Quantitative testing method of total organic carbon content of micron-sized powder material

Abstract

The application provides a quantitative testing method for total organic carbon content of a micron-sized powder material, which comprises the following steps: providing the micron-sized powder material with a preset mass M; mixing the micron-sized powder material with distilled water to obtain a solid-liquid mixture; heating the solid-liquid mixture and the distilled water as a blank control group to a preset temperature, so that the first material is dissolved in the distilled water; filtering and concentrating the solid-liquid mixture to obtain a test solution; detecting the total organic carbon content of the test solution and the distilled water as a blank control group to obtain a first total organic carbon content N1 of the test solution and a second total organic carbon content N0 of the distilled water; and determining the total organic carbon content of the micron-sized powder material. The testing method is safe and simple in operation steps, and the raw materials and equipment used are easy to obtain. The interference of other substances in the micron-sized powder material is excluded, and the total organic carbon content in the micron-sized powder material can be quantitatively tested more clearly.

Description

Technical Field

[0001] This invention relates to the field of testing total organic carbon (TOC, unit: mg / L), and more specifically, to a quantitative testing method for the total organic carbon content of micron-sized powder materials. Background Technology

[0002] Total carbon refers to the total content of organic carbon, inorganic carbon, and elemental carbon present in water. Total organic carbon refers to the carbon content of dissolved or suspended organic matter in water (usually expressed as mass concentration), and is a comprehensive indicator that represents the total amount of organic matter in water. Inorganic carbon refers to the carbon content of elemental carbon, carbon dioxide, carbon monoxide, carbides, cyanates, cyanide, and thiocyanate present in water.

[0003] With the increasing demand for lightweight, stress-resistance, and interlaminar toughness in high-end carbon fiber applications such as aerospace, carbon fiber reinforced composites are widely used in manufacturing fields that require tensile and compressive stresses, such as aircraft structural components, wind turbine blades, and turbines, due to their excellent strength and impact resistance. A micron-sized powder material is being used as a toughening material to improve the structural components' resistance to high-temperature and high-humidity environments and their stress impact resistance outside the carbon fiber alignment direction. This material is being applied in the manufacturing of high-end carbon fiber and its products, including in aerospace applications.

[0004] The surfactants used in the preparation of this type of micron-sized powder material are the main contributors and primary source of organic carbon in the toughening material. Surfactants are substances that, when added in small amounts, can significantly alter the interfacial state of a solution system. In the preparation of micron-sized powder materials, surfactants play a role in dispersing, blocking, and protecting, effectively preventing the agglomeration of this type of powder material in the early stages of molding.

[0005] Faced with the reality that domestic research on composite materials for high-end fields such as aerospace is lagging behind and the ability to independently formulate materials is poor, there is currently no systematic, clear and mature method for the qualitative and quantitative characterization of total organic carbon in micron-sized powder materials mainly composed of polyethersulfone, polyurethane, polyamide, polyimide and polycarbonate. This restricts the rapid development of my country's carbon fiber industry and composite materials such as prepregs.

[0006] Therefore, it is of great significance to propose a quantitative test method for the total organic carbon content of micron-sized powder materials that is simple to operate and provides accurate test results. Summary of the Invention

[0007] The purpose of this invention is to overcome the above-mentioned deficiencies in the prior art and to provide a quantitative test method for the total organic carbon content of micron-sized powder materials.

[0008] To achieve the above objectives, the present invention adopts the following technical solution:

[0009] This invention provides a method for quantitatively testing the total organic carbon content of micron-sized powder materials, comprising the following steps:

[0010] Provide a micron-sized powder material of a predetermined mass M, the micron-sized powder material comprising a first material that is soluble in water and a second material that is insoluble in water;

[0011] Micron-sized powder material is mixed with distilled water in a first container to obtain a solid-liquid mixture of a first preset volume; the first container containing the solid-liquid mixture and the second container containing the first preset volume of distilled water are heated to a preset temperature so that the first material dissolves in the distilled water;

[0012] The solid-liquid mixture in the first container is filtered and concentrated to obtain a test solution of a second preset volume V.

[0013] The total organic carbon content of the test solution and the distilled water in the second container was detected to obtain the first total organic carbon content N1 of the test solution and the second total organic carbon content N0 of the distilled water in the second container.

