Outdoor portable in-situ hydrogen permeation measurement device

Abstract

This invention discloses an outdoor portable in-situ hydrogen permeation measurement device, comprising a cavity, a sealing plug on the opening at the upper end of the cavity, a NaOH aqueous solution inside the cavity, and an auxiliary electrode and a reference electrode inside the cavity. The upper ends of the auxiliary electrode and the reference electrode extend outside the cavity and are connected to an electrochemical workstation. The cross-section of the cavity is a rectangle extending left and right. A magnetic shielding layer is provided on the outer side and lower end of the cavity. Magnetic adsorbers for adsorbing the object to be measured are provided on the left and right sides of the magnetic shielding layer. A liquid guide port corresponding to the opening at the lower end of the cavity is provided at the lower part of the magnetic shielding layer, and a rectangular groove is provided on the lower surface of the magnetic shielding layer around the liquid guide port. This invention is characterized by facilitating in-situ hydrogen permeation measurement outdoors, automatically shielding electromagnetic interference, mitigating the impact of environmental temperature changes, good stability, and high measurement accuracy.

Description

Technical Field

[0001] This invention relates to the field of non-destructive measurement of materials and electrochemical safety assessment of special equipment, and in particular to an outdoor portable in-situ hydrogen permeation measuring device suitable for online measurement. Background Technology

[0002] In the production, liquefaction, high-pressure storage, transmission pipelines, and various hydrogen-related industrial applications (such as petrochemicals and metallurgy), metal equipment (especially widely used iron-based alloy pipelines and storage tanks) inevitably needs to be exposed to high-pressure, high-purity hydrogen or highly corrosive hydrogen-related media such as hydrogen sulfide for a long time.

[0003] Hydrogen molecules readily undergo catalytic dissociation on metal surfaces, reducing to small, active hydrogen atoms. These active hydrogen atoms possess exceptional penetrability, easily overcoming the energy barrier of the metal surface to invade and diffuse into the metal lattice. Subsequently, they accumulate in large quantities at hydrogen traps such as grain boundaries, dislocations, non-metallic inclusions, or localized micro-defects. As the local hydrogen atom concentration continues to increase, hydrogen atoms spontaneously recombine to form hydrogen molecules, generating enormous localized expansion pressure at micro-defects. This leads to irreversible and severe material degradation phenomena: hydrogen-induced cracking (HIC), hydrogen embrittlement (HE), hydrogen-induced blistering (HB), and stress-directed hydrogen-induced cracking (SOHIC).

[0004] Hydrogen damage typically lies dormant within materials, manifesting macroscopically as brittle fracture without warning, preceded by almost no obvious macroscopic plastic deformation. It can easily lead to sudden tearing, leakage, or even catastrophic explosions in high-pressure hydrogen-related equipment. Therefore, in-situ, online real-time monitoring of hydrogen permeation flux in in-service hydrogen-related equipment, and accurate acquisition of key parameters such as the effective hydrogen diffusion coefficient and apparent hydrogen flux within the material, are of significant engineering strategic importance and urgent practical need for scientifically assessing the hydrogen damage sensitivity of equipment, establishing risk-based inspection (RBI) dynamic assessment models, and accurately predicting the remaining safe life of the equipment. Summary of the Invention

[0005] The purpose of this invention is to overcome the shortcomings of existing hydrogen permeation measurement devices that cannot perform hydrogen permeation measurements in outdoor industrial sites with strong electromagnetic interference and large temperature differences, and to provide an outdoor portable in-situ hydrogen permeation measurement device suitable for online measurement.

[0006] To achieve the above objectives, the present invention adopts the following technical solution: An outdoor portable in-situ hydrogen permeation measurement device includes a cavity, a sealing plug on the opening at the upper end of the cavity, an aqueous NaOH solution inside the cavity, and an auxiliary electrode and a reference electrode inside the cavity. The upper ends of the auxiliary electrode and the reference electrode extend outside the cavity and are connected to an electrochemical workstation. The cross-section of the cavity is a rectangle extending left and right. A magnetic shielding layer is provided on the outer and lower surfaces of the cavity. Magnetic adsorbers for adsorbing the measured object are provided on the left and right sides of the magnetic shielding layer. A liquid guide port corresponding to the opening at the lower end of the cavity is provided at the lower part of the magnetic shielding layer. A rectangular groove is provided on the lower surface of the magnetic shielding layer around the liquid guide port. The magnetic shielding layer inside the groove has a convex structure with reversed top and bottom. A slot is provided on the upper side wall of the groove. It also includes a detachable connecting base connected to the convex structure and the slot.

