CN110806440A - A coulometric micro water meter - Google Patents

Abstract

The present application discloses a coulometric micro-water meter, including a sampling device, a detection device, and a data processing device, wherein the sampling device includes a sample tray and a sampling assembly, and the sample tray is provided with a liquid carrier bottle and at least one sample The carrier liquid bottle is filled with dry insulating oil, and the sample bottle is filled with the oil sample to be tested; the sampling assembly includes a sampling tube, a sampling head communicated with the sampling tube, a five-element pump, a sample injection Pipe, waste liquid pipe and waste liquid bottle, the use of the sampling device can realize the automatic sampling of the oil sample to be measured, which improves the accuracy, detection speed and automation degree of moisture content detection. The coulometric micro-water meter of the present application is simple in structure, easy to operate, and has strong operability, and can be widely used.

Description

A coulometric micro water meter

technical field

The present application relates to the technical field of improvement of insulating oil micro-water meter, in particular to a coulometric micro-water meter.

Background technique

Electrical insulating oil is a kind of lubricating oil prepared from deeply refined lubricating base oil and adding antioxidants. It is used in electrical equipment such as transformers, oil-immersed switches, transformers, capacitors and cables. An important quality monitoring indicator of electrical insulating oil is moisture content. Moisture can reduce the breakdown voltage of electrical insulating oil, increase the dielectric loss factor and accelerate the aging of insulating oil. Therefore, in the electrical insulating oil in operation, if there is a trace amount of moisture. , it will cause great harm to the electrical properties and physical and chemical properties of the insulating medium, and in severe cases, the paper insulation will be permanently damaged, resulting in reduced operating reliability and life of oil-filled electrical equipment, and even lead to insulation accidents.

In order to prevent the occurrence of the above problems, in the actual application process, it is necessary to regularly measure the moisture content of the running electrical insulating oil. At present, the method for measuring moisture content in electrical insulating oil is Coulomb titration, which adopts an electrolytic current automatic control system to ensure high sensitivity and high speed in the analysis process. However, manual sampling is required during the measurement process (the sampling volume is 1 mL ) is added to the detector for detection. In the process of manual sampling, the sampling error caused by human factors is relatively large, thus affecting the accuracy of the detected moisture content.

SUMMARY OF THE INVENTION

The present application provides a coulometric micro-water meter to solve the problem of low detection accuracy of the existing coulometric micro-water meter.

The present application provides a coulometric micro-water meter, including a sampling device, a detection device, and a data processing device, wherein the sampling device includes a sample tray and a sampling assembly, and the sample tray is provided with a carrier liquid bottle and at least a A sample bottle, the carrier liquid bottle is filled with dry insulating oil, and the sample bottle is filled with an oil sample to be tested; the sampling assembly includes a sampling tube, a sampling head communicated with the sampling tube, a five-element pump, Sampling tube, waste tube and waste bottle;

The detection device includes an electrolysis assembly, the electrolysis assembly includes a sealed oil cup and positive and negative electrodes, the sealed oil cup is provided with a liquid inlet, and the liquid inlet communicates with the liquid inlet pipe of the sampling assembly, The sealed oil cup is filled with a test liquid, and the test liquid is used for redox reaction with water molecules in the oil sample to be tested during the electrolysis process; the positive and negative electrodes are connected to the data processing device, and are used for the electrolysis process The voltage data in the device is sent to the data processing device;

The data processing device includes a controller, a data processor and a display. The controller is used to control the data processing module to calculate the micro-water content of the oil sample to be tested according to the above-mentioned voltage data, and to control the display to display the calculated micro-water content. .

