A system and method for determining the diffusible hydrogen and residual hydrogen content in a bulk metal

Abstract

The application discloses a kind of determination system and method of diffusion hydrogen and residual hydrogen content in bulk metal, it is related to alloy trace element analysis technical field, system includes: angle-adjustable vacuum tube type program-controlled heating furnace, condenser tube, remote temperature table, trace bubble flowmeter, gas bag with quick connector, temperature program control machine, temperature feedback low-temperature constant-temperature circulator and gas chromatograph, angle-adjustable vacuum tube type program-controlled heating furnace is built in the bulk metal material to be measured, according to the first heating temperature curve and the second heating temperature curve of temperature program control machine output, the bulk metal material to be measured is heated in batches, so that the bulk metal material to be measured releases diffusion hydrogen and residual hydrogen in batches, so that the measurement of diffusion hydrogen and residual hydrogen is released in batches is realized.

Description

Technical Field

[0001] This invention relates to the field of trace element analysis technology for alloys, and in particular to a system and method for determining the content of diffusible hydrogen and residual hydrogen in bulk metals. Background Technology

[0002] During manufacturing, processing, construction, and subsequent service, hydrogen atoms can accumulate in metallic materials. The diffusion of hydrogen atoms to areas of stress concentration within the metal can lead to localized embrittlement, a phenomenon known as hydrogen embrittlement. Determining the hydrogen content in metallic materials is a crucial method for studying hydrogen embrittlement, and accurately measuring the hydrogen content within a metallic material is key to evaluating its hydrogen embrittlement resistance.

[0003] In existing technologies, hydrogen content measurement devices generally employ thermal conductivity detectors. These detectors measure the thermal conductivity of different gas components diffusing from a metallic material, converting the gas concentration into an electrical signal to determine the hydrogen volume. However, because existing devices cannot perform staged heating of the metallic material, they cannot measure the staged release of diffusing and residual hydrogen from the metallic material. Summary of the Invention

[0004] The purpose of this invention is to provide a system and method for determining the content of diffusible hydrogen and residual hydrogen in bulk metals, so as to solve the problem that it is impossible to measure the fractional release of diffusible hydrogen and residual hydrogen in metallic materials.

[0005] To achieve the above objectives, the present invention provides the following solution:

[0006] A system for determining the content of diffusible hydrogen and residual hydrogen in bulk metal, comprising:

[0007] Angle-adjustable vacuum tube type programmable heating furnace, condenser tube, remote temperature meter, micro bubble flow meter, gas bag with quick connector, temperature program controller, temperature feedback low temperature constant temperature circulator and gas phase mass spectrometer.

[0008] The adjustable-angle vacuum tube programmable heating furnace contains the bulk metal material to be tested. The bulk metal material to be tested is heated in stages according to the first heating temperature curve and the second heating temperature curve output by the temperature program controller, so that the bulk metal material to be tested releases diffused hydrogen and residual hydrogen in stages.

[0009] The angle-adjustable vacuum tube programmable heating furnace is used to heat the bulk metal material to be tested according to the first heating temperature curve and output diffused hydrogen mixed gas; the angle-adjustable vacuum tube programmable heating furnace is also used to continue heating the bulk metal material to be tested according to the second heating temperature curve and output residual hydrogen mixed gas.

[0010] The temperature program controller is connected to the angle-adjustable vacuum tube programmable heating furnace and is used to control the first heating temperature curve and the second heating temperature curve.

[0011] The inlet of the condenser tube is connected to the angle-adjustable vacuum tube type programmable heater, and the condenser tube is used to cool and output the diffused hydrogen mixture and the residual hydrogen mixture.

[0012] The remote temperature gauge is connected to the outlet of the condenser tube and is used to detect the temperature of the diffused hydrogen mixture and the residual hydrogen mixture at the outlet of the condenser tube and transmit the temperature to the temperature feedback low-temperature constant temperature circulator.

