A method and apparatus for determining the relative molecular mass and distribution of resins
Patent Information
- Application Number
- CN202310251096.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-03-10
- Publication Date
- 2026-08-21
- Estimated Expiration
- 2043-03-10
AI Technical Summary
[0003]然而,目前国内测定树脂相对分子质量的方法存在一些漏洞,比如考马斯亮蓝法、凯氏定氮法等方法,由于每一批样品染色程度的差异,会对实验结果有一定的影响,而现有的单一凝胶过滤色谱法,分辨率较低,也会对实验结果有一定的影响
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Figure CN116448905B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of relative molecular mass determination, and particularly to a method and apparatus for determining the relative molecular mass and distribution of resins. Background Technology
[0002] Currently, with the widespread use of resin products globally, people have increasingly higher requirements for resins. Resins with different relative molecular masses can be used to produce different products. Therefore, the accuracy of measuring the relative molecular mass of resins is also becoming increasingly important.
[0003] However, current methods for determining the relative molecular mass of resins in China have some shortcomings. For example, methods such as the Coomassie brilliant blue method and the Kjeldahl nitrogen determination method can affect the experimental results due to differences in the degree of staining of each batch of samples. The existing single gel filtration chromatography method has low resolution, which can also affect the experimental results.
[0004] Therefore, the present invention provides a method and apparatus for determining the relative molecular mass and distribution of resins. Summary of the Invention
[0005] This invention provides a method and apparatus for determining the relative molecular mass and distribution of resins. By randomly grouping resin samples and using a gel chromatography instrument and a concentration detector for detection, the detected resin sample data can be more accurate, resulting in a more precise relative molecular mass of the resin and a more accurate molecular mass distribution.
[0006] This invention provides a method for determining the relative molecular mass and distribution of a resin, comprising: Step 1: Place the resin collector at the target location to obtain the target resin sample; Step 2: Perform two-group detection on the target resin sample using gel chromatography to obtain the first resin elution time and the second resin elution time, and obtain the first concentration change value and the second concentration change value of the two groups of samples with the help of a concentration detector; Step 3: Obtain the average rinsing time of the first resin based on the first resin rinsing time and the second resin rinsing time; obtain the average concentration change value of the first resin based on the first concentration change value and the second concentration change value. Step 4: Obtain standard resin samples and perform analysis using gel permeation chromatography to obtain the standard resin elution time; Step 5: Based on the standard resin rinsing time, obtain the standard curves corresponding to different resin molecular weights. Process the average rinsing time of the first resin and compare it with the standard curves to obtain the relative molecular mass of the target resin. Combine the change value of the average concentration of the first resin to obtain the molecular mass distribution of the target resin.
[0007] In one possible implementation, a resin collector is placed at a corresponding location on the target tree to obtain a target resin sample, including: Step 11: Place the resin collector at the target location and collect the raw resin liquid from the target within a preset time. Step 12: Add the original resin solution to a preset solvent and stir and dissolve it thoroughly to obtain the treated resin solution; Step 13: Based on the fusion of the treated resin liquid and the buffer solution, and the mixture is shaken on a shaker, the target resin sample is obtained.
[0008] In one possible implementation, the target resin sample is subjected to two-group detection based on gel chromatography to obtain the first resin elution time and the second resin elution time, and the first concentration change value and the second concentration change value of the two groups of samples are obtained with the assistance of a concentration detector, including: Step 21: Divide the obtained target resin sample into several small samples, and randomly group the small samples to obtain two groups of resin test samples. Then, detect the two groups of resin test samples based on gel chromatography. Step 22: Based on the detection results, the first resin rinsing time and the second resin rinsing time of different components in the two groups of resin test samples on the separation column are obtained respectively. Step 23: While the gel chromatography instrument is performing the detection, the concentration of the separation column of the gel chromatography instrument is detected in real time based on the concentration detector, so as to obtain the first concentration change value and the second concentration change value corresponding to the two sets of resin test samples.
[0009] In one possible implementation, the average rinsing time of the first resin is obtained based on the first resin rinsing time and the second resin rinsing time, including: Step 31: Based on the obtained first resin rinsing time and second resin rinsing time, generate corresponding first rinsing time curves and second rinsing time curves, and perform overlapping processing on the corresponding identical components in the first rinsing time curves and second rinsing time curves. If the overlap of the same segment of the broken line is higher than the preset overlap, calculate the first average rinsing time of the first rinsing time and the second rinsing time under the corresponding segment of the broken line. Conversely, the two sets of samples were retested to obtain new first resin rinsing times and second resin rinsing times.