Optionally, the quintuple pump includes a rotating disk and a motor, and the rotating disk is provided with a sample measuring cavity, a washing liquid cavity and No. 1-5 communication pipes, wherein the No. 1-3 communication pipes are connected to the sample measurement chamber. The cavity is communicated, and the communication pipes No. 4 and 5 are communicated with the lotion cavity,

The angle between the No. 1 and No. 2 communication pipes matches the angle between the sampling pipe and the waste liquid pipe;

The angle between the No. 2 and No. 3 communicating pipes matches the angle between the sampling pipe and the sampling pipe;

The angle between the No. 4 and No. 5 communicating pipes matches the angle between the sampling pipe and the waste liquid pipe.

Optionally, the sampling assembly includes a sample introduction support, and the sample introduction support is used for erecting the quintuple pump.

Optionally, the sample disk is a rotating disk.

Optionally, an air pressure balance port is provided on the sealed oil cup.

Optionally, the detection device further includes a magnetic stirrer, and accordingly, a magnetic rotor is provided in the sealed oil cup.

Optionally, the positive electrode and the negative electrode are connected to the controller of the data processing device through a data connection line and a data terminal.

Optionally, the data processing device further includes a setting keyboard.

Optionally, the coulometric micro-water meter further includes a printer connected to the data processing device, and the printer is used to print the micro-water content of the oil sample to be tested.

The application provides a coulometric micro-water meter, including a sample injection device, a detection device and a data processing device, wherein the sample injection device can realize automatic sample injection of the oil sample to be measured, which improves the accuracy of detection of moisture content, and the detection of Speed and degree of automation. In addition, the Coulometric micro-water meter of the present application has a simple structure, is easy to operate, has strong operability, and can be widely used.

Description of drawings

In order to illustrate the technical solutions of the present application more clearly, the accompanying drawings required in the embodiments will be briefly introduced below. Obviously, for those of ordinary skill in the art, without creative work, the Additional drawings can be obtained from these drawings.

Fig. 1 is the structural representation of the Coulomb method micro-water meter of the application;

FIG. 2 is a schematic structural diagram of the five-element pump of the present application.

The symbols in Figure 1-2 are respectively indicated as: 1-Sampling device, 11-Sample tray, 111-Carrier bottle, 112-Sample bottle, 12-Sampling tube, 121-Sampling head, 13-Pentinary pump, 131 -Sampling cavity, 132-washing liquid cavity, 14-injection tube, 15-waste liquid tube, 16-waste liquid bottle, 17-injection bracket, 18-base, 2-detection device, 21-sealed oil cup, 211-liquid inlet, 212-air pressure balance port, 22-positive and negative electrodes, 23-data terminal, 24-magnetic stirrer, 25-magnetic rotor, 3-data processing device, 31-display, 32-setting keyboard , 33-printer.

Detailed ways

The present application provides a coulometric micro-water meter for measuring the moisture content in electrical insulating oil. Through automatic sampling of the oil sample to be measured, the problem of large errors caused by artificial sampling is avoided, and the accuracy of moisture content detection is improved. degree, detection speed and degree of automation.

FIG. 1 is a schematic structural diagram of a coulometric micro-water meter of the application. As shown in FIG. 1 , the coulometric micro-water meter includes a sampling device 1 , a detection device 2 and a data processing device 3 , wherein the sampling device 1 includes a sample tray 11 With the sampling assembly, the sample tray 11 is provided with a carrier liquid bottle 111 and at least one sample bottle 112, the liquid carrier bottle 111 contains dry insulating oil, and the sample bottle 112 contains the oil sample to be tested; the sampling assembly includes a sampling tube 12, The sampling head 121 , the quintuple pump 13 , the sampling pipe 14 , the waste liquid pipe 15 and the waste liquid bottle 16 communicated with the waste liquid pipe 15 are connected with the sampling pipe 12 . In the present application, the bottle mouth of the carrier bottle 111 or a certain sample bottle 112 is sealed with soft rubber, and the sampling head 121 can be easily inserted and pulled out. In addition, the number of sample bottles is multiple, which can prevent multiple oil samples to be tested, so as to realize the continuous detection of multiple oil samples to be tested, thereby improving the detection efficiency.

