CN104181028A - Device capable of achieving automatic high-flux volatilization of small-volume solvent - Google Patents
Device capable of achieving automatic high-flux volatilization of small-volume solvent Download PDFInfo
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- CN104181028A CN104181028A CN201410325464.XA CN201410325464A CN104181028A CN 104181028 A CN104181028 A CN 104181028A CN 201410325464 A CN201410325464 A CN 201410325464A CN 104181028 A CN104181028 A CN 104181028A
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Abstract
The invention belongs to the field of analytical chemistry and relates to a device and a method capable of achieving the automatic high-flux volatilization of a small-volume solvent. The device is composed of a sealed cavity, a solvent plate heating module, a temperature controller, a vacuum pump, a pressure controller, a pressure change monitoring module and a condensing system, wherein transparent windows are arranged at four surfaces of the sealed cavity; an air pumping plate is arranged at the top of the cavity; the bottom of the cavity is made of a thermal conductive material and is tightly bonded with the solvent heating module. According to the device, arbitrary pieces of the small volume solvent is put into the sealed cavity to be heated, a negative pressure is realized, and the high-flux and rapid volatilization of the small volume solve is realized; as shown by use results, the heating temperature, negative pressure or solvent volatilization time can be adjusted accordingly to establish different solve volatilization procedures.
Description
Technical field
The invention belongs to analytical chemistry field, relate to a kind of device of realizing the high throughput automated volatilization of small size solvent; This device can be used for accelerating sample pretreatment speed.
Background technology
At analysis field, sample pre-treatments is in sample analysis, to take time and effort more part conventionally; Wherein, volatilization organic solvent, realizing sample concentration and solvent switch is the common operation steps of sample pre-treatments.In prior art, mainly comprise that for the mode of solvent evaporates rotary evaporation is concentrated and nitrogen blowing is concentrated; Though the concentrated evaporation rate of described rotary evaporation is fast, can be used for tens of volatilizations to hundreds of milliliters of large volume solvents, a solvent that conventionally once can only volatilize, in the time processing a large amount of sample, speed is slow; Though described nitrogen blowing concentrates volatilization when can be used for many parts of organic solvents, and make up that rotary evaporation is concentrated is not suitable for several milliliters or the shortcoming of small size solvent evaporates more, but its nitrogen flow consistance purging for every part of solvent is difficult to control, often cause every part of solvent evaporates speed inconsistent, and because the size of every road nitrogen flow is difficult to repetition between each use, the needed time while causing being difficult for calculating each certain solvent of purging volatilization to certain volume, be difficult to realize the robotization of solvent evaporates.
High flux and robotization are one of directions of modern Sample Pretreatment Technique Used development.Above-mentioned rotary evaporation is concentrated concentrates with nitrogen blowing the high flux and the robotization that all do not realize solvent evaporates simultaneously; Meanwhile, reducing with an organic solvent, reducing costs, reduce Health cost and the environmental pollution of solvent to analyst is also trend and the demand of modern Sample Pretreatment Technique Used.Current, to set up in environment, food and biological monitoring analytical approach, the solvent volume that need to volatilize generally, between hundreds of microlitres are to several milliliters, is all drawn close to reducing this trend of solvent use amount.
Therefore, be badly in need of at present a kind of volatilization device of realizing small size solvent high flux and robotization, to adapt to the needs of modern Sample Pretreatment Technique Used development.
Summary of the invention
The object of the invention is to overcome the defect of prior art, a kind of device and method of realizing the high throughput automated volatilization of small size solvent is provided.
Device of the present invention can heat and form negative pressure to the many parts of small size solvents of inserting in airtight cavity, accelerates the evaporation rate of solvent; Change by controlling negative pressure pressure in solvent evaporates time or monitoring airtight cavity, realize high flux and robotization volatilization to small size solvent.
