CN105784887A - Ageing device for thermal desorption pipes and ageing method thereof - Google Patents
Ageing device for thermal desorption pipes and ageing method thereof Download PDFInfo
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- CN105784887A CN105784887A CN201610132825.8A CN201610132825A CN105784887A CN 105784887 A CN105784887 A CN 105784887A CN 201610132825 A CN201610132825 A CN 201610132825A CN 105784887 A CN105784887 A CN 105784887A
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- thermal desorption
- pipe
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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
- G01N30/14—Preparation by elimination of some components
Abstract
The invention provides an ageing device for thermal desorption pipes and an ageing method thereof, and relates to the technical field of ageing thermal desorption pipes.The ageing device comprises a hollow base and multiple flowing-out gas channel pipes, wherein a gas flowing-in opening and multiple gas flowing-out opening are formed in the hollow base, and thermal desorption pipes or choke plugs are installed at gas outlet ends of the flowing-out gas channel pipes.Different from the mode that a commercial ageing device uses a heating pipe sleeve or heating module for heating the thermal desorption pipes, the mode of air heating in an oven is adopted, temperature is more uniform and accurate, no cold point or overheated point exists, the ageing device is low in manufacturing cost, and therefore device cost is greatly reduced.
Description
Technical field
The present invention relates to the aging technical field of thermal desorption pipe, particularly relate to aging equipment and the aging method thereof of a kind of thermal desorption pipe.
Background technology
Thermal desorption pipe is commonly used for the primary articles during thermal desorption is analyzed, and is equipped with rustless steel or the glass tubing of one or more solid absorbents.During sampling, air or other gaseous samples process from pipe, compound blowout, in pipe, rear is carried out Instrumental Analysis by heating desorption by the adsorbent that the compound carried is loaded in pipe.
In general, thermal desorption pipe is requirement Reusability, it is both needed to through overaging before using every time, under high temperature and certain inert gas, in being tested last time, in pipe internal adsorption agent, the compound of residual purges away, it is ensured that the cleaning of thermal desorption pipe, reduces background noise, improve accuracy and the reliability of experimental result, reduce use cost.
Aging method to thermal desorption pipe at present, a kind of is use the aging procedure that thermal desorption instrument carries to carry out aging, and this method one batch is only capable of processing a small amount of thermal desorption pipe, the shortcoming that there is operating time length.Furthermore it is also possible to use special commercialization ageing device to carry out aging to thermal desorption pipe, this instrument is thermal desorption pipe to be heated by heating pipe box, and heats pipe box and be usually present temperature and control instability, the problem such as be heated uneven.
Summary of the invention
The shortcoming of prior art in view of the above, the technical problem to be solved in the present invention is in that to provide aging equipment and the aging method thereof of the thermal desorption pipe of a kind of features simple structure, easily operated, homogeneous heating.
In order to solve above-mentioned technical problem, the present invention provides the aging equipment of a kind of thermal desorption pipe, including: hollow base, described hollow base is provided with gas inflow entrance and several gas flow outlet；Several flow out gas circuit pipe, and the inlet end of described outflow gas circuit pipe connects with corresponding described gas flow outlet, and thermal desorption pipe or silently is installed in the outlet side of described outflow gas circuit pipe.
Preferably, the aging equipment of described thermal desorption pipe is positioned in baking oven.
Preferably, described gas inflow entrance is arranged at the top of described hollow base.
Preferably, several gas flow outlet are distributed in the side of described hollow base.
Preferably, each described gas flow outlet is connected with described outflow gas circuit pipe by corresponding pedestal adaptor.
Preferably, the outlet side of each described outflow gas circuit pipe is provided with body adaptor.
Preferably, described outflow gas circuit pipe is vertically arranged, and the inlet end of described outflow gas circuit pipe is in the lower section of the outlet side of described outflow gas circuit pipe.
The invention still further relates to the aging method of a kind of aging equipment adopting above-described thermal desorption pipe, comprise the following steps: be arranged on the corresponding outlet side flowing out gas circuit pipe by needing to carry out aging thermal desorption pipe, the outlet side of outflow gas circuit pipe not installing thermal desorption pipe is installed silently；Putting in baking oven by the aging equipment of thermal desorption pipe, by described gas inflow entrance, working gas is passed into described hollow base, working gas respectively through after flowing out gas circuit pipe, goes out from thermal desorption pipe flow again；Opening baking oven, make the temperature of described baking oven raise, carry out aging to described thermal desorption pipe, the compound remained in the pipe of described thermal desorption pipe is carried over along with working gas.