[0013] The temperature feedback low-temperature constant temperature circulator is connected to the inlet of the condenser tube, the outlet of the condenser tube, and the remote temperature gauge, respectively. The temperature feedback low-temperature constant temperature circulator is used to control the temperature of the diffused hydrogen mixture in the condenser tube to 25°C based on the temperature of the diffused hydrogen mixture at the outlet of the condenser tube, and to control the temperature of the residual hydrogen mixture in the condenser tube to 25°C based on the temperature of the residual hydrogen mixture at the outlet of the condenser tube.

[0014] One end of the micro-bubble flow meter is connected to the outlet of the condenser tube, and the other end of the micro-bubble flow meter is connected to the gas bag with quick-connect fitting. The micro-bubble flow meter is used to measure the total amount of the diffused hydrogen mixture gas collected by the gas bag with quick-connect fitting and the total amount of the residual hydrogen mixture gas.

[0015] The gas chromatograph-mass spectrometer is used to detect the percentage of diffuse hydrogen and the percentage of residual hydrogen in the gas bag with quick-connect fitting.

[0016] Optionally, it also includes: a vacuum pump and a vacuum gauge;

[0017] The vacuum pump is connected to the angle-adjustable vacuum tube type programmable heating furnace and is used to evacuate the angle-adjustable vacuum tube type programmable heating furnace.

[0018] The vacuum gauge is connected to the angle-adjustable vacuum tube type programmable heater, the vacuum pump, and the condenser tube, respectively. The vacuum gauge is used to detect the vacuum environment inside the angle-adjustable vacuum tube type programmable heater.

[0019] Optionally, it may also include: a vent valve;

[0020] The vent valve is connected to the condenser and the microbubble flow meter respectively, and is used to vent air from the system; the system is a system for measuring the diffusible hydrogen and residual hydrogen content in bulk metal.

[0021] Optionally, the air bag with quick-connect fitting includes:

[0022] Airbag A and airbag B;

[0023] The gas bag a is used to collect the diffused hydrogen mixture;

[0024] The b-bag is used to collect the residual hydrogen mixture.

[0025] Optionally, the gas bag with quick-connect fitting is an aluminum-plastic composite film gas sampling bag.

[0026] Optionally, it also includes:

[0027] Nitrogen cylinder, float flow meter, first valve, second valve, third valve, fourth valve, fifth valve and sixth valve;

[0028] The nitrogen cylinder is used to store nitrogen.

[0029] The first valve is connected to the nitrogen cylinder and is used to control the opening and closing of the nitrogen cylinder;

[0030] The second valve is connected to the first valve and the float flow meter respectively, and is used to control the nitrogen flow rate output by the nitrogen cylinder to be less than the maximum limit flow rate of the micro-bubble flow meter by adjusting the opening value according to the nitrogen flow rate value displayed by the float flow meter.

[0031] The third valve is located between the angle-adjustable vacuum tube type programmable heater and the float flow meter, and is used to control the on / off connection between the angle-adjustable vacuum tube type programmable heater and the float flow meter.

[0032] The fourth valve is located between the vacuum gauge and the inlet of the condenser tube, and is used to control the connection and disconnection between the angle-adjustable vacuum tube programmable heater and the condenser tube.

[0033] The fifth valve is located between the vacuum gauge and the vacuum pump, and is used to control the on / off connection between the angle-adjustable vacuum tube programmable heating furnace and the vacuum pump.

[0034] The sixth valve is located between the outlet of the condenser tube and the microbubble flow meter, and is used to control the on / off connection between the condenser tube and the microbubble flow meter.

[0035] Optionally, the microbubble flow meter is placed horizontally, and the ambient temperature of the microbubble flow meter is 25°C and the ambient air pressure is 1 atmosphere.

[0036] Optionally, the angle-adjustable vacuum tube programmable heater is an angle-adjustable vacuum tube programmable heater with at least two inner diameter specifications.

[0037] To achieve the above objectives, the present invention also provides another solution:

[0038] A system for determining the content of diffusible hydrogen and residual hydrogen in bulk metal, comprising:

[0039] The temperature program controller controls the first heating temperature curve and the second heating temperature curve, so that the angle-adjustable vacuum tube programmable heating furnace heats the block metal material to be tested in stages according to the first heating temperature curve and the second heating temperature curve, and outputs diffused hydrogen mixture gas and residual hydrogen mixture gas in stages.

