Nuclear magnetic resonance fiber oil content standard sample and preparation method thereof
By using filler materials with specific particle size and viscosity, as well as sealing components, the uniformity and stability issues of fiber standards were resolved, thus achieving accuracy in nuclear magnetic resonance testing and convenience in equipment calibration.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- SUZHOU NIUMAG ELECTRONICS TECH
- Filing Date
- 2023-04-24
- Publication Date
- 2026-05-29
Smart Images
Figure CN116429536B_ABST
Abstract
Description
Technical Field
[0001] This application relates to the field of nuclear magnetic resonance testing technology, specifically to a nuclear magnetic resonance fiber oil content standard and its preparation method. Background Technology
[0002] Compared with traditional extraction methods for testing fiber oil content, nuclear magnetic resonance (NMR) offers advantages such as high accuracy, good repeatability, convenience, and environmental friendliness. However, as an interval analysis method, NMR results require proper calibration to be translated into fiber oil content. This necessitates establishing a relationship curve between oil mass and NMR signal intensity, which requires calibration using samples with known oil content. Therefore, fiber standards are crucial for NMR testing of fiber oil content.
[0003] In addition, the NMR equipment used for testing the oil content of fibers is subject to hardware deviations due to factors such as ambient temperature, equipment aging, and different production batches. This can lead to different results when the same NMR equipment tests the oil content of the same sample at different times or when different NMR equipment tests the same sample. Therefore, a set of fiber standard samples with good accuracy and stability can be used as a reference to effectively correct the deviation of the NMR equipment.
[0004] Currently, fiber standards are typically prepared using fiber samples with known oil content from the production line. While these samples are simple to prepare, they cannot be stored for long periods and are generally discarded after use. Another method involves mixing oil with organic powder to prepare fiber standards; however, this method often results in uneven mixing of the organic powder and oil, and the added oil tends to cause the organic powder to clump together, leading to poor sample uniformity and stability.
[0005] Therefore, developing a fiber oil content standard sample suitable for NMR fiber oil content testing, with good uniformity and stability, has become a technical problem that needs to be solved by those skilled in the art. Summary of the Invention
[0006] This application provides a standard sample for the oil content of nuclear magnetic resonance fibers and its preparation method. The standard sample is suitable for testing the oil content of nuclear magnetic resonance fibers and has good uniformity and stability.
[0007] To solve one or more of the above-mentioned technical problems, the technical solution adopted in this application is:
[0008] This application provides a standard sample for the oil content of nuclear magnetic resonance fiber, the standard sample comprising: a sample tube, a sealing assembly, and a filler;
[0009] The sample tube is a cylindrical structure with one end open. The material of the sample tube is a material that does not contain hydrogen. The sealing component is disposed in the sample tube and forms a first receiving space with the sample tube. The filler is disposed in the first receiving space.
[0010] The filler includes a first filler and a second filler. The first filler is a solid material without hydrogen with a particle size of 0.2-1.0 mm, and the second filler is a liquid material containing hydrogen. The kinematic viscosity of the second filler is <100 cst, and the T2 relaxation time of the second filler is less than 1000 ms.
[0011] Furthermore, the first filler includes one of silica, fluorinated ethylene propylene copolymer, and polytetrafluoroethylene;
[0012] And / or,
[0013] The second filler includes one of the following: copper sulfate aqueous solution, manganese chloride aqueous solution, natural oils, silicone oil, mineral oil, and polyether.
[0014] Furthermore, the mass of the second filler is 0-1.0g.
[0015] Furthermore, the sealing assembly includes a first sealing unit and a second sealing unit, which are fixedly connected. The first sealing unit is disposed at one end close to the first accommodating space, and the second sealing unit is disposed at one end away from the first accommodating space.
[0016] Furthermore, the first sealing unit includes a sealing sheet, a first column connected to the sealing sheet, and a second column connected to the first column. The diameter of the sealing sheet is larger than the inner diameter of the sample tube. The sealing sheet is disposed in the sample tube by an interference fit. The diameter of the first column is smaller than the inner diameter of the sample tube. The diameter of the second column is equal to the inner diameter of the sample tube. The sealing sheet, the first column, the second column, and the sample tube form a second receiving space.
[0017] Furthermore, the first sealing unit is provided with a through hole, which communicates with the first accommodating space.
