A method and apparatus for detecting the aluminium carbide content
By designing a gas detection device and a method for reacting aluminum carbide with water to generate methane gas, the problems of impurity interference and equipment complexity in aluminum carbide detection were solved, and a simple and accurate measurement of aluminum carbide content was achieved.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- XINJIANG UNIVERSITY
- Filing Date
- 2026-04-01
- Publication Date
- 2026-06-23
Smart Images
Figure CN122259748A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of analytical chemistry, and specifically to a method and apparatus for detecting aluminum carbide content. Background Technology
[0002] Aluminum carbide is an important industrial compound, typically with the chemical formula Al₄C₃. It is widely used in the metallurgical industry as an intermediate or alloying additive, and as a catalyst in chemical synthesis. In certain advanced materials fields, such as carbon-aluminum composites, the formation and content of aluminum carbide significantly affect the material's properties. However, industrially prepared aluminum carbide products are usually not pure substances, often containing impurities such as aluminum nitride and aluminum oxide. Notably, aluminum carbide possesses a unique chemical property: it can undergo a hydrolysis reaction with water, producing methane gas (CH₄) and aluminum hydroxide, as shown in the following reaction formula:
[0003] This reaction is highly specific—among common aluminum-containing impurities, such as aluminum nitride, although it can also react with water to produce ammonia (NH3), its reaction conditions, rate, and types of product gases are significantly different from those of aluminum carbide; while aluminum oxide and other similar impurities basically do not react with water. Therefore, by quantitatively detecting the volume or concentration of methane gas produced by the hydrolysis of aluminum carbide, the actual content of aluminum carbide in the sample can be indirectly and accurately calculated.
[0004] Existing testing methods face numerous challenges: impurities such as aluminum nitride in industrial aluminum carbide are difficult to separate effectively, causing inconvenience for precision instruments in component analysis and reducing the accuracy of measurement results; traditional detection methods relying on large instruments suffer from problems such as expensive equipment, cumbersome operation, and long cycles, making it difficult to meet the needs of rapid on-site testing; at the same time, there is a lack of practical means to easily monitor changes in the detection process. Therefore, there is an urgent need in this field for an aluminum carbide content detection method and device that can overcome the above shortcomings and provide easy observation, high accuracy, simple operation, and low cost. Summary of the Invention
[0005] To address the problems of component interference, equipment measurement accuracy and operational complexity, and the inability to monitor the detection process in existing technologies for detecting aluminum carbide, this invention provides a method and apparatus for detecting aluminum carbide content.
[0006] An apparatus for detecting aluminum carbide content includes a constant temperature water bath 1, a round-bottom flask 2, a rubber stopper I 3, a right-angle tube I 4, a rubber tube I 5, a three-way valve 6, a rubber tube II 7, a rubber tube III 8, a right-angle tube II 9, a thermometer 10, a rubber stopper II 11, a specially made measuring cylinder 12, a right-angle tube III 13, a rubber tube IV 14, a right-angle tube IV 15, a rubber stopper III 16, a glass tube 17, a conical flask 18, and a gas chromatograph 19. The round-bottom flask 2 is located in the constant temperature water bath 1. The rubber stopper I 3 is inserted into the mouth of the round-bottom flask 2. The inlet end of the right-angle tube I 4 is connected to the round-bottom flask 2 via the rubber stopper I 3, and the outlet end is connected to the inlet end of the rubber tube I 5. The other end of rubber tube I5 is connected to one port of three-way valve 6, and the other two ports of three-way valve 6 are connected to rubber tube II7 and rubber tube III8 respectively; the other end of rubber tube II7 is connected to the gas inlet of gas chromatograph 19; the other end of rubber tube III8 is connected to the inlet of right-angle tube II9, and the outlet of right-angle tube II9, thermometer 10 and the inlet of right-angle tube III13 are embedded together with rubber stopper II11 and installed at the mouth of special measuring cylinder 12; the outlet of right-angle tube III13 is connected to the inlet of right-angle tube IV15 through rubber tube IV14; the outlet of right-angle tube IV15 and glass tube 17 are embedded together with rubber stopper III16 and installed at the mouth of conical flask 18.