[0007] Magnetic adsorbers are used to adsorb in-situ hydrogen permeation measurement devices onto the container, pipe, or plate being measured, which serves as the working electrode. The magnetic shielding layer provides thermal isolation, mitigating the impact of external environmental temperature fluctuations on the NaOH aqueous solution, stabilizing the Arrhenius reaction and diffusion kinetic constants of the liquid phase inside the cavity, and ensuring the stability and accuracy of the measurement. It can also convert and dissipate radio frequency and power frequency alternating electromagnetic interference (EMI) in the industrial environment into micro-heat energy, ensuring the accuracy of hydrogen permeation measurement. Furthermore, it can forcibly "absorb" and constrain the stray leakage flux radiated inward by the magnetic adsorber. The connecting base facilitates connection to the surfaces of various types of smooth, high-curvature containers, laboratory plates, pipes, or spherical tanks to meet different measurement requirements.

[0008] Preferably, the magnetic shielding layer comprises a buffer layer, an alternating electromagnetic shielding mesh layer, and an iron outer shell connected sequentially from the inside out.

[0009] Preferably, the cavity is made of polytetrafluoroethylene (PTFE) material with a thickness of 2mm-5mm.

[0010] The cavity, made of polytetrafluoroethylene (PTFE), possesses extremely strong corrosion resistance and chemical inertness. It is non-brittle at cryogenic temperatures and does not melt at high temperatures, making it suitable for extreme temperature conditions. It is non-stick and easy to clean: with extremely low surface energy, materials do not easily adhere to it or form scale, and it can be cleaned simply by rinsing. It has good insulation properties, with a dielectric constant of 2.0-2.1 and extremely low high-frequency loss, making it suitable for high-frequency / high-voltage insulation scenarios. It has extremely high chemical inertness and electrical insulation, defining the lateral fluid and electrical boundaries of the cavity and cutting off the conductive path for leakage of minute measurement currents to the external metal structure.

[0011] Preferably, the buffer layer is made of an aerogel composite material with a nanoscale porous network structure and has a thickness of 3mm-5mm.

[0012] The buffer layer tightly covers the outside of the cavity and has extremely low thermal conductivity. It establishes a thermally isolated vacuum zone between the NaOH aqueous solution and the outdoor atmospheric environment, which can suppress the impact of external temperature fluctuations and stabilize the Arrhenius reaction and diffusion kinetic constants of the liquid phase system inside the cavity.

[0013] Preferably, the alternating electromagnetic shielding mesh layer is made of permalloy woven or wound, with a thickness of 2mm-3mm.

[0014] The variable electromagnetic shielding layer covers the outside of the buffer layer, converting radio frequency and power frequency alternating electromagnetic radiation interference (EMI) in the field space into micro-heat energy and dissipating it, preventing it from coupling to the micro-current signal acquisition circuit of the electrochemical workstation.

[0015] Preferably, the outer shell is machined from DT4 electrical pure iron with a thickness of 5mm-8mm.

[0016] The outer shell serves as both the main rigid frame of the device to resist external mechanical impacts and the forced absorption and constraint of stray leakage magnetic flux radiating inward from the magnetic adsorber, thereby creating a safe zone with zero magnetic field inside the cavity and avoiding the Lorentz deflection interference of the static magnetic field on the electrolyte ions.

[0017] Preferably, the connecting base includes a base body, an opening in the base body adapted to the convex structure, and a retainer on the upper part of the base body that can cooperate with the retainer groove; the lower surface of the base body is flat, and a sealing gasket is provided on the lower surface of the base body.

[0018] The aforementioned connection base is suitable for magnetic adsorption connection with smooth, large-curvature containers or laboratory strips to measure the hydrogen permeation of the containers or laboratory strips.

