle type extraction device adsorbed target thing
Spectrometer carries out quantitative detecting analysis.Needle type extraction device has following clear superiority：(1) to the enrichment of target compound
Ability is strong；(2) rate of recovery, the degree of accuracy and precision are high；(3) easily realize that sample stores.But it also has some shortcomings, than
Such as:Due to receiving the limitation of gas chromatograph injection port, the adsorbent of filling causes adsorbance few less；Needle type extraction device is penetrating
Property it is poor, extract gas required for time length；It is not easy to seal during stored sample.
The content of the invention
The purpose of the present invention is a kind of device for the high bioaccumulation efficiency for being applied to absorption Environmental Trace benzene homologues of invention, should
Device has the advantages of enrichment time is short, simple to operate, specific selective is high, and the device can overcome existing pin type extraction extraction
The permeability that occurs in technology is poor, reappearance is low, prepares the shortcomings of difficult, and can be combined with gas-chromatography, easy to use,
A new abstraction technique is provided for the accurate analysis and detection of trace gas.The purpose of the present invention is by following technology
What scheme was realized：
A kind of needle type extraction device for concentrating volatile benzene homologues, described needle type extraction device are included with needle stand
Stainless steel syringe needle, the dilatation syringe being removably tightly connected with needle stand and dilatation syringe afterbody are by being tightly connected bottom
The connected reinforcing gas operated device of seat, the air extractor or gas injection dress being removably tightly connected with reinforcing gas operated device afterbody
Put；Solid-phase adsorbent is filled with the dilatation syringe, syringe outer wall is provided with heat-transfer device, and the heat-transfer device is connected with temperature
Instrument is controlled, the dilatation syringe is heat-conducting metal material.
Further, the heat-transfer device be dilatation syringe outside uniform winding heating wire, the head and the tail both ends of heating wire
Connect temperature controller.
Further, the air extractor is sampling pump or syringe, and the gas injection device is syringe.
Further, the reinforcing gas operated device is made up of heat-insulated material.
Further, the solid-phase adsorbent is molecular fiber coating imprinted polymer, and molecular engram fiber coat polymerize
The preparation process of thing：It is to be according to the amount ratio of material by benzoic acid, 4-vinylpridine, ethyleneglycol dimethacrylate (EDMA)
1:3:20 ratio is dissolved in toluene:Lauryl alcohol volume ratio is 1:In 12.5 solution, and AIBN initiators are added, ultrasound mixes
After be coated on fiber, polymerize 24 hours, then with volume ratio be 1:4 0.2mol/LNaOH solution and absolute ethyl alcohol mixed liquor
Elution, prepare molecular engram fiber coat print compound.
Further, the dilatation syringe is copper.
Further, the dilatation syringe length is 22 ~ 28mm, and external diameter is 4 ~ 5mm, and internal diameter is 2.5 ~ 3.5mm.
Further, stainless steel syringe needle is tip and length is 30 ~ 50mm.
For the application method of the needle type extraction device of concentrating volatile benzene homologues, comprise the following steps：
1）Before to sample, dilatation syringe is first heated to 280 DEG C of 5 ~ 10min of aging；
2）Adsorbent is inserted in dilatation syringe after the cooling of dilatation syringe, is tightly connected syringe needle；
3）Insert the needle into sampling source, sampled with air extractor；
4）After completing sampling, air extractor is replaced with into gas injection device, gas injection device extracts part inert gas in advance；
5）Start temperature controller, start to heat dilatation syringe；
6）When the temperature of the heat-transfer device of dilatation syringe reaches assigned temperature, gas chromatograph injection port is inserted the needle into, is pushed away
Dynamic gas injection device makes inert gas by adsorbent, while is realized by the high temperature of syringe to the heat of target substance in sample gas
Desorption, and then detected after gas-chromatography separates.
The beneficial effects of the invention are as follows：
（1）Increase the internal diameter of extraction equipment, operation is easier, and filler preparation is more uniform, reproducible.（2）Permeability is good,
Shorten sample time.（3）The amount of filling adsorbing medium increases, and increases the service life.（3）During stored sample, better tightness, drop
Low loss late.
Below in conjunction with the accompanying drawings and embodiment is described in further detail to the present invention.
Brief description of the drawings
Fig. 1 is needle type extraction device overall structure diagram of the present invention.