[0010] In one possible implementation, a standard resin sample is obtained and analyzed using gel permeation chromatography to determine the standard resin elution time, including: Step 41: Obtain several standard resin samples with different molecular weights, and perform detection on each standard resin sample based on gel permeation chromatography; Step 42: Based on the detection results, obtain the standard resin rinsing time of several standard resin samples on the separation column.
[0011] In one possible implementation, a standard curve corresponding to different resin molecular weights is obtained based on the standard resin rinsing time. The average rinsing time of the first resin is processed and compared with the standard curve to obtain the relative molecular mass of the target resin, including: Step 51: Construct a standard curve for the standard resin rinsing time of each standard resin sample; The horizontal axis of the standard broken line represents the components of the standard resin sample, and the vertical axis represents the elution time of different components in the standard resin sample on the separation column. Step 52: Obtain the first fold line corresponding to the target resin sample based on the average rinsing time of the first resin, and compare the first fold line with each standard fold line one by one; ; ; Where T1 is the point comparison result between the first polyline and the corresponding standard polyline; For the first standard broken line The rinsing time corresponding to each point; The first broken line The rinsing time corresponding to each point; 1 is the recording error coefficient in the process of determining the rinsing time of the i-th point in the first broken line; T1 represents the allowable difference value in the line comparison process; T2 represents the comparison result between the first line and all the same segment lines corresponding to the adjacent components in the corresponding standard line. For the first standard broken line The rinsing time corresponding to each broken line segment; The first broken line The rinsing time corresponding to each broken line segment; 2. To determine the first broken line in the first broken line The error coefficient recorded during the rinsing time corresponding to each polyline segment, where m represents the number of points in the first polyline; m-1 represents the number of polyline segments in the first polyline. Sort the comparison results of all points for the same first polyline by size to obtain the first comparison sequence. At the same time, sort the comparison results of all segments for the same first polyline by size to obtain the second comparison column. The first comparison sequence is truncated according to a preset range of points, and the second comparison sequence is truncated according to a preset range of segments. Determine whether the same standard resin exists in the first and second cutting results; If there exists, and there is only one identical standard resin, then the relative molecular mass of the target resin is obtained based on the identical standard resin. If there exists, and there is more than one identical standard resin, then the reference value of the corresponding identical standard resin can be obtained based on the point comparison results and segment comparison results of each identical standard resin. Based on the reference value and the relative molecular mass of the corresponding standard resin, the weighted average of the relative molecular mass is obtained to obtain the relative molecular mass of the target resin. If it does not exist, the first standard resin corresponding to the first minimum value is obtained from the first cutting result and the second standard resin corresponding to the second minimum value is obtained from the second cutting result, as reference resins for the target resin.
[0012] In one possible implementation, the molecular weight distribution of the target resin is obtained by combining the change in the average concentration of the first resin, including: Step 01: Based on the comparison results of the first broken line, obtain the relative molecular mass of the target resin and determine the relative molecular mass of different components in the target resin; Step 02: Correspond one by one to the relative molecular mass of the different components and the average concentration change of the first resin; Step 03: Based on the corresponding results, determine the molecular concentration of the components corresponding to different relative molecular masses in the target resin, thereby obtaining the molecular mass distribution of the target resin.
[0013] This invention provides an apparatus for determining the relative molecular mass and distribution of a resin, comprising: Sample acquisition unit: Places the resin collector at the target location to obtain the target resin sample; Processing and detection unit: Based on gel chromatography, the target resin sample is divided into two groups for detection to obtain the first resin elution time and the second resin elution time. Based on the concentration detector, the first concentration change value and the second concentration change value of the two groups of samples are obtained. Data processing unit: Obtains the average rinsing time of the first resin based on the first resin rinsing time and the second resin rinsing time; Obtains the average concentration change value of the first resin based on the first concentration change value and the second concentration change value. Standard determination unit: Obtain standard resin samples and perform analysis using gel chromatography to obtain the standard resin elution time; Comparative analysis unit: Based on the standard resin rinsing time, standard curves corresponding to different resin molecular weights are obtained. The average rinsing time of the first resin is processed and compared with the standard curves to obtain the relative molecular mass of the target resin. Combined with the change value of the average concentration of the first resin, the molecular mass distribution of the target resin is obtained.
