CN108169417B - Intelligent dynamic swelling degree testing device and testing method - Google Patents
Intelligent dynamic swelling degree testing device and testing method Download PDFInfo
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Abstract
The invention discloses an intelligent dynamic swelling degree testing device which comprises a vertically arranged sliding rod and a horizontal lifting tray connected with the sliding rod through a fixing knob, wherein a solution cup is arranged on the lifting tray, a sample cup is arranged above the solution cup, a liquid seepage hole is formed in the bottom of the sample cup, a displacement sensor is arranged above the sample cup, a sensor testing tray is connected to the lower portion of the displacement sensor, a sample cup fixer is arranged between the displacement sensor and the sensor testing tray, the displacement sensor is electrically connected with a digital display instrument, a digital display screen and a control button are arranged on the digital display instrument, and the displacement sensor is communicated with a computer. The invention also provides an intelligent dynamic swelling degree test method. The method is easy to operate, large-data-volume continuous testing is realized, and labor cost is reduced; the applicability of the sample to be detected is strong.
Description
Technical Field
The invention relates to a swelling degree testing device and method, in particular to an intelligent dynamic testing device and method for polymer swelling degree, and belongs to the technical field of polymer performance characterization.
Background
The crosslinked polymer has swelling property, and the swelling balance is substantially the thermodynamic balance between the crosslinked network and the solvent, and the dynamic balance can be changed along with the external factors such as solvent environment, temperature and the like. The measurement of the swelling degree of the crosslinked polymer is of great significance for the study of the crosslinked structure of the polymer, the interaction between the polymer and a solvent, the influence of temperature on the swelling property of the polymer, and the like.
The swelling degree test methods reported in the literature at present mainly comprise a weighing method and a volume measuring method, most of the swelling degree test methods adopt simple laboratory tests, and universal standard test methods and instruments are lacked. The weighing method is that the polymer with known mass is soaked in a solvent within a certain time, after the polymer reaches the swelling equilibrium, the excess solvent is quickly filtered and removed, and the swelling degree of the polymer is evaluated by calculating the weight gain. The method has complex process and low test precision, can not solve the problem that how to separate the swelling body from the solvent without influencing the swelling equilibrium state of the swelling body, and can not record the continuous dynamic change of the swelling degree along with the time in real time. The volume measurement method generally selects a graduated glass column with a certain pipe diameter to convert volume information into height information, is a simpler and more reasonable test method, but the continuous dynamic test of the swelling degree cannot be realized in the mode of reading scale values by visual observation at present, and has low accuracy and intelligence level. Therefore, the design of a novel swelling degree testing method and device has important practical value.
Disclosure of Invention
The invention overcomes the defects of the traditional swelling degree test technology, provides an intelligent dynamic test device and a test method for polymer swelling degree, and fills the blank of the current intelligent dynamic test method and instrument for swelling degree.
One of the objectives of the present invention is to provide an intelligent dynamic swelling degree testing device, which comprises:
the slide bar of perpendicular setting, the horizontal lift tray that links to each other through fixed knob with the slide bar, be provided with the solution cup on the lift tray, solution cup top is provided with the sample cup, the sample cup bottom is provided with the liquid infiltration hole, displacement sensor is installed to the sample cup top, the displacement sensor sub-unit connection has the sensor test dish, be provided with the sample cup fixer between displacement sensor and sensor test dish, displacement sensor is connected with the digital display appearance electricity, there are digital display screen and control button on the digital display appearance, displacement sensor still communicates with the computer.
The further scheme is as follows: in order to control the temperature during the swelling degree test, a temperature control water inlet and a temperature control water outlet are respectively arranged on the solution cup, and the temperature control water inlet is positioned below the temperature control water outlet.
The further scheme is as follows: in order to maintain the temperature, a temperature control jacket is also arranged outside the solution cup.
The further scheme is as follows: the sample cup is smaller than the solution cup and can be placed into the solution cup.
The further scheme is as follows: the size of the sensor test disc is the same as that of the cross section of the inner side of the sample cup.
The further scheme is as follows: the intelligent dynamic swelling degree testing device comprises two sets of devices which are positioned on two sides of the sliding rod and are the same.
