Automatic drainage micro water content tester

Abstract

This utility model belongs to the field of trace moisture determination technology, specifically relating to an automatic draining trace moisture analyzer, including an electrolytic cell and a main unit. The electrolytic cell includes an anode chamber and a cathode chamber, with a ceramic filter plate between the anode and cathode chambers to prevent the diffusion of iodine molecules. The anode chamber includes a sample inlet tube, a measuring electrode, a drain outlet, and a stir bar for stirring reagents. The cathode chamber includes a liquid inlet, an electrolytic electrode, and a drying tube for holding color-changing silica gel. The main unit includes a computer control system, a keyboard, a display screen, electrolytic electrode sockets, measuring electrode sockets, and an automatic liquid addition and drainage assembly. The computer control system is used to monitor the electrolysis state of the electrolytic cell in real time, calculate the moisture content, and control the automatic liquid addition and drainage assembly to discharge waste liquid from the electrolytic cell through the drain outlet. The display screen is used to display the electrolysis curve and moisture content in real time. It can simplify the liquid addition and drainage operation, improve detection efficiency, significantly improve measurement accuracy, and provide stable and reliable measurement.

Description

Technical Field

[0001] This utility model belongs to the field of trace moisture determination technology, specifically relating to an automatic draining trace moisture analyzer. Background Technology

[0002] A trace moisture analyzer is a precision analytical instrument specifically designed for accurately determining extremely low moisture content in substances. It is widely used in industries such as petroleum, chemical, power, railway, pesticides, pharmaceuticals, and environmental protection. In the field of trace moisture determination, traditional methods (such as drying and gas chromatography) often suffer from low accuracy, complex operation, and long processing times. Karl Fischer coulometric titration, as a classic method for trace moisture determination, offers advantages such as high accuracy and speed. However, traditional Karl Fischer coulometric titrators often suffer from low automation and complex operation. Therefore, developing a high-precision, high-efficiency, and easy-to-operate trace moisture analyzer based on the Karl Fischer coulometric titration method is particularly important. Utility Model Content

[0003] The purpose of this invention is to provide an automatic liquid draining trace moisture analyzer to solve the problems of low measurement accuracy, complex operation, and long measurement cycle in the existing technology.

[0004] To solve the above-mentioned technical problems, this utility model provides the following technical solution:

[0005] An automatic draining trace moisture analyzer includes an electrolytic cell and a main unit. The electrolytic cell includes an anode chamber and a cathode chamber, with a ceramic filter plate between them to separate the anode and cathode chambers and prevent iodine molecules in the anode chamber from diffusing into the cathode chamber. The top of the anode chamber has an inlet tube and a detachable measuring electrode. The inlet tube has a detachable inlet stopcock. The anode chamber has a drain port and a stir bar for stirring reagents. The top of the cathode chamber has an inlet port, a detachable electrolytic electrode, and a drying tube. The inlet port has a detachable sealing plug, and the drying tube holds color-changing silica gel. The main unit includes a computer control system, and a keyboard, display screen, electrolytic electrode socket, measuring electrode socket, and automatic draining / filling assembly electrically connected to the computer control system. The electrolytic electrode socket and measuring electrode socket are used to connect the electrolytic electrode and measuring electrode, respectively. The computer control system monitors the electrolysis state of the electrolytic cell in real time, calculates the moisture content, and controls the automatic draining / filling assembly to discharge waste liquid from the electrolytic cell through the drain port. The display screen shows the electrolysis curve and moisture content in real time.

[0006] Furthermore, the automatic liquid addition and drainage assembly includes a liquid addition and drainage control switch, an air pump, a three-way solenoid valve, a reagent bottle, and a sealed bottle; the liquid addition and drainage control switch and the air pump are mounted on the main unit, and the three-way solenoid valve is mounted on the drain port of the electrolytic cell. The liquid addition and drainage control switch, the air pump, and the three-way solenoid valve are all electrically connected to the computer control system. The reagent bottle is connected to the air pump through a reagent bottle air tube, and the waste liquid bottle is connected to the air pump through a waste liquid bottle air tube. The computer control system can control the positive or negative pressure output of the air pump according to the signal sent by the liquid addition and drainage control switch, and control the three-way solenoid valve to switch the passage between the electrolytic cell and the waste liquid bottle or the reagent bottle.

