CN112557248A - Soluble component flux segregation device and testing method - Google Patents
Soluble component flux segregation device and testing method Download PDFInfo
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- CN112557248A CN112557248A CN202011434553.XA CN202011434553A CN112557248A CN 112557248 A CN112557248 A CN 112557248A CN 202011434553 A CN202011434553 A CN 202011434553A CN 112557248 A CN112557248 A CN 112557248A
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- 230000004907 flux Effects 0.000 title claims abstract description 33
- 238000005204 segregation Methods 0.000 title claims abstract description 27
- 238000012360 testing method Methods 0.000 title claims description 19
- 239000002904 solvent Substances 0.000 claims abstract description 203
- 239000007788 liquid Substances 0.000 claims abstract description 40
- 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 20
- 238000007599 discharging Methods 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 238000010998 test method Methods 0.000 claims abstract description 3
- 238000007789 sealing Methods 0.000 claims description 49
- 238000005452 bending Methods 0.000 claims description 12
- 239000003795 chemical substances by application Substances 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 230000010355 oscillation Effects 0.000 claims description 10
- 238000002360 preparation method Methods 0.000 claims description 9
- 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
- 239000011148 porous material Substances 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 239000002699 waste material Substances 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 238000002955 isolation Methods 0.000 claims description 4
- 238000012545 processing Methods 0.000 claims description 3
- 238000002791 soaking Methods 0.000 abstract description 5
- 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
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical group [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000010828 elution Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000006261 foam material Substances 0.000 description 3
- 238000001816 cooling Methods 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000000502 dialysis Methods 0.000 description 2
- 238000011978 dissolution method 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
- 239000011780 sodium chloride Substances 0.000 description 2
- 229920002943 EPDM rubber Polymers 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 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
- 238000012827 research and development Methods 0.000 description 1
- 230000000452 restraining effect Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- 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 component flux segregation device and a test method. The method comprises the steps of firstly soaking 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 guide module, automatically discharging all the solvent in the sample bearing module into the solvent bearing module when the total liquid level in the sample bearing module reaches a specific height, simultaneously carrying out segregation of soluble components in the sample into the solvent bearing module, continuously volatilizing, condensing and guiding the solvent in the solvent bearing module, continuously introducing a pure solvent into the sample bearing module, continuously carrying the soluble components in the sample into the solvent bearing module through continuous soaking and automatic liquid discharge until all the soluble components are segregated, and enabling the sample in the sample bearing module to not contain the soluble components.
Description
Technical Field
The invention belongs to the technical field of material preparation technology and performance test, and particularly relates to a soluble component flux segregation device and a soluble component flux segregation test method.
Background
In the preparation process of the rubber and plastic foam material, a pore-forming technology by a dissolution method of urea, sodium chloride and the like becomes an important pore-forming mode due to higher environmental protection degree. However, in the stage of removing pore-forming agents such as urea, sodium chloride and the like, a cross-linked sample is required to be soaked in pure water, heated, stirred or vibrated for a certain time (Liupeng wave, Liudalong, Xuweng. an open-cell type silicon rubber foam material, a preparation method and application thereof. CN 1884378A [ P ].2006-12-27. Song Tao, Fu Yi, Anyou and the like. an ethylene propylene diene monomer based microporous foam material and a preparation method thereof. CN 105348655A [ P ].2016-02-24. Song Tao, Yangjiang nan, Anyou and the like. an organic reinforced type silicon rubber foam material and a preparation method thereof CN 107815123A [ P ]. 2018-03-20.). In the actual operation process, in order to ensure that the pore-forming agent can be removed as much as possible, water needs to be changed for many times until all the pore-forming agent in the sample is eluted and separated. Therefore, the operation burden of experimenters is increased, and simultaneously, a large amount of waste liquid is generated. This is particularly significant when the sample size is large. This is very disadvantageous for serial development and mass production. Therefore, research and development of a device and a testing method which can overcome the defects and realize quantitative automatic segregation have positive significance, and the device and the testing method have important significance for promoting popularization and application of a dissolution method pore-forming technology.
Disclosure of Invention
An object of the present invention is to solve at least the above problems and/or disadvantages and to provide at least the advantages described hereinafter.
