Novel closed metal analysis sampling device
By designing a closed metal analysis and sampling device, the corrosion and cross-contamination of the sampling pipeline are solved, efficient and safe sample analysis and resource utilization are achieved, and the accuracy and working efficiency of the analysis results are improved.
Patent Information
- Application Number
- CN202421926067.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-08-09
- Publication Date
- 2025-07-22
- Estimated Expiration
- 2034-08-09
AI Technical Summary
When existing sampling devices face samples with extreme chemical properties such as strong acids and strong alkalis, they are prone to corrosion, residues or cross-contamination of the sampling pipeline, affecting the accuracy and reliability of the analysis results. At the same time, they fail to effectively utilize gas resources, which poses safety risks.
A closed metal analysis sampling device is designed, including sampling tanks, helium cylinders, nitrogen cylinders, vacuum buffer bottles and gas chromatographs. It is connected through the main pipe and equipped with control components such as valves and pressure reducers to achieve accurate control and safe transfer of gas, and integrate sampling and analysis functions.
It ensures the safety and accuracy of the sampling process, reduces analysis errors, improves work efficiency, realizes the reuse of gas resources, and reduces the risk of environmental pollution.
Smart Images
Figure CN223139491U_ABST
Abstract
Description
Technical Field
[0001] This application relates to the technical field of chemical metal analysis, and more specifically, to a novel airtight metal analysis sampling device. Background Art
[0002] In today's rapidly developing chemical industry and the field of high-purity electronic gas manufacturing, accurately analyzing the metal element content has become a crucial link in ensuring product quality and safety. The samples to be tested in these industries often carry extreme chemical properties such as strong acids and strong alkalis, as well as potential toxicity and harmfulness, and are prone to reacting with the components in the air. Therefore, the sampling process must be carried out in a highly airtight and safe environment. However, when dealing with such complex samples, the existing sampling devices often face challenges due to design limitations. During the sampling process, the characteristics of the sample itself may inadvertently cause corrosion, residue, or cross-contamination to the sampling pipeline, which not only increases the complexity of subsequent analysis work but also seriously damages the accuracy and reliability of the analysis results.
[0003] After the detection is completed, the remaining gas is often directly introduced into the absorbent for treatment to eliminate potential safety hazards. However, this approach ignores the valuable resources or reuse value that may still be contained in the gas, resulting in unnecessary resource waste and environmental burden.
[0004] Given the special nature of the sample, if the sampling process cannot achieve complete airtightness, it not only threatens the health and safety of operators but also may trigger environmental pollution incidents, posing a potential threat to the production environment and the ecosystem.
[0005] In view of the significant defects and deficiencies in the above background art, this application aims to provide an airtight metal analysis sampling device that combines high safety and pollution-free through innovative design. Summary of the Utility Model
[0006] Based on the above problems, this application proposes a novel airtight metal analysis sampling device to solve the technical problems that during the sampling process, the characteristics of the sample itself may inadvertently cause corrosion, residue, or cross-contamination to the sampling pipeline, which not only increases the complexity of subsequent analysis work but also seriously damages the accuracy and reliability of the analysis results.
[0007] To solve the above technical problems, the technical solution adopted by this utility model is:
[0008] A novel airtight metal analysis sampling device, comprising a sampling tank, a steel cylinder to be tested, a helium cylinder, a nitrogen cylinder respectively connected to the sampling tank through a main pipe, and a vacuum buffer bottle connected to the sampling tank through the main pipe;
[0009] A gas chromatograph is provided between the sampling tank and the helium gas cylinder, and a balance is provided below the sampling tank.
[0010] In a specific feasible embodiment, a sample outlet and a sample inlet are provided on the sampling tank. The steel cylinder to be tested, the helium gas cylinder, the nitrogen gas cylinder, and the gas chromatograph are connected to the sample inlet through the main pipe. The vacuum buffer bottle is connected to the sample outlet through the main pipe. Valves are installed between the sample outlet and the sample inlet and the main pipe.
[0011] In a specific feasible embodiment, vacuum pumps are connected to both the vacuum buffer bottle and the steel cylinder to be tested and the helium gas cylinder.
[0012] In a specific feasible embodiment, a pressure reducer and a first mass flowmeter are provided between the nitrogen gas cylinder and the main pipe.