[0018] Furthermore, the second column is provided with a mounting hole, and the mounting hole is provided with an internal thread. The second sealing unit includes a third column, a fourth column connected to the third column, and a sealing cap. The third column is provided with an external thread that matches the internal thread. The third column can move along a preset direction through the internal thread provided in the mounting hole. The sealing cap is fitted onto one end of the sample tube opening, and the sealing cap seals the sample tube by adhesive sealing.
[0019] Furthermore, the materials of the first sealing unit, the third column, and the fourth column are materials that do not contain hydrogen.
[0020] Furthermore, the materials of the first sealing unit, the third column, and the fourth column include polytetrafluoroethylene.
[0021] Furthermore, a set consists of four or more of the aforementioned nuclear magnetic resonance fiber oil content standards.
[0022] Preferably, a set consists of eight NMR fiber oil content standards.
[0023] This application also provides a method for preparing the above-mentioned nuclear magnetic resonance fiber oil content standard sample, the preparation method comprising:
[0024] The second filler and the first filler are placed into the sample tube in sequence and mixed evenly. The height of the mixture of the first filler and the second filler is the first preset value.
[0025] The first sealing unit is placed into the sample tube and comes into contact with the first filler and the second filler, and the second preset atmospheric pressure is extracted;
[0026] The second sealing unit is placed into the sample tube and connected to the first sealing unit. The sealing cap in the second sealing unit and the sample tube are sealed by adhesive sealing.
[0027] According to the specific embodiments provided in this application, the following technical effects are disclosed:
[0028] This application provides a standard sample for the oil content of nuclear magnetic resonance (NMR) fibers and its preparation method. A hydrogen-free solid material with a particle size of 0.2-1.0 mm is used to simulate the fiber filaments in oil-containing fibers, while a hydrogen-containing liquid material with a kinematic viscosity <100 cSt and a T2 relaxation time <1000 ms is used to simulate the fiber oil. This solves the problems of poor mixing and uniformity in existing fiber standard samples made from powdered materials. The first filler provided in this application has good flowability, ensuring good uniformity of the prepared fiber standard sample. Simultaneously, the first filler has high strength, is not easily deformed, and has good stability. The second filler provided in this application has a kinematic viscosity <100 cSt, allowing for better mixing with the first filler and ensuring good uniformity and stability of the final prepared fiber standard sample.
[0029] Furthermore, this application employs a sealing component to isolate the filler from the external environment, and removes residual gas from the sample tube through vacuum extraction, preventing oxidation and deterioration of the filler and thus extending the service life of the fiber standard. Additionally, because the residual gas in the sample tube is removed, the filler in the fiber standard is in a vacuum state, resulting in a fiber standard with a certain degree of thermal insulation, less affected by ambient temperature, and thus a wider range of applicable environments.
[0030] Furthermore, the second filler used in this application is closer to the properties of fiber oil in actual oil-containing fibers, making it suitable for testing the oil content of various fibers. At the same time, the eight nuclear magnetic resonance fiber oil content standard samples form a set, which broadens the testing range of oil content.
[0031] Furthermore, this application obtains the standard sample by directly placing the filler in the sample tube and sealing it. When performing fiber oil content testing or NMR equipment calibration, the standard sample can be directly placed in the NMR equipment for testing, which is convenient and quick to use, and the structure is also more aesthetically pleasing. Attached Figure Description
[0032] To more clearly illustrate the technical solutions in the embodiments of this application or the prior art, the drawings used in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this application. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.
[0033] Figure 1 This is a schematic diagram of the structure of the nuclear magnetic resonance fiber oil content standard provided in the embodiments of this application;
[0034] Figure 2 A schematic diagram of the structure of the first sealing unit of the nuclear magnetic resonance fiber oil content standard sample provided in an embodiment of this application, taken from one direction.
[0035] Figure 3 This is a schematic diagram of the structure of the first sealing unit of the nuclear magnetic resonance fiber oil content standard sample provided in an embodiment of this application from another direction.
[0036] Figure 4 A schematic diagram of the structure of the second sealing unit for the nuclear magnetic resonance fiber oil content standard sample provided in this application embodiment;
[0037] Figure 5 A flowchart illustrating the method for preparing the oil content standard of nuclear magnetic resonance fiber provided in this application embodiment;
[0038] Figure 6 The calibration curve between the oil mass and the corresponding nuclear magnetic resonance signal in the fiber standard sample when the echo time is 10ms is provided for the embodiments of this application;
[0039] Figure 7 The calibration curve between the oil mass and the corresponding nuclear magnetic resonance signal in the fiber standard sample when the echo time is 2.5ms is provided for the embodiments of this application. Detailed Implementation
[0040] The technical solutions in the embodiments of this application will be clearly and completely described below. Obviously, the described embodiments are only some embodiments of this application, and not all embodiments. Based on the embodiments in this application, all other embodiments obtained by those skilled in the art are within the scope of protection of this application.