To achieve these objects and other advantages in accordance with the purpose of the invention, there is provided a soluble fraction flux segregation apparatus comprising:
a solvent bearing module, comprising:
the side surface of the bottom of the solvent tank is provided with a waste liquid discharge pipe with a manual valve;
a vibration pump arranged at the center of the inner bottom of the solvent tank;
a heater disposed at an inner bottom edge of the solvent tank;
a controller which is arranged outside the solvent tank and is connected with the heater;
the at least four supporting springs are arranged at the bottom of the inner side of the solvent tank and are uniformly arranged around the vibration pump;
a sample support module disposed within the solvent tank, the sample support module comprising:
the inner side of the sample pool is provided with an automatic liquid discharging device;
the at least four oscillating supports are uniformly arranged at the bottom of the sample cell and are in matched connection with the at least four supporting springs of the solvent tank; the bottom of the sample cell is in contact with the top of the vibration pump;
the condensation diversion module is connected above the solvent bearing module; the condensation diversion module comprises:
the inner periphery of the sealing cover is provided with a flow guide skirt; the sealing cover is buckled and connected on the solvent tank;
an annular condenser disposed at the center of the top of the sealing cover; a window is arranged in the middle of the annular condenser;
and the safety valve is arranged at the top of the sealing cover.
Preferably, four corners of the bottom of the outer side of the solvent tank are provided with casters; and sample cell handles are arranged on two sides of the outside of the sample cell.
Preferably, a groove is arranged at the upper edge of the solvent tank, and a sealing ring is arranged in the groove.
Preferably, the heater is an annular heating tube.
Preferably, the sample cell is a box with an open upper part; the automatic liquid discharging device is a U-shaped pipe and is downwards fixed on the inner side of the sample pool through a fixing block, a pipe orifice on one side of the U-shaped pipe extends out of the bottom of the sample pool and is communicated with the solvent groove, and a pipe orifice on the other side of the U-shaped pipe extends into a circular groove in the bottom of the sample pool; and the pipe wall of the pipe orifice at one side extending out of the bottom of the sample pool is hermetically arranged with the sample pool through a sealing sleeve.
Preferably, the at least four oscillation struts are connected with the at least four supporting springs of the solvent tank in a matching manner: the inner diameter of each oscillation strut is slightly larger than the outer diameter of the supporting spring, and the oscillation struts are sleeved on the springs to realize matched connection.
Preferably, the edge of sealed lid is provided with extension portion I, evenly is provided with a plurality of couples in the extension portion, the edge in solvent groove is provided with extension portion II, is provided with a plurality of hasps corresponding with a plurality of couples on extension portion II, and the lock that realizes sealed lid and solvent groove through the phase-match connection of a plurality of hasps and a plurality of couples is connected.
Preferably, the flow 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 arranged in a suspended manner; and sealing cover handles are arranged on two sides of the outside of the sealing cover.
Preferably, the annular condenser is internally provided with a containing cavity, and the annular condenser is provided with a water inlet and a water outlet which are communicated with the containing cavity.
The invention also provides a method for testing by adopting the soluble component flux segregation device, which comprises the following steps:
step one, putting a sample bearing module into a solvent bearing module, so that at least four oscillating support columns are sleeved in at least four supporting springs and are adjusted to be stable;
step two, the weight of the cut is maAfter the sample to be processed is pretreated, the sample to be processed is flatly placed at the bottom of the inner side of the sample pool of the sample bearing module; wherein, the pretreatment mode is as follows: when the density of the sample is small, the sample can be wrapped by dialyzing paper and then put into a metal mesh bag; when the types of samples which can be processed in the same batch are more, the grid with the scale marks can be arranged at the bottom of the sample pool of the sample bearing module, and then the samples are fixed in different lattices；
Injecting a certain volume of solvent into the sample pool of the sample bearing module, and enabling the solvent to submerge 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 inside a sample pool of the sample bearing module;
placing the sealing cover of the condensation diversion module on the upper part of the solvent tank of the solvent bearing module, and buckling and connecting the sealing cover and the solvent tank;
opening the controller, setting the temperature, controlling the heater to continuously heat the solvent in the solvent tank of the solvent bearing module to volatilize the solvent, starting the vibration pump to vibrate the sample pool, and eliminating the concentration gradient of the liquid in the sample pool of the sample bearing module so as to be beneficial to dissolving soluble components;
seventhly, after the sample is fully dissolved out and the soluble components in the sample are separated, closing the controller, slightly pulling out the safety valve after the temperature of the device is reduced to the room temperature, unloading the residual internal pressure, opening the sealing cover connected in a buckling way, taking out the sample, drying and weighing to obtain mb；
Step eight, when the method is used for processing the porous material prepared by the physical pore-forming method, the m is calculated according to the total mass of the added physical pore-forming agent in the sample preparation stageaAnd mbThe difference between the two can judge whether the pore-forming agent is completely dissolved out and removed; when the gel content test of the batch samples is performed, (m) of the corresponding samples is calculated, respectivelyb×100)/maAnd obtaining the gel content value gel% of each sample respectively.