[0014] The total organic carbon content of the micron-sized powder material is determined based on the preset mass M, the second preset volume V, the first total organic carbon content N1, and the second total organic carbon content N0.

[0015] The first material in the micron-sized powder material includes polyvinyl alcohol, and the second material includes one or more of polyethersulfone, polyurethane, polyamide, polyimide and polycarbonate.

[0016] A solid-liquid mixture of micron-sized powder material and distilled water is mixed in a first container to obtain a first predetermined volume of solid-liquid mixture, comprising:

[0017] Micron-sized powder material and distilled water are placed in the first container;

[0018] The first container is subjected to ultrasonic oscillation for a first preset duration to obtain a solid-liquid mixture.

[0019] The first preset duration is 20-40 mins, and the frequency of ultrasonic oscillation is 50-80 Hz.

[0020] Heating a first container containing a solid-liquid mixture and a second container containing a first preset volume of distilled water to a preset temperature includes:

[0021] A first condenser is installed at the opening of the first container, and a second condenser is installed at the opening of the second container;

[0022] The first container and the second container are heated, and the water vapor evaporated in the first container is condensed and refluxed through the first condenser, and the water vapor evaporated in the second container is condensed and refluxed through the second condenser.

[0023] The heating time for the first and second containers is 2 to 3 hours.

[0024] The solid-liquid mixture in the first container is filtered and concentrated, including:

[0025] The solid-liquid mixture of the first material in a dissolved state is filtered through a filtration device, and the resulting filtrate is used to form a test solution.

[0026] Filtering and concentrating the solid-liquid mixture in the first container also includes:

[0027] The first container and the filter device are cleaned with distilled water to obtain a first cleaning solution;

[0028] The first cleaning solution is mixed with the filtrate to obtain a mixed solution;

[0029] The mixed solution is heated and concentrated to a second preset volume V to obtain the test solution.

[0030] The mixed solution is heated and concentrated to a second preset volume to obtain a test solution, comprising:

[0031] The mixed solution was added to a rotary evaporator for rotary evaporation to obtain the first concentrated solution;

[0032] The rotary evaporator after rotary evaporation was cleaned with distilled water to obtain a second cleaning solution;

[0033] The first concentrate and the second cleaning solution are mixed and distilled water is added to a second preset volume V to obtain the test solution.

[0034] Based on the preset mass M, the second preset volume V, the first total organic carbon content N1, and the second total organic carbon content N0, the total organic carbon content of the micron-sized powder material is determined, including:

[0035] The total organic carbon content of micron-sized powder materials is calculated using the following formula:

[0036] TOC = (N1 - N0) * V / (1000 * M);

[0037] Wherein, TOC (mg / L) represents the total organic carbon content; N1 (mg / L) represents the total organic carbon content of the test solution; N0 (mg / L) represents the total organic carbon content of the distilled water in the second container; V (ml) represents the volume of the test solution; 1000 represents the conversion value between ml and L; and M (g) represents the mass of the micron-sized powder material.

[0038] The present invention provides a method for quantitatively testing the total organic carbon content of micron-sized powder materials. The method involves providing a preset mass of micron-sized powder material, mixing the powder material with distilled water to obtain a solid-liquid mixture, heating the solid-liquid mixture and distilled water (as a blank control group) to a preset temperature to dissolve the powder material in the water, filtering and concentrating the mixture to obtain a test solution, and detecting the total organic carbon content of the test solution and the distilled water to obtain a first total organic carbon content and a second total organic carbon content of the distilled water. The total organic carbon content of the micron-sized powder material is determined based on these two values. This testing method is safe and simple to operate, uses readily available raw materials and equipment, eliminates interference from other substances in the micron-sized powder material, and can accurately quantify the total organic carbon content in the micron-sized powder material. Attached Figure Description

[0039] To more clearly illustrate the technical solutions in the embodiments of the present invention, the accompanying drawings used in the description of the embodiments will be briefly introduced below. Obviously, the accompanying drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0040] Figure 1 This is a schematic diagram of a quantitative testing method for the total organic carbon content of micron-sized powder materials, which is an exemplary embodiment of the present invention.

[0041] Figure 2 This is a schematic diagram illustrating an exemplary embodiment of the present invention, showing the process of mixing micron-sized powder material with distilled water in a first container to obtain a solid-liquid mixture of a first preset volume.

