CN113466003A - Sample preparation method and sample preparation device for testing sample containing metal foreign matters in ultrahigh molecular weight polyethylene - Google Patents
Sample preparation method and sample preparation device for testing sample containing metal foreign matters in ultrahigh molecular weight polyethylene Download PDFInfo
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- CN113466003A CN113466003A CN202110685024.5A CN202110685024A CN113466003A CN 113466003 A CN113466003 A CN 113466003A CN 202110685024 A CN202110685024 A CN 202110685024A CN 113466003 A CN113466003 A CN 113466003A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
Abstract
The invention discloses a sample preparation method and a sample preparation device for testing a sample containing metal foreign matters in ultra-high molecular weight polyethylene.
Description
Technical Field
The invention relates to a testing technology of an ultra-high molecular weight polyethylene material, in particular to a sample preparation method and a sample preparation device for testing a sample containing metal foreign matters in the ultra-high molecular weight polyethylene.
Background
With the continuous improvement of the technical development level, the detection requirements and detection means for the materials are also continuously improved. In the lithium battery diaphragm industry, if metal impurities such as copper, iron, zinc, nickel and the like exist in the material, the material is applied to downstream battery products, the diaphragm of the material has the risk of being pierced, and the piercing can cause fatal influence on the battery, so that the introduction of metal foreign matters is particularly important from the source, and the detection control of the metal foreign matters is included in the detection content of the raw material ultra-high molecular weight polyethylene.
The device is a functional device capable of automatically identifying and judging the type of impurities, particle pollutants with a sample to be detected are intercepted on the surface of a filter membrane, and the size, the quantity and the components of the contained particle pollutants are analyzed by the filter membrane by adopting methods such as a microscope observation method, an instrument analysis method and the like.
The cleanliness tester is used as one of main analysis means for controlling the content of the metallic foreign matters in the ultra-high molecular weight polyethylene, but reports on sample preparation are few, because the content of the metallic foreign matters possibly existing in the ultra-high molecular weight polyethylene is few, the sampling is difficult or crude, most of the samples are prepared and tested by adopting a direct contact mode at present, the sampling mode cannot ensure complete sampling of materials, most of the obtained samples are the ultra-high molecular weight polyethylene, so that the detection and control of the metallic foreign matters in the raw materials are limited, and the subsequent product quality is influenced.
Disclosure of Invention
In view of the above, the present invention is to provide a sample preparation method and a sample preparation device for testing a sample containing metal foreign matters in ultra-high molecular weight polyethylene, which solve the problem that the existing sample preparation and testing adopts a direct contact manner, but cannot ensure complete sampling of the material.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
the invention provides a sample preparation method for testing a sample containing metal foreign matters in ultrahigh molecular weight polyethylene, which comprises the steps of adding a first deionized water, ultrahigh molecular weight polyethylene and a surfactant in a preset proportion into a first container to generate a first solution; sleeving a pipe sleeve on a magnetic rod body for sealing, and placing the magnetic rod body into the first container to be stirred by a sample preparation device; taking out the magnetic rod body from the first container, placing the magnetic rod body into a second container, adding second deionized water, and stirring by the sample preparation device; taking the pipe sleeve of the magnetic rod body down, placing the pipe sleeve into a third container, and adding third deionized water for cleaning to generate a second solution; performing suction filtration treatment and drying treatment on the second solution to obtain a sample; wherein the sample contains a metallic foreign matter.
Furthermore, before the step of adding a first deionized water, an ultra-high molecular weight polyethylene and a surfactant in a preset proportion into a first container to generate a first solution, the method further comprises the step of adding a fourth deionized water into a fourth container, placing the fourth container into the magnetic rod body, and stirring and cleaning the fourth container by using the sample preparation device.
Further, after the step of taking out the magnetic rod body from the first container, placing the magnetic rod body into a second container, adding a second deionized water, and stirring by the sample preparation device, the method further comprises the step of performing secondary adsorption on the inner wall surface of the second container by using the magnetic rod body.
Furthermore, before the step of performing suction filtration and drying treatment on the second solution to obtain a sample, the method further comprises the step of sucking the floating material of the second solution by a dropper to perform primary filtration.
Furthermore, a magnetic block is arranged below the third container.
Further, the preset ratio is 500:50:1, and the surfactant is an emulsifier free of metal elements.