Fig. 2 is needle cylinder surface heat-transfer device structural representation；
Fig. 3 is reinforcing gas operated device sectional view；
Fig. 4 is needle type extraction device scheme of installation；
Fig. 5 is that needle type extraction device extracts sample schematic diagram；
Fig. 6 is extraction equipment after the completion of extraction to gas chromatographic sample introduction schematic diagram；
Fig. 7 is the gas chromatogram that Determination of Trace Benzene post analysis are extracted using apparatus of the present invention.
Reference：1. syringe needle；2. needle stand；3. dilatation syringe；4. adsorbent；5. it is tightly connected base；6 reinforce air guide dress
Put；7. airtight connection syringe base；8 temperature controllers；9. the source of sampling（Gas sampling or collection device）；10. air extractor
（Large volume syringe or gas samping pump）；11. gas injection device（Small size syringe）；12. inert gas；13. injection port；
14. gas chromatograph；15. heating wire.
Embodiment
Embodiment 1
As shown in Fig. 1 ~ 4, a kind of needle type extraction device for concentrating volatile benzene homologues, described needle type extraction device includes
High temperature resistant stainless steel syringe needle 1 with needle stand 2, the dilatation syringe 3 being removably tightly connected with needle stand 2 and dilatation pin
3 afterbodys of cylinder are by being tightly connected the connected reinforcing gas operated device 6 of base 5, removably connecting with reinforcing the afterbody of gas operated device 6
The air extractor 10 or gas injection device 11 connect；Solid-phase adsorbent 4 is filled with the dilatation syringe 3, syringe outer wall, which is provided with, leads
Thermal（It is heating wire 15 in the present embodiment）, the heat-transfer device is connected with temperature controller 8, and the dilatation syringe 3 is heat conduction gold
Belong to material（It is copper in the present embodiment）.
Air extractor 10 is sampling pump or large volume syringe in the present embodiment, and the gas injection device 11 is injected for small size
Device.During mounting of syringe, reinforce between gas operated device 6 and syringe and be provided with airtight connection syringe base 7.
Reinforce gas operated device 6 to be made up of heat-insulated material, its concrete structure is shown in Fig. 3, its internal setting Heat insulated conduit.It is heat-insulated to lead
The effect of pipe is the temperature too high air-tightness for influenceing syringe and syringe connected interface when avoiding the syringe from heating；Air guide acts on, and borrows
Help inert gas in syringe that the determinand desorbed is pushed into separation analysis in gas chromatograph.Syringe both ends can be with close
Lidstock, so as to stored sample.
Solid-phase adsorbent is molecular fiber coating imprinted polymer, or the adsorbent using other media as carrier.Molecule prints
The preparation process of mark fiber coat polymer：It is to press benzoic acid, 4-vinylpridine, ethyleneglycol dimethacrylate (EDMA)
Amount ratio according to material is 1:3:20 ratio is dissolved in toluene:Lauryl alcohol volume ratio is 1:In 12.5 solution, and add AIBN
Initiator, ultrasound mix after be coated on fiber, polymerize 24 hours, then with volume ratio be 1:4 0.2mol/LNaOH solution with
Absolute ethyl alcohol mixed liquor elutes, and prepares molecular engram fiber coat print compound.
Dilatation syringe length is 22 ~ 28mm（It is preferred that 25mm）, external diameter is 4 ~ 5mm（It is preferred that 4.5mm）, internal diameter is 2.5 ~ 3.5mm（It is excellent
Select 3mm）.
Stainless steel syringe needle is tip and length is 30 ~ 50mm, to facilitate sample collection and convenient and gas chromatograph sampling
Mouth connection.
The present embodiment device includes two parts：Syringe：Long 25 millimeters, internal diameter is 3 millimeters of the copper syringe of high temperature resistant,
Syringe one end can be tightly connected high temperature resistant stainless steel pin, and the other end can both be tightly connected gas samping pump, can seal again
Connect medical standard syringe.The inside of syringe is filled one section of adsorbent and can flexibly dismantled as extraction media, syringe both ends,
It is easy to fill extraction media.2nd, heat-transfer device（Outer vaporizer）：It is made up of resistance wire of the uniform winding in syringe outer wall, with
3A12V power voltage supplies heat, it is possible to achieve to the accurate temperature controlling of syringe.The design and invention of the device are according to gas-chromatography
The structure and principle of injection port and carry out, the sample that outer vaporizer can gasify inside syringe, stainless steel syringe needle can be with gas
The injection port of chromatography is connected.