[0007] Furthermore, the computer control system includes a data acquisition module, a microprocessor, and a data storage module. The data acquisition module is used to acquire electrical signals from the measuring electrode and the electrolysis electrode. The microprocessor is used to automatically store the blank current based on the signals acquired by the data acquisition module and a preset blank current storage algorithm, and to calculate the moisture content according to a preset formula and output it to the display screen. The data storage module is used to store historical test data.

[0008] Furthermore, it also includes a sample injection assembly, which includes a liquid injector, a solid injector, and a gas injector; the liquid injector is a syringe with a needle; the solid injector includes a detachably connected injection bend and a cap; the gas injector includes a gas storage tank and a gas delivery pipe, the gas delivery pipe is used to deliver the gas in the gas storage tank to the electrolytic cell, and the gas delivery pipe is equipped with a pump body that can control the gas flow rate of the gas delivery pipe.

[0009] Furthermore, the host is also equipped with a temperature sensor for detecting ambient temperature, and the data acquisition module can acquire the ambient temperature detected by the temperature sensor and output a temperature drift compensation signal.

[0010] Furthermore, the host computer is also equipped with a thermal printer, which is used to automatically print test data and historical records.

[0011] Furthermore, the host is also equipped with a stirring speed knob that is electrically connected to the computer control system. The computer control system can control the rotation speed of the stir bar in the electrolytic cell according to the signal emitted by the stirring speed knob.

[0012] Furthermore, the host is also equipped with an RS232 interface and a cooling fan. The RS232 interface can be used for data communication with external devices, and the cooling fan is used to reduce the operating temperature of the host.

[0013] Furthermore, the connections between the measuring electrode and the anode chamber, the electrolytic electrode and the cathode chamber, the drying tube and the cathode chamber, and the sample inlet tube and the sample inlet stopcock are all sealed with ground joints and are provided with a vacuum grease sealing layer.

[0014] Furthermore, the host is provided with an electrolytic cell holder for mounting an electrolytic cell.

[0015] Compared with the prior art, the present invention has the following beneficial technical effects:

[0016] 1. This utility model, by embedding a dynamic blank current register algorithm in the microprocessor, can deduct environmental moisture interference and drift tracking during the electrolysis reaction in real time, so that the measurement sensitivity can reach 0.1μg, realize stable measurement across the entire temperature threshold (5~40℃), and significantly improve the measurement accuracy.

[0017] 2. By setting up a computer control system and an automatic liquid addition / discharge component, this utility model can realize unmanned operation of one-button liquid addition / discharge, which can not only improve operating efficiency, but also avoid operators coming into contact with toxic reagents and improve safety.

[0018] 3. This utility model, by setting up a sample injection component, can be used to measure liquid, solid and gas samples. It has good versatility, can meet the measurement needs of different industries, and has broad market application prospects. Attached Figure Description

[0019] Figure 1 This is a schematic diagram of the structure of the electrolytic cell of this utility model;

[0020] Figure 2 This is a top view of the main unit of this utility model;

[0021] Figure 3 This is a side view of the host unit of this utility model;

[0022] Figure 4 This is a rear view of the main unit of this utility model;

[0023] Figure 5 This is a schematic diagram of the solid sampler of this utility model;

[0024] Figure 6 This is a schematic diagram illustrating the use of the solid sampler of this utility model;

[0025] Figure 7 This is a schematic diagram illustrating the use of the gas sampler of this utility model;

[0026] In the picture:

[0027] Anode chamber 1, cathode chamber 2, measuring electrode 3, sample inlet tube 4, sample inlet stopcock 5, stir bar 6, electrolytic electrode 7, drying tube 8, color-changing silica gel 9, ceramic filter plate 10, electrolytic cell base 11, keyboard 12, display screen 13, electrolytic electrode socket 14, measuring electrode socket 15, liquid addition / discharge control switch 16, reagent bottle gas tube socket 17, waste liquid bottle gas tube socket 18, thermal printer 19, stirring speed knob 20, RS232 interface 21, cooling fan 22, integrated power switch 23, sample inlet bend 24, cover 25, gas storage tank 26, gas delivery pipe 27, pump body 28. Detailed Implementation

[0028] The following detailed description illustrates the specific implementation method:

[0029] Example

[0030] An automatic liquid discharge trace moisture analyzer includes an electrolytic cell, a main unit, and a sample injection assembly.

[0031] like Figure 1 As shown, the electrolytic cell includes a detachably connected anode chamber 1 and cathode chamber 2. Cathode chamber 2 is located inside anode chamber 1, and a drain port is provided at the bottom of anode chamber 1. A detachable measuring electrode 3 is provided at the top of anode chamber 1, and a sample inlet tube 4 communicating with its interior is also provided on anode chamber 1. A detachable sample inlet stopcock 5 is provided at the inlet of sample inlet tube 4. A stir bar 6 for stirring reagents is placed at the bottom of anode chamber 1. A liquid inlet, a detachable electrolytic electrode 7, and a drying tube 8 are provided at the top of cathode chamber 2. A detachable sealing plug is provided inside the liquid inlet, and the drying tube 8 is used to place color-changing silica gel 9. A ceramic filter plate 10 is provided at the bottom of cathode chamber 2. The ceramic filter plate 10 is used to separate anode chamber 1 and cathode chamber 2, preventing iodine molecules in anode chamber 1 from diffusing into cathode chamber 2. The connections between anode chamber 1 and cathode chamber 2, measuring electrode 3 and anode chamber 1, electrolytic electrode 7 and cathode chamber 2, drying tube 8 and cathode chamber 2, and sample inlet tube 4 and sample inlet stopcock 5 are all sealed with ground joints and coated with vacuum grease.

[0032] like Figure 2-4 As shown, the main unit includes a computer control system, and a keyboard 12, a display screen 13, an electrolysis electrode socket 14, a measuring electrode socket 15, an automatic liquid addition and drainage assembly, a temperature sensor, a thermal printer 19, and a stirring speed knob 20, all electrically connected to the computer control system. The computer control system is used to monitor the electrolysis curve of the electrolytic cell in real time, calculate the moisture content, and control the automatic liquid addition and drainage assembly to discharge the waste liquid in the electrolytic cell from the drain port. The electrolysis electrode socket 14 and the measuring electrode socket 15 are used to connect the electrolysis electrode 7 and the measuring electrode 3, respectively. The display screen 13 is used to display the electrolysis curve and moisture content in real time, the temperature sensor is used to detect the ambient temperature, the thermal printer 19 is used to automatically print test data and historical records, and the stirring speed knob 20 is used to adjust the rotation speed of the stir bar 6.

[0033] The automatic liquid addition and drainage assembly includes a liquid addition and drainage control switch 16, an air pump, a three-way solenoid valve, a reagent bottle, and a sealed bottle. The liquid addition and drainage control switch 16 is located on the main unit, and the air pump is located inside the main unit. The main unit has a reagent bottle air tube inlet 17 and a waste liquid bottle air tube inlet 18 connected to the air pump. The three-way solenoid valve is located at the drain port of the electrolytic cell. The liquid addition and drainage control switch 16, the air pump, and the three-way solenoid valve are all electrically connected to the computer control system. The reagent bottle is connected to the air pump through a reagent bottle air tube, and the waste liquid bottle is connected to the air pump through a waste liquid bottle air tube. The computer control system can control the positive or negative pressure output of the air pump and control the three-way solenoid valve to switch the passage between the electrolytic cell and the waste liquid bottle or the reagent bottle according to the signal sent by the liquid addition and drainage control switch 16.