Further, the magnetic field strength of the magnetic rod body is 3000GS, 6000GS, 8000GS, 10000GS or 12000 GS; and the magnetic field intensity of the magnetic block is 6000 GS.
The invention also provides a sample preparation device for testing a sample containing metal foreign matters in the ultra-high molecular weight polyethylene, which comprises a stirring mechanism, a sample preparation device and a sample preparation device, wherein the stirring mechanism comprises a rotating shaft, a main wheel, a driven wheel, a transmission piece and a rotating disc, the rotating shaft is pivoted with the main wheel, the transmission piece is sleeved on the main wheel and the driven wheel, the main wheel and the driven wheel are arranged at opposite positions, the rotating disc comprises a shaft piece, and the rotating disc is pivoted with the driven wheel through the shaft piece; the embedded piece is provided with a hole and is pivoted with the turntable; the fixing rod comprises a rod body, a fixing and locking piece and a fixing piece, the rod body is connected with the fixing piece, the rod body is inserted into the hole of the embedding piece and is locked by the fixing and locking piece, and the fixing rod is connected with the turntable through the embedding piece; the container comprises an accommodating space, a first protruding part and a second protruding part, the first protruding part is provided with an opening, and the first protruding part and the second protruding part are fixed through the fixing piece of the fixing rod; the stirring mechanism drives the main wheel to rotate through the rotating shaft, the main wheel drives the transmission part to enable the driven wheel to rotate, the driven wheel drives the shaft part to rotate, the rotary disc is enabled to rotate, and the embedded part pivoted with the rotary disc drives the fixed rod to rotate so as to drive the container to rotate for stirring.
The container further comprises a cover body, wherein the cover body corresponds to the opening of the first protruding part, so that when the cover body covers the opening, the accommodating space of the container is in a closed state.
Further, the stirring device further comprises a driving unit electrically connected with the rotating shaft of the stirring mechanism so as to drive the rotating shaft to rotate.
The invention has the following beneficial effects:
the invention provides a sample preparation method and a sample preparation device for testing a sample containing metal foreign matters in ultra-high molecular weight polyethylene.
Drawings
FIG. 1 is a flow chart of a sample preparation method for testing metallic foreign matters in ultra-high molecular weight polyethylene provided by the invention; and
fig. 2 is a schematic diagram of a sample preparation device for testing metal foreign matters in ultra-high molecular weight polyethylene provided by the invention.
Fig. 3 is an exploded perspective view of a sample preparation device for testing metal foreign matters contained in ultra-high molecular weight polyethylene according to the present invention.
Description of component reference numerals
1 sample preparation device
2 stirring mechanism
21 wheel axle
22 main wheel
23 driven wheel
24 driving member
25 rotating disc
251 axle element
3 fitting piece
31 holes
4 fixed rod
41 rod body
42 locking piece
43 fixing element
5 Container
51 accommodating space
52 first projection
521 opening
53 second projection
54 cover body
6 drive unit
S1-S5 Steps 1-5
Detailed Description
The following detailed description of embodiments of the invention refers to the accompanying drawings. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, the combination of values between the endpoints of each range, the endpoints of each range and the individual values, and the individual values can be combined with each other to yield one or more new ranges of values, which ranges of values are to be considered as specifically disclosed herein.
Referring to fig. 1, the present invention provides a flow chart of a sample preparation method for testing metal foreign matters contained in ultra-high molecular weight polyethylene, wherein the sample preparation method comprises the following steps:
s1, adding a first deionized water, an ultra-high molecular weight polyethylene and a surfactant in a first container according to a preset proportion to generate a first solution;
s2, sleeving a pipe sleeve on a magnetic rod body for sealing, and placing the magnetic rod body into the first container to be stirred by a sample preparation device;
s3, taking out the magnetic rod body from the first container, putting the magnetic rod body into a second container, adding second deionized water, and stirring by the sample preparation device;
s4, taking the pipe sleeve of the magnetic rod body down, placing the pipe sleeve into a third container, adding third deionized water for cleaning, and arranging a magnetic block below the third container to generate a second solution; and
and S5, performing suction filtration and drying treatment on the second solution to obtain a sample.
In step S1, in the preferred embodiment, the predetermined ratio is 500; 50; 1, adding 500ml of first deionized water, 50g of ultra-high molecular weight polyethylene and 1g of surfactant into a first container, wherein the first container is a container of a sample preparation device, but not limited to the container, and the quantitative amount of the ultra-high molecular weight polyethylene 50g is a fluctuation range which can fluctuate between 50 and 100g, and actually depends on the apparent density and the actual density of the material.