After being sampled using the device, sample is sent into by the sample after the gasification of outer vaporizer by the thrust of injector for medical purpose
To gas-chromatography splitter and detector to separate and detect.The device not only has the functions such as sampling, but also with preferable
Stored sample function.When detection in real time can not be realized to sample, used after can sampling, syringe needle is pulled down, extraction is filled
Both ends sealing is put, sample storage is carried out, carries out subsequent analysis as needed.
Embodiment 2
Gas extraction is carried out using the needle type extraction device for concentrating volatile benzene homologues described in embodiment 1 in the present embodiment
Take and sample introduction, comprise the following steps：
1）Before to sample, dilatation syringe 3 is first heated to 280 DEG C of 5 ~ 10min of aging；
2）Adsorbent 4 is inserted in syringe after syringe cooling, is tightly connected syringe needle 1；
3）Syringe needle 1 is inserted in sampling source 9, with air extractor 10（Using pump）Sampling；
4）After completing sampling, air extractor 10 is replaced with into gas injection device 11（5ml injector for medical purpose）, gas injection device extracts in advance
Part inert gas 12；
5）Start temperature controller 8, start to heat dilatation syringe 3；
6）When the temperature of the heat-transfer device of dilatation syringe 3 reaches assigned temperature, syringe needle 1 is inserted into gas chromatograph injection port
13, promote gas injection device to make inert gas 12 by adsorbent 4, while realized by the high temperature of syringe to using target in gas
The thermal desorption of material, and then detected after gas-chromatography separates.
It is that extraction process is described in detail exemplified by extracting the four of low concentration kinds of benzene homologues calibrating gas below.With lazy
Property gas prepare the benzene of trace, toluene, ethylbenzene, the calibrating gas of ortho-xylene in gas sampling bag, by needle type extraction device
With simple gas pump or large volume gas-tight syringe（Air extractor 10）Connection, is adopted as shown in figure 5, needle point is inserted into gas
Sample bag（Sampling source 9）In, open gas pump or pull syringe（Air extractor 10）Push rod, make the calibrating gas in sampler bag
By adsorbent 4, four kinds of object gas are adsorbed by adsorbent.After the completion of extraction, remove large volume syringe or using pump, change
To draw the small size gas-tight syringe of a small amount of inert gas in advance（Gas injection device 11）, prepare with gas chromatograph be combined into
Row thermal desorption and analysis.As shown in fig. 6, insert the needle into the injection port 13 of gas-chromatography, the push rod of pushing syringe makes lazy
Property gas realize pyrolysis to four kinds of target substances by adsorbent, while by means of the high temperature of the outer vaporizer of device itself
Inhale.Four kinds of materials after desorption after gas-chromatography post separation by being detected.Testing result is as shown in Figure 7.
Claims (9)
- A kind of 1. needle type extraction device for concentrating volatile benzene homologues, it is characterised in that：Described needle type extraction device includes the stainless steel syringe needle with needle stand, the expansion being removably tightly connected with needle stand Hold syringe, with dilatation syringe afterbody by be tightly connected reinforcing gas operated device that base is connected and reinforcing gas operated device afterbody with The air extractor or gas injection device that removably is tightly connected；Solid-phase adsorbent is filled with the dilatation syringe, outside syringe Wall is provided with heat-transfer device, and the heat-transfer device is connected with temperature controller, and the dilatation syringe is heat-conducting metal material.
- 2. the needle type extraction device according to claim 1 for concentrating volatile benzene homologues, it is characterised in that：It is described to lead Hot charging is set to the heating wire of uniform winding outside dilatation syringe, the head and the tail both ends connection temperature controller of heating wire.
- 3. the needle type extraction device according to claim 1 for concentrating volatile benzene homologues, it is characterised in that：It is described to take out Device of air is sampling pump or syringe, and the gas injection device is syringe.
- 4. the needle type extraction device according to claim 1 for concentrating volatile benzene homologues, it is characterised in that：It is described to add Gu gas operated device is made up of heat-insulated material.
- 5. the needle type extraction device according to claim 1 for concentrating volatile benzene homologues, it is characterised in that：It is described solid Phase adsorbent is molecular engram fiber coat polymer, the preparation process of molecular engram fiber coat polymer：Be by benzoic acid, 4-vinylpridine, ethyleneglycol dimethacrylate are 1 according to the amount ratio of material:3:20 ratio is dissolved in toluene:Lauryl alcohol Volume ratio is 1:In 12.5 solution, and AIBN initiators being added, ultrasound is coated on fiber after mixing, and is polymerize 24 hours, then It is 1 with volume ratio:4 0.2mol/LNaOH solution elutes with absolute ethyl alcohol mixed liquor, prepares molecular engram fiber coat print Compound.