[0042] Figure 3 This is a schematic diagram illustrating a process of heating a first container containing a solid-liquid mixture and a second container containing a first preset volume of distilled water to a preset temperature, as an exemplary embodiment of the present invention.

[0043] Figure 4 This is a schematic diagram illustrating the process of filtering and concentrating a solid-liquid mixture in a first container, as an exemplary embodiment of the present invention.

[0044] Figure 5 This is a schematic diagram illustrating the process of heating and concentrating a mixed solution to a second preset volume V to obtain a test solution, which is an exemplary embodiment of the present invention. Detailed Implementation

[0045] In related technologies, the determination process for total organic carbon (TOC) involves acidifying the water sample, then stripping it of carbonates with nitrogen to eliminate interference. A certain amount of water sample is then injected into an oxygen stream with a known oxygen content and fed into a quartz combustion tube using platinum-steel as a catalyst. The sample is burned at a high temperature of 900–950°C, and the amount of CO2 produced during combustion is measured using a non-dispersive infrared gas analyzer. The TOC content of the water sample is then calculated. This testing method is complex, requires the use of reactive gases, is prone to significant errors, and the high-temperature testing conditions are quite demanding.

[0046] Based on this, an exemplary embodiment of the present invention provides a method for quantitatively testing the total organic carbon content of micron-sized powder materials, such as... Figure 1 As shown, this quantitative testing method includes the following steps:

[0047] Step S100: Provide a micron-sized powder material of a preset mass M, the micron-sized powder material including a first material that is soluble in water and a second material that is insoluble in water;

[0048] Step S200: Mix the micron-sized powder material with distilled water in a first container to obtain a solid-liquid mixture of a first preset volume; heat the first container containing the solid-liquid mixture and the second container containing the first preset volume of distilled water to a preset temperature so that the first material dissolves in the distilled water;

[0049] Step S300: Filter and concentrate the solid-liquid mixture in the first container to obtain a test solution of a second preset volume V;

[0050] Step S400: Detect the total organic carbon content of the test solution and the distilled water in the second container to obtain the first total organic carbon content N1 of the test solution and the second total organic carbon content N0 of the distilled water in the second container;

[0051] Step S500: Determine the total organic carbon content of the micron-sized powder material based on the preset mass M, the second preset volume V, the first total organic carbon content N1, and the second total organic carbon content N0.

[0052] The quantitative testing method for the total organic carbon content of micron-sized powder materials provided in this embodiment firstly provides a preset weight M of micron-sized powder material. The micron-sized powder material is mixed with distilled water in a first container to obtain a first preset volume of solid-liquid mixture. A first preset volume of distilled water is added to a second container as a blank control group. The first and second containers are simultaneously heated to a preset temperature so that the first material is completely dissolved in the distilled water. The solid-liquid mixture in the first container is filtered and concentrated to obtain a second preset volume V of test solution. The total organic carbon content of the test solution and the distilled water in the second container is detected. For example, the test solution and distilled water are placed in a total organic carbon (TOC) analyzer for detection to obtain the first total organic carbon content N1 of the test solution and the second total organic carbon content N0 of the distilled water in the second container. Based on the preset mass M, the second preset volume V, the first total organic carbon content N1, and the second total organic carbon content N0, the total organic carbon content of the micron-sized powder material can be calculated.

[0053] For example, the SieversInnovOx ES laboratory-grade total organic carbon (TOC) analyzer can be used for detection, which can effectively ensure the accuracy of the test results.

[0054] The testing method includes the preparation of the test solution (sample), sample testing, and data processing. The method is safe and simple to operate, and the raw materials and equipment used are readily available. It eliminates the interference of other substances in micron-sized powder materials and can accurately quantify the total organic carbon content in micron-sized powder materials.

[0055] In step S100, the micron-sized powder material can be used as a toughening material for carbon fiber reinforced composite materials to improve the structural components' resistance to high temperature and humidity environments and their stress impact performance outside the carbon fiber alignment direction. The organic carbon in the micron-sized powder material originates from a first material that is soluble in water. This first material is a surfactant used in the preparation of the micron-sized powder material. The micron-sized powder material also includes a second material that is insoluble in water. This second material is a major component of the micron-sized powder material but is not a source of organic carbon in the micron-sized powder material. For example, the preset mass M of the micron-sized powder material can be 4.0 to 8.0 g, such as 4.0 g, 6.0 g, or 8.0 g.