In addition, the surfactant is an emulsifier without metal elements, and tween can be adopted as the surfactant in the embodimentMetallic element-free emulsifiers such as span, but not limited thereto, surfactants act to modify the surface tension of the solution, usually ultra high molecular weight polyethylene having a density of less than 1g/cm3Therefore, after a trace amount of surfactant is added, because the molecules of the surfactant have unique amphipathy, one end of the molecules is a hydrophilic polar group, and the other end of the molecules is an oleophilic nonpolar group, the two phases are both regarded as the components of the phase through the affinity of different parts in the molecules with respect to the two phases respectively, the molecules are arranged between the two phases, the surfaces of the two phases are equivalent to be transferred into the interior of the molecules, and the surface tension is reduced, so that a sample originally floating on the surface of pure water is temporarily dissolved in the pure water to generate a first solution.
Before executing step S1, pre-cleaning is performed including steps S01-S02:
s01, adding a fourth deionized water into a fourth container, placing the fourth container into the magnetic rod body, and stirring and cleaning the magnetic rod body by the sample preparation device; and
firstly, a 12000GS magnetic rod body is put into a fourth container, fourth deionized water is added to ensure that the fourth deionized water reaches the liquid level which can exceed the magnetic rod body, and the fourth container is stirred and cleaned by a sample preparation device, wherein the fourth container is the container of the sample preparation device.
S02, adding a fifth deionized water into the first container for stirring and cleaning.
And adding fifth deionized water into the first container in the same manner, and stirring and cleaning by using a sample preparation device.
Through the pre-cleaning steps of steps S01-S02, the magnetic rod and the first container can be cleaned well, so as to avoid impurities during mixing and stirring.
As shown in step S2, in the preferred embodiment, the magnetic field strength of the magnetic rod may be 3000GS, 6000GS, 8000GS, 10000GS or 12000GS, so that 12000GS with the highest magnetic field strength is also used to facilitate the absorption of the metal foreign objects, and a pipe sleeve is sleeved during the use, wherein the pipe sleeve may be made of plastic, because the material thereof is polyethylene, which will not cause deviation of the result of the final detection of the metal foreign objects, and the plastic is easy to unseal.
In step S3, after the first stirring, the magnetic rod sleeved with the sleeve is taken out of the first container, and taken into the second container, and a second deionized water is added, specifically, the second deionized water covers the magnetic rod, and the sample preparation device is used to perform the second stirring, wherein the second container is a container of the sample preparation device.
Specifically, when the magnetic rod body is not placed in the second container, the deionized water washing bottle can be used for washing the mixture on the magnetic rod body and the pipe sleeve into the second container until no mixture is visible on the surface of the magnetic rod body, and then the magnetic rod body is placed in the second container and stirred for 5 minutes.
After step S3 is executed, step S31 is included:
and S31, performing secondary adsorption on the inner wall surface of the second container by using the magnetic rod body.
After the stirring of the second time is accomplished, use clean gloves, place the magnetic rod body in the second container and carry out the secondary absorption to second container inner wall surface, the secondary absorption here is because prevent that the second container is in the stirring process, has the metallic foreign matter because centrifugal force and attached to the inner wall surface, and the metallic foreign matter that probably remains in the second container is adsorbed thoroughly to this method, reaches the effect of abundant absorption.
In step S4, after the second stirring is completed, the magnetic rod is taken out and the pipe sleeve is taken down, specifically, one end of the pipe sleeve is cut and turned over for 90 degrees, the magnetic rod is drawn out, the taken-down pipe sleeve is placed in a third container, and the magnetic material on the pipe sleeve is cleaned with third deionized water until no residue is visible on the surface of the pipe sleeve.
Here, a magnet with a strength of 6000GS is placed at the bottom of the third container, and the inner wall of the third container is rinsed with deionized water until no mixture solution remains on the inner wall of the third container, and in the process, the magnet cannot leave the bottom of the third container to generate a second solution, wherein the third container is a beaker, but not limited thereto.
