CN103983504A - Positive pressure surface layer high temperature rapid condensation method - Google Patents
Positive pressure surface layer high temperature rapid condensation method Download PDFInfo
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- CN103983504A CN103983504A CN201310051353.XA CN201310051353A CN103983504A CN 103983504 A CN103983504 A CN 103983504A CN 201310051353 A CN201310051353 A CN 201310051353A CN 103983504 A CN103983504 A CN 103983504A
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Abstract
The invention belongs to the technical field of chemical analysis, relates to a sample extract condensation method, and in particular relates to a positive pressure surface layer high temperature rapid condensation method and an experimental device thereof. According to the method, a gas blowing experimental device is used to purging the surface of an organic solvent by a high temperature gas for realization of rapid condensation of a sample extract; the gas blowing experimental device is composed of a positive pressure gas distribution system, a high temperature gas generating system and a sample positioning frame, the device generates a positive pressure high temperature gas flow with the adjustable flow rate for blowing the surface of the extract, by heating from a surface layer to an inside layer, bumping phenomenon and solvent condensation reflux appeared in a traditional nitrogen blowing concentrator can be avoided, and by use of large-diameter gas blowing pipe, the contact area of the gas flow and the extract can be increased, and the evaporation speed of the extract can be increased; the gas blowing experimental device has the advantages of simple structure, flexible operation and strong scalability.
Description
Technical field
The invention belongs to chemical analysis technology field, relate to the method for concentration of sample extraction liquid, be specifically related to the quick method for concentration of a kind of malleation top layer high temperature and experimental provision thereof.The method adopts high-temperature gas to purge organic solvent surface, and organic solvent, by top layer layer high-temperature heating inwards, is realized to the concentrated fast of sample extraction liquid.
Background technology
Nitrogen blows concentration technique and is mainly used in the concentrated sample extraction liquid that contains organic solvent, reaches solvent replacement or improves the objects such as sensitivity for analysis.The nitrogen of prior art blows concentration technique generally to be realized by Nitrogen evaporator, and the device that wherein adopted is comprised of gas distributing system, Sample location frame, heating arrangement three parts conventionally; Nitrogen blows in concentration process, nitrogen is after gas distributing system is adjusted flow, by gas blow pipe, form gas flow purging and be fixed on the organic solvent in the sample hose on Sample location frame, Sample location is placed in heating arrangement, by water-bath or the fast mode of electric heating, the organic solvent in sample hose is heated, accelerate the volatilization of organic solvent, reach the object of concentrated organic solvent.Its feature of said method is that the purge gas that nitrogen blows concentrating instrument is normal temperature, organic solvent is carried out to integral body heating, therefore exist following not enough: one, because purge gas is normal temperature, cause when concentrated organic solvent, organic solvent top temperature is lower than organic solvent temperature, and condensing reflux appears in the organic solvent of volatilization, the evaporation rate of the organic solvent that slowed down; Two, owing to heating organic solvent is whole, when heating-up temperature surpasses organic solvent boiling point, there is bumping in organic solvent, easily causes the recovery of target analytes to reduce; Three, because the fast heating of water-bath or electric heating belongs to bottom-heated pattern, the position of heating arrangement is fixed, and when sampling receptacle is placed in heating module, vision is extremely restricted, and causes sample solution volatilization progress degree to be difficult to observe, and operates extremely not convenient; And heating module is subject to volume restrictions, difficult realization purges the change of sample hose maximum quantity simultaneously, and expansion dirigibility is poor.Therefore, the present invention with provide a kind of to organic solvent by top layer layer high-temperature heating inwards, realize the quick concentrated method of sample extraction liquid.