[0014] Other features and advantages of the present invention will be set forth in the following description, and will be apparent in part from the description, or may be learned by practicing the invention. The technical solutions of the present invention will now be described in further detail with reference to the accompanying drawings and embodiments. Attached Figure Description
[0015] The accompanying drawings are provided to further illustrate the invention and form part of the specification. They are used in conjunction with embodiments of the invention to explain the invention and do not constitute a limitation thereof. In the drawings: Figure 1 This is a flowchart illustrating a method for determining the relative molecular mass and distribution of a resin according to an embodiment of the present invention. Figure 2 This is another flowchart of a method for determining the relative molecular mass and distribution of resin according to an embodiment of the present invention; Figure 3 This is a structural diagram of an apparatus for determining the relative molecular mass and distribution of resin according to an embodiment of the present invention. Detailed Implementation
[0016] The preferred embodiments of the present invention will be described below with reference to the accompanying drawings. It should be understood that the preferred embodiments described herein are for illustration and explanation only and are not intended to limit the present invention.
[0017] Example 1: This invention provides a method for determining the relative molecular mass and distribution of a resin, such as... Figure 1 As shown, it includes: Step 1: Place the resin collector at the target location to obtain the target resin sample; Step 2: Perform two-group detection on the target resin sample using gel chromatography to obtain the first resin elution time and the second resin elution time, and obtain the first concentration change value and the second concentration change value of the two groups of samples with the help of a concentration detector; Step 3: Obtain the average rinsing time of the first resin based on the first resin rinsing time and the second resin rinsing time; obtain the average concentration change value of the first resin based on the first concentration change value and the second concentration change value. Step 4: Obtain standard resin samples and perform analysis using gel permeation chromatography to obtain the standard resin elution time; Step 5: Based on the standard resin rinsing time, obtain the standard curves corresponding to different resin molecular weights. Process the average rinsing time of the first resin and compare it with the standard curves to obtain the relative molecular mass of the target resin. Combine the change value of the average concentration of the first resin to obtain the molecular mass distribution of the target resin.
[0018] In this embodiment, the resin collector is a container used to collect resin from trees in a forest. It can be made at home or a professional collector can be purchased.
[0019] In this embodiment, the target location refers to a suitable location on the target tree for resin collection. For example, for the convenience of the experiment, the location where the tree is about half a person's height can be used as the target location.
[0020] In this embodiment, the target resin sample refers to the original resin liquid obtained by treating it with a preset solvent and then fusing it with a buffer solution.
[0021] In this embodiment, the binary group detection involves randomly dividing the obtained target value sample into two groups for detection.
[0022] In this embodiment, the first resin elution time and the second resin elution time refer to the elution time of the current sample obtained by flowing the target resin sample into the separation column of the gel chromatography instrument and then using different elution times for molecules of different sizes.
[0023] In this embodiment, the first concentration change value and the second concentration change value refer to the concentration change values of the target sample detected in real time by the concentration detector during the operation of the gel chromatography instrument.
[0024] In this embodiment, the first average rinsing time of the resin refers to the average rinsing time of the resin obtained by the first rinsing time and the second rinsing time, and the overlapping of the two lines. If the overlap between the two lines is higher than the preset overlap, the average rinsing time of the first rinsing time and the second rinsing time is obtained.
[0025] In this embodiment, the first average resin concentration change value refers to the corresponding line obtained based on the first concentration change value and the second concentration change value, and the line is overlapped. If the overlap between the two lines is higher than the preset overlap, the average concentration change corresponding to the first concentration change value and the second concentration change value is obtained, and the first average resin concentration change value is obtained.
[0026] In this embodiment, the standard resin sample refers to a resin sample obtained by processing a standard resin whose molecular weight has been determined.
[0027] In this embodiment, the standard resin elution time refers to the elution time of the standard resin sample in the separation column of the gel chromatography instrument.
[0028] In this embodiment, the resin molecular weight refers to the relative molecular mass of the resin.
[0029] In this embodiment, the standard broken line refers to the broken line obtained based on the standard numerical rinsing time corresponding to the standard resin.
[0030] In this embodiment, the molecular weight distribution of the target resin is determined based on the concentration values corresponding to components with different relative molecular weights in the target resin.
[0031] The beneficial effects of the above technical solution are: by randomly grouping resin samples and using gel chromatography and concentration detector for detection, the detected resin sample data can be more accurate, more precise relative molecular mass of resin can be obtained, and at the same time, a more accurate molecular mass distribution can be obtained.
[0032] Example 2: Based on Example 1, a resin collector is placed at the corresponding position of the target tree to obtain a target resin sample, including: Step 11: Place the resin collector at the target location and collect the raw resin liquid from the target within a preset time. Step 12: Add the original resin solution to a preset solvent and stir and dissolve it thoroughly to obtain the treated resin solution; Step 13: Based on the fusion of the treated resin liquid and the buffer solution, and the mixture is shaken on a shaker, the target resin sample is obtained.
