CN112557248B - Soluble fraction flux segregation device and testing method - Google Patents
Soluble fraction flux segregation device and testing method Download PDFInfo
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- CN112557248B CN112557248B CN202011434553.XA CN202011434553A CN112557248B CN 112557248 B CN112557248 B CN 112557248B CN 202011434553 A CN202011434553 A CN 202011434553A CN 112557248 B CN112557248 B CN 112557248B
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- 230000004907 flux Effects 0.000 title claims abstract description 29
- 238000012360 testing method Methods 0.000 title claims abstract description 20
- 238000005204 segregation Methods 0.000 title abstract description 7
- 239000002904 solvent Substances 0.000 claims abstract description 193
- 239000007788 liquid Substances 0.000 claims abstract description 41
- 238000009833 condensation Methods 0.000 claims abstract description 23
- 230000005494 condensation Effects 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 21
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 238000007789 sealing Methods 0.000 claims description 51
- 238000000926 separation method Methods 0.000 claims description 19
- 238000005452 bending Methods 0.000 claims description 15
- 239000003795 chemical substances by application Substances 0.000 claims description 11
- 230000010355 oscillation Effects 0.000 claims description 9
- 238000002360 preparation method Methods 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 238000000502 dialysis Methods 0.000 claims description 8
- 229910052751 metal Inorganic materials 0.000 claims description 8
- 239000002184 metal Substances 0.000 claims description 8
- 230000009286 beneficial effect Effects 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- 239000011148 porous material Substances 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 238000010998 test method Methods 0.000 claims description 5
- 239000002699 waste material Substances 0.000 claims description 5
- 238000002203 pretreatment Methods 0.000 claims description 2
- 238000004891 communication Methods 0.000 claims 1
- 238000007599 discharging Methods 0.000 abstract description 4
- 238000007654 immersion Methods 0.000 abstract description 2
- 230000001276 controlling effect Effects 0.000 description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 5
- 239000004202 carbamide Substances 0.000 description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 238000010828 elution Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000006261 foam material Substances 0.000 description 3
- 230000004308 accommodation Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000007667 floating Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 229920002379 silicone rubber Polymers 0.000 description 2
- 239000004945 silicone rubber Substances 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 229920002943 EPDM rubber Polymers 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000002984 plastic foam Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000000452 restraining effect Effects 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
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Abstract
The invention discloses a soluble fraction flux segregation device and a testing method. The method comprises the steps of firstly immersing a pretreated sample in a sample bearing module which is filled with a certain volume of solvent in advance, continuously volatilizing the solvent in the solvent bearing module through continuous controllable heating, continuously entering the sample bearing module through a condensation flow guiding module, automatically discharging all the solvent in the sample bearing module into the solvent bearing module after the total liquid level in the sample bearing module reaches a specific height, simultaneously bringing the soluble matters in the sample into the solvent bearing module, continuously introducing the pure solvent into the sample bearing module through continuous volatilizing, condensation and flow guiding of the solvent in the solvent bearing module, and continuously bringing the soluble matters in the sample into the solvent bearing module through continuous immersion and automatic liquid discharging until all the soluble matters are separated, so that the sample in the sample bearing module does not contain soluble matters any more.
Description
Technical Field
The invention belongs to the technical field of material preparation technology and performance test, and particularly relates to a soluble fraction flux segregation device and a test method.
Background
In the preparation process of rubber and plastic foam materials, a solution method pore-forming technology by means of urea, sodium chloride and the like becomes an important pore-forming mode due to the high environmental protection degree. However, in the stage of removing pore-forming agents such as urea and sodium chloride, the crosslinked sample must be immersed in pure water, and heated and stirred or vibrated for a certain period of time (Liu Pengbo, liu Daolong, xuwen. An open-cell silicone rubber foam material and its preparation method and use: CN 1884378A [ P ].2006-12-27. Song Hongtao, fu Yibei, an You, etc.. An ethylene-propylene-diene monomer-based microcellular foam material and its preparation method: CN 105348655A [ P ].2016-02-24, song Hongtao, yang Jiangna, an You, etc.. An organic reinforcing silicone rubber foam material and its preparation method: CN 107815123A [ P ].2018-03-20 ]. In the actual operation, in order to ensure that the pore-forming agent can be removed as much as possible, water needs to be changed many times until the pore-forming agent in the sample is eluted and isolated. Therefore, the operation burden of the experimenters is increased, and a large amount of waste liquid is generated. This is particularly pronounced when the sample size is large. This is very disadvantageous for series development and mass production. Therefore, the research and development of the device and the testing method capable of overcoming the defects and realizing the automatic segregation in flux have very positive significance, and have very important significance for promoting the popularization and application of the solution method pore-forming technology.
