CN105784887B - The aging equipment and its aging method of thermal desorption pipe - Google Patents

The aging equipment and its aging method of thermal desorption pipe Download PDF

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Publication number
CN105784887B
CN105784887B CN201610132825.8A CN201610132825A CN105784887B CN 105784887 B CN105784887 B CN 105784887B CN 201610132825 A CN201610132825 A CN 201610132825A CN 105784887 B CN105784887 B CN 105784887B
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pipe
thermal desorption
aging
gas
gas circuit
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CN201610132825.8A
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CN105784887A (en
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任雯黎
刘百战
陈磊
吴达
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Shanghai Tobacco Group Co Ltd
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Shanghai Tobacco Group Co Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/06Preparation
    • G01N30/14Preparation by elimination of some components

Abstract

The present invention provides a kind of aging equipment and its aging method of the thermal desorption pipe being related to thermal desorption pipe aging technical field, and aging equipment includes:Hollow base, the hollow base are equipped with gas inflow entrance and several gas flow outlets;The inlet end of several outflow gas circuit pipes, the outflow gas circuit pipe is connected with the corresponding gas flow outlet, and thermal desorption pipe or silently is installed in the outlet side for flowing out gas circuit pipe.It is different using heating pipe sleeve or heating module heating to be carried out to thermal desorption pipe from commercialization ageing device, the present invention is in such a way that air in baking oven heats, more uniform temperature, accurately, without any cold spot, heat spot;And cost is extremely low, and instrument cost is greatly saved.