[0033] In this embodiment, the resin collector is a container used to collect resin from trees in a forest. It can be made at home or a professional collector can be purchased.
[0034] In this embodiment, the target location refers to a suitable location on the target tree for resin collection. For example, for the convenience of the experiment, the location where the tree is about half a person's height can be used as the target location.
[0035] In this embodiment, the original resin liquid refers to the resin liquid collected directly through the resin collector. It is generally in a solid, semi-solid, or liquid state, and the collected resin varies depending on the tree species.
[0036] In this embodiment, a preset solvent is used to dilute the high concentration of the original resin solution. For example, alcohols (such as ethanol), esters (such as ethyl acetate and dibutyl phthalate), ketones (such as acetone), solvent gasoline, toluene, etc. can all be used as non-reactive diluents for epoxy resin.
[0037] In this embodiment, processing the resin solution refers to adding the original resin solution into a preset solvent and then dissolving it through thorough stirring to obtain the solution.
[0038] In this embodiment, the buffer solution is used to adjust the pH value of the treated resin solution, so that the treated resin solution can be kept in a relatively neutral solution, which facilitates detection and reduces instrument wear. For example, the buffer solution can be an ammonium acetate buffer solution.
[0039] In this embodiment, the target resin sample refers to the original resin liquid obtained by treating it with a preset solvent and then fusing it with a buffer solution.
[0040] The beneficial effects of the proposed technical solution are: by processing the collected resin liquid, the processed resin sample can be more easily tested, reducing instrument wear and tear, thereby obtaining more accurate resin sample test results.
[0041] Example 3: Based on Example 2, the target resin samples were subjected to two-group detection using gel chromatography to obtain the first resin elution time and the second resin elution time. Furthermore, the first and second concentration changes of the two groups of samples were obtained with the assistance of a concentration detector. Figure 2 As shown, it includes: Step 21: Divide the obtained target resin sample into several small samples, and randomly group the small samples to obtain two groups of resin test samples. Then, detect the two groups of resin test samples based on gel chromatography. Step 22: Based on the detection results, the first resin rinsing time and the second resin rinsing time of different components in the two groups of resin test samples on the separation column are obtained respectively. Step 23: While the gel chromatography instrument is performing the detection, the concentration of the separation column of the gel chromatography instrument is detected in real time based on the concentration detector, so as to obtain the first concentration change value and the second concentration change value corresponding to the two sets of resin test samples.
[0042] In this embodiment, the target resin sample refers to the original resin liquid obtained by treating it with a preset solvent and then fusing it with a buffer solution.
[0043] In this embodiment, a small sample refers to dividing the obtained target resin sample into several equal parts, with each part being a small sample of the target resin.
[0044] In this embodiment, the resin test sample refers to a resin test sample obtained by randomly dividing several small samples into two groups.
[0045] In this embodiment, the gel chromatography instrument is mainly used for the detection of molecular weight and molecular weight distribution of aqueous and oily polymers, as well as the qualitative and quantitative analysis of sugars, alcohols, fatty acids and lipids. The gel chromatography instrument includes equipment such as gel columns and column ovens.
[0046] In this embodiment, the first resin elution time and the second resin elution time refer to the elution time of the current sample obtained by flowing the target resin sample into the separation column of the gel chromatography instrument and then using different elution times for molecules of different sizes.
[0047] In this embodiment, the concentration detector refers to a detector that can detect the concentration of a solution and obtain real-time concentration changes.
[0048] In this embodiment, the first concentration change value and the second concentration change value refer to the concentration change values of the target sample collected in real time by the concentration detector during the operation of the gel chromatography instrument.
[0049] The beneficial effect of the above technical solution is that by classifying the resin samples and randomly dividing them into two groups for testing, the test results can be more accurate, thereby obtaining a more precise relative molecular mass of the resin.
[0050] Example 4: Based on Example 3, the average rinsing time of the first resin is obtained based on the first resin rinsing time and the second resin rinsing time, including: Step 31: Based on the obtained first resin rinsing time and second resin rinsing time, generate corresponding first rinsing time curves and second rinsing time curves, and perform overlapping processing on the corresponding identical components in the first rinsing time curves and second rinsing time curves. If the overlap of the same segment of the broken line is higher than the preset overlap, calculate the first average rinsing time of the first rinsing time and the second rinsing time under the corresponding segment of the broken line. Conversely, the two sets of samples were retested to obtain new first resin rinsing times and second resin rinsing times.
[0051] In this embodiment, the first resin elution time and the second resin elution time refer to the elution time of the current sample obtained by flowing the target resin sample into the separation column of the gel chromatography instrument and then using different elution times for molecules of different sizes.