Disclosure of Invention
It is an object of the present invention to address at least the above problems and/or disadvantages and to provide at least the advantages described below.
To achieve these objects and other advantages and in accordance with the purpose of the invention, there is provided a soluble fraction flux separation apparatus comprising:
a solvent-borne module, comprising:
a solvent tank, the bottom side of which is provided with a waste liquid discharge pipe with a manual valve;
a vibration pump provided at the center of the inner bottom of the solvent tank;
A heater provided at an inner bottom edge of the solvent tank;
A controller which is arranged outside the solvent tank and is connected with the heater;
at least four supporting springs which are arranged at the bottom of the inner side of the solvent tank and are uniformly arranged around the vibration pump;
a sample carrier module disposed within a solvent tank, the sample carrier module comprising:
the inner side of the sample cell is provided with an automatic liquid drain device;
The at least four oscillation support posts are uniformly arranged at the bottom of the sample tank and are in matched connection with at least four supporting springs of the solvent tank; the bottom of the sample pool is contacted with the top of the vibration pump;
the condensation diversion module is connected above the solvent bearing module; the condensation diversion module comprises:
The periphery of the sealing cover is provided with a flow guiding skirt; the sealing cover is buckled and connected to the solvent tank;
an annular condenser provided at the center of the top of the sealing cover; a window is arranged in the middle of the annular condenser;
And a safety valve provided at the top of the sealing cover.
Preferably, four corners of the outer bottom of the solvent tank are provided with casters; sample cell handles are arranged on two sides of the outer part of the sample cell.
Preferably, a groove is formed in the upper edge of the solvent tank, and a sealing ring is arranged in the groove.
Preferably, the heater is a ring-shaped heating tube.
Preferably, the sample cell is a box with an open upper part; the automatic liquid draining device is a U-shaped pipe which is downwards fixed on the inner side of the sample tank through a fixed block, one pipe orifice of one side of the U-shaped pipe extends out of the bottom of the sample tank and is communicated with the solvent tank, and the pipe orifice of the other side extends into a circular groove at the bottom of the sample tank; and the pipe wall of the pipe orifice at one side extending out of the bottom of the sample tank is sealed with the sample tank through a sealing sleeve.
Preferably, the at least four oscillation support posts are connected with at least four supporting springs of the solvent tank in a matching way: the inner diameter of each oscillating strut is slightly larger than the outer diameter of the supporting spring, and the oscillating struts are sleeved on the springs to realize matched connection.
Preferably, the edge of sealed lid is provided with epitaxial portion I, evenly is provided with a plurality of couples on the epitaxial portion, the edge of solvent groove is provided with epitaxial portion II, is provided with a plurality of catches corresponding with a plurality of couples on the epitaxial portion II, realizes the lock of sealed lid and solvent groove and is connected through the phase-match connection of a plurality of catches and a plurality of couples.
Preferably, the guide skirt is a bending plate, and the bending angle of the bending plate is an obtuse angle; one surface of the bending plate is connected to the sealing cover, and the other surface of the bending plate is suspended; sealing cover handles are arranged on two sides of the outer portion of the sealing cover.
Preferably, the annular condenser is internally provided with a containing cavity, and a water inlet and a water outlet which are communicated with the containing cavity are arranged on the annular condenser.