As described in step S5, the second solution is poured into a suction flask for suction filtration to obtain a sample containing magnetic impurities, and preferably, a supernatant of the second solution is sucked out using a plastic dropper before the suction filtration step is performed, and compared with the step of directly suction-filtering the obtained second solution, the step of sucking out the supernatant of the second solution can remove the scum and resin floating in the supernatant of the second solution, so as to improve the accuracy of the test.
And then placing the obtained sample of the magnetic impurities on a slide used by a clean tester, and performing a drying treatment to generate a sample, wherein the sample contains the metal impurities, and preferably, the drying treatment is drying for 20 minutes in an oven at 60 ℃, but not limited thereto.
Fig. 2 is a schematic diagram of a sample preparation device for testing metal foreign matters in ultra-high molecular weight polyethylene according to the present invention, and is shown in the figure. The sample preparation device 1 includes a stirring mechanism 2, a fitting member 3, and a container 5, and is described in detail as follows:
the stirring mechanism 2 includes a wheel shaft 21, a main wheel 22, a driven wheel 23, a transmission member 24 and a turntable 25, wherein the wheel shaft 21 is pivoted with the main wheel 22, the transmission member 24 is sleeved on the main wheel 22 and the driven wheel 23, and the main wheel 22 and the driven wheel 23 are disposed at opposite positions, i.e., when the main wheel 22 rotates, the transmission member 24 is driven to rotate, and further the driven wheel 23 is driven to rotate, the turntable 25 further includes a shaft member 251, the shaft member 251 enables one side of the turntable 25 to be pivoted with the driven wheel 23, and the other side of the turntable 25 is pivoted with the embedded member 3, wherein the embedded member 3 has a hole 31.
The fixing rod 4 includes a rod body 41, a locking member 42 and a fixing member 43, the rod body 41 is connected with the fixing member 43, and the connection may be a locking manner or welding fixation, but not limited thereto, the rod body 41 is inserted into the hole 31 of the engaging member 3, and the locking member 42 locks the rod body 41 on the engaging member 3, so that the fixing rod 4 is connected and fixed with the turntable 25 through the engaging member 3.
The container 5 includes an accommodating space 51, a first protrusion 52 and a second protrusion 53, wherein the first protrusion 52 has an opening 521, the first protrusion 52 and the second protrusion 53 are both fixed by the fixing member 43 of the fixing rod 4 and are respectively connected with the rotating discs 25 of the two stirring mechanisms 2 through the two engaging members 3 into a whole, the container 5 is the first container, the second container and the fourth container in the foregoing method, wherein the container 5 further includes a cover 54, the cover 54 corresponds to the opening 521 of the first protrusion 52, so that the cover 54 covers the opening 521, and the accommodating space 51 of the container 5 is in a sealed state.
The sample preparation device 1 further comprises a pressing rod 5 and a driving unit 6, wherein the pressing rod comprises a rod body 51 and a second rod body 52, the rod body 51 is disposed on the first protruding portion 52 of the container 5, and the second rod body is disposed on the second protruding portion 53 of the container 5 to fix the container 5, so that the container 5 does not move when the stirring and shaking are performed, and the driving unit 6 is electrically connected with the rotating shaft 21 of the stirring mechanism 2 to drive the rotating shaft 21 to rotate.
In the preferred embodiment, the whole operation mode is that the stirring mechanism 2 drives the rotating shaft 21 to rotate through the driving unit 6, and then drives the main wheel 22 to rotate through the rotating shaft 21, the main wheel 22 drives the transmission member 24 to rotate the driven wheel 23, the driven wheel 23 drives the shaft 251 to rotate, so that the rotating disc 25 rotates, the fixing rod 4 is driven to rotate by the engaging member 3 pivoted to the rotating disc 25, and the fixing member 43 of the fixing rod 4 drives the container 5 to rotate, so as to stir the liquid and the magnetic rod in the container 5.
The system appearance device that the present case used, compare down with ordinary agitator, its ordinary agitator is only manual stirring, the operation mode is comparatively crude, and the stirring degree is even inadequately, consequently, can not make the magnetic rod body and the sample in the solution fully contact, simultaneously because manual stirring, can make solution expose in the air at stirring in-process, solution spill takes place easily, perhaps the impurity impression testing result that probably exists in the air, on the contrary, the system appearance device that the present case adopted, the operation is thus simple, the stirring environment is sealed, can not influence solution and expose or excessively contact with the air, and can make by stirring solution dispersion even, thereby make the sample fully contact in the magnetic rod body and the solution.