The invention also provides an intelligent dynamic swelling degree test method, which mainly adopts the intelligent dynamic swelling degree test device and specifically comprises the following steps:
and hanging the solid sample and the sample cup on a sample cup holder together, enabling the sensor test disc to be in contact with the solid sample, adjusting the reading of the displacement sensor, and setting a zero point. And (4) filling the solution cup with the test solution, lifting the lifting tray to enable the test solution in the solution cup to flow into the sample cup, and immediately starting testing. The solid sample swells to generate upward displacement, so that the sensor test disc can sense the displacement distance, the displacement sensor generates displacement signals and transmits the displacement signals to the computer, the real-time change data of the displacement along with the time is recorded according to the time step set by the control button, and the computer draws a curve.
The further scheme is as follows:
the solid sample corresponds to the diameter of the sample cup.
The further scheme is as follows:
the solid sample is directly machined from a block sample or pressed from a powder sample by an oil press.
The further scheme is as follows:
the powder sample is pressed by an oil press, and the method comprises the following specific steps:
① placing a circular pad with hole on the bottom of the sample cup, and placing a piece of filter paper on the pad;
② weighing powder sample with balance, placing into a sample cup, and gently vibrating to make the end face of the sample flat;
③ placing the pressing rod in, rotating left and right slightly to contact with the end face of the sample;
④ placing on the oil press platform, pressurizing and maintaining constant pressure for enough time, opening the pressure relief valve to relieve pressure when the sample is pressed into sheet;
⑤ the press bar was removed, the height H of the sheet sample was measured, and a piece of filter paper was placed on top of the formed sheet sample.
⑥ hanging the pressed sample and the sample cup on a rack, pressing the test disc of the sensor on the sheet sample, and adjusting the zero point.
It should be noted that, in step ①, a circular pad with holes is used, the holes are provided for the solvent to penetrate into the sample cup from the holes, and the sample is soaked in the solvent to swell.
In step ⑤, the sheet sample is first swelled to become deformed due to the contact of the surface with the solvent, and a piece of filter paper is placed to press on the sample to ensure the flatness of the upper end surface of the sample and the accuracy of the measured displacement data.
In step ⑥, after pressing the sample, the sample cup, pad, filter paper, and sample are hung on the rack as a whole, so the device has two sets of sample cups, and the sample is directly hung for testing after pressing.
Compared with the prior art, the invention has the beneficial effects that: the intelligent dynamic swelling degree test method and the intelligent dynamic swelling degree test device overcome the defects of the traditional test method, realize paperless intelligent data acquisition by being connected with a computer, are simple and easy to operate, realize large-data-volume continuous test and reduce labor cost; the sample to be detected has strong applicability, and can adopt samples in various forms such as powder, block and the like; the sample and the solvent do not need to be separated in the whole test process, the operation is simple, and the accuracy and the reproducibility of data are good; the swelling characteristic research of the polymer at different temperatures can be realized by combining the double-layer jacket glass cup and connecting the temperature control equipment; and two channels are adopted, so that two samples can be tested simultaneously to improve the testing efficiency.
Drawings
Fig. 1 is a schematic structural diagram of the intelligent dynamic swelling degree testing device of the present invention.
FIG. 2 is a swelling curve obtained from the test in example 1.
FIG. 3 is a swelling curve obtained from the test in example 2.
FIG. 4 is a swelling curve obtained from the test in example 3.
Detailed Description
The invention is further described with reference to the following figures and specific embodiments.
As shown in fig. 1, an embodiment of the present invention provides an intelligent dynamic swelling degree testing apparatus, including: slide bar 13 of perpendicular setting, the horizontal lift tray 11 that links to each other through fixed knob 12 with slide bar 13, be provided with solution cup 1 on the lift tray 11, solution cup 1 top is provided with sample cup 2, there is sample 15 in the sample cup 2, 2 bottoms of sample cup are provided with liquid infiltration hole 8, displacement sensor 4 is installed to the sample cup top, displacement sensor sub-unit connection has sensor test disc 7, be provided with sample cup fixer 3 between displacement sensor 4 and sensor test disc 7, displacement sensor is connected with the digital display appearance electricity, there are digital display screen 5 and control button 6 on the digital display appearance, displacement sensor still communicates with the computer.