[0056] In step S200, the micron-sized powder material and distilled water are mixed in a first container with a first preset volume. At the same time, distilled water of the same first preset volume is placed in a second container and used as a blank control group for subsequent tests. In order to completely dissolve the first material in the water, the first container is heated to a preset temperature. Simultaneously, the second container containing distilled water, as a blank control group, also needs to be heated to the same preset temperature.

[0057] In step S300, after the first container is heated, the organic carbon source in the micron-sized powder material, i.e., the first material, has completely dissolved in the water. Since the second material is insoluble in water, it can be removed from the micron-sized powder material by filtering the solid-liquid mixture in the first container. After filtration, the first material is retained in the filtrate, and the filtrate is concentrated to a second preset volume V to obtain the test solution.

[0058] In step S400, the prepared test sample solution and the distilled water in the second container, which serves as a blank control group, are placed in a total organic carbon (TOC) analyzer to detect the total organic carbon content, thereby obtaining the first total organic carbon content N1 of the test solution and the second total organic carbon content N0 of the distilled water in the second container of the blank control group.

[0059] In step S500, the total organic carbon content of the micron-sized powder material is calculated based on the preset mass M, the second preset volume V, the first total organic carbon content N1, and the second total organic carbon content N0. This test method is safe and simple to operate and can quantitatively test the total organic carbon content in micron-sized powder materials.

[0060] For example, before the test operation, the instruments required for the test can be cleaned with a 0.2-0.5 wt% sodium persulfate aqueous solution. Sodium persulfate has strong oxidizing properties and can thoroughly clean the instruments and eliminate impurities that may interfere with the test. After cleaning with sodium persulfate aqueous solution, continue to clean with distilled water, and finally clean with hot water to ensure that the instruments required for the test are completely clean and to ensure the accuracy of the test results.

[0061] In one embodiment of the present invention, the first material in the micron-sized powder material includes polyvinyl alcohol, and the second material includes one or more of polyethersulfone, polyurethane, polyamide, polyimide and polycarbonate.

[0062] Polyvinyl alcohol (PVA) is the surfactant used in the preparation of this micron-sized powder material, and it is also the main contributor and source of organic carbon in this micron-sized powder material. Surfactants are substances that can significantly change the interfacial state of a solution system with a small amount added. Surfactants play a role in dispersing, blocking, and protecting the micron-sized powder material during its preparation, effectively preventing agglomeration in the early stages of molding. Therefore, PVA is an indispensable substance in the preparation of this micron-sized powder material. In this embodiment, the PVA used in the preparation of the micron-sized powder material is PVA 1788. Polyethersulfone, polyurethane, polyamide, polyimide, and polycarbonate are thermoplastic polymers with excellent comprehensive properties and are the main components of this micron-sized powder material. The resulting micron-sized powder material is white, powdery, without clusters or foreign matter. This micron-sized powder material can work synergistically with the resin matrix on carbon fibers, and the downstream products are carbon fiber reinforced prepregs and composite materials, mainly used to enhance the toughness and impact resistance of the composite materials.

[0063] like Figure 2 As shown, in one embodiment, mixing micron-sized powder material with distilled water in a first container to obtain a solid-liquid mixture of a first preset volume includes: placing the micron-sized powder material and distilled water in the first container; and subjecting the first container to ultrasonic oscillation for a first preset duration to obtain the solid-liquid mixture. Exemplarily, the first container can be a 250ml conical flask. When mixing the micron-sized powder material and distilled water, the first container containing the micron-sized powder material and distilled water can be shaken clockwise for 1-2 minutes, and then subjected to ultrasonic oscillation using high-frequency ultrasonic waves in an ultrasonic cleaning tank to disperse the agglomerated particles. This ensures that the micron-sized powder material is completely dispersed, preventing agglomeration from adversely affecting subsequent test results.

[0064] In one embodiment, the first preset duration is 20–40 mins, and the ultrasonic oscillation frequency is 50–80 Hz. This design ensures that the micron-sized powder material is completely dispersed, preventing agglomeration, which would be detrimental to subsequent testing processes and affect test results.