Example 1
Putting the 12000GS magnetic rod body into a fourth container, adding fourth deionized water to enable the fourth deionized water to reach a liquid level which can exceed the magnetic rod body, stirring and cleaning by a sample preparation device, and adding a proper amount of fifth deionized water into the first container, and stirring and cleaning by the sample preparation device.
Adding 500ml of first deionized water, 50g of ultra-high molecular weight polyethylene and 1g of surfactant into the cleaned first container to generate a first solution, sleeving the cleaned magnetic rod body with a plastic pipe, sealing, placing the magnetic rod body into the first container, and stirring the magnetic rod body and the first solution together for 5 minutes by using a sample preparation device.
After the stirring, take out the magnetism body of rod, and use the second deionized water to wash the mixture on the magnetism body of rod and the pipe box in the second container, after no macroscopic mixture on the surface of the magnetism body of rod, put into the second container again the magnetism body of rod to pour into the second deionized water, make the second deionized water reach the liquid level that can surpass the magnetism body of rod, once more, stir the magnetism body of rod and first solution for 5 minutes together with the system appearance device.
After stirring, using clean gloves, performing secondary adsorption on the surface of the inner wall of a second container by a magnetic rod body placed in the second container, taking out the magnetic rod body, cutting and turning over one end of a pipe sleeve sleeved on the magnetic rod body for 90 degrees, drawing out the magnetic rod body, placing the pipe sleeve taken down into a third container with a magnetic block with the strength of 6000GS at the bottom, cleaning the magnetic substance on the pipe sleeve and the inner wall of the third container by third deionized water until no visible residues exist on the surface of the pipe sleeve and the inner wall of the third container, and generating a second solution after cleaning.
And finally, sucking out the supernatant of the second solution by using a plastic dropper to remove the froth and the resin floating in the supernatant of the second solution, performing suction filtration, and drying for 20 minutes in an oven at 60 ℃ to generate a sample.
Example 2
The 12000GS magnetic rod body is placed into a fourth container, fourth deionized water is added, the fourth deionized water reaches the liquid level which can exceed the magnetic rod body, stirring cleaning is carried out by manual stirring, and a proper amount of fifth deionized water is added into the first container, and stirring cleaning is carried out by manual stirring.
Adding 500ml of first deionized water, 50g of ultra-high molecular weight polyethylene and 1g of surfactant into the cleaned first container to generate a first solution, sleeving the cleaned magnetic rod body with a plastic pipe, sealing, placing the magnetic rod body in the first container, and manually stirring the magnetic rod body and the first solution for 5 minutes.
After the stirring, take out the magnetism body of rod, and use the second deionized water to wash the mixture on the magnetism body of rod and the pipe box in the second container, after no macroscopic mixture on the surface of the magnetism body of rod, put into the second container again the magnetism body of rod to pour into the second deionized water, make the second deionized water reach the liquid level that can surpass the magnetism body of rod, once more, stir the magnetism body of rod and first solution for 5 minutes together with manual stirring.
After stirring, using clean gloves, performing secondary adsorption on the surface of the inner wall of a second container by a magnetic rod body placed in the second container, taking out the magnetic rod body, cutting and turning over one end of a pipe sleeve sleeved on the magnetic rod body for 90 degrees, drawing out the magnetic rod body, placing the pipe sleeve taken down into a third container with a magnetic block with the strength of 6000GS at the bottom, cleaning the magnetic substance on the pipe sleeve and the inner wall of the third container by third deionized water until no visible residues exist on the surface of the pipe sleeve and the inner wall of the third container, and generating a second solution after cleaning.
And finally, sucking out the supernatant of the second solution by using a plastic dropper to remove the froth and the resin floating in the supernatant of the second solution, performing suction filtration, and drying for 20 minutes in an oven at 60 ℃ to generate a sample.
Example 3
Putting the 12000GS magnetic rod body into a fourth container, adding fourth deionized water to enable the fourth deionized water to reach a liquid level which can exceed the magnetic rod body, stirring and cleaning by a sample preparation device, and adding a proper amount of fifth deionized water into the first container, and stirring and cleaning by the sample preparation device.
Adding 500ml of first deionized water, 50g of ultra-high molecular weight polyethylene and 1g of surfactant into the cleaned first container to generate a first solution, sleeving the cleaned magnetic rod body with a plastic pipe, sealing, placing the magnetic rod body into the first container, and stirring the magnetic rod body and the first solution together for 5 minutes by using a sample preparation device.
