CN217033723U - Pour point and condensation point measuring device - Google Patents
Pour point and condensation point measuring device Download PDFInfo
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- CN217033723U CN217033723U CN202220816034.8U CN202220816034U CN217033723U CN 217033723 U CN217033723 U CN 217033723U CN 202220816034 U CN202220816034 U CN 202220816034U CN 217033723 U CN217033723 U CN 217033723U
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Abstract
The utility model belongs to the field of petrochemical industry, and particularly relates to a pour point and pour point measuring device, and more particularly relates to a pour point and pour point measuring device for petroleum and petroleum products thereof. The utility model judges whether the oil sample is solidified or not by measuring the change of the resistance twice before and after inclination, overcomes the defect that the error is larger only by manual judgment in the existing measuring method, and has simple and reliable related resistance measuring structure and wide application range.
Description
Technical Field
The utility model belongs to the field of petrochemical industry, and particularly relates to a pour point and pour point measuring device, and more particularly relates to a pour point and pour point measuring device for petroleum and petroleum products.
Background
The highest temperature when petroleum products such as diesel oil, lubricating oil, insulating oil, hydraulic oil and the like are cooled to a liquid level without moving under test conditions is called as a condensation point; the lowest temperature at which an oil can flow when cooled under specified conditions is known as the pour point. When the temperature falls below the condensation point of the oil, the oil loses its normal fluidity at all, and when the temperature reaches or exceeds the pour point of the oil, the oil is able to flow. Pour and pour points are important indicators for the low temperature fluidity of oils.
The current national standard for measuring the condensation point of petroleum products is GB 510-2018 petroleum product condensation point determination method, which is to put a sample in a specified test tube, incline the test tube at 45 ℃ and keep the test tube for 1min when the sample is cooled to an expected temperature, observe whether the liquid surface moves or not, and the highest temperature when the sample is cooled to the liquid surface and does not move is called the condensation point. The current national standard for measuring the pour point of petroleum products is GB/T3535-2006 "pour point determination method for petroleum products", which comprises the steps of preheating a sample, cooling the preheated sample at a specified rate, checking the fluidity of the preheated sample at intervals of 3 ℃, and recording the lowest temperature at which the preheated sample can flow as the pour point. The two methods define a basic method for measuring the condensation point and the pour point, whether a sample moves or flows needs to be judged manually, and an automatic micro-condensation point tester is only suitable for testing the diesel fraction sample without the additive and cannot be used for testing the diesel fraction sample with the additive. In recent years, there have been applications and ideas related to measurement of pour point and pour point by capacitance method, camera image recognition method, pressure method, laser method, X-ray method, photoelectric method, ultrasonic method, vibration method, near infrared spectroscopy, and the like.
CN200420070208.2 discloses a pour point detector for petroleum and petroleum products, which uses optical fiber reflection method to detect the pour point of petroleum products, when the oil surface of the sample is perpendicular to the detecting optical fiber, the emitted light is reflected by the oil surface and received, and high voltage signal is output through an amplifier, when the two positions are not perpendicular, the emitting tube is refracted and scattered by the oil surface, and the amplifier outputs low voltage signal, but the structure of the detector is complex, and the sensitivity is low. CN201410338186.1 discloses a practical measuring instrument, which can measure the pour point of petroleum and petroleum products quickly, when the sample is not frozen, the measuring instrument can detect the pressure change through a pressure sensor, the liquid level of the sample rises, so as to measure the pour point of the oil product, and the pour point temperature plus one degree is the pour point of the sample, but the pour point obtained by using the measuring instrument is often inaccurate and has larger error. CN201921475203.0 has related to a full-automatic pour point tester that adopts pressure detection, measures the pour point of oil through setting up pressure sensor and infrared thermometer, subtracts several degrees and obtains the pour point of oil again, though this kind of tester simple structure has solved the problem that needs a plurality of cold baths to frequently operate in traditional method, but the pour point of survey has the problem that the accuracy is lower yet. CN201610044124.9 discloses a crude oil condensation point measuring device based on ultrasonic technology and a measuring method thereof, and the measuring method can judge whether an oil sample is gelled or not by judging the flowing condition of a sample to be measured in a condensation point test tube by measuring the attenuation change of the amplitude of sound waves, thereby reducing the measuring error of the crude oil condensation point. However, this method requires recording the pulse echoes reflected many times, and repeatedly comparing the attenuation degree of the detected waveform pattern with the first waveform, which makes the operation more complicated.
Therefore, a novel and accurate pour point and condensation point measuring device is urgently needed to be provided, the measuring device can not only reduce errors of manual judgment, but also guarantee the consistency of experimental operation at every time, and meanwhile, the device needs to be simple in structure, high in detection efficiency and wide in application range.
SUMMERY OF THE UTILITY MODEL
The utility model aims to provide a pour point and pour point measuring device which is simple and stable in structure, can realize full-automatic measurement, not only completely meets the regulations in GB/T3535-.
In order to achieve the above object, the present invention provides a pour point and pour point measuring device comprising:
the measuring system comprises a resistance measuring system, a temperature control system and a vertically arranged oil sample cylinder; a plug is arranged at the top of the oil sample cylinder, a sample inlet is formed in the plug, and an annular marking line is arranged on the cylinder wall of the oil sample cylinder; the resistance measuring system comprises a resistance meter, two leads, a first comb-shaped metal wire group and a second comb-shaped metal wire group, wherein the two conducting wires are positioned at two sides of the first tooth comb-shaped metal wire group and the second tooth comb-shaped metal wire group, the first tooth comb-shaped metal wire group and the second tooth comb-shaped metal wire group both comprise a plurality of metal wires which are fixed on the inner wall of the oil sample cylinder and are parallel to the bottom of the oil sample cylinder, the first tooth comb-shaped metal wire group and the second tooth comb-shaped metal wire group are arranged in a mutually crossed way, and is respectively connected with the anode and the cathode of a resistance meter through leads, the metal wire at the top of the inner wall of the oil sample cylinder is positioned 2-5 mm below the annular marking, the distance between the adjacent metal wires is 0.02-0.10 mm, the length of the metal wire is less than half of the perimeter of the oil sample cylinder, one end of the metal wire is connected with a conducting wire on one side, and the other end of the metal wire is 3-5 mm away from the conducting wire on the other side in the direction of the cylinder wall of the oil sample cylinder; the temperature control system comprises a temperature sensor and a temperature regulator, the temperature sensor is arranged in the center of the oil sample cylinder, and the temperature regulator is arranged on the periphery of the oil sample cylinder and used for regulating the temperature of the oil sample;
a drive system for controlling rotation of the measurement system;
and the control system is used for automatically controlling the pour point and pour point measuring device.
Preferably, the wire diameter is 0.025mm to 0.100 mm.
Preferably, the number of the metal wires is 25 or more, and more preferably, the number of the metal wires is 25 to 111.
Preferably, the thermostat comprises a heating module and a cooling module; the heating module comprises a heating wire, and the refrigerating module comprises a multistage semiconductor refrigerator and a heat dissipation copper pipe.
Preferably, the oil sample cylinder is a glass measuring cylinder; the drive system includes a stepper motor.
Preferably, the distance between the detection end of the temperature sensor and the bottom of the oil sample cylinder is 8-10 mm, and the distance between the annular marking and the bottom of the oil sample cylinder is 30-60 mm.
Preferably, the pour point and condensation point measuring device further comprises an automatic sample feeding system, an automatic blowdown system and a liquid level sensor, and the oil sample cylinder is further provided with a drain outlet; the automatic sample introduction system is connected with the sample inlet, and the automatic blowdown system is connected with the blowdown port; the liquid level sensor is arranged in the oil sample cylinder.
Preferably, the automatic sample feeding system comprises a flexible oil inlet pipe, an oil inlet pump and a sample feeding oil cup; the automatic sewage draining system comprises a flexible sewage draining pipe and a sewage draining pump.
Preferably, the sample inlet, the oil inlet pump and the sample adding oil cup are connected through the flexible oil inlet pipe.
