JPH0326940A - Method and instrument for measuring kinematic viscosity of liquid - Google Patents

Abstract

PURPOSE:To enable a sample to be surely discharged even at a room temperature by measuring a time for which the sample passes a measuring sphere, accommodating the sample in a viscosimeter in a large volume chamber, mixing a washing solvent and the sample in the chamber and discharging a resultant mixture via a discharge tube. CONSTITUTION:After a time required for passing measuring spheres 7 and 8 is measured, the inside of a viscosimeter 1 is washed. That is, after passing the measuring sphere 8 by sucking a sample by a vacuum pump 37, the sample is accommodated in a first blend sphere 9 to stay therein. The sample which has been accumulated in an excess sample sink 4 is accommodated in a second blend sphere 10 to stay therein. Then a washing solvent is fed into the viscosimeter 1. While dissolving the sample attached to the inside of the viscosimeter 1, the solvent reaches the blend spheres 9 and 10 and is mixed with the sample in the blend spheres 9 and 10. A resultant mixture is discharged from discharge tubes 11 and 12. Thus, the sample keeps a fluidity even at a room temperature and can be surely discharged.

Description

[Detailed Description of the Invention] [Field of Industrial Application] Thurs.: PIJ1 relates to a method and device for measuring the viscosity of liquids using a run-tweet fax viscometer, and particularly to cleaning and sample discharging steps after measurement. This article relates to an improved method and device for measuring the viscosity of liquids. [Prior art] As a method for measuring the kinematic viscosity of petroleum and petroleum products, JIS
Various methods have been standardized in K 2283, but among them, the method using a Lantzzeit 7x viscometer is widely used because it has the advantage of being able to measure the viscosity of not only transparent liquids but also opaque liquids. There is. Conventionally, a liquid kinematic viscosity measuring device using a Lanz-Zeitfuchs viscometer has been disclosed in Japanese Utility Model Publication No. 1983-35022 filed by the applicant of the present application. This measuring device realizes automatic measurement by installing a photoelectric converter in the measuring section of a Lant-Zeitfuchs viscometer, and connects a suction pump to the sample extraction port to automatically remove the sample inside the viscometer. It was now possible to discharge the liquid. [Problems to be solved] In the conventional liquid kinematic viscosity measuring device described above, in the sample discharge process after the measurement, the sample temperature drops to near room temperature in the discharge pipe led outside of the thermostatic chamber. In the case of samples with low fluidity at room temperature, such as heavy oil with a high wax content, there was a risk that the fluidity would be lost in the discharge pipe and the discharge pipe would be blocked. The present invention has been made to solve these problems, and its purpose is to provide a method and device for measuring the kinematic viscosity of a liquid, which can maintain the fluidity of a sample even at room temperature and reliably discharge the sample. ．． [Means for Solving the Problems] In order to achieve the above object, the method for measuring liquid kinematic viscosity of the present invention includes sending a sample from a sample reservoir to a measuring sphere, and then measuring the time it takes for the sample to pass through the measuring sphere. Then, before the sample inside the viscometer reaches the discharge pipe, the sample is stored in a large volume chamber, and a cleaning solvent is placed in the room and mixed with the sample, and this mixture is discharged through the discharge pipe. It is as follows. Further, the liquid kinematic viscosity measuring device of the present invention is a device for measuring the kinematic viscosity of a liquid sample based on the time it takes for the sample sent from the sample reservoir to pass through the measuring bulb, and in which there is a gap between the measuring bulb and the discharge pipe. , each has a blending sphere with a volume larger than the volume of the discharged sample. [Example] Hereinafter, an example of this JAIjll will be explained based on the drawings. FIG. 1 is a front cross-sectional view showing a first embodiment of the invention of a liquid kinematic viscosity measuring device, and FIG. MS2 is a front cross-sectional view showing an enlarged view of the viscometer of the same device. This example shows a manual kinematic viscosity measuring device. ...are multiple viscometers with different kinematic viscosity measurement ranges. These viscometers 1 are made of glass, and as shown enlarged in FIG.
Sample reservoir 3, excess sample reservoir 4, inverted U-shaped tube 5, capillary tube 6, measuring bulbs 7, 8, first and second blending bulbs 9, 10, discharge tube 1
1.12. Inlet 2 has a wide mouth,
Liquid samples and cleaning solutions are injected from here. The test T4 reservoir 3 is formed below the injection port 2, and has an overflow part 3a at a certain height.
