JP4542682B2 - Sample preparation device for measuring particles in oil - Google Patents

Description

[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a sample adjustment device for measuring particles in oil, which adjusts a measurement sample for measuring the amount of particles and the size of particles contained in oil such as fuel oil.
[0002]
[Prior art]
Conventionally, fuel oils such as heavy oil and lubricating oils contain fine particles such as catalysts used in the manufacturing process. Since there is a risk of causing damage, etc., the oil is cleaned by separating and removing with water etc. with a centrifuge etc., but if the amount of particles in the oil and the size of the particles are unknown, Since the operation conditions such as the rotation speed of the centrifuge and the sludge discharge time interval cannot be set to conditions suitable for the separation of the contained particles, the separation of the fine particles becomes insufficient and the internal combustion engine There was a risk of causing trouble.
[0003]
Conventionally, as a device for measuring particles in a liquid, a photodetector that irradiates laser light to a microcell through which a sample liquid (hereinafter also simply referred to as a sample) circulates and provides a shadow blocked by the particles on the opposite side. Laser light blocking measuring instruments that detect and measure the amount of particles and the size of particles in a sample are used, but this measuring instrument uses liquids with good light transmission and low viscosity. Can be measured directly with the sample solution as it is, but it is difficult to measure directly with a sample with high viscosity like heavy oil and low light transmittance. The solution is diluted with a solvent, supplied to a microcell and measured, and the solvent of the microcell is manually cleaned. Furthermore, oil diluted with a solvent or the like is filtered with a filter paper, and the particles captured on the filter paper are washed with a solvent such as xylene, then dried with a dryer, and observed with a magnifying glass or the like, and compared with a reference photograph. There is also a method of qualitatively determining whether it can be used.
[0004]
[Problems to be solved by the invention]
In the conventional apparatus and method for measuring particles in a liquid, since the sample is diluted and washed with a solvent by hand, there is a problem that the work environment is deteriorated because it takes time and uses a solvent. . In addition, there is a problem that unevenness in cleaning is likely to cause measurement errors.
[0005]
The present invention has been made in view of the above-mentioned problems, and fully automates the adjustment operation of the sample for measuring particles in oil after sampling the sample liquid, and performs operations such as dilution and washing with a solvent without manual operation. By providing a sample preparation device for measuring particles in oil that can cause no deterioration of the working environment, the amount and size of particles in the sample can be measured safely and quickly, and Since measurement errors can be reduced, fine particles can be reliably obtained by setting the operating conditions suitable for the separation of particles contained in oil, such as the number of revolutions of the centrifuge and the sludge discharge time interval. It was made for the purpose of eliminating the risk of causing damage to the internal combustion engine.
[0007]
[Means for Solving the Problems]
The gist of the present invention for achieving the above object is that, in the invention according to claim 1 , a sample pot provided with a temperature control means for storing a fixed amount of the collected sample liquid and adjusting the temperature, and a dilution A dilution tank provided with temperature control means for storing liquid, and a dilution mixing tank provided with temperature control means for mixing the sample liquid from the sample pot and the dilution liquid from the dilution tank to obtain a diluted sample liquid; A dilution supply pump for supplying the dilution liquid from the dilution liquid tank to the sample pot and the dilution mixing tank, and a filter for capturing particles in the diluted sample liquid provided in the diluted sample liquid extraction flow path of the dilution mixing tank; A sample preparation apparatus for measuring particles in oil, comprising pressurized gas supply means for supplying pressurized gas to a sample pot, a dilution / mixing tank, and a filter. With the above configuration, the sample adjustment operation for particle measurement after collection of the sample liquid is fully automated, the amount of particles in the oil can be measured quickly, and measurement errors due to cleaning unevenness and external particle contamination are caused. Therefore, an accurate measurement result can be obtained, and therefore it can be reflected in the operation under an appropriate condition such as a centrifuge, and there is no possibility of causing a failure in the internal combustion engine or the like.
