CN104458970B - A kind of thermal desorption device - Google Patents
A kind of thermal desorption device Download PDFInfo
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- CN104458970B CN104458970B CN201310419737.2A CN201310419737A CN104458970B CN 104458970 B CN104458970 B CN 104458970B CN 201310419737 A CN201310419737 A CN 201310419737A CN 104458970 B CN104458970 B CN 104458970B
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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
- G01N30/12—Preparation by evaporation
- G01N2030/126—Preparation by evaporation evaporating sample
- G01N2030/128—Thermal desorption analysis
Abstract
The present invention relates to sample detection technical field, it is thermal desorption device that is a kind of and gas chromatograph coupling, be mainly used in solid-phase microextraction rod, stir bar sorptive extraction, bundling capillary pipe solid phase micro-extraction pipe and fill the thermal desorption of adsorption column, by the trace components fast desorption of institute's adsorption and enrichment out.This device is by heating tube, and internal lining pipe, O-ring seal, internal lining pipe pressure cap, internal lining pipe base, the adiabatic ring of internal lining pipe base, desorption device base, sample conveying tube, desorb purges gas circuit, desorption distributary gas circuit, and heater strip and temperature control element composition.Sample component completes thermal desorption in internal lining pipe, and the heating of sample conveying tube is completed jointly by the heat transfer of cap on heating tube and gas phase chromatic spectrum sample feeder, and by the adiabatic environmental protection temperature of internal lining pipe base.When desorption temperature 300 DEG C, this thermal desorption device is residual lower than 0.1% to the component desorb of boiling point less than 430 DEG C, the advantage such as have desorb sample channel cold area free, firing rate is fast, power consumption is low.
Description
Technical field
The present invention relates to sample detection technical field, belong to analytical chemistry sample pretreatment apparatus, for a kind of with the thermal desorption device of gas chromatograph coupling, be mainly used in solid-phase microextraction rod, stir bar sorptive extraction, bundling capillary pipe solid phase micro-extraction pipe and fill the thermal desorption of adsorption column, by the trace components fast desorption of institute's adsorption and enrichment out.
Background technology
Solid phase micro-extraction technique (SPME) is dissolved on extraction Stationary liquid by the target components absorption in sample or absorption, to reach the object of enrich target component, is a kind of important Sample Pretreatment Technique Used during organic micro-pollutant is analyzed.Due to simple to operate, not with an organic solvent, concentration effect is good, this technology is developed rapidly.Solid phase micro-extraction technique is general with gas chromatograph coupling, and analysis thing gets off from desorb extraction phase by the mode of employing thermal desorption, and the analysis thing desorbed is incorporated in gas chromatographic column and analyzes by desorb carrier gas.Detect because the target components be enriched to can enter gas chromatograph completely, drastically increase the sensitivity of analytical approach.The desorb of fiber pin type solid-phase microextraction directly can complete in gas chromatographic sample introduction device, thus avoids the special thermal desorption device of use.Solid-phase microextraction rod, stir bar sorptive extraction, bundling capillary pipe solid phase micro-extraction pipe and fill other the solid phase micro-extraction device such as adsorption column and then need special thermal desorption device to complete desorb and chromatography column feed materials.
In the prior art, the device (Chinese patent: ZL200410046349.5) for sorptive bar solid phase extraction hot parser can desorb boiling point T completely
bpthe component that specific heat desorption temperature T is lower slightly.In this Patent design, the region A of sample conveying tube is exported to from internal lining pipe, and there is cold-zone in the region B between sample conveying tube to chromatic spectrum sample feeder, make thermal desorption high boiling component out residual in A and B two regions, reduce sample recovery rate and desorb repeatability, and boiling point can not distillate higher than the component of thermal desorption temperature.Meanwhile, the design be not fixedly connected with between desorption device with gas chromatographic sample introduction device, in use desorption device fixedly need external unit auxiliary fixing.In addition, desorb carrier gas introduces from the pressure cap of internal lining pipe, uses very inconvenient.