Preferably, the flow of described working gas is 50-150mL/min.
Preferably, the temperature of described baking oven raises and reaches 300 °-400 °.
Some thermal desorption pipes can as required, be carried out aging by assembly of the invention simultaneously, simple to operation, flexible and efficient, saves the working time, reduces experimental cost.Using heating pipe box or heating module to be heated different to thermal desorption pipe from commercialization ageing device, the present invention adopts the mode that baking oven air heat, more uniform temperature, accurate, without any cold spot, heat spot；And cost is extremely low, is greatly saved instrument cost.
Accompanying drawing explanation
Fig. 1 is shown as the structural representation of the aging equipment of the thermal desorption pipe of embodiment 1.
Fig. 2 is shown as the vertical view internal structure schematic diagram of the aging equipment of the thermal desorption pipe of embodiment 1.
Fig. 3 is shown as using the aging thermal desorption pipe chromatogram of aging equipment of embodiment 1.
Fig. 4 is shown as the chromatogram of the aging thermal desorption pipe of commodity in use ageing device.
Fig. 5 is shown as that the thermal desorption pipe after aging to the aging equipment of thermal desorption pipe and aging method that adopt embodiment 1 is used for thermal desorption method and measures the thermal desorption-gas chromatography/mass spectrometry chromatogram of the Nicotiana tabacum L. effusion thing produced in certain brand cigarette cut tobacco drying.
Thermal desorption-gas chromatography/mass spectrometry chromatogram that Fig. 6 is shown as in surrounding air menthol.
Fig. 7 is shown as using the chromatogram remaining menthol in the aging thermal desorption pipe of aging equipment of embodiment 1.
Fig. 8 is shown as remaining in the thermal desorption pipe of commodity in use ageing device the chromatogram of menthol.
Drawing reference numeral explanation
100 hollow bases
110 gas inflow entrances
120 gas flow outlet
200 flow out gas circuit pipe
210 inlet ends flowing out gas circuit pipe
220 outlet sides flowing out gas circuit pipe
300 thermal desorption pipes
400 silently
500 baking ovens
610 pedestal adaptors
620 body adaptors
710 seal fixing nut
800 flow into gas circuit pipe
Detailed description of the invention
By particular specific embodiment, embodiments of the present invention being described below, those skilled in the art the content disclosed by this specification can understand other advantages and effect of the present invention easily.
Refer to accompanying drawing.Notice, the structure of this specification institute accompanying drawings depicted, ratio, size etc., all only in order to coordinate the disclosed content of description, understand for those skilled in the art and read, it is not limited to the enforceable qualifications of the present invention, therefore do not have technical essential meaning, the adjustment of the modification of any structure, the change of proportionate relationship or size, under not affecting effect that the present invention can be generated by and the purpose that can reach, all should still drop on disclosed technology contents and obtain in the scope that can contain.Simultaneously, in this specification cited as " on ", D score, "left", "right", " centre " and " one " etc. term, it is merely convenient to understanding of narration, and it is not used to limit the enforceable scope of the present invention, the change of its relativeness or adjustment, changing under technology contents without essence, when being also considered as the enforceable category of the present invention.
Embodiment 1
As depicted in figs. 1 and 2, the aging equipment of the thermal desorption pipe of the present embodiment includes: hollow base 100, and hollow base 100 is provided with gas inflow entrance 110 and several gas flow outlet 120；Several flow out gas circuit pipe 200, the inlet end 210 flowing out gas circuit pipe 200 connects with corresponding gas flow outlet 120, flow out gas circuit pipe 200 to connect with hollow base 100, thermal desorption pipe 300 or silently 400 are installed in the outlet side 220 flowing out gas circuit pipe 200, the aging equipment of thermal desorption pipe is positioned in baking oven 500, in the present embodiment, the quantity flowing out gas circuit pipe 200 is 10, and the gas inflow entrance 110 of hollow base 100 connects an inflow gas circuit pipe 800.