[0010]
Note that filter paper or filter cloth can be used as the filter material of the filter, but it is preferable to use filter paper because of its ability to capture particles and ease of measurement, and the particles captured by the filter material of the filter. As a method of measuring the amount of particles and the size of the particles, a method of observing with a magnifier or the like and comparing with a reference photograph to judge qualitative use may be used. Measures using a device that magnifies the image with a digital camera, captures it as electronic information data with a digital camera, processes it as a computer image, and measures it as a numerical value. This is preferable because it is possible. However, the measuring device used in the present invention is not limited to this device.
[0011]
DETAILED DESCRIPTION OF THE INVENTION
Embodiments of the present invention will be described with reference to the drawings. FIG. 1 is a system diagram of a sample preparation device for measuring particles in oil according to an embodiment of the present invention.
[0012]
Reference numeral 1 is a sample pot for storing a certain amount of collected sample liquid, which is sealed with a lid member having a sample inlet (not shown) whose upper surface can be opened, and a sample discharge supply pipe b is connected to the bottom. In order to adjust the temperature of the sample solution, it is provided in the heater 16 of the temperature control means, and the heater 16 is controlled to a predetermined temperature based on the temperature measured by the thermometer 19. In addition, in order to discharge the sample liquid under the pressure of pressurized gas such as nitrogen or air, a pressurized gas supply pipe a1 is connected, and further, the interior is washed with a diluting liquid. The provided diluent injection pipe h2 is connected. The sample pot 1 preferably has a connection structure such as a joint with a stopper that can be easily detached from a connection pipe such as the sample discharge supply pipe b for sampling, if necessary. As can be seen, it is also preferable to imprint a scale indicating the capacity on the side wall of the sample pot 1.
[0013]
Reference numeral 2 is a dilution mixing tank for mixing the sample liquid supplied from the sample discharge supply pipe b connected to the sample pot 1 and the dilution liquid supplied from the dilution liquid supply pipe h1 connected to the dilution liquid tank 3, The upper surface is sealed with an openable lid member, and the diluted sample discharge pipe c, which is a diluted sample solution extraction channel, is connected to the bottom, and is provided in the heater 17 of the temperature control means for adjusting the temperature of the diluted sample. The heater 17 is controlled to a predetermined temperature based on the temperature measured by the thermometer 20. Further, a pressurized gas supply pipe a2 is connected to discharge the diluted sample at a pressure of a pressurized gas such as nitrogen or air.
[0014]
The diluted sample discharge pipe c includes a circulation channel pipe f which is a circulation path of the diluted sample liquid and a diluted sample liquid withdrawing provided with a circulation pump 8 which circulates the diluted sample liquid in the diluted mixing tank 2 through the three-way valve 11. A particle capturing channel main pipe d as a channel is branched and connected. Further, the particle trapping channel tube d is branched by a pressurized gas supply tube e branched from the pressurized gas supply main tube j via the three-way valve 14 and a particle trapping channel tube d1 as a diluted sample liquid extraction channel. Connected. Further, the particle trapping channel tube d1 is provided with a filter 5 for trapping particles in the diluted sample solution with a filter medium such as filter paper or filter cloth. The filter 5 has a sample solution as a channel for extracting the diluted sample solution. A discharge pipe d2 is connected.
[0015]
Further, the pressurized gas supply pipes a1 and a2 are connected to the pressurized gas supply main pipe a through the three-way valve 10, and the pressurized gas supply main pipe a is connected to the pressurized gas supply means 6 such as a gas cylinder. The pressurized gas supply main pipe j is branched and provided with a pressurized gas supply pipe e for supplying the pressurized gas to the filter 5 via the three-way valve 15 and drying the filter medium. Note that the pressurized gas supply means 6 for supplying the pressurized gas to the pressurized gas supply pipes a1, a2 and e may be provided separately for each pipe. In this case, the three-way valves 10 and 15 are unnecessary, but there is a problem that the entire equipment becomes excessive. The pressurized gas supply pipe e and the three-way valves 14 and 15 to be supplied to the filter 5 need not be provided, but are preferably provided in order to quickly and surely dry the filter medium.