[0040] The temperature feedback low-temperature constant temperature circulator controls the temperature of the diffused hydrogen mixture and the residual hydrogen mixture in the condenser to 25°C based on the temperature of the diffused hydrogen mixture and the residual hydrogen mixture at the outlet of the condenser detected by the remote temperature gauge, and outputs the diffused hydrogen mixture and the residual hydrogen mixture.

[0041] A microbubble flow meter measures the total amount of the diffused hydrogen mixture collected by a gas bag with a quick-connect fitting and the total amount of the residual hydrogen mixture.

[0042] The percentage of diffusing hydrogen and the percentage of residual hydrogen in the gas bag with quick-connect fitting were detected by gas chromatography-mass spectrometry.

[0043] The content of diffuse hydrogen and the content of residual hydrogen are calculated based on the total amount of the diffuse hydrogen mixture, the total amount of the residual hydrogen mixture, the percentage of diffuse hydrogen, and the percentage of residual hydrogen.

[0044] Optionally, the first heating temperature curve heats the bulk metal material to be tested to 400°C and holds it at that temperature for 30 minutes until the diffusible hydrogen in the bulk metal material to be tested is completely released; the second heating temperature curve heats the bulk metal material to be tested to 650°C and holds it at that temperature for 30 minutes until the residual hydrogen in the bulk metal material to be tested is completely released.

[0045] According to specific embodiments provided by the present invention, the present invention discloses the following technical effects:

[0046] The present invention provides a system and method for determining the content of diffusible hydrogen and residual hydrogen in bulk metals. This system uses a temperature programmable controller to program and control a first and second heating temperature curve of an angle-adjustable vacuum tube type programmable heating furnace. The furnace heats the bulk metal material according to the first heating temperature curve, causing it to release diffusible hydrogen. Heating continues according to the second heating temperature curve, causing the metal material to release residual hydrogen, thus achieving the measurement of diffusible hydrogen and residual hydrogen released in stages. Attached Figure Description

[0047] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0048] Figure 1 This is a schematic diagram of the system for determining the content of diffusible hydrogen and residual hydrogen in bulk metals provided by the present invention.

[0049] Symbol explanation:

[0050] Nitrogen cylinder—1, adjustable-angle vacuum tube type programmable heater—2, vacuum gauge—3, condenser tube—4, remote temperature gauge—5, micro bubble flow meter—6, vent valve—7, gas bag with quick connector—8, float flow meter—9, temperature program controller—10, vacuum pump—11, temperature feedback low-temperature constant temperature circulator—12, gas chromatograph-mass spectrometer—13, first valve—14, third valve—15, second valve—16, fourth valve—17, fifth valve—18, sixth valve—19. Detailed Implementation

[0051] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0052] The purpose of this invention is to provide a system and method for determining the content of diffusible hydrogen and residual hydrogen in bulk metal. The system uses a temperature programmable controller 10 to program and control a first heating temperature curve and a second heating temperature curve of an angle-adjustable vacuum tube programmable heating furnace 2. The angle-adjustable vacuum tube programmable heating furnace 2 heats the bulk metal material according to the first heating temperature curve, causing it to release diffusible hydrogen. Heating continues according to the second heating temperature curve, causing the bulk metal material to release residual hydrogen, thus achieving the measurement of diffusible hydrogen and residual hydrogen released in stages.

[0053] To make the above-mentioned objects, features and advantages of the present invention more apparent and understandable, the present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.

[0054] Example 1

[0055] like Figure 1 As shown, the present invention provides a system for determining the content of diffusible hydrogen and residual hydrogen in bulk metal, which mainly includes: an angle-adjustable vacuum tube type programmable heating furnace 2, a condenser 4, a remote temperature meter 5, a micro bubble flow meter 6, a gas bag with quick connector 8, a temperature program controller 10, a temperature feedback low temperature constant temperature circulator 12, and a gas phase mass spectrometer 13.

[0056] The adjustable-angle vacuum tube programmable heating furnace 2 contains the bulk metal material to be tested. The bulk metal material to be tested is heated in stages according to the first heating temperature curve and the second heating temperature curve output by the temperature program controller 10, so that the bulk metal material to be tested releases diffused hydrogen and residual hydrogen in stages.