Particularly, the device that this realizes the high throughput automated volatilization of small size solvent, is characterized in that, is made up of airtight cavity, solvent plate heating module, temperature controller, vacuum pump, pressure controller, pressure variation monitoring module and condenser system; The four sides of described airtight cavity is equipped with transparent window, and evacuating plate is installed at top, and bottom adopts Heat Conduction Material preparation and holds tightly together with solvent plate heating module;
Described solvent plate heating module is opposite to the many parts of synchronous homogeneous heatings of small size solvent in airtight cavity, by extremely required heating-up temperature of temperature controller feedback adjusting; Described vacuum pump vacuumizes airtight cavity, forms negative pressure, by extremely required negative pressure pressure of pressure controller feedback adjusting; The solvent vapo(u)r that volatilization forms under heating and negative pressure, is extracted out after airtight cavity by vacuum pump, is again condensed into liquid in described condenser system; Described pressure variation monitoring module monitors airtight cavity internal pressure changes, and controls the startup of described vacuum pump and the heating of solvent plate and stops according to the solvent evaporates time of pressure changing or setting, controls the opening and closing of described airtight cavity;
In the present invention, the many parts of small size solvents of inserting in airtight cavity are heated and form negative pressure, change by controlling negative pressure pressure in solvent evaporates time or monitoring airtight cavity, realize high flux and the robotization volatilization of small size solvent;
In the present invention, by being controlled under certain heating-up temperature and negative pressure pressure, solvent evaporates, to the required time of certain volume, is evaporated into certain volume by solvent robotization;
In the present invention, the time that while using solvent evaporates extremely dry, in airtight cavity, negative pressure pressure remains unchanged, solvent robotization evaporated into dry as instruction solvent evaporates to dry index;
In the present invention, small size solvent refers to that solvent volume is less than 5mL;
In the present invention, described device comprises rectangle or square airtight cavity, solvent plate heating module, temperature controller, vacuum pump, pressure controller, pressure variation monitoring module and condenser system, transparent window is all equipped with at described airtight cavity four sides, while needs, can cover lucifuge, evacuating plate is installed at its top, bottom adopts Heat Conduction Material (as steel plate or copper coin), holds tightly together with solvent plate heating module;
In the present invention, described airtight cavity top evacuating plate is porous plate;
In the present invention, described pressure variation monitoring module can be monitored negative pressure pressure in airtight cavity and be changed, and controls closing and opening of vacuum system, heating system and airtight cavity;
In the present invention, start to evaporating into when dry at solvent flashing, in described airtight cavity, negative pressure pressure is through 3 stages: volatilize the phase fast at solvent, and negative pressure pressure fast rise; Closely volatilize the phase at solvent, negative pressure pressure level-off; Volatilize the phase at solvent, negative pressure pressure remains unchanged; By the variation of monitoring airtight cavity pressure, can judge solvent evaporates progress; Therefore, device of the present invention adopts the duration that in airtight cavity, negative pressure pressure remains unchanged, and the index volatilizing as instruction solvent, realizes robotization solvent is volatilized; Described device can accurately be controlled the negative pressure pressure in airtight cavity and the heating-up temperature to solvent, required time when measurable solvent is concentrated into certain volume, therefore, by controlling the solvent evaporates time, can realize robotization by solvent evaporates to certain volume.
In embodiments of the invention,
The length of described airtight cavity be 30cm, width be 20cm, highly for 12cm, (length is that 13cm, width are 8.5cm, highly are 5cm can to hold 4 standards, 96 hole sample panel; Every pore volume is 2mL); Transparent window (can cover lucifuge while needs), the progress of observable solvent evaporates and situation are all equipped with in four sides; Evacuating plate is installed at its top; Bottom adopts Heat Conduction Material (as steel plate or copper coin), holds tightly together with solvent plate heating module;
Described solvent plate heating module can be to the many parts of synchronous homogeneous heatings of small size solvent on solvent plate, and heating-up temperature scope is between 40 DEG C to 150 DEG C;
Described temperature controller, by negative feedback control solvent plate heating module, maintains the temperature value of airtight cavity bottom temp in setting;
Described vacuum pump can drop to 100pa left and right by minimum the pressure in airtight cavity, provides solvent evaporates needed negative pressure pressure;
Described pressure controller, by negative feedback control vacuum pump, maintains the interior negative pressure pressure of airtight cavity in setting value;
Described condenser system: adopt time condensation system that the solvent vapo(u)r volatilizing is condensed into liquid again.