[0019] Preferably, the lower surface of the seat is arc-shaped, and the lower surface of the seat is connected to the arc-shaped pipe connecting plate, and a sealing gasket is provided on the lower surface of the arc-shaped pipe connecting plate.

[0020] The connecting base with the arc-shaped pipe connecting plate is suitable for connecting to the surface of pipes or spherical tanks. By setting the arc-shaped pipe connecting plate with different curvature, it can be connected to the surface of pipes or spherical tanks of different sizes and models, so as to measure the hydrogen permeation of pipes or spherical tank materials of different sizes and models.

[0021] Preferably, the magnetic adsorbent includes two lower iron blocks, two upper iron blocks, a lower bar magnet extending left and right between the two lower iron blocks, and two upper bar magnets extending left and right between the two upper iron blocks; the upper bar magnets are mounted on a plastic handle; the two lower iron blocks and the two upper iron blocks are connected by magnetic attraction; the lower bar magnets are magnetically connected to the two lower iron blocks respectively; the two upper bar magnets are magnetically connected to the upper iron blocks respectively; and the lower iron blocks of the two magnetic adsorbents near the outer shell are magnetically connected to the left and right sides of the outer shell respectively.

[0022] The structure of the magnetic adsorber makes it simple and convenient to adsorb and desorb the magnetic adsorber onto the object being tested.

[0023] Preferably, a cavity protective plug is provided on the opening at the lower end of the cavity.

[0024] After the measurement is completed, the NaOH aqueous solution inside the cavity is drawn out, the inside of the cavity is cleaned, the opening at the lower end of the cavity is closed with the cavity protective plug, and the sealing plug is placed on the opening at the upper end of the cavity to keep the inside of the cavity clean.

[0025] Therefore, the present invention has the following beneficial effects: The cavity has extremely strong corrosion resistance, extremely high chemical inertness and electrical insulation, which can cut off the conductive path of leakage of small measurement current to the external metal structure. The buffer layer establishes a thermally isolated vacuum zone between the NaOH aqueous solution and the outdoor atmospheric environment, which smooths out the impact of sudden external temperature fluctuations, stabilizes the Arrhenius reaction and diffusion kinetic constant of the liquid phase inside the cavity, and ensures the stability and accuracy of the measurement. The variable electromagnetic shielding layer converts radio frequency and power frequency alternating electromagnetic interference (EMI) in the industrial field into micro-heat energy and dissipates it, ensuring the accuracy of hydrogen permeation measurement. The outer shell serves as the main load-bearing rigid frame and can forcibly "absorb" and constrain the stray leakage magnetic flux radiating inward from the magnetic adsorber. The connecting base facilitates connection to the surfaces of various types of smooth, high-curvature containers, laboratory plates, pipes, or spherical tanks to meet different measurement requirements. It facilitates in-situ hydrogen permeation measurement outdoors, can automatically shield against electromagnetic interference and smooth out the impact of external temperature fluctuations, has good stability, and high measurement accuracy. Attached Figure Description

[0026] Figure 1 This is a schematic diagram of the structure of the present invention; Figure 2 yes Figure 1 A magnified view of a portion of the cavity and magnetic shielding layer; Figure 3 This is a cross-sectional view of the connecting base of the present invention; Figure 4 This is another cross-sectional view of the connecting base of the present invention; Figure 5 This is a schematic diagram of the magnetic adsorber and the pipe under test according to the present invention. Detailed Implementation

[0027] The present invention will now be further described with reference to the accompanying drawings and specific embodiments.