Description

The aging equipment and its aging method of thermal desorption pipe
Technical field
The present invention relates to thermal desorption pipe aging technical fields, aging equipment more particularly to a kind of thermal desorption pipe and its old Change method.
Background technology
Thermal desorption pipe is commonly used for the primary articles in thermal desorption analysis, is equipped with one or more solid absorbents not Become rusty steel or glass tube.When sampling, air or other gaseous samples pass through from pipe, the absorption that the compound of carrying is loaded in pipe Agent is adsorbed in pipe, after by heating desorption by compound blow out carry out Instrumental Analysis.
In general, thermal desorption pipe is requirement Reusability, is both needed to before each use by aging, in high temperature and centainly Inert gas under, will test in middle pipe that remaining compound purges away in adsorbent last time, and ensure the cleaning of thermal desorption pipe, Reduce background noise, improve the accuracy and reliability of experimental result, reduces use cost.
At present to the aging method of thermal desorption pipe, one is the aging procedures for using thermal desorption instrument included to carry out aging, this Kind one batch of method is only capable of handling a small amount of thermal desorption pipe, haves the shortcomings that operating time length.Furthermore it is also possible to use dedicated quotient Product ageing device carries out aging to thermal desorption pipe, and this instrument is to be heated to thermal desorption pipe by heating pipe sleeve, and heat Usually there is the problems such as temperature control is unstable, and uneven heating is even in pipe sleeve.
Invention content
In view of the foregoing deficiencies of prior art, the technical problem to be solved in the present invention is to provide a kind of structure letter Just the aging equipment and its aging method of, easily operated, homogeneous heating thermal desorption pipe.
In order to solve the above technical problem, the present invention provides a kind of aging equipments of thermal desorption pipe, including:Hollow base, The hollow base is equipped with gas inflow entrance and several gas flow outlets;Several outflow gas circuit pipes, the outflow gas circuit The inlet end of pipe is connected with the corresponding gas flow outlet, and thermal desorption pipe or bored is installed in the outlet side of the outflow gas circuit pipe Head.
Preferably, the aging equipment of the thermal desorption pipe is positioned in baking oven.
Preferably, the gas inflow entrance is set to the top of the hollow base.
Preferably, several gas flow outlets are distributed in the side of the hollow base.
Preferably, each gas flow outlet is connect by corresponding pedestal adapter with the outflow gas circuit pipe.
Preferably, the outlet side of each outflow gas circuit pipe is equipped with tube body adapter.
Preferably, the outflow gas circuit pipe is vertically arranged, and the inlet end of the outflow gas circuit pipe is in the outflow gas circuit The lower section of the outlet side of pipe.
The invention further relates to a kind of aging methods of the aging equipment using above-described thermal desorption pipe, including following step Suddenly:The outlet side that the thermal desorption pipe for carrying out aging will be needed to be mounted on corresponding outflow gas circuit pipe, is not installing thermal desorption pipe It flows out and is installed silently on the outlet side of gas circuit pipe;The aging equipment of thermal desorption pipe is put into baking oven, working gas is passed through into institute State gas inflow entrance and be passed through the hollow base, working gas again respectively by flowing out gas circuit pipe after, flowed out from thermal desorption pipe;It opens Baking oven is opened, the temperature of the baking oven is made to increase, aging is carried out to the thermal desorption pipe, remainingization in the pipe of the thermal desorption pipe Object is closed as working gas is carried over.
Preferably, the flow of the working gas is 50-150mL/min.
Preferably, the temperature raising of the baking oven reaches 300 ° -400 °.
The device of the invention can be as needed, while carrying out agings to several thermal desorption pipes, simple to operation, flexibly and Efficiently, the working time is saved, experimental cost is reduced.With commercialization ageing device using heating pipe sleeve or heating module to thermal desorption pipe It is different to carry out heating, the present invention uses in baking oven by the way of air heating, more uniform temperature, accurate, without any cold spot, overheats Point;And cost is extremely low, and instrument cost is greatly saved.
Description of the drawings
Fig. 1 is shown as the structural schematic diagram 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 the thermal desorption pipe chromatogram of the aging equipment aging using embodiment 1.
Fig. 4 is shown as the chromatogram of the thermal desorption pipe of commodity in use ageing device aging.
Fig. 5 is shown as the aging equipment that will use the thermal desorption pipe of embodiment 1 and the thermal desorption pipe after aging method aging Thermal desorption-gas chromatography/mass spectrometry color of the tobacco effusion object generated in certain brand cigarette cut tobacco drying is measured for thermal desorption method Spectrogram.
Fig. 6 is shown as thermal desorption-gas chromatography/mass spectrometry chromatogram of menthol in surrounding air.
Fig. 7 is shown as remaining the chromatogram of menthol in the thermal desorption pipe using the aging equipment aging of embodiment 1.
Fig. 8 is shown as remaining the chromatogram of menthol in the thermal desorption pipe of commodity in use ageing device.
Drawing reference numeral explanation
100 hollow bases
110 gas inflow entrances
120 gas flow outlets
200 outflow gas circuit pipes
The inlet end of 210 outflow gas circuit pipes
The outlet side of 220 outflow gas circuit pipes
300 thermal desorption pipes
400 silently
500 baking ovens
610 pedestal adapters
620 tube body adapters
710 sealing fixing nuts
800 flow into gas circuit pipe
Specific implementation mode