Described evacuating plate is pressed ad-hoc location (as shown in Figure 4), on orifice plate, bore the aspirating hole of 17 8mm bleeding, gas circuit is placed in bleeds in orifice plate, and steam is converged by outer circumferential center, steam is taken away by vacuum pump through center extraction hole, is conducive to make the evaporation rate in diverse location solvent consistent.
Further, the invention provides a kind of method that realizes the high throughput automated volatilization of small size solvent based on said apparatus, it is characterized in that, it comprises: the many parts of small size solvents of inserting in airtight cavity are heated and form negative pressure, change by controlling negative pressure pressure in solvent evaporates time or monitoring airtight cavity, realize high flux and the robotization volatilization of small size solvent.
In the inventive method, described heating-up temperature scope is between 40 DEG C to 150 DEG C; Described negative pressure pressure is 100pa.
In the inventive method, the time that while using solvent evaporates extremely dry, in airtight cavity, negative pressure pressure remains unchanged is as indicating solvent evaporates to dry index.
In the inventive method, described small size solvent refers to that solvent volume is less than 5mL.
In the present invention, get with needing solvent flashing in actual sample analysis and form identical solvent in 96 hole sample panel, be placed in described airtight cavity, in the analysis of simulation actual sample, need volume and the umber of solvent flashing; Do not occur splashing under the prerequisite of bumping ensureing that testing compound does not lose with solvent, by adjusting heating-up temperature and negative pressure pressure, optimum heating-up temperature, negative pressure pressure and volatilization time while finding solvent evaporates to certain volume, as the parameter of solvent evaporates in actual sample is analyzed, realize robotization by solvent evaporates to certain volume; By the solvent striking point observing with the naked eye from described airtight cavity transparent window, judge that when the duration that in airtight cavity, negative pressure pressure remains unchanged be how many times, can think that solvent has been concentrated into by volatilization dry, between now, be concentrated into dry index as automatically controlling solvent, realize robotization by solvent evaporates to dry.
Described pressure variation monitoring module: in the time that the solvent evaporates time reaches setting value, this module is closed vacuum pump and heating module power supply, opens described airtight cavity simultaneously, stops the volatilization to solvent, realizes robotization by solvent evaporates to certain volume; The time remaining unchanged when described airtight cavity internal pressure reaches setting value, thinks when solvent is volatilized, and this module is closed vacuum pump and heating module power supply, opens airtight cavity simultaneously, realizes robotization by solvent evaporates to dry.
The invention has the advantages that,
In described device, airtight cavity can expand, the small size solvent that can simultaneously volatilize arbitrarily part, thus the high flux of realizing small size solvent volatilizees simultaneously; Due in same airtight cavity, solvent is subject to identical heating-up temperature and negative pressure pressure, can improve the consistance between many parts of solvent evaporates simultaneously; Solvent vapo(u)r is again condensed into liquid by this device, reclaims solvent, reduces solvent discharge; And user can adjust heating-up temperature, negative pressure pressure or solvent evaporates time as required, set up different solvents volatilization program; Apparatus of the present invention safety and environmental protection, mode of operation simple and flexible, applicability is good.
Brief description of the drawings
Fig. 1 is the structural representation that the present invention realizes the device of the high throughput automated volatilization of small size solvent;
Fig. 2 is the side schematic view of airtight cavity in device of the present invention;
Fig. 3 is negative pressure pressure temporal evolution simulation drawing in airtight cavity described in the concentration process of device of the present invention;
Fig. 4 is aspirating hole position and steam flow schematic top plan view on the evacuating plate of device of the present invention.