[0007] Furthermore, the inlet end of the right-angle tube I4 can be flush with the bottom of the rubber stopper I3, or it can extend into the round-bottom flask 2, but it cannot come into contact with the reactants in the round-bottom flask 2.
[0008] A method for detecting aluminum carbide content includes the following steps: S1: Sample taking, taking samples to be tested from various sites on the aluminum carbide raw material; S2: Weighing and grinding. Weigh approximately 0.1g of aluminum carbide sample using a 0.01g balance and grind until the particle size is 0.1mm or less. S3: As Figure 1The gas detection device is set up as shown. Sufficient purified water is added to the constant temperature water bath 1, and sufficient distilled water is added to the round-bottom flask 2. The special measuring cylinder 12 is filled with distilled water and plugged with rubber stopper II 11. The bottom of thermometer 10 should be flush with the bottom of rubber stopper II 11. One end of right-angle tube II 9 inserted into rubber stopper II 11 should be flush with the bottom of rubber stopper II 11. One end of right-angle tube III 13 inserted into rubber stopper II 11 should extend 0.5 cm above the bottom of the special measuring cylinder 12. The valve in the three-way valve 6 connected to the gas chromatograph detector 19 is closed. The valve in the three-way valve 6 connected to the round-bottom flask 2 and the special measuring cylinder 12 is opened. The aluminum carbide sample is poured into the round-bottom flask 2, and rubber stopper I 3 is quickly inserted into the mouth of the round-bottom flask 2. The valve in the three-way valve 6 connected to the gas chromatograph detector 19 is closed. The power supply to the constant temperature water bath 1 is turned on, and the water bath temperature is controlled between 50 and 80°C. S4: After the aluminum carbide sample reacts completely with water, read the gas volume in the special graduated cylinder 12, and press the thermometer 10 downward into the middle of the gas in the special graduated cylinder 12. After the thermometer 10 reading stabilizes, record the reading; close the valve connected to the rubber tube I5 of the three-way valve 6, open the valve connected to the gas chromatograph 19 of the three-way valve 6, start the gas chromatograph 19, and perform gas composition analysis. S5: Take the average value of the measurement results and substitute it into the function model for calculating aluminum carbide content:
[0009] in, r Indicates the relative content of aluminum carbide in the sample; λ Indicates the correction factor; m The mass of the sample weighed for gas detection is expressed in grams. V The volume of gas collected in the specially made graduated cylinder 12 is expressed in mL. M Indicates the molar mass of aluminum carbide; Vc The volume of one mole of gas is expressed in mL. R This represents the corrected methane dissolution constant, which is the amount of methane that can be dissolved in water in the round-bottom flask 2 and the special graduated cylinder 12, in mL; Correction coefficient λ To summarize the relevant research, the following empirical formula was derived:
[0010] in, α This indicates the percentage of methane content in a gas as measured by a gas chromatograph. P 0 The pressure measured in millimeters of mercury is the atmospheric pressure at 0°C. W Indicates in t The saturated vapor pressure of water at ℃, in millimeters of mercury; t0 Indicates the ambient temperature during sample testing, in °C; t This indicates the gas temperature reading from thermometer 10, in °C. S6: Repeat steps S2 to S5 twice, and then take the arithmetic mean of the three calculation results.
[0011] Furthermore, multiple samplings were performed at various locations on the aluminum carbide raw material, including selections at the surface, interior, and bottom of the aluminum carbide raw material, with each location sampled three times.
[0012] Compared with existing aluminum carbide detection methods, the present invention has the following advantages.