[0057] The angle-adjustable vacuum tube programmable heating furnace 2 heats the bulk metal material to be tested according to the first heating temperature curve and outputs a diffused hydrogen mixture gas; after the diffused hydrogen mixture gas is collected, the angle-adjustable vacuum tube programmable heating furnace 2 continues to heat the bulk metal material to be tested according to the second heating temperature curve and outputs a residual hydrogen mixture gas.

[0058] The temperature program controller 10 is connected to the angle-adjustable vacuum tube programmable heater 2 to control the first heating temperature curve and the second heating temperature curve.

[0059] The inlet of the condenser tube 4 is connected to the angle-adjustable vacuum tube type programmable heater 2, cooling and outputting the diffused hydrogen mixture and the residual hydrogen mixture. Specifically, a vacuum gauge 3 is installed between the inlet of the condenser tube 4 and the angle-adjustable vacuum tube type programmable heater 2, and a vacuum pump 11 is connected to the vacuum gauge 3. Before heating the angle-adjustable vacuum tube type programmable heater 2, the vacuum pump 11 evacuates the angle-adjustable vacuum tube type programmable heater 2. The vacuum gauge 3 is used to determine whether the vacuum pump 11 has completed evacuating the angle-adjustable vacuum tube type programmable heater 2. When the evacuation is completed, heating of the angle-adjustable vacuum tube type programmable heater 2 begins.

[0060] The remote temperature gauge 5 is connected to the outlet of the condenser tube 4 to detect the temperature of the diffused hydrogen mixture and the residual hydrogen mixture at the outlet of the condenser tube 4 and transmits the temperature to the temperature feedback low-temperature constant temperature circulator 12.

[0061] The temperature feedback low-temperature constant temperature circulator 12 is connected to the inlet of the condenser tube 4, the outlet of the condenser tube 4, and the remote temperature meter 5, respectively. Based on the temperature of the diffused hydrogen mixture and the temperature of the residual hydrogen mixture at the outlet of the condenser tube 4 detected by the remote temperature meter 5, the temperature of the diffused hydrogen mixture and the residual hydrogen mixture in the condenser tube 4 is controlled to be 25°C.

[0062] One end of the microbubble flow meter 6 is connected to the outlet of the condenser 4, and the other end is connected to the gas bag 8 with a quick-connect fitting. It measures the total amount of the diffused hydrogen mixture gas collected by the gas bag 8 with the quick-connect fitting and the total amount of the residual hydrogen mixture gas.

[0063] Specifically, the gas bag 8 with quick-connect fittings includes: gas bag a and gas bag b; gas bag a is used to collect the diffused hydrogen mixture; gas bag b is used to collect the residual hydrogen mixture. The gas bag 8 with quick-connect fittings can be an aluminum-plastic composite membrane gas sampling bag. The quick-connect fittings are used to facilitate the replacement of the gas bags during the experiment and to facilitate the separate collection and measurement of the diffused hydrogen mixture and the residual hydrogen mixture. Furthermore, to avoid the influence of external factors such as vibration, the microbubble flow meter 6 must be placed horizontally, and the ambient temperature of the microbubble flow meter 6 must be 25°C, and the ambient air pressure must be 1 atmosphere.

[0064] The gas chromatograph-mass spectrometer 13 is used to detect the percentage of diffusing hydrogen and the percentage of residual hydrogen in the gas bag 8 with quick-connect fittings. Specifically, the diffusing hydrogen mixture and the residual hydrogen mixture can be extracted from the gas bag using a sampling needle and then placed into the gas chromatograph 13 for detection.

[0065] Furthermore, this application also includes: a nitrogen cylinder 1, a float flow meter 9, a first valve 14, a second valve 16, a vent valve 7, a third valve 15, a fourth valve 17, a fifth valve 18, and a sixth valve 19.