[0065] like Figure 3 As shown, in one embodiment, heating a first container containing a solid-liquid mixture and a second container containing a first preset volume of distilled water to a preset temperature includes: setting a first condenser at the opening of the first container and setting a second condenser at the opening of the second container; heating the first container and the second container, and condensing and refluxing the water vapor evaporated in the first container through the first condenser, and condensing and refluxing the water vapor evaporated in the second container through the second condenser.

[0066] When the first material is polyvinyl alcohol (PVA), PVA can be completely dissolved in water at a temperature not lower than 75°C. Therefore, to ensure that PVA is completely dissolved and extracted into water, the first container needs to be heated. Similarly, the second container containing distilled water is heated simultaneously as a blank control group. For example, the first and second containers can be placed in an oil bath at a temperature set at 102±1°C. This temperature setting ensures that PVA is completely dissolved in water and that the solid-liquid mixture in the first container and the distilled water in the second container reach boiling. Condensers are then installed at the openings of the first and second containers for reflux condensation. This allows the liquid phase in the first container to continuously cycle through boiling, condensation, and reflux, resulting in a more uniform and stable solid-liquid mixture dispersion system. This further ensures the complete dissolution of PVA and improves the accuracy and reliability of the test results.

[0067] In addition, stirring paddles can be installed in the first and second containers respectively, and the stirring speed can be set to 200-250 rpm to fully mix the micron-sized powder material in the first container with distilled water, so that polyvinyl alcohol can be completely dissolved in the water.

[0068] In one embodiment, the heating time for the first and second containers is 2 to 3 hours. This design ensures that the solid-liquid mixture in the first container is continuously heated, refluxed, and condensed, making the solid-liquid mixture system more uniform and stable.

[0069] In one embodiment, filtering and concentrating the solid-liquid mixture in the first container includes: filtering the solid-liquid mixture in a dissolved state through a filtration device, and using the resulting filtrate to form a test solution. After shaking, ultrasonic oscillation, and heating under reflux and condensation, the powder material in the first container is completely dispersed in the water, and the organic carbon source in the micron-sized powder material, namely polyvinyl alcohol, is also completely dissolved in the water. At this point, filtering and separating the solid-liquid mixture in the first container can yield the sample solution required for testing. Exemplarily, the filtration device is a membrane filtration device with a filter cloth having a pore size of 0.5 μm. This design allows for complete and rapid solid-liquid separation of the solid-liquid mixture in the first container, completely dissolving and extracting the polyvinyl alcohol into the water to initially obtain the required test solution.

[0070] like Figure 4As shown, in one embodiment, filtering and concentrating the solid-liquid mixture in the first container further includes: washing the first container and the filter device with distilled water to obtain a first cleaning solution; mixing the first cleaning solution with the filtrate to obtain a mixed solution; and heating and concentrating the mixed solution to a second preset volume V to obtain a test solution. After filtering and separating the solid-liquid mixture in the first container, rinsing the first container and the filter device with distilled water can completely collect any residual polyvinyl alcohol in the first container and the filter device, avoiding residual loss of polyvinyl alcohol during sample preparation and its adverse effect on the test results. Concentrating the cleaning solution and the filtrate to a preset volume V can, on the one hand, increase the concentration of the test solution, thereby improving the accuracy of the test results; on the other hand, it allows for the calculation of the final total organic carbon content of the micron-sized powder material based on the preset volume V for subsequent TOC test results.

[0071] like Figure 5 As shown, in one embodiment, the mixed solution is heated and concentrated to a second preset volume V to obtain a test solution, including: adding the mixed solution to a rotary evaporator for rotary evaporation to obtain a first concentrate; cleaning the rotary evaporator after rotary evaporation with distilled water to obtain a second cleaning solution; mixing the first concentrate and the second cleaning solution and adding distilled water to the second preset volume V to obtain the test solution. Adding the solution after mixing the cleaning solution and filtrate to the rotary evaporator for heating and rotary evaporation to concentrate to the preset volume V can increase the concentration of the test solution, thereby improving the accuracy of the test results. Cleaning the rotary evaporator after rotary evaporation with distilled water, and combining the cleaning solution and the concentrate to a final volume of the second preset volume V, can completely collect the polyvinyl alcohol remaining in the rotary evaporator, avoiding residual loss of polyvinyl alcohol during sample preparation and its adverse effect on the test results. Exemplarily, the rotary evaporator is used in an oil bath at a temperature set to 102±1℃ for rotary evaporation, concentrating the filtrate to 50-70 ml, and combining it with the cleaning water used to clean the rotary evaporator, then making a final volume in a 100 ml sample bottle.