Embodiment
Embodiment 1
As shown in Figure 2, this realizes the device of the high throughput automated volatilization of small size solvent, is made up of airtight cavity, solvent plate heating module, temperature controller, vacuum pump, pressure controller, pressure variation monitoring module and condenser system; The four sides of described airtight cavity is equipped with transparent window, and evacuating plate is installed at top, and bottom adopts Heat Conduction Material preparation and holds tightly together with solvent plate heating module;
The length of described airtight cavity be 30cm, width be 20cm, highly for 12cm, (length is that 13cm, width are 8.5cm, highly are 5cm can to hold 4 standards, 96 hole sample panel; Every pore volume is 2mL); Transparent window (can cover lucifuge while needs), the progress of observable solvent evaporates and situation are all equipped with in four sides; Evacuating plate is installed at its top; Bottom adopts Heat Conduction Material (as steel plate or copper coin), holds tightly together with solvent plate heating module;
Described solvent plate heating module can be to the many parts of synchronous homogeneous heatings of small size solvent on solvent plate, and heating-up temperature scope is between 40 DEG C to 150 DEG C;
Described temperature controller, by negative feedback control solvent plate heating module, maintains the temperature value of airtight cavity bottom temp in setting;
Described vacuum pump can drop to 100pa left and right by minimum the pressure in airtight cavity, provides solvent evaporates needed negative pressure pressure;
Described pressure controller, by negative feedback control vacuum pump, maintains the interior negative pressure pressure of airtight cavity in setting value;
Described condenser system: adopt time condensation system that the solvent vapo(u)r volatilizing is condensed into liquid again.
Described evacuating plate is pressed ad-hoc location (as shown in Figure 4), on orifice plate, bore the aspirating hole of 17 8mm bleeding, gas circuit is placed in bleeds in orifice plate, steam is converged by outer circumferential center, steam is taken away by vacuum pump through center extraction hole, is conducive to make the evaporation rate in diverse location solvent consistent;
When use, get with needing solvent flashing in actual sample analysis and form identical solvent in 96 hole sample panel, be placed in described airtight cavity, in the analysis of simulation actual sample, need volume and the umber of solvent flashing; Do not occur splashing under the prerequisite of bumping ensureing that testing compound does not lose with solvent, by adjusting heating-up temperature and negative pressure pressure, optimum heating-up temperature, negative pressure pressure and volatilization time while finding solvent evaporates to certain volume, as the parameter of solvent evaporates in actual sample is analyzed, realize robotization by solvent evaporates to certain volume; By the solvent striking point observing with the naked eye from described airtight cavity transparent window, judge that when the duration that in airtight cavity, negative pressure pressure remains unchanged be how many times, can think that solvent has been concentrated into by volatilization dry, between now, be concentrated into dry index as automatically controlling solvent, realize robotization by solvent evaporates to dry.
Described pressure variation monitoring module: in the time that the solvent evaporates time reaches setting value, this module is closed vacuum pump and heating module power supply, opens described airtight cavity simultaneously, stops the volatilization to solvent, realizes robotization by solvent evaporates to certain volume; The time remaining unchanged when described airtight cavity internal pressure reaches setting value, thinks when solvent is volatilized, and this module is closed vacuum pump and heating module power supply, opens airtight cavity simultaneously, realizes robotization by solvent evaporates to dry.
The result of embodiment shows, this is realized in the device of the high throughput automated volatilization of small size solvent, and described airtight cavity can expand, the small size solvent that can simultaneously volatilize arbitrarily part, thus the high flux of realizing small size solvent volatilizees simultaneously; Due in same airtight cavity, solvent is subject to identical heating-up temperature and negative pressure pressure, has improved the consistance between many parts of solvent evaporates simultaneously; Solvent vapo(u)r is again condensed into liquid by described device, reclaims solvent, reduces solvent discharge; And user can adjust heating-up temperature, negative pressure pressure or solvent evaporates time as required, set up different solvents volatilization program; In addition, described equipment safety environmental protection, mode of operation simple and flexible, applicability is good.