When this device uses, it is arranged on the corresponding outlet side 220 flowing out gas circuit pipe 200 by needing to carry out aging thermal desorption pipe 300, the outlet side 220 of outflow gas circuit pipe 200 not installing thermal desorption pipe 300 is installed silently 400, owing to not installing the outflow gas circuit pipe 200 of thermal desorption pipe 300 compared with the outflow gas circuit pipe 200 installing thermal desorption pipe 300, it it is the passage that resistance is less, arrange and silently 400 play sealing function, to avoid the outflow gas circuit pipe 200 that working gas never installs thermal desorption pipe 300 to flow out；Being put into by the aging equipment of thermal desorption pipe in baking oven 500, by flowing into gas circuit pipe 800, working gas is passed into hollow base 100, working gas respectively through flowing out gas circuit pipe 200, flows out from thermal desorption pipe 300 again；Opening baking oven 500, make the temperature of baking oven 500 raise, carry out aging to thermal desorption pipe 300, the compound remained in the pipe of thermal desorption pipe 300 is carried over along with working gas.
Commercialization ageing device uses heating pipe box or heating module that thermal desorption pipe 300 is heated difference, and the present invention adopts baking oven 500 air mode of heating, more uniform temperature, accurately, without any cold spot, heat spot.And cost is extremely low, is greatly saved instrument cost.Some thermal desorption pipes 300 can as required, be carried out aging by assembly of the invention simultaneously, simple to operation, flexible and efficient, saves the working time, reduces experimental cost.
Aging equipment for the ease of thermal desorption pipe is positioned in baking oven 500, gas inflow entrance 110 is arranged at the top of hollow base 100, several gas flow outlet 120 are distributed in the side of hollow base 100, this structure is easy to working gas and is passed into outflow gas circuit pipe 200 by hollow base 100, and enables working gas to be further separated in several outflow gas circuit pipes 200.
Each gas flow outlet 120 is connected with flowing out gas circuit pipe 200 by corresponding pedestal adaptor 610, and pedestal adaptor 610 is pedestal switching nut, and pedestal adaptor 610 is easy to gas flow outlet 120 and installation and the dismounting of flowing out gas circuit pipe 200.
The outlet side 220 of each outflow gas circuit pipe 200 is provided with body adaptor 620, and body adaptor 620 is body switching nut, and body adaptor 620 is easy to flow out installation and the dismounting of gas circuit pipe 200 and body adaptor 620.
Flowing out gas circuit pipe 200 to be vertically arranged, the inlet end 210 flowing out gas circuit pipe 200 is in the lower section of the outlet side 220 flowing out gas circuit pipe 200, and this structure is easy to the aging equipment of thermal desorption pipe and is positioned in baking oven 500, also allows for working gas and discharges.
Adopt the aging method of the aging equipment of the thermal desorption pipe of the present embodiment, comprise the following steps: be arranged on the corresponding outlet side 220 flowing out gas circuit pipe 200 by needing to carry out aging thermal desorption pipe 300, the outlet side 220 of outflow gas circuit pipe 200 not installing thermal desorption pipe 300 is installed silently 400；Being put in baking oven 500 by the aging equipment of thermal desorption pipe, make working gas enter in inflow gas circuit pipe 800, pass into hollow base 100 by gas inflow entrance 110 afterwards, working gas respectively through after flowing out gas circuit pipe 200, flows out from thermal desorption pipe 300 again；Opening baking oven 500, make the temperature of baking oven 500 raise, the temperature of baking oven 500 raises and reaches 300 °-400 °, at high temperature, carries out aging to thermal desorption pipe 300, and the compound remained in the pipe of thermal desorption pipe 300 is carried over along with working gas.
The flow of working gas is 50-150mL/min, and the flow of working gas ensure that working gas flows in thermal desorption pipe 300 and can be taken out of by the compound of the residual in thermal desorption pipe 300；Working gas is noble gas, and in the present embodiment, the noble gas of employing can be helium or nitrogen.
Embodiment 2
As depicted in figs. 1 and 2, stand-by thermal desorption pipe 300 is inserted in the aging equipment of thermal desorption pipe of embodiment 1, adopt the aging method of embodiment 1, thermal desorption pipe 300 and the junction of body adaptor 620 adopt the fixing nut 710 of sealing to be fixed, the outflow gas circuit pipe 200 not used adopts silently 400 to be blocked, in order to avoid gas leakage.Being arranged at by this aging equipment in baking oven 500, open working gas helium, the flow regulating working gas is 100mL/min, sets baking oven 500 program and makes baking oven 500 heat up, from 40 DEG C, rise to 330 DEG C with 20 DEG C/min, keeps 15min；It is cooled to 40 DEG C with 20 DEG C/min again, namely completes the aging of thermal desorption pipe 300.