The invention also provides a method for testing by adopting the soluble fraction flux segregation device, which comprises the following steps:
Step one, placing a sample bearing module into a solvent bearing module, sleeving at least four oscillating struts into at least four supporting springs, and adjusting to be stable;
Step two, pretreating a sample to be treated, which is cut and has the weight of m a, and horizontally placing the sample at the bottom of the inner side of a sample pool of the sample bearing module; the pretreatment method comprises the following steps: when the density of the sample is smaller, the sample can be wrapped by dialysis paper and then put into a metal mesh bag; when the types of the samples which can be processed in the same batch are more, a grid with scale marks can be arranged at the bottom of a sample cell of the sample carrying module, and then the samples are fixed in different grids;
Step three, injecting a certain volume of solvent into the sample cell of the sample bearing module, and enabling the solvent to pass through the sample to ensure that the sample is completely soaked in the solvent;
Step four, injecting a certain volume of solvent into a solvent tank of the solvent bearing module, and ensuring that the liquid level height of the solvent does not exceed the liquid level height in a sample cell of the sample bearing module;
Step five, placing a sealing cover of the condensation diversion module on the upper part of a solvent tank of the solvent bearing module, and buckling and connecting the sealing cover;
Step six, opening a controller, setting the temperature, controlling a heater to continuously heat the solvent in the solvent tank of the solvent bearing module to volatilize the solvent, starting a vibration pump to vibrate the sample tank, and enabling the liquid in the sample tank of the sample bearing module to eliminate the concentration gradient so as to be beneficial to dissolving soluble components;
Step seven, after the sample is sufficiently dissolved out and soluble components in the sample are isolated, closing a controller, after the temperature of the device is reduced to room temperature, slightly pulling a safety valve, unloading residual internal pressure, opening a sealing cover in buckled connection, taking out the sample, drying and weighing to obtain m b;
Step eight, when the porous material prepared by the physical pore-forming method is processed, according to the total mass of the physical pore-forming agent added in the sample preparation stage, whether the pore-forming agent is completely dissolved out and removed can be judged by calculating the difference between m a and m b; when the gel content test of the batch samples is performed, the (m b×100)/ma) of the corresponding samples is calculated, respectively, so that the gel content value gel% of each sample can be obtained.
The invention provides a soluble fraction flux segregation device and a testing method, the device comprises a sample bearing module, a solvent bearing module and a condensation flow guiding module, wherein the sample bearing module is a functional unit for bearing samples, adjusting the states of the samples or marking and arranging different types of samples, the solvent bearing module is a functional unit for bearing soluble fraction solvents in a dissolved-out sample, and simultaneously continuously and controllably heating the solvents, and the condensation flow guiding module is a functional unit for condensing solvent vapor and guiding the solvent vapor into the sample bearing module. The method comprises the steps of firstly immersing a pretreated sample in a sample bearing module which is filled with a certain volume of solvent in advance, continuously volatilizing the solvent in the solvent bearing module through continuous controllable heating, continuously entering the sample bearing module through a condensation flow guiding module, automatically discharging all the solvent in the sample bearing module into the solvent bearing module after the total liquid level in the sample bearing module reaches a specific height, simultaneously bringing dissolved soluble matters into the solvent bearing module, continuously introducing pure solvent into the sample bearing module through continuous volatilizing, condensation and flow guiding of the solvent in the solvent bearing module, and continuously bringing the soluble matters contained in the sample into the solvent bearing module through continuous immersion and automatic liquid drainage until all the soluble matters are dissolved out, so that the sample in the sample bearing module does not contain soluble matters any more.
The invention at least comprises the following beneficial effects: the device has simple structural design and is convenient for practical control, and the test method saves time and labor, avoids frequent replacement of the solvent, and greatly reduces the use amount of the solvent; the shape of the sample is not particularly required, and the sample with smaller density only needs to be pretreated and fixed (such as wrapping dialysis paper and a metal net) so as to be fully soaked, thereby improving the elution efficiency; meanwhile, the types of samples which can be processed in the same batch are not particularly required, and the samples are fixed in different grids to avoid floating and mixing only by arranging the grids at the bottom of the sample bearing module; the method is particularly suitable for flux treatment of samples containing soluble parts and batch treatment of serial formula samples, such as treatment of porous materials prepared by physical pore-forming methods such as urea and the like, and gel content test of batch samples. In addition, the device is also convenient for recycling the soluble components and the solvent.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Description of the drawings:
FIG. 1 is a schematic diagram of the overall structure of a soluble fraction flux separation device of the present invention;
FIG. 2 is a schematic view of the overall structure of the soluble fraction flux separation device of the present invention from another perspective;
FIG. 3 is a schematic top view of a soluble fraction flux separation device of the present invention (without condensing diversion module);
FIG. 4 is a schematic view of the structure of a sample carrying module of the soluble fraction flux separation device of the present invention;
FIG. 5 is a schematic diagram of the structure of a sample carrier module of the soluble fraction flux separation device of the present invention from another view;
FIG. 6 is a schematic view of the condensate diversion module of the soluble fraction flux separation device of the present invention;
FIG. 7 is a schematic cross-sectional view of a soluble fraction flux separation apparatus of the present invention;
Fig. 8 is a schematic view of the structure of the latch and hook of the soluble fraction flux separating device of the present invention.
The specific embodiment is as follows:
The present invention is described in further detail below with reference to the drawings to enable those skilled in the art to practice the invention by referring to the description.
It will be understood that terms, such as "having," "including," and "comprising," as used herein, do not preclude the presence or addition of one or more other elements or groups thereof.