In the present application, the sample tray 11 is a rotating disk. The sample tray 11 is provided with a liquid carrier bottle 111 and several sample bottles 112. Each sample bottle 112 contains an oil sample to be tested. 11, the sampling head 121 can be made to correspond to the carrier liquid bottle 111 or a certain sample bottle 112, so as to complete the extraction process of the dry insulating oil or the oil sample to be tested. Of course, the sampling head 121 can also be set as a mobile type, and the accurate sampling of the dry insulating oil or the oil sample to be tested is completed through the relative displacement between the sampling head 121 and the rotating disk.

In this application, the quintuple pump 13 is used for quantitative sampling of the oil sample to be measured. FIG. 2 is a schematic structural diagram of the quintuple pump of the application. As shown in FIG. 2 , the quintuple pump 13 includes a rotating disk and a motor. There are sample measuring chamber 131 , washing liquid chamber 132 and No. 1-5 connecting pipes, wherein No. 1-3 connecting pipes are communicated with sample measuring chamber 131 , and No. 4 and No. 5 connecting pipes are connected with washing liquid chamber 132 . The relative positions between the No. 1-5 communicating pipes can be adjusted according to the positions between the sampling pipe 12, the sampling pipe 14 and the waste liquid pipe 15. In this application, the angle between the No. 1 and No. 2 communicating pipes is The angle between the sampling pipe 12 and the waste liquid pipe 15 is matched, the angle between the connecting pipes No. 2 and No. 3 is matched with the angle between the sampling pipe 14 and the sampling pipe 12, and the angle between No. 4 and No. 5 is matched. The angle between the communication pipes matches the angle between the sampling pipe 12 and the waste liquid pipe 15 .

In order to facilitate fixing the positions between the five-element pump 13, the sampling pipe 12, the sampling pipe 14 and the waste liquid pipe 15, in this application, the sampling assembly also includes a sampling support 17, and the sampling support 17 is used for erecting the five-element pump 13. , Correspondingly, the sampling pipe 12 , the sampling pipe 14 and the waste liquid pipe 15 are set correspondingly according to the position of the five-element pump 13 . In order to facilitate the fixing of the sample introduction support 17, the sample introduction device 1 of the present application further includes a base 18, and the base 18 is provided with a sample tray 11 and a sample introduction support 17, and the sample introduction support 17 can be fixedly arranged on the base 18 or can be movably connected. On the base 18, the sample injection support 17 can move relative to the sample tray 11 on the base 18, so as to facilitate sampling.

The process of cleaning the pipeline by using the five-element pump 13 specifically includes: rotating the sample plate 11, controlling the sampling tube 12, so that the sampling head 121 corresponds to the carrier liquid bottle 111, and then rotating the rotating plate, so that the No. 3 connecting tube is aligned with the sampling tubes 12, 2 The No. 3 connecting pipe is aligned with the sampling pipe 14, the motor is started, and the dry insulating oil is extracted from the carrier liquid bottle 111. The dry insulating oil enters the sampling chamber 131 from the No. 3 connecting pipe, and then enters the sampling pipe 14 through the No. 2 connecting pipe. The sampling tube and the sampling tube can be cleaned until the charge amount of the two electrodes in the sealed oil cup 21 remains unchanged by entering the sampling tube 14 into the sealed oil cup 21 .