The invention provides a soluble component flux segregation device and a testing method, the device comprises a sample bearing module, a solvent bearing module and a condensation diversion module, wherein the sample bearing module is a functional unit for bearing a sample, adjusting the state of the sample or marking and arranging different types of samples, the solvent bearing module is a functional unit for bearing a soluble component solvent in a dissolved sample and continuously and controllably heating the solvent, and the condensation diversion module is a functional unit for condensing solvent steam and guiding the solvent steam into the sample bearing module. The method comprises the steps of soaking 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 diversion module, automatically discharging all the solvent in the sample bearing module into the solvent bearing module when the total liquid level in the sample bearing module reaches a specific height, simultaneously bringing dissolved soluble components into the solvent bearing module, continuously volatilizing, condensing and diverting the solvent in the solvent bearing module, continuously introducing pure solvent into the sample bearing module, continuously bringing the soluble components contained in the sample into the solvent bearing module through continuous soaking and automatic liquid discharge until the soluble components are completely dissolved out, and enabling the sample in the sample bearing module not to contain soluble components.
The invention at least comprises the following beneficial effects: the device provided by the invention is simple in structural design and convenient to actually operate and control, and the testing method is time-saving and labor-saving, so that not only is the frequent replacement of the solvent avoided, but also the usage amount of the solvent is greatly reduced; the shape of the sample is not specially required, and the sample with low density is only required to be pretreated and fixed (such as wrapping dialysis paper and a metal net) to be fully soaked so as to improve the elution efficiency; meanwhile, the types of samples which can be processed in the same batch have no special requirements, and only the grid is arranged at the bottom of the sample bearing module, and then the samples are fixed in different lattices to avoid floating and mixing; the method is particularly suitable for flux treatment of samples containing soluble components and batch treatment of samples of a serialized formula, 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 convenient for recycling soluble components and solvents.
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 view of the overall structure of a soluble fraction flux segregation apparatus according to the present invention;
FIG. 2 is a schematic view of the overall structure of another view of the soluble fraction flux segregating unit of the present invention;
FIG. 3 is a schematic diagram of the top view structure of the soluble fraction flux segregation device of the present invention (without the condensation diversion module);
FIG. 4 is a schematic diagram of the structure of a sample support module of the soluble fraction flux isolation apparatus of the present invention;
FIG. 5 is a schematic diagram of another perspective structure of a sample support module of the soluble fraction flux isolation apparatus of the present invention;
FIG. 6 is a schematic structural view of a condensation flow guide module of the soluble component flux segregation apparatus of the present invention;
FIG. 7 is a schematic sectional view showing a flux segregating means for soluble components according to the present invention;
FIG. 8 is a schematic view of the structure of the latch and hook of the soluble fraction flux segregation device of the present invention.
The specific implementation mode is as follows:
the present invention is further described in detail below with reference to the attached drawings so that those skilled in the art can implement the invention by referring to the description text.
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.