[0041] As described in the background section, current fiber standards typically use fiber samples with known oil content from the production line. While these samples are simple to prepare, they cannot be stored for long periods and are generally discarded after use. Another method involves mixing oil with organic powder to prepare fiber standards; however, this method often results in uneven mixing of the organic powder and oil, and the organic powder tends to clump together after the addition of oil, leading to poor sample uniformity and stability. Therefore, this application provides a nuclear magnetic resonance fiber oil content standard and its preparation method. This standard is suitable for testing the oil content of nuclear magnetic resonance fibers and exhibits good uniformity and stability.
[0042] Figure 1 This is a schematic diagram of the structure of the nuclear magnetic resonance fiber oil content standard provided in the embodiments of this application; Figure 2 A schematic diagram of the structure of the first sealing unit of the nuclear magnetic resonance fiber oil content standard sample provided in an embodiment of this application, taken from one direction. Figure 3 This is a schematic diagram of the structure of the first sealing unit of the nuclear magnetic resonance fiber oil content standard sample provided in an embodiment of this application from another direction. Figure 4 This is a schematic diagram of the structure of the second sealing unit for the NMR fiber oil content standard sample provided in an embodiment of this application. Figure 1 As shown, and also refer to Figure 2 , Figure 3 and Figure 4 The nuclear magnetic resonance fiber oil content standard sample includes a sample tube 100, a sealing assembly 200, and a filler; the sealing assembly 200 includes a first sealing unit 210 and a second sealing unit 220, wherein the first sealing unit 210 includes a sealing sheet 211, a first column 212, and a second column 213, and the second sealing unit 220 includes a third column 221, a fourth column 222, and a sealing cap 223; the filler includes a first filler and a second filler.
[0043] The sample tube 100 is a cylindrical structure with one open end. The sealing component 200 is disposed in the sample tube 100 and forms a first receiving space 300 with the sample tube 100. The first receiving space 300 is used to place the filler. Since nuclear magnetic resonance mainly tests the signal of hydrogen, and the nuclear magnetic resonance signal of the standard sample is provided by the filler, the material of the sample tube 100 used to place the filler is a hydrogen-free material. As an illustrative example only and not a limitation on the scope of protection, the material of the sample tube 100 includes one of silica, fluorinated ethylene propylene copolymer, and polytetrafluoroethylene. It can be selected according to actual needs without departing from the inventive concept of this application, and no specific limitation is made here. As a preferred embodiment, the sample tube 100 is colorless and transparent glass. Using colorless and transparent glass makes it easier to observe the state of the filler placed in the sample tube 100, especially during the standard sample preparation process, to observe whether the first filler and the second filler are mixed evenly. The sample tube 100 has a diameter of 10-60 mm and a height of 20-250 mm. It should be noted that the diameter and height of the sample tube 100 are compatible with the NMR equipment used with the fiber standard. In this embodiment, the filler providing the NMR signal is directly placed in the sample tube 100 and sealed to obtain the fiber standard. When testing the fiber oil content or calibrating the NMR equipment, the fiber standard can be directly placed into the NMR equipment for testing. This method is convenient, quick, and aesthetically pleasing.
[0044] This application uses fillers to simulate oil-containing fibers. The fillers include a first filler and a second filler. The first filler simulates the filaments in the oil-containing fibers, and the second filler simulates the oil in the fibers. The first filler is a hydrogen-free solid material with a particle size of 0.2-1.0 mm. This is merely an illustrative example and not a limitation on the scope of protection. The first filler includes one of silica, fluorinated ethylene propylene copolymer, and polytetrafluoroethylene. It can be selected according to actual needs without departing from the inventive concept of this application, and no specific limitation is made here. Using a hydrogen-free solid material with a particle size of 0.2-1.0 mm as the first filler ensures a certain filling density and good flowability. Adding the second filler prevents clumping, resulting in uniform and thorough mixing of the sample. Furthermore, the 0.2-1.0 mm hydrogen-free solid material has high strength, is not easily deformed, and has good stability. More specifically, the particle size of the first filler can be 0.2 mm, 0.4 mm, 0.6 mm, 0.8 mm, 1.0 mm, and specific values between the above values. Due to space limitations and for the sake of brevity, this invention will not exhaustively list the specific values included in the range.