[0066] The nitrogen cylinder 1 is used to store nitrogen gas; the first valve 14 is used to control the opening and closing of the nitrogen cylinder 1; the second valve 16, based on the nitrogen flow rate value output by the nitrogen cylinder 1 displayed by the float flowmeter 9, controls the nitrogen flow rate output by the nitrogen cylinder 1 to be less than the maximum limit flow rate of the micro-bubble flowmeter 6 by adjusting the opening value; the vent valve 7 is used to vent air from the system at the beginning of the experiment, specifically, this system is a system for determining the diffusible hydrogen and residual hydrogen content in the bulk metal; the third valve 15 is used to control the connection and disconnection between the angle-adjustable vacuum tube programmable heater 2 and the float flowmeter 9; the fourth valve 17 is used to control the connection and disconnection between the angle-adjustable vacuum tube programmable heater 2 and the condenser tube 4; the fifth valve 18 is used to control the connection and disconnection between the angle-adjustable vacuum tube programmable heater 2 and the vacuum pump 11; the sixth valve 19 is used to control the connection and disconnection between the condenser tube 4 and the micro-bubble flowmeter 6.

[0067] Example 2

[0068] Existing devices for determining hydrogen content in materials generally employ thermal conductivity detectors to measure the concentration of different components and convert it into an electrical signal to determine the volume of hydrogen gas. This integrated detection device is not only expensive, but also can only detect materials with small dimensions, which cannot meet the needs of determining hydrogen content in large-sized materials. In particular, for bulk metal specimens in the hydrogen embrittlement experiment, it is currently difficult to determine hydrogen content due to their generally large size.

[0069] In this embodiment, multiple adjustable-angle vacuum tube programmable heating furnaces 2 with different inner diameters can be set up to allow for the replacement of the appropriate size of the adjustable-angle vacuum tube programmable heating furnace 2 according to the size of the block metal material to be measured, thereby improving the flexibility and efficiency of the measurement.

[0070] Example 3

[0071] This embodiment provides a method for determining the content of diffusible hydrogen and residual hydrogen in bulk metals. This method is applied to the determination system for the content of diffusible hydrogen and residual hydrogen in bulk metals described in Embodiments 1 and 2.

[0072] The temperature program controller 10 controls the first heating temperature curve and the second heating temperature curve, so that the angle-adjustable vacuum tube programmable heating furnace 2 heats the block metal material to be tested in stages according to the first heating temperature curve and the second heating temperature curve, and releases diffused hydrogen and residual hydrogen in stages, and outputs diffused hydrogen mixed gas and residual hydrogen mixed gas in stages.

[0073] The temperature feedback low-temperature constant temperature circulator 12 controls the temperature of the diffused hydrogen mixture and the residual hydrogen mixture in the condenser tube 4 to 25°C based on the temperature of the diffused hydrogen mixture and the residual hydrogen mixture detected by the remote temperature gauge 5 at the outlet of the condenser tube 4, and outputs the diffused hydrogen mixture and the residual hydrogen mixture.

[0074] The microbubble flow meter 6 measures the total amount of the diffused hydrogen mixture collected by the gas bag 8 with quick-connect fitting and the total amount of the residual hydrogen mixture.

[0075] Gas chromatography-mass spectrometry 13 detects the percentage of diffuse hydrogen and the percentage of residual hydrogen in the gas bag 8 with quick-connect fitting.

[0076] The content of diffuse hydrogen and the content of residual hydrogen are calculated based on the total amount of the diffuse hydrogen mixture, the total amount of the residual hydrogen mixture, the percentage of diffuse hydrogen, and the percentage of residual hydrogen.

[0077] Specifically, the first heating temperature curve heats the bulk metal material to be tested to 400°C and holds it at that temperature for 30 minutes until the diffusible hydrogen in the bulk metal material to be tested is completely released; the second heating temperature curve heats the bulk metal material to be tested to 650°C and holds it at that temperature for 30 minutes until the residual hydrogen in the bulk metal material to be tested is completely released.

[0078] Furthermore, the specific implementation steps of the method for determining the diffusible hydrogen and residual hydrogen content in the bulk metal are as follows:

[0079] Step 1: Open the first valve 14, the third valve 15, the fourth valve 17, and the vent valve 7 that control the nitrogen cylinder 1; close the fifth valve 18 and the sixth valve 19; adjust the opening of the second valve 16, which controls the nitrogen flow rate from the nitrogen cylinder 1, to its maximum; and close the first valve 14, the second valve 16, the third valve 15, the fourth valve 17, and the vent valve 7 after the vent valve 7 has purged all the air from the system. The system described herein is a system for determining the diffusible hydrogen and residual hydrogen content in the bulk metal.