Figures 1 to 8 show a soluble fraction flux separation device of the invention comprising:
a solvent-borne module, which is a functional unit for bearing a solvent in a solvent-out sample while continuously controllably heating the solvent, the solvent-borne module comprising:
a solvent tank 11, the bottom side of which is provided with a waste liquid discharge pipe 13 with a manual valve 12 for discharging waste liquid after the test;
a vibration pump 14 provided at the center of the inner bottom of the solvent tank 11; the vibration pump is used for providing continuous vibration, so that the sample cell is fully soaked;
A heater 15 provided at an inner bottom edge of the solvent tank 11; the heater is used for continuously heating the solvent to evaporate the solvent, and simultaneously increasing the dissolution degree of the soluble components in the solvent as much as possible;
A controller 16 provided outside the solvent tank 11 and connected to the heater 15; the controller 16 is used for controlling the heater to continuously heat and can monitor the actual temperature;
at least four supporting springs 17 which are provided at the inner bottom of the solvent tank 11 and uniformly arranged around the vibration pump 14; the support spring is used for restraining the oscillation support column so as to keep the sample cell in dynamic balance when oscillation needs to be provided;
The sample bearing module is arranged in the solvent tank 11 and is a functional unit for bearing samples, adjusting the states of the samples or marking and arranging different types of samples; the sample carrier module comprises:
A sample cell 21, the inner side of which is provided with an automatic liquid drain 23;
At least four oscillation support posts 24 uniformly arranged at the bottom of the sample cell 21, and the at least four oscillation support posts 24 are connected with the at least four support springs 17 of the solvent tank 11 in a matching manner; the bottom of the sample cell 21 is in contact with the top of the vibration pump 14;
The condensation diversion module is connected above the solvent bearing module 1; the condensation flow guiding module is a functional unit for condensing the solvent vapor and guiding the solvent vapor into the sample bearing module; the condensation diversion module comprises:
a sealing cover 31, the inner periphery of which is provided with a diversion skirt 32; the sealing cover 31 is buckled and connected to the solvent tank 11; the flow guiding skirt is used for guiding the condensed solvent into the sample bearing module;
an annular condenser 33 provided at the top center of the sealing cover 31; the middle part of the annular condenser 33 is provided with a window 34; the annular condenser is used for accelerating the cooling efficiency of the solvent vapor; the window is used for observing the internal state of the sample bearing module in real time;
a safety valve 35 provided at the top of the sealing cap 31; the safety valve is used for safety pressure relief when the vapor pressure is too high;
In the technical scheme, a sample bearing module is put into a solvent bearing module, so that at least four oscillating struts are sleeved in at least four supporting springs and are regulated to be stable; placing the tailored sample to be treated on the bottom of the inner side of a sample cell of the sample carrying module; injecting a certain volume of solvent into the sample cell of the sample carrying module, and enabling the solvent to pass through the sample to ensure that the sample is completely soaked in the solvent; injecting a certain volume of solvent into the solvent tank of the solvent bearing module, and ensuring that the liquid level of the solvent does not exceed the liquid level of the sample tank of the sample bearing module; the sealing cover of the condensation diversion module is arranged at the upper part of the solvent tank of the solvent bearing module and is buckled and connected; the controller is opened, the temperature is set, the heater is controlled to continuously heat the solvent in the solvent tank of the solvent bearing module to evaporate the solvent, the evaporated solvent is cooled into the sample tank through the condensation flow guide module, and when the liquid level in the sample tank exceeds the top of the automatic liquid draining device, the automatic liquid draining device drains the solvent in the sample tank into the solvent tank, and the solvent is circulated for multiple times, so that multiple elution of sheets in the sample tank is realized; simultaneously starting a vibration pump to vibrate the sample tank, so that the liquid in the sample tank of the sample bearing module eliminates the concentration gradient, and is favorable for dissolving soluble components; after the sample is sufficiently dissolved out, the controller is closed, after the temperature of the device is reduced to room temperature, the safety valve is slightly pulled out, so that the residual internal pressure is unloaded, the sealing cover which is buckled and connected is opened, and the sample is taken out.