In order to control the temperature during the swelling degree test, a temperature control water inlet 10 and a temperature control water outlet 9 are respectively arranged on the solution cup, and the temperature control water inlet is positioned below the temperature control water outlet.
In order to maintain the temperature, a temperature control jacket 14 is also provided outside the solution cup.
The sample cup is smaller than the solution cup and can be placed into the solution cup.
The size of the sensor test disc is the same as that of the cross section of the inner side of the sample cup.
The intelligent dynamic swelling degree testing device comprises two sets of devices which are positioned on two sides of the sliding rod and are the same.
Another embodiment of the present invention provides an intelligent dynamic swelling degree test method, including the following steps:
(1) mounting of
① placing the intelligent dynamic swelling degree test device on an experimental platform (the platform needs to be horizontal without vibration and wind);
② connecting the host computer with the computer by data interface and connecting the power line;
③ the optical disk is inserted into the computer and the data acquisition software is installed.
(2) Temperature setting
① if room temperature testing is to be performed, this step can be omitted;
② the solution cup is connected with the water bath kettle by a hose, the temperature of the water bath kettle is set to a required value, and the water circulation is started.
(3) Sample preparation (taking the powder sample as an example, if the block sample is directly machined into a circular piece with the same diameter as the sample cup)
① preparing a small hand hydraulic press, a press bar, a sample cup, an electronic balance, a stopwatch, and a filter paper (corresponding to the diameter of the sample cup);
② placing a circular pad with hole on the bottom of the sample cup, and placing a piece of filter paper on the pad;
③ weighing powder sample with balance, placing into a sample cup, and gently vibrating to make the end face of the sample flat;
④ placing the pressing rod in, rotating left and right slightly to contact with the end face of the sample;
⑤ placing on the oil press platform, pressurizing and maintaining constant pressure for enough time, opening the pressure relief valve to relieve pressure when the sample is pressed into sheet;
⑥ the press bar was removed, the height H of the sheet sample was measured, and a piece of filter paper was placed on top of the formed sheet sample.
⑦ hanging the pressed sample and the sample cup on a rack, pressing the test disc of the sensor on the sheet sample, and adjusting the zero point.
(4) Beginning test
① opening a host switch of the intelligent dynamic swelling degree test device, running data acquisition software on a computer, setting a port, and if the 1 st path (corresponding to the left sample) and the 2 nd path (corresponding to the right sample) show numbers, indicating that the equipment connection is successful;
② setting appropriate data acquisition time step according to the swelling rate of the sample, and clicking the start button on the screen to run the software;
③ adjusting the lifting tray to a proper height, fixing with a fixed knob, injecting solvent into the liquid cup until the solvent flows into the sample cup from the upper part of the sample cup, and the sample immediately begins to swell, and the computer begins to record data and draw in real time;
④ testing for a certain time, the swelling curve gradually tends to level, which indicates that the test end point is reached at this time, and the test can be stopped by clicking the "end" button, the value of the stable swelling curve level is △ H;
⑤ selects the "export to EXCEL" software to automatically export data to the EXCEL form, save the data, and the test ends.
(5) Data analysis
Swelling degree:
Q=△V/V=△H/H
wherein, △ V-volume change of the swelling end point sample;
v-initial volume of sample;
△ H-height change of swelling end point sample, reading out by recording data by the device, namely the highest point value;
h-initial height of the sample, obtained by direct measurement of sample size.
The intelligent dynamic swelling degree test method is specifically described in three more specific examples.
Example 1:
a sample to be tested: 1 route: PVB; 2-path: CAB
Solvent: ethyl acetate
The implementation process comprises the following steps:
(1) mounting of
① placing the intelligent dynamic swelling degree test device on an experimental platform (the platform needs to be horizontal without vibration and wind);
② connecting the host computer with the computer by data interface and connecting the power line;
③ the optical disk is inserted into the computer and the data acquisition software is installed.
(2) Temperature setting
And testing at room temperature without setting temperature.