[0080] Step 2: Load the block metal material to be tested into the angle-adjustable vacuum tube programmable heating furnace 2. By adjusting the angle of the angle-adjustable vacuum tube programmable heating furnace 2, the block metal material to be tested is placed on the baffle inside the angle-adjustable vacuum tube programmable heating furnace 2 and located in the center position.

[0081] Step 3: Open the fifth valve 18 and use the vacuum pump 11 to evacuate the angle-adjustable vacuum tube programmable heating furnace 2. When the vacuum gauge 3 shows that the evacuation is complete, close the fifth valve 18.

[0082] Step 4: Control the first heating temperature curve of the angle-adjustable vacuum tube programmable heating furnace 2 through the temperature program controller 10, raise the temperature to 400℃ and keep it constant for 30 minutes until the diffusible hydrogen in the block metal material to be tested is completely released.

[0083] Step 5: Temperature feedback low-temperature constant temperature circulator 12 controls the temperature of the diffused hydrogen mixture at the outlet of the condenser tube 4 to 25°C based on the temperature of the diffused hydrogen mixture at the outlet of the condenser tube 4 output by the remote temperature meter 5. Then, it opens the first valve 14, the third valve 15, and the fourth valve 17, and connects the micro-bubble flow meter 6 to the gas bag a of the gas bag 8 with a quick connector. Then, it opens the sixth valve 19 and controls the opening value of the second valve 16 by observing the reading of the float flow meter 9, so that the nitrogen flow rate output by the nitrogen cylinder 1 is less than the maximum limit flow rate of the micro-bubble flow meter 6.

[0084] Step Six: After all the diffused hydrogen mixture has entered the a gas bag, close the second valve 16 and the sixth valve 19, disconnect the a gas bag from the micro-bubble flow meter 6, and read the total amount of diffused hydrogen mixture from the micro-bubble flow meter 6 and record it as V. dif .

[0085] Step 7: Close the third valve 15 and the fourth valve 17, and control the second heating temperature curve of the angle-adjustable vacuum tube programmable heating furnace 2 through the temperature program controller 10 to raise the temperature to 650°C and maintain it at a constant temperature for 30 minutes until the residual hydrogen in the block metal material to be tested is completely released.

[0086] Step 8: Reset the metering data of the micro-bubble flow meter 6 to zero, connect the micro-bubble flow meter 6 to the b-bag of the gas bag 8 with quick connector, open the third valve 15, the fourth valve 17 and the sixth valve 19, and control the opening value of the second valve 16 by observing the float flow meter 9, so that the nitrogen flow rate output by the nitrogen cylinder 1 is less than the maximum limit flow rate of the micro-bubble flow meter 6.

[0087] Step 9: After all the residual hydrogen mixture has entered the b-bag, close the first valve 14, the second valve 16, the third valve 15, the fourth valve 17, and the sixth valve 19. Disconnect the b-bag from the micro-bubble flow meter 6, and read the total amount of the residual hydrogen mixture from the micro-bubble flow meter 6 and record it as V. rem .

[0088] Step 10: Extract the diffuse hydrogen mixture from the gas bag a and analyze it using a gas chromatograph-mass spectrometer 13. The percentage of diffuse hydrogen is denoted as P. dif The residual hydrogen mixture in the b gas bag is extracted and analyzed by the gas chromatograph-mass spectrometer 13. The percentage of residual hydrogen is denoted as P. rem .

[0089] The diffusible hydrogen content H released by the bulk metal material to be tested dif for:

[0090] .

[0091] The residual hydrogen content H released by the bulk metal material to be tested rem for:

[0092] .

[0093] The total hydrogen content H released by the bulk metal material to be tested tot for:

[0094] .

[0095] The various embodiments in this specification are described in a progressive manner, with each embodiment focusing on the differences from other embodiments. The same or similar parts between the various embodiments can be referred to each other.