Preferably, the drain outlet and the drain pump are connected through the flexible drain pipe.
Compared with the prior art, the utility model has the following advantages:
1. the utility model has simple and stable structure, not only completely meets the requirements in GB/T3535-2006 and GB/T510-2018, but also has wide application range, can measure the small volume resistivity of 1.0 multiplied by 1015Omega m colorless transparent oil samples, such as transformer oil, are also suitable for colored oil samples, including diesel oil, turbine oil and fire-resistant oil containing additives, having an electrical resistivity of equal volume of less than 1.0X 1015Pour point and pour point of omega m liquid oil sample.
2. According to the utility model, whether the oil sample is solidified is judged by setting the resistance measuring system to measure the change of the resistance twice before and after the inclination, so that a large error caused by manual judgment is avoided.
3. The utility model has accurate measuring result, can realize full-automatic measurement, overcomes the defect that the experimental sample needs to be frequently taken out to the ambient temperature for observation in the traditional measuring process, and ensures the consistency of each experimental operation.
Additional features and advantages of the utility model will be set forth in the detailed description which follows.
Drawings
The above and other objects, features and advantages of the present invention will become more apparent by describing in more detail exemplary embodiments thereof with reference to the attached drawings, in which like reference numerals generally represent like parts throughout.
FIG. 1 shows a front view of a glass measuring cylinder in an embodiment of the present invention.
FIG. 2 shows a side view of a glass measuring cylinder in an embodiment of the present invention.
FIG. 3 shows a schematic representation of the non-solidified oil sample in the glass cylinder after tilting to an angle of 45 ° to the horizontal in the measurement of the solidification point according to one embodiment of the present invention.
Figure 4 shows a schematic representation of the solidification of an oil sample in a glass cylinder after tilting to an angle of 45 deg. to the horizontal in a measurement of the solidification point according to one embodiment of the present invention.
FIG. 5 shows a schematic of the non-solidified oil sample in the glass cylinder after tilting to a horizontal position in the pour point measurement in one embodiment of the present invention.
Fig. 6 shows a schematic of the solidification of an oil sample in a glass cylinder after tilting to a horizontal position in a pour point measurement according to an embodiment of the present invention.
Figure 7 shows a pour point measurement apparatus in one embodiment of the utility model.
Description of the reference numerals:
1. a plug; 2. a wire; 3. an annular marking line; 4. a metal wire; 5. a glass measuring cylinder; 6. a temperature sensor; 7. oil sample; 8. a liquid level; 9. a power source; 10. a control system; 11. an oil inlet pump; 12. an oil inlet pump control signal; 13. a sample adding oil cup; 14. a flexible oil inlet pipe; 15. a heating wire; 16. a multistage semiconductor refrigerator; 17. a heat dissipation copper pipe; 18. heating wire control signals; 19. a multi-stage semiconductor refrigerator control signal; 20. measuring a resistance value control signal; 21. measuring a temperature control signal; 22. a coolant inlet; 23. a coolant outlet; 24. a stepping motor; 25. a stepper motor control signal; 26. a sewage pump; 27. a flexible blow-off pipe; 28. a blowdown pump control signal; 29. discharging an oil sample; 30. the rotation direction of the glass measuring cylinder; 31. and measuring the rotation axis of the system.
Detailed Description
Preferred embodiments of the present invention will be described in more detail below. While the following describes preferred embodiments of the present invention, it should be understood that the present invention may be embodied in various forms and should not be limited by the embodiments set forth herein.
The utility model provides a pour point and pour point measuring device, comprising:
the measuring system comprises a resistance measuring system, a temperature control system and a vertically arranged oil sample cylinder; a plug is arranged at the top of the oil sample cylinder, a sample inlet is arranged on the plug, and an annular marking line is arranged on the cylinder wall of the oil sample cylinder; the resistance measuring system comprises a resistance meter, two leads, a first comb-shaped metal wire group and a second comb-shaped metal wire group, wherein the two lead wires are positioned at two sides of the first tooth comb-shaped metal wire group and the second tooth comb-shaped metal wire group, the first tooth comb-shaped metal wire group and the second tooth comb-shaped metal wire group both comprise a plurality of metal wires which are fixed on the inner wall of the oil sample cylinder and are parallel to the bottom of the oil sample cylinder, the first tooth comb-shaped metal wire group and the second tooth comb-shaped metal wire group are arranged in a mutually crossed way, and is respectively connected with the anode and the cathode of a resistance instrument through leads, the metal wire at the top of the inner wall of the oil sample cylinder is positioned 2-5 mm below the annular marking, the distance between the adjacent metal wires is 0.02-0.10 mm, the length of the metal wire is less than half of the perimeter of the oil sample cylinder, one end of the metal wire is connected with a conducting wire on one side, and the other end of the metal wire is 3-5 mm away from the conducting wire on the other side in the direction of the cylinder wall of the oil sample cylinder; the temperature control system comprises a temperature sensor and a thermostat, the temperature sensor is arranged in the center of the oil sample cylinder, and the thermostat is arranged on the periphery of the oil sample cylinder and used for adjusting the temperature of the oil sample;
a drive system for controlling rotation of the measurement system;
and the control system is used for automatically controlling the pour point and condensation point measuring device.
In the present invention, the oil sample cylinder is preferably a glass measuring cylinder.
In the utility model, the resistance instrument is connected with the control system, and the control system judges whether the oil sample is condensed or not by monitoring the change of the resistance. In order to reduce the pitch of the measuring electrodes and increase the area of the measuring electrodes, the diameter of the wire is preferably 0.025mm to 0.100 mm. Meanwhile, in order to reduce the measurement difficulty when measuring a high-resistivity oil sample, such as insulating oil, and improve the stability and reliability of the measurement, preferably, the number of the metal wires is more than 25, and further preferably, the number of the metal wires is 25 to 111.
In the present invention, the measurement of the resistance is not limited to the use of the comb-shaped metal wire set, and other forms satisfying the present invention can also be applied to the above scheme, for example, the metal wire is replaced by a metal sheet, and two sets of the first comb-shaped metal sheet set and the second comb-shaped metal sheet set are arranged to be mutually arranged in an intersecting manner.
In the present invention, preferably, the thermostat includes a heating module and a cooling module; the heating module comprises a heating wire, and the refrigerating module comprises a multistage semiconductor refrigerator and a heat dissipation copper pipe. Wherein, utilize the heating wire to heat oil appearance in oil appearance section of thick bamboo and the bucket, utilize multistage semiconductor refrigerator to cool off oil appearance in oil appearance section of thick bamboo and the section of thick bamboo. Meanwhile, in order to take away heat generated during the working period of the multistage semiconductor refrigerator, a heat dissipation copper pipe is arranged outside the multistage semiconductor refrigerator, and a coolant is introduced into the heat dissipation copper pipe. The coolant is water or antifreeze as is conventionally used by those skilled in the art.
In the utility model, the control system controls the temperature control system to heat and cool the oil sample in the oil sample cylinder according to the regulations in GB/T510-2018 and GB/T3535-2006. Specifically, in the heating/cooling process, the temperature sensor monitors the temperature of the oil sample in real time and feeds the temperature back to the control system, and the control system adjusts the temperature of the temperature regulator according to the fed-back temperature value to heat/cool the oil sample. The temperature sensor in the pour point measuring device is conventionally arranged and immersed in an oil sample, preferably, the distance between the detection end of the temperature sensor and the bottom of the oil sample cylinder is 8-10 mm, and the distance between the annular marked line and the bottom of the oil sample cylinder is 30-60 mm.