[0045] The second filler is a hydrogen-containing liquid material with a kinematic viscosity <100 cSt and a T2 relaxation time <1000 ms. This hydrogen-containing liquid material with a kinematic viscosity <100 cSt and a T2 relaxation time <1000 ms is closer to the properties of the oil in oil-containing fibers and also possesses better stability. Using this material can better simulate the oil in oil-containing fibers, resulting in more accurate markings on fiber standards prepared using this material. Furthermore, the hydrogen-containing liquid material with a kinematic viscosity <100 cSt and a T2 relaxation time <1000 ms can mix better with the first filler, ensuring the uniformity and stability of the final fiber standard. This is merely an illustrative example and not a limitation on the scope of protection. The second filler includes one of the following: copper sulfate aqueous solution, manganese chloride aqueous solution, natural oils, silicone oil, mineral oil, and polyether. It can be selected according to actual needs without departing from the inventive concept of this application, and no specific limitation is made here. Furthermore, a set consists of four or more NMR fiber oil content standard samples; preferably, a set consists of eight NMR fiber oil content standard samples, including one fiber standard sample with a second filler mass of 0g. This fiber standard sample with a second filler mass of 0g is used to test the substrate signal of the NMR device. It should be noted that the oil content of the fiber standard sample is obtained by converting the mass of the second filler; that is, the larger the mass of the second filler, the higher the oil content of the corresponding fiber standard sample. Furthermore, the range of oil content of the fiber standard sample should include the range of oil content of the fiber to be tested, and the mass of the second filler in the fiber standard sample is 0-1.0g.
[0046] To prevent the filler from oxidizing and deteriorating upon contact with air, this application employs a sealing assembly 200 to isolate the filler from the external environment. The sealing assembly 200 includes a first sealing unit 210 and a second sealing unit 220. The first sealing unit 210 is located at one end near the first receiving space 300, and the second sealing unit 220 is located at the end away from the first receiving space 300. The first sealing unit 210 and the second sealing unit 220 are fixedly connected. In one specific embodiment, the first sealing unit 210 and the second sealing unit 220 can be connected by threads.
[0047] Furthermore, the first sealing unit 210 includes a sealing sheet 211, a first column 212 connected to the sealing sheet 211, and a second column 213 connected to the first column 212. In this embodiment, the sealing sheet 211 abuts against the filler. During the preparation of the fiber standard sample, the filler is first placed into the sample tube 100, and then the first sealing unit 210 is placed into the sample tube 100, whereby the sealing sheet 211 compacts the filler. To further prevent air from the external environment from entering the filler, the diameter of the sealing sheet 211 is larger than the inner diameter of the sample tube 100, and the sealing sheet 211 is disposed in the sample tube 100 by an interference fit. The first column 212 connects the second column 213 and the sealing plate 211. The diameter of the first column 212 is smaller than the inner diameter of the sample tube 100, and the diameter of the second column 213 is equal to the inner diameter of the sample tube 100. The sealing plate 211, the first column 212, the second column 213, and the sample tube 100 form a second receiving space 400, which provides a buffer space for the sealing plate 211 to deform during the sealing process. The first sealing unit 210 is provided with a through hole 215, which communicates with the first receiving space 300. The vacuum device removes the gas in the first receiving space 300 through the through hole 215, thereby avoiding oxidation of the filler and extending the service life of the fiber standard. In addition, since the gas is removed, the filler in the fiber standard is in a vacuum state, and the prepared fiber standard has a certain heat insulation effect, is less affected by the ambient temperature, and can be used in a wider range of environments. In practice, after the vacuum device and the through hole 215 are connected to extract 0.3-0.5 atmospheres of pressure, the second sealing unit 220 is placed into the sample tube 100 for the next sealing step. The second column 213 is also provided with a mounting hole 214, which has an internal thread. The second sealing unit 220 is threadedly connected to the first sealing unit 210 through the internal thread in the mounting hole 214.