[0096] This document uses specific examples to illustrate the principles and implementation methods of the present invention. The descriptions of the above embodiments are only for the purpose of helping to understand the method and core ideas of the present invention. Furthermore, those skilled in the art will recognize that, based on the ideas of the present invention, there will be changes in the specific implementation methods and application scope. Therefore, the content of this specification should not be construed as a limitation of the present invention.

Claims

1. A system for determining the content of diffusible hydrogen and residual hydrogen in bulk metal, characterized in that, include: Angle-adjustable vacuum tube type programmable heating furnace, condenser tube, remote temperature meter, micro bubble flow meter, gas bag with quick connector, temperature program controller, temperature feedback low temperature constant temperature circulator and gas phase mass spectrometer. The adjustable-angle vacuum tube programmable heating furnace contains the bulk metal material to be tested. The bulk metal material to be tested is heated in stages according to the first heating temperature curve and the second heating temperature curve output by the temperature program controller, so that the bulk metal material to be tested releases diffused hydrogen and residual hydrogen in stages. The angle-adjustable vacuum tube programmable heating furnace is used to heat the bulk metal material to be tested according to the first heating temperature curve and output diffused hydrogen mixed gas; the angle-adjustable vacuum tube programmable heating furnace is also used to continue heating the bulk metal material to be tested according to the second heating temperature curve and output residual hydrogen mixed gas. The temperature program controller is connected to the angle-adjustable vacuum tube programmable heating furnace and is used to control the first heating temperature curve and the second heating temperature curve. The inlet of the condenser tube is connected to the angle-adjustable vacuum tube type programmable heater, and the condenser tube is used to cool and output the diffused hydrogen mixture and the residual hydrogen mixture. The remote temperature gauge is connected to the outlet of the condenser tube and is used to detect the temperature of the diffused hydrogen mixture and the residual hydrogen mixture at the outlet of the condenser tube and transmit the temperature to the temperature feedback low-temperature constant temperature circulator. The temperature feedback low-temperature constant temperature circulator is connected to the inlet of the condenser tube, the outlet of the condenser tube, and the remote temperature gauge, respectively. The temperature feedback low-temperature constant temperature circulator is used to control the temperature of the diffused hydrogen mixture in the condenser tube to 25°C based on the temperature of the diffused hydrogen mixture at the outlet of the condenser tube, and to control the temperature of the residual hydrogen mixture in the condenser tube to 25°C based on the temperature of the residual hydrogen mixture at the outlet of the condenser tube. One end of the micro-bubble flow meter is connected to the outlet of the condenser tube, and the other end of the micro-bubble flow meter is connected to the gas bag with quick-connect fitting. The micro-bubble flow meter is used to measure the total amount of the diffused hydrogen mixture gas collected by the gas bag with quick-connect fitting and the total amount of the residual hydrogen mixture gas. The gas chromatograph-mass spectrometer is used to detect the percentage of diffuse hydrogen and the percentage of residual hydrogen in the gas bag with quick-connect fitting.

2. The system for determining the content of diffusible hydrogen and residual hydrogen in bulk metal according to claim 1, characterized in that, Also includes: Vacuum pumps and vacuum gauges; The vacuum pump is connected to the angle-adjustable vacuum tube type programmable heating furnace and is used to evacuate the angle-adjustable vacuum tube type programmable heating furnace. The vacuum gauge is connected to the angle-adjustable vacuum tube type programmable heater, the vacuum pump, and the condenser tube, respectively. The vacuum gauge is used to detect the vacuum environment inside the angle-adjustable vacuum tube type programmable heater.

3. The system for determining the content of diffusible hydrogen and residual hydrogen in bulk metal according to claim 2, characterized in that, Also includes: Vent valve; The vent valve is connected to the condenser and the micro-bubble flow meter respectively, and is used to vent air from the system. The system is a system for determining the content of diffusible hydrogen and residual hydrogen in bulk metals.

4. The system for determining the content of diffusible hydrogen and residual hydrogen in bulk metals according to claim 3, characterized in that, The air bag with quick-connect fittings includes: Airbag A and airbag B; The gas bag a is used to collect the diffused hydrogen mixture; The b-bag is used to collect the residual hydrogen mixture.