Illustrate that embodiments of the present invention, those skilled in the art can be by this explanations by particular specific embodiment below Content disclosed by book understands other advantages and effect of the present invention easily.
Please refer to attached drawing.It should be clear that structure, ratio, size etc. depicted in this specification institute accompanying drawings, only coordinating It is enforceable to be not limited to the present invention so that those skilled in the art understands and reads for the revealed content of specification Qualifications, therefore do not have technical essential meaning, the modification of any structure, the change of proportionate relationship or the adjustment of size, It does not influence under the effect of present invention can be generated and the purpose that can reach, should all still fall in disclosed technology contents It obtains in the range of capable of covering.Meanwhile cited such as "upper", "lower", "left", "right", " centre " and " one " in this specification Term, be merely convenient to being illustrated for narration, rather than to limit the scope of the invention, the change of relativeness or Adjustment, in the case where changing technology contents without essence, when being also considered as the enforceable scope 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, hollow base 100 are equipped with gas inflow entrance 110 and several gas flow outlets 120;Several outflow gas circuit pipes 200, flow out gas circuit pipe 200 Inlet end 210 and corresponding gas flow outlet 120 connect, outflow gas circuit pipe 200 be connected to hollow base 100, outflow gas circuit Thermal desorption pipe 300 or silently 400 is installed in the outlet side 220 of pipe 200, and the aging equipment of thermal desorption pipe is positioned in baking oven 500, In the present embodiment, the quantity of outflow gas circuit pipe 200 is 10, one inflow gas of connection on the gas inflow entrance 110 of hollow base 100 Road pipe 800.
The present apparatus is in use, will need the thermal desorption pipe 300 for carrying out aging to be mounted on going out for corresponding outflow gas circuit pipe 200 Gas end 220 installs silently 400, due to not installing on the outlet side 220 for the outflow gas circuit pipe 200 for not installing thermal desorption pipe 300 The outflow gas circuit pipe 200 of thermal desorption pipe 300 is that resistance is smaller compared with the outflow gas circuit pipe 200 of installation thermal desorption pipe 300 Channel, setting silently 400 play sealing function, the outflow gas circuit pipe 200 of thermal desorption pipe 300 are never installed to avoid working gas Outflow;The aging equipment of thermal desorption pipe is put into baking oven 500, working gas is passed through hollow bottom by flowing into gas circuit pipe 800 Seat 100, working gas respectively by flowing out gas circuit pipe 200, flow out again from thermal desorption pipe 300;Baking oven 500 is opened, baking oven 500 is made Temperature increase, aging is carried out to thermal desorption pipe 300, remaining compound is with working gas quilt in the pipe of thermal desorption pipe 300 It takes out of.
Commercialization ageing device carries out heating difference using heating pipe sleeve or heating module to thermal desorption pipe 300, and the present invention adopts It is more uniform temperature, accurate with air mode of heating in baking oven 500, without any cold spot, heat spot.And cost is extremely low, greatlys save Instrument cost.The device of the invention can be as needed, while carrying out aging to several thermal desorption pipes 300, simple to operation, Flexibly and efficiently, the working time is saved, reduces experimental cost.
It is positioned in baking oven 500 for the ease of the aging equipment of thermal desorption pipe, gas inflow entrance 110 is set to hollow bottom The top of seat 100, several gas flow outlets 120 are distributed in the side of hollow base 100, which passes through convenient for working gas Hollow base 100 is passed through outflow gas circuit pipe 200, and working gas is enable to be further separated into several outflow gas circuit pipes 200.
Each gas flow outlet 120 is connect by corresponding pedestal adapter 610 with outflow gas circuit pipe 200, pedestal switching Part 610 be pedestal transfer nut, pedestal adapter 610 convenient for gas flow outlet 120 with outflow gas circuit pipe 200 installation with tear open It unloads.
The outlet side 220 of each outflow gas circuit pipe 200 is equipped with tube body adapter 620, and tube body adapter 620 turns for tube body Connected nut, tube body adapter 620 are convenient for the installation and dismounting of outflow gas circuit pipe 200 and tube body adapter 620.
Outflow gas circuit pipe 200 is vertically arranged, and the inlet end 210 of outflow gas circuit pipe 200 is in the outlet of outflow gas circuit pipe 200 The lower section at end 220, the structure are positioned over convenient for the aging equipment of thermal desorption pipe in baking oven 500, also allow for working gas discharge.
Using the aging method of the aging equipment of the thermal desorption pipe of the present embodiment, include the following steps:It will need to carry out old The thermal desorption pipe 300 of change is mounted on the outlet side 220 of corresponding outflow gas circuit pipe 200, in the outflow for not installing thermal desorption pipe 300 Silently 400 are installed on the outlet side 220 of gas circuit pipe 200;The aging equipment of thermal desorption pipe is put into baking oven 500, work gas is made Body, which enters, to be flowed into gas circuit pipe 800, is passed through hollow base 100 by gas inflow entrance 110 later, working gas leads to respectively again After overcurrent goes out gas circuit pipe 200, flowed out from thermal desorption pipe 300;Baking oven 500 is opened, the temperature of baking oven 500 is made to increase, baking oven 500 Temperature raising reaches 300 ° -400 °, at high temperature, remaining in the pipe of thermal desorption pipe 300 to the progress aging of thermal desorption pipe 300 Compound is carried over working gas.
The flow of working gas is 50-150mL/min, and the flow of working gas ensure that working gas in thermal desorption pipe Flowing can take the remaining compound in thermal desorption pipe 300 out of in 300;Working gas is inert gas, in the present embodiment, The inert gas used can be helium or nitrogen.