(3) Pressed samples
① preparing a small hand hydraulic press, a press bar, a sample cup, an electronic balance, a stopwatch, and a filter paper (corresponding to the diameter of the sample cup);
② placing a circular pad with hole on the bottom of the sample cup, and placing a piece of filter paper on the pad;
③ weighing PVB and CAB powder samples with balance, respectively placing into two sample cups, and gently vibrating to make the end faces of the samples flat;
④ placing the pressing rod in, rotating left and right slightly to contact with the end face of the sample;
⑤ placing on the oil press platform, pressurizing and maintaining constant pressure for enough time, opening the pressure relief valve to relieve pressure when the sample is pressed into sheet;
⑥ the press bar is removed and the height H of the sheet sample is measured1And H2And a piece of filter paper was placed on the formed sheet sample.
⑦ hanging the pressed sample and the sample cup on a rack as required, pressing the test disc of the sensor on the sheet sample, and adjusting the zero point.
(4) Beginning test
① opening a host switch of the intelligent dynamic swelling degree test device, running data acquisition software on a computer, setting a port, and displaying numbers on the 1 st path and the 2 nd path to show that the equipment is successfully connected at the moment;
② setting the data acquisition time step length to 1min, and clicking the start button on the screen to run the software;
③ adjusting the lifting tray to a proper height, fixing with a fixed knob, injecting ethyl acetate into the liquid cup until the ethyl acetate flows into the sample cup from the upper part of the sample cup, and the sample immediately begins to expand, and the computer begins to record data and draw in real time, and the drawing is as shown in figure 2;
④ when the test is carried out for a sufficient time, the swelling curve gradually becomes horizontal, which indicates that the test is terminated when the test is completed, the "end" button is clicked to stop the test, and the value of the stable level of the swelling curve is △ H1And △ H2;
⑤ selects the "export to EXCEL" software to automatically export data to the EXCEL form, save the data, and the test ends.
(5) Data analysis
Swelling degree:
QPVB-Ethyl acetate=△H1/H1
QCAB-Ethyl acetate=△H2/H2
Wherein, △ H1Reading 2.33mm, H1The measured value was 3.99mm, and Q was calculatedPVB-Ethyl acetate=58.4%;
△H2Reading 1.94mm, H2The measurement value was 3.20mm, and Q was calculatedCAB-Ethyl acetate=60.6%。
Example 2:
a sample to be tested: 1 route: PVB; 2-path: CAB
Solvent: anhydrous ethanol
The implementation process comprises the following steps:
(1) mounting of
① placing the intelligent dynamic swelling degree test device on an experimental platform (the platform needs to be horizontal without vibration and wind);
② connecting the host computer with the computer by data interface and connecting the power line;
③ the optical disk is inserted into the computer and the data acquisition software is installed.
(2) Temperature setting
The solution cup is connected with the water bath kettle by a hose, the temperature of the water bath kettle is set to be 30 ℃, and water circulation is started.
(3) Pressed samples
① preparing a small hand hydraulic press, a press bar, a sample cup, an electronic balance, a stopwatch, and a filter paper (corresponding to the diameter of the sample cup);
② placing a circular pad with hole on the bottom of the sample cup, and placing a piece of filter paper on the pad;
③ weighing PVB and CAB powder samples with balance, respectively placing into two sample cups, and gently vibrating to make the end faces of the samples flat;
④ placing the pressing rod in, rotating left and right slightly to contact with the end face of the sample;
⑤ placing on the oil press platform, pressurizing and maintaining constant pressure for enough time, opening the pressure relief valve to relieve pressure when the sample is pressed into sheet;
⑥ the press bar is removed and the height H of the sheet sample is measured1And H2And a piece of filter paper was placed on the formed sheet sample.
⑦ hanging the pressed sample and the sample cup on a rack, pressing the test disc of the sensor on the sheet sample, and adjusting the zero point.
(4) Beginning test
① opening a host switch of the intelligent dynamic swelling degree test device, running data acquisition software on a computer, setting a port, and displaying numbers on the 1 st path and the 2 nd path to show that the equipment is successfully connected at the moment;
② setting the data acquisition time step length to 30s, and clicking the start button on the screen to run the software;
③ adjusting the lifting tray to a proper height, fixing with a fixed knob, injecting anhydrous ethanol into the liquid cup until the anhydrous ethanol flows into the sample cup from the upper part of the sample cup, and allowing the sample to immediately expand, and allowing the computer to record data and draw in real time, wherein the drawing is as shown in FIG. 3;
④ when the test is carried out for a sufficient time, the swelling curve gradually becomes horizontal, which indicates that the test is terminated when the test is completed, the "end" button is clicked to stop the test, and the value of the stable level of the swelling curve is △ H1And △ H2;
⑤ selects the "export to EXCEL" software to automatically export data to the EXCEL form, save the data, and the test ends.