- 6. the needle type extraction device according to claim 1 for concentrating volatile benzene homologues, it is characterised in that：The expansion It is copper to hold syringe.
- 7. the needle type extraction device according to claim 1 for concentrating volatile benzene homologues, it is characterised in that：The expansion It is 22 ~ 28mm to hold syringe length, and external diameter is 4 ~ 5mm, and internal diameter is 2.5 ~ 3.5mm.
- 8. the needle type extraction device according to claim 1 for concentrating volatile benzene homologues, it is characterised in that：Stainless steel Syringe needle is tip and length is 30 ~ 50mm.
- 9. the application method of the needle type extraction device according to claim 1 for concentrating volatile benzene homologues, its feature It is：Comprise the following steps：1）Before to sample, dilatation syringe is first heated to 280 DEG C of 5 ~ 10min of aging；2）Adsorbent is inserted in dilatation syringe after the cooling of dilatation syringe, is tightly connected syringe needle；3）Insert the needle into sampling source, sampled with air extractor；4）After completing sampling, air extractor is replaced with into gas injection device, gas injection device extracts part inert gas in advance；5）Start temperature controller, start to heat dilatation syringe；6）When the temperature of the heat-transfer device of dilatation syringe reaches 160 ~ 280 DEG C, gas chromatograph injection port is inserted the needle into, is pushed away Dynamic gas injection device makes inert gas by adsorbent, while is realized by the high temperature of syringe to the heat of target substance in sample gas Desorption, and then detected after gas-chromatography separates.
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| CN201711349709.2A CN107860853A (en) | 2017-12-15 | 2017-12-15 | A kind of needle type extraction device and its application method for concentrating volatile benzene homologues |
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| CN201711349709.2A CN107860853A (en) | 2017-12-15 | 2017-12-15 | A kind of needle type extraction device and its application method for concentrating volatile benzene homologues |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109725096A (en) * | 2019-02-15 | 2019-05-07 | 上海市农业科学院 | A kind of collection method and device of floral disc of sunflower volatile matter |
| CN110715832A (en) * | 2019-10-22 | 2020-01-21 | 好维股份有限公司 | Active sampler for breath detection and gas chromatography combined analysis method |
| CN112156497A (en) * | 2020-09-28 | 2021-01-01 | 南方医科大学 | Liquid-liquid electro-extraction device for enriching trace analytes and capable of realizing two phases of non-aqueous mutual solution and application of liquid-liquid electro-extraction device |
| CN114264535A (en) * | 2021-11-29 | 2022-04-01 | 曼哈格检测技术股份有限公司 | Method for preparing solution of volatile solute |
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| CN204502469U (en) * | 2015-03-10 | 2015-07-29 | 福建中烟工业有限责任公司 | A kind of needle-based solid-phase extraction column |
| CN207571088U (en) * | 2017-12-15 | 2018-07-03 | 吉林化工学院 | A kind of needle type extraction device for concentrating volatile benzene homologues |
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2017
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102636595A (en) * | 2012-04-13 | 2012-08-15 | 延边大学 | Continuous gas in-tube solid phase microextraction device combined with gas chromatography for use |
| CN103995069A (en) * | 2014-05-23 | 2014-08-20 | 吉林大学 | Micro-needle trapping device for emergently monitoring volatile and semi-volatile organic compounds and use method |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109725096A (en) * | 2019-02-15 | 2019-05-07 | 上海市农业科学院 | A kind of collection method and device of floral disc of sunflower volatile matter |
| CN110715832A (en) * | 2019-10-22 | 2020-01-21 | 好维股份有限公司 | Active sampler for breath detection and gas chromatography combined analysis method |
| CN112156497A (en) * | 2020-09-28 | 2021-01-01 | 南方医科大学 | Liquid-liquid electro-extraction device for enriching trace analytes and capable of realizing two phases of non-aqueous mutual solution and application of liquid-liquid electro-extraction device |
| CN114264535A (en) * | 2021-11-29 | 2022-04-01 | 曼哈格检测技术股份有限公司 | Method for preparing solution of volatile solute |
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