Summary of the invention
For overcoming the defect designed in existing patented technology, the invention provides a kind of thermal desorption device.In the apparatus, region A between internal lining pipe outlet and sample conveying tube is heated by heating tube and desorb carrier gas, and being incubated by thermal insulation material the cold spot eliminating A district, the part B that sample conveying tube draws pyrolysis haustorium is heated by the heat conduction of cap on gas chromatographic sample introduction device.The cold-zone of sample transfer stream is eliminated in above-mentioned design, significantly reduces the residual of sample component, improves thermal desorption efficiency, save heat energy simultaneously.
For achieving the above object, a kind of thermal desorption device provided by the invention, comprises heating tube, heater strip, outer sleeve, internal lining pipe, internal lining pipe pressure head, desorption device upper cover, internal lining pipe pressure cap, internal lining pipe base, the adiabatic ring of internal lining pipe base, sample conveying tube fastening pressure cap, sample conveying tube, desorption device base, desorb purges gas circuit and desorb shunting gas circuit, it is characterized in that:
Heating tube, outer sleeve and internal lining pipe are the hollow cylindrical structure of upper/lower terminal opening, and coaxially arrange; Heating tube outside wall surface is wound with heater strip, and heating tube is placed in outer sleeve inside, and outer sleeve, for the protection of heating tube, is placed with internal lining pipe in heating tube; Be provided with desorption device upper cover in outer sleeve upper end open place, lower ending opening place is provided with resolver base;
Be provided with internal lining pipe pressure head in the upper end open place of internal lining pipe, the lower end of internal lining pipe pressure head is provided with groove, and on groove side wall, radial direction is provided with an annular groove, is provided with the first O-ring seal in annular groove; The upper end of internal lining pipe is stretched out in heating tube, is placed in the lower end groove of internal lining pipe pressure head through the first O-ring seal, is sealed between internal lining pipe pressure head and the inner chamber of heating tube by the first O-ring seal; The upper end outside wall surface of internal lining pipe pressure head is radially provided with annular protrusion and forms first order ring-shaped step, the lower end outer wall face of internal lining pipe pressure head radially caves inward and forms second level ring-shaped step, the second O-ring seal and the 3rd O-ring seal is placed respectively on first order ring-shaped step, second level ring-shaped step, an annular groove is radially provided with in the middle of two-stage step, annular groove is provided with through hole, leads in the lower end groove of internal lining pipe pressure head as the first aperture;
Desorption device upper cover is a cylinder, upper end internal face is radially recessed to form first order ring-shaped step, lower end inner wall face is radially provided with annular protrusion and forms second level ring-shaped step, desorption device upper cover internal face above first order ring-shaped step is provided with internal thread, be provided with through hole between first order ring-shaped step and second level ring-shaped step, purge gas circuit as parsing; Internal lining pipe pressure head is placed in desorption device upper cover, and internal lining pipe pressure head and desorption device upper cover are connected by the two-stage step arranged respectively above them, resolves the annular groove purging gas circuit middle with internal lining pipe pressure head two-stage step and is connected; First aperture of desorb sweep gas route internal lining pipe pressure head enters, with the inner space of internal lining pipe; The externally threaded internal lining pipe pressure cap of band is provided with in the upper end open place of desorption device upper cover, the internal thread of desorption device upper cover upper end inwall and the external thread of internal lining pipe pressure cap outer peripheral edges are screwed, both can spin fixing, compress the second O-ring seal and the 3rd O-ring seal of internal lining pipe pressure head outside, sealed between desorption device upper cover and internal lining pipe pressure head whereby;
The adiabatic ring of internal lining pipe base is the hollow cylindrical structure of a upper/lower terminal opening, and inside is provided with internal lining pipe base; The upper end of internal lining pipe base is provided with groove, on groove side wall, radial direction is provided with an annular groove, the 4th O-ring seal is provided with in annular groove, the lower end of internal lining pipe is stretched out in heating tube, be placed in the upper recess of internal lining pipe base through the 4th O-ring seal, sealed by the 4th O-ring seal between internal lining pipe base and heating tube inner chamber; Through hole is provided with, as desorption distributary gas circuit in internal lining pipe base upper recess lower side wall; Internal lining pipe base lower end is provided with tapped groove, is provided with through hole between internal lining pipe base upper recess and lower end groove;
Be provided with through hole with externally threaded sample conveying tube fastening pressure cap central axis place, internal lining pipe base and sample conveying tube fastening pressure cap are screwed by the screw thread on it; The upper end of sample conveying tube is passed sample conveying tube fastening pressure cap, after its outer sheathed kapillary cutting ferrule, is stretched to the through hole of internal lining pipe base, the intracavity inter-connection of sample conveying tube and internal lining pipe again; The lower end of sample conveying tube is connected with gas chromatographic sample introduction device through sample introduction pad; The lower end of sample conveying tube fastening pressure cap is provided with groove, and the groove of sample conveying tube fastening pressure cap is buckled on the nut of gas chromatographic sample introduction device; Nut is for compressing sample introduction pad;
Desorption device base is hollow closed container, and closed container upper/lower terminal is provided with opening, and the lower end of outer sleeve and the adiabatic ring of internal lining pipe base are set in desorption device base by closed container upper/lower terminal opening.