(5) Data analysis
Swelling degree:
QPVB-Anhydrous ethanol=△H1/H1
QCAB-Anhydrous ethanol=△H2/H2
Wherein, △ H1Reading 1.19mm, H1The measured value was 1.97mm, and Q was calculatedPVB-Anhydrous ethanol=60.4%;
△H2Reading 1.13mm, H2The measured value was 1.93mm, and Q was calculatedCAB-Anhydrous ethanol=58.5%。
Example 3:
a sample to be tested: f2314
Solvent: 1 route: ethyl acetate; 2-path: anhydrous ethanol
The implementation process comprises the following steps:
(1) mounting of
① placing the intelligent dynamic swelling degree test device on an experimental platform (the platform needs to be horizontal without vibration and wind);
② connecting the host computer with the computer by data interface and connecting the power line;
③ the optical disk is inserted into the computer and the data acquisition software is installed.
(2) Temperature setting
The solution cup is connected with the water bath kettle by a hose, the temperature of the water bath kettle is set to be 30 ℃, and water circulation is started.
(3) Pressed samples
① preparing a small hand hydraulic press, a press bar, a sample cup, an electronic balance, a stopwatch, and a filter paper (corresponding to the diameter of the sample cup);
② placing a circular pad with hole on the bottom of the sample cup, and placing a piece of filter paper on the pad;
③ weighing F2314 powder sample with balance, placing into two sample cups, and gently vibrating to make the end face of the sample flat;
④ placing the pressing rod in, rotating left and right slightly to contact with the end face of the sample;
⑤ placing on the oil press platform, pressurizing and maintaining constant pressure for enough time, opening the pressure relief valve to relieve pressure when the sample is pressed into sheet;
⑥ the press bar is removed and the height H of the sheet sample is measured1And H2And a piece of filter paper was placed on the formed sheet sample.
⑦ hanging the pressed sample and the sample cup on a rack, pressing the test disc of the sensor on the sheet sample, and adjusting the zero point.
(4) Beginning test
① opening a host switch of the intelligent dynamic swelling degree test device, running data acquisition software on a computer, setting a port, and displaying numbers on the 1 st path and the 2 nd path to show that the equipment is successfully connected at the moment;
② setting the data acquisition time step size to 60s, and clicking the start button on the screen to run the software;
③ adjusting the lifting tray to a proper height and fixing with a fixed knob, injecting ethyl acetate into the left liquid cup and injecting absolute ethanol into the right liquid cup until the solvent flows into the sample cup from the upper part of the sample cup, wherein the sample immediately begins to swell, and the computer begins to record data and draw in real time, and the drawing is as shown in figure 4;
④ when the test is carried out for a sufficient time, the swelling curve gradually becomes horizontal, which indicates that the test is terminated when the test is completed, the "end" button is clicked to stop the test, and the value of the stable level of the swelling curve is △ H1And △ H2;
⑤ selects the "export to EXCEL" software to automatically export data to the EXCEL form, save the data, and the test ends.
(5) Data analysis
Swelling degree:
Qf2314-acetic acid ethyl ester=△H1/H1
QF2314-Anhydrous ethanol=△H2/H2
Wherein, △ H1Reading 2.68mm, H1The measurement value was 0.87mm, and Q was calculatedF2314-acetic acid ethyl ester=308.0%;
△H2Reading 0mm, H2The measurement value was 0.87mm, and Q was calculatedF2314-Anhydrous ethanolWhen the value is 0, F2314 shows no swelling phenomenon in absolute ethyl alcohol.
Although the present invention has been described herein with reference to the illustrated embodiments thereof, which are intended to be preferred embodiments of the present invention, it is to be understood that the invention is not limited thereto, and that numerous other modifications and embodiments can be devised by those skilled in the art that will fall within the spirit and scope of the principles of this disclosure.