It communicates with surplus reservoir 4 via a. The inverted U-shaped tube 5 has one end connected to the bottom of the sample reservoir 3, and is provided to cause the sample to flow down into the capillary tube 6 using the siphon principle. The measuring spheres 7 and 8 are connected to the capillary tube 6 and are connected to the upper part of the capillary tube 6. Time markers a, b, and c are placed at the center and bottom, and the kinematic viscosity of the sample is determined by the time taken for the sample flowing through the capillary tube 6 to pass through each of the time markers. The first blending sphere 9 is formed between the connection l3 of the discharge pipe 11 and the measuring sphere 8, and the second blending sphere 1O is formed between the connection l4 of the discharge pipe 12 and the after-effect sample reservoir 4. It has been done. These blending spheres 9,10 form a large volume chamber for mixing the sample and cleaning solvent. That is, the first blending bulb 9 has a larger volume than the volume of the sample that passes through the measuring bulb 8 and is discharged via the discharge pipe 11, and the second blending bulb 1O accumulates in the excess sample reservoir 4. 41 is a volume larger than the sample volume. Here, each blend sphere 9.10
In order for the sample to remain in the chamber and mix with the cleaning solvent, the size of each blending bulb 9, 10 should be 1.5 to 5 times, preferably 2 to 3 times, the volume of the discharged sample. Conversely, if each blending bulb 9,to has a volume smaller than 1.5 times the volume of the discharged sample, the sample will not remain in the blending bulb 9,10 and will pass through as it is, resulting in insufficient mixing with the cleaning solvent. turn into. Incidentally, the volume of the sample discharged through the discharge pipe 1l remains constant because the surplus sample overflows from the overflow part 3a into the surplus sample reservoir 4 during sample injection. Further, the volume of the sample stored in the surplus sample reservoir 4 can be kept approximately constant by collecting a predetermined amount into a beaker or the like in advance, or by injecting the sample while observing the surplus sample reservoir 4. The above-mentioned viscometer 1 has a constant temperature bath 20 as shown in FIG.
There are various arrangements inside. Further, 30 is a vacuum controller, in which a discharge pipe 11.12 extending from the main body 31 connects to the blending ball 9.10, and a solenoid valve 32 inside the main body 31 for opening and closing these discharge pipes 11.12. , 33.34. 35 is a waste liquid tank, which is connected to the vacuum controller 30 through piping 36 and also to the vacuum pump 37 through piping 38. 40 is a solenoid valve for opening the waste liquid tank 35 to the atmosphere. Next, an example of a liquid kinematic viscosity measuring method using the above-mentioned kinematic viscosity measuring device will be explained. ■ First, use an appropriate viscometer 1 based on the expected viscosity of the sample.
, and connect the discharge pipes 11 and 12 to the connections l3 and 14. The temperature inside the constant temperature bath 20 is constant (for example, 120f).
0.03℃). ■ Collect an almost constant amount (for example, about -30mffi) of the sample into a beaker and insert it into the injection port 2.
Inject more. A certain amount of the injected sample accumulates in the sample reservoir 3, and a small amount overflows and accumulates in the surplus sample reservoir 4. In this state, keep the sample at a constant temperature for a certain period of time (for example, 20 minutes). ■ Activate the vacuum pump 37 and at the same time operate the solenoid valve 3.
3,34. 40 and open the solenoid valve 32. As a result, the sample in the sample reservoir 3 is absorbed, and the inverted U-shaped tube 5
and flows down inside the capillary tube 6. When the tip of the sample is at approximately the same height as the upper measuring sphere 8, the vacuum pump 37
At the same time, the solenoid valves 33, 34, and 40 are opened and the solenoid valve 32 is closed. The sample is then exposed to the atmosphere, and then gradually flows to the measuring spheres 7 and 8 using the siphon principle. Observing this flow, the tip of the sample is aligned with the time markers a and b.
, measure the time it takes to pass through c. The measured time is a value proportional to the viscosity of the sample, and by multiplying this value by a specific coefficient, the kinematic viscosity of the sample can be determined. ■ After measuring the kinematic viscosity of the sample using the above steps, clean the inside of the viscometer, drain the sample, and dry it. (a) That is, the vacuum pump 37 is operated and the solenoid valves 33, 34 . 40 and open the solenoid valve 32 to aspirate the sample inside the viscometer. The sample that has passed through the measurement sphere 8 and the sample that has accumulated in the surplus sample reservoir 4 is
After a while, it is accommodated in each blend sphere 9 and 10 and remains inside. (a) When the sample from the sample reservoir 3 to the first blending bulb 9 or from the excess sample reservoir 4 to the second blending bulb 10 is accommodated in each blending bulb 9, 10, the viscometer The sound of air passing through is generated. When you hear this sound of air passing, inject a cleaning solvent (xylene, toluene, or a mixture of these with acetone in equal amounts, a chlorinated organic solvent, etc.) from the injection port 2. The cleaning solvent reaches each blend sphere 9.10 while dissolving the sample adhering to the inside of the viscometer. Meanwhile, the sample in the blending bulbs 9 and 10 continues to stagnate, and the mixture of cleaning solvent and sample that has flowed in flows out of each blending bulb 9 and 10, passes through the discharge pipes 11 and 12, and enters the waste liquid tank 35. It will be collected. (c) After that, the vacuum pump 37 continues to suction the inside of the viscometer for a while, and the inside is dried by the air flowing in from the injection port 2 and the heat of the constant temperature bath 20. When the drying is completed, the vacuum bomb 37
