CN107703240A - A kind of gas-chromatography programmed temperature sampling system and method using eddy current effect - Google Patents
A kind of gas-chromatography programmed temperature sampling system and method using eddy current effect Download PDFInfo
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- CN107703240A CN107703240A CN201711218666.4A CN201711218666A CN107703240A CN 107703240 A CN107703240 A CN 107703240A CN 201711218666 A CN201711218666 A CN 201711218666A CN 107703240 A CN107703240 A CN 107703240A
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- 238000005070 sampling Methods 0.000 title claims abstract description 55
- 238000004817 gas chromatography Methods 0.000 title claims abstract description 34
- 230000000694 effects Effects 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 15
- 239000007789 gas Substances 0.000 claims abstract description 83
- 238000002347 injection Methods 0.000 claims abstract description 52
- 239000007924 injection Substances 0.000 claims abstract description 52
- 230000001105 regulatory effect Effects 0.000 claims abstract description 23
- 239000006200 vaporizer Substances 0.000 claims abstract description 14
- 239000000112 cooling gas Substances 0.000 claims abstract description 7
- 238000002309 gasification Methods 0.000 claims description 21
- 238000005057 refrigeration Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 7
- 238000000935 solvent evaporation Methods 0.000 claims description 7
- 238000009413 insulation Methods 0.000 claims description 5
- 238000013461 design Methods 0.000 claims description 4
- 238000005259 measurement Methods 0.000 claims description 3
- 230000009467 reduction Effects 0.000 claims description 3
- 230000006835 compression Effects 0.000 claims 1
- 238000007906 compression Methods 0.000 claims 1
- 239000007788 liquid Substances 0.000 description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 238000001816 cooling Methods 0.000 description 7
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 230000035945 sensitivity Effects 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 229910002092 carbon dioxide Inorganic materials 0.000 description 3
- 239000001569 carbon dioxide Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 108010085603 SFLLRNPND Proteins 0.000 description 1
- 239000012491 analyte Substances 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000003965 capillary gas chromatography Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000010892 electric spark Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000004186 food analysis Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000005220 pharmaceutical analysis Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004227 thermal cracking Methods 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
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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
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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
- G01N2030/121—Preparation by evaporation cooling; cold traps
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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
- G01N2030/127—PTV evaporation
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Abstract
A kind of gas-chromatography programmed temperature sampling system using vortex refrigerating effect, including compressed gas regulating valve, vortex tube and programmed temperature sampling mouth, it is characterized in that, described programmed temperature sampling implication chamber outer wall is provided with heater and temperature sensor, cold-trap is externally provided with past, described cold-trap is wrapped in described vaporizer and described heater and temperature sensor, and is provided with cooling gas inlet and outlet with space and the passage that can accommodate cooling gas, described cold-trap；Compressed gas is connected through the compressed gas regulating valve by pipeline with vortex tube inlet, and vortex tube cold side outlet is connected with the cold-trap entrance of programmed temperature sampling mouth by pipeline.A kind of gas-chromatography programmed temperature sampling method using vortex refrigerating effect, comprise the following steps：S1 injection port hot stages, S2 injection port cold stages, S3 injector temperature equilibrium stages, S4 injection port temperature rise periods.
Description
Technical field
The present invention relates to detecting instrument field, more particularly to a kind of gas-chromatography programmed temperature sampling system（PTV）And
Method.
Background technology
Improve the eternal topic that sensitivity for analysis is almost analytical chemistry.For gas chromatographic analysis, instrument system
The person of making and analysis worker always try the method for manufacturing highly sensitive instrument and developing high spirit degree of respecting.Especially in environment point
In terms of analysis, Pharmaceutical Analysis and food analysis, it is exactly that this requirement promotes to have very high requirement to sensitivity about regulation method
The development of instrument, and the development of instrument has the person that makes law making to propose higher detection sensitivity requirement, this interaction is circulation
Reciprocal.
Carrier of traditional gas chromatographic sample introduction mode using bushing pipe as solvent evaporation.Due to expansion rate when organic solvent vaporizes
Greatly, boiling point is relatively low, and the volume of bushing pipe can not increase substantially, therefore the sampling volume of gas-chromatography is generally limited by 5 μ L
Below.