[0052] In this embodiment, the first elution time curve and the second elution time curve are obtained by sorting and connecting the first resin elution time and the second resin elution time of the target resin in a preset order. The vertical axis of the first elution time curve and the second elution time curve represent the components of the resin sample, and the horizontal axis represents the elution time of different components in the resin sample on the separation column.
[0053] In this embodiment, "identical components" refers to the same components contained in the test results of the two groups of resin test samples.
[0054] In this embodiment, the preset overlap refers to the minimum overlap value between the first rinsing time line and the second rinsing time line, set based on the differences in the historical line curves.
[0055] In this embodiment, the first average rinsing time of the resin refers to the average rinsing time of the resin obtained by the first rinsing time and the second rinsing time, and the overlapping of the two lines. If the overlap between the two lines is higher than the preset overlap, the average rinsing time of the first rinsing time and the second rinsing time is obtained.
[0056] The beneficial effects of the proposed technical solution are: by separately testing the two groups of resin samples and adjusting based on the test results, the test results can be made more accurate, thereby obtaining a more precise relative molecular mass of the resin and simultaneously obtaining a more accurate molecular mass distribution.
[0057] Example 5: Based on Example 4, standard resin samples were obtained and analyzed using gel permeation chromatography to determine the standard resin elution time, including: Step 41: Obtain several standard resin samples with different molecular weights, and perform detection on each standard resin sample based on gel permeation chromatography; Step 42: Based on the detection results, obtain the standard resin rinsing time of several standard resin samples on the separation column.
[0058] In this embodiment, the standard resin sample refers to a resin sample obtained by processing a standard resin whose molecular weight has been determined.
[0059] In this embodiment, the gel chromatography instrument is mainly used for the detection of molecular weight and molecular weight distribution of aqueous and oily polymers, as well as the qualitative and quantitative analysis of sugars, alcohols, fatty acids and lipids. The gel chromatography instrument includes equipment such as gel columns and column ovens.
[0060] In this embodiment, the standard resin elution time refers to the elution time of the standard resin sample in the separation column of the gel chromatography instrument.
[0061] The beneficial effect of the above technical solution is that by testing the standard resin sample, the rinsing time of the standard resin is obtained, and then compared with the rinsing time of the target resin sample, the relative molecular mass can be obtained more accurately.
[0062] Example 6: Based on Example 5, standard curves corresponding to different resin molecular weights were obtained based on the standard resin rinsing time. The average rinsing time of the first resin was processed and compared with the standard curves to obtain the relative molecular mass of the target resin, including: Step 51: Construct a standard curve for the standard resin rinsing time of each standard resin sample; The horizontal axis of the standard broken line represents the components of the standard resin sample, and the vertical axis represents the elution time of different components in the standard resin sample on the separation column. Step 52: Obtain the first fold line corresponding to the target resin sample based on the average rinsing time of the first resin, and compare the first fold line with each standard fold line one by one; ; ; Where T1 is the point comparison result between the first polyline and the corresponding standard polyline; For the first standard broken line The rinsing time corresponding to each point; The first broken line The rinsing time corresponding to each point; 1 is the recording error coefficient in the process of determining the rinsing time of the i-th point in the first broken line; T1 represents the allowable difference value in the line comparison process; T2 represents the comparison result between the first line and all the same segment lines corresponding to the adjacent components in the corresponding standard line. For the first standard broken line The rinsing time corresponding to each broken line segment; The first broken line The rinsing time corresponding to each broken line segment; 2. To determine the first broken line in the first broken line The error coefficient recorded during the rinsing time corresponding to each polyline segment, where m represents the number of points in the first polyline; m-1 represents the number of polyline segments in the first polyline. Sort the comparison results of all points for the same first polyline by size to obtain the first comparison sequence. At the same time, sort the comparison results of all segments for the same first polyline by size to obtain the second comparison column. The first comparison sequence is truncated according to a preset range of points, and the second comparison sequence is truncated according to a preset range of segments. Determine whether the same standard resin exists in the first and second cutting results; If there exists, and there is only one identical standard resin, then the relative molecular mass of the target resin is obtained based on the identical standard resin. If there exists, and there is more than one identical standard resin, then the reference value of the corresponding identical standard resin can be obtained based on the point comparison results and segment comparison results of each identical standard resin. Based on the reference value and the relative molecular mass of the corresponding standard resin, the weighted average of the relative molecular mass is obtained to obtain the relative molecular mass of the target resin. If it does not exist, the first standard resin corresponding to the first minimum value is obtained from the first cutting result and the second standard resin corresponding to the second minimum value is obtained from the second cutting result, as reference resins for the target resin.