FIGS. 1 to 8 show a soluble fraction flux segregation apparatus of the present invention, comprising:
the solvent bears the module, it is the functional unit that is used for bearing the soluble fraction solvent in the elution sample, and is continuously controllable heating to this solvent simultaneously, and the solvent bears the module and includes:
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 as to realize full soaking in the sample pool;
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 dissolving 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 disposed at the bottom of the inner side of the solvent tank 11 and uniformly arranged around the vibration pump 14; the supporting spring is used for restraining the oscillating support to keep the sample pool in dynamic balance when oscillation needs to be provided;
the sample bearing module is arranged in the solvent tank 11, and the sample bearing module is a functional unit for bearing samples, adjusting the state of the samples or marking and arranging different types of samples; the sample support module comprises:
a sample cell 21 provided with an automatic drain 23 inside;
at least four oscillating supports 24 uniformly arranged at the bottom of the sample cell 21, wherein the at least four oscillating supports 24 are matched and connected with the at least four supporting springs 17 of the solvent tank 11; 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 diversion module is a functional unit which condenses the solvent vapor and diverts 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 flow guiding skirt 32; the sealing cover 31 is buckled and connected on the solvent tank 11; the diversion skirt is used for guiding the condensed solvent into the sample bearing module;
an annular condenser 33 provided at the center of the top of the sealing cover 31; a window 34 is arranged in the middle of the annular condenser 33; 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 safely releasing pressure when the steam pressure is overlarge;
in the technical scheme, the sample bearing module is placed in the solvent bearing module, so that at least four oscillating support columns are sleeved in at least four supporting springs and are adjusted to be stable; horizontally placing the cut sample to be processed at the bottom of the inner side of the sample cell of the sample bearing module; injecting a certain volume of solvent into the sample cell of the sample bearing module, and enabling the solvent to submerge the sample to ensure that the sample is completely soaked in the solvent; 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 the sample pool of the sample bearing module; placing the sealing cover of the condensation diversion module on the upper part of the solvent tank of the solvent bearing module, and buckling and connecting the sealing cover and the solvent tank; opening the controller, setting the temperature, controlling the heater to continuously heat the solvent in the solvent tank of the solvent bearing module to evaporate the solvent, cooling the evaporated solvent into the sample tank through the condensation diversion module, discharging the solvent in the sample tank into the solvent tank through the automatic liquid drainage device when the liquid level in the sample tank exceeds the top of the automatic liquid drainage device, and circulating for many times to realize multiple dissolving-out of the sheets in the sample tank; meanwhile, starting a vibration pump to vibrate the sample cell, so that the concentration gradient of the liquid in the sample cell of the sample bearing module is eliminated, and the soluble components are dissolved favorably; and after the sample is fully dissolved out, closing the controller, slightly pulling out the safety valve after the temperature of the device is reduced to the room temperature, unloading the residual internal pressure, opening the sealing cover in buckling connection, and taking out the sample.
The device provided by the invention is simple in structural design and convenient to actually operate and control, and the testing method is time-saving and labor-saving, so that not only is the frequent replacement of the solvent avoided, but also the usage amount of the solvent is greatly reduced; the shape of the sample is not specially required, and the sample with low density is only required to be pretreated and fixed (such as wrapping dialysis paper and a metal net) to be fully soaked so as to improve the elution efficiency; meanwhile, the types of samples which can be processed in the same batch have no special requirements, and only the grid is arranged at the bottom of the sample bearing module, and then the samples are fixed in different lattices to avoid floating and mixing; the method is particularly suitable for flux treatment of samples containing soluble components and batch treatment of samples of a serialized formula, 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 convenient for recycling soluble components and solvents.
In the above technical solution, four corners of the bottom of the solvent tank 11 are provided with casters 18; for supporting the solvent tank and facilitating the transfer of the entire apparatus; and sample cell handles 27 are arranged on two sides of the outside of the sample cell.
In the above technical scheme, a groove is formed in the upper edge of the solvent tank, and a sealing ring 19 is arranged in the groove, so that the sealing performance between the solvent bearing module and the condensation diversion module in the test stage is enhanced.
In the above technical solution, the heater is an annular heating pipe.
In the technical scheme, the sample cell is a box-shaped object with an open upper part; the automatic liquid discharging device 23 is a U-shaped tube and is fixed on the inner side of the sample pool through a fixing block 25, a tube orifice 231 on one side of the U-shaped tube extends out of the bottom of the sample pool to be communicated with the solvent groove 11, and a tube orifice 232 on the other side of the U-shaped tube extends into a circular groove 26 on the bottom of the sample pool; and the pipe wall of the pipe orifice 231 at one side extending out of the bottom of the sample pool is hermetically arranged with the sample pool through the sealing sleeve 28, and by adopting the mode, when the liquid level in the sample pool exceeds the top of the U-shaped pipe, the siphon principle of the U-shaped pipe is utilized to realize automatic liquid drainage and drain the solvent in the sample pool to the solvent tank.
In the above technical solution, the at least four oscillation pillars are connected to the at least four support springs of the solvent tank in a matching manner: the inner diameter of each oscillation support post is slightly larger than the outer diameter of the supporting spring, the oscillation support posts are sleeved on the springs to realize matching connection, and the mode is adopted to ensure that the sample cell keeps dynamic balance during the test.