[0013] This invention discloses a method and apparatus for detecting aluminum carbide content. The designed gas detection device utilizes a three-way valve 6 to connect a round-bottom flask 3, a specially designed graduated cylinder 12, and a gas chromatograph 19. By adjusting the various valves of the three-way valve 6, the gas generated by the reaction between the sample and water can be either introduced into the specially designed graduated cylinder 12 for volume measurement and quantitative analysis, or introduced into the gas chromatograph 19 for qualitative analysis. The quantitative and qualitative analysis of the gas is performed in the same device, simplifying the detection steps and improving the accuracy and efficiency of gas detection.
[0014] This invention discloses a method and apparatus for detecting aluminum carbide content. The gas generated by the reaction of the sample with water at various points on the sample to be tested is introduced into a specially designed measuring cylinder 12 via a three-way valve 6. The volume of the generated gas can be obtained through the measuring cylinder 12. The gas generated by the reaction of the sample with water is then introduced into a gas chromatograph 19 for detection via the three-way valve 6. The gas chromatograph 19 accurately determines the methane content in the generated gas, thus obtaining the data required for calculating the aluminum carbide content function model. The data acquisition is direct and convenient, greatly simplifying the detection operation.
[0015] This invention discloses a method and apparatus for detecting aluminum carbide content. The method employs a functional model for calculating aluminum carbide content to further process the test results. The functional model for calculating aluminum carbide content is modified based on the actual temperature of the generated gas obtained from thermometer 10, the methane content in the generated gas accurately measured by gas chromatograph 19, and empirical formulas. This further improves the accuracy of the functional model for calculating aluminum carbide content, resulting in more accurate detection of aluminum carbide content in the sample and enhanced detection precision.
[0016] This invention discloses a method and apparatus for detecting aluminum carbide content. The method uses a constant temperature water bath 1 to heat the sample and distilled water in a round-bottom flask 2, which promotes the reaction and greatly shortens the testing time. Furthermore, the instruments used are mostly glassware, making the detection process clearly visible and enabling monitoring of the detection process and prediction of the detection results.
[0017] This invention discloses a method and apparatus for detecting aluminum carbide content. The main instruments used include a constant temperature water bath 1, a round bottom flask 2, a thermometer 10, a specially made measuring cylinder 12, a conical flask 18, and a gas chromatograph 19. The apparatus is low in cost, simple to assemble, easy to carry, and has a low barrier to entry for use, making it simple and convenient to operate. Attached Figure Description
[0018] Figure 1 This is a front view of an apparatus for detecting aluminum carbide content. Detailed Implementation
[0019] The technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings of the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. All other embodiments obtained by those skilled in the art based on the embodiments of the present invention without creative effort are within the scope of protection of the present invention.
[0020] In the description of this invention, it should be noted that the terms "top," "bottom," "one side," "the other side," "front," "rear," "middle part," "inner," "top," and "bottom," etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are used only for the convenience of describing the invention and for 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. Therefore, they should not be construed as limitations on the invention. The terms "first," "second," and "third" are used for descriptive purposes only and should not be construed as indicating or implying relative importance. Furthermore, unless otherwise explicitly specified and limited, the terms "installed," "connected," and "linked" 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 communication of two components. Those skilled in the art can understand the specific meaning of the above terms in this invention based on the specific circumstances.
