Sample pretreatment device before detection of metal elements in electronic chlorine

Abstract

The utility model belongs to the technical field of sample treatment at the earlier stage of metal element detection, and particularly discloses a sample pretreatment device before detection of metal elements in electronic chlorine, which comprises an electronic gas steel cylinder, the electronic gas steel cylinder is connected with at least two stages of pretreatment structures connected in series through a pipeline, and each pretreatment structure comprises a first absorber; a first microbubble generator connected with a pipeline is arranged in the first absorber, the first absorber is connected with a second absorber through a series pipeline, a second microbubble generator connected with the series pipeline is arranged in the second absorber, and a tail gas outlet is formed in the second absorber; according to the multi-stage series pretreatment structure disclosed by the utility model, micro-bubbles with smaller diameters are generated through the micro-bubble generator, so that the contact area of gas and liquid can be increased, and the retention time of the bubbles in water can be prolonged, thereby improving the mass transfer effect in the dissolving process of metal elements in the gas and improving the removal effect of the metal elements in chlorine.

Description

Technical Field

[0001] The utility model belongs to the technical field of pre-sample processing before metal element detection, and in particular relates to a sample pre-processing device before metal element detection in electronic chlorine. Background Art

[0002] The electronics industry has very high requirements for chlorine gas. The purity of chlorine gas must be above 99.999%, and there are also separate requirements for the content of other impurities, such as the content of metal elements in the gas. Generally speaking, the content of metal elements in electronic chlorine gas can be detected using instruments such as ICP-MS. Before testing, how to dissolve the metal elements in the chlorine gas into "high-purity water" is a key issue. Especially for chlorine gas with low solubility in water, the water absorption of metal elements in chlorine gas is difficult, which is also an important link in whether the test results can truly reflect the content of metal elements in electronic chlorine gas.

[0003] The removal of metal elements from existing electronic chlorine is mostly carried out using ordinary Monglier gas absorption bottles. Monglier gas absorption bottles will produce large bubbles in the water body. The bubble diameter is generally around 1-8 mm. The bubbles are discrete and rise rapidly, resulting in insufficient gas-liquid contact. The substances in the bubbles cannot be well dissolved in the water body, affecting the water body's absorption effect on the metal elements in the gas. Due to the short contact time between the gas and the liquid, the water body has a poor absorption effect on the metal elements in the bubbles. Utility Model Content

[0004] In order to solve the above problems, this patent provides a sample pretreatment device before detecting metal elements in electronic chlorine, which can improve the removal effect of metal elements in electronic chlorine.

[0005] Based on the above objectives, the present invention is achieved through the following technical solutions:

[0006] A sample pretreatment device before detecting metal elements in electronic chlorine gas comprises an electronic gas cylinder, which is connected to a pretreatment structure of at least two stages connected in series via a pipeline. The pretreatment structure comprises a first absorber, in which a first microbubble generator connected to the pipeline is provided, the first absorber is connected to a second absorber via the series pipeline, in which a second microbubble generator connected to the series pipeline is provided, and the second absorber is provided with an exhaust gas outlet.

[0007] Preferably, the first microbubble generator and the second microbubble generator are both cup-shaped structures, the first microbubble generator is connected to the pipeline through a thread; the second microbubble generator is connected to the series pipeline through a thread.

[0008] Preferably, the first absorber and the second absorber are both cylindrical structures.

[0009] Preferably, a gas flow meter is arranged on the pipeline, and a gas outlet is arranged on the pipeline close to the first absorber.

[0010] Preferably, a gas cylinder valve and a pressure reducing valve are arranged on the electronic gas cylinder, a control valve is arranged on the pipeline close to the electronic gas cylinder, an absorption valve is arranged on the first absorber, and an exhaust valve is arranged on the gas outlet.

[0011] Preferably, the first micro-bubble generator is arranged at the lower part of the first absorber, the second micro-bubble generator is arranged at the lower part of the second absorber, the tail gas outlet is arranged at the upper part of the second absorber, and the serial pipeline is arranged at the top of the first absorber.