The device has simple structural design and is convenient for practical control, and the test method saves time and labor, avoids frequent replacement of the solvent, and greatly reduces the use amount of the solvent; the shape of the sample is not particularly required, and the sample with smaller density only needs to be pretreated and fixed (such as wrapping dialysis paper and a metal net) so as to be fully soaked, thereby improving the elution efficiency; meanwhile, the types of samples which can be processed in the same batch are not particularly required, and the samples are fixed in different grids to avoid floating and mixing only by arranging the grids at the bottom of the sample bearing module; the method is particularly suitable for flux treatment of samples containing soluble parts and batch treatment of serial formula samples, such as treatment of porous materials prepared by physical pore-forming methods such as urea and the like, and gel content test of batch samples. In addition, the device is also convenient for recycling the soluble components and the solvent.
In the above technical solution, casters 18 are provided at four corners of the outer bottom of the solvent tank 11; for supporting the solvent tank and facilitating transfer of the entire device; sample cell handles 27 are provided on both sides of the outside of the sample cell.
In the above technical scheme, the upper edge of the solvent tank is provided with a groove, and a sealing ring 19 is arranged in the groove, which is used for strengthening the tightness between the solvent bearing module and the condensation diversion module in the test stage.
In the above technical scheme, the heater is an annular heating pipe.
In the technical scheme, the sample cell is a box with an open upper part; the automatic liquid drain device 23 is a U-shaped pipe which is downwards fixed on the inner side of the sample cell through a fixed block 25, one side pipe orifice 231 of the U-shaped pipe extends out of the bottom of the sample cell and is communicated with the solvent tank 11, and the other side pipe orifice 232 extends into a circular groove 26 at the bottom of the sample cell; and the pipe wall of the pipe orifice 231 at one side extending out of the bottom of the sample tank is sealed with the sample tank by the sealing sleeve 28, in this way, when the liquid level in the sample tank exceeds the top of the U-shaped pipe, the siphon principle of the U-shaped pipe is utilized to realize automatic liquid discharge, and the solvent in the sample tank is discharged to the solvent tank.
In the above technical scheme, the at least four oscillation support posts and the at least four support springs of the solvent tank are connected in a matching way: the inner diameter of each oscillating strut is slightly larger than the outer diameter of the supporting spring, and the oscillating struts are sleeved on the springs to realize matched connection.
In the technical scheme, the sealing cover is buckled and connected on the solvent tank in the following manner: the edge of sealed lid 32 is provided with epi portion I37, evenly is provided with a plurality of couples 41 on epi portion I37, the edge of solvent tank 11 is provided with epi portion II 110, is provided with a plurality of catches 42 corresponding with a plurality of couples on epi portion II, realizes the lock connection of sealed lid and solvent tank through the assorted connection of a plurality of catches 42 and a plurality of couples 41.
In the above technical scheme, the guide skirt is a bending plate, and the bending angle of the bending plate is an obtuse angle; one surface of the bending plate is connected to the sealing cover, and the other surface of the bending plate is suspended; sealing cover handles 36 are arranged on two sides of the outer part of the sealing cover 31, and the sealing cover handles are convenient for assembling and disassembling the condensation diversion module.
In the above technical scheme, the inside of annular condenser has the accommodation cavity, and is provided with water inlet and the delivery port that holds the cavity intercommunication on annular condenser, lets in cold water through the water inlet to annular condenser's accommodation cavity to discharge through the delivery port.
Example 1:
a method for testing using the above-described soluble fraction flux separation device, comprising the steps of:
Step one, placing a sample bearing module into a solvent bearing module, sleeving at least four oscillating struts into at least four supporting springs, and adjusting to be stable;
step two, wrapping the cut sample to be treated with the weight of m a by using dialysis paper, then placing the wrapped sample into a metal mesh bag, and horizontally placing the wrapped sample at the bottom of the inner side of a sample pool of the sample bearing module;
Step three, injecting a certain volume of solvent into the sample cell of the sample bearing module, and enabling the solvent to pass through the sample to ensure that the sample is completely soaked in the solvent;
Step four, injecting a certain volume of solvent into a solvent tank of the solvent bearing module, and ensuring that the liquid level height of the solvent does not exceed the liquid level height in a sample tank of the sample bearing module;
Step five, placing a sealing cover of the condensation diversion module on the upper part of a solvent tank of the solvent bearing module, and buckling and connecting the sealing cover;
Step six, opening a controller, setting the temperature, controlling a heater to continuously heat the solvent in the solvent tank of the solvent bearing module to volatilize the solvent, starting a vibration pump to vibrate the sample tank, and enabling the liquid in the sample tank of the sample bearing module to eliminate the concentration gradient so as to be beneficial to dissolving soluble components;
Step seven, after the sample is sufficiently dissolved out and soluble components in the sample are isolated, closing a controller, after the temperature of the device is reduced to room temperature, slightly pulling a safety valve, unloading residual internal pressure, opening a sealing cover in buckled connection, taking out the sample, drying and weighing to obtain m b;
And step eight, when the porous material prepared by the physical pore-forming method is processed, according to the total mass of the physical pore-forming agent added in the sample preparation stage, whether the pore-forming agent is completely dissolved and removed can be judged by calculating the difference between m a and m b.