Application of the large volume sample injection technology in capillary gas chromatography can reduce the test limit of analysis method, improve and divide
Analyse sensitivity and precision.It is mainly real by temperature programming-solvent air defense pattern based on temperature programming vaporisation techniques (PTV technologies)
Existing large volume sample injection, i.e. sample enter cold bushing pipe, solvent and part low boiling component with carrier gas from distributing with liquid condition
Mouth emptying.After most of solvent, which volatilizees, to be vented, second of sample introduction can be carried out, above solvent vent process is repeated, until complete
Into required sample size.After enough determinands are have accumulated in bushing pipe, testing sample is transferred to chromatographic column by rise gasification room temperature
In, so as to reach large volume sample injection effect.Its advantage is analyte under minimum injector temperature rather than constant
At a high temperature of vaporize so that the possibility of sample thermal cracking minimizes, while still allow a large amount of analytes to vaporize.
Cooling method is generally that liquid nitrogen or liquid titanium dioxide are added in the cold-trap of PTV injection ports by the way of now
Carbon, or use semiconductor refrigerating mode.Liquid nitrogen or liquid carbon dioxide its shortcoming are maintenance cost height, due to liquid nitrogen and liquid
The reason for state carbon dioxide absorbs heat, it is easy to gasify, no matter use is without using liquid all can also consume with the time.Semiconductor
The refrigerating efficiency of refrigeration modes is again less high, is unfavorable for promoting the use of.
The content of the invention
In view of the above the shortcomings that prior art, it is an object of the invention to overcome the refrigeration side of traditional PTV injection ports
The shortcomings that formula, there is provided a kind of gas-chromatography programmed temperature sampling system and method using vortex refrigerating effect, it is existing for solving
There is the problem of in technology.
In order to achieve the above objects and other related objects, the present invention provides a kind of gas-chromatography using vortex refrigerating effect
Programmed temperature sampling system, including compressed gas regulating valve, vortex tube and programmed temperature sampling mouth, it is characterised in that described
Programmed temperature sampling implication chamber outer wall is provided with heater and temperature sensor, and cold-trap, described cold-trap bag are externally provided with past
Described vaporizer and described heater and temperature sensor are wrapped up in, and with the space that can accommodate cooling gas and is led to
Road, described cold-trap are provided with cooling gas inlet and outlet；Compressed gas passes through pipeline and whirlpool through the compressed gas regulating valve
Flow tube entrance is connected, and vortex tube cold side outlet is connected with the cold-trap entrance of programmed temperature sampling mouth by pipeline.
Further, a kind of gas-chromatography programmed temperature sampling system using vortex refrigerating effect, it is characterised in that described
Vortex tube also include hot gas end regulating valve, and for adjusting the controller of hot gas end regulating valve.
Further, a kind of gas-chromatography programmed temperature sampling system using vortex refrigerating effect, it is characterised in that described
Hot gas end governor valve control device be electromagnetic controller, hot gas end regulating valve can be controlled according to the control signal of receiving.
Further, a kind of gas-chromatography programmed temperature sampling system using vortex refrigerating effect, it is characterised in that also wrap
Gas compressor and gas-drying apparatus are included, gas-drying apparatus is located between outlet and the vortex tube inlet of compressor.
Further, a kind of gas-chromatography programmed temperature sampling system using vortex refrigerating effect, it is characterised in that also wrap
Include a vortex tube, with original vortex tube form multi-stage vortex refrigeration system, wherein the cold side outlet of first order vortex tube with
The entrance of second level vortex tube is connected, and second level vortex tube cold side outlet is connected with the cold-trap entrance of programmed temperature sampling mouth.
Further, a kind of gas-chromatography programmed temperature sampling system using vortex refrigerating effect, it is characterised in that in institute
The pipeline being connected between the vortex tube cold side outlet stated and described programmed temperature sampling mouth cold-trap entrance is provided with temperature sensor
And flow sensor.
Further, a kind of gas-chromatography programmed temperature sampling system using vortex refrigerating effect, it is characterised in that described
Cold-trap be hollow pipeline, be wound on described injection port gasification chamber outer wall.
Further, a kind of gas-chromatography programmed temperature sampling system using vortex refrigerating effect, it is characterised in that in institute
The pipeline being connected between the vortex tube cold side outlet stated and described programmed temperature sampling mouth cold-trap entrance is provided with heat-insulation layer, described
Cold-trap outer wall also be provided with heat-insulation layer.