[0048] The second sealing unit 220 includes a third column 221, a fourth column 222 connected to the third column 221, and a sealing cap 223. The diameter of the third column 221 is smaller than the diameter of the fourth column 222. The third column 221 is provided with an external thread that matches the internal thread in the mounting hole 214. The third column 221 can move along a preset direction through the internal thread in the mounting hole 214. The preset direction is the axial direction of the sample tube 100. When the second sealing unit 220 and the first sealing unit 210 are connected, the third column 221 moves along a direction close to the second column 213 through the internal thread in the mounting hole 214. Furthermore, the diameter of the fourth column 222 is smaller than the inner diameter of the sample tube 100 to facilitate the second sealing unit 220 entering the sample tube 100 and connecting with the first sealing unit 210. A sealing cap 223 is fitted onto one end of the sample tube 100 opening and sealed with adhesive to prevent air from entering the fiber standard and affecting its stability. In one specific embodiment, photosensitive adhesive can be used to seal the sealing cap 223 and the sample tube 100. Photosensitive adhesive has a fast bonding speed and the bonding process is easy to control. The photosensitive adhesive is cured by uniformly irradiating with an ultraviolet lamp for 5-20 minutes.
[0049] Furthermore, since nuclear magnetic resonance (NMR) primarily tests the signal of hydrogen, and the NMR signal of this fiber standard is provided by the filler material, the materials of the first sealing unit 210, the third column 221, and the fourth column 222, which serve a sealing function, are materials that do not contain hydrogen. This is merely an illustrative example and not a limitation on the scope of protection. The materials of the first sealing unit 210, the third column 221, and the fourth column 222 include polytetrafluoroethylene (PTFE). These materials can be selected according to actual needs without departing from the inventive concept of this application, and no specific limitations are made here.
[0050] Corresponding to the aforementioned NMR fiber oil content standard, this application also provides a method for preparing the aforementioned NMR fiber oil content standard, such as... Figure 5 As shown, the preparation method includes:
[0051] S1: Place the second filler and the first filler into the sample tube in sequence and mix them evenly. The height of the mixture of the first filler and the second filler is the first preset value.
[0052] Furthermore, the number of individual fiber samples and the mass of the second filler in each fiber sample can be determined based on the oil content range of the fiber to be tested. For example, when the oil content range of the fiber to be tested is relatively large, in order to make one set of standards applicable to the testing of oil content of multiple fibers, the number of individual fiber samples in one set of standards can be increased, such as 8. During the process of dripping the second filler into the sample tube, care should be taken to prevent the second filler from touching the sample tube wall.
[0053] Furthermore, the first filler is added to the sample tube containing the second filler, and the mixture is shaken to ensure uniform mixing. The heights of the first and second fillers are selected based on the uniformity region of the applicable NMR equipment. In this embodiment, the first preset value is 10-100 mm.
[0054] S2: Place the first sealing unit into the sample tube and make contact with the first filler and the second filler, and extract the second preset atmospheric pressure.
[0055] Specifically, after the first sealing unit is placed into the sample tube and comes into contact with the uniformly mixed first and second fillers, a second preset atmospheric pressure is drawn. By drawing the second preset atmospheric pressure, air in the second containment space can be removed, which can slow down the oxidation of the fillers and provide insulation, resulting in better stability of the prepared fiber standard sample. In this embodiment, the second preset value is 0.3-0.5, and the time for drawing 0.3-0.5 atmospheres is 3-8 minutes. Preferably, the time for drawing 0.3-0.5 atmospheres is 5 minutes.
[0056] S3: Place the second sealing unit into the sample tube and connect it to the first sealing unit, and seal the sealing cap in the second sealing unit and the sample tube by adhesive sealing.
[0057] Specifically, the third column in the second sealing unit is screwed into the mounting hole on the second column in the first sealing unit via an internal thread towards the first receiving space. Next, the sealing cap in the second sealing unit is fitted onto one end of the sample tube opening, and the sample tube is sealed using adhesive to prevent air from the environment from entering the fiber standard and affecting its stability.
[0058] In one specific implementation, photosensitive adhesive is used to seal the sealing cap and the sample tube. The photosensitive adhesive has a fast bonding speed and the bonding process is easy to control. The photosensitive adhesive is cured by uniformly irradiating with a UV lamp for 5-20 minutes.
[0059] The embodiments of the present invention will be described in more detail below through examples. However, the embodiments of the present invention are not limited to these examples.