Example 2:
a method for testing using the above-described soluble fraction flux separation device, comprising the steps of:
Step one, placing a sample bearing module into a solvent bearing module, sleeving at least four oscillating struts into at least four supporting springs, and adjusting to be stable;
step two, wrapping the cut sample to be treated with the weight of m a by using dialysis paper, then placing the wrapped sample into a metal mesh bag, and horizontally placing the wrapped sample at the bottom of the inner side of a sample pool of the sample bearing module;
Step three, injecting a certain volume of solvent into the sample cell of the sample bearing module, and enabling the solvent to pass through the sample to ensure that the sample is completely soaked in the solvent;
Step four, injecting a certain volume of solvent into a solvent tank of the solvent bearing module, and ensuring that the liquid level height of the solvent does not exceed the liquid level height in a sample tank of the sample bearing module;
Step five, placing a sealing cover of the condensation diversion module on the upper part of a solvent tank of the solvent bearing module, and buckling and connecting the sealing cover;
Step six, opening a controller, setting the temperature, controlling a heater to continuously heat the solvent in the solvent tank of the solvent bearing module to volatilize the solvent, starting a vibration pump to vibrate the sample tank, and enabling the liquid in the sample tank of the sample bearing module to eliminate the concentration gradient so as to be beneficial to dissolving soluble components;
Step seven, after the sample is sufficiently dissolved out and soluble components in the sample are isolated, closing a controller, after the temperature of the device is reduced to room temperature, slightly pulling a safety valve, unloading residual internal pressure, opening a sealing cover in buckled connection, taking out the sample, drying and weighing to obtain m b;
and step eight, calculating the (m b×100)/ma) of the corresponding sample, and obtaining gel content values gel% of the sample respectively.
Example 3:
a method for testing using the above-described soluble fraction flux separation device, comprising the steps of:
Step one, placing a sample bearing module into a solvent bearing module, sleeving at least four oscillating struts into at least four supporting springs, and adjusting to be stable;
step two, pretreating a sample to be treated, which is tailored with the weight of m a (when the density of the sample is smaller, the sample can be wrapped by dialysis paper and then put into a metal mesh bag, and a plurality of samples (m a1、ma2 and …) which are respectively weighed are fixed in different grids which are arranged at the bottom of a sample bearing module and provided with grids with scale marks;
Step three, injecting a certain volume of solvent into the sample cell of the sample bearing module, and enabling the solvent to pass through the sample to ensure that the sample is completely soaked in the solvent;
step four, injecting a certain volume of solvent into a solvent tank of the solvent bearing module, and ensuring that the liquid level height of the solvent is not more than the limit of the liquid level height in a sample pool of the sample bearing module;
Step five, placing a sealing cover of the condensation diversion module on the upper part of a solvent tank of the solvent bearing module, and buckling and connecting the sealing cover;
Step six, opening a controller, setting the temperature, controlling a heater to continuously heat the solvent in the solvent tank of the solvent bearing module to volatilize the solvent, starting a vibration pump to vibrate the sample tank, and enabling the liquid in the sample tank of the sample bearing module to eliminate the concentration gradient so as to be beneficial to dissolving soluble components;
Step seven, after the sample is sufficiently dissolved out and soluble components in the sample are completely separated, closing a controller, after the temperature of the device is reduced to room temperature, slightly pulling a safety valve, unloading residual internal pressure, opening a sealing cover in buckled connection, taking out the sample, drying and weighing to obtain (m b1、mb2 and …);
And step eight, when the method is used for treating the porous material prepared by a physical pore-forming method such as urea, the total mass of the physical pore-forming agent is added according to the sample preparation stage, and whether the pore-forming agent is completely dissolved and removed can be judged by respectively calculating the difference between m a and m b.