[0072] In one embodiment, determining the total organic carbon content of the micron-sized powder material based on a preset mass M, a second preset volume V, a first total organic carbon content N1, and a second total organic carbon content N0 includes: calculating the total organic carbon content of the micron-sized powder material using the following formula:

[0073] TOC = (N1 - N0) * V / (1000 * M);

[0074] Wherein, TOC (mg / L) represents the total organic carbon content; N1 (mg / L) represents the total organic carbon content of the test solution; N0 (mg / L) represents the total organic carbon content of the distilled water in the second container; V (ml) represents the volume of the test solution; 1000 represents the conversion value between ml and L; and M (g) represents the mass of the micron-sized powder material.

[0075] The following is a specific example of a quantitative test method for the total organic carbon content of micron-sized powder materials.

[0076] Clean the glassware used in the test process with a 0.5 wt% sodium persulfate aqueous solution, then rinse with distilled water, and finally with hot water. Weigh 8.0 g of micron-sized powder material and place it in a 250 ml Erlenmeyer flask, add 100 ml of distilled water, and shake the flask clockwise for 2 minutes. Then, sonicate at 80 Hz for 40 minutes in an ultrasonic cleaning bath to disperse the agglomerated particles. Transfer the dispersed solid-liquid mixture in the Erlenmeyer flask to a 1 L three-necked flask, rinse the Erlenmeyer flask with distilled water, add the rinse water to the three-necked flask, and then add distilled water to the three-necked flask to a final volume of 500 ml. Simultaneously, add 500 ml of distilled water to another three-necked flask as a blank control. Set the oil bath temperature in the oil bath to 102℃. Place two three-necked flasks in the oil bath and connect condensers, thermometers, and stirrers to the top of the flasks. Set the stirring speed to 250 rpm, allowing water vapor to condense into water in the condenser and reflux back into the three-necked flasks. Maintain this reflux condensation condition for 3 hours. Add filter cloth (0.5 μm pore size) to the membrane filtration device. Add the hot solid-liquid mixture obtained after condensation in the three-necked flasks to the membrane filtration device for filtration, and rinse the flasks and filtration device with appropriate distilled water. Transfer the filtrate and the rinsing water from rinsing the flasks and filtration device to a 1L rotary evaporator. Rotate the evaporator in an oil bath at 102℃ to concentrate the filtrate to 50-70 ml and pour it into a 100 ml sample bottle. Rinse the 1L rotary evaporator with a small amount of distilled water and pour the rinsing water into the 100 ml sample bottle. Accurately dilute to 100 ml to obtain the required test solution. 1 ml of the test solution was placed in a SieversInnovOx ES laboratory-grade total organic carbon (TOC) analyzer, and the TOC result of the test solution was 59 mg / L. 1 ml of the blank control group distilled water was placed in the SieversInnovOx ES laboratory-grade total organic carbon (TOC) analyzer, and the TOC result of the blank control group distilled water was 0.03 mg / L. The TOC calculation formula for this micron-sized powder material is: TOC (mg / g) = (59 - 0.03) * 100 / (1000 * 8.0). After calculation, the TOC result of this micron-sized powder material is 0.73 mg / g.

[0077] In another embodiment, a total organic carbon (TOC) analyzer can be connected to an automatic calculation device. The results measured by the TOC analyzer can be transmitted to the automatic calculation device for automatic calculation. By pre-inputting the TOC calculation formula for micron-sized powder materials into the automatic calculation device, integrated automatic detection of testing and calculation can be achieved, directly obtaining the total organic carbon content of micron-sized powder materials, saving calculation time and simplifying the testing steps.

[0078] The above embodiments are only used to illustrate the technical solutions of this application, and are not intended to limit it. Although this application has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some of the technical features; and these modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the embodiments of this application.