[0060] Example 1
[0061] This application provides a method for preparing an oil content standard sample of nuclear magnetic resonance fiber, comprising the following steps:
[0062] 1. Take 8 sample tubes and drop different masses of silicone oil with a kinematic viscosity of 50 cst into each of the 8 sample tubes. During the process of adding silicone oil to the sample tubes, the silicone oil should not touch the tube wall. The mass of silicone oil is shown in Table 1.
[0063] Table 1 Mass of silicone oil in fiber standard samples
[0064] Fiber standard sample number 0 1 2 3 4 5 6 7 silicone oil mass / mg 0 2.0 4.0 8.0 16.0 32.0 64.0 128.0
[0065] Note: Fiber standard No. 0 is used to test the substrate signal of NMR equipment.
[0066] 2. Fill each sample tube with silica particles with a diameter of 0.4-0.6 mm, shake to mix the silica and silicone oil evenly, and the height of silica and silicone oil after mixing should be 4 cm.
[0067] 3. Place the first sealing unit into the sample tube and bring it into contact with the well-mixed silica and silicone oil, and draw 0.3-0.4 atmospheres of pressure.
[0068] 4. Place the second sealing unit into the sample tube and connect it to the first sealing unit. Seal the sealing cap in the second sealing unit and the sample tube using an adhesive sealing method.
[0069] The uniformity, oil content stability, and temperature stability of the NMR fiber standard sample provided in Example 1 were tested.
[0070] 1. Uniformity test
[0071] Due to surface relaxation, the relaxation time of non-uniform samples (i.e., silicone oil is not uniformly distributed in silica) is relatively longer than that of uniform samples (i.e., silicone oil is uniformly distributed in silica). At the same echo time, the silicone oil mass and the corresponding NMR signal in the standard sample are unlikely to show a linear relationship. Therefore, the uniformity of silicone oil distribution in the standard sample can be determined by the linear relationship between the silicone oil mass and the corresponding NMR signal. Table 2 shows the NMR signal of the fiber standard sample with an echo time of 10.0 ms; Table 3 shows the NMR signal of the fiber standard sample with an echo time of 2.5 ms. Figure 6 The calibration curve is shown for the relationship between the silicone oil mass and the corresponding nuclear magnetic resonance signal in the fiber standard when the echo time is 10.0 ms. Figure 7 This is a calibration curve showing the relationship between the silicone oil mass and the corresponding NMR signal in the fiber standard at an echo time of 2.5 ms. Figure 6 and Figure 7As shown, the correlation coefficients of the calibration curves are both greater than 0.999 when the echo times are 2.5ms and 10ms, indicating that the fiber standard prepared in this application has good uniformity.
[0072] Table 2. Nuclear magnetic resonance signals of fiber standards with an echo time of 10.0 ms.
[0073] Fiber standard sample number Nuclear magnetic resonance signal 1 161 2 276 3 635 4 1406 5 2832 6 5716 7 11830
[0074] Table 3. Nuclear magnetic resonance signals of fiber standards with an echo time of 2.5 ms.
[0075] Fiber standard sample number Nuclear magnetic resonance signal 1 366 2 521 3 934 4 1703 5 3367 6 6582 7 12975
[0076] 2. Oil content stability test
[0077] Oil content stability tests were conducted on fiber standard samples No. 2, 5, and 7 prepared in Example 1, with samples taken every 5 days. The test results are shown in Table 4. As can be seen from Table 4, there is no significant trend in the oil content stability of the fiber standard samples prepared in this application, indicating that the oil content stability of the fiber standard samples prepared in this application is superior.
[0078] Table 4 Results of oil content stability test of fiber standard samples
[0079]
[0080] 3. Temperature stability test
[0081] Fiber samples No. 2, 6, and 7 were selected for temperature stability testing. Tests were conducted on fiber samples No. 2, 6, and 7 at different storage temperatures, with parallel samples used for each temperature test. The storage temperatures for the fiber samples were 5℃, 10℃, 40℃, and 45℃, and the storage time for the fiber samples at each temperature was 20 days. Fiber samples stored at the above temperatures were tested every 5 days. The test results are shown in Tables 5, 6, and 7. As can be seen from the tests in Tables 5, 6, and 7, there was no significant trend in the temperature stability of the fiber samples stored at different temperatures, indicating that the fiber samples prepared in this application have superior temperature stability.