The process of obtaining a quantitative oil sample to be tested by using the quintuple pump 13 specifically includes:

Step 1, select a sample chamber 131 with a suitable specification, for example, a sample chamber 131 of 1ml, 1.5ml, 2ml or 5ml can be selected. Of course, those skilled in the art can select a sample chamber 131 with a corresponding specification according to actual needs, which belongs to this specification. the scope of protection applied for;

Step 2, cleaning the sample chamber 131, which specifically includes: rotating the sample plate 11 so that the sampling head 121 corresponds to the carrier liquid bottle 111; then, rotating the rotating plate to align the No. 1 connecting tube with the sampling tube 12 and the No. 2 connecting tube Waste liquid pipe 15, start the motor, extract dry insulating oil from the carrier liquid bottle 111, the dry insulating oil enters the sample chamber 131 from the No. 1 connecting pipe, clean the test sample, and the cleaned dry insulating oil passes through the No. 2 connecting pipe Enter the waste liquid bottle 16 to complete the cleaning process of the sample chamber 131;

Step 3, extracting the oil sample to be tested, which specifically includes: rotating the sample disc 11 so that the sampling head 121 corresponds to the sample bottle 112 of the oil sample to be tested, starting the motor, extracting the oil sample to be tested from the sample bottle 112, and making the sample chamber 131 Filled with oil sample to be tested;

Step 4, using dry insulating oil to expel the oil sample to be tested in the sample chamber 131 to the detection device 2, which specifically includes: rotating the sample disk 11 so that the sampling head 121 corresponds to the carrier liquid bottle 111; then, rotating the rotating disk to make the 4 The No. 1 connecting pipe is aligned with the sampling pipe 12, the No. 5 connecting pipe is aligned with the waste liquid pipe 15, the motor is started, the dry insulating oil is extracted from the carrier liquid bottle 111, the oil sample to be tested in the No. 1 connecting pipe is removed, and the No. 1 connecting pipe is Fill with dry insulating oil; after that, rotate the rotating disk to align the No. 3 connecting pipe with the sampling pipe 12 and the No. 2 connecting pipe with the sampling pipe 14, start the motor, extract the dry insulating oil from the carrier liquid bottle 111, and use the dry insulating oil The oil pushes the oil sample to be measured in the sample chamber 131 to the detection device 2, and the quantitative acquisition of the oil sample to be measured is completed. It should be noted that in this process, there is also a small amount of oil sample to be tested in the No. 2 connecting pipe. If the diameter of the No. 2 connecting pipe is small, the oil sample to be tested in the No. 2 connecting pipe can be ignored; if the No. 2 connecting pipe has a small diameter The diameter of the No. 2 connecting pipe is large, so the oil sample to be tested in the No. 2 connecting pipe cannot be ignored. When designing the capacity of the sample chamber 131, the capacity of the No. 2 connecting pipe should be considered to reduce the sampling error. It should be noted that in the above process, the sampling action of the sampling head 121 and the rotation action of the sample disc 11 and the rotating disc can be implemented by corresponding motors, which belong to the prior art and will not be described in detail here.

In this application, the detection device 2 includes an electrolysis assembly, the electrolysis assembly includes a sealed oil cup 21 and positive and negative electrodes 22, the sealed oil cup 21 is provided with a liquid inlet 211, and the liquid inlet 211 is communicated with the liquid inlet pipe of the sampling assembly, The sealed oil cup 21 is filled with a test liquid, and the test liquid is used for redox reaction with water molecules in the oil sample to be tested during the electrolysis process; the positive and negative electrodes 22 are connected to the data processing device 3, and are used for the voltage during the electrolysis process. The data is sent to the data processing device 3 . In the present application, the positive electrode and the negative electrode 22 are connected to the controller of the data processing device 3 through a data connection line and a data terminal 23 .

In order to prevent the moisture of the outside air from entering the sealed oil cup 21 and affecting the experimental data, the sealed oil cup 21 in this application has good sealing performance, and an air pressure balance port 212 is provided on the sealed oil cup 21 to facilitate the test. The oil sample can smoothly enter the sealed oil cup 21 through the liquid inlet pipe. The air pressure balance port 212 communicates with the air and the inside of the sealed bottle to balance the air pressure inside and outside the sealed oil cup 21 .