Claims

1. A method for quantitatively testing the total organic carbon content of a micron-sized powder material, characterized by, Includes the following steps: A micron-sized powder material of a predetermined mass M is provided, wherein the micron-sized powder material comprises a first material that is soluble in water and a second material that is insoluble in water; the first material is a surfactant used in the preparation process of the micron-sized powder material. The micron-sized powder material is mixed with distilled water in a first container to obtain a first preset volume of solid-liquid mixture; the first container containing the solid-liquid mixture and the second container containing the first preset volume of distilled water are heated to a preset temperature so that the first material dissolves in the distilled water; The solid-liquid mixture in the first container is filtered and concentrated to obtain a test solution of a second preset volume V. The total organic carbon content of the test solution and the distilled water in the second container is detected to obtain the first total organic carbon content N1 of the test solution and the second total organic carbon content N0 of the distilled water in the second container. The total organic carbon content of the micron-sized powder material is determined based on the preset mass M, the second preset volume V, the first total organic carbon content N1, and the second total organic carbon content N0. The step of heating the first container containing the solid-liquid mixture and the second container containing the first preset volume of distilled water to a preset temperature includes: setting a first condenser at the opening of the first container and setting a second condenser at the opening of the second container; heating the first container and the second container, and condensing and refluxing the water vapor evaporated in the first container through the first condenser, and condensing and refluxing the water vapor evaporated in the second container through the second condenser.

2. The method of quantitatively testing the total organic carbon content of a micrometer-scale powder material according to claim 1, characterized in that, The first material includes polyvinyl alcohol, and the second material includes one or more of polyethersulfone, polyurethane, polyamide, polyimide and polycarbonate.

3. The quantitative test method for total organic carbon content of micron-sized powder materials according to claim 1, characterized in that, The step of mixing the micron-sized powder material with distilled water in a first container to obtain a solid-liquid mixture of a first predetermined volume includes: The micron-sized powder material and distilled water are placed in the first container; The first container is subjected to ultrasonic oscillation for a first preset duration to obtain the solid-liquid mixture.

4. The quantitative test method for total organic carbon content of micron-sized powder materials according to claim 3, characterized in that, The first preset duration is 20~40 mins, and the frequency of the ultrasonic oscillation is 50~80 Hz.

5. The quantitative test method for total organic carbon content of micron-sized powder materials according to claim 1, characterized in that, The heating time for the first container and the second container is 2 to 3 hours.

6. The quantitative test method for total organic carbon content of micron-sized powder materials according to claim 1, characterized in that, The filtering and concentration of the solid-liquid mixture in the first container includes: The solid-liquid mixture in which the first material is in a dissolved state is filtered through a filtration device, and the resulting filtrate is used to form the test solution.

7. The quantitative test method for total organic carbon content of micron-sized powder materials according to claim 6, characterized in that, The step of filtering and concentrating the solid-liquid mixture in the first container further includes: The first container and the filter device are cleaned with distilled water to obtain a first cleaning solution; The first cleaning solution is mixed with the filtrate to obtain a mixed solution; The mixed solution is heated and concentrated to a second preset volume V to obtain the test solution.

8. The quantitative test method for total organic carbon content of micron-sized powder materials according to claim 7, characterized in that, The step of heating and concentrating the mixed solution to a second preset volume V to obtain the test solution includes: The mixed solution was added to a rotary evaporator for rotary evaporation to obtain a first concentrated solution; The rotary evaporator after rotary evaporation is cleaned with distilled water to obtain a second cleaning solution. The first concentrate and the second cleaning solution are mixed and distilled water is added to the second preset volume V to obtain the test solution.

9. The quantitative test method for total organic carbon content of micron-sized powder materials according to claim 7, characterized in that, The step of determining the total organic carbon content of the micron-sized powder material based on the preset mass M, the second preset volume V, the first total organic carbon content N1, and the second total organic carbon content N0 includes: The total organic carbon content of the micron-sized powder material is calculated using the following formula: ； Wherein, TOC (mg / g) represents the total organic carbon content; N1 (mg / L) represents the total organic carbon content of the test solution; N0 (mg / L) represents the total organic carbon content of the distilled water in the second container; V (ml) represents the volume of the test solution; 1000 represents the conversion value between ml and L; and M (g) represents the mass of the micron-sized powder material.

Images