Embodiment 2
As depicted in figs. 1 and 2, for use thermal desorption pipe 300 is inserted into the aging equipment of thermal desorption pipe of embodiment 1, Using the aging method of embodiment 1, thermal desorption pipe 300 and the junction of tube body adapter 620 are added using sealing fixing nut 710 With fixation, the use of outflow gas circuit pipe 200 not used silently 400 is blocked, in order to avoid gas leakage.This aging equipment is set to baking oven In 500, working gas helium is opened, the flow for adjusting working gas is 100mL/min, and setting 500 program of baking oven makes baking oven 500 Heating rises to 330 DEG C with 20 DEG C/min, keeps 15min from 40 DEG C;40 DEG C are cooled to 20 DEG C/min again, that is, completes thermal desorption The aging of pipe 300.
The thermal desorption of the thermal desorption pipe 300 of the present embodiment aging-gas chromatography/mass spectrometry chromatogram is shown in Fig. 3.Using identical reality Condition is tested, thermal desorption-gas chromatography/mass spectrometry chromatogram of the thermal desorption pipe 300 of commodity in use ageing device is shown in Fig. 4.
As seen from the figure, compared with the aging techniques of commodity in use ageing device, the thermal desorption pipe 300 of this implementation aging is used Impurities are less, and background is clean, low noise.Test accuracy and reliability higher.
To heat be used for using the thermal desorption pipe 300 after the aging equipment of the thermal desorption pipe of embodiment 1 and aging method aging Desorption method measures the tobacco effusion object generated in certain brand cigarette cut tobacco drying, will be using the thermal desorption pipe of the present embodiment aging 300, under conditions of sampling flow 200mL/min, trap time 10min, the tobacco of continuous online trapping cut tobacco drying generation Escape object, the tobacco effusion object generated in the rear analysis cut tobacco drying using thermal desorption.
Thermal desorption instrument condition
Helium, 15.7psi;The pre-blowing time:5min;Valve temperature:200℃;Transmission line temperature:220℃;Level-one desorption temperature: 250 DEG C, 30min is kept, flow is desorbed:50mL/min, import shunting:50mL/min;Two level desorption temperature:250 DEG C, heating speed Rate:20 DEG C/min, keep 4min;Outlet manifold:30mL/min.
GC conditions
Agilent DB-WAX capillary chromatographic columns, i.d. × 0.25 μm 60m × 0.32mm df;Carrier gas is high-pure helium Gas, transmission line temperature are 220 DEG C, temperature programming:40 DEG C, 5min is kept, 200 DEG C is risen to 4 DEG C/min, keeps 15min, total score Analyse time 60min.
Mass Spectrometry Conditions
Mode, electron energy 70eV are ionized using EI, ion source is 230 DEG C, and level four bars temperature is 150 DEG C, and quality is swept Retouch range:35~350amu, mass spectrograph detection mode:Full scan carries out spectrum library with NIST and Wiley standard spectrums library to data Retrieval.It obtains spectrogram and sees Fig. 5.Obtained qualitative, quantitative is as a result, i.e. certain brand cigarette cut tobacco drying tobacco escapes the important fragrance of object The testing result of ingredient, is shown in Table 1.
The testing result of certain the brand cigarette cut tobacco drying tobacco effusion important fragrance component of object of table 1
Embodiment 3
The thermal desorption pipe 300 of 1 aging of embodiment will be used, in sampling flow 200mL/min, the item of trap time 30min It is continuous to trap mentholated cigarette production environment air under part, the menthol in thermal desorption method determination of the environment air is used later.
Thermal desorption and GC/MS analysis conditions are:
Thermal desorption instrument condition:High pure air 105.5kPa, 15.3psi;Valve temperature:200℃;Pre-blowing:1min;Level-one is de- It is attached:250 DEG C, 5min;Two level is desorbed:250 DEG C, 4min;Transmission line temperature:230℃.
Chromatographic column:DB-Wax capillary columns, i.d. × 0.25 μm 60m × 0.32mm df;Carrier gas:He;Temperature program: 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.Library is composed using WILEY7N and NIST05 spectrums library is retrieved.It obtains spectrogram and sees Fig. 6.
The aging of thermal desorption pipe 300
Aging equipment and aging method, the commercialization ageing device aging of embodiment 1, the aging under similarity condition is respectively adopted The thermal desorption pipe 300 of environment menthol is acquired.300 DEG C of aging temperature, ageing time 15min.Later, heat is de- after measuring aging The content of menthol is remained in attached pipe 300, obtained result is shown in Fig. 6 to Fig. 8 and table 2.As it can be seen that aging equipment of the present invention can will be warm The compound adsorbed in desorption pipe 300 is substantially completely blown out, and residual is extremely low, and the influence to subsequent experimental is minimum, is experimental precision Provide guarantee.
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, the residual compounds that can will be adsorbed in pipe Blowout, realizes recycling for thermal desorption pipe 300, reduces experiment spending.Meanwhile compared with the ageing device of commercialization, this Invention device is heated evenly, and temperature control is more accurate, and use is more flexible, and cost is less expensive, is greatly reducing the same of experimental cost When, the performance of instrument is improved, to provide a kind of good aging technological means for technical staff.
To sum up, the present invention effectively overcomes various shortcoming in the prior art and has high industrial utilization.
The above-described embodiments merely illustrate the principles and effects of the present invention, and is not intended to limit the present invention.It is any ripe The personage for knowing this technology can all carry out modifications and changes to above-described embodiment without violating the spirit and scope of the present invention.Cause This, institute is complete without departing from the spirit and technical ideas disclosed in the present invention by those of ordinary skill in the art such as At all equivalent modifications or change, should by the present invention claim be covered.