Summary of the invention
The object of the invention is to overcome the defect of prior art, the quick method for concentration of a kind of malleation top layer high temperature and experimental provision thereof are provided.The method is used air-blowing experimental provision to purge organic solvent surface by high temperature hot gas, to organic solvent, by top layer layer high-temperature heating inwards, can effectively avoid organic solvent solvent bumping and condensing reflux, make solvent fast volatilization realize concentrating fast of sample extraction liquid.The air-blowing experimental provision that this method relates to is simple in structure, flexible operation, and extendability is strong.
The quick method for concentration of malleation of the present invention top layer high temperature, it is characterized in that, it comprises, use air-blowing experimental provision to purge organic solvent surface by high temperature hot gas, to organic solvent by top layer inwards layer high-temperature heating, solvent is volatilized fast, and solvent vapo(u)r is taken away by hot gas simultaneously, realizes sample extraction liquid concentrated fast.
In the present invention, by the high-temperature gas of certain flow rate and pressure, to solvent by top layer the high-temperature heating to nexine, solvent is volatilized fast, in the present invention, conventionally adopt the high-temperature gases such as nitrogen, air or helium;
In the present invention, high-temperature gas gas flow temperature is 80-200 ℃.
In the present invention, high-temperature gas flow is each gas blow pipe 2-20L/min.
The invention provides the air-blowing experimental provision of realizing said method, this experimental provision is comprised of barotropic gas gas distributing system, high-temperature gas generation system and Sample location frame, wherein, described barotropic gas gas distributing system comprises gas source and flow controlling unit, described high-temperature gas generation system comprises heat generation unit and temperature control unit, and described Sample location frame comprises gas blow pipe stationary installation, sample hose fixed mount, sample hose fixed mount lifting regulator.
Particularly, air-blowing experimental provision of the present invention, is characterized in that, barotropic gas gas distributing system, high-temperature gas generation system and Sample location frame, consists of; Described barotropic gas gas distributing system connects high-temperature gas generation system and Sample location frame successively; Described gas distributing system can be the gas flow that each gas blow pipe provides 2-20L/min; Described high-temperature gas generation system is between malleation gas distributing system and Sample location frame; Described high-temperature gas generation system can produce the gas flow of temperature between 80-200 ℃;
Described barotropic gas gas distributing system comprises gas source 1 and flow controlling unit 2;
Described high-temperature gas generation system comprises heat generation unit 3, resistance wire 4 and temperature control unit 5;
Described Sample location frame comprises joint 6, gas blow pipe stationary installation 7, gas blow pipe 8, sample hose 9, sample hose fixed mount 10 and sample hose fixed mount lifting regulator 11;
In the present invention, described gas source 1 is connection traffic control module 2, heat generation unit 3 successively, in heat generation unit 3, be provided with resistance wire 4, temperature control unit 5 connects and controls heat generation unit 3, the opposite side of this heat generation unit 3 connects gas blow pipe stationary installation 7 by joint 6, described gas blow pipe 8 is fixedly connected in gas blow pipe stationary installation 7 and is placed in sample hose 9, described sample hose 9 is fixed on sample hose fixed mount 10, and this sample hose fixed mount 10 is placed on sample hose fixed mount lifting regulator 11;
In the present invention, described high-temperature gas generation system is between barotropic gas gas distributing system and Sample location frame, and the temperature of the gas flow of its generation is 80-200 ℃; In embodiments of the invention, described gas source 1 adopts steel cylinder source nitrogen;
In the present invention, adopt resistance wire 4 energising producing heats, gas flow is crossed resistance wire surface and is heated, and by the control to resistance wire both end voltage, regulates the temperature of air-flow;
In the present invention, the internal diameter of described gas blow pipe 8 is 3-10mm;
In the present invention, by described joint 6, can change easily the gas blow pipe stationary installation 7 that different number gas blow pipes are installed;
In the present invention, by described sample hose fixed mount lifting regulator 11, can adjust easily gas blow pipe 8 and be contained in the distance between the solvent surface of 9 li of sample hoses.