In the above technical scheme, the manner that the sealing cover is buckled and connected on the solvent tank is as follows: the edge of sealed lid 32 is provided with extension I37, evenly is provided with a plurality of couples 41 on the extension I37, the edge of solvent groove 11 is provided with extension II 110, is provided with on the extension II with a plurality of hasps 42 that a plurality of couples are corresponding, and the lock that realizes sealed lid and solvent groove through a plurality of hasps 42 and a plurality of phase-to-phase connection of couple 41 is connected.
In the technical scheme, the flow 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 arranged in a suspended manner; and sealing cover handles 36 are arranged on two sides of the outside of the sealing cover 31 and are convenient for assembling and disassembling the condensation diversion module.
In the technical scheme, the annular condenser is internally provided with the containing cavity, the annular condenser is provided with the water inlet and the water outlet which are communicated with the containing cavity, and cold water is introduced into the containing cavity of the annular condenser through the water inlet and is discharged through the water outlet.
Example 1:
a method for testing by adopting the soluble component flux segregation device comprises the following steps:
step one, putting a sample bearing module into a solvent bearing module, so that at least four oscillating support columns are sleeved in at least four supporting springs and are adjusted to be stable;
step two, the weight of the cut is maThe sample to be processed is wrapped by dialyzing paper and then put into a metal mesh bag, and is flatly placed at the bottom of the inner side of a sample pool of the sample bearing module;
injecting a certain volume of solvent into the sample pool of the sample bearing module, and ensuring that the solvent is submerged in 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 inside a sample pool of the sample bearing module;
placing the sealing cover of the condensation diversion module on the upper part of the solvent tank of the solvent bearing module, and buckling and connecting the sealing cover and the solvent tank;
opening the controller, setting the temperature, controlling the heater to continuously heat the solvent in the solvent tank of the solvent bearing module to volatilize the solvent, starting the vibration pump to vibrate the sample pool, and eliminating the concentration gradient of the liquid in the sample pool of the sample bearing module so as to be beneficial to dissolving soluble components;
seventhly, after the sample is fully dissolved out and the soluble components in the sample are separated, closing the controller, and slightly pulling the device after the temperature of the device is reduced to the room temperatureA safety valve for opening the sealing cover after the residual internal pressure is unloaded, taking out the sample, drying and weighing to obtain mb；
Step eight, when the method is used for processing the porous material prepared by the physical pore-forming method, the m is calculated according to the total mass of the added physical pore-forming agent in the sample preparation stageaAnd mbThe difference between the two can judge whether the pore-forming agent is completely dissolved out and removed.
Example 2:
a method for testing by adopting the soluble component flux segregation device comprises the following steps:
step one, putting a sample bearing module into a solvent bearing module, so that at least four oscillating support columns are sleeved in at least four supporting springs and are adjusted to be stable;
step two, the weight of the cut is maThe sample to be processed is wrapped by dialyzing paper and then put into a metal mesh bag, and is flatly placed at the bottom of the inner side of a sample pool of the sample bearing module;
injecting a certain volume of solvent into the sample pool of the sample bearing module, and ensuring that the solvent is submerged in 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 inside a sample pool of the sample bearing module;
placing the sealing cover of the condensation diversion module on the upper part of the solvent tank of the solvent bearing module, and buckling and connecting the sealing cover and the solvent tank;
opening the controller, setting the temperature, controlling the heater to continuously heat the solvent in the solvent tank of the solvent bearing module to volatilize the solvent, starting the vibration pump to vibrate the sample pool, and eliminating the concentration gradient of the liquid in the sample pool of the sample bearing module so as to be beneficial to dissolving soluble components;
seventhly, after the sample is fully dissolved out and the soluble components in the sample are separated, closing the controller, slightly pulling the safety valve after the temperature of the device is reduced to the room temperature, unloading the residual internal pressure, and opening the buckled connectionSealing the cover, taking out the sample, drying and weighing to obtain mb；
Step eight, calculating (m) of corresponding samplesb×100)/maAnd obtaining the gel content value gel% of the samples respectively.