After the stirring, take out the magnetism body of rod, and use the second deionized water to wash the mixture on the magnetism body of rod and the pipe box in the second container, after no macroscopic mixture on the surface of the magnetism body of rod, put into the second container again the magnetism body of rod to pour into the second deionized water, make the second deionized water reach the liquid level that can surpass the magnetism body of rod, once more, stir the magnetism body of rod and first solution for 5 minutes together with the system appearance device.
After stirring, using clean gloves, performing secondary adsorption on the surface of the inner wall of a second container by a magnetic rod body placed in the second container, taking out the magnetic rod body, cutting and turning over one end of a pipe sleeve sleeved on the magnetic rod body by 90 degrees, drawing out the magnetic rod body, placing the taken-off pipe sleeve into a third container, cleaning the magnetic substance on the pipe sleeve and the inner wall of the third container by third deionized water until no visible residues exist on the surface of the pipe sleeve and the inner wall of the third container, generating a second solution after cleaning, finally directly performing suction filtration treatment on the second solution, and drying for 20 minutes in an oven at 60 ℃ to generate a sample.
After experimental detection, the method is divided into the following 5 sample preparation methods, and the data obtained by the obtained samples in the detection process are compared to verify that the method is the optimal sample preparation method, and the detailed description is as follows:
the detection method comprises the steps of placing a slide glass with a sample on a scanning table by using a cleanliness tester, enabling a light source to directly irradiate the surface of the slide glass for result analysis, automatically analyzing relevant information such as sizes/quantities of metal particles, non-metal particles and fibers contained in a filter membrane by using the cleanliness tester, and sequentially arranging default particles from large to small according to the length, wherein a polarizer on the cleanliness tester is adjusted to further judge metal and nonmetal.
The 1 st sample preparation method is example 1 of the present invention, and the detection results are shown in the following table:
TABLE 1 test results of the first sample preparation method (example 1)
The second sample preparation method is a conventional common sampling test method, in which a clean and dust-free plastic bag is sleeved with a clean magnetic rod, the plastic bag is stirred for 5 minutes, powder adsorbed by the magnetic rod in the plastic bag is collected and placed on a slide glass to be analyzed by a cleanliness tester, and the test results are as follows:
TABLE 2 second sample preparation method test results
The third sample preparation method is that the conventional magnet method is used for determining the foreign matters of the anode material, a sample to be detected and pure water are put into a plastic wide-mouth bottle, the wide-mouth bottle is sleeved in an outer ring magnet, the magnetic foreign matters absorbed in the bottle by the outer ring magnet are collected after being stirred by a jar mill, the stirred material is continuously added into the sample to be detected, a 300-plus-350-mesh screen is used for sieving to obtain the processed sample, and the number of the magnetic and non-magnetic foreign matters in the sample is detected by using an electron microscope (SEM) and an energy distributor X-ray spectrum (EDS), and the detection results are as follows:
TABLE 3 test results of the third sample preparation method
The fourth sample preparation method is example 2 of the present invention, and the test results are shown in the following table:
TABLE 4 test results of the fourth sample preparation method (example 2)
The fifth sample preparation method is example 3 of the present invention, and the detection results are shown in the following table:
TABLE 5 test results of the fifth sample preparation method (example 3)
As can be seen from the above, in the 5 sample preparation methods, the accuracy obtained by the sampling detection by the first sample preparation method (example 1) is the highest, and the number and types of the metals and non-metals involved in the detection are the largest, so that the sample preparation method and the sample preparation apparatus according to the present invention can solve the problem that the conventional techniques are difficult to sample or cannot sample completely.
By combining the embodiment 1, the embodiment 2 and the embodiment 3, and as can be seen from tables 1 to 5, the sample preparation method and the sample preparation device thereof of the present invention significantly improve the accuracy of the sample preparation, and greatly increase the number and the total types of the detected metals and non-metals, so that the present invention has a very high industrial application value.
The above matters related to the common general knowledge are not described in detail and can be understood by those skilled in the art.
The present invention is not intended to be limited to the particular embodiments shown and described, but is to be accorded the widest scope consistent with the principles and novel features disclosed herein. The technical scope of the present invention is not limited to the content of the specification, and must be determined according to the scope of the claims.