Stop. As described above, place the sample in the viscometer into each blend sphere 9. lO
The sample, which loses its fluidity at room temperature, is removed from the discharge pipe 1 outside the thermostatic chamber 20 by collecting the sample and mixing it with a cleaning solvent.
1.12 It is possible to prevent it from clumping inside and to perform sufficient cleaning. Additionally, the time required for the cleaning process can be shortened, and the sample inside the viscometer can be sufficiently removed with approximately three minutes of cleaning. Furthermore, since the series of operations from sample collection to measurement, washing, and drying can be performed with the viscometer 1 attached to the thermostatic bath 20, these series of operations can be facilitated. Next, a second embodiment of the invention of a liquid kinematic viscosity measuring device will be described based on the drawings. Figure 3 is a front cross-sectional view showing a second embodiment in which the kinematic viscosity of the vessel can be measured automatically. Note that the same parts as in FIG. 1 shown above are given the same reference numerals, and detailed explanations of those parts will be omitted. In the apparatus of this embodiment, photoelectric converters 51, 52, 53 are provided at the bottom and top of each measuring bulb 7, 8 for detecting the liquid level of the sample passing through the measuring bulb 7.8.
A time display unit 54 is connected to these photoelectric converters so that the time of passage of the sample can be measured. Further, an injection pipe 56 from a cleaning liquid container 55 is inserted into the injection port 2, and the cleaning liquid can be injected through an injection pump 57 provided in the middle of the injection pipe. The operation for measuring the kinematic viscosity of a liquid sample is performed by the sequence control unit 5.
This was carried out in accordance with the instructions of No. 8. Ru. The sequence control unit 58 includes electromagnetic valves 59, 60, 61 and a pump 57 necessary for measuring the viscosity of the vessel and cleaning and drying the viscometer.
．． 62 operating programs are input. According to the automatic dynamic viscosity measurement device described above, a series of steps in the dynamic viscosity measurement method, from the start of measurement to measurement, washing, sample discharge, and drying, can be automatically performed as follows. In other words, after the sample is injected and the sample in the sample reservoir 3 reaches a constant temperature, the solenoid valves 59, 60, 61 and the vacuum pump 62 are controlled by commands from the sequence control unit 58 to inject the sample into the capillary tube 6. suction to the specified position. ■ Then, the inside of the viscometer 1 is opened to atmospheric pressure and the sample is made to flow gradually using the siphon principle, and the liquid level of the sample passing through the measuring ball 7.8 is detected by photoelectric converters 51, 52, Based on the detection signal, the time required for the sample to pass through the measuring spheres 7 and 8 is displayed on the time display section 54. The kinematic viscosity of the sample can be calculated by multiplying the displayed time by the viscometer constant calibrated in advance. ■ After completing the above operations, clean the inside of viscometer 1. (B) First, close the IT magnetic valve 61 and 't'
Open the ttm valves 59 and 60 and aspirate the sample with the vacuum pump 62. After passing through the measuring sphere 8, the sample is accommodated in the first blending sphere 9 and remains therein. On the other hand, the sample accumulated in the surplus sample reservoir 4 is accommodated in the second blending sphere IO and remains therein. (o) Next, operate the injection bomb 57 to remove the cleaning solvent (
xylene, toluene, or a mixture of these with acetone in equal amounts, a chlorinated mechanical solvent, etc.) is fed into the viscometer 1. The cleaning solvent reaches each blending bulb 9, 10 while dissolving the sample adhering to the inside of the viscometer, and mixes vigorously with the sample within each blending bulb 9, 10. This mixture of sample and cleaning solvent then exits each blending bulb 9.10 and is collected through a discharge pipe 11.12 into a waste tank (not shown in Figure 3). When the sample is discharged and washed in this manner, the injection pump 57 is stopped. (c) Leave the vacuum pump 62 in operation and suck air into the viscometer 1 from injection day 2. Then,
The inside of the viscometer 1 is dried by this flowing air and the heat inside the constant temperature bath 20. When drying is completed, vacuum pump 6
2 and the solenoid valves 59 and 60 are stopped, and the series of viscosity measurement operations is completed. [Effects of the Invention] As explained above, according to the method for measuring liquid kinematic viscosity of the present invention, the sample and cleaning solvent are mixed and discharged in a large-volume room, so fluidity is maintained even at room temperature. This has the effect of ensuring reliable discharge and rapid cleaning. Further, according to the liquid viscosity measuring device of the present invention, the above-mentioned measuring method can be carried out efficiently, and the sample can be reliably discharged and the cleaning time can be shortened.