[0063] In this embodiment, the standard resin sample refers to a resin sample obtained by processing a standard resin whose molecular weight has been determined.
[0064] In this embodiment, the standard resin elution time refers to the elution time of the standard resin sample in the separation column of the gel chromatography instrument.
[0065] In this embodiment, the standard broken line refers to the corresponding broken line obtained based on the standard resin rinsing time.
[0066] In this embodiment, the vertical axis of the standard broken line represents the components of the standard resin sample, and the horizontal axis represents the rinsing time of different components in the standard resin sample on the separation column.
[0067] In this embodiment, the first broken line refers to the corresponding broken line obtained based on the average elution time of the first resin, wherein the vertical axis of the broken line represents the components of the resin sample, and the horizontal axis represents the elution time of different components in the resin sample on the separation column.
[0068] In this embodiment, the point comparison result refers to the result obtained by comparing the corresponding points on the first broken line and the standard broken line, and the segment comparison result refers to the result obtained by comparing the broken line segments between two corresponding points on the first broken line and the standard broken line.
[0069] In this embodiment, the recording error coefficient refers to the coefficient corresponding to the error between the accurate time of resin sample rinsing and the time collected by the detector.
[0070] In this embodiment, the first comparison sequence refers to the sequence obtained by sorting the comparison results of all points of the same first broken line by size, and the second comparison sequence refers to the sequence obtained by sorting the comparison results of all segments of the same first broken line by size.
[0071] In this embodiment, the first selection is to filter the first comparison sequence according to the preset range of points to obtain partial data that meets the preset range of points, and the first selection is to filter the second comparison sequence according to the preset range of segments to obtain partial data that meets the preset range of segments.
[0072] In this embodiment, the reference value of the standard resin refers to the reference value of the target resin to the relative molecular mass of standard resins with different relative molecular masses. For example, if the first and second cutting results contain the same standard resin, and the number of the same standard resin is not less than one, if the point comparison result of standard resin 1 is 0.41 and the segment comparison result is 0.4, the point comparison result of standard resin 2 is 0.32 and the segment comparison result is 0.3, and the point comparison result of standard resin 3 is 0.28 and the segment comparison result is 0.29, then the reference value of standard resin 1 is 0.405, the reference value of standard resin 2 is 0.31, and the reference value of standard resin 3 is 0.285. If the relative molecular mass of standard resin 1 is 12900, the relative molecular mass of standard resin 2 is 13000, and the relative molecular mass of standard resin 3 is 13200, then the relative molecular mass of the target resin obtained based on the reference value of the standard resin is the weighted average of the relative molecular masses, 12899.5.
[0073] In this embodiment, the weighted average value refers to the relative molecular mass value obtained by weighting the reference value of the standard resin with the corresponding relative molecular mass.
[0074] In this embodiment, the reference resin refers to the first standard resin corresponding to the first minimum value obtained from the first cutting result and the second standard resin corresponding to the second minimum value obtained from the second cutting result when there is no identical standard resin in the first cutting result and the second cutting result, which are used as the reference resin for the target resin.
[0075] The beneficial effect of the above technical solution is that by comparing the standard fold line corresponding to the standard resin sample with the first fold line corresponding to the target resin sample, and discussing the comparison results by category, a more accurate relative molecular mass of the target resin can be obtained according to different situations.
[0076] Example 7: Based on Example 6, the molecular weight distribution of the target resin is obtained by combining the average concentration change value of the first resin, including: Step 01: Based on the comparison results of the first broken line, obtain the relative molecular mass of the target resin and determine the relative molecular mass of different components in the target resin; Step 02: Correspond one by one to the relative molecular mass of the different components and the average concentration change of the first resin; Step 03: Based on the corresponding results, determine the molecular concentration of the components corresponding to different relative molecular masses in the target resin, thereby obtaining the molecular mass distribution of the target resin.
[0077] In this embodiment, the first broken line refers to the corresponding broken line obtained based on the average elution time of the first resin, wherein the vertical axis of the broken line represents the components of the resin sample, and the horizontal axis represents the elution time of different components in the resin sample on the separation column.
[0078] In this embodiment, the relative molecular mass of different components in the target resin refers to the relative molecular mass corresponding to different components in the target resin. Because resin is a polymer compound, it will contain several components with different relative molecular masses, such as resin acids, resin alcohols, resin hydrocarbons and some of their higher polymers. These components are mostly diterpenes and triterpenes derivatives, and sometimes lignans.