In the present invention, preferably, the driving system includes a stepping motor. The stepping motor drives the whole measuring system to rotate by a set angle along the rotating axis of the measuring system, namely, when a condensation point is measured, the measuring system is inclined to a position forming an included angle of 45 degrees with the horizontal plane, and the measuring system returns after staying for 1 min; when measuring the pour point, the measuring system was tilted to the horizontal position and returned to the position after 5 s. In the tilting process, if the sample is not solidified, the metal wire immersed in the oil sample is exposed to the air, and the resistance value between the two wires is greatly changed compared with the resistance value in the non-tilting state; if the sample is solidified, the metal wire is always immersed in the oil sample, and the resistance value between the two wires is not obviously changed. And the period control system judges whether the sample is solidified or not by comparing whether the difference between the resistance value between the two inclined wires and the resistance value in the non-inclined state is greater than or equal to 0-1 times of the resistance value in the non-inclined state or not, and instructs the measuring system to continue measuring or not according to the judgment.
In order to realize the automatic measurement of the pour point and the freezing point, preferably, the pour point measuring device further comprises an automatic sample feeding system, an automatic blowdown system and a liquid level sensor, and the oil sample cylinder is further provided with a drain outlet; the automatic sample introduction system is connected with the sample inlet, and the automatic sewage discharge system is connected with the sewage discharge port; the liquid level sensor is arranged in the oil sample cylinder. The control system monitors whether the liquid level of the oil sample reaches the annular marking line through a signal fed back by the liquid level sensor, and then controls the starting and stopping of the automatic sample feeding system. Meanwhile, the control system receives the resistance value fed back by the resistance instrument, and judges whether the oil sample is condensed or not by calculating the difference value between the two measured resistance values, so as to control the start and stop of the automatic sewage disposal system. Preferably, the automatic sample feeding system comprises a flexible oil inlet pipe, an oil inlet pump and a sample adding oil cup, and the automatic sewage discharging system comprises a flexible sewage discharging pipe and a sewage discharging pump. According to the conventional arrangement of a person skilled in the art, the sample inlet, the oil inlet pump and the sample adding oil cup are connected through the flexible oil inlet pipe, and the drain outlet and the sewage pump are connected through the flexible sewage discharge pipe.
Example 1
A pour point and pour point measuring device, as shown in fig. 7, comprising: a measuring system, a stepping motor 24, a control system 10, an automatic sample feeding system, an automatic sewage discharging system and a liquid level sensor, wherein,
the measuring system comprises a resistance measuring system, a temperature control system and a vertically arranged glass measuring cylinder 5; the inner diameter of the glass measuring cylinder 5 is 20mm, the top of the glass measuring cylinder 5 is provided with a plug 1, the bottom of the glass measuring cylinder 5 is provided with a sewage discharge outlet, the plug is provided with a sample inlet, the cylinder wall of the glass measuring cylinder 5 is provided with an annular marking 3, and the distance between the annular marking 3 and the bottom of the oil sample cylinder is 54 mm; the resistance measuring system comprises a resistance instrument, two leads, a first tooth comb-shaped metal wire group and a second tooth comb-shaped metal wire group, wherein the two leads are positioned at two sides of the first tooth comb-shaped metal wire group and the second tooth comb-shaped metal wire group, the first tooth comb-shaped metal wire group and the second tooth comb-shaped metal wire group both comprise 55 metal wires which are fixed on the inner wall of the glass measuring cylinder 5 and are parallel to the bottom of the glass measuring cylinder 5, the first tooth comb-shaped metal wire group and the second tooth comb-shaped metal wire group are mutually crossed and arranged and are respectively connected with the anode and the cathode of the resistance instrument through leads, the metal wire 4 at the top of the inner wall of the glass measuring cylinder 5 is positioned 2mm below the annular marking 3, the diameter of the metal wire 4 is 0.025mm, the length of the metal wire is 29mm, the two leads are fixed on the inner wall of the glass measuring cylinder 5 and are positioned at two sides of the first tooth comb-shaped metal wire group and the second tooth comb-shaped metal wire group, one end of the metal wire 4 is connected with one side of the lead, the other end of the glass measuring cylinder is 3mm away from the conducting wire on the other side along the direction of the cylinder wall of the glass measuring cylinder 5, and the distance between the adjacent metal wires is 0.02 mm; the temperature control system comprises a temperature sensor 6 and a thermostat, wherein the temperature sensor 6 is arranged in the center of the glass measuring cylinder 5, the temperature measuring part of the temperature sensor 6 is 8mm away from the bottom of the oil sample cylinder 5, the thermostat is arranged on the periphery of the glass measuring cylinder 5 and comprises a heating module and a refrigerating module, the heating module comprises a heating wire 15, and the refrigerating module comprises a multistage semiconductor refrigerator 16 and a heat dissipation copper pipe 17.
The automatic sample introduction system is connected with the sample inlet, and the automatic blowdown system is connected with the blowdown port; the liquid level sensor is arranged in the glass measuring cylinder 5. The automatic sample introduction system comprises a flexible oil inlet pipe 14, an oil inlet pump 11 and a sample adding oil cup 13, wherein a sample inlet, the oil inlet pump 11 and the sample adding oil cup 13 are connected through the flexible oil inlet pipe 14. The automatic sewage system comprises a flexible sewage pipe 27 and a sewage pump 26, and the sewage outlet and the sewage pump 26 are connected through the flexible sewage pipe 27.
The pour point and condensation point measuring device is used for measuring the condensation point of the great wall I-10 transformer oil, the expected condensation point is-30 ℃, the oil sample meets the product standard, dehydration is not needed, and the specific measuring method is as follows:
1) heating the I-10 transformer oil sample to 50 ℃, then cooling to 35 ℃, and placing the sample in a sample adding oil cup 13. And starting an oil inlet pump 11, and introducing the great wall I-10 transformer oil sample into the vertically arranged glass measuring cylinder 5 through a flexible oil inlet pipe 14. When the oil sample reaches the annular marked line 3, the liquid level sensor transmits a signal to the control system 10, the oil inlet pump 11 is closed, and feeding is stopped.
2) The control system 10 starts the multi-stage semiconductor refrigerator 16 to cool the oil sample in the glass measuring cylinder 5 at a certain speed, and simultaneously, the coolant is introduced into the heat dissipation copper pipe to dissipate heat of the multi-stage semiconductor refrigerator 16. In the cooling process, the temperature sensor 6 monitors the temperature value of the oil sample in real time and feeds the temperature value back to the control system 10.
3) When the oil sample is cooled to-30 ℃, the control system starts the resistance meter and records the resistance value 8.195 multiplied by 10 at the moment12Omega, then the control system controls the stepping motor 24 to drive the glass measuring cylinder 5 to incline to the horizontal for 45 degrees along the rotating axis 31 of the measuring system to the opposite direction of the metal wire 4 and keep for 1min, the resistance value at the moment is recorded as exceeding the measuring range of the resistance instrument, Rx is larger than 1 multiplied by 1013Ω，Rn＝8.195×1012And omega, | Rx-Rn | > 0.1 XRn, judging that the oil sample is not solidified, and driving the stepping motor 24 to restore the glass measuring cylinder 5 to the vertical state by the control system 10.
4) Reheating the oil sample to 50 deg.C, cooling to-32 deg.C, and controlling the system 10 to start the resistance meter, and recording the resistance value 8.233 × 1012Ω, and then controlled by the control system 10The stepping motor 24 drives the glass measuring cylinder 5 to incline to the horizontal direction along the rotating axis 31 of the measuring system to the opposite side of the metal wire 4 to form an angle of 45 degrees and keep for 1min, the resistance value at the moment is recorded as exceeding the measuring range of the resistance meter, Rx is more than 1 multiplied by 1013Ω，Rn＝8.233×1012Omega, | Rx-Rn | > 0.1 XRn, judge that the oil sample is not solidified, and the control system 10 drives the stepping motor 24 to restore the glass measuring cylinder 5 to the vertical state.
