Liquid sample aeration and strong oxidation device and method of use

Abstract

The application belongs to the field of experimental sample oxidation, and particularly relates to a liquid sample aeration strong oxidation device and a use method. The device comprises an air pump, an air purification device, an aeration oxidation pipe, a gas bottle, a high-voltage direct-current power supply and a reflux condenser pipe. The aeration oxidation pipe is fixed in the gas bottle, metal electrodes are arranged on the inner side of the lower part of the aeration oxidation pipe and the outer side of the bottom of the gas bottle respectively, and the two metal electrodes are connected with the high-voltage direct-current power supply. Clean air is sent into the aeration oxidation pipe through the air pump and the air purification device, and enters the liquid sample through the through hole at the bottom of the pipe. Plasma discharge is formed between the two metal electrodes, oxygen in the air is oxidized, free radicals, ozone and other active substances are generated through the plasma discharge process, and the dissolved components and suspended matters in the solution are strongly oxidized. The reflux condenser pipe cools and refluxes the volatile solvent in the sample to the gas bottle. The device has simple structure and convenient operation, and different degrees of oxidation of the liquid sample can be realized by changing the electrification time.

Description

Technical Field

[0001] This invention belongs to the field of experimental sample oxidation, specifically an aeration oxidation device and its usage method. Background Technology

[0002] To obtain samples with different degrees of oxidation, traditional chemical oxidation methods, such as strong oxidants like hydrogen peroxide, have limited effect on oxidizing metals and introduce impurities. Therefore, a highly efficient oxidation method that does not introduce impurities is needed. Summary of the Invention

[0003] In view of the shortcomings of existing technologies, the purpose of this invention is to provide a liquid sample aeration strong oxidation device and its usage method that can conveniently and efficiently oxidize samples without introducing impurities.

[0004] The liquid sample aeration and strong oxidation device provided by this invention includes: an air pump 1, an air purification device 2, an aeration and oxidation tube 3, a gas cylinder 5, a high-voltage DC power supply 10, and a reflux condenser tube 13; wherein: The air pump 1 is used to provide an air source; specifically, an air compressor or a blower can be used. The air purification device 2 has its inlet connected to the air pump 1 and is used to purify the air supplied by the air pump, including removing organic matter, water vapor and particulate matter, etc.; specifically, it is a purification device using activated carbon or molecular sieve as purification materials. The aeration oxidation tube 3 is cylindrical, with an air inlet 4 on the upper side. The air inlet 4 is connected to the air outlet of the air purification device 2, using purified gas as the air source for aeration. The entire aeration oxidation tube 3 is placed in the ventilation bottle 5, and the upper part of the oxidation tube is fixed by the opening on the ventilation bottle cap 12. A metal electrode 7 is provided on the lower inner bottom of the aeration oxidation tube 3, and several small through holes 8 are arranged in a ring at the bottom of the aeration oxidation tube 3, so that the aeration gas entering the aeration oxidation tube 3 can be evenly introduced into the sample to be oxidized, providing oxygen for the ozone generated in the plasma discharge process, and at the same time mixing the sample and oxidizing it uniformly. The inner diameter of the aeration oxidation tube is 1~3 mm, and the length is 120~150 mm, slightly larger than the height of the ventilation bottle. The venting bottle 5 is used to hold the sample 6 to be oxidized; the lower end of the aeration oxidation tube 3 is placed in the sample 6 to be oxidized; a metal electrode 9 is provided on the outside of the bottom through hole 8 of the venting bottle 5. The two poles of the high-voltage DC power supply 10 are respectively connected to the metal electrode 7 at the bottom of the inner side of the aeration oxidation tube 3 and the metal electrode 9 at the outer side of the bottom of the ventilation bottle; the high-voltage DC power supply 10 causes plasma discharge between the two metal electrodes, generating active substances such as free radicals and ozone, which strongly oxidize the dissolved components and suspended matter in the solution.

[0005] The present invention can adjust the electric field between the two metal electrodes by changing the distance between the lower metal electrode 7 of the aeration oxidation tube and the bottom metal electrode 9 of the air bottle; the distance between the two electrodes is adjustable within the range of 1.5~3.5 mm. The ventilation bottle 5 has a ventilation port 11 on its side, and the reflux condenser 13 is connected to the ventilation port 11. The reflux condenser 13 is specifically a serpentine, spherical, or straight condenser. Since a large amount of heat is also generated during the plasma discharge process, the solvent in the liquid sample will evaporate. The reflux condenser 13 cools the evaporated solvent in the liquid sample and refluxes it back into the ventilation bottle 5 to ensure that the volume of the solvent in the oxidized sample remains unchanged.