Described thermal desorption device, the adiabatic ring of internal lining pipe base described in it is made by the high temperature resistant and materials processing of thermal insulation, can be high temperature polymeric materials or pottery, high temperature polymeric materials be as bakelite, teflon, polyetheretherketone, polyethersulfone ketone or polyimide.
Described thermal desorption device, described in it, heating tube outside wall surface is provided with thermopair, and thermopair is connected with a temperature controller by wire with heater strip.
Described thermal desorption device, heating tube, outer sleeve, internal lining pipe pressure head, resolver upper cover, internal lining pipe pressure cap described in it, internal lining pipe base, sample conveying tube fastening pressure cap is made by stainless steel material or other metal materials.
Described thermal desorption device, internal lining pipe described in it is quartz or the glass tube of lower end closing in.
Described thermal desorption device, sample conveying tube described in it is with the quartz capillary of polyimide protective finish or the inwall stainless steel capillary through process of deactivating.
When adopting said apparatus to carry out thermal desorption, start-up temperature controller heats heating tube, and the component in internal lining pipe is heated and is desorbed.Desorb sweep gas enters internal lining pipe from the first aperture of internal lining pipe pressure head, enters gas chromatography carry out compartment analysis with the component desorbed through sample conveying tube; Desorption distributary gas circuit is used for where necessary the constituent part desorbed being discharged desorption device, prevents gas chromatographic column from transshipping.
Enter in the process of gas chromatographic sample introduction device at the sample component steam of thermal desorption by sample conveying tube, if the temperature of sample conveying tube is more much lower than internal lining pipe inside, constituent part steam-condensation will be caused inner at sample conveying tube, gas chromatographic sample introduction device cannot be entered, cause desorb to remain.For the component that boiling point is higher, residual phenomena is more serious.In said apparatus, internal lining pipe base can remain on higher temperature by the heat transfer of heating tube; Meanwhile, sample conveying tube fastening pressure cap remains on higher temperature by the heat transfer of cap on gas chromatographic sample introduction device.Like this, sample conveying tube just can be heated by internal lining pipe base and sample conveying tube fastening pressure cap, and is incubated by the adiabatic ring of internal lining pipe base, it is made to remain on higher temperature, effectively eliminate cold-zone, avoid components condense that desorb gets off in sample conveying tube, cause desorb to remain.For the desorb of high boiling component, effect highly significant.
And in prior art (Chinese patent: ZL200410046349.5), sample conveying tube outer peripheral edges cover has metal capillary for heat conduction with to sample conveying tube heating, but the thermal capacitance of metal capillary is little, rapid heat dissipation, can not play good heating and thermal insulation effect.
Thermal desorption device of the present invention has the following advantages:
1. device volume is small and exquisite, is easy to fixing, auxiliary fixing without the need to external unit during use, operates more simple and convenient.
2. firing rate is fast, and temperature control error is little, and power consumption is low.
3. sample transfer process cold area free, the complete noresidue of desorb, improves sensitivity and the accuracy of analysis.
4. there is the function of thermal desorption split sampling, effectively prevent analytical column overload, improve chromatographic resolution efficiency.
5. applied range, may be used for the pre-treatment of the samples such as environmental sample, biological sample, food, beverage.