5) Reheating the oil sample to 50 deg.C, cooling to-34 deg.C, controlling system 10 to start the resistance meter, and recording the resistance value at this time of 8.242 × 1012Omega, then the control system 10 controls the stepping motor 24 to drive the glass measuring cylinder 5 to incline to the horizontal direction along the rotating axis 31 of the measuring system to the opposite side of the metal wire 4 to form an angle of 45 degrees and keep for 1min, the resistance value at the moment is recorded as exceeding the measuring range of the resistance meter, Rx is more than 1 multiplied by 1013Ω，Rn＝8.242×1012And omega, | Rx-Rn | > 0.1Rn, judging that the oil sample is not solidified, and driving the stepping motor 24 to restore the glass measuring cylinder 5 to the vertical state by the control system 00.
6) Reheating the oil sample to 50 deg.C, cooling to-36 deg.C, and controlling the system 10 to start the resistance meter, and recording the resistance value 8.186 × 1012Omega, then the control system 10 controls the stepping motor 24 to drive the glass measuring cylinder 5 to incline to the horizontal direction along the rotating axis 31 of the measuring system to the opposite side of the metal wire 4 to form an angle of 45 degrees and keep for 1min, and the resistance value at the time is recorded as 8.197 multiplied by 1012Ω，|Rx-Rn|＝1.1×1010Ω，0.1×Rn＝8.186×1011Omega, | Rx-Rn | < 0.1 XRn, judging the solidification of the oil sample, and measuring the solidification point of the great wall I-10 transformer oil to be-36 ℃.
7) The control system 10 determines that the measurement is complete and opens the drain, starts the drain pump 26 and drains the great wall I-10 transformer oil out of the device through the flexible drain 27.
Example 2
A pour point measuring device, as shown in figure 7, comprising: a measuring system, a stepping motor 24, a control system 10, an automatic sample feeding system, an automatic sewage discharging system and a liquid level sensor, wherein,
the measuring system comprises a resistance measuring system, a temperature control system and a vertically arranged glass measuring cylinder 5; the inner diameter of the glass measuring cylinder 5 is 19mm, the top of the glass measuring cylinder 5 is provided with a plug 1, the bottom of the glass measuring cylinder 5 is provided with a sewage discharge outlet, the plug is provided with a sample inlet, the cylinder wall of the glass measuring cylinder 5 is provided with an annular marking 3, and the distance between the annular marking 3 and the bottom of the oil sample cylinder is 30 mm; the resistance measuring system comprises a resistance instrument, two leads, a first tooth comb-shaped metal wire group and a second tooth comb-shaped metal wire group, wherein the two leads are positioned at two sides of the first tooth comb-shaped metal wire group and the second tooth comb-shaped metal wire group, the first tooth comb-shaped metal wire group and the second tooth comb-shaped metal wire group respectively comprise 25 metal wires which are fixed on the inner wall of the glass measuring cylinder 5 and are parallel to the bottom of the glass measuring cylinder 5, the first tooth comb-shaped metal wire group and the second tooth comb-shaped metal wire group are mutually crossed and arranged and are respectively connected with the anode and the cathode of the resistance instrument through leads, a metal wire 4 at the top of the inner wall of the glass measuring cylinder 5 is positioned 5mm below an annular marking 3, the diameter of the metal wire 4 is 0.025mm, the length of the metal wire 4 is 27mm, the two leads are fixed on the inner wall of the glass measuring cylinder 5 and are positioned at two sides of the first tooth comb-shaped metal wire group and the second tooth comb-shaped metal wire group, one end of the metal wire 4 is connected with one side of the lead, the other end is 4mm away from the conducting wire on the other side in the direction of the cylinder wall of the glass measuring cylinder 5, and the distance between the adjacent metal wires is 0.02 mm; the temperature control system comprises a temperature sensor 6 and a thermostat, wherein the temperature sensor 6 is arranged in the center of the glass measuring cylinder 5, the temperature measuring part of the temperature sensor 6 is 9mm away from the bottom of the oil sample cylinder 5, the thermostat is arranged on the periphery of the glass measuring cylinder 5 and comprises a heating module and a refrigerating module, the heating module comprises a heating wire 15, and the refrigerating module comprises a multistage semiconductor refrigerator 16 and a heat dissipation copper pipe 17.
The automatic sample introduction system is connected with the sample inlet, and the automatic blowdown system is connected with the blowdown port; the liquid level sensor is arranged in the glass measuring cylinder 5. The automatic sample introduction system comprises a flexible oil inlet pipe 14, an oil inlet pump 11 and a sample adding oil cup 13, wherein a sample inlet, the oil inlet pump 11 and the sample adding oil cup 13 are connected through the flexible oil inlet pipe 14. The automatic sewage system comprises a flexible sewage pipe 27 and a sewage pump 26, and the sewage outlet and the sewage pump 26 are connected through the flexible sewage pipe 27.
The pour point measuring device is used for measuring the pour point of-10 # commercial diesel oil (containing additives), the expected pour point is-12 ℃, and the volume resistivity is 9.3 multiplied by 1012Omega.m, the oil sample meets the productStandard, without dehydration, the specific measurement method is as follows:
1) heating a-10 # commercial diesel oil sample to 50 ℃, then cooling to 35 ℃, and placing in the sample adding oil cup 13. Starting an oil inlet pump 11, and introducing a-10 # commercial diesel oil sample into the vertically arranged glass measuring cylinder 5 through a flexible oil inlet pipe 14. When the oil sample reaches the annular marking 3, the liquid level sensor transmits a signal to the control system 10, the oil inlet pump 11 is closed, and feeding is stopped.
2) The control system 10 starts the multistage semiconductor refrigerator 16 to cool the oil sample in the glass measuring cylinder 5 at the speed of 1.0 ℃/min, and simultaneously, the coolant is introduced into the heat dissipation copper pipe 17 to dissipate heat of the multistage semiconductor refrigerator 16. In the cooling process, the temperature sensor 6 monitors the temperature value of the oil sample in real time and feeds the temperature value back to the control system 10.
3) When the oil sample is cooled to-12 ℃, the control system 10 starts the resistance meter and records the resistance value 4.573 multiplied by 10 at the moment12Omega, then the control system 10 controls the stepping motor 24 to drive the glass measuring cylinder 5 to incline to the horizontal direction along the rotating axis 31 of the measuring system to the opposite side of the metal wire 4 to form an angle of 45 degrees and keep for 1min, and the resistance value 4.675x10 at the moment is recorded12Ω，Rx＝4.675×1012Ω，Rn＝4.573×1012Omega, | Rx-Rn | < 0.1 XRn, the oil sample is judged to be solidified, and the control system 10 drives the stepping motor 24 to restore the glass measuring cylinder 5 to the vertical state.
4) Reheating the oil sample to 50 deg.C, cooling to-10 deg.C, and controlling the system 10 to start the resistance meter, and recording the resistance value 4.682 × 1012Omega, then the control system 10 controls the stepping motor 24 to drive the glass measuring cylinder 5 to incline to the horizontal direction along the rotating axis 31 of the measuring system to the opposite side of the metal wire 4 to form an angle of 45 degrees and keep for 1min, the resistance value at the moment is recorded as exceeding the measuring range of the resistance meter, Rx is more than 1 multiplied by 1013Ω，Rn＝4.682×1012Omega, | Rx-Rn | > 0.1Rn, judging that the oil sample is not solidified, and measuring that the solidification point of the oil sample is-12 ℃.
5) The control system 10 judges that the measurement is finished, opens the sewage outlet, starts the sewage pump 26, and discharges the-10 # commodity diesel oil sample out of the device through the flexible sewage pipe 27.