[0012] Preferably, micro-pores are uniformly arranged on the first micro-bubble generator and the second micro-bubble generator, and the materials of the micro-pores are tetrafluoro sintered materials.

[0013] Preferably, the height-diameter ratio of the first absorber and the second absorber is 2:1-4:1, and the volume is 400-500ml.

[0014] Compared with the prior art, the present application has the following beneficial effects:

[0015] 1. The present application realizes the removal of metal elements in electronic chlorine gas through the multi-stage serial pretreatment structure, the first micro-bubble generator and the second micro-bubble generator generate micro-bubbles with small diameters, which can increase the contact area of gas and liquid and increase the residence time of bubbles in water, thereby increasing the mass transfer effect of the metal element dissolution process in the gas and improving the removal effect of metal elements in chlorine gas, and realizing the efficient removal of metal elements in chlorine gas.

[0016] 2. Micro-bubbles generally refer to micro-bubbles with diameters of 10-50μm existing in water, compared with the bubbles (with diameters of 1-8mm) generated by a meng's gas absorption bottle, the micro-bubbles have smaller diameters, and the mass transfer characteristics and interface properties are significantly different from those of traditional bubbles, (1) large specific surface area; the micro-bubbles generated by the first micro-bubble generator and the second micro-bubble generator have large specific surface areas, and the specific surface area of bubbles can be represented as S / V=3 / r. When the volume of bubbles is unchanged, the specific surface area of bubbles is inversely proportional to the bubble radius, and the specific surface area of bubbles with a radius of 10μm is theoretically 100 times that of bubbles with a radius of 1mm; (2) long residence time in water; traditional bubbles have large diameters, small contact surface areas with water, and short residence times, and the bubbles quickly rise to the water surface and break and disappear. However, the micro-bubbles generated by the first micro-bubble generator and the second micro-bubble generator of the present application rise slowly in water; the rising speed of bubbles with a diameter of 1mm in water is 6m / min, and the rising speed of bubbles with a diameter of 10μm is 0.003m / min, which is 1 / 2000 of the former.

[0017] 3. The utility model increases the specific surface area of ​​the bubbles themselves under a certain volume by using the first and second microbubble generators to generate microbubbles with smaller diameters. Since the rising speed of bubbles with smaller diameters in water is slower, the rising speed of the bubbles in water can be slowed down, thereby increasing the contact time between the bubbles and the water body. This can increase the contact area between the bubbles and water, increase the residence time of the gas in the water, improve the mass transfer effect of the dissolution process of metal elements in the gas in the water body, and achieve the purpose of removing metal elements from electronic chlorine.

[0018] 4. The utility model utilizes the principle that water absorbs metal elements in gas. By increasing the mass transfer area and time, and effectively utilizing the unique properties inherent in "micron" bubbles, it can increase the contact area between bubbles and water and increase the residence time of gas in water, thereby increasing the mass transfer effect of the dissolution process of metal elements in gas and improving the removal effect of metal elements in chlorine. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1 It is a schematic diagram of the process of the utility model in Example 1;

[0020] Figure 2 Schematic diagram of the structure of the first microbubble generator and the second microbubble generator in Example 1.

[0021] In the figure, 1. Electronic gas cylinder; 2. Gas flow meter; 3. First absorber; 4. Second absorber; 5. First microbubble generator; 6. Second microbubble generator; 7. Tail gas outlet; 8. Gas exhaust outlet; 9. Pipeline; 10. Series pipeline. DETAILED DESCRIPTION

[0022] The present invention is further described below through specific embodiments, but the scope of the present invention is not limited thereto.