[0013] In a specific feasible embodiment, a pressure gauge and a second mass flowmeter are provided between the vacuum buffer bottle and the sample outlet.
[0014] In a specific feasible embodiment, pressure reducers are connected between the steel cylinder to be tested and the helium gas cylinder and the main pipe.
[0015] In a specific feasible embodiment, a temperature-controlled heating jacket is provided on the steel cylinder to be tested.
[0016] Positive effects of the present utility model:
[0017] The entire device adopts a closed design. From the steel cylinder to be tested, the helium gas cylinder, the nitrogen gas cylinder to the sampling tank and the vacuum buffer bottle, they are all connected through the main pipe and equipped with valve control, effectively preventing gas leakage and ensuring the accuracy and safety of sampling.
[0018] It integrates multiple functions such as sampling, gas injection, vacuum treatment, gas analysis, and mass measurement, greatly simplifying the operation process and improving work efficiency. Especially the setting of the gas chromatograph and the balance enables direct gas component analysis and mass determination after sampling, reducing errors during the sample transfer process.
[0019] By setting components such as pressure reducers and mass flowmeters, the gas flow rate and pressure can be precisely controlled to ensure the accuracy of sampling and analysis. At the same time, the design of the heating jacket allows temperature control of the gas to be tested, further improving the reliability of sampling.
[0020] The flow direction of the gas and the sampling process can be flexibly adjusted according to needs through valve control between each part to adapt to different analysis requirements. For example, the connection of the vacuum pump to the steel cylinder to be tested and the helium gas cylinder facilitates vacuum treatment of the system before sampling to remove impurities and residual gases.
[0021] The nitrogen gas cylinder, as an inert gas source, can be used to displace or dilute the potentially harmful or flammable gases during the sampling process, improving the safety of the operation. Meanwhile, the setting of the vacuum buffer bottle also plays a role in buffering and protecting, preventing the sudden pressure change that may occur during the sampling process. Brief Description of the Drawings
[0022] In order to more clearly illustrate the technical solutions in the embodiments of the present application or the prior art, the following will briefly introduce the drawings required for use in the description of the embodiments or the prior art. Obviously, the drawings in the following description are only the embodiments of the present application. For those of ordinary skill in the art, other drawings can be obtained according to the provided drawings without creative efforts.
[0023] Figure 1 It is a schematic structural diagram of an embodiment of the present utility model;
[0024] Description of the Reference Numerals in the Drawings
[0025] 1. Sampling tank; 2. Steel cylinder to be tested; 3. Helium gas cylinder; 4. Nitrogen gas cylinder; 5. Main pipe; 6. Vacuum buffer bottle; 7. Gas chromatograph; 8. Sampling inlet; 9. Sampling outlet; 10. Valve; 11. Vacuum pump; 12. Pressure reducer; 13. First mass flowmeter; 14. Pressure gauge; 15. Second mass flowmeter; 16. Balance. Detailed Embodiments
[0026] The following will clearly and completely describe the technical solutions in the embodiments of the present application with reference to the drawings in the embodiments of the present application. Obviously, the described embodiments are only a part of the embodiments of the present application, rather than all of the embodiments. Based on the embodiments of the present application, all other embodiments obtained by those of ordinary skill in the art without creative efforts belong to the scope of protection of the present application.
[0027] Embodiment 1
[0028] As Figure 1 shown, a new type of closed metal analysis sampling device includes a sampling tank 1, a steel cylinder to be tested 2, a helium gas cylinder 3, a nitrogen gas cylinder 4 respectively connected to the sampling tank 1 through a main pipe 5, and a vacuum buffer bottle 6 connected to the sampling tank 1 through the main pipe 5; the inner liner of the sampling tank 1 is made of polytetrafluoroethylene. The sampling tank 1, as the main storage and reaction container for the sample, the airtight design of the sampling tank 1 ensures the purity of the sample during the sampling, transfer and analysis processes, avoiding external contamination and cross-contamination between samples.