[0034] By combining a computer control system with an automatic liquid addition / discharge assembly, unmanned operation with one-button liquid addition / discharge can be achieved. This not only simplifies operation and improves efficiency, but also avoids operator contact with toxic reagents, enhancing safety and greatly improving the working environment.

[0035] The computer control system includes a data acquisition module, a microprocessor, and a data storage module. The data acquisition module is used to acquire electrical signals output by the measuring electrode 3, the electrolysis electrode 7, and the temperature sensor. The microprocessor is a 32-bit embedded microprocessor. The microprocessor is used to automatically store the blank current based on the signals acquired by the data acquisition module, combined with a preset temperature drift compensation formula and blank current storage algorithm. It is also used to calculate the moisture content according to the preset formula and output it to the display screen 13. Furthermore, it is used to control the rotation speed of the stir bar 6 in the electrolysis cell according to the signal emitted by the stirring speed knob 20. The data storage module is used to store historical test data.

[0036] Employing a 32-bit embedded microprocessor as the main control core and embedding a mini operating system, the device utilizes a dynamic blank current register algorithm embedded in the microprocessor to deduct environmental moisture interference and drift tracking during the electrolysis reaction in real time. This enables a measurement sensitivity of 0.1 μg and achieves stable measurement across the entire temperature range (5–40℃), significantly improving measurement accuracy. The device offers fast measurement speed and reliable stability. The display screen 13 can display the electrolysis curve in real time, facilitating real-time observation of the reagent status. Historical data is stored through the data storage module for easy retrieval.

[0037] The sample introduction assembly includes a liquid injector, a solid injector, and a gas injector; the liquid injector is a syringe with a needle; such as Figure 5 As shown, the solid sampler includes a detachably connected injection elbow 24 and a cap 25; as Figure 7As shown, the gas injector includes a gas storage tank 26 and a gas delivery pipe 27. The gas delivery pipe 27 is used to deliver the gas in the gas storage tank 26 to the electrolytic cell. The gas delivery pipe 27 is equipped with a pump body 28 that can control the gas flow rate of the gas delivery pipe 27.

[0038] By setting up the sample introduction component, it can be used to measure liquid, solid and gas samples, has good versatility, can meet the measurement needs of different industries, and has broad market application prospects.

[0039] The main unit is also equipped with an electrolytic cell base 11, an RS232 interface 21, a cooling fan 22, and an integrated power switch 23. The electrolytic cell base 11 is used to install the electrolytic cell, the RS232 interface 21 can be used for data communication with external devices, the cooling fan 22 is used to reduce the operating temperature of the main unit, and the integrated power switch 23 is used to turn the power of the main unit on or off.

[0040] The specific implementation is as follows:

[0041] 1. Instrument self-calibration: Plug in the power supply, press the integrated power switch 23, press any key to enter the test interface, and the instrument will automatically perform a self-test to check whether each component is working properly.

[0042] 2. Cleaning, drying and assembly of the electrolytic cell: Clean the electrolytic cell and related components with a cleaning agent, dry them in an oven, and then remove them to cool naturally; install the color-changing silica gel 9 into the drying tube 8, install the silica gel pad into the injection stopcock 5 and screw it into the stud, and place the stir bar 6; apply vacuum grease to the ground joint of the electrolytic cell, and then assemble all components (except the drying tube 8 and the sealing plug); inject electrolyte into the electrolytic cell through the inlet and sealing port of the drying tube 8 in the fume hood, and after the liquid levels in the cathode chamber 2 and the anode chamber 1 are basically horizontal, install the drying tube 8 and the sealing plug; install the electrolytic cell onto the electrolytic cell base 11.

[0043] 3. Reagent adjustment and blank current removal: Adjust the stirrer speed to an appropriate value, and then inject pure water into the electrolytic cell for reagent adjustment; after adjustment, remove the blank current to ensure that the instrument is in an initial equilibrium state; if the electrolysis curve is relatively high or the measurement indication is unstable, tilt and rotate the electrolytic cell to absorb the moisture on the cell wall until the electrolysis curve is low and stable.