A kind of gas-chromatography programmed temperature sampling method using vortex refrigerating effect, whirlpool is utilized applied to described one kind
Flow the gas-chromatography programmed temperature sampling system of refrigeration effect, it is characterised in that comprise the following steps：
S1 injection port hot stages：When system starts, injection port is in the condition of high temperature, and compressed air controls through control valve
Into total gas flow in vortex tube, gas produces cold and hot two strands of gas through generator in vortex tube, and wherein cold end gas is by whirlpool
Flow tube cold side outlet is discharged, and enters injection port cold-trap entrance through pipeline, injection port is cooled, real-time by temperature sensor
Measurement gasification room temperature.
S2 injector temperature equilibrium stages：When temperature, which reaches, sets temperature, reduced and entered in vortex tube by control valve
Total tolerance, reduce swirl control cold, open heater, by dynamic equilibrium, the control of injection port vaporizer is being set
Temperature, inject sample.
The S3 injection port temperature rise periods：Compressed gas control valve is closed, stops the total gas flow entered in vortex tube；By entering
Sample mouth heater is gradually heated up, sample solvent evaporation, sample gasification, and the sample after gasification is separated into chromatographic system.
Further, a kind of gas-chromatography programmed temperature sampling method using vortex refrigerating effect, applied to described one
Kind utilizes the gas-chromatography programmed temperature sampling system of vortex refrigerating effect, it is characterised in that comprises the following steps：
S1 injection port hot stages：When system starts, injection port is in the condition of high temperature, and compressed air controls through control valve
Into total gas flow in vortex tube, gas produces cold and hot two strands of gas through generator in vortex tube, opens big compressed gas control
Valve increases the total tolerance entered in vortex tube, regulation vortex tube hot junction regulating valve, increases cold end gas output, accelerates injector temperature
Reduction, cold end gas discharged by vortex tube cold side outlet, enters injection port cold-trap entrance through pipeline, injection port is dropped
Temperature, measure gasification room temperature in real time by temperature sensor.
S2 injection port cold stages：When injector temperature is reduced close to room temperature, vortex tube hot junction regulating valve is gradually adjusted,
Increase hot junction gas ratio, reduce cold end gas ratio, gradually reduce cold end gas temperature；
S3 injector temperature equilibrium stages：When temperature, which reaches, sets temperature, reduced by control valve total into vortex tube
Tolerance, swirl control cold is reduced, opens heater, by dynamic equilibrium, injection port vaporizer is controlled in design temperature,
Inject sample.
The S4 injection port temperature rise periods：Compressed gas control valve is closed, stops the total gas flow entered in vortex tube；By entering
Sample mouth heater is gradually heated up, sample solvent evaporation, sample gasification, and the sample after gasification is separated into chromatographic system.
Vortex tube is a kind of very simple energy separation device of structure, and it is by nozzle, minor air cell, separation orifice and cold
Hot two end pipes composition.Compressed gas expands in nozzle during work, then tangentially enters vortex tube with very high speed.
When air-flow rotates at a high speed in vortex tube, the unequal two parts air-flow of stagnation temperature is separated into after vortex converts, in center
The gas flow temperature at position is low, and the gas flow temperature in outer layer position is high, adjusts hot and cold stream ratio, can obtain optimal refrigeration effect
Effect or should be heated.Caused cold air is minimum to can reach subzero 46 DEG C, and without the part of motion.The characteristics of vortex tube:
1. low cost, non-maintaining；
2. temperature °F (- 46 ° to+127 DEG C) from -50 °F of to 260；
3. flow rate SCFM (SLPM of 28 to 4248) from 1 to 100；
4. refrigerating capacity maximum can reach 6000 Btu/hr. (1512 Kcal/hr.)；
5. manufactured using the stainless steel of high intensity, anticorrosive, anti-oxidant, high temperature resistance；
6. not electricity consumption, without any chemical substance, do not have electric spark generation；
7. small volume, in light weight, Anti-knocking；
8. it is rapid to produce cold air, and can pass through valve quick regulation.
The beneficial effects of the present invention are a kind of new gas-chromatography programmed temperature sampling system is devised, the system is filled
Divide the characteristics of make use of vortex tube, freezed using vortex tube end air flow, maintenance easy to operate simple in construction；By vortex tube
Freeze to cool to injection port vaporizer, without using the liquid nitrogen or liquid carbon dioxide for being difficult to safeguard, drop
Low cost, has great practical value and promotional value.By adjusting vortex tube hot gas end regulating valve, accelerate refrigeration speed
Degree, cost is saved, improve efficiency.Injector temperature is controlled by dynamic equilibrium, quick and precisely.