During use, the gases at high pressure that gas source is 1 li, under the effect of malleation, flow into flow controlling unit 2, obtain the gas flow of required flow after adjustment; Air-flow enters heat generation unit 3, and air-flow, when resistance wire 4, is heated on the surface of resistance wire 4, and the temperature of air-flow can be controlled by temperature control unit 5; Obtain after temperature required air-flow, gas is imported into gas blow pipe stationary installation 7, by gas blow pipe 8, purging is contained in the solvent surface of 9 li of sample hoses, sample hose 9 is placed on sample hose fixed mount 10, sample hose fixed mount 10 is placed on sample hose fixed mount lifting regulator 11, by sample hose fixed mount lifting regulator 11, adjusts heavy caliber gas blow pipes 8 and the distance being contained between the solvent surface of 9 li of sample hoses, concentrates the sample extraction liquid that contains organic solvent.
Use result shows, air-blowing experimental provision of the present invention adopts electrical heating resistance wire to produce heat, forming high-temperature gas air-flow purges solvent surface, organic solvent is realized from top layer to the heating of nexine, having avoided traditional nitrogen to blow concentrating instrument carries out integral body to organic solvent and is heated to the bumping phenomenon that boiling point occurs when above, therefore, more than gas temperature can be elevated to organic solvent boiling point, thereby accelerated the volatilization of solvent; Meanwhile, the solvent vapo(u)r of generation is taken out of sample hose by hot gas, has avoided the organic solvent having volatilized to occur condensing reflux, is conducive to the volatilization of solvent; Described gas blow pipe guarantees that there is larger contact area on high-temperature gas air-flow and organic solvent surface, accelerates the volatilization of solvent, can not cause splashing of organic solvent simultaneously; Described gas distributing system can be easily separated with sample hose stationary installation, is convenient for changing the gas blow pipe stationary installation that different number gas blow pipes are housed, and changes the quantity of each concentrating sample; Described sample hose fixed mount lifting regulator 11 can conveniently be adjusted the distance of gas blow pipe lower end and organic solvent upper surface, guarantees the purging effect of gas the best.
For the ease of understanding, below by the drawings and specific embodiments, the present invention is described in detail.It needs to be noted, specific embodiments and the drawings are only in order to illustrate, obviously those skilled in the art can carry out various corrections or change to the present invention according to explanation herein, within these corrections and change also will be included this patent scope in.
Accompanying drawing explanation
Fig. 1 is the structural representation of concentrating instrument of the present invention,
Wherein, 1 is that gas source of the gas, 2 is that flow controlling unit, 3 is that heat generation unit, 4 is that resistance wire, 5 is that temperature control unit, 6 is that joint, 7 is that gas blow pipe stationary installation, 8 is that gas blow pipe, 9 is that sample hose, 10 is that sample hose fixed mount, 11 is sample hose fixed mount lifting regulator.
Embodiment
Embodiment 1
As shown in Figure 1, air-blowing experimental provision of the present invention, is comprised of barotropic gas gas distributing system, high-temperature gas generation system and Sample location frame; Described barotropic gas gas distributing system connects high-temperature gas generation system and Sample location frame successively;
Described barotropic gas gas distributing system comprises gas source 1 and flow controlling unit 2; Described high-temperature gas generation system comprises heat generation unit 3, resistance wire 4 and temperature control unit 5; Described Sample location frame comprises joint 6, gas blow pipe stationary installation 7, gas blow pipe 8, sample hose 9, sample hose fixed mount 10 and sample hose fixed mount lifting regulator 11;
Described source of the gas 1 is connection traffic control module 2, heat generation unit 3 successively, in heat generation unit 3, be provided with resistance wire 4, temperature control unit 5 connects and controls heat generation unit 3, the opposite side of this heat generation unit 3 connects gas blow pipe stationary installation 7 by joint 6, described gas blow pipe 8 is fixedly connected in gas blow pipe stationary installation 7 and is placed in sample hose 9, described sample hose 9 is fixed on sample hose fixed mount 10, and this sample hose fixed mount 10 is placed on sample hose fixed mount lifting regulator 11;
Described high-temperature gas generation system is between barotropic gas gas distributing system and Sample location frame, and the temperature of the air-flow of its generation is 80 ℃; In the present embodiment, source of the gas 1 adopts steel cylinder source nitrogen;
In this air-blowing experimental provision, resistance wire 4 energising producing heats, nitrogen flows through resistance wire surface and is heated, and by the control to resistance wire both end voltage, regulates the temperature of stream of nitrogen gas; The internal diameter of described gas blow pipe 8 is 3mm; By described joint 6, can change easily the gas blow pipe stationary installation 7 that different number gas blow pipes are installed; By described sample hose fixed mount lifting regulator 11, can adjust easily gas blow pipe 8 and be contained in the distance between the solvent surface of 9 li of sample hoses.