[0006] The operating procedure for the above-mentioned liquid sample aeration strong oxidation device is as follows: Step 1: Put 10-30 ml of the liquid sample 6 to be oxidized into the gas bottle 5; Step 2: Fix the aeration oxidation tube 3 into the air bottle 5 through the cap of the air bottle 12. The distance between the lower metal electrode 7 of the aeration oxidation tube and the bottom metal electrode 9 of the air bottle is 1.5~3.5 mm. Step 3: Turn on the reflux condenser 13 and ensure that the temperature of the reflux condenser 13 is maintained below 5 ℃; then turn on the air pump 1 and control the air pump flow rate to 1~5 L / min. The air supplied by the air pump enters the aeration oxidation tube 3 through the air purification device 2. Step 4: Connect the inner bottom metal electrode 7 of the aeration oxidation tube 3 and the outer bottom metal electrode 8 of the air bottle 5 to the two poles of the high voltage DC power supply, and turn on the high voltage DC power supply with a voltage of 10~30 KV. Step 5: For a certain sample, perform time gradient oxidation to obtain oxidation efficiency curves corresponding to different times; then determine the discharge time according to the required degree of oxidation. When the liquid sample 6 reaches the expected degree of oxidation, turn off the high voltage DC power supply and the air pump, and take out the sample for testing.

[0007] The beneficial effects of this invention are as follows: Aeration is uniformly introduced into the sample to be oxidized through the aeration oxidation tube, providing oxygen for the ozone generated during the plasma discharge process. Simultaneously, the sample is mixed, and uniform oxidation occurs between the two metal electrodes, forming a plasma discharge that oxidizes oxygen in the air. This plasma discharge process generates free radicals and ozone, among other active substances, which strongly oxidize dissolved components and suspended solids in the solution. The results are as follows: Figure 5 As shown, the present invention oxidizes Fe ions in the sample with an oxidation efficiency of approximately 97%. Compared with traditional chemical oxidation methods using strong oxidants, the present invention avoids introducing interference from other chemical substances into the sample and can oxidize the sample efficiently. Attached Figure Description

[0008] Figure 1This is a schematic diagram of the liquid sample aeration and strong oxidation device of the present invention.

[0009] Figure 2 This is a cross-sectional view of the aeration oxidation pipe structure of the present invention.

[0010] Figure 3 This is a schematic diagram of the small holes in the cylindrical layout at the bottom of the cylindrical aeration oxidation tube in the device of the present invention.

[0011] Figure 4 This is a top view of the structure of the vent bottle cap in the device of the present invention.

[0012] Figure 5 Experimental data graphs of the apparatus and method of the present invention.

[0013] The following numbers are labeled in the diagram: 1 is the air pump, 2 is the air purification device, 3 is the aeration oxidation tube, 4 is the inlet of the aeration oxidation tube, 5 is the air supply bottle, 6 is the liquid sample to be oxidized, 7 is the lower metal electrode of the aeration oxidation tube, 8 is the small through hole, 9 is the bottom metal electrode of the air supply bottle, 10 is the high-voltage DC power supply, 11 is the exhaust port of the air supply bottle, 12 is the cap of the air supply bottle, and 13 is the reflux condenser tube. Implementation

[0014] The present invention will be further described below with reference to the accompanying drawings and embodiments.

[0015] Example: See Figure 1 It includes: 1. Air pump; 2. Air purification device; 3. Aeration oxidation tube; 4. Aeration oxidation tube inlet; 5. Gas bottle; 6. Sample to be oxidized; 7. Lower metal electrode of the aeration oxidation tube; 8. Cylindrical hole; 9. Bottom metal electrode of the gas bottle; 10. High voltage DC power supply; 11. Gas bottle exhaust port; 12. Gas bottle cap; 13. Reflux condenser tube.

[0016] In this implementation example, air pump 1 is used to provide the air source, specifically an air compressor, with a flow rate of 3 L / min, which varies depending on the size of the device and the oxidation rate.

[0017] In this implementation case, the air purification device can remove organic matter, water vapor and particulate matter from the gas supplied by the gas supply device, specifically activated carbon or molecular sieves and bag filters, cartridge filters or electrostatic precipitators.