[Brief explanation of drawings]

Fig. 1 is a front cross-sectional view showing a first embodiment of the invention of a liquid kinematic viscosity measuring device, Fig. 2 is a front cross-sectional view showing an enlarged viscometer of the same device, and Fig. 3 is a front cross-sectional view showing a viscometer of the device according to the invention. FIG. 7 is a front view showing a second embodiment. 1: Viscometer 2: Inlet 3: Sample reservoir 4: Surplus sample reservoir 5: Inverted U-shaped tube 6: Capillary tube 7.8: Measuring bulb 9: First blending bulb 10: Second blending bulb 11.12 + discharge Pipe 20: Constant temperature bath 30: Vacuum controller 35: Waste liquid tank 37: Vacuum pump 51.52,
53: Photoelectric converter 54: Time display section 58: Sequence control section

Claims (2)

[Claims] (1) Send the sample from the sample reservoir to the measurement bulb, then measure the time it takes for the sample to pass through the measurement bulb, and then transfer the sample inside the viscometer to a large-volume chamber before it reaches the discharge pipe. 1. A method for measuring the kinematic viscosity of a liquid, the method comprising: storing a cleaning solvent in the chamber, mixing it with a sample, and discharging this mixture through a discharge pipe. (2) In a device that measures the kinematic viscosity of a liquid sample based on the time it takes for the sample sent from the sample reservoir to pass through a measuring sphere,
A kinematic viscosity measuring device for a liquid, characterized in that blending bulbs each having a volume larger than the capacity of the discharged sample are provided between the measurement bulb and the discharge pipe.