[0082] Table 5. Temperature stability test results of fiber standard sample No. 2
[0083]
[0084]
[0085] Table 6. Temperature stability test results of fiber standard sample No. 6
[0086]
[0087] Table 7. Temperature stability test results of fiber standard sample No. 7
[0088]
[0089] The above provides a detailed description of the NMR fiber oil content standard and its preparation method. Specific examples have been used to illustrate the principles and implementation methods of this application. The descriptions of these embodiments are merely for the purpose of helping to understand the method and core ideas of this application. Furthermore, those skilled in the art will recognize that modifications may be made to the specific implementation methods and application scope based on the ideas of this application. Therefore, the content of this specification should not be construed as a limitation of this application.
[0090] In the description of this application, it should be understood that the terms "vertical," "parallel," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," and "outer," etc., indicating orientation or positional relationships based on the orientation or positional relationships shown in the accompanying drawings, are used only for the convenience of describing this application and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation, and therefore should not be construed as a limitation on this application. Furthermore, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of indicated technical features. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of this application, unless otherwise stated, "a plurality of" means two or more.
[0091] In the description of this application, it should be noted that, unless otherwise expressly specified and limited, the terms "installation," "connection," and "linking" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; and they can refer to the internal connection between two components. Those skilled in the art can understand the specific meaning of the above terms in this application based on the specific circumstances.
[0092] The above description is only a preferred embodiment of this application and is not intended to limit this application. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of this application should be included within the protection scope of this application.
Claims
1. A standard sample for the oil content of nuclear magnetic resonance fibers, characterized in that, The standard sample includes: a sample tube, a sealing assembly, and a filler; The sample tube is a cylindrical structure with one end open. The material of the sample tube is a material that does not contain hydrogen. The sealing component is disposed in the sample tube and forms a first receiving space with the sample tube. The filler is disposed in the first receiving space. The sealing assembly includes a first sealing unit and a second sealing unit, which are fixedly connected. The first sealing unit is disposed at one end close to the first accommodating space, and the second sealing unit is disposed at one end away from the first accommodating space. The first sealing unit includes a sealing sheet, a first column connected to the sealing sheet, and a second column connected to the first column. The diameter of the sealing sheet is larger than the inner diameter of the sample tube. The sealing sheet is disposed in the sample tube by an interference fit and abuts against the filler. The diameter of the first column is smaller than the inner diameter of the sample tube, and the diameter of the second column is equal to the inner diameter of the sample tube. The sealing sheet, the first column, the second column, and the sample tube form a second accommodating space. The first sealing unit is provided with a through hole, which communicates with the first accommodating space; The second column is provided with a mounting hole, and the mounting hole is provided with an internal thread. The second sealing unit includes a third column, a fourth column connected to the third column, and a sealing cap. The third column is provided with an external thread that matches the internal thread. The third column can move along a preset direction through the internal thread provided in the mounting hole. The sealing cap is sleeved on one end of the sample tube opening, and the sealing cap seals the sample tube by adhesive sealing. The filler includes a first filler and a second filler. The first filler is a solid material without hydrogen with a particle size of 0.2-1.0 mm, and the second filler is a liquid material containing hydrogen. The kinematic viscosity of the second filler is <100 cst, and the T2 relaxation time of the second filler is less than 1000 ms.
2. The nuclear magnetic resonance fiber oil content standard sample according to claim 1, characterized in that, The first filler includes one of silica, fluorinated ethylene propylene copolymer, and polytetrafluoroethylene; And / or, The second filler includes one of the following: copper sulfate aqueous solution, manganese chloride aqueous solution, natural oils, silicone oil, and polyether.
3. The nuclear magnetic resonance fiber oil content standard sample according to claim 1, characterized in that, The first sealing unit, the third column, and the fourth column are made of materials that do not contain hydrogen.
4. The nuclear magnetic resonance fiber oil content standard sample according to claim 3, characterized in that, The materials of the first sealing unit, the third column, and the fourth column include polytetrafluoroethylene.
5. A method for preparing an oil content standard sample of nuclear magnetic resonance fiber as described in any one of claims 1 to 4, characterized in that, The preparation method includes: The second filler and the first filler are placed into the sample tube in sequence and mixed evenly. The height of the mixture of the first filler and the second filler is the first preset value. The first sealing unit is placed into the sample tube and comes into contact with the first filler and the second filler, and the second preset atmospheric pressure is extracted; The second sealing unit is placed into the sample tube and connected to the first sealing unit. The sealing cap in the second sealing unit and the sample tube are sealed by adhesive sealing.