[0018] In this embodiment, the aeration oxidation tube 3 is made of quartz with a wall thickness of 1.5 mm and an internal dimension of 2 mm. The diameter of the cylindrical aeration oxidation tube 3 and the opening diameter of the air bottle cap 12 are both 25 mm to ensure a stable connection and good airtightness. The length of the aeration oxidation tube 3 is 140 mm, slightly longer than the air bottle, which allows for adjustment of the distance between the lower metal electrode 7 of the cylindrical aeration oxidation tube and the bottom metal electrode 9 of the air bottle, thereby regulating the electric field between the two metal electrodes. In this case, the distance is 2 mm, which is adjusted according to the high-voltage DC power supply voltage and the required oxidation efficiency. The bottom of the cylindrical aeration oxidation tube has through holes 8 with a diameter of 1 mm, and several through holes are evenly distributed in a ring to ensure uniform airflow distribution.

[0019] In this embodiment, the height of the vent bottle 5 is 60 mm. The cap 12 of the vent bottle 5 is of GL45 specification, with a through hole in the middle. The diameter of the through hole is 25 mm, which is the same as the outer diameter of the cylindrical aeration oxidation tube 3, and is used to fix the cylindrical aeration oxidation tube 3. The vent bottle 5 has an exhaust port 11 with a diameter of 6 mm, which is used to discharge the oxidized air. The vent bottle 5 is used to hold the sample 6 to be oxidized, with a sample volume of 10~30 ml. In this case, 10 ml is added to ensure that the sample liquid level is higher than the cylindrical hole 8 of the cylindrical aeration oxidation tube.

[0020] In this implementation example, the high-voltage DC power supply 10 is an adjustable power supply, which can adjust the voltage between the two metal electrodes as needed. In this example, the voltage is 10 kV.

[0021] In this embodiment, the reflux condenser 13 is a serpentine condenser that cools and refluxes the solvent volatilized in the sample back to the gas bottle, ensuring that the volume of the solvent in the oxidized sample remains unchanged.

[0022] The method used in this example is: Step 1: Put 10 ml of the Fe ion-containing sample into gas bottle 5; Step 2: Fix the cylindrical aeration oxidation tube 3 into the air bottle 5 through the air bottle cap 12; Step 3: Turn on air pump 1. The air pump flow rate is 3 L / min. The air supplied by the air pump enters the cylindrical aeration oxidation tube 3 through the air purification device 2. Step 4: Connect the metal electrodes of the lower part 7 of the cylindrical aeration oxidation tube and the bottom 8 of the air bottle to the high voltage DC power supply 10 and turn on the high voltage DC power supply 10. The power supply voltage is 10 KV. Step 5: Discharge time lasts for 30 minutes to remove Fe from the sample. 2+ All oxidized to Fe 3+ Turn off the high-voltage DC power supply and the air pump, remove the sample, and determine the Fe content using o-phenanthroline molecular absorption spectroscopy. 2+ Content, results as follows Figure 5As shown, the Fe ions in the sample were oxidized using this embodiment and method, and compared with the hydrogen peroxide chemical oxidation method.

[0023] The apparatus and method of the present invention can remove Fe from a sample. 2+ Highly efficient oxidation; Fe in the sample before oxidation is shown in the figure. 2+ The content was 15 mg / L, and the concentration after oxidation using this example and method was 0.4 mg / L; while the Fe content after oxidation using hydrogen peroxide chemical oxidation was... 2+ The concentration of 3.5 mg / L is higher than that obtained by the apparatus and method of the present invention after oxidation. As described above, the apparatus and method of the present invention have a better effect on strong oxidation of dissolved components and suspended solids in solution.