Brief description of the drawings
Fig. 1 show the schematic diagram of the gas-chromatography programmed temperature sampling system of the present invention；
Wherein：1. compressed air inlet, 2. compressed air regulating valves；3. vortex tube inlet；4. vortex tube；5. vortex tube hot junction is adjusted
Save valve；6. vortex tube hot junction exports；7. vortex tube cold side outlet；8. injection port cooling air cooling trap entrance；9. cold-trap；10. heating
Device；11. vaporizer；12. temperature sensor；13. injection port cooling air cooling trap outlet；14. injection port cooling air cooling trap goes out
Mouthful；15. bushing pipe；16. injection port.
Embodiment
With reference to embodiment, the present invention is further elaborated.
As shown in the figure：A kind of gas-chromatography programmed temperature sampling system using eddy current effect, including compressed gas regulation
Valve 2, vortex tube 4 and programmed temperature sampling mouth 16, it is characterised in that the described outer wall of 16 vaporizer of programmed temperature sampling mouth 11 is set
There are heater 10 and temperature sensor 12, toward cold-trap 9 is externally provided with, bushing pipe 15 is located in the vaporizer 11, and described is cold
Trap 9 is wrapped in described vaporizer 15 and described heater 10 and temperature sensor 12, and described cold-trap 9 is provided with cooling gas
Body entrance 8 and outlet 13,14；Compressed gas is connected by pipeline 1 through the compressed gas regulating valve 2 with vortex tube inlet 3, whirlpool
Flow tube cold side outlet 7 is connected with the cold-trap entrance 8 of programmed temperature sampling mouth.Vortex tube hot junction outlet 6 communicates with air.
Further, vortex tube also includes hot gas end regulating valve 5, and for adjusting the control of hot gas end regulating valve
Device.
Further, the controller is electromagnetic controller, and hot gas end regulating valve can be controlled according to the control signal of receiving.
Further, in addition to a gas compressor and gas-drying apparatus, gas-drying apparatus be located at the outlet of compressor with
Between vortex tube inlet.
Further, in addition to a vortex tube, composition multi-stage vortex refrigeration system, the cold end of wherein first order vortex tube go out
Mouth is connected with the entrance of second level vortex tube, the cold-trap entrance phase of second level vortex tube cold side outlet and programmed temperature sampling mouth
Even.
Further, the pipeline being connected between cold-trap entrance of the vortex tube cold side outlet with programmed temperature sampling mouth, which is provided with, to be protected
Warm layer, cold-trap outer wall also are provided with heat-insulation layer.
Further, the pipeline being connected between cold-trap entrance of the vortex tube cold side outlet with programmed temperature sampling mouth is provided with temperature
Spend sensor and flow sensor.
Embodiment one
The carrying out practically process of the system is：When system starts, injection port is in the condition of high temperature, and compressed air is through control
Total gas flow that the control of valve 2 enters in vortex tube 4, gas is through vortex tube 4, and interior generator produces cold and hot two strands of gas, wherein cold
End gas is discharged by vortex tube cold side outlet 7, enters injection port cold-trap entrance through pipeline, injection port is cooled, passes through temperature
The measurement gasification room temperature of sensor 12 is spent, when temperature, which reaches, sets temperature.Reduced and entered in vortex tube 4 by control valve 2
Total tolerance, swirl control cold is reduced, open heater 10, by dynamic equilibrium, the control of injection port vaporizer is being set
Temperature.Sample is injected, closing control valve 2, stops the total gas flow entered in vortex tube 4.Gradually heated up by heater 10,
Sample solvent evaporation, sample gasification, the sample after gasification are separated into chromatographic system.
Embodiment two
The carrying out practically process of the system is：When system starts, injection port is in the condition of high temperature, and compressed air is through control
Total gas flow that the control of valve 2 enters in vortex tube 4, the gas of vortex tube 4 produce cold and hot two strands of gas through generator in vortex tube 4
Body, open big control valve 2 and increase the total tolerance entered in vortex tube 4, regulation vortex tube hot junction regulating valve 5, increase cold end gas output,
Accelerate the reduction of injector temperature.Cold end gas is discharged by vortex tube cold side outlet 7, enters injection port cold-trap entrance through pipeline,
Injection port is cooled, gasification room temperature is measured by temperature sensor 12, when temperature is reduced close to room temperature, gradually adjustment
Hot junction regulating valve 5, cold end gas temperature is gradually reduced, when temperature, which reaches, sets temperature, reduced by control valve 2 and enter vortex
Total tolerance in pipe 4, swirl control cold is reduced, open heater 10, filled by the refrigerating capacity and heating of controlled vortex flow pipe
Dynamic equilibrium between the heating power put, injection port vaporizer is controlled in design temperature.Injection sample, closing control valve 2,
Stop the total gas flow entered in vortex tube 4.Gradually heated up by heater 10, sample solvent evaporation, sample gasification, gasification
Sample afterwards is separated into chromatographic system.