[0028] Example like Figures 1-2 The illustrated embodiment is an outdoor portable in-situ hydrogen permeation measurement device, including a cavity 1, a sealing plug 11 located at the opening at the upper end of the cavity, a NaOH aqueous solution 13 located inside the cavity, an auxiliary electrode 14 and a reference electrode 15 located inside the cavity; the upper ends of the auxiliary electrode and the reference electrode both extend outside the cavity and are connected to an electrochemical workstation; the cross-section of the cavity is a rectangle extending left and right; a magnetic shielding layer 2 is provided on the outer surface and lower end surface of the cavity; magnetic adsorbers 3 for adsorbing the object to be measured are respectively provided on the left and right sides of the magnetic shielding layer; a liquid guide port corresponding to the opening at the lower end of the cavity is provided at the lower part of the magnetic shielding layer; a rectangular groove 21 is provided on the lower surface of the magnetic shielding layer around the liquid guide port; the magnetic shielding layer inside the groove has a convex structure 22 with upside down reversible shape; a slot 23 is provided on the upper side wall of the groove; and a detachable connecting base 4 is also included, which is connected to the convex structure and the slot. A cavity protective plug 12 is provided at the opening at the lower end of the cavity.

[0029] The magnetic shielding layer includes a buffer layer 24, an alternating electromagnetic shielding mesh layer 25, and an iron outer shell 26, which are connected sequentially from the inside to the outside.

[0030] The cavity is made of polytetrafluoroethylene (PTFE) material with a thickness of 5mm; the buffer layer is made of aerogel composite material with a nanoscale porous network structure with a thickness of 2mm; the alternating electromagnetic shielding mesh layer is made of permalloy woven or wound with a thickness of 3mm; and the outer shell is machined from DT4 electrical pure iron with a thickness of 6mm.

[0031] like Figure 3 As shown, the connecting base includes a base body 41, an opening 42 adapted to the convex structure inside the base body, and a card slot 43 on the upper part of the base body that can cooperate with the card slot; the lower surface of the base body is flat, and a sealing gasket is provided on the lower surface of the base body.

[0032] like Figure 4 As shown, the lower surface of the seat is arc-shaped, and the lower surface of the seat is connected to the arc-shaped pipe connecting plate 44. A sealing gasket is provided on the lower surface of the arc-shaped pipe connecting plate. Figures 3-4 As shown, a sealing ring 45 is also provided.

[0033] like Figure 1 , Figure 5 As shown, the magnetic adsorber includes two lower iron blocks 31, two upper iron blocks 32, a lower bar magnet 33 extending left and right between the two lower iron blocks, and two upper bar magnets 34 extending left and right between the two upper iron blocks; the upper bar magnets are mounted on a plastic handle 35; the two lower iron blocks and the two upper iron blocks are connected by magnetic attraction; the lower bar magnets are magnetically attracted to the two lower iron blocks respectively, and the two upper bar magnets are magnetically attracted to the upper iron blocks respectively; the lower iron blocks of the two magnetic adsorbers near the outer shell are magnetically attracted to the left and right sides of the outer shell respectively.

[0034] In-situ hydrogen permeation measurement of the outdoor pipeline under test using this invention: Step 1: Clean and grind the surface of the pipe to be tested. Select a connecting base with an arc-shaped pipe connecting plate. Align the connecting base with the convex structure and slot of the in-situ hydrogen permeation measuring device and seal it so that the sealing gasket at the bottom of the connecting base contacts the ground part of the pipe to be tested. Step 2: Rotate the plastic handle so that the N and S poles of the lower and upper bar magnets of the magnetic attractor are aligned. Figure 1 As shown, the strong magnetic attraction generated by the two upper bar magnets of the magnetic adsorber firmly attracts the pipe to be tested, so that the sealing gasket seals the connection base to the pipe to be tested. Step 3: Remove the sealing plug from the opening at the top of the cavity, slowly inject 0.2 mol / L NaOH aqueous solution into the cavity until the NaOH aqueous solution completely submerges the vertically suspended auxiliary electrode and reference electrode, and then cover the opening at the top of the cavity with the sealing plug. Step 4: Connect the auxiliary electrode, reference electrode, and the test pipeline (which serves as the working electrode) to the electrochemical workstation, and set the constant potential polarization parameters in the electrochemical workstation. Step 5: Once the potential of the electrochemical workstation stabilizes, start the measurement program, monitor and record the hydrogen permeation current density in real time, and plot the hydrogen permeation curve. Step 6: After the electrochemical workstation has been in operation for 96 hours, shut it down. Disconnect the auxiliary electrode, reference electrode, and the tested pipeline from the electrochemical workstation. Use a pump to remove the NaOH aqueous solution from the chamber. Rotate the plastic handle to align the N and S poles of the lower and upper bar magnets of the magnetic adsorber. Figure 5 As shown in the figure, the in-situ hydrogen permeation measuring device is removed from the surface of the pipe being measured; Clean the inside of the cavity thoroughly, close the opening at the bottom of the cavity with the cavity protector, and cover the opening at the top of the cavity with the sealing plug to keep the inside of the cavity clean.