The thermal desorption of the thermal desorption pipe 300 that the present embodiment is aging-gas chromatography/mass spectrometry chromatogram is shown in Fig. 3.Adopting same experimental conditions, the thermal desorption of the thermal desorption pipe 300 of commodity in use ageing device-gas chromatography/mass spectrometry chromatogram is shown in Fig. 4.
As seen from the figure, compared with the aging techniques of commodity in use ageing device, thermal desorption pipe 300 impurities using this enforcement aging is less, and background is clean, and noise is low.Experiment accuracy and reliability are higher.
Thermal desorption pipe 300 after aging to the aging equipment of thermal desorption pipe and aging method that adopt embodiment 1 is used for thermal desorption method and measures the Nicotiana tabacum L. effusion thing produced in certain brand cigarette cut tobacco drying, the thermal desorption pipe 300 that the present embodiment is aging will be adopted, at sampling flow 200mL/min, when trap time 10min, the Nicotiana tabacum L. effusion thing of online trapping cut tobacco drying generation continuously, the rear Nicotiana tabacum L. using thermal desorption to analyze generation in cut tobacco drying effusion thing.
Thermal desorption instrument condition
Helium, 15.7psi；Pre-blowing time: 5min；Valve temperature: 200 DEG C；Transmission line temperature: 220 DEG C；One-level desorption temperature: 250 DEG C, keeps 30min, desorption flow: 50mL/min, and import taps: 50mL/min；Two grades of desorption temperatures: 250 DEG C, heating rate: 20 DEG C/min, keep 4min；Outlet manifold: 30mL/min.
GC conditions
AgilentDB-WAX capillary chromatographic column, 60m × 0.32mmi.d. × 0.25 μm df；Carrier gas is high-purity helium, and transmission line temperature is 220 DEG C, temperature programming: 40 DEG C, keeps 5min, rises to 200 DEG C with 4 DEG C/min, keeps 15min, bulk analysis time 60min.
Mass Spectrometry Conditions
Adopting EI to ionize mode, electron energy is 70eV, and ion source is 230 DEG C, and level Four bar temperature is 150 DEG C, mass scan range: 35～350amu, mass spectrograph detection mode: full scan, uses NIST and Wiley standard spectrum storehouse that data are carried out library searching.Obtain spectrogram and see Fig. 5.The qualitative, quantitative result obtained, the i.e. testing result of certain brand cigarette cut tobacco drying Nicotiana tabacum L. effusion important fragrance component of thing, in Table 1.
The testing result of certain brand cigarette cut tobacco drying Nicotiana tabacum L. of table 1 effusion important fragrance component of thing
Embodiment 3
The thermal desorption pipe 300 that embodiment 1 is aging will be adopted, at sampling flow 200mL/min, when trap time 30min, trapping mentholated cigarette production environment air continuously, use thermal desorption method to measure the menthol in surrounding air afterwards.
Thermal desorption and GC/MS analysis condition be:
Thermal desorption instrument condition: high pure air 105.5kPa, 15.3psi；Valve temperature: 200 DEG C；Pre-blowing: 1min；One-level desorption: 250 DEG C, 5min；Two grades of desorptions: 250 DEG C, 4min；Transmission line temperature: 230 DEG C.
Chromatographic column: DB-Wax capillary column, 60m × 0.32mmi.d. × 0.25 μm df；Carrier gas: He；Heating schedule: 150 DEG C, 5 DEG C/min rises to 185 DEG C, then rises to 230 DEG C with 30 DEG C/min, keeps 6.5min.
Mass spectrograph detection mode: SIM.Use WILEY7N to compose storehouse and NIST05 composes storehouse and retrieves.Obtain spectrogram and see Fig. 6.
Thermal desorption pipe 300 aging
It is respectively adopted the aging equipment of embodiment 1 and aging method, commercialization ageing device aging, the aging thermal desorption pipe 300 having gathered environment menthol under similarity condition.Aging temperature 300 DEG C, ageing time 15min.Afterwards, measuring the content remaining menthol in aging after heat desorption pipe 300, the result obtained is shown in Fig. 6 to Fig. 8 and table 2.Visible, the compound of absorption in thermal desorption pipe 300 can substantially completely be blown out by aging equipment of the present invention, remains extremely low, and the impact of subsequent experimental is minimum, provides guarantee for experimental precision.