The temperature and uninterrupted of cold airflow can be by adjusting vortex tube hot gas end valve gate control.Vortex tube hot gas brings out gas
Ratio is higher, then the temperature of vortex tube cold air end air-flow is lower, and flow is also accordingly reduced, otherwise vortex tube hot gas brings out gas ratio
Example is lower, then the temperature of vortex tube cold air end air-flow is higher, and flow also accordingly increases.
Embodiment three
Compressed-air-storing in air accumulator, is entered vortex tube by compressor through gas-drying apparatus by control valve.
The present invention is not limited to embodiments described above.The description to embodiment is intended to describe and said above
Bright technical scheme, above-mentioned embodiment is only schematical, is not restricted.This is not being departed from
In the case of invention objective and scope of the claimed protection, one of ordinary skill in the art may be used also under the enlightenment of the present invention
The specific conversion of many forms is made, these are belonged within protection scope of the present invention.
Claims (10)
1. a kind of gas-chromatography programmed temperature sampling system using vortex refrigerating effect, including compressed gas regulating valve, vortex
Pipe and programmed temperature sampling mouth, it is characterised in that described programmed temperature sampling implication chamber outer wall is provided with heater and temperature
Sensor is spent, toward cold-trap is externally provided with, described cold-trap is wrapped in described vaporizer and described heater and temperature passes
Sensor, and it is provided with cooling gas inlet and outlet with space and the passage that can accommodate cooling gas, described cold-trap；Compression
Gas is connected through the compressed gas regulating valve by pipeline with vortex tube inlet, vortex tube cold side outlet and programmed temperature sampling
The cold-trap entrance of mouth is connected by pipeline.
2. a kind of gas-chromatography programmed temperature sampling system using vortex refrigerating effect according to claim 1, it is special
Sign is that described vortex tube also includes hot gas end regulating valve, and for adjusting the controller of hot gas end regulating valve.
3. a kind of gas-chromatography programmed temperature sampling system using vortex refrigerating effect according to claim 2, it is special
Sign is that described hot gas end governor valve control device is electromagnetic controller, according to the control signal of receiving hot gas end can be controlled to adjust
Save valve.
4. a kind of gas-chromatography programmed temperature sampling system using vortex refrigerating effect according to claim 1, it is special
Sign is, in addition to gas compressor and gas-drying apparatus, gas-drying apparatus be located at the outlet of compressor and vortex tube inlet it
Between.
5. a kind of gas-chromatography programmed temperature sampling system using vortex refrigerating effect according to claim 1, it is special
Sign is, in addition to a vortex tube, and multi-stage vortex refrigeration system, wherein first order vortex tube are formed with original vortex tube
Cold side outlet is connected with the entrance of second level vortex tube, and the cold-trap of second level vortex tube cold side outlet and programmed temperature sampling mouth enters
Mouth is connected.
6. a kind of gas-chromatography programmed temperature sampling system using vortex refrigerating effect according to claim 1, it is special
Sign is that the pipeline being connected between described vortex tube cold side outlet and described programmed temperature sampling mouth cold-trap entrance is provided with
Temperature sensor and flow sensor.
7. a kind of gas-chromatography programmed temperature sampling system using vortex refrigerating effect as claimed in claim 1, its feature
It is, described cold-trap is hollow pipeline, is wound on described injection port gasification chamber outer wall.
8. any of which according to claim 1-7 utilizes the gas-chromatography programmed temperature sampling system of vortex refrigerating effect
System, it is characterised in that be connected between described vortex tube cold side outlet and described programmed temperature sampling mouth cold-trap entrance
Pipeline is provided with heat-insulation layer, and described cold-trap outer wall also is provided with heat-insulation layer.