Claims (7)
1. The utility model provides a swelling degree intelligence dynamic testing arrangement which characterized in that includes:
the device comprises a vertically arranged sliding rod and a horizontal lifting tray connected with the sliding rod through a fixed knob, wherein a solution cup is arranged on the lifting tray, a sample cup is arranged above the solution cup, a liquid seepage hole is formed in the bottom of the sample cup, a displacement sensor is arranged above the sample cup, a sensor testing tray is connected to the lower portion of the displacement sensor, a sample cup fixer is arranged between the displacement sensor and the sensor testing tray, the displacement sensor is electrically connected with a digital display, a digital display screen and a control button are arranged on the digital display, and the displacement sensor is communicated with a computer;
a temperature control water inlet and a temperature control water outlet are respectively arranged on the solution cup, and the temperature control water inlet is positioned below the temperature control water outlet; the size of the sensor test disc is the same as that of the cross section of the inner side of the sample cup; the intelligent dynamic swelling degree testing device comprises two sets of devices which are positioned on two sides of the sliding rod and are the same.
2. The intelligent dynamic swelling capacity testing device according to claim 1, wherein:
a temperature control jacket is also arranged outside the solution cup.
3. The intelligent dynamic swelling capacity testing device according to claim 1, wherein:
the sample cup is smaller than the solution cup and can be placed into the solution cup.
4. An intelligent dynamic swelling capacity testing method, which is characterized by adopting the intelligent dynamic swelling capacity testing device of any one of claims 1 to 3, and comprises the following steps:
hanging the solid sample and the sample cup on a sample cup holder together, enabling a sensor testing disc to be in contact with the solid sample, adjusting the reading of a displacement sensor, and setting a zero point; filling the solution cup with the test solution, lifting the lifting tray to enable the test solution in the solution cup to flow into the sample cup, and immediately starting testing; the solid sample swells to generate upward displacement, so that the sensor test disc can sense the displacement distance, the displacement sensor generates displacement signals and transmits the displacement signals to the computer, the real-time change data of the displacement along with the time is recorded according to the time step set by the control button, and the computer draws a curve.
5. The intelligent dynamic swelling capacity testing method according to claim 4, wherein:
the solid sample corresponds to the diameter of the sample cup.
6. The intelligent dynamic swelling capacity testing method according to claim 4, wherein:
the solid sample is directly machined from a block sample or pressed from a powder sample by an oil press.
7. The intelligent dynamic swelling capacity testing method according to claim 6, wherein:
the powder sample is pressed by an oil press, and the method comprises the following specific steps:
① placing a circular pad with hole on the bottom of the sample cup, and placing a piece of filter paper on the pad;
② weighing powder sample with balance, placing into a sample cup, and gently vibrating to make the end face of the sample flat;
③ placing the pressing rod in, rotating left and right slightly to contact with the end face of the sample;
④ placing on the oil press platform, pressurizing and maintaining constant pressure for enough time, opening the pressure relief valve to relieve pressure when the sample is pressed into sheet;
⑤ taking out the press bar, measuring the height H of the sheet sample, and placing a piece of filter paper on the formed sheet sample;
⑥ hanging the pressed sample and the sample cup on a rack, pressing the test disc of the sensor on the sheet sample, and adjusting the zero point.
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CN2124471U (en) * | 1991-12-27 | 1992-12-09 | 南开大学 | Swelling capacity tester |
CN102313756A (en) * | 2010-07-09 | 2012-01-11 | 中科合成油技术有限公司 | Automatic swelling measuring device and swelling measuring method for coal |
US9557315B2 (en) * | 2013-07-29 | 2017-01-31 | Schlumberger Technology Corporation | Confining pressure measurement for zonal isolation evaluation |
CN106969995A (en) * | 2017-02-27 | 2017-07-21 | 江苏天和制药有限公司 | A kind of solid powder swellbility detection method |
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2017
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Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN2124471U (en) * | 1991-12-27 | 1992-12-09 | 南开大学 | Swelling capacity tester |
CN102313756A (en) * | 2010-07-09 | 2012-01-11 | 中科合成油技术有限公司 | Automatic swelling measuring device and swelling measuring method for coal |
US9557315B2 (en) * | 2013-07-29 | 2017-01-31 | Schlumberger Technology Corporation | Confining pressure measurement for zonal isolation evaluation |
CN106969995A (en) * | 2017-02-27 | 2017-07-21 | 江苏天和制药有限公司 | A kind of solid powder swellbility detection method |
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