[0029] A gas chromatograph 7 is provided between the sampling tank 1 and the helium gas cylinder 3. By directly integrating the gas chromatograph 7 between the sampling tank 1 and the helium gas cylinder 3, immediate analysis after sampling is achieved, reducing errors and the risk of contamination during sample transfer, and improving the accuracy and efficiency of analysis. A balance 16 is provided below the sampling tank 1. The design of the balance 16 below the sampling tank 1 enables real-time measurement of the mass change of the sample during sampling and analysis, providing an important basis for quantitative analysis and further enhancing the accuracy of the analysis results.
[0030] An outlet 9 and an inlet 8 are provided on the sampling tank 1. The steel cylinder 2 to be measured, the helium gas cylinder 3, the nitrogen gas cylinder 4, and the gas chromatograph 7 are connected to the inlet 8 through the main pipe 5, and the vacuum buffer bottle 6 is connected to the outlet 9 through the main pipe 5. Valves 10 are installed between the outlet 9 and the inlet 8 and the main pipe 5. The designs of the inlet 8 and the outlet 9, combined with the control of the valves 10, make the sampling process more flexible and controllable.
[0031] Vacuum pumps 11 are connected to both the vacuum buffer bottle 6 and the steel cylinder 2 to be measured and the helium gas cylinder 3. As a buffer and regulating device for gas flow, the vacuum buffer bottle 6 can absorb pressure fluctuations in the system and protect other components from impact. At the same time, the connection with the vacuum pumps 11 enables the system to be evacuated before sampling to remove impurities and residual gases, improving the purity of the sampling.
[0032] A pressure reducer 12 and a first mass flowmeter 13 are provided between the nitrogen gas cylinder 4 and the main pipe 5. A pressure gauge 14 and a second mass flowmeter 15 are provided between the vacuum buffer bottle 6 and the outlet 9. Pressure reducers 12 and mass flowmeters are provided at the nitrogen gas cylinder 4 and the vacuum buffer bottle 6, which can precisely control the gas flow rate and pressure, ensuring stability and repeatability during sampling and analysis.
[0033] A temperature-controlled heating jacket is provided on the steel cylinder 2 to be measured. The temperature-controlled heating jacket on the steel cylinder 2 to be measured allows the sample to be heated as needed to change its physical or chemical state, facilitating subsequent analysis and detection. This design increases the adaptability and flexibility of the device.
[0034] Embodiment 2
[0035] This embodiment is a method embodiment based on the structure of the above embodiment. The difference between this embodiment and the above embodiment lies in the detailed description of the method. A new type of closed metal analysis sampling method includes the following steps:
[0036] A. After processing the sampling tank 1, connect the device and set the reading of the balance 16 to zero;
[0037] B. Pressurize the 5-way sampling main pipe with helium to 0.00 - 0.2 MPa and vacuum pump to less than -0.095 for 1 - 2 hours for gas chromatography analysis of the 5-way sampling main pipe, and the pipeline analysis is qualified.
[0038] C. Then heat the cylinder to be tested 2, and the gas to be tested vaporizes into gas. Open the pressure reducer 12 of the cylinder to be tested 2, and the gas to be tested fills the 5-way sampling main pipe, then close the cylinder to be tested 2.
[0039] D. Lower the room temperature through the air conditioner to liquefy the gas to be tested in the 5-way sampling main pipe. Open the valve 10 of the sampling tank 1 to make the sample to be tested flow into the sampling tank 1, and then close the valve 10 of the sampling tank 1.
[0040] E. Adjust the air conditioner to 30 - 35 °C to vaporize the sample to be tested in the sampling tank 1. Open the nitrogen cylinder, set the opening of the first mass flowmeter 13 to 15 - 30%, open the valve 10 at the sample inlet 8 and the valve 10 at the sample outlet 9 of the sampling tank 1, and adjust the opening of the second mass flowmeter 15 by maintaining the pressure constant through the signal transmitted by the pressure gauge 14.
[0041] F. Purge with nitrogen through the sample inlet 8 and evacuate through the sample outlet 9 to blow away the gas of the sample to be tested in the sampling tank 1, and maintain for 15 - 30 hours, then the sampling is completed.
[0042] The specific steps for treating the sampling tank 1 in step A are as follows: Immerse the inner liner of the sampling tank 1 in 0.5 - 1.5 mol / L hydrochloric acid for 3 - 6 hours, then wash it with high-purity water. After that, immerse the inner liner in 0.5 - 1.5 mol / L nitric acid for 3 - 6 hours to remove the metal impurities on the surface of the inner liner of the sampling tank 1. After washing, dry it, and the drying temperature is 60 - 80 °C and the time is 3 - 5 hours.