[0044] 4. Instrument calibration: Calibrate with pure water. Inject 0.1 μL of pure water and verify that the displayed value is within 100 ± 10 μg to confirm that the accuracy meets the standard.

[0045] 5. Sample moisture determination:

[0046] (1) Liquid (insulating oil) testing

[0047] ① Select a liquid injector of appropriate capacity, rinse with the sample to be tested 2 to 3 times, and extract the sample for later use.

[0048] ② Press the Start key on keyboard 12, and the display screen 13 will be reset;

[0049] ③ Inject the sample into the electrolyte in the anode chamber 1 through the injection stopcock 5. Insert the needle tip into the liquid, avoiding contact with the cell wall or electrode. After injection, the sample is automatically titrated. When the endpoint is reached, the buzzer sounds, indicating that the status is normal. The display screen 13 shows the water content. The water content is automatically calculated and stored according to the selected formula and input data.

[0050] ④ Enter new data according to the prompts on display screen 13. The computer control system will automatically calculate the new moisture content based on the currently measured moisture content and automatically store the data.

[0051] (2) Solid

[0052] ① Adopting such Figure 5 The solid sampler shown was washed with water, dried, and then weighed.

[0053] ②Replace the cover immediately after removing the 25mm sample.

[0054] ③ Weigh the solid sampler containing the sample; the sample weight is the difference between the two weighings.

[0055] ④ Press the Start key (12) on the keyboard to reset;

[0056] ⑤ Remove the sample inlet stopcock 5 from the electrolytic cell, as follows: Figure 6 Insert the solid sampler as shown by the solid line, and wait for the display screen 13 to count to the measurement endpoint, so that the water that has entered the anode chamber 1 is fully absorbed by the electrolyte;

[0057] ⑥ Press the Start button again to reset, such as Figure 6 Rotate the solid sampler 180 degrees as shown by the dotted line to allow the sample to fall into the electrolyte (do not allow it to contact the cell wall or electrodes). At the end of the measurement, remove the solid sampler and insert the injection stopcock 5 (the method for determining the water content of solids and liquids is the same).

[0058] (3) Gas

[0059] Adopting such Figure 7 The gas sampler shown is connected to the electrolytic cell; during the measurement, about 150 ml of electrolyte is injected into the anode chamber 1, and the gas flow rate is controlled at 100 ml / min and kept stable; if the electrolyte is significantly reduced, about 20 ml of ethylene glycol is injected to replenish it.

[0060] The above descriptions are merely embodiments of this utility model. Commonly known technical solutions and / or characteristics are not described in detail here. It should be noted that those skilled in the art can make various modifications and improvements without departing from the technical solution of this utility model. These modifications and improvements should also be considered within the scope of protection of this utility model, and will not affect the effectiveness of the implementation of this utility model or the practicality of the patent. The scope of protection claimed in this application should be determined by the content of its claims, and the specific embodiments described in the specification can be used to interpret the content of the claims.

Claims

1. An automatic liquid draining trace moisture analyzer, comprising an electrolytic cell and a main unit, characterized in that: The electrolytic cell includes an anode chamber (1) and a cathode chamber (2). A ceramic filter plate (10) is provided between the anode chamber (1) and the cathode chamber (2). The ceramic filter plate (10) is used to separate the anode chamber (1) and the cathode chamber (2) to prevent iodine molecules in the anode chamber (1) from diffusing to the cathode chamber (2). The top of the anode chamber (1) is provided with a sample inlet tube (4) and a detachable measuring electrode (3). The inlet of the sample inlet tube (4) is provided with a detachable sample inlet stopcock (5). The anode chamber (1) is provided with a drain port and a stir bar (6) for stirring reagents. The top of the cathode chamber (2) is provided with a liquid inlet, a detachable electrolytic electrode (7), and a drying tube (8). The liquid inlet is provided with a drain port and a stir bar (6) for stirring reagents. The disassembled sealing plug and drying tube (8) are used to place the color-changing silica gel (9); the host includes a computer control system, as well as a keyboard (12), display screen (13), electrolytic electrode socket (14), measuring electrode socket (15), and automatic liquid addition and drainage assembly that are electrically connected to the computer control system. The electrolytic electrode socket (14) and measuring electrode socket (15) are used to connect the electrolytic electrode (7) and the measuring electrode (3), respectively. The computer control system is used to monitor the electrolysis status of the electrolytic cell in real time, calculate the moisture content, and control the automatic liquid addition and drainage assembly to discharge the waste liquid in the electrolytic cell from the drain port. The display screen (13) is used to display the electrolysis curve and moisture content in real time.