[0079] In this embodiment, the first average resin concentration change value refers to the corresponding line obtained based on the first concentration change value and the second concentration change value, and the line is overlapped. If the overlap between the two lines is higher than the preset overlap, the average concentration change corresponding to the first concentration change value and the second concentration change value is obtained, and the first average resin concentration change value is obtained.
[0080] In this embodiment, molecular concentration refers to the concentration value corresponding to components with different relative molecular masses in the resin.
[0081] In this embodiment, the distribution of the molecular weight of the target resin refers to determining the content of different components in the resin based on the concentration change value in the target resin, and then determining the distribution of the molecular weight of the target resin by combining the relative molecular weight of each component.
[0082] The beneficial effects of the above technical solution are: real-time detection is performed by a concentration detector, and the concentration of different components in the target resin is obtained based on the detection results, thereby obtaining a more accurate molecular weight distribution.
[0083] Example 8: This invention provides an apparatus for determining the relative molecular mass and distribution of resins, such as... Figure 3 As shown, it includes: Sample acquisition unit: Places the resin collector at the target location to obtain the target resin sample; Processing and detection unit: Based on gel chromatography, the target resin sample is divided into two groups for detection to obtain the first resin elution time and the second resin elution time. Based on the concentration detector, the first concentration change value and the second concentration change value of the two groups of samples are obtained. Data processing unit: Obtains the average rinsing time of the first resin based on the first resin rinsing time and the second resin rinsing time; Obtains the average concentration change value of the first resin based on the first concentration change value and the second concentration change value. Standard determination unit: Obtain standard resin samples and perform analysis using gel chromatography to obtain the standard resin elution time; Comparative analysis unit: Based on the standard resin rinsing time, standard curves corresponding to different resin molecular weights are obtained. The average rinsing time of the first resin is processed and compared with the standard curves to obtain the relative molecular mass of the target resin. Combined with the change value of the average concentration of the first resin, the molecular mass distribution of the target resin is obtained.
[0084] The beneficial effects of the above technical solution are: by randomly grouping resin samples and using gel chromatography and concentration detector for detection, the detected resin sample data can be more accurate, more precise relative molecular mass of resin can be obtained, and at the same time, a more accurate molecular mass distribution can be obtained.
[0085] Obviously, those skilled in the art can make various modifications and variations to this invention without departing from the spirit and scope of this invention.
Claims
1. A method for determining the relative molecular mass and distribution of a resin, characterized in that, include: Step 1: Place the resin collector at the target location to obtain the target resin sample; Step 2: Perform two-group detection on the target resin sample using gel chromatography to obtain the first resin elution time and the second resin elution time, and obtain the first concentration change value and the second concentration change value of the two groups of samples with the help of a concentration detector; Step 3: Obtain the average rinsing time of the first resin based on the first resin rinsing time and the second resin rinsing time; obtain the average concentration change value of the first resin based on the first concentration change value and the second concentration change value. Step 4: Obtain standard resin samples and perform analysis using gel permeation chromatography to obtain the standard resin elution time; Step 51: Construct a standard curve for the standard resin rinsing time of each standard resin sample; The horizontal axis of the standard broken line represents the components of the standard resin sample, and the vertical axis represents the elution time of different components in the standard resin sample on the separation column. Step 52: Obtain the first fold line corresponding to the target resin sample based on the average rinsing time of the first resin, and compare the first fold line with each standard fold line one by one; Where T1 is the point comparison result between the first polyline and the corresponding standard polyline; For the first standard broken line The rinsing time corresponding to each point; The first broken line The rinsing time corresponding to each point; 1 is the recording error coefficient in the process of determining the rinsing time of the i-th point in the first broken line; T1 represents the allowable difference value in the line comparison process; T2 represents the comparison result between the first line and all the same segment lines corresponding to the adjacent components in the corresponding standard line. For the first standard broken line The rinsing time corresponding to each broken line segment; The first broken line The rinsing time corresponding to each broken line segment; 2. To determine the first broken line in the first broken line The error coefficient recorded during the rinsing time corresponding to each polyline segment, where m represents the number of points in the first polyline; m-1 represents the number of polyline segments in the first polyline. Sort the comparison results of all points for the same first polyline by size to obtain the first comparison sequence. At the same time, sort the comparison results of all segments for the same first polyline by size to obtain the second comparison column. The first comparison sequence is truncated according to a preset range of points, and the second comparison sequence is truncated according to a preset range of segments. Determine whether the same standard resin exists in the first and second cutting results; If there exists, and there is only one identical standard resin, then the relative molecular mass of the target resin is obtained based on the identical standard resin. If there exists, and there is more than one identical standard resin, then the reference value of the corresponding identical standard resin can be obtained based on the point comparison results and segment comparison results of each identical standard resin. Based on the reference value and the relative molecular mass of the corresponding standard resin, the weighted average of the relative molecular mass is obtained to obtain the relative molecular mass of the target resin. If it does not exist, the first standard resin corresponding to the first minimum value is obtained from the first cutting result and the second standard resin corresponding to the second minimum value is obtained from the second cutting result, as reference resins for the target resin.