[0021] The present invention will now be described in further detail with reference to the accompanying drawings. Example
[0022] A method and apparatus for detecting aluminum carbide content, such as Figure 1 As shown, the system includes a constant temperature water bath 1, a round bottom flask 2, a rubber stopper I 3, a right-angle tube I 4, a rubber tube I 5, a three-way valve 6, a rubber tube II 7, a rubber tube III 8, a right-angle tube II 9, a thermometer 10, a rubber stopper II 11, a special measuring cylinder 12, a right-angle tube III 13, a rubber tube IV 14, a right-angle tube IV 15, a rubber stopper III 16, a glass tube 17, a conical flask 18, and a gas chromatograph detector 19. S1: Sample taking. Aluminum carbide with an analytical purity of 99.0% was used as the sample raw material. Multiple samples were taken at various sites in the aluminum carbide raw material, including the surface, interior and bottom of the aluminum carbide raw material. Each site was sampled 3 times. S2: Weighing and grinding. Weigh 0.1125g of aluminum carbide sample using a balance with a mass of 0.01%, and grind it until the particle size of the sample is 0.1mm or less. S3: As Figure 1 The gas detection device is constructed as shown. The round-bottom flask 2 is located in a constant-temperature water bath 1. Sufficient purified water is added to the constant-temperature water bath 1. 220 mL of distilled water is added to the round-bottom flask 2. The inlet end of the right-angle tube I4 is inserted with a rubber stopper I3, and the outlet end is connected to the inlet end of the rubber tube I5. The other end of the rubber tube I5 is connected to one port of a three-way valve 6. The other two ports of the three-way valve 6 are connected to rubber tubes II7 and III8, respectively. The other end of the rubber tube II7 is connected to the gas inlet of the gas chromatograph 19. The valve in the three-way valve 6 connected to the gas chromatograph 19 is closed, and the valve in the three-way valve 6 connected to the round-bottom flask 2 and the special measuring cylinder 12 is opened. The special measuring cylinder 12 is filled with distilled water. The other end of the rubber tube III8 is connected to the inlet of the right-angle tube II9. The thermometer 10 is connected to the rubber stopper II 11, with the bottom of the thermometer 10 flush with the bottom of the rubber stopper II 11. One end of the right-angle tube II 9 is inserted into the rubber stopper II 11, with the port flush with the bottom of the rubber stopper II 11. One end of the right-angle tube III 13 is inserted into the rubber stopper II 11, with the port extending 0.5 cm above the bottom of the special measuring cylinder 12. The other end of the right-angle tube III 13 is connected to the inlet end of the right-angle tube IV 15 via the rubber tube IV 14. The outlet end of the right-angle tube IV 15 is inserted into the rubber stopper III 16 along with the glass tube 17 and installed at the mouth of the conical flask 18. The aluminum carbide sample is poured into the round-bottom flask 2, and the rubber stopper I 3 is quickly inserted into the mouth of the round-bottom flask 2. The power supply of the constant temperature water bath 1 is turned on and the switch is turned on, and the water bath temperature is controlled at 50℃. S4: After the aluminum carbide sample reacts completely with water, the gas volume in the special graduated cylinder 12 is read as 50 mL. The thermometer 10 is then pressed downwards into the middle of the gas in the special graduated cylinder 12. After the thermometer 10 reading stabilizes, the temperature reading is recorded as 31.2℃. The valve connected to the rubber tube I5 of the three-way valve 6 is closed, and the valve connected to the gas chromatograph 19 of the three-way valve 6 is opened. The gas chromatograph 19 is started, and the gas enters the gas chromatograph 19. The gas composition of the gas generated by the reaction is analyzed. S5: Take the average value of the measurement results and substitute it into the function model for calculating the aluminum carbide content:
[0023] in, r Indicates the relative content of aluminum carbide in the sample; λ Indicates the correction factor; m The mass of the sample weighed for gas detection is expressed in grams. V The volume of gas collected in the specially made graduated cylinder 12 is expressed in mL. M Indicates the molar mass of aluminum carbide; Vc The volume of one mole of gas is expressed in mL. R This represents the corrected methane dissolution constant, which is the amount of methane that can be dissolved in water in the round-bottom flask 2 and the special graduated cylinder 12, in mL; Correction coefficient λ To summarize the relevant research, the following empirical formula was derived:
[0024] in, α This indicates the percentage of methane content in a gas as measured by a gas chromatograph. P 0 The pressure measured in millimeters of mercury is the atmospheric pressure at 0°C. W Indicates in t The saturated vapor pressure of water at ℃, in millimeters of mercury; t 0 Indicates the ambient temperature during sample testing, in °C; t This indicates the gas temperature reading from thermometer 10, in °C. For detailed data, please refer to Table 1. S6: Under the same reaction conditions, weigh 0.1054g and 0.1036g of aluminum carbide sample respectively and repeat steps S2 to S5 twice. The arithmetic mean of the three calculation results is used to obtain the sample purity of 97.4%. Example
[0025] This embodiment is based on the aforementioned embodiment. In this embodiment, aluminum carbide with an analytical purity of 95.0% is used as the sample raw material. 0.1129g, 0.1036g, and 0.1130g of aluminum carbide samples were weighed for the experiment. In this embodiment, the water bath temperature was controlled at 65℃. Specific data are detailed in Table 1. The arithmetic mean of the three calculation results yielded a sample purity of 94.6%. Example
[0026] This embodiment is based on the previous embodiment. In this embodiment, aluminum carbide with an analytical purity of 80.0% is used as the sample raw material. 0.1130g, 0.1220g and 0.1034g of aluminum carbide samples are weighed for the experiment. In this embodiment, the water bath temperature is controlled at 80℃. The specific data are detailed in Table 1. The arithmetic mean of the three calculation results is used to obtain the sample purity of 79.6%. Example
[0027] This embodiment is based on the aforementioned embodiment. In this embodiment, aluminum carbide with an analytical purity of 65.0% is used as the sample raw material. 0.1131g, 0.1093g, and 0.1020g of aluminum carbide samples are weighed for the experiment. In this embodiment, the water bath temperature is controlled at 70℃. Specific data are detailed in Table 1. The arithmetic mean of the three calculation results is used to obtain a sample purity of 66.2%.
[0028] Examples 1-4 use a method and apparatus for detecting aluminum carbide content, and the detection results are shown in Table 1.
[0029] Table 1. Test results of samples 1-4
[0030] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above, and that the invention can be implemented in other specific forms without departing from its spirit or essential characteristics. Therefore, the embodiments should be considered in all respects as exemplary and non-limiting, and the scope of the invention is defined by the appended claims rather than the foregoing description. Thus, all variations falling within the meaning and scope of equivalents of the claims are intended to be included within the present invention. No reference numerals in the claims should be construed as limiting the scope of the claims.
[0031] Furthermore, it should be understood that although this specification describes embodiments, not every embodiment contains only one independent technical solution. This narrative style is merely for clarity. Those skilled in the art should consider the specification as a whole, and the technical solutions in each embodiment can also be appropriately combined to form other embodiments that can be understood by those skilled in the art.
Claims
1. An apparatus for detecting aluminum carbide content, comprising a constant temperature water bath (1), a round-bottom flask (2), a rubber stopper I (3), a right-angle tube I (4), a rubber tube I (5), a three-way valve (6), a rubber tube II (7), a rubber tube III (8), a right-angle tube II (9), a thermometer (10), a rubber stopper II (11), a specially made measuring cylinder (12), a right-angle tube III (13), a rubber tube IV (14), a right-angle tube IV (15), a rubber stopper III (16), a glass tube (17), an Erlenmeyer flask (18), and a gas chromatograph (19), characterized in that... The round-bottom flask (2) is located in a constant-temperature water bath (1). A rubber stopper I (3) is inserted into the mouth of the round-bottom flask (2). The inlet end of the right-angle tube I (4) is connected to the round-bottom flask (2) through the rubber stopper I (3), and the outlet end is connected to the inlet end of the rubber tube I (5). The other end of the rubber tube I (5) is connected to one port of a three-way valve (6), and the other two ports of the three-way valve (6) are connected to rubber tube II (7) and rubber tube III (8) respectively. The other end of the rubber tube II (7) is connected to the gas inlet of the gas chromatograph (19). Connected; the other end of rubber tube Ⅲ (8) is connected to the inlet end of right angle tube Ⅱ (9), the outlet end of right angle tube Ⅱ (9), thermometer (10) and the inlet end of right angle tube Ⅲ (13) are embedded together in rubber stopper Ⅱ (11) and installed at the mouth of special measuring cylinder (12); the outlet end of right angle tube Ⅲ (13) is connected to the inlet end of right angle tube Ⅳ (15) through rubber tube Ⅳ (14); the outlet end of right angle tube Ⅳ (15) and glass tube (17) are embedded together in rubber stopper Ⅲ (16) and installed at the mouth of conical flask (18).