During use, the high pressure nitrogen that source nitrogen is 1 li, under the effect of malleation, flows into flow controlling unit 2, obtains the stream of nitrogen gas of required flow after adjustment; Air-flow enters heat generation unit 3, when nitrogen is flowed through resistance wire 4, on the surface of resistance wire 4, be heated, and the temperature of stream of nitrogen gas can be controlled by temperature control unit 5; Obtain after temperature required stream of nitrogen gas, nitrogen is imported into gas blow pipe stationary installation 7, by gas blow pipe 8, purging is contained in the solvent surface of 9 li of sample hoses, sample hose 9 is placed on sample hose fixed mount 10, sample hose fixed mount 10 is placed on sample hose fixed mount lifting regulator 11, by sample hose fixed mount lifting regulator 11, adjusts heavy caliber gas blow pipes 8 and the distance being contained between the solvent surface of 9 li of sample hoses, concentrates the sample extraction liquid that contains organic solvent.
Embodiment 2
As shown in Figure 1, air-blowing experimental provision of the present invention, is comprised of barotropic gas gas distributing system, high-temperature gas generation system and Sample location frame; Described barotropic gas gas distributing system connects high-temperature gas generation system and Sample location frame successively; Described barotropic gas gas distributing system comprises gas source 1 and flow controlling unit 2; Described high-temperature gas generation system comprises heat generation unit 3, resistance wire 4 and temperature control unit 5; Described Sample location frame comprises joint 6, gas blow pipe stationary installation 7, gas blow pipe 8, sample hose 9, sample hose fixed mount 10 and sample hose fixed mount lifting regulator 11; Described source of the gas 1 is connection traffic control module 2, heat generation unit 3 successively, in heat generation unit 3, be provided with resistance wire 4, temperature control unit 5 connects and controls heat generation unit 3, the opposite side of this heat generation unit 3 connects gas blow pipe stationary installation 7 by joint 6, described gas blow pipe 8 is fixedly connected in gas blow pipe stationary installation 7 and is placed in sample hose 9, described sample hose 9 is fixed on sample hose fixed mount 10, and this sample hose fixed mount 10 is placed on sample hose fixed mount lifting regulator 11;
Described high-temperature gas generation system is between barotropic gas gas distributing system and Sample location frame, and the temperature of the air-flow of its generation is 100 ℃; In the present embodiment, source of the gas 1 adopts steel cylinder source nitrogen;
In this air-blowing experimental provision, resistance wire 4 energising producing heats, nitrogen flows through resistance wire surface and is heated, and by the control to resistance wire both end voltage, regulates the temperature of stream of nitrogen gas; The internal diameter of described gas blow pipe 8 is 8mm; By described joint 6, can change easily the gas blow pipe stationary installation 7 that different number gas blow pipes are installed; By described sample hose fixed mount lifting regulator 11, can adjust easily gas blow pipe 8 and be contained in the distance between the solvent surface of 9 li of sample hoses.