Accompanying drawing explanation
Accompanying drawing described herein is used to provide a further understanding of the present invention, forms a application's part, does not form inappropriate limitation of the present invention, in the accompanying drawings:
Fig. 1 is the structural representation of thermal desorption device of the present invention, wherein 1. heating tubes, 2. heater strip, 3. outer sleeve, 4. internal lining pipe, 5. internal lining pipe pressure head, 6. desorption device upper cover, 7. internal lining pipe pressure cap, 8. internal lining pipe base, 9. the adiabatic ring of internal lining pipe base, 10. sample conveying tube fastening pressure cap, 11. sample conveying tubes, 12. desorption device bases, 13. desorbs purge gas circuit, 14. desorption distributary gas circuits, 15. first O-ring seals, 16. second O-ring seals, 17. the 3rd O-ring seals, 18. first apertures, 19. the 4th O-ring seals, 20. kapillary cutting ferrules, 21. solid-phase microextraction rods, 11A. sample conveying tube region A, 11B. sample conveying tube region B.
Fig. 2 is the chromatographic comparison figure of application examples 1, and wherein A is for adopting the chromatogram of device thermal desorption described in embodiment 1, and B is the chromatogram of thermal desorption when adiabatic for internal lining pipe base ring being changed into stainless steel material.
Fig. 3 is the stratographic analysis figure of application examples 2, and wherein A is the chromatogram of first time desorb after extraction, and B is the chromatogram of second time desorb.Peak in figure is successively: 1. luxuriant and rich with fragrance, 2. anthracene, 3. fluoranthene, 4. pyrene.
Fig. 4 is the stratographic analysis figure of application examples 3.Peak in figure is successively: 1. phenol, 2.2-chlorophenol, 3.2,6-xylenol, 4.2-nitrophenols, 5.2,4-Dichlorophenol, 6.2,4,6-trichlorophenol.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is described, is used for explaining the present invention in this illustrative examples of the present invention and explanation, but not as a limitation of the invention.
Embodiment 1
As shown in Figure 1, a kind of thermal desorption device, by heating tube 1, heater strip 2, outer sleeve 3, internal lining pipe 4, internal lining pipe pressure head 5, desorption device upper cover 6, internal lining pipe pressure cap 7, internal lining pipe base 8, the adiabatic ring 9 of internal lining pipe base, sample conveying tube fastening pressure cap 10, sample conveying tube 11, desorption device base 12, desorb purges gas circuit 13, desorption distributary gas circuit 14, and temperature control component composition, is characterized in that:
Heating tube 1, outer sleeve 3 and internal lining pipe 4 are the hollow cylindrical structure of upper/lower terminal opening, and coaxially arrange; Heating tube 1 outside wall surface is wound with heater strip 2, and is provided with thermopair, thermopair is connected with a temperature controller by wire with heater strip 2; It is inner that heating tube 1 is placed in outer sleeve 3, and outer sleeve 3, for the protection of heating tube 1, is placed with internal lining pipe 4 in heating tube 1; The quartz ampoule that internal lining pipe 4 reduces for bottom diameter, the built-in solid-phase microextraction rod 21 needing thermal desorption; Be provided with desorption device upper cover 6 in outer sleeve 3 upper end open place, lower ending opening place is provided with resolver base 12;
Be provided with internal lining pipe pressure head 5 in the upper end open place of internal lining pipe 4, the lower end of internal lining pipe pressure head 5 is provided with groove, and on groove side wall, radial direction is provided with an annular groove, is provided with the first O-ring seal 15 in annular groove; The upper end of internal lining pipe 4 is stretched out in heating tube 1, is placed in the lower end groove of internal lining pipe pressure head 5 through the first O-ring seal 15, is sealed between the inner chamber of internal lining pipe pressure head 5 and heating tube 1 by the first O-ring seal 15; The upper end outside wall surface of internal lining pipe pressure head 5 is radially provided with annular protrusion and forms first order ring-shaped step, the lower end outer wall face of internal lining pipe pressure head 5 radially caves inward and forms second level ring-shaped step, the second O-ring seal 16 and the 3rd O-ring seal 17 is placed respectively on first order ring-shaped step, second level ring-shaped step, an annular groove is radially provided with in the middle of two-stage step, annular groove is provided with through hole, leads in the lower end groove of internal lining pipe pressure head 5 as the first aperture 18;