In order to make the electrolytic reaction in the sealed oil cup 21 more sufficient, the detection device 2 further includes a magnetic stirrer 24 . Correspondingly, the sealed oil cup 21 is provided with a magnetic rotor 25 . During the electrolysis reaction, the magnetic rotor 25 can agitate the detection solution, so as to ensure that the electrolysis reaction is sufficient and fast.

The data processing device 3 includes a controller, a data processor and a display 31. The controller is used to control the data processing module to calculate the micro water content of the oil sample to be tested according to the above voltage data, and control the display 31 to display the calculated micro water content. Of course, the controller is also used to control the action of the quintuple pump 13 , including controlling the rotation of the rotating disk and the start and stop of the motor. The control process can be realized by using the prior art, and will not be described in detail here. In addition, the controller is also used to control the rotation of the sample tray 11 and the action of the sampling head 121, and the control process can be realized by using the prior art, which will not be described in detail here.

In this application, the coulometric micro-water meter further includes a printer 33 connected to the data processing device 3 , and the printer 33 is used to print the micro-water content of the oil sample to be measured.

In the present application, the data processing device 3 further includes a setting keyboard 32 , and the keyboard is used to control the start and stop of the sample feeding device 1 , the detection device 2 and the operation of the printer 33 . In order to facilitate the cleaning of the sample chamber 131 and the pipes in the instrument, in the present application, the keyboard includes a cleaning button, and a one-key operation of the cleaning process can be realized through the cleaning button.

In this application, the principle of calibrating the micro-water content specifically includes: the test liquid is iodine, pyridine and methanol, when there is water in the sealed oil cup 21, the iodine is reduced by sulfur dioxide, and in the presence of pyridine and methanol, hydrogen iodine is generated Acid pyridine and methyl hydrogen sulfate pyridine, the reaction formula is as follows:

H ₂ O+I ₂ +SO ₂ +3C ₅ H ₅ N——→2C ₅ H ₅ N·HI+C ₅ H ₅ N·SO ₃

C ₅ H ₅ N·SO ₃ +CH ₃ OH——→C ₅ H ₅ N·HSO ₄ CH ₃ ,

During electrolysis, the electrodes react as follows:

Anode: 2I ^- -2e——→I ₂ ,

Cathode: 2H ⁺ +2e——→2I ^- , I ₂ +2e——→2I ^- ,

The iodine produced in the electrolysis process reacts with the water molecules in the oil sample to be tested to generate hydroiodic acid, until all the water in the oil sample to be tested is reacted, and the reaction end point is indicated by a detection unit composed of a pair of platinum electrodes. In the whole process, sulfur dioxide is consumed, and its consumption is equal to the number of moles of water.

According to Faraday's law of electrolysis, the amount of electricity used in electrolysis is proportional to the amount of iodine, that is, electrolysis of 1 mol of iodine and consumption of 1 mol of water requires twice the electricity of 96493C. The calculation formula is as follows:

which is

In formula (1): m/μg is the moisture in the oil sample to be tested, Q/mC is the electrolytic electricity, and 18 is the relative mass of water.

According to the injection volume of the oil sample to be tested, the moisture content is calculated according to the formula (2):

In formula (2): ρ/mg·L ^-1 is the moisture content in the oil sample to be tested, m/mg is the moisture in the sample to be tested, and V/mL is the injection volume of the oil sample to be tested.

打印检测结果。The use process of the coulometric micro-water meter of the present application is as follows: add the test liquid to the sealed oil cup, add the oil sample to be tested to the sample bottle on the sample tray, and add dry insulating oil to the carrier liquid bottle; by setting the keyboard, set the Relevant parameters, including sampling volume, injection port, etc.; click the cleaning button on the setting keyboard, suck the dry insulating oil from the carrier liquid bottle, and pass it into the sealed oil cup, so that the pipeline is filled with dry oil samples, and wait until the two electrodes are charged. Click the sample button on the setting keyboard, and the oil samples to be tested will be tested in turn; after the test is completed, the test results will be displayed on the display, and the test results include electrolytic electricity Q and water content

Print the test results.