Claims (10)
1. A sample preparation method for testing a sample containing metal foreign matters in ultra-high molecular weight polyethylene comprises the following steps:
adding a first deionized water, an ultra-high molecular weight polyethylene and a surfactant in a first container according to a preset proportion to generate a first solution;
sleeving a pipe sleeve on a magnetic rod body for sealing, and placing the magnetic rod body into the first container to be stirred by a sample preparation device;
taking out the magnetic rod body from the first container, placing the magnetic rod body into a second container, adding second deionized water, and stirring by the sample preparation device;
taking the pipe sleeve of the magnetic rod body down, putting the pipe sleeve into a third container, adding third deionized water for cleaning, and generating a second solution; and
carrying out suction filtration treatment and drying treatment on the second solution to obtain a sample;
wherein the sample contains a metallic foreign matter.
2. The method as claimed in claim 1, further comprising the steps of adding a predetermined ratio of a first deionized water, an ultrahigh molecular weight polyethylene and a surfactant into a first container to form a first solution, wherein the first container is filled with the first deionized water, the ultrahigh molecular weight polyethylene and the surfactant, and the step of:
adding fourth deionized water into a fourth container, placing the fourth container into the magnetic rod body, and stirring and cleaning the fourth container by using the sample preparation device; and
and adding fifth deionized water into the first container for stirring and cleaning.
3. The method as claimed in claim 1, further comprising the steps of taking out the magnetic rod from the first container, placing the magnetic rod into a second container, adding a second deionized water, and stirring the sample with the sample preparation device, wherein the step of adding a second deionized water comprises:
and carrying out secondary adsorption on the inner wall surface of the second container by using the magnetic rod body.
4. The method as claimed in claim 1, further comprising the steps of, before the step of performing suction filtration and drying on the second solution to obtain a sample:
and sucking the floating substance of the second solution by a drop tube for preliminary filtration.
5. The method as claimed in claim 1, wherein a magnet is disposed under the third container in the step of removing the sleeve of the magnetic rod and placing the sleeve into a third container, adding a third deionized water for cleaning, and generating a second solution.
6. The sample preparation method for testing the samples containing the metallic foreign matters in the ultra-high molecular weight polyethylene according to claim 1, wherein the preset ratio is 500:50:1, and the surfactant is an emulsifier without a metallic element.
7. The method for sampling an ultra-high molecular weight polyethylene having a metallic foreign substance according to claim 5, wherein the magnetic field intensity of the magnetic rod body is 3000GS, 6000GS, 8000GS, 10000GS, or 12000 GS; and the magnetic field intensity of the magnetic block is 6000 GS.
8. A sample preparation device for testing a sample containing metal foreign matters in ultra-high molecular weight polyethylene, comprising:
the stirring mechanism comprises a rotating shaft, a main wheel, a driven wheel, a transmission piece and a rotating disc, wherein the rotating shaft is pivoted with the main wheel, the transmission piece is sleeved on the main wheel and the driven wheel, the main wheel and the driven wheel are arranged at opposite positions, the rotating disc comprises a shaft piece, and the rotating disc and the driven wheel are pivoted through the shaft piece;
the embedded piece is provided with a hole and is pivoted with the turntable;
the fixing rod comprises a rod body, a fixing and locking piece and a fixing piece, the rod body is connected with the fixing piece, the rod body is inserted into the hole of the embedding piece and is locked by the fixing and locking piece, and the fixing rod is connected with the turntable through the embedding piece; and
a container, including an accommodating space, a first protruding portion and a second protruding portion, the first protruding portion having an opening, the first protruding portion and the second protruding portion being fixed by the fixing member of the fixing rod;
the stirring mechanism drives the main wheel to rotate through the rotating shaft, the main wheel drives the transmission part to enable the driven wheel to rotate, the driven wheel drives the shaft part to rotate, the rotary disc is enabled to rotate, and the embedded part pivoted with the rotary disc drives the fixed rod to rotate so as to drive the container to rotate for stirring.
9. The apparatus as claimed in claim 8, wherein the container further comprises a cover corresponding to the opening of the first protrusion, such that the receiving space of the container is sealed when the cover covers the opening.
10. The apparatus as claimed in claim 8, further comprising:
and the driving unit is electrically connected with the rotating shaft of the stirring mechanism so as to drive the rotating shaft to rotate.
Priority Applications (1)
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