[0035] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. An outdoor portable in-situ hydrogen permeation measurement device, characterized in that, The device includes a cavity (1), a sealing plug (11) on the opening at the upper end of the cavity, an aqueous solution of NaOH in the cavity (13), an auxiliary electrode (14) and a reference electrode (15) in the cavity; the upper ends of the auxiliary electrode and the reference electrode extend out of the cavity and are connected to the electrochemical workstation; the cross-section of the cavity is a rectangle extending from left to right; a magnetic shielding layer (2) is provided on the outer side and the lower end of the cavity; magnetic adsorbers (3) for adsorbing the test object are provided on the left and right sides of the magnetic shielding layer; a liquid guide port corresponding to the opening at the lower end of the cavity is provided at the lower part of the magnetic shielding layer; a rectangular groove (21) is provided on the lower surface of the magnetic shielding layer around the liquid guide port; the magnetic shielding layer inside the groove has a convex structure (22) with the top and bottom reversed; a slot (23) is provided on the upper side wall of the groove; and a detachable connecting base (4) is connected to the convex structure and the slot.

2. The portable outdoor in-situ hydrogen permeation measurement device according to claim 1, characterized in that, The magnetic shielding layer includes a buffer layer (24), an alternating electromagnetic shielding mesh layer (25), and an iron outer shell (26) connected sequentially from the inside to the outside.

3. The portable outdoor in-situ hydrogen permeation measurement device according to claim 1, characterized in that, The cavity is made of polytetrafluoroethylene (PTFE) with a thickness of 2mm-5mm.

4. The portable outdoor in-situ hydrogen permeation measuring device according to claim 2, characterized in that, The buffer layer is made of aerogel composite material with a nanoscale porous network structure and has a thickness of 3mm-5mm.

5. The portable outdoor in-situ hydrogen permeation measurement device according to claim 2, characterized in that, The alternating electromagnetic shielding mesh layer is made of permalloy woven or wound, with a thickness of 2mm-3mm.

6. The portable outdoor in-situ hydrogen permeation measurement device according to claim 2, characterized in that, The outer shell is machined from DT4 electrical pure iron with a thickness of 5mm-8mm.

7. The portable outdoor in-situ hydrogen permeation measurement device according to claim 1, characterized in that, The connecting base includes a base body (41), an opening (42) adapted to the convex structure in the base body, and a card slot (43) on the upper part of the base body that can cooperate with the card slot; the lower surface of the base body is flat, and a sealing gasket is provided on the lower surface of the base body.

8. The portable outdoor in-situ hydrogen permeation measurement device according to claim 7, characterized in that, The lower surface of the seat is arc-shaped and is connected to the arc-shaped pipe connecting plate (44). A sealing gasket is provided on the lower surface of the arc-shaped pipe connecting plate.

9. The outdoor portable in-situ hydrogen permeation measuring device according to claim 2, 3, 4, 5, 6, or 7, characterized in that, The magnetic adsorber includes two lower iron blocks (31), two upper iron blocks (32), a lower bar magnet (33) extending left and right between the two lower iron blocks, and two upper bar magnets (34) extending left and right between the two upper iron blocks; the upper bar magnets are mounted on a plastic handle (35); the two lower iron blocks and the two upper iron blocks are connected by magnetic attraction; the lower bar magnets are magnetically attracted to the two lower iron blocks respectively; the two upper bar magnets are magnetically attracted to the upper iron blocks respectively; the lower iron blocks of the two magnetic adsorbers near the outer shell are magnetically attracted to the left and right sides of the outer shell respectively.

10. The portable outdoor in-situ hydrogen permeation measuring device according to claim 1, characterized in that, A cavity protection plug (12) is provided on the opening at the lower end of the cavity.

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