Claims (7)

1. a kind of aging equipment of thermal desorption pipe, which is characterized in that including:
Hollow base (100), the hollow base (100) are equipped with gas inflow entrance (110) and several gas flow outlets (120);
Several outflow gas circuit pipes (200), the inlet end (210) of the outflow gas circuit pipe (200) and the corresponding gas stream Export (120) connection, outlet side (220) the installation thermal desorption pipe (300) or silently (400) of the outflow gas circuit pipe (200); The aging equipment of the thermal desorption pipe is positioned in baking oven (500);
The gas inflow entrance (110) is set to the top of the hollow base (100);
The outflow gas circuit pipe (200) is vertically arranged, and the inlet end (210) of the outflow gas circuit pipe (200) is in the outflow The lower section of the outlet side (220) of gas circuit pipe (200).
2. the aging equipment of thermal desorption pipe according to claim 1, it is characterised in that:Several gas flow outlets (120) It is distributed in the side of the hollow base (100).
3. the aging equipment of thermal desorption pipe according to claim 1, it is characterised in that:Each gas flow outlet (120) it is connect with the outflow gas circuit pipe (200) by corresponding pedestal adapter (610).
4. the aging equipment of thermal desorption pipe according to claim 1, it is characterised in that:Each outflow gas circuit pipe (200) outlet side (220) is equipped with tube body adapter (620).
5. the aging method of the aging equipment using the thermal desorption pipe described in any one of claim 1-4, it is characterised in that: Include the following steps:
The outlet side (220) that the thermal desorption pipe (300) for carrying out aging will be needed to be mounted on corresponding outflow gas circuit pipe (200), It does not install and is installed silently (400) on the outlet side (220) of the outflow gas circuit pipe (200) of thermal desorption pipe (300);
The aging equipment of thermal desorption pipe is put into baking oven (500), working gas is passed through by the gas inflow entrance (110) The hollow base (100), working gas again respectively by flowing out gas circuit pipe (200) after, flowed out from thermal desorption pipe (300);
Baking oven (500) is opened, the temperature of the baking oven (500) is made to increase, aging is carried out to the thermal desorption pipe (300), it is described Remaining compound is carried over working gas in the pipe of thermal desorption pipe (300).
6. the aging equipment of thermal desorption pipe according to claim 5, it is characterised in that:The flow of the working gas is 50-150mL/min。
7. the aging equipment of thermal desorption pipe according to claim 5, it is characterised in that:The temperature liter of the baking oven (500) Up to 300 DEG C -400 DEG C.
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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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JPH07275601A (en) * 1994-04-08 1995-10-24 Hitachi Ltd Automatic solid-phase extracting apparatus with solid-phase extraction column reproducing function
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CN2884202Y (en) * 2006-03-20 2007-03-28 深港产学研基地 Multi-functional aging test dry oven
CN101337178A (en) * 2008-04-25 2009-01-07 浙江树人大学 Development of novel absorbent in adsorption heat desorption pipe
CN202361796U (en) * 2011-11-24 2012-08-01 上海欧萨环境资源管理咨询有限公司 Ageing oven
CN103226139A (en) * 2013-03-18 2013-07-31 上海烟草集团有限责任公司 Process for analyzing gas-phase total components in cigarette mainstream smoke through airbag-thermal desorption-gas chromatography/mass spectrometry method
CN204439604U (en) * 2015-03-16 2015-07-01 常州磐诺仪器有限公司 A kind of VOC thermal desorption pipe

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS58148959A (en) * 1982-02-28 1983-09-05 Shimadzu Corp Aging method of glass column
JPH07275601A (en) * 1994-04-08 1995-10-24 Hitachi Ltd Automatic solid-phase extracting apparatus with solid-phase extraction column reproducing function
CN2773662Y (en) * 2005-03-18 2006-04-19 曾建强 Ageing furnace of pyrolyzing tube
CN2884202Y (en) * 2006-03-20 2007-03-28 深港产学研基地 Multi-functional aging test dry oven
CN101337178A (en) * 2008-04-25 2009-01-07 浙江树人大学 Development of novel absorbent in adsorption heat desorption pipe
CN202361796U (en) * 2011-11-24 2012-08-01 上海欧萨环境资源管理咨询有限公司 Ageing oven
CN103226139A (en) * 2013-03-18 2013-07-31 上海烟草集团有限责任公司 Process for analyzing gas-phase total components in cigarette mainstream smoke through airbag-thermal desorption-gas chromatography/mass spectrometry method
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