Claims

1. A liquid sample aeration and strong oxidation device, characterized in that, include: Air pump (1), air purification device (2), aeration oxidation tube (3), air supply bottle (5), high voltage DC power supply (10), reflux condenser tube (13); wherein: The air pump (1) is used to provide an air source; The air purification device (2) has its inlet connected to the air pump (1) for purifying the air supplied by the air pump, including removing organic matter, water vapor and particulate matter. The aeration oxidation tube (3) is a cylindrical tube with gas guiding partition channels on both the side wall and bottom wall. An air inlet (4) connected to the gas guiding partition channels on the side wall is provided on the upper side. The air inlet (4) is connected to the air outlet of the air purification device (2) to use purified gas as the air source for aeration. The entire aeration oxidation tube (3) is placed in a ventilation bottle (5), and the upper part of the cylindrical tube is fixed through the opening on the bottle cap (12). A first metal electrode (7) is provided on the bottom inner side of the lower part of the aeration oxidation tube (3), and an annular opening is provided at the bottom of the aeration oxidation tube (3). The arrangement of several small through holes (8) allows the aeration gas entering the aeration oxidation tube (3) to enter the liquid sample to be oxidized evenly, providing oxygen for the ozone generated during the plasma discharge process, and at the same time mixing the liquid sample to be oxidized, so that it is oxidized evenly; the gas entering from the air inlet (4) enters the guide partition channel at the bottom of the tube through the guide partition channel on the side of the tube, and then exits from several small through holes at the bottom of the aeration oxidation tube (3), and the first metal electrode (7) is located at the bottom inner side of the lower part of the aeration oxidation tube (3), so that the gas will not come into contact with the first metal electrode (7) during the gas transportation process. The ventilation bottle (5) is used to hold the liquid sample (6) to be oxidized; the lower end of the aeration oxidation tube (3) is placed in the liquid sample (6) to be oxidized; a second metal electrode (9) is provided on the outer side of the bottom of the ventilation bottle (5). The two poles of the high-voltage DC power supply (10) are respectively connected to the first metal electrode (7) at the bottom of the inner side of the aeration oxidation tube (3) and the second metal electrode (9) at the bottom of the ventilation bottle; the high-voltage DC power supply (10) causes plasma discharge between the two metal electrodes, generating free radicals and ozone, which strongly oxidize the dissolved components and suspended matter in the liquid sample to be oxidized. The ventilation bottle (5) has a ventilation and exhaust port (11) on its side, and the reflux condenser (13) is connected to the ventilation and exhaust port (11). The reflux condenser (13) is used to cool and reflux the solvent volatilized in the liquid sample to be oxidized back into the ventilation bottle (5) to ensure that the volume of the solvent in the oxidized liquid sample remains unchanged.

2. The liquid sample aeration and strong oxidation device according to claim 1, characterized in that, The air purification device (2) is a purification device that uses activated carbon or molecular sieve as purification material.

3. The liquid sample aeration and strong oxidation device according to claim 1, characterized in that, The ventilation bottle (5) is cylindrical in shape, with a height of 60 mm and a bottom diameter of 55 mm. This size is suitable for processing 5-30 ml of liquid samples to be oxidized. The size of the ventilation bottle (5) can be adjusted according to actual needs.

4. The liquid sample aeration and strong oxidation device according to claim 1, characterized in that, The inner diameter of the aeration oxidation tube (3) is 1~3 mm and the length is 120~150 mm, which is greater than the height of the air bottle.

5. The liquid sample aeration and strong oxidation device according to claim 1, characterized in that, The reflux condenser (13) is a serpentine, spherical, or straight condenser.

6. The liquid sample aeration and strong oxidation device according to claim 1, characterized in that, The cap (12) of the ventilation bottle is of GL45 specification and is compatible with the aeration oxidation tube (3), and can be adjusted according to actual needs.

7. The liquid sample aeration and strong oxidation device according to claim 1, characterized in that, The electric field between the two metal electrodes can be adjusted by changing the distance between the first metal electrode (7) at the bottom of the aeration oxidation tube and the second metal electrode (9) at the bottom of the air bottle; the distance between the two electrodes can be adjusted within the range of 1.5~3.5 mm.

8. The method of using the liquid sample aeration and strong oxidation device as described in any one of claims 1-7, characterized in that, The specific operating procedure is as follows: Step 1: Put 10-30 ml of the liquid sample to be oxidized (6) into the gas-breathing bottle (5); Step 2: Fix the cylindrical aeration oxidation tube (3) in the air bottle (5) through the air bottle cap (12). The distance between the first metal electrode (7) at the bottom of the aeration oxidation tube and the second metal electrode (9) at the bottom of the air bottle is 1.5~3.5 mm. Step 3: Turn on the reflux condenser (13) and the air pump (1), control the air pump flow rate to 1~5 L / min, and the air supplied by the air pump enters the cylindrical aeration oxidation tube (3) through the air purification device (2); Step 4: Connect the first metal electrode (7) at the bottom inside the cylindrical aeration oxidation tube (3) and the second metal electrode (9) at the bottom outside the air bottle (5) to the two poles of the high voltage DC power supply, and turn on the high voltage DC power supply with a voltage of 10~30 KV. Step 5: Determine the discharge time according to the required degree of oxidation. When the liquid sample (6) to be oxidized reaches the expected degree of oxidation, turn off the high voltage DC power supply, turn off the air pump, and take out the liquid sample for testing.

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