Menthol content in 2 three kinds of thermal desorption pipes 300 of table
Therefore, the aging method of a kind of thermal desorption pipe 300 provided by the invention, it is possible to the residual compounds blowout will adsorbed in pipe, it is achieved that recycling of thermal desorption pipe 300, reduces experiment spending.Meanwhile, compared with commercial ageing device, apparatus of the present invention are heated evenly, temperature control is more accurate, uses more flexible, and cost is less expensive, while greatly reducing experimental cost, improve the performance of instrument, thus providing a kind of good aging technological means for technical staff.
To sum up, the present invention effectively overcomes various shortcoming of the prior art and has high industrial utilization.
Above-described embodiment is illustrative principles of the invention and effect thereof only, not for the restriction present invention.Above-described embodiment all under the spirit and category of the present invention, can be modified or change by any those skilled in the art.Therefore, art has usually intellectual such as modifying without departing from all equivalences completed under disclosed spirit and technological thought or change, must be contained by the claim of the present invention.
Claims (10)
1. the aging equipment of a thermal desorption pipe, it is characterised in that including:
Hollow base (100), described hollow base (100) is provided with gas inflow entrance (110) and several gas flow outlet (120)；
Several flow out gas circuit pipe (200), the inlet end (210) of described outflow gas circuit pipe (200) connects with corresponding described gas flow outlet (120), and thermal desorption pipe (300) or silently (400) is installed in the outlet side (220) of described outflow gas circuit pipe (200).
2. the aging equipment of thermal desorption pipe according to claim 1, it is characterised in that: the aging equipment of described thermal desorption pipe is positioned in baking oven (500).
3. the aging equipment of thermal desorption pipe according to claim 1, it is characterised in that: described gas inflow entrance (110) is arranged at the top of described hollow base (100).
4. the aging equipment of thermal desorption pipe according to claim 1, it is characterised in that: several gas flow outlet (120) are distributed in the side of described hollow base (100).
5. the aging equipment of thermal desorption pipe according to claim 1, it is characterised in that: each described gas flow outlet (120) is connected with described outflow gas circuit pipe (200) by corresponding pedestal adaptor (610).
6. the aging equipment of thermal desorption pipe according to claim 1, it is characterised in that: the outlet side (220) of each described outflow gas circuit pipe (200) is provided with body adaptor (620).
7. the aging equipment of thermal desorption pipe according to claim 1, it is characterized in that: described outflow gas circuit pipe (200) is vertically arranged, the inlet end (210) of described outflow gas circuit pipe (200) is in the lower section of the outlet side (220) of described outflow gas circuit pipe (200).
8. adopt in claim 1-7 the aging method of the aging equipment of thermal desorption pipe described in any one, it is characterised in that: comprise the following steps:
It is arranged on the corresponding outlet side (220) flowing out gas circuit pipe (200) by needing to carry out aging thermal desorption pipe (300), installs silently (400) the outlet side (220) of outflow gas circuit pipe (200) not installing thermal desorption pipe (300) is upper；The aging equipment of thermal desorption pipe is put in baking oven (500), working gas is passed into described hollow base (100) by described gas inflow entrance (110), working gas is again respectively through, after flowing out gas circuit pipe (200), flowing out from thermal desorption pipe (300)；
Opening baking oven (500), make the temperature of described baking oven (500) raise, carry out aging to described thermal desorption pipe (300), the compound remained in the pipe of described thermal desorption pipe (300) is carried over along with working gas.
9. the aging equipment of thermal desorption pipe according to claim 8, it is characterised in that: the flow of described working gas is 50-150mL/min.
10. the aging equipment of thermal desorption pipe according to claim 9, it is characterised in that: the temperature of described baking oven (500) raises and reaches 300 °-400 °.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108295786A (en) * | 2018-04-13 | 2018-07-20 | 绿城农科检测技术有限公司 | A kind of thermal desorption ageing device |
| CN110548734A (en) * | 2018-05-30 | 2019-12-10 | 株式会社岛津制作所 | Collector tube aging device and flow control method for collector tube aging |
| CN110548735A (en) * | 2018-05-30 | 2019-12-10 | 株式会社岛津制作所 | Multi-channel flow output device |
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| CN108295786A (en) * | 2018-04-13 | 2018-07-20 | 绿城农科检测技术有限公司 | A kind of thermal desorption ageing device |
| CN110548734A (en) * | 2018-05-30 | 2019-12-10 | 株式会社岛津制作所 | Collector tube aging device and flow control method for collector tube aging |
| CN110548735A (en) * | 2018-05-30 | 2019-12-10 | 株式会社岛津制作所 | Multi-channel flow output device |
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| CN105784887B (en) | 2018-09-25 |
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