Example 3
A pour point and pour point measuring device, as shown in fig. 7, comprising: a measuring system, a stepping motor 24, a control system 10, an automatic sample feeding system, an automatic sewage discharging system and a liquid level sensor, wherein,
the measuring system comprises a resistance measuring system, a temperature control system and a vertically arranged glass measuring cylinder 5; the inner diameter of the glass measuring cylinder 5 is 30mm, the top of the glass measuring cylinder 5 is provided with a plug 1, the bottom of the glass measuring cylinder 5 is provided with a sewage discharge outlet, the plug is provided with a sample inlet, the cylinder wall of the glass measuring cylinder 5 is provided with an annular marking 3, and the distance between the annular marking 3 and the bottom of the oil sample cylinder is 54 mm;
the resistance measuring system comprises a resistance instrument, two leads, a first tooth comb-shaped metal wire group and a second tooth comb-shaped metal wire group, wherein the two leads are positioned at two sides of the first tooth comb-shaped metal wire group and the second tooth comb-shaped metal wire group, the first tooth comb-shaped metal wire group comprises 24 metal wires which are fixed on the inner wall of the glass measuring cylinder 5 and are parallel to the bottom of the glass measuring cylinder 5, the second tooth comb-shaped metal wire group comprises 25 metal wires which are fixed on the inner wall of the glass measuring cylinder 5 and are parallel to the bottom of the glass measuring cylinder 5, the first tooth comb-shaped metal wire group and the second tooth comb-shaped metal wire group are mutually arranged in a cross way and are respectively connected with the anode and the cathode of the resistance instrument through leads, the metal wire 4 at the top on the inner wall of the glass measuring cylinder 5 is positioned 5mm below the annular marking 3, the diameter of the metal wire 4 is 0.02mm, the length of the metal wire is 30mm, the two leads are fixed on the inner wall of the glass measuring cylinder 5 and are positioned at two sides of the first tooth comb-shaped metal wire group and the second tooth comb-shaped metal wire group, one end of the metal wire 4 is connected with a lead on one side, the other end of the metal wire is 3mm away from the lead on the other side along the direction of the cylinder wall of the glass measuring cylinder 5, and the distance between every two adjacent metal wires is 0.025 mm; the temperature control system comprises a temperature sensor 6 and a thermostat, wherein the temperature sensor 6 is arranged in the center of the glass measuring cylinder 5, the detection end of the temperature sensor 6 is 3mm away from the liquid level of a sample to be detected in the glass measuring cylinder 5, the thermostat is arranged on the periphery of the glass measuring cylinder 5 and comprises a heating module and a refrigerating module, the heating module comprises a heating wire 15, and the refrigerating module comprises a multistage semiconductor refrigerator 16 and a heat dissipation copper pipe 17.
The automatic sample introduction system is connected with the sample inlet, and the automatic blowdown system is connected with the blowdown port; the liquid level sensor is arranged in the glass measuring cylinder 5. The automatic sample feeding system comprises a flexible oil feeding pipe 14, an oil feeding pump 11 and a sample adding oil cup 13, wherein a sample inlet, the oil feeding pump 11 and the sample adding oil cup 13 are connected through the flexible oil feeding pipe 14. The automatic sewage system comprises a flexible sewage pipe 27 and a sewage pump 26, and the sewage outlet and the sewage pump 26 are connected through the flexible sewage pipe 27.
The pour point of the great wall I-10 transformer oil is measured by using the pour point measuring device, the expected pour point is-36 ℃, and the specific measurement method is as follows:
1) heating the oil sample of the great wall I-10 transformer oil to 45 ℃, cooling to 15 ℃, and placing the sample in a sample adding oil cup 13. And starting an oil inlet pump 11, and leading the oil sample of the great wall I-10 transformer into the vertically arranged glass measuring cylinder 5 through a flexible oil inlet pipe 14. When the oil sample reaches the annular marked line 3, the liquid level sensor transmits a signal to the control system 10, the oil inlet pump 11 is closed, and feeding is stopped.
2) The control system 10 starts the multistage semiconductor refrigerator 16 to cool the oil sample in the glass measuring cylinder 5 at a certain speed, and simultaneously, the coolant is introduced into the heat dissipation copper pipe to dissipate heat of the multistage semiconductor refrigerator 16. In the cooling process, the temperature sensor 6 monitors the temperature value of the oil sample in real time and feeds the temperature value back to the control system 10.
3) When the oil sample is cooled to-18 ℃, the control system 10 starts the resistance meter and records the resistance value 8.115 multiplied by 10 at the moment12Omega, then the control system 10 controls the stepping motor 24 to drive the glass measuring cylinder 5 to incline to the horizontal position along the rotating axis 31 of the measuring system to the opposite direction of the metal wire 4 and keep the horizontal position for 5s, the resistance value at the moment is recorded to exceed the measuring range of the resistance meter, Rx is more than 1 multiplied by 1013Ω，Rn＝8.115×1012And omega, | Rx-Rn | > 0.1 XRn, judging that the oil sample is not solidified, and driving the stepping motor 24 to restore the glass measuring cylinder 5 to the vertical state by the control system 10.
4) The oil sample is continuously cooled to-21 ℃, the control system 10 starts the resistance meter, and the resistance value of the resistance at the moment is recorded as 8.182 multiplied by 1012Omega, then the control system 10 controls the stepping motor 24 to drive the glass measuring cylinder 5 to incline to the horizontal at 45 degrees along the direction of the rotating axis 31 of the measuring system to the opposite side of the metal wire 4 and keep for 1min, the resistance value at the moment is recorded as exceeding the measuring range of the resistance meter, Rx is larger than 1 multiplied by 1013Ω，Rn＝8.182×1012And omega, | Rx-Rn | > 0.1 XRn, judging that the oil sample is not solidified, and driving the stepping motor 24 to restore the glass measuring cylinder 5 to the vertical state by the control system 10.
5) The oil sample is continuously cooled to-24 ℃, the control system 10 starts the resistance meter, and the resistance value at the moment is recorded as 8.176 multiplied by 1012Omega, then the control system 10 controls the stepping motor 24 to drive the glass measuring cylinder 5 to incline to the horizontal position along the rotating axis 31 of the measuring system to the opposite direction of the metal wire 4 and keep the horizontal position for 5s, the resistance value at the moment is recorded to exceed the measuring range of the resistance meter, Rx is more than 1 multiplied by 1013Ω，Rn＝8.176×1012Omega, | Rx-Rn | > 0.1 XRn, judge that the oil sample is not solidified, and the control system 10 drives the stepping motor 24 to restore the glass measuring cylinder 5 to the vertical state.
6) The oil sample is continuously cooled to-27 ℃, the control system 10 starts the resistance meter, and the resistance value at the moment is recorded as 8.172 multiplied by 1012Omega, then the control system 10 controls the stepping motor 24 to drive the glass measuring cylinder 5 to incline to the horizontal position along the rotating axis 31 of the measuring system to the opposite direction of the metal wire 4 and keep the horizontal position for 5s, the resistance value at the moment is recorded to exceed the measuring range of the resistance meter, Rx is more than 1 multiplied by 1013Ω，Rn＝8.172×1012Omega, | Rx-Rn | > 0.1 XRn, judge that the oil sample is not solidified, and the control system 10 drives the stepping motor 24 to restore the glass measuring cylinder 5 to the vertical state.
7) The oil sample is continuously cooled to-30 ℃, the control system 10 starts the resistance meter, and the resistance value of the resistance at the moment is recorded as 8.179 multiplied by 1012Omega, then the control system 10 controls the stepping motor 24 to drive the glass measuring cylinder 5 to incline to the horizontal position along the rotating axis 31 of the measuring system to the opposite direction of the metal wire 4 and keep the horizontal position for 5s, the resistance value at the moment is recorded to exceed the measuring range of the resistance meter, Rx is more than 1 multiplied by 1013Ω，Rn＝8.172×1012Omega, | Rx-Rn | > 0.1 XRn, judge that the oil sample is not solidified, and the control system 10 drives the stepping motor 24 to restore the glass measuring cylinder 5 to the vertical state.
8) The oil sample is continuously cooled to-33 ℃, the control system 10 starts the resistance meter, and the resistance value of the resistor at the moment is recorded as 8.168 multiplied by 1012Omega, then the control system 10 controls the stepping motor 24 to drive the glass measuring cylinder 5 to move along the rotating axis 31 of the measuring system to the opposite side of the metal wire 4Inclining to the horizontal position and keeping for 5s, recording the resistance value of the resistor at the moment as exceeding the measuring range of the resistance meter, wherein Rx is more than 1 multiplied by 1013Ω，Rn＝8.168×1012And omega, | Rx-Rn | > 0.1 XRn, judging that the oil sample is not solidified, and driving the stepping motor 24 to restore the glass measuring cylinder 5 to the vertical state by the control system 10.