2. The trace moisture analyzer according to claim 1, characterized in that: The automatic liquid addition and drainage assembly includes a liquid addition and drainage control switch (16), an air pump, a three-way solenoid valve, a reagent bottle, and a sealed bottle. The liquid addition and drainage control switch (16) and the air pump are installed on the main unit, and the three-way solenoid valve is installed at the drain port of the electrolytic cell. The liquid addition and drainage control switch (16), the air pump, and the three-way solenoid valve are all electrically connected to the computer control system. The reagent bottle is connected to the air pump through a reagent bottle air pipe, and the waste liquid bottle is connected to the air pump through a waste liquid bottle air pipe. The computer control system can control the positive or negative pressure output of the air pump according to the signal sent by the liquid addition and drainage control switch (16), and control the three-way solenoid valve to switch the passage between the electrolytic cell and the waste liquid bottle or the reagent bottle.

3. The trace moisture analyzer according to claim 2, characterized in that: The computer control system includes a data acquisition module, a microprocessor, and a data storage module. The data acquisition module is used to acquire electrical signals from the measuring electrode (3) and the electrolysis electrode (7). The microprocessor is used to automatically store blank current based on the signals acquired by the data acquisition module and a preset blank current storage algorithm, and to calculate the moisture content according to the preset formula and output it to the display screen (13). The data storage module is used to store historical test data.

4. The trace moisture analyzer according to any one of claims 1 to 3, characterized in that: It also includes a sample injection assembly, which includes a liquid injector, a solid injector and a gas injector; the liquid injector is a syringe with a needle; the solid injector includes a detachably connected injection bend (24) and a cap (25); the gas injector includes a gas storage tank (26) and a gas delivery pipe (27), the gas delivery pipe (27) is used to deliver the gas in the gas storage tank (26) to the electrolytic cell, and the gas delivery pipe (27) is equipped with a pump body (28) that can control the gas flow rate of the gas delivery pipe (27).

5. The trace moisture analyzer according to claim 4, characterized in that: The host is also equipped with a temperature sensor for detecting ambient temperature. The data acquisition module can collect the ambient temperature detected by the temperature sensor and output a temperature drift compensation signal.

6. The trace moisture analyzer according to claim 5, characterized in that: The host computer is also equipped with a thermal printer (19), which is used to automatically print test data and historical records.

7. The trace moisture analyzer according to claim 6, characterized in that: The host is also equipped with a stirring speed knob (20) that is electrically connected to the computer control system. The computer control system can control the rotation speed of the stir bar (6) in the electrolytic cell according to the signal sent by the stirring speed knob (20).

8. The trace moisture analyzer according to claim 7, characterized in that: The host is also equipped with an RS232 interface (21) and a cooling fan (22). The RS232 interface (21) can be used for data communication with external devices, and the cooling fan (22) is used to reduce the operating temperature of the host.

9. The trace moisture analyzer according to claim 8, characterized in that: The connections between the measuring electrode (3) and the anode chamber (1), the electrolytic electrode (7) and the cathode chamber (2), the drying tube (8) and the cathode chamber (2), and the sample inlet tube (4) and the sample inlet stopcock (5) are all sealed with ground joints and have a vacuum grease sealing layer.

10. The trace moisture analyzer according to claim 9, characterized in that: The host is equipped with an electrolytic cell holder (11) for installing an electrolytic cell.

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