Example 4:
a method for testing using the above-described soluble fraction flux separation device, comprising the steps of:
Step one, placing a sample bearing module into a solvent bearing module, sleeving at least four oscillating struts into at least four supporting springs, and adjusting to be stable;
step two, pretreating a sample to be treated, which is tailored with the weight of m a (when the density of the sample is smaller, the sample can be wrapped by dialysis paper and then put into a metal mesh bag, and a plurality of samples (m a1、ma2 and …) which are respectively weighed are fixed in different grids which are arranged at the bottom of a sample bearing module and provided with grids with scale marks;
Step three, injecting a certain volume of solvent into the sample cell of the sample bearing module, and enabling the solvent to pass through the sample to ensure that the sample is completely soaked in the solvent;
step four, injecting a certain volume of solvent into a solvent tank of the solvent bearing module, and ensuring that the liquid level height of the solvent is not more than the limit of the liquid level height in a sample pool of the sample bearing module;
Step five, placing a sealing cover of the condensation diversion module on the upper part of a solvent tank of the solvent bearing module, and buckling and connecting the sealing cover;
Step six, opening a controller, setting the temperature, controlling a heater to continuously heat the solvent in the solvent tank of the solvent bearing module to volatilize the solvent, starting a vibration pump to vibrate the sample tank, and enabling the liquid in the sample tank of the sample bearing module to eliminate the concentration gradient so as to be beneficial to dissolving soluble components;
Step seven, after the sample is sufficiently dissolved out and soluble components in the sample are completely separated, closing a controller, after the temperature of the device is reduced to room temperature, slightly pulling a safety valve, unloading residual internal pressure, opening a sealing cover in buckled connection, taking out the sample, drying and weighing to obtain (m b1、mb2 and …);
And step eight, when gel content testing of batch samples is carried out, respectively calculating the (m b×100)/ma) of the corresponding samples, and respectively obtaining gel content values gel% of the samples.
Although embodiments of the present invention have been disclosed above, it is not limited to the details and embodiments shown and described, it is well suited to various fields of use for which the invention would be readily apparent to those skilled in the art, and accordingly, the invention is not limited to the specific details and illustrations shown and described herein, without departing from the general concepts defined in the claims and their equivalents.
Claims (5)
1. A method for testing with a soluble fraction flux separation device comprising the steps of:
Step one, placing a sample bearing module into a solvent bearing module, sleeving at least four oscillating struts into at least four supporting springs, and adjusting to be stable;
Step two, pretreating a sample to be treated, which is cut and has the weight of m a, and horizontally placing the sample at the bottom of the inner side of a sample pool of the sample bearing module; the pretreatment method comprises the following steps: when the density of the sample is smaller, the sample can be wrapped by dialysis paper and then put into a metal mesh bag; when the types of the samples which can be processed in the same batch are more, a grid with scale marks can be arranged at the bottom of a sample cell of the sample carrying module, and then the samples are fixed in different grids;
Step three, injecting a certain volume of solvent into the sample cell of the sample bearing module, and enabling the solvent to pass through the sample to ensure that the sample is completely soaked in the solvent;
Step four, injecting a certain volume of solvent into a solvent tank of the solvent bearing module, and ensuring that the liquid level height of the solvent does not exceed the liquid level height in a sample cell of the sample bearing module;
Step five, placing a sealing cover of the condensation diversion module on the upper part of a solvent tank of the solvent bearing module, and buckling and connecting the sealing cover;
Step six, opening a controller, setting the temperature, controlling a heater to continuously heat the solvent in the solvent tank of the solvent bearing module to volatilize the solvent, starting a vibration pump to vibrate the sample tank, and enabling the liquid in the sample tank of the sample bearing module to eliminate the concentration gradient so as to be beneficial to dissolving soluble components;
Step seven, after the sample is sufficiently dissolved out and soluble components in the sample are isolated, closing a controller, after the temperature of the device is reduced to room temperature, slightly pulling a safety valve, unloading residual internal pressure, opening a sealing cover in buckled connection, taking out the sample, drying and weighing to obtain m b;
Step eight, when the porous material prepared by the physical pore-forming method is processed, according to the total mass of the physical pore-forming agent added in the sample preparation stage, whether the pore-forming agent is completely dissolved out and removed can be judged by calculating the difference between m a and m b; when gel content testing of batch samples is carried out, respectively calculating (m b×100）/ma of corresponding samples, namely respectively obtaining gel content values gel of the samples;