The application provides a coulometric micro-water meter, including a sample injection device, a detection device and a data processing device, wherein the sample injection device can realize automatic sample injection of the oil sample to be measured, which improves the accuracy of detection of moisture content, and the detection of Speed and degree of automation. In addition, the Coulometric micro-water meter of the present application has a simple structure, is easy to operate, has strong operability, and can be widely used.

The above-described embodiments of the present application do not limit the protection scope of the present application.

Claims (9)

1. The coulometric method micro-water meter is characterized by comprising a sample feeding device (1), a detection device (2) and a data processing device (3), wherein the sample feeding device (1) comprises a sample disc (11) and a sampling assembly, a liquid carrying bottle (111) and at least one sample bottle (112) are arranged on the sample disc (11), dry insulating oil is contained in the liquid carrying bottle (111), and an oil sample to be detected is contained in the sample bottle (112); the sampling assembly comprises a sampling tube (12), a sampling head (121) communicated with the sampling tube (12), a quinary pump (13), a sample inlet tube (14), a waste liquid tube (15) and a waste liquid bottle (16);

the detection device (2) comprises an electrolytic assembly, the electrolytic assembly comprises a sealed oil cup (21) and a positive electrode (22) and a negative electrode (22), a liquid inlet (211) is formed in the sealed oil cup (21), the liquid inlet (211) is communicated with a liquid inlet pipe of the sampling assembly, a test liquid is contained in the sealed oil cup (21), and the test liquid is used for carrying out redox reaction with water molecules in an oil sample to be detected in the electrolytic process; the positive electrode (22) and the negative electrode (22) are connected to a data processing device (3) and are used for sending voltage data in the electrolytic process to the data processing device (3);

the data processing device (3) comprises a controller, a data processor and a display (31), wherein the controller is used for controlling the data processing module to calculate the micro water content of the oil sample to be measured according to the voltage data, and controlling the display (31) to display the calculated micro water content.

2. The coulometric micro-water meter according to claim 1, characterized in that the quinary pump (13) comprises a rotating disk and a motor, the rotating disk is provided with a sample measuring cavity (131), a washing liquid cavity (132) and a No. 1-5 communicating pipe, wherein the No. 1-3 communicating pipe is communicated with the sample measuring cavity (131), the No. 4 and No. 5 communicating pipes are communicated with the washing liquid cavity (132),

the included angle between the No. 1 communicating pipe and the No. 2 communicating pipe is matched with the included angle between the sampling pipe (12) and the waste liquid pipe (15);

the included angle between the No. 2 and No. 3 communicating pipes is matched with the included angle between the sampling pipe (14) and the sampling pipe (12);

the included angle between the No. 4 and No. 5 communicating pipes is matched with the included angle between the sampling pipe (12) and the waste liquid pipe (15).

3. The coulometric microammeter according to claim 1, characterized in that the sampling assembly comprises a sample holder (17), the sample holder (17) being used to mount the quinary pump (13).

4. The coulometric microammeter according to claim 1, characterized in that the sample disk (11) is a rotating disk.

5. The coulometric microaqueometer according to claim 1, characterized in that the sealing oil cup (21) is provided with a gas pressure balancing port (212).

6. The coulometric microammeter according to claim 1, characterized in that said detection device (2) further comprises a magnetic stirrer (24), and correspondingly, a magnetic rotor (25) is provided in said sealed oil cup (21).

7. The coulometric microassay device according to claim 1, characterized in that said positive and negative electrodes (22) are connected to the controller of said data processing device (3) by means of data connection lines and data terminals (23).

8. The coulometric micro-water meter according to claim 1, characterized in that the data processing device (3) further comprises a setup keyboard (32).

9. The coulometric micro-water meter according to claim 1, characterized in that it further comprises a printer (33) connected to the data processing device (3), the printer (33) being used to print the micro-water content of the oil sample to be measured.

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