9) The oil sample is continuously cooled to-36 ℃, the control system 10 starts the resistance meter, and the resistance value of the resistance at the moment is recorded as 8.172 multiplied by 1012Omega, then the control system 10 controls the stepping motor 24 to drive the glass measuring cylinder 5 to incline to the horizontal position along the rotating axis 31 of the measuring system to the opposite direction of the metal wire 4 and keep the horizontal position for 5s, and the resistance value 8.187 multiplied by 10 of the resistance at the moment is recorded12Ω，|Rx-Rn|＝1.5×1010Ω，0.1×Rn＝8.172×1011Omega, | Rx-Rn | < 0.1 XRn, judging the solidification of the oil sample, and measuring the pour point of the great wall I-10 transformer oil to be-33 ℃.
10) The control system 10 determines that the measurement is complete and opens the drain, starts the drain pump 26 and drains the great wall I-10 transformer oil sample out of the device through the flexible drain 27.
Example 4
A pour point measuring device comprising: a measuring system, a stepping motor 24, a control system 10, an automatic sample feeding system, an automatic sewage discharging system and a liquid level sensor, wherein,
the measuring system comprises a resistance measuring system, a temperature control system and a vertically arranged glass measuring cylinder 5; the inner diameter of the glass measuring cylinder 5 is 32mm, the top of the glass measuring cylinder 5 is provided with a plug 1, the bottom of the glass measuring cylinder 5 is provided with a sewage discharge outlet, the plug is provided with a sample inlet, the wall of the glass measuring cylinder 5 is provided with an annular marking 3, and the distance between the annular marking 3 and the bottom of the oil sample cylinder is 54 mm; the resistance measuring system comprises a resistance instrument, two leads, a first comb-shaped metal wire group and a second comb-shaped metal wire, wherein the two leads are positioned at two sides of the first comb-shaped metal wire group and the second comb-shaped metal wire group, the first comb-shaped metal wire group comprises 55 metal wires which are fixed on the inner wall of the glass measuring cylinder 5 and are parallel to the bottom of the glass measuring cylinder 5, the second comb-shaped metal wire group comprises 56 metal wires which are fixed on the inner wall of the glass measuring cylinder 5 and are parallel to the bottom of the glass measuring cylinder 5, the first comb-shaped metal wire group and the second comb-shaped metal wire group are mutually arranged in a cross way and are respectively connected with the anode and the cathode of the resistance instrument through leads, the metal wire 4 at the top of the inner wall of the glass measuring cylinder 5 is positioned below an annular marking 3 by 5mm, the diameter of the metal wire 4 is 0.025mm, the length of the metal wire is 30mm, the two leads are fixed on the inner wall of the glass measuring cylinder 5 and are positioned at two sides of the first comb-shaped metal wire group and the second comb-shaped metal wire group, one end of each metal wire 4 is connected with a lead on one side, the other end of each metal wire is 4mm away from the lead on the other side in the direction of the cylinder wall of the glass measuring cylinder 5, and the distance between every two adjacent metal wires is 0.02 mm; the temperature control system comprises a temperature sensor 6 and a thermostat, the temperature sensor 6 is arranged in the center of the glass measuring cylinder 5, the detection end of the temperature sensor 6 is 3mm away from the liquid level of a sample to be measured in the glass measuring cylinder 5, the thermostat is arranged on the periphery of the glass measuring cylinder 5 and comprises a heating module and a refrigerating module, the heating module comprises a heating wire 15, and the refrigerating module comprises a multistage semiconductor refrigerator 16 and a heat dissipation copper pipe 17.
The automatic sample introduction system is connected with the sample inlet, and the automatic blowdown system is connected with the blowdown port; the liquid level sensor is arranged in the glass measuring cylinder 5. The automatic sample feeding system comprises a flexible oil feeding pipe 14, an oil feeding pump 11 and a sample adding oil cup 13, wherein a sample inlet, the oil feeding pump 11 and the sample adding oil cup 13 are connected through the flexible oil feeding pipe 14. The automatic sewage system comprises a flexible sewage pipe 27 and a sewage pump 26, and the sewage outlet and the sewage pump 26 are connected through the flexible sewage pipe 27.
The pour point of-10 # commercial diesel oil (containing additive) was measured using the above pour point measuring device, and the expected pour point was-9 deg.C and the volume resistivity was 9.3X 1012Ω · m, the specific measurement method is as follows:
1) heating a-10 # commercial diesel oil sample to 45 ℃, cooling to 24 ℃, and placing in the sample adding oil cup 13. Starting an oil inlet pump 11, and leading a-10 # commercial diesel oil sample into the vertically arranged glass measuring cylinder 5 through a flexible oil inlet pipe 14. When the oil sample reaches the annular marked line 3, the liquid level sensor transmits a signal to the control system 10, the oil inlet pump 11 is closed, and feeding is stopped.
2) The control system 10 starts the multi-stage semiconductor refrigerator 16 to cool the oil sample in the glass measuring cylinder 5 at a certain speed, and simultaneously, the cooling agent is introduced into the heat dissipation copper pipe 17 to dissipate heat of the multi-stage semiconductor refrigerator 16. In the cooling process, the temperature sensor 6 monitors the temperature value of the oil sample in real time and feeds the temperature value back to the control system 10.
3) When the oil sample is cooled to 0 ℃, the control system 10 starts the resistance meter and records the resistance value 4.077 multiplied by 10 at the moment12Omega, then the control system 10 controls the stepping motor 24 to drive the glass measuring cylinder 5 to incline to the horizontal position along the rotating axis 31 of the measuring system to the opposite direction of the metal wire 4 and keep the horizontal position for 5s, the resistance value at the moment is recorded to exceed the measuring range of the resistance meter, Rx is more than 1 multiplied by 1013θ，Rn＝4.077x1012Omega, | Rx-Rn | > 0.1 XRn, judge that the oil sample is not solidified, and the control system 10 drives the stepping motor 24 to restore the glass measuring cylinder 5 to the vertical state.
4) The oil sample is continuously cooled to-3 ℃, the control system 10 starts the resistance meter, and the resistance value of the resistor at the moment is recorded as 4.084 multiplied by 1012Omega, then the control system 10 controls the stepping motor 24 to drive the glass measuring cylinder 5 to incline to the horizontal direction along the rotating axis 31 of the measuring system to the opposite side of the metal wire 4 to form an angle of 45 degrees and keep for 1min, the resistance value at the moment is recorded as exceeding the measuring range of the resistance meter, Rx is more than 1 multiplied by 1013Ω，Rn＝4.084×1012Omega, | Rx-Rn | > 0.1 XRn, judge that the oil sample is not solidified, and the control system 10 drives the stepping motor 24 to restore the glass measuring cylinder 5 to the vertical state.
5) The oil sample is continuously cooled to-6 ℃, the control system 10 starts the resistance meter, and the resistance value of the resistance at the moment is recorded to be 4.043 multiplied by 1012Omega, then the control system 10 controls the stepping motor 24 to drive the glass measuring cylinder 5 to incline to the horizontal position along the rotating axis 31 of the measuring system to the opposite direction of the metal wire 4 and keep the horizontal position for 5s, the resistance value at the moment is recorded to exceed the measuring range of the resistance meter, Rx is more than 1 multiplied by 1013Ω，Rn＝4.043×1012And omega, | Rx-Rn | > 0.1 XRn, judging that the oil sample is not solidified, and driving the stepping motor 24 to restore the glass measuring cylinder 5 to the vertical state by the control system 10.