5. The system for determining the content of diffusible hydrogen and residual hydrogen in bulk metal according to claim 4, characterized in that, The gas bag with quick-connect fitting is an aluminum-plastic composite film gas sampling bag.

6. The system for determining the content of diffusible hydrogen and residual hydrogen in bulk metal according to claim 4, characterized in that, Also includes: Nitrogen cylinder, float flow meter, first valve, second valve, third valve, fourth valve, fifth valve and sixth valve; The nitrogen cylinder is used to store nitrogen. The first valve is connected to the nitrogen cylinder and is used to control the opening and closing of the nitrogen cylinder; The second valve is connected to the first valve and the float flow meter respectively, and is used to control the nitrogen flow rate output by the nitrogen cylinder to be less than the maximum limit flow rate of the micro-bubble flow meter by adjusting the opening value according to the nitrogen flow rate value displayed by the float flow meter. The third valve is located between the angle-adjustable vacuum tube type programmable heater and the float flow meter, and is used to control the on / off connection between the angle-adjustable vacuum tube type programmable heater and the float flow meter. The fourth valve is located between the vacuum gauge and the inlet of the condenser tube, and is used to control the connection and disconnection between the angle-adjustable vacuum tube programmable heater and the condenser tube. The fifth valve is located between the vacuum gauge and the vacuum pump, and is used to control the on / off connection between the angle-adjustable vacuum tube programmable heating furnace and the vacuum pump. The sixth valve is located between the outlet of the condenser tube and the microbubble flow meter, and is used to control the on / off connection between the condenser tube and the microbubble flow meter.

7. The system for determining the content of diffusible hydrogen and residual hydrogen in bulk metals according to claim 1, characterized in that, The microbubble flow meter is placed horizontally, and the ambient temperature of the microbubble flow meter is 25°C and the ambient air pressure is 1 atmosphere.

8. The system for determining the content of diffusible hydrogen and residual hydrogen in bulk metal according to claim 1, characterized in that, The angle-adjustable vacuum tube programmable heater is an angle-adjustable vacuum tube programmable heater with at least two inner diameter specifications.

9. A method for determining the content of diffusible hydrogen and residual hydrogen in bulk metal, applied to the system for determining the content of diffusible hydrogen and residual hydrogen in bulk metal according to any one of claims 1-8, characterized in that, include: The temperature program controller controls the first heating temperature curve and the second heating temperature curve, so that the angle-adjustable vacuum tube programmable heating furnace heats the block metal material to be tested in stages according to the first heating temperature curve and the second heating temperature curve, and outputs diffused hydrogen mixture gas and residual hydrogen mixture gas in stages. The temperature feedback low-temperature constant temperature circulator controls the temperature of the diffused hydrogen mixture and the residual hydrogen mixture in the condenser to 25°C based on the temperature of the diffused hydrogen mixture and the residual hydrogen mixture at the outlet of the condenser detected by the remote temperature gauge, and outputs the diffused hydrogen mixture and the residual hydrogen mixture. A microbubble flow meter measures the total amount of the diffused hydrogen mixture collected by a gas bag with a quick-connect fitting and the total amount of the residual hydrogen mixture. The percentage of diffusing hydrogen and the percentage of residual hydrogen in the gas bag with quick-connect fitting were detected by gas chromatography-mass spectrometry. The content of diffuse hydrogen and the content of residual hydrogen are calculated based on the total amount of the diffuse hydrogen mixture, the total amount of the residual hydrogen mixture, the percentage of diffuse hydrogen, and the percentage of residual hydrogen.

10. The method for determining the content of diffusible hydrogen and residual hydrogen in bulk metal according to claim 9, characterized in that, The first heating temperature curve heats the bulk metal material to be tested to 400°C and holds it at that temperature for 30 minutes until the diffusible hydrogen in the bulk metal material to be tested is completely released; the second heating temperature curve heats the bulk metal material to be tested to 650°C and holds it at that temperature for 30 minutes until the residual hydrogen in the bulk metal material to be tested is completely released.

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