[0023] Example 1

[0024] A sample pretreatment device before detecting metal elements in electronic chlorine gas, the structure of which is as follows Figure 1-2 As shown, it includes an electronic gas cylinder 1, which is connected to at least two-stage pretreatment structures in series through a pipeline 9. The pretreatment structure includes a first absorber 3, in which a first microbubble generator 5 connected to the pipeline 9 is provided. The first absorber 3 is connected to a second absorber 4 through a series pipeline 10, in which a second microbubble generator 6 connected to the series pipeline 10 is provided, and an exhaust gas outlet 7 is provided on the second absorber 4.

[0025] The first and second microbubble generators 5 and 6 are both cup-shaped structures. The first microbubble generator 5 is threadedly connected to the pipeline 9; the second microbubble generator 6 is also threadedly connected to the series pipeline 10. Both the first and second absorbers 3 and 4 are cylindrical structures. A gas flowmeter 2 is installed on the pipeline 9. A gas outlet 8 is provided on the side of the pipeline 9 near the first absorber 3.

[0026] The electronic gas cylinder 1 is equipped with a gas cylinder valve and a pressure reducing valve. A control valve is installed on the pipeline 9 near the electronic gas cylinder 1 of the gas flowmeter 2. The first absorber 3 is equipped with an absorption valve. The gas outlet 8 is equipped with an exhaust valve. The first microbubble generator 5 is located below the first absorber 3, the second microbubble generator 6 is located below the second absorber 4, and the exhaust outlet 7 is located above the second absorber 4.

[0027] Micropores are evenly distributed on the first microbubble generator 5 and the second microbubble generator 6. The height-to-diameter ratio of the first absorber 3 to the second absorber 4 is 2:1-4:1, and the volume is 400-500 ml.

[0028] Installation instructions: (1) Wash the custom-made perfluorinated pipeline 9, the series pipeline 10, the first absorber 3, the second absorber 4, the PTFE end cap, the PTFE connecting terminal fittings, the first microbubble generator of the custom-made PTFE sintered micropores and the second microbubble generator (high-purity water index: resistivity: 18.2MΩ.cm@25℃) with nitric acid solution, soak, and wash multiple times. Dry all the components for later use.

[0029] (2) Perform the following operations in a dust-free room: add about 400 grams of water (which can be measured by weighing) to the first absorber 3 and the second absorber 4, and assemble the various parts in sequence. Wear disposable gloves during the assembly process.

[0030] (3) With the tail gas valve on the tail gas outlet 7 closed (the channel connected to the tail gas outlet 7), open the exhaust valve (the channel connected to the gas outlet 8). Then, slowly open the gas cylinder valve and the pressure reducing valve on the electronic gas cylinder 1, and adjust the gas flow rate of the flow meter to reach the required flow rate (generally controlled at 20-100 ml / min). After adjusting the flow rate, open the absorption valve of the absorption gas path and the tail gas valve on the tail gas outlet 7 respectively; and close the exhaust valve of the gas outlet 8.

[0031] (4) Gas path switching: switch from the flow regulating gas path to the absorption gas path, open the tail gas valve on the tail gas outlet 7 (the channel connected to the tail gas outlet 77), close the exhaust valve (the channel connected to the gas outlet 8), and start timing for measuring the total ventilation volume; the ventilation volume varies depending on the type of gas and the content of metal elements in the gas. Generally, under the condition of a flow rate of 20-100 ml / min, the recommended ventilation time is 15-120 minutes.

[0032] (5) At the outlet of the tail gas outlet 7, connect a 10% weight concentration alkali solution absorption bottle and add enough alkali solution to ensure that all the chlorine is absorbed. The alkali solution should be weighed before and after ventilation to measure the total amount of chlorine consumed.

[0033] (6) Connect a 10% by weight alkali solution absorption bottle to the gas outlet 8 and add enough alkali solution to ensure that all the chlorine gas is absorbed. The alkali solution does not need to be measured before and after ventilation.

[0034] (7) After the absorption process is completed, the liquids in the first absorber 3 and the second absorber 4 are mixed and poured into another container, and water is added to 1000 ml. The 1000 ml sample is the sample to be tested that has absorbed the metal elements in the gas. The sample can be used for detection by ICP or ICP-MS instruments.