A kind of 9. gas-chromatography programmed temperature sampling method using vortex refrigerating effect, applied to one described in claim 1
Kind utilizes the gas-chromatography programmed temperature sampling system of vortex refrigerating effect, it is characterised in that comprises the following steps：
S1 injection port hot stages：When system starts, injection port is in the condition of high temperature, and compressed air controls through control valve
Into total gas flow in vortex tube, gas produces cold and hot two strands of gas through generator in vortex tube, and wherein cold end gas is by whirlpool
Flow tube cold side outlet is discharged, and enters injection port cold-trap entrance through pipeline, injection port is cooled, real-time by temperature sensor
Measurement gasification room temperature；
S2 injector temperature equilibrium stages：When temperature, which reaches, sets temperature, reduced by control valve total into vortex tube
Tolerance, swirl control cold is reduced, opens heater, by dynamic equilibrium, injection port vaporizer is controlled in design temperature,
Inject sample；
The S3 injection port temperature rise periods：Compressed gas control valve is closed, stops the total gas flow entered in vortex tube；Pass through injection port
Heater is gradually heated up, sample solvent evaporation, sample gasification, and the sample after gasification is separated into chromatographic system.
10. a kind of gas-chromatography programmed temperature sampling method using vortex refrigerating effect according to claim 9, application
In a kind of gas-chromatography programmed temperature sampling system using vortex refrigerating effect described in claim 2, it is characterised in that bag
Include following steps：
S1 injection port hot stages：When system starts, injection port is in the condition of high temperature, and compressed air controls through control valve
Into total gas flow in vortex tube, gas produces cold and hot two strands of gas through generator in vortex tube, opens big compressed gas control
Valve increases the total tolerance entered in vortex tube, regulation vortex tube hot junction regulating valve, increases cold end gas output, accelerates injector temperature
Reduction, cold end gas discharged by vortex tube cold side outlet, enters injection port cold-trap entrance through pipeline, injection port is dropped
Temperature, measure gasification room temperature in real time by temperature sensor；
S2 injection port cold stages：When injector temperature is reduced close to room temperature, vortex tube hot junction regulating valve, increase are gradually adjusted
Hot junction gas ratio, cold end gas ratio is reduced, gradually reduces cold end gas temperature；
S3 injector temperature equilibrium stages：When temperature, which reaches, sets temperature, reduced by control valve total into vortex tube
Tolerance, swirl control cold is reduced, opens heater, by dynamic equilibrium, injection port vaporizer is controlled in design temperature,
Inject sample；
The S4 injection port temperature rise periods：Compressed gas control valve is closed, stops the total gas flow entered in vortex tube；Pass through injection port
Heater is gradually heated up, sample solvent evaporation, sample gasification, and the sample after gasification is separated into chromatographic system.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109991272A (en) * | 2019-04-08 | 2019-07-09 | 包头稀土研究院 | Magnetothermal effect measuring instrument temperature regulating device and temperature control method |
| CN112684078A (en) * | 2020-12-16 | 2021-04-20 | 广东省测试分析研究所（中国广州分析测试中心） | Method for improving chromatographic peak capacity of solid phase microextraction sample injection mode |
| CN113203913A (en) * | 2021-07-06 | 2021-08-03 | 海拓仪器(江苏)有限公司 | Small-sized quick cold-hot impact testing device |
| CN113552272A (en) * | 2021-09-22 | 2021-10-26 | 南通市安特速医疗科技有限公司 | Automatic sample introduction device for gas chromatograph |
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2017
- 2017-11-28 CN CN201711218666.4A patent/CN107703240A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109991272A (en) * | 2019-04-08 | 2019-07-09 | 包头稀土研究院 | Magnetothermal effect measuring instrument temperature regulating device and temperature control method |
| CN112684078A (en) * | 2020-12-16 | 2021-04-20 | 广东省测试分析研究所（中国广州分析测试中心） | Method for improving chromatographic peak capacity of solid phase microextraction sample injection mode |
| CN112684078B (en) * | 2020-12-16 | 2024-03-29 | 广东省测试分析研究所（中国广州分析测试中心） | Method for improving chromatographic peak capacity of solid-phase microextraction sample injection mode |
| CN113203913A (en) * | 2021-07-06 | 2021-08-03 | 海拓仪器(江苏)有限公司 | Small-sized quick cold-hot impact testing device |
| WO2023279622A1 (en) * | 2021-07-06 | 2023-01-12 | 海拓仪器(江苏)有限公司 | Small rapid cold and hot impact testing device |
| US12061225B2 (en) | 2021-07-06 | 2024-08-13 | Hitop Instrument (Jiangsu) Co., Ltd. | Small-sized fast cold and hot shock test devices |
| CN113552272A (en) * | 2021-09-22 | 2021-10-26 | 南通市安特速医疗科技有限公司 | Automatic sample introduction device for gas chromatograph |
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Application publication date: 20180216 |