[0043] Method principle
[0044] Through the immersion treatment with hydrochloric acid and nitric acid, the metal impurities on the surface of the inner liner of the sampling tank 1 can be effectively removed, ensuring the purity inside the sampling tank 1 and reducing the interference factors in the analysis process.
[0045] Use helium pressurization and vacuum pumping to displace the 5-way sampling main pipe, and confirm through gas chromatography analysis that there are no impurities and residual gases in the pipeline, ensuring the purity and accuracy of sampling.
[0046] Vaporize the gas by heating the cylinder to be tested 2, and use the temperature difference (heating first and then cooling) to liquefy the gas in the sampling tank 1, ensuring that the gas to be tested can enter the sampling tank 1 completely and purely.
[0047] The sample to be tested in the sampling tank 1 is gasified by adjusting the temperature, and nitrogen is introduced for purging and vacuum suction to further clean the environment in the sampling tank 1 in preparation for subsequent immediate analysis.
[0048] The gas chromatograph 7 is used to analyze the sample immediately after sampling, which reduces the error and contamination risk during the sample transfer process and improves the accuracy and efficiency of the analysis. At the same time, the mass change of the sample is measured in real time by the balance 16, which provides an important basis for quantitative analysis.
[0049] The results of 22 metal elements detected in the sampling tank by ICP-MS are shown in the table
[0050]
[0051] Finally, it should be noted that, in this article, relational terms such as first and second, etc. are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Moreover, the terms "include", "comprise" or any other variants thereof are intended to cover non-exclusive inclusion, so that a process, method, article or device including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, article or device. In the absence of further restrictions, the elements defined by the sentence "comprise a ..." do not exclude the presence of other identical elements in the process, method, article or device including the elements.
[0052] The above description of the disclosed embodiments enables those skilled in the art to implement or use the present application. Various modifications to these embodiments will be apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present application. Therefore, the present application will not be limited to the embodiments shown herein, but will conform to the widest scope consistent with the principles and novel features disclosed herein.
Claims
1. A novel airtight metal analysis sampling device, characterized in that, It includes a sampling tank (1), a steel cylinder to be measured (2), a helium gas cylinder (3), a nitrogen gas cylinder (4) which are respectively connected to the sampling tank (1) through a main pipe (5), and a vacuum buffer bottle (6) connected to the sampling tank (1) through the main pipe (5); A gas chromatograph (7) is arranged between the sampling tank (1) and the helium gas cylinder (3), and a balance (16) is arranged below the sampling tank (1).
2. The novel airtight metal analysis sampling device according to claim 1, wherein An outlet (9) and an inlet (8) are arranged on the sampling tank (1). The steel cylinder to be measured (2), the helium gas cylinder (3), the nitrogen gas cylinder (4) and the gas chromatograph (7) are connected to the inlet (8) through the main pipe (5). The vacuum buffer bottle (6) is connected to the outlet (9) through the main pipe (5). Valves (10) are installed between the outlet (9) and the inlet (8) and the main pipe (5).
3. A novel hermetic metal analysis sampling device according to claim 1, characterized in that, Vacuum pumps (11) are connected between the vacuum buffer bottle (6) and the steel cylinder to be measured (2) and the helium gas cylinder (3).
4. A novel closed metal analysis sampling device according to claim 1, characterized in that, A pressure reducer (12) and a first mass flowmeter (13) are arranged between the nitrogen gas cylinder (4) and the main pipe (5).
5. A novel hermetic metal analysis sampling device according to claim 2, characterized in that, A pressure gauge (14) and a second mass flowmeter (15) are arranged between the vacuum buffer bottle (6) and the outlet (9).
6. The novel hermetic metal analysis sampling device according to claim 1, characterized in that, Pressure reducers (12) are connected between the steel cylinder to be measured (2) and the helium gas cylinder (3) and the main pipe (5).
7. A novel airtight metal analysis sampling device according to claim 1, characterized in that, A temperature - controllable heating jacket is arranged on the steel cylinder to be measured (2).