Wherein the soluble fraction flux separation device comprises:
a solvent-borne module, comprising:
a solvent tank, the bottom side of which is provided with a waste liquid discharge pipe with a manual valve;
a vibration pump provided at the center of the inner bottom of the solvent tank;
A heater provided at an inner bottom edge of the solvent tank;
A controller which is arranged outside the solvent tank and is connected with the heater;
at least four supporting springs which are arranged at the bottom of the inner side of the solvent tank and are uniformly arranged around the vibration pump;
a sample carrier module disposed within a solvent tank, the sample carrier module comprising:
the inner side of the sample cell is provided with an automatic liquid drain device;
The at least four oscillation support posts are uniformly arranged at the bottom of the sample tank and are in matched connection with at least four supporting springs of the solvent tank; the bottom of the sample pool is contacted with the top of the vibration pump;
the condensation diversion module is connected above the solvent bearing module; the condensation diversion module comprises:
The periphery of the sealing cover is provided with a flow guiding skirt; the sealing cover is buckled and connected to the solvent tank;
an annular condenser provided at the center of the top of the sealing cover; a window is arranged in the middle of the annular condenser;
A safety valve provided at the top of the sealing cover;
The heater is an annular heating pipe;
The sample cell is a box-shaped object with an open upper part; the automatic liquid draining device is a U-shaped pipe which is downwards fixed on the inner side of the sample tank through a fixed block, one pipe orifice of one side of the U-shaped pipe extends out of the bottom of the sample tank and is communicated with the solvent tank, and the pipe orifice of the other side extends into a circular groove at the bottom of the sample tank; the pipe wall of the pipe orifice at one side extending out of the bottom of the sample tank is sealed with the sample tank through a sealing sleeve;
the edge of the sealing cover is provided with an extension part I, a plurality of hooks are uniformly arranged on the extension part, the edge of the solvent tank is provided with an extension part II, a plurality of catches corresponding to the plurality of hooks are arranged on the extension part II, and the sealing cover is connected with the solvent tank in a buckling manner through the matched connection of the plurality of catches and the plurality of hooks;
The guide skirt is a bending plate, and the bending angle of the bending plate is an obtuse angle; one surface of the bending plate is connected to the sealing cover, and the other surface of the bending plate is suspended; sealing cover handles are arranged on two sides of the outer portion of the sealing cover.
2. The method for performing the test using the soluble fraction flux separation apparatus according to claim 1, wherein casters are provided at four corners of the outer bottom of the solvent tank; sample cell handles are arranged on two sides of the outer part of the sample cell.
3. The method for testing by using a soluble fraction flux separation device according to claim 1, wherein a groove is arranged at the upper edge of the solvent tank, and a sealing ring is arranged in the groove.
4. The method of testing with a soluble fraction flux separation apparatus of claim 1, wherein the at least four oscillation supports are matingly connected to at least four support springs of a solvent tank by: the inner diameter of each oscillating strut is slightly larger than the outer diameter of the supporting spring, and the oscillating struts are sleeved on the springs to realize matched connection.
5. The method of testing with a soluble fraction flux separation apparatus of claim 1, wherein the annular condenser has a receiving cavity therein and a water inlet and a water outlet are provided on the annular condenser in communication with the receiving cavity.
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| GB1434617A (en) * | 1972-05-25 | 1976-05-05 | Comitato Nazionale Per Lenergi | Distillation apparatus for trace analysis |
| US5347844A (en) * | 1992-01-14 | 1994-09-20 | Fisons Instruments, S.P.A. | Process and device for vaporization injections in equipments for gas chromatographic analysis |
| US8596340B1 (en) * | 2010-10-13 | 2013-12-03 | Horn-Barber Technologies, LLC | Apparatus for heating liquid samples for analysis |
| CN104181028A (en) * | 2014-07-09 | 2014-12-03 | 复旦大学 | Device capable of achieving automatic high-flux volatilization of small-volume solvent |
| CN211014219U (en) * | 2019-11-21 | 2020-07-14 | 湖北航天化学技术研究所 | Device suitable for slightly soluble component solubility on-line measuring |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1434617A (en) * | 1972-05-25 | 1976-05-05 | Comitato Nazionale Per Lenergi | Distillation apparatus for trace analysis |
| US5347844A (en) * | 1992-01-14 | 1994-09-20 | Fisons Instruments, S.P.A. | Process and device for vaporization injections in equipments for gas chromatographic analysis |
| US8596340B1 (en) * | 2010-10-13 | 2013-12-03 | Horn-Barber Technologies, LLC | Apparatus for heating liquid samples for analysis |
| CN104181028A (en) * | 2014-07-09 | 2014-12-03 | 复旦大学 | Device capable of achieving automatic high-flux volatilization of small-volume solvent |
| CN211014219U (en) * | 2019-11-21 | 2020-07-14 | 湖北航天化学技术研究所 | Device suitable for slightly soluble component solubility on-line measuring |
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