[0035] (8) With the total gas mass, the content of metal elements in the electron gas can be calculated according to the corresponding calculation formula.

[0036] Operation instructions: (1) Close the absorption valve entering the first absorber 3, open the control valve at the bottom of the gas flow meter 2 and the exhaust valve on the gas outlet 8, then slowly open the gas cylinder valve and the pressure reducing valve, and adjust the flow of the gas flow meter 2 to the required value; (2) Open the absorption valve entering the first absorber 3, slowly close the exhaust valve on the gas outlet 8, and start timing; (3) The gas first enters the first absorber 3 with high-purity water along the pipeline 9, and passes through the micropores on the first microbubble generator 5 to discharge tiny bubbles in the direction of the peripheral direction of the micropores on the wall of the first microbubble generator 5. The tiny bubbles come into contact with the water, and the gas The metal elements in the chlorine gas are absorbed into the water. As the bubbles float upward, the metal elements in the gas are continuously absorbed by the water. The gas enters the second absorber 4 from the top outlet of the first absorber 3 along the series pipeline 10 and is processed by the second microbubble generator 6, and the process of absorbing metal elements in the first absorber 3 is carried out. After that, the gas that has been completely absorbed by the water is discharged from the tail gas outlet 7, completing the secondary absorption of the metal elements in the chlorine gas. (4) The absorption liquid in the first absorber 3 and the second absorber 4 are poured into the same large container and mixed. The liquid is the sample for IC-PAS detection of metal elements.

[0037] The above description is only a preferred embodiment of the present invention, but is not limited to the above examples. Any modifications, equivalent replacements and improvements made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.

Claims

1. A sample pretreatment device before detecting metal elements in electronic chlorine, characterized in that: It includes an electronic gas cylinder, which is connected to at least two-level pretreatment structures in series through a pipeline. The pretreatment structure includes a first absorber, in which a first microbubble generator connected to the pipeline is provided. The first absorber is connected to a second absorber through a series pipeline, in which a second microbubble generator connected to the series pipeline is provided, and the second absorber is provided with an exhaust gas outlet.

2. The sample pretreatment device before detecting metal elements in electronic chlorine according to claim 1 is characterized in that: The first microbubble generator and the second microbubble generator are both cup-shaped structures. The first microbubble generator is connected to the pipeline through a thread; the second microbubble generator is connected to the series pipeline through a thread.

3. The sample pretreatment device before detecting metal elements in electronic chlorine according to claim 2, characterized in that: The first absorber and the second absorber are both cylindrical structures.

4. The sample pretreatment device before detecting metal elements in electronic chlorine according to claim 3 is characterized in that: A gas flow meter is provided on the pipeline, and a gas outlet is provided on the pipeline on the side of the gas flow meter close to the first absorber.

5. The sample pretreatment device before detecting metal elements in electronic chlorine according to claim 4 is characterized in that: The electronic gas cylinder is provided with a gas cylinder valve and a pressure reducing valve; the gas flow meter is provided with a control valve on the pipeline close to the electronic gas cylinder; the first absorber is provided with an absorption valve; and the gas outlet is provided with an exhaust valve.

6. The sample pretreatment device before detecting metal elements in electronic chlorine according to claim 1, characterized in that: The first microbubble generator is arranged at the lower part of the first absorber, the second microbubble generator is arranged at the lower part of the second absorber, and the tail gas outlet is arranged at the upper part of the second absorber.

7. The sample pretreatment device before detecting metal elements in electronic chlorine according to claim 2, characterized in that: The first microbubble generator and the second microbubble generator are both distributed with micropores.

8. The sample pretreatment device before detecting metal elements in electronic chlorine according to claim 3 is characterized in that: The height-to-diameter ratio of the first absorber and the second absorber is 2:1-4:1, and the volume is 400-500 ml.

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