Example 3:
a method for testing by adopting the soluble component flux segregation device comprises the following steps:
step one, putting a sample bearing module into a solvent bearing module, so that at least four oscillating support columns are sleeved in at least four supporting springs and are adjusted to be stable;
step two, the weight of the cut is maThe sample to be treated is pretreated (when the density of the sample is low, the sample can be wrapped by dialyzing paper and put into a metal mesh bag, and a plurality of samples (m) are weighed respectivelya1、ma2…) are fixed in different lattices of a grid with scale marks, which is arranged at the bottom of the sample bearing module; the sample cell is horizontally placed at the bottom of the inner side of the sample cell of the sample bearing module;
injecting a certain volume of solvent into the sample pool of the sample bearing module, and ensuring that the solvent is submerged in 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 inside a sample pool of the sample bearing module;
placing the sealing cover of the condensation diversion module on the upper part of the solvent tank of the solvent bearing module, and buckling and connecting the sealing cover and the solvent tank;
opening the controller, setting the temperature, controlling the heater to continuously heat the solvent in the solvent tank of the solvent bearing module to volatilize the solvent, starting the vibration pump to vibrate the sample pool, and eliminating the concentration gradient of the liquid in the sample pool of the sample bearing module so as to be beneficial to dissolving soluble components;
seventhly, after the sample is fully dissolved out and the soluble components in the sample are separated, closing the controller, slightly pulling the safety valve after the temperature of the device is reduced to the room temperature, and enabling the residual internal pressureAfter unloading, the snap-fit closure is opened, the sample is removed, dried and weighed to give (m)b1、mb2、…)；
Step eight, when the method is used for treating the porous material prepared by physical pore-forming methods such as urea and the like, the m is respectively calculated according to the total mass of the added physical pore-forming agents in the sample preparation stageaAnd mbThe difference between the two can judge whether the pore-forming agent is completely dissolved out and removed.
Example 4:
a method for testing by adopting the soluble component flux segregation device comprises the following steps:
step one, putting a sample bearing module into a solvent bearing module, so that at least four oscillating support columns are sleeved in at least four supporting springs and are adjusted to be stable;
step two, the weight of the cut is maThe sample to be treated is pretreated (when the density of the sample is low, the sample can be wrapped by dialyzing paper and put into a metal mesh bag, and a plurality of samples (m) are weighed respectivelya1、ma2…) are fixed in different lattices of a grid with scale marks, which is arranged at the bottom of the sample bearing module; the sample cell is horizontally placed at the bottom of the inner side of the sample cell of the sample bearing module;
injecting a certain volume of solvent into the sample pool of the sample bearing module, and ensuring that the solvent is submerged in 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 inside a sample pool of the sample bearing module;
placing the sealing cover of the condensation diversion module on the upper part of the solvent tank of the solvent bearing module, and buckling and connecting the sealing cover and the solvent tank;
opening the controller, setting the temperature, controlling the heater to continuously heat the solvent in the solvent tank of the solvent bearing module to volatilize the solvent, starting the vibration pump to vibrate the sample pool, and eliminating the concentration gradient of the liquid in the sample pool of the sample bearing module so as to be beneficial to dissolving soluble components;
step seven, after the sample is fully dissolved out and the soluble components in the sample are separated, closing the controller, slightly pulling out the safety valve after the temperature of the device is reduced to the room temperature, unloading the residual internal pressure, opening the sealing cover connected in a buckling way, taking out the sample, drying and weighing to obtain (m)b1、mb2、…)；
Step eight, when the gel content of the batch samples is tested, respectively calculating the (m) of the corresponding samplesb×100)/maAnd obtaining the gel content value gel% of each sample respectively.
While embodiments of the invention have been described above, it is not limited to the applications set forth in the description and the embodiments, which are fully applicable in various fields of endeavor to which the invention pertains, and further modifications may readily be made by those skilled in the art, it being understood that the invention is not limited to the details shown and described herein without departing from the general concept defined by the appended claims and their equivalents.
Claims (10)
1. A soluble fraction flux segregation device, comprising:
a solvent bearing module, comprising:
the side surface of the bottom of the solvent tank is provided with a waste liquid discharge pipe with a manual valve;
a vibration pump arranged at the center of the inner bottom of the solvent tank;
a heater disposed at an inner bottom edge of the solvent tank;
a controller which is arranged outside the solvent tank and is connected with the heater;
the at least four supporting springs are arranged at the bottom of the inner side of the solvent tank and are uniformly arranged around the vibration pump;
a sample support module disposed within the solvent tank, the sample support module comprising:
the inner side of the sample pool is provided with an automatic liquid discharging device;
the at least four oscillating supports are uniformly arranged at the bottom of the sample cell and are in matched connection with the at least four supporting springs of the solvent tank; the bottom of the sample cell is in contact with the top of the vibration pump;
the condensation diversion module is connected above the solvent bearing module; the condensation diversion module comprises:
the inner periphery of the sealing cover is provided with a flow guide skirt; the sealing cover is buckled and connected on the solvent tank;
an annular condenser disposed at the center of the top of the sealing cover; a window is arranged in the middle of the annular condenser;
and the safety valve is arranged at the top of the sealing cover.