Desorption device upper cover 6 is a cylinder, upper end internal face is radially recessed to form first order ring-shaped step, lower end inner wall face is radially provided with annular protrusion and forms second level ring-shaped step, desorption device upper cover 6 internal face above first order ring-shaped step is provided with internal thread, be provided with through hole between first order ring-shaped step and second level ring-shaped step, purge gas circuit 13 as parsing; Internal lining pipe pressure head 5 is placed in desorption device upper cover 6, and internal lining pipe pressure head 5 and desorption device upper cover 6 are connected by the two-stage step arranged respectively above them, resolves the annular groove purging gas circuit 13 middle with internal lining pipe pressure head 5 two-stage step and is connected; Desorb purges gas circuit 13 and is entered, with the inner space of internal lining pipe 4 by the first aperture 18 of internal lining pipe pressure head 5; The externally threaded internal lining pipe pressure cap 7 of band is provided with in the upper end open place of desorption device upper cover 6, the internal thread of desorption device upper cover 6 upper end inwall and the external thread of internal lining pipe pressure cap 7 outer peripheral edges are screwed, both can spin fixing, compress the second O-ring seal 16 and the 3rd O-ring seal 17 of internal lining pipe pressure head 5 outside, sealed between desorption device upper cover 6 and internal lining pipe pressure head 5 whereby;
The adiabatic ring 9 of internal lining pipe base is the hollow cylindrical bakelite of a upper/lower terminal opening, and inside is provided with internal lining pipe base 8; The upper end of internal lining pipe base 8 is provided with groove, on groove side wall, radial direction is provided with an annular groove, the 4th O-ring seal 19 is provided with in annular groove, the lower end of internal lining pipe 4 is stretched out in heating tube 1, be placed in the upper recess of internal lining pipe base 8 through the 4th O-ring seal 19, sealed by the 4th O-ring seal 19 between internal lining pipe base 8 and heating tube 1 inner chamber; Through hole is provided with, as desorption distributary gas circuit 14 in internal lining pipe base 8 upper recess lower side wall; Internal lining pipe base 8 lower end is provided with tapped groove, is provided with through hole between internal lining pipe base 8 upper recess and lower end groove;
Be provided with through hole with externally threaded sample conveying tube fastening pressure cap 10 central axis place, internal lining pipe base 8 and sample conveying tube fastening pressure cap 10 are screwed by the screw thread on it; The upper end of sample conveying tube 11 is passed sample conveying tube fastening pressure cap 10, after its outer sheathed kapillary cutting ferrule 20, is stretched to the through hole of internal lining pipe base 8, the intracavity inter-connection of sample conveying tube 11 and internal lining pipe 4 again; The lower end of sample conveying tube 11 is connected with gas chromatographic sample introduction device through sample introduction pad; The lower end of sample conveying tube fastening pressure cap 10 is provided with groove, and the groove of sample conveying tube fastening pressure cap 10 is buckled on the nut of gas chromatographic sample introduction device; Nut is for compressing sample introduction pad;
Desorption device base 12 is hollow closed container, and closed container upper/lower terminal is provided with opening, and the lower end of outer sleeve 3 and the adiabatic ring 9 of internal lining pipe base are set in desorption device base 12 by closed container upper/lower terminal opening.
Wherein heating tube 1, outer sleeve 3, internal lining pipe pressure head 5, resolver upper cover 6, internal lining pipe pressure cap 7, internal lining pipe base 8, sample conveying tube fastening pressure cap 10 is stainless steel.Sample conveying tube 11 is the quartz capillary with polyimide protective finish of internal diameter 0.10mm.
Application examples 1
Adopt the thermal desorption device described in embodiment 1, using nitrogen as desorb sweep gas, regulate air-flow size, close desorption distributary gas circuit.Connect one before gas chromatographic column and retain interval pre-column.Start-up temperature controller heats heating tube 1, and the material that desorb is got off from solid phase micro-extraction device 21 is desorbed sweep gas and is brought in gas chromatography by sample conveying tube 11 and carry out compartment analysis.Solid-phase microextraction rod to be coated with Stationary liquid be dimethyl silicone polymer, thickness is 60 μm, and after extracting 30 minutes to the hexachloro-benzene standard model that is 800 μ g/L of concentration in 15mL water sample, put into internal lining pipe and carry out thermal desorption, the chromatogram obtained is Fig. 2 A.After changing adiabatic for internal lining pipe base ring into stainless steel material, under similarity condition, the chromatogram obtained is Fig. 2 B.