6) The oil sample is continuously cooled to-9 ℃, the control system 10 starts the resistance meter, and the resistance value of the resistance at the moment is recorded to be 4.043 multiplied by 1012Omega, then the control system 10 controls the stepping motor 24 to drive the glass measuring cylinder 5 to incline to the horizontal position along the rotating axis 31 of the measuring system towards the opposite direction of the metal wire 4 and keep the horizontal position for 5s, and the resistance value of the resistor at the moment is recorded as superRange of resistance meter, Rx > 1 × 1013Ω，Rn＝4.043×1012Omega, | Rx-Rn | > 0.1 XRn, judge that the oil sample is not solidified, and the control system 10 drives the stepping motor 24 to restore the glass measuring cylinder 5 to the vertical state.
7) The oil sample is continuously cooled to-12 ℃, the control system 10 starts the resistance meter, and the resistance value of the resistance at the moment is recorded to be 4.094 multiplied by 1012Omega, then the control system 10 controls the stepping motor 24 to drive the glass measuring cylinder 5 to incline to the horizontal position along the rotating axis 31 of the measuring system to the opposite direction of the metal wire 4 and keep the horizontal position for 5s, and the resistance value 4.080 multiplied by 10 of the resistance at the moment is recorded12Ω，|Rx-Rn|＝1.4×1010Ω，0.1×Rn＝4.094×1011Omega, | Rx-Rn | < 0.1 XRn, judging the solidification of the oil sample, and measuring the pour point of the-10 # commercial diesel oil to be-9 ℃.
8) The control system 10 determines that the measurement is finished, opens the drain, starts the drain pump 26, and discharges the-10 # commodity diesel oil sample out of the device through the flexible drain pipe 27.
Example 5
A pour point measuring device, as shown in figure 7, comprising: a measuring system, a stepping motor, a control system, an automatic sample feeding system, an automatic sewage discharging system and a liquid level sensor,
the measuring system comprises a resistance measuring system, a temperature control system and a vertically arranged glass measuring cylinder 5; the inner diameter of the glass measuring cylinder 5 is 32mm, the top of the glass measuring cylinder 5 is provided with a plug 1, the bottom of the glass measuring cylinder 5 is provided with a sewage discharge outlet, the plug is provided with a sample inlet, the cylinder wall of the glass measuring cylinder 5 is provided with an annular marking 3, and the distance between the annular marking 3 and the bottom of the oil sample cylinder is 54 mm; the resistance measuring system comprises a resistance instrument, two leads, a first comb-shaped metal wire group and a second comb-shaped metal wire, wherein the two leads are positioned at two sides of the first comb-shaped metal wire group and the second comb-shaped metal wire group, the first comb-shaped metal wire group comprises 12 metal wires which are fixed on the inner wall of the glass measuring cylinder 5 and are parallel to the bottom of the glass measuring cylinder 5, the second comb-shaped metal wire group comprises 13 metal wires which are fixed on the inner wall of the glass measuring cylinder 5 and are parallel to the bottom of the glass measuring cylinder 5, the first comb-shaped metal wire group and the second comb-shaped metal wire group are mutually arranged in a cross way and are respectively connected with the anode and the cathode of the resistance instrument through leads, the metal wire 4 at the top of the inner wall of the glass measuring cylinder 5 is positioned below an annular marking 3 by 5mm, the diameter of the metal wire 4 is 0.04mm, the length of the metal wire is 27mm, the two leads are fixed on the inner wall of the glass measuring cylinder 5 and are positioned at two sides of the first comb-shaped metal wire group and the second comb-shaped metal wire group, one end and one side wire of wire 4 are connected, the other end is 4mm apart from opposite side wire on the section of thick bamboo wall direction along glass graduated flask 5, the interval of adjacent wire is 0.04mm temperature control system and includes temperature sensor 6 and thermoregulator, temperature sensor 6 sets up in glass graduated flask 5 central authorities, the sample liquid level that awaits measuring 3mm in the distance glass graduated flask 5 of the 6 sense terminals of temperature sensor, the thermoregulator sets up in glass graduated flask 5 periphery, including heating module and refrigeration module, the module of heating includes heater strip 15, refrigeration module includes multistage semiconductor cooler 16 and heat dissipation copper pipe 17.
The automatic sample introduction system is connected with the sample inlet, and the automatic blowdown system is connected with the blowdown port; the liquid level sensor is arranged in the glass measuring cylinder 5. The automatic sample introduction system comprises a flexible oil inlet pipe 14, an oil inlet pump 11 and a sample adding oil cup 13, wherein a sample inlet, the oil inlet pump 11 and the sample adding oil cup 13 are connected through the flexible oil inlet pipe 14. The automatic sewage system comprises a flexible sewage pipe 27 and a sewage pump 26, and the sewage outlet and the sewage pump 26 are connected through the flexible sewage pipe 27.
The pour point of a commercially available Tallides 46# phosphate fire-resistant oil was measured using the above pour point measuring device, and the expected pour point was-17 ℃ and the volume resistivity was 7.4X 109Ω · m, the specific measurement method is as follows:
1) heating a-10 # commercial diesel oil sample to 45 ℃, cooling to 24 ℃, and placing in the sample adding oil cup 13. Starting an oil inlet pump 11, and introducing a-10 # commercial diesel oil sample into the vertically arranged glass measuring cylinder 5 through a flexible oil inlet pipe 14. When the oil sample reaches the annular marked line 3, the liquid level sensor transmits a signal to the control system 10, the oil inlet pump 11 is closed, and feeding is stopped.
2) The control system 10 starts the multistage semiconductor refrigerator 16 to cool the oil sample in the glass measuring cylinder 5 at a certain speed, and simultaneously, the coolant is introduced into the heat dissipation copper pipe 17 to dissipate heat of the multistage semiconductor refrigerator 16. In the cooling process, the temperature sensor 6 monitors the temperature value of the oil sample in real time and feeds the temperature value back to the control system 10.
3) When the oil sample is cooled to-8 ℃, the control system 10 starts the resistance meter and records the resistance value 3.588 multiplied by 10 at the moment7Omega, then the control system 10 controls the stepping motor 24 to drive the glass measuring cylinder 5 to incline to the horizontal position along the rotating axis 31 of the measuring system to the opposite direction of the metal wire 4 and keep the horizontal position for 5s, the resistance value at the moment is recorded to exceed the measuring range of the resistance meter, Rx is more than 1 multiplied by 1013Ω，Rn＝4.077×1012Omega, | Rx-Rn | > 0.1 XRn, judge that the oil sample is not solidified, and the control system 10 drives the stepping motor 24 to restore the glass measuring cylinder 5 to the vertical state.
4) The oil sample is continuously cooled to-11 ℃, the control system 10 starts the resistance meter, and the resistance value of the resistance at the moment is recorded as 3.556 multiplied by 107Omega, then the control system 10 controls the stepping motor 24 to drive the glass measuring cylinder 5 to incline to the horizontal direction along the rotating axis 31 of the measuring system to the opposite side of the metal wire 4 to form an angle of 45 degrees and keep for 1min, the resistance value at the moment is recorded as exceeding the measuring range of the resistance meter, Rx is more than 1 multiplied by 1013Ω，Rn＝4.084×1012Omega, | Rx-Rn | > 0.1 XRn, judge that the oil sample is not solidified, and the control system 10 drives the stepping motor 24 to restore the glass measuring cylinder 5 to the vertical state.
5) The oil sample is further cooled to-14 ℃, the control system 10 starts the resistance meter, and the resistance value of the resistance at the moment is recorded as 3.544 multiplied by 107Omega, then the control system 10 controls the stepping motor 24 to drive the glass measuring cylinder 5 to incline to the horizontal position along the rotating axis 31 of the measuring system to the opposite direction of the metal wire 4 and keep the horizontal position for 5s, the resistance value at the moment is recorded to exceed the measuring range of the resistance meter, Rx is more than 1 multiplied by 1013Ω，Rn＝4.043×1012And omega, | Rx-Rn | > 0.1 XRn, judging that the oil sample is not solidified, and driving the stepping motor 24 to restore the glass measuring cylinder 5 to the vertical state by the control system 10.