2. The device for detecting aluminum carbide content according to claim 1, characterized in that... The inlet end of the right-angle tube I (4) can be flush with the bottom of the rubber stopper I (3) or it can extend into the round-bottom flask (2), but it cannot come into contact with the reactants in the round-bottom flask (2).
3. A method for detecting aluminum carbide content, comprising the following steps, characterized in that: S1: Sample taking, taking samples to be tested from various sites on the aluminum carbide raw material; S2: Weighing and grinding. Weigh approximately 0.1g of aluminum carbide sample using a 0.01g balance and grind until the particle size is 0.1mm or less. S3: As shown in Figure 1, construct a gas detection device. Add sufficient pure water to the constant temperature water bath (1) and sufficient distilled water to the round bottom flask (2). Fill the special measuring cylinder (12) with distilled water and insert the rubber stopper II (11). The bottom of the thermometer (10) should be flush with the bottom of the rubber stopper II (11). The end of the right-angle tube II (9) inserted into the rubber stopper II (11) should be flush with the bottom of the rubber stopper II (11). The end of the right-angle tube III (13) inserted into the rubber stopper II (11) should extend into the special measuring cylinder (11). 12) At 0.5cm above the bottom, close the valve in the three-way valve (6) connected to the gas chromatograph (19), open the valve in the three-way valve (6) connected to the round-bottom flask (2) and the special measuring cylinder (12), pour the aluminum carbide sample into the round-bottom flask (2) and quickly insert the rubber stopper I (3) into the mouth of the round-bottom flask (2); close the valve in the three-way valve (6) connected to the gas chromatograph (19); turn on the power of the constant temperature water bath (1) and turn on the switch to control the water bath temperature between 50~80℃; S4: After the aluminum carbide sample reacts completely with water, read the gas volume in the special graduated cylinder (12) and press the thermometer (10) down into the middle of the gas in the special graduated cylinder (12). Record the reading after the thermometer (10) reading stabilizes. Close the valve connected to the rubber tube I (5) of the three-way valve (6), open the valve connected to the gas chromatograph (19) of the three-way valve (6), start the gas chromatograph (19), and perform gas composition analysis. S5: Take the average value of the measurement results and substitute it into the function model for calculating aluminum carbide content: in, r Indicates the relative content of aluminum carbide in the sample; λ Indicates the correction factor; m The mass of the sample weighed for gas detection is expressed in grams. V The volume of gas collected in the specially made graduated cylinder (12) is expressed in mL. M Indicates the molar mass of aluminum carbide; Vc The volume of one mole of gas is expressed in mL. R The corrected methane dissolution constant is the amount of methane that can be dissolved in water in the round-bottom flask (2) and the special graduated cylinder (12), in mL; Correction coefficient λ To summarize the relevant research, the following empirical formula was derived: in, α This indicates the percentage of methane content in a gas as measured by a gas chromatograph. P 0 The pressure measured in millimeters of mercury is the atmospheric pressure at 0°C. W Indicates in t The saturated vapor pressure of water at ℃, in millimeters of mercury; t 0 Indicates the ambient temperature during sample testing, in °C; t The reading indicates the gas temperature as read from the thermometer (10), in °C; S6: Repeat steps S2 to S5 twice, and then take the arithmetic mean of the three calculation results.
4. The method for detecting aluminum carbide content according to claim 3, characterized in that... Samples were taken multiple times at various locations on the aluminum carbide raw material, including the surface, interior, and bottom of the raw material, with each location sampled three times.