The desorption condition of Fig. 2 A is:
Spectrogram 1. first time desorb (280 DEG C, 5min), spectrogram 2. second time desorb (280 DEG C, 5min); The solution of Fig. 2 B
Suction condition is:
Spectrogram 1. first time desorb (280 DEG C, 5min), spectrogram 2. second time desorb (280 DEG C, 5min), spectrogram 3. third time desorb (300 DEG C, 5min), spectrogram 4. the 4th desorb (300 DEG C, 10min), spectrogram 5. the 5th desorb (280 DEG C, 5min).
As seen from the figure, for the hexachloro-benzene that boiling point is 325 DEG C, as long as adopt the thermal desorption device desorb of the adiabatic ring of internal lining pipe base once to get final product complete desorb, then desorb four ability elementary solutions are needed to suck full the thermal desorption device that adiabatic for this internal lining pipe base ring changes stainless steel material into.Can find out that the heat insulation effect of the adiabatic ring of internal lining pipe base effectively eliminates cold-zone from this comparison diagram, improve thermal desorption efficiency.
Application examples 2
Adopt the thermal desorption device described in embodiment 1, thermal desorption is carried out to solid-phase microextraction rod.Solid-phase microextraction rod to be coated with Stationary liquid be dimethyl silicone polymer, thickness is 60 μm, after extracting 30 minutes, puts into internal lining pipe and carries out thermal desorption the Reference Materials of PAHs that is 20 μ g/L of concentration in 15mL water sample.The boiling point of component is followed successively by: luxuriant and rich with fragrance (340 DEG C), anthracene (340 DEG C), fluoranthene (375 DEG C), 4. pyrene (404 DEG C).Desorption condition is: rise to 280 DEG C of desorbs 5 minutes from 40 DEG C in 1.5 minutes, and desorb sweep gas is nitrogen, and flow is 3mL/min, closes desorption distributary gas circuit.After analysis completes, carry out second time thermal desorption to check the residual condition of first time thermal desorption, analysis of spectra as shown in Figure 3.Result shows that thermal desorption device is less than 0.1% to the disposable desorb of component of boils up till 404 DEG C is residual.
Application examples 3
Adopt the thermal desorption device described in embodiment 1, thermal desorption is carried out to solid-phase microextraction rod.Solid-phase microextraction rod to be coated with Stationary liquid be polyethersulfone ketone, thickness is 60 μm, after extracting 30 minutes, puts into internal lining pipe and carries out thermal desorption the phenols standard model that is 200 μ g/L of concentration in 15mL water sample.Desorption condition is: rise to 250 DEG C of desorbs 3 minutes from 40 DEG C in 1.5 minutes, and desorb sweep gas is nitrogen, and flow is 3mL/min, and close desorption distributary gas circuit, analysis of spectra as shown in Figure 4.
Application examples 4
Adopt the thermal desorption device described in embodiment 1, thermal desorption is carried out to solid-phase microextraction rod.Solid-phase microextraction rod to be coated with Stationary liquid be dimethyl silicone polymer, thickness is 60 μm, after extracting 60 minutes, puts into internal lining pipe and carries out thermal desorption the organophosphorus pesticide in 15mL fruit juice.Desorption condition is: rise to 260 DEG C of desorbs 5 minutes from 40 DEG C in 1.5 minutes, and desorb sweep gas is nitrogen, and flow is 3mL/min, closes desorption distributary gas circuit.
Embodiment 5
Adopt the thermal desorption device described in embodiment 1, thermal desorption is carried out to solid-phase microextraction rod.Using helium as desorb sweep gas, adjust flux is 3mL/min, opens desorption distributary gas circuit, and regulates shunt ratio to be 5:1.To be coated with Stationary liquid be dimethyl silicone polymer in solid-phase microextraction rod institute, and thickness is 70 μm, after extracting 30 minutes, puts into internal lining pipe to the organo-chlorine pesticide in 20mL milk, and insertion thermal desorption device carries out thermal desorption.Desorption condition is: rise to 300 DEG C of desorbs 5 minutes from 40 DEG C in 1.5 minutes.Gas chromatography electron capture detector (ECD) detects, and Monitoring lower-cut reaches 0.2ng/L.