During use, the high pressure nitrogen that source nitrogen is 1 li, under the effect of malleation, flows into flow controlling unit 2, obtains the stream of nitrogen gas of required flow after adjustment; Air-flow enters heat generation unit 3, when nitrogen is flowed through resistance wire 4, on the surface of resistance wire 4, be heated, and the temperature of stream of nitrogen gas can be controlled by temperature control unit 5; Obtain after temperature required stream of nitrogen gas, nitrogen is imported into gas blow pipe stationary installation 7, by gas blow pipe 8, purging is contained in the solvent surface of 9 li of sample hoses, sample hose 9 is placed on sample hose fixed mount 10, sample hose fixed mount 10 is placed on sample hose fixed mount lifting regulator 11, by sample hose fixed mount lifting regulator 11, adjusts heavy caliber gas blow pipes 8 and the distance being contained between the solvent surface of 9 li of sample hoses, concentrates the sample extraction liquid that contains organic solvent.
Embodiment 3
As shown in Figure 1, air-blowing experimental provision of the present invention, is comprised of barotropic gas gas distributing system, high-temperature gas generation system and Sample location frame; Described barotropic gas gas distributing system connects high-temperature gas generation system and Sample location frame successively; Described barotropic gas gas distributing system comprises gas source 1 and flow controlling unit 2; Described high-temperature gas generation system comprises heat generation unit 3, resistance wire 4 and temperature control unit 5; Described Sample location frame comprises joint 6, gas blow pipe stationary installation 7, gas blow pipe 8, sample hose 9, sample hose fixed mount 10 and sample hose fixed mount lifting regulator 11; Described source of the gas 1 is connection traffic control module 2, heat generation unit 3 successively, in heat generation unit 3, be provided with resistance wire 4, temperature control unit 5 connects and controls heat generation unit 3, the opposite side of this heat generation unit 3 connects gas blow pipe stationary installation 7 by joint 6, described gas blow pipe 8 is fixedly connected in gas blow pipe stationary installation 7 and is placed in sample hose 9, described sample hose 9 is fixed on sample hose fixed mount 10, and this sample hose fixed mount 10 is placed on sample hose fixed mount lifting regulator 11;
Described high-temperature gas generation system is between barotropic gas gas distributing system and Sample location frame, and the temperature of the air-flow of its generation is 200 ℃; In the present embodiment, source of the gas 1 adopts steel cylinder source nitrogen;
In this air-blowing experimental provision, resistance wire 4 energising producing heats, nitrogen flows through resistance wire surface and is heated, and by the control to resistance wire both end voltage, regulates the temperature of stream of nitrogen gas; The internal diameter of described gas blow pipe 8 is 10mm; By described joint 6, can change easily the gas blow pipe stationary installation 7 that different number gas blow pipes are installed; By described sample hose fixed mount lifting regulator 11, can adjust easily gas blow pipe 8 and be contained in the distance between the solvent surface of 9 li of sample hoses.
During use, the high pressure nitrogen that source nitrogen is 1 li, under the effect of malleation, flows into flow controlling unit 2, obtains the stream of nitrogen gas of required flow after adjustment; Air-flow enters heat generation unit 3, when nitrogen is flowed through resistance wire 4, on the surface of resistance wire 4, be heated, and the temperature of stream of nitrogen gas can be controlled by temperature control unit 5; Obtain after temperature required stream of nitrogen gas, nitrogen is imported into gas blow pipe stationary installation 7, by gas blow pipe 8, purging is contained in the solvent surface of 9 li of sample hoses, sample hose 9 is placed on sample hose fixed mount 10, sample hose fixed mount 10 is placed on sample hose fixed mount lifting regulator 11, by sample hose fixed mount lifting regulator 11, adjusts heavy caliber gas blow pipes 8 and the distance being contained between the solvent surface of 9 li of sample hoses, concentrates the sample extraction liquid that contains organic solvent.