2. The method for determining the relative molecular mass and distribution of a resin as described in claim 1, characterized in that, The resin collector is placed at the corresponding location on the target tree to obtain the target resin sample, including: Step 11: Place the resin collector at the target location and collect the raw resin liquid from the target within a preset time. Step 12: Add the original resin solution to a preset solvent and stir and dissolve it thoroughly to obtain the treated resin solution; Step 13: Based on the fusion of the treated resin liquid and the buffer solution, and the mixture is shaken on a shaker, the target resin sample is obtained.
3. The method for determining the relative molecular mass and distribution of a resin as described in claim 2, characterized in that, Based on gel permeation chromatography, the target resin samples were analyzed in two groups to obtain the elution times of the first and second resins. Furthermore, the first and second concentration changes of the two groups of samples were obtained with the assistance of a concentration detector, including: Step 21: Divide the obtained target resin sample into several small samples, and randomly group the small samples to obtain two groups of resin test samples. Then, detect the two groups of resin test samples based on gel chromatography. Step 22: Based on the detection results, the first resin rinsing time and the second resin rinsing time of different components in the two groups of resin test samples on the separation column are obtained respectively. Step 23: While the gel chromatography instrument is performing the detection, the concentration of the separation column of the gel chromatography instrument is detected in real time based on the concentration detector, so as to obtain the first concentration change value and the second concentration change value corresponding to the two sets of resin test samples.
4. The method for determining the relative molecular mass and distribution of a resin as described in claim 3, characterized in that, The average rinsing time of the first resin is obtained based on the first resin rinsing time and the second resin rinsing time, including: Step 31: Based on the obtained first resin rinsing time and second resin rinsing time, generate corresponding first rinsing time curves and second rinsing time curves, and perform overlapping processing on the corresponding identical components in the first rinsing time curves and second rinsing time curves. If the overlap of the same segment of the broken line is higher than the preset overlap, calculate the first average rinsing time of the first rinsing time and the second rinsing time under the corresponding segment of the broken line. Conversely, the two sets of samples were retested to obtain new first resin rinsing times and second resin rinsing times.
5. The method for determining the relative molecular mass and distribution of a resin as described in claim 4, characterized in that, Obtain standard resin samples and perform analysis using gel permeation chromatography to determine the standard resin elution time, including: Step 41: Obtain several standard resin samples with different molecular weights, and perform detection on each standard resin sample based on gel permeation chromatography; Step 42: Based on the detection results, obtain the standard resin rinsing time of several standard resin samples on the separation column.
6. The method for determining the relative molecular mass and distribution of a resin as described in claim 1, characterized in that, The molecular weight distribution of the target resin is obtained by combining the change in the average concentration of the first resin, including: Step 01: Based on the comparison results of the first broken line, obtain the relative molecular mass of the target resin and determine the relative molecular mass of different components in the target resin; Step 02: Correspond one by one to the relative molecular mass of the different components and the average concentration change of the first resin; Step 03: Based on the corresponding results, determine the molecular concentration of the components corresponding to different relative molecular masses in the target resin, thereby obtaining the molecular mass distribution of the target resin.
7. An apparatus for determining the relative molecular mass and distribution of a resin, characterized in that, include: Sample acquisition unit: Places the resin collector at the target location to obtain the target resin sample; Processing and detection unit: Based on gel chromatography, the target resin sample is divided into two groups for detection to obtain the first resin elution time and the second resin elution time. Based on the concentration detector, the first concentration change value and the second concentration change value of the two groups of samples are obtained. Data processing unit: Obtains the average rinsing time of the first resin based on the first resin rinsing time and the second resin rinsing time; Obtains the average concentration change value of the first resin based on the first concentration change value and the second concentration change value. Standard determination unit: Obtain standard resin samples and perform analysis using gel chromatography to obtain the standard resin elution time; Comparative analysis unit: Based on the standard resin rinsing time, standard curves corresponding to different resin molecular weights are obtained. The average rinsing time of the first resin is processed and compared with the standard curves to obtain the relative molecular mass of the target resin. Combined with the change value of the average concentration of the first resin, the molecular mass distribution of the target resin is obtained.
Citation Information
Patent Citations
Qualitative and quantitative method for analyzing macromolecular carbohydrate
CN114441684A