2. The soluble fraction flux segregation device according to claim 1, wherein casters are provided at four corners of the outside bottom of the solvent tank; and sample cell handles are arranged on two sides of the outside of the sample cell.
3. The soluble fraction flux segregation device according to claim 1, wherein a groove is provided at an upper edge of the solvent tank, and a seal ring is provided in the groove.
4. The soluble fraction flux segregation device of claim 1, wherein said heater is an annular heating tube.
5. The soluble fraction flux segregation device according to claim 1, wherein said sample cell is a box with an open upper part; the automatic liquid discharging device is a U-shaped pipe and is downwards fixed on the inner side of the sample pool through a fixing block, a pipe orifice on one side of the U-shaped pipe extends out of the bottom of the sample pool and is communicated with the solvent groove, and a pipe orifice on the other side of the U-shaped pipe extends into a circular groove in the bottom of the sample pool; and the pipe wall of the pipe orifice at one side extending out of the bottom of the sample pool is hermetically arranged with the sample pool through a sealing sleeve.
6. The fractional flux isolation apparatus of claim 1, wherein said at least four oscillation struts are matingly connected to at least four support springs of the solvent tank in a manner that: the inner diameter of each oscillation strut is slightly larger than the outer diameter of the supporting spring, and the oscillation struts are sleeved on the springs to realize matched connection.
7. The soluble flux segregation device according to claim 1, wherein 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 lock catches corresponding to the hooks are arranged on the extension part II, and the locking connection of the sealing cover and the solvent tank is realized through the matching connection of the lock catches and the hooks.
8. The soluble fraction flux segregation device of claim 1, wherein the deflector skirt is a bent plate and the bent angle of the bent 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 arranged in a suspended manner; and sealing cover handles are arranged on two sides of the outside of the sealing cover.
9. Soluble fraction flux segregation device according to claim 1, characterized in that the inside of the annular condenser has a receiving cavity and that a water inlet and a water outlet are provided on the annular condenser communicating with the receiving cavity.
10. A method of testing using the fractional flux isolation apparatus of any of claims 1 to 9, comprising the steps of:
step one, putting a sample bearing module into a solvent bearing module, so that at least four oscillating support columns are sleeved in at least four supporting springs and are adjusted to be stable;
step two, the weight of the cut is maAfter the sample to be processed is pretreated, the sample to be processed is flatly placed at the bottom of the inner side of the sample pool of the sample bearing module; wherein, the pretreatment mode is as follows: when the density of the sample is small, the sample can be wrapped by dialyzing paper and then put into a metal mesh bag; when the types of samples which can be processed in the same batch are more, the grid with the scale marks can be placedFixing the sample in different lattices at the bottom of the sample pool of the sample bearing module;
injecting a certain volume of solvent into the sample pool of the sample bearing module, and enabling the solvent to submerge 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 inside a sample pool of the sample bearing module;
placing the sealing cover of the condensation diversion module on the upper part of the solvent tank of the solvent bearing module, and buckling and connecting the sealing cover and the solvent tank;
opening the controller, setting the temperature, controlling the heater to continuously heat the solvent in the solvent tank of the solvent bearing module to volatilize the solvent, starting the vibration pump to vibrate the sample pool, and eliminating the concentration gradient of the liquid in the sample pool of the sample bearing module so as to be beneficial to dissolving soluble components;
seventhly, after the sample is fully dissolved out and the soluble components in the sample are separated, closing the controller, slightly pulling out the safety valve after the temperature of the device is reduced to the room temperature, unloading the residual internal pressure, opening the sealing cover connected in a buckling way, taking out the sample, drying and weighing to obtain mb；
Step eight, when the method is used for processing the porous material prepared by the physical pore-forming method, the m is calculated according to the total mass of the added physical pore-forming agent in the sample preparation stageaAnd mbThe difference between the two can judge whether the pore-forming agent is completely dissolved out and removed; when the gel content test of the batch samples is performed, (m) of the corresponding samples is calculated, respectivelyb×100)/maAnd obtaining the gel content value gel% of each sample respectively.
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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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2020
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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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