Above-described embodiment shows the concentrated result of sample extraction liquid, the quick method for concentration of malleation of the present invention top layer high temperature, use air-blowing experimental provision by high-temperature gas, the solvent surface high-temp of sample extraction liquid to be heated, the heating to nexine by top layer to solvent, solvent is volatilized fast, solvent vapo(u)r is taken away by hot gas simultaneously, realizes the concentrated fast of sample extraction liquid; Related air-blowing experimental provision is simple in structure, flexible operation, and extendability is strong.
Claims (8)
1. the quick method for concentration of malleation top layer high temperature, it is characterized in that, it comprises, use air-blowing experimental provision to purge organic solvent surface by high temperature hot gas, to organic solvent by top layer inwards layer high-temperature heating, solvent is volatilized fast, and solvent vapo(u)r is taken away by hot gas simultaneously, realizes sample extraction liquid concentrated fast.
2. by method claimed in claim 1, it is characterized in that, described air-blowing gas adopts nitrogen, air or helium, and gas flow temperature is 80-200 ℃, and gas flow is 2-20L/min.
3. the quick concentrated air-blowing experimental provision of malleation top layer high temperature, is characterized in that, barotropic gas gas distributing system, high-temperature gas generation system and Sample location frame, consists of; Described barotropic gas gas distributing system connects high-temperature gas generation system and Sample location frame successively;
Described barotropic gas gas distributing system comprises source of the gas (1) and flow controlling unit (2);
Described high-temperature gas generation system comprises heat generation unit (3), resistance wire (4) and temperature control unit (5);
Described Sample location frame comprises joint (6), gas blow pipe stationary installation (7), gas blow pipe (8), sample hose (9), sample hose fixed mount (10) and sample hose fixed mount lifting regulator (11);
Described source of the gas (1) is connection traffic control module (2) successively, heat generation unit (3), in heat generation unit (3), be provided with resistance wire (4), temperature control unit (5) connects and controls heat generation unit (3), the opposite side of this heat generation unit (3) connects gas blow pipe stationary installation (7) by joint (6), described gas blow pipe (8) is fixedly connected in gas blow pipe stationary installation (7), and be placed in sample hose (9), described sample hose (9) is fixed on sample hose fixed mount (10), this sample hose fixed mount (10) is placed on sample hose fixed mount lifting regulator (11).
4. by the quick concentrated air-blowing experimental provision of malleation claimed in claim 3 top layer high temperature, it is characterized in that, described high-temperature gas generation system is between barotropic gas gas distributing system and Sample location frame, and the temperature of the air-flow of its generation is 80-200 ℃.
5. by the quick concentrated air-blowing experimental provision of malleation claimed in claim 3 top layer high temperature, it is characterized in that, described source of the gas (1) adopts nitrogen, air or helium.
6. by the quick concentrated air-blowing experimental provision of malleation claimed in claim 3 top layer high temperature, it is characterized in that, described source of the gas (1) adopts steel cylinder source nitrogen.
7. by the quick concentrated air-blowing experimental provision of malleation claimed in claim 3 top layer high temperature, it is characterized in that, the internal diameter of described gas blow pipe (8) is 3-10mm.
8. by the quick concentrated air-blowing experimental provision of malleation claimed in claim 3 top layer high temperature, it is characterized in that, described gas blow pipe stationary installation (7) can be changed.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310051353.XA CN103983504B (en) | 2013-02-08 | 2013-02-08 | A kind of malleation top layer high temperature rapid concentration method |
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| CN201310051353.XA CN103983504B (en) | 2013-02-08 | 2013-02-08 | A kind of malleation top layer high temperature rapid concentration method |
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| CN106370506A (en) * | 2016-11-03 | 2017-02-01 | 北京普立泰科仪器有限公司 | Method and device for improving concentration speed of diameter-variable concentration cup |
| WO2019014887A1 (en) * | 2017-07-20 | 2019-01-24 | 汎锶科艺股份有限公司 | Surface enhanced raman spectroscopy detection method for detecting pesticide residue |
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