6) The oil sample is continuously cooled to-17 ℃, the control system 10 starts the resistance meter, and the resistance value of the resistance at the moment is recorded to be 3.540 multiplied by 107Omega, then the control system 10 controls the stepping motor 24 to drive the glass measuring cylinder 5 to incline to the horizontal position along the rotating axis 31 of the measuring system to the opposite direction of the metal wire 4 and keep the horizontal position for 5s, the resistance value at the moment is recorded to exceed the measuring range of the resistance meter, Rx is more than 1 multiplied by 1013Ω，Rn＝4.043×1012And omega, | Rx-Rn | > 0.1 XRn, judging that the oil sample is not solidified, and driving the stepping motor 24 to restore the glass measuring cylinder 5 to the vertical state by the control system 10.
7) The oil sample is continuously cooled to-20 ℃, the control system 10 starts the resistance meter, and the resistance value of the resistance at the moment is recorded as 3.537 multiplied by 107Omega, then the control system 10 controls the stepping motor 24 to drive the glass measuring cylinder 5 to incline to the horizontal position along the rotating axis 31 of the measuring system to the opposite direction of the metal wire 4 and keep the horizontal position for 5s, the resistance value at the moment is recorded to exceed the measuring range of the resistance meter, Rx is more than 1 multiplied by 1013Ω，Rn＝4.043×1012And omega, | Rx-Rn | > 0.1 XRn, judging that the oil sample is not solidified, and driving the stepping motor 24 to restore the glass measuring cylinder 5 to the vertical state by the control system 10.
8) The oil sample is continuously cooled to-23 ℃, the control system 10 starts the resistance meter, and the resistance value of the resistance at the moment is recorded as 3.590 multiplied by 107Omega, then the control system 10 controls the stepping motor 24 to drive the glass measuring cylinder 5 to incline to the horizontal position along the rotating axis 31 of the measuring system towards the opposite direction of the metal wire 4 and keep the horizontal position for 5s, and the resistance value 3.571 multiplied by 10 of the resistance at the moment is recorded7Ω，|Rx-Rn|＝1.9×105ΩΩ，0.1×Rn＝3.590×106Omega, | Rx-Rn | < 0.1 XRn, oil sample solidification is judged, and the pour point of the commercial tylidede 46# phosphate fire-resistant oil is measured to be-20 ℃.
8) The control system 10 determines that the measurement is complete and opens the drain and activates the drain pump 26 to discharge the commercially available tylidede 46# phosphate anti-fuel sample out of the device through the flexible drain 27.
Comparative example 1
The condensation point of the great wall I-10 transformer oil in the example 1 is measured by using the condensation point measuring method described in GB/T510-2018, and the condensation point of the great wall I-10 transformer oil is measured to be-36 ℃.
Comparative example 2
The condensation point of the-10 # commercial diesel oil (containing the additive) in the example 2 is measured by using the condensation point measuring method described in GB/T510-2018, and the condensation point of the-10 # commercial diesel oil (containing the additive) is measured to be-12 ℃.
Comparative example 3
The pour point of the great wall I-10 transformer oil in example 3 was determined by the pour point measurement method described in GB/T3535-2006, and the pour point of the great wall I-10 transformer oil was determined to be-33 ℃.
Comparative example 4
The pour point of the-10 # commercial diesel oil (containing the additive) in example 4 was measured by the pour point measuring method described in GB/T3535-.
Comparative example 5
The pour point of the tulide 46# phosphate fire-resistant oil in the example 5 is measured by the pour point measuring method described in GB/T3535-2006, and the pour point of the tulide 46# phosphate fire-resistant oil is measured to be-21 ℃.
As is clear from examples 1 to 5 and test examples 1 to 5, the pour points measured by the pour point measuring method in GB/T3535-2006 were consistent with the pour points measured by the measuring apparatus of the present invention. The method for measuring the condensation point in GB/T510-2018 is consistent with the condensation point measured by the measuring device of the utility model. Therefore, the pour point and the condensation point measuring device provided by the utility model can measure the volume resistivity of less than 1.0 multiplied by 1015The condensation point of a colorless and transparent oil sample of Ω · m, such as transformer oil, can also be measured as a colored oil sample, including diesel oil, turbine oil and antifuel oil containing additives having an equivalent volume resistivity of less than 1.0 × 1015Omega · m condensation point of the liquid oil sample.
While embodiments of the present invention have been described above, the above description is illustrative, not exhaustive, and not limited to the disclosed embodiments. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments.
Claims (10)
1. A pour point measuring device, comprising:
the measuring system comprises a resistance measuring system, a temperature control system and a vertically arranged oil sample cylinder; a plug is arranged at the top of the oil sample cylinder, a sample inlet is formed in the plug, and an annular marking line is arranged on the cylinder wall of the oil sample cylinder; the resistance measuring system comprises a resistance meter, two leads, a first comb-shaped metal wire group and a second comb-shaped metal wire group, wherein the two lead wires are positioned at two sides of the first tooth comb-shaped metal wire group and the second tooth comb-shaped metal wire group, the first tooth comb-shaped metal wire group and the second tooth comb-shaped metal wire group both comprise a plurality of metal wires which are fixed on the inner wall of the oil sample cylinder and are parallel to the bottom of the oil sample cylinder, the first tooth comb-shaped metal wire group and the second tooth comb-shaped metal wire group are arranged in a mutually crossed way, and is respectively connected with the anode and the cathode of a resistance meter through leads, the metal wire at the top of the inner wall of the oil sample cylinder is positioned 2-5 mm below the annular marking, the distance between the adjacent metal wires is 0.02-0.10 mm, the number of the metal wires is more than 25, one end of each metal wire is connected with a lead on one side, and the other end of each metal wire is 3-5 mm away from a lead on the other side in the direction of the cylinder wall of the oil sample cylinder; the temperature control system comprises a temperature sensor and a temperature regulator, the temperature sensor is arranged in the center of the oil sample cylinder, and the temperature regulator is arranged on the periphery of the oil sample cylinder and used for regulating the temperature of the oil sample;
a drive system for controlling rotation of the measurement system;
and the control system is used for automatically controlling the pour point and condensation point measuring device.
2. The pour point measuring device of claim 1, wherein the wire diameter is between 0.025mm and 0.100 mm; the length of the metal wire is less than half of the perimeter of the oil sample cylinder.
3. The pour point measuring device of claim 2, wherein the number of wires is 25 to 111.
4. The pour point measurement device of claim 1, wherein the thermostat comprises a heating module and a cooling module; the heating module comprises heating wires, and the refrigerating module comprises a multistage semiconductor refrigerator and a heat dissipation copper pipe.
5. The pour point measuring device of claim 1, wherein the oil sample cylinder is a glass cylinder; the drive system includes a stepper motor.
6. The pour point measuring device of claim 1, wherein the sensing end of the temperature sensor is 8-10 mm from the bottom of the oil sample cylinder, and the annular gauge line is 30-60 mm from the bottom of the oil sample cylinder.
7. The pour point and pour point measuring device according to any one of claims 1 to 6, further comprising an automatic sample feeding system, an automatic blowdown system and a liquid level sensor, wherein the oil sample cylinder is further provided with a drain outlet;
the automatic sample introduction system is connected with the sample inlet, and the automatic blowdown system is connected with the blowdown port; the liquid level sensor is arranged in the oil sample cylinder.
8. The pour point measuring device of claim 7, wherein said automated sample injection system comprises a flexible oil feed tube, an oil feed pump, and a sample addition oil cup; the automatic sewage draining system comprises a flexible sewage draining pipe and a sewage draining pump.
9. The pour point measuring device of claim 8, wherein the sample inlet, the oil feed pump, and the sample addition oil cup are connected by the flexible oil feed tube.
10. The pour point measuring device of claim 8, wherein said drain and drain pump are connected by said flexible drain.
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| CN202220816034.8U CN217033723U (en) | 2022-04-08 | 2022-04-08 | Pour point and condensation point measuring device |
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