Application examples 6
Thermal desorption device as described in Example 1.Wherein internal lining pipe is substituted by bundling capillary pipe solid phase micro-extraction pipe.In bundling capillary pipe solid phase micro-extraction pipe be coated with the dimethyl silicone polymer that Stationary liquid is phenyl modification, thickness is 7 μm, is the chlorobenzene class standard sample extraction of 1 μ g/L after 1.5 minutes, puts into thermal desorption device and carry out thermal desorption concentration in 250mL water sample.Desorption condition is: rise to 260 DEG C of desorbs 4 minutes from 40 DEG C in 1.5 minutes, and desorb sweep gas is nitrogen, and flow is 3mL/min, closes desorption distributary gas circuit.Gas chromatographic analysis result shows, this thermal desorption device to the component thermal desorption efficiency of bundling capillary pipe solid phase micro-extraction pipe adsorption and enrichment up to more than 99% (boiling point≤300 DEG C).
Application examples 7
Thermal desorption device as described in Example 1.Wherein fill ketjenblack EC and carbonaceous molecular sieve in internal lining pipe as filling adsorption column, after using aspiration pump to extract 10 minutes with the speed of 200mL/min to the volatile organic matter in air, put into heating tube and carry out thermal desorption.Desorption condition is: rise to 300 DEG C of desorbs 10 minutes from 40 DEG C in 1.5 minutes, and desorb sweep gas is helium, and flow is 4mL/min, closes desorption distributary gas circuit.Gas chromatographic analysis result shows that the thermal desorption efficiency of thermal desorption device to adsorption column is high.
Claims (6)
1. a thermal desorption device, comprise heating tube (1), heater strip (2), outer sleeve (3), internal lining pipe (4), internal lining pipe pressure head (5), desorption device upper cover (6), internal lining pipe pressure cap (7), internal lining pipe base (8), the adiabatic ring (9) of internal lining pipe base, sample conveying tube fastening pressure cap (10), sample conveying tube (11), desorption device base (12), desorb purges gas circuit (13) and desorption distributary gas circuit (14), it is characterized in that:
Heating tube (1), outer sleeve (3) and internal lining pipe (4) are the hollow cylindrical structure of upper/lower terminal opening, and coaxially arrange; Heating tube (1) outside wall surface is wound with heater strip (2), it is inner that heating tube (1) is placed in outer sleeve (3), outer sleeve (3), for the protection of heating tube (1), is placed with internal lining pipe (4) in heating tube (1); Be provided with desorption device upper cover (6) in outer sleeve (3) upper end open place, lower ending opening place is provided with resolver base (12);
Internal lining pipe pressure head (5) is provided with in the upper end open place of internal lining pipe (4), the lower end of internal lining pipe pressure head (5) is provided with groove, on groove side wall, radial direction is provided with an annular groove, is provided with the first O-ring seal (15) in annular groove; The upper end of internal lining pipe (4) is stretched out in heating tube (1), be placed in the lower end groove of internal lining pipe pressure head (5) through the first O-ring seal (15), sealed by the first O-ring seal (15) between the inner chamber of internal lining pipe pressure head (5) and heating tube (1); The upper end outside wall surface of internal lining pipe pressure head (5) is radially provided with annular protrusion and forms first order ring-shaped step, the lower end outer wall face of internal lining pipe pressure head (5) radially caves inward and forms second level ring-shaped step, the second O-ring seal (16) and the 3rd O-ring seal (17) is placed respectively on first order ring-shaped step, second level ring-shaped step, an annular groove is radially provided with in the middle of two-stage step, annular groove is provided with through hole, leads in the lower end groove of internal lining pipe pressure head (5) as the first aperture (18);
Desorption device upper cover (6) is a cylinder, upper end internal face is radially recessed to form first order ring-shaped step, lower end inner wall face is radially provided with annular protrusion and forms second level ring-shaped step, desorption device upper cover (6) internal face above first order ring-shaped step is provided with internal thread, be provided with through hole between first order ring-shaped step and second level ring-shaped step, purge gas circuit (13) as parsing; Internal lining pipe pressure head (5) is placed in desorption device upper cover (6), internal lining pipe pressure head (5) and desorption device upper cover (6) are connected by the two-stage step arranged respectively above them, resolve the annular groove purging