[0016]
The dilution mixing tank 2 is provided with stirring means 9 such as a stirring blade type stirrer, a paddle type stirrer, or a rotor type stirrer using magnetic force.
[0017]
Reference numeral 3 is a diluent tank for storing a diluent of a solvent such as benzene or xylene, the upper surface of which is sealed with a cover member that can be opened, and a diluent supply pipe g is connected to the bottom to control the temperature of the diluent. In order to adjust, it is provided in the heater 18 of the temperature control means, and the heater 18 is controlled to a predetermined temperature based on the temperature measured by the thermometer 21. The diluent supply pipe g is provided with a diluent supply pump 7 and a diluent flow meter 4 for measuring the diluent supply amount, and is connected to the three-way valve 12. The three-way valve 12 is connected with a circulation channel pipe f.
[0018]
The three-way valve 12 to which the circulation channel pipe f and the diluent supply pipe g are connected is connected to a diluent pipe h that shares the diluent channel and the circulation channel. The diluent pipe h passes through the three-way valve 13. The diluting liquid supply pipe h1 connected to the diluting / mixing tank 2 and the diluting liquid injection pipe h2 connected to the sample pot are branched and connected.
[0019]
In the above-described configuration, the diluent flow meter 4 is provided in the diluent supply pipe g. However, if an appropriate diluent is supplied, such as a configuration in which the operation of the diluent supply pump 7 is controlled. The diluent flow meter 4 is not always necessary. Further, the circulation channel pipe f and the diluent supply pipe g are connected via the three-way valve 12, but the circulation channel pipe f is directly connected to the dilution mixing tank 2 and only the diluent supply pipe g is connected to the three-way valve. The structure connected to 13 may be sufficient and this invention is not limited to the said structure.
[0020]
Although not shown in the above, temperature control of the heater 16, heater 17 and heater 18, etc., opening and closing of the three-way valve 10, three-way valve 11, three-way valve 12, three-way valve 13, three-way valve 14 and three-way valve 15 and the like. A control device for automatically controlling the control, various measuring devices such as the diluent flow meter 4 and the operation stop of the diluent supply pump 7 and the like is provided.
[0021]
The operation of measuring particles in heavy fuel oil using the apparatus having the above-described configuration will be described below.
A predetermined amount of sample liquid is collected with a syringe or the like and injected from the sample injection port of the sample pot 1, or the sample pot 1 is removed and a predetermined amount is collected with a scale marked on the side wall. After the sample liquid is heated by the heater 16 of the temperature control means and reaches a predetermined temperature, a pressurized gas such as nitrogen or air from the pressurized gas supply means 6 such as a gas cylinder is supplied to the pressurized gas supply main pipe. j, the three-way valve 15, the pressurized gas supply main a and the three-way valve 10 are supplied from the pressurized gas supply pipe a 1, and the sample liquid is discharged from the sample discharge supply pipe b at that pressure and supplied to the dilution mixing tank 2. At the same time, the diluent is injected from the diluent injection tube h2 to clean the inside of the sample pot 1, and is supplied to the dilution mixing tank 2 with the gas pressure in the same manner as the sample solution.
[0022]
The sample solution supplied to the dilution / mixing tank 2 is extracted from the diluent supply pipe g of the diluent tank 3 with a diluent supply pump 7, and the diluent supply amount is measured with the diluent flow meter 4. The mixture is diluted with the diluent supplied to the dilution / mixing tank 2 through the three-way valve 12, the diluent pipe h, and the diluent supply pipe h1.
[0023]
Mixing and dilution of the sample liquid and the diluting liquid are stirred and mixed by the stirring means 9 and extracted from the diluted sample discharge supply pipe c through the three-way valve 11 and the circulation pump 8, and the circulation channel pipe f and the three-way valve. 12, the mixture is circulated to the dilution / mixing tank 2 through the dilution liquid pipe h and the dilution liquid supply pipe h1, so that the particles are efficiently mixed and the particles are reliably dispersed.