Claims (13)
1. a device of realizing the high throughput automated volatilization of small size solvent, is characterized in that, is made up of airtight cavity, solvent plate heating module, temperature controller, vacuum pump, pressure controller, pressure variation monitoring module and condenser system; The four sides of described airtight cavity is equipped with transparent window, and evacuating plate is installed at top, bottom adopt Heat Conduction Material preparation and with solvent plate heating module close adhesion.
2. device as claimed in claim 1, is characterized in that, the length of described airtight cavity be 30cm, width be 20cm, highly for 12cm, hold 4 standards, 96 hole sample panel.
3. device as claimed in claim 1, is characterized in that, described solvent plate heating module is to the many parts of synchronous homogeneous heatings of small size solvent on solvent plate, and heating-up temperature scope is between 40 DEG C to 150 DEG C.
4. device as claimed in claim 1, is characterized in that, described temperature controller, by negative feedback control solvent plate heating module, maintains the temperature value of airtight cavity bottom temp in setting.
5. device as claimed in claim 1, is characterized in that, described vacuum pump is by minimum the pressure in the airtight cavity 100pa left and right that drops to.
6. device as claimed in claim 1, is characterized in that, described pressure controller, by negative feedback control vacuum pump, maintains the interior negative pressure pressure of airtight cavity in setting value.
7. device as claimed in claim 1, is characterized in that, described condenser system adopts time condensation system that the solvent vapo(u)r volatilizing is condensed into liquid again.
8. device as claimed in claim 1, is characterized in that, the top evacuating plate of described airtight cavity is porous plate.
9. the device as described in claim 1 or 8, is characterized in that, described evacuating plate bores the aspirating hole of 17 8mm by ad-hoc location bleeding on orifice plate, and gas circuit is placed in bleeds in orifice plate.
10. the method that realizes the high throughput automated volatilization of small size solvent of the device based on claim 1, it is characterized in that, it comprises: the many parts of small size solvents of inserting in airtight cavity are heated and form negative pressure, change by controlling negative pressure pressure in solvent evaporates time or monitoring airtight cavity, realize high flux and the robotization volatilization of small size solvent.
11. methods as claimed in claim 10, is characterized in that, described heating-up temperature scope is between 40 DEG C to 150 DEG C; Described negative pressure pressure is 100pa.
12. methods as claimed in claim 10, is characterized in that, the time that while using solvent evaporates extremely dry, in airtight cavity, negative pressure pressure remains unchanged is as indicating solvent evaporates to dry index.
13. methods as claimed in claim 10, is characterized in that, described small size solvent refers to that solvent volume is less than 5mL.
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| CN201410325464.XA CN104181028A (en) | 2014-07-09 | 2014-07-09 | Device capable of achieving automatic high-flux volatilization of small-volume solvent |
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Cited By (3)
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| CN105445312A (en) * | 2015-01-04 | 2016-03-30 | 宁波英飞迈材料科技有限公司 | Micro-region heating device |
| CN107290202A (en) * | 2016-03-31 | 2017-10-24 | 庞英明 | A kind of nitrogen blows concentrating instrument |
| CN112557248A (en) * | 2020-12-10 | 2021-03-26 | 中国工程物理研究院核物理与化学研究所 | Soluble component flux segregation device and testing method |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105445312A (en) * | 2015-01-04 | 2016-03-30 | 宁波英飞迈材料科技有限公司 | Micro-region heating device |
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| CN112557248A (en) * | 2020-12-10 | 2021-03-26 | 中国工程物理研究院核物理与化学研究所 | Soluble component flux segregation device and testing method |
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