gas circuit (13) middle with internal lining pipe pressure head (5) two-stage step and are connected; Desorb purges gas circuit (13) and is entered, with the inner space of internal lining pipe (4) by first aperture (18) of internal lining pipe pressure head (5); The externally threaded internal lining pipe pressure cap (7) of band is provided with in the upper end open place of desorption device upper cover (6), the internal thread of desorption device upper cover (6) upper end inwall and the external thread of internal lining pipe pressure cap (7) outer peripheral edges are screwed, both can spin fixing, compress outside the second O-ring seal (16) of internal lining pipe pressure head (5) and the 3rd O-ring seal (17), sealed between desorption device upper cover (6) and internal lining pipe pressure head (5) whereby;
The adiabatic ring (9) of internal lining pipe base is the hollow cylindrical structure of a upper/lower terminal opening, and inside is provided with internal lining pipe base (8); The upper end of internal lining pipe base (8) is provided with groove, on groove side wall, radial direction is provided with an annular groove, the 4th O-ring seal (19) is provided with in annular groove, the lower end of internal lining pipe (4) is stretched out in heating tube (1), be placed in the upper recess of internal lining pipe base (8) through the 4th O-ring seal (19), sealed by the 4th O-ring seal (19) between internal lining pipe base (8) and heating tube (1) inner chamber; Through hole is provided with, as desorption distributary gas circuit (14) in internal lining pipe base (8) upper recess lower side wall; Internal lining pipe base (8) lower end is provided with tapped groove, is provided with through hole between internal lining pipe base (8) upper recess and lower end groove;
Be provided with through hole with externally threaded sample conveying tube fastening pressure cap (10) central axis place, internal lining pipe base (8) and sample conveying tube fastening pressure cap (10) are screwed by the screw thread on it; The upper end of sample conveying tube (11) is passed sample conveying tube fastening pressure cap (10), after its outer sheathed kapillary cutting ferrule (20), is stretched to the through hole of internal lining pipe base (8), the intracavity inter-connection of sample conveying tube (11) and internal lining pipe (4) again; The lower end of sample conveying tube (11) is connected with gas chromatographic sample introduction device through sample introduction pad; The lower end of sample conveying tube fastening pressure cap (10) is provided with groove, and the groove of sample conveying tube fastening pressure cap (10) is buckled on the nut of gas chromatographic sample introduction device; Nut is for compressing sample introduction pad;
Desorption device base (12) is hollow closed container, closed container upper/lower terminal is provided with opening, and the lower end of outer sleeve (3) and the adiabatic ring (9) of internal lining pipe base are set in desorption device base (12) by closed container upper/lower terminal opening.
2. thermal desorption device according to claim 1, is characterized in that:
The adiabatic ring (9) of described internal lining pipe base is made by the high temperature resistant and materials processing of thermal insulation, and be high temperature polymeric materials or pottery, high temperature polymeric materials is bakelite, teflon, polyetheretherketone, polyethersulfone ketone or polyimide.
3. thermal desorption device according to claim 1, is characterized in that:
Be provided with thermopair in heating tube (1) outside wall surface, thermopair is connected with a temperature controller by wire with heater strip (2).
4. thermal desorption device according to claim 1, is characterized in that:
Described heating tube (1), outer sleeve (3), internal lining pipe pressure head (5), resolver upper cover (6), internal lining pipe pressure cap (7), internal lining pipe base (8), sample conveying tube fastening pressure cap (10) is made by stainless steel material or other metal materials.
5. thermal desorption device according to claim 1, is characterized in that:
The quartz that described internal lining pipe (4) closes up for lower end or glass tube.
6. thermal desorption device according to claim 1, is characterized in that:
Described sample conveying tube (11) is with the quartz capillary of polyimide protective finish or the inwall stainless steel capillary through process of deactivating.
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| CN111141858B (en) * | 2018-11-06 | 2021-07-27 | 中国科学院大连化学物理研究所 | Device of thermal analyzer interface |
| CN109718631A (en) * | 2018-12-21 | 2019-05-07 | 北京放射性核素实验室 | A kind of assembly type adsorption-desorption device |
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