[0024]
After the diluted sample is circulated for a predetermined time, the circulation is stopped, the pressurized gas is supplied from the pressurized gas supply pipe a2 to the dilution mixing tank 2, and the flow path of the three-way valve 11 is connected to the particle capturing flow pipe d. The diluted sample is extracted from the dilution / mixing tank 2 to the particle capturing channel tube d with the pressure of the pressurized gas.
[0025]
The diluted sample supplied to the particle capturing channel tube d is supplied to the filter 5 through the three-way valve 14 and the particle capturing channel tube d1, and the particles are captured by a filter medium such as filter paper of the filter 5 to discharge the sample liquid. It is discharged out of the system from the pipe d2. After the entire diluted sample in the dilution / mixing tank 2 is circulated, the diluted solution is supplied into the dilution / mixing tank 2 for cleaning, and the particles are circulated in the same manner as the diluted sample and captured by the filter medium of the filter 5. Wash etc.
[0026]
After the cleaning is completed, the pressurized gas is supplied to the filter 5 through the pressurized gas supply pipe e, the three-way valve 14, and the particle capturing flow path pipe d1 for a predetermined time to dry the filter medium. In the case where the pressurized gas supply pipe e is not provided, the pressurized gas supplied to the dilution mixing tank 2 is circulated through the flow path of the diluted sample to dry the filter medium, but there is a problem that the drying efficiency is poor. . The dried filter medium is removed from the filter 5, and the particle amount and particle size of the particles are measured by an appropriate particle measuring means. In addition, as a measuring means, the device that enlarges the particles on the filter medium with a microscope, captures it as electronic information data with a digital camera, processes the computer image, and measures it as a numerical value is more artificially measured. This is preferable because it does not cause an error and can be quantitatively grasped.
[0027]
In the above, temperature control of the heater 16, the heater 17 and the heater 18, the three-way valve 10, the three-way valve 11, the three-way valve 12, the three-way valve 13, the three-way valve 14 and the three-way valve 15, and the like, the diluent flow rate Various measuring devices such as the total 4 and the operation stop of the diluent supply pump 7 and the circulation pump 8 are automatically controlled by a control device (not shown).
[0028]
【The invention's effect】
In the present invention, the sample adjustment operation for particle measurement after sampling the sample liquid is fully automated, the amount of particles in oil can be measured quickly, and measurement errors due to cleaning unevenness and external particle contamination may occur. This is a sample preparation device for particle measurement in oil that can obtain accurate measurement results and therefore can be reflected in operation under appropriate conditions such as a centrifuge and does not cause damage to the internal combustion engine etc. .
[Brief description of the drawings]
FIG. 1 is a system diagram of a sample preparation apparatus for measuring particles in oil according to an embodiment of the present invention.
1: Sample pot 2: Dilution mixing tank 3: Dilution liquid tank 4: Dilution liquid flow meter 5: Filter 6: Pressurized gas supply means 7: Dilution liquid supply pump 8: Circulation pump 9: Stirring means 10, 11, 12 , 13, 14, 15: three-way valves 16, 17, 18: heaters 19, 20, 21: thermometer

Claims (1)

A sample pot provided with a temperature control means for storing a certain amount of sample liquid collected and adjusting the temperature, a dilution tank provided with a temperature control means for storing a diluent, and a sample liquid from the sample pot; A dilution and mixing tank provided with temperature control means for mixing the diluent from the diluent tank to obtain a diluted sample solution; and a diluent supply pump for supplying the diluent from the diluent tank to the sample pot and the dilution and mixing tank, respectively. , A filter for capturing particles in the diluted sample liquid in the diluted sample liquid extraction flow path of the diluted mixing tank with a filter medium, and a pressurized gas supply for supplying pressurized gas to the sample pot, the diluted mixing tank and the filter, respectively. And a sample preparation device for measuring particles in oil.

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