WO2003100387A1 - Device for measuring stringiness of liquid material and stringiness measuring method - Google Patents

Device for measuring stringiness of liquid material and stringiness measuring method Download PDF

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Publication number
WO2003100387A1
WO2003100387A1 PCT/JP2003/006544 JP0306544W WO03100387A1 WO 2003100387 A1 WO2003100387 A1 WO 2003100387A1 JP 0306544 W JP0306544 W JP 0306544W WO 03100387 A1 WO03100387 A1 WO 03100387A1
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WO
WIPO (PCT)
Prior art keywords
liquid
sample
test liquid
measuring
spinnability
Prior art date
Application number
PCT/JP2003/006544
Other languages
French (fr)
Japanese (ja)
Inventor
Tatsuji Nishihara
Yasuaki Kakinoki
Hiroshi Kamei
Kiyomitsu Ishikawa
Original Assignee
Kitakyushu Foundation For The Advancement Of Industry, Science And Technology
Kabushikikaisha Ishikawa Ironworks Co. Ltd.
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Kitakyushu Foundation For The Advancement Of Industry, Science And Technology, Kabushikikaisha Ishikawa Ironworks Co. Ltd. filed Critical Kitakyushu Foundation For The Advancement Of Industry, Science And Technology
Priority to AU2003241768A priority Critical patent/AU2003241768A1/en
Publication of WO2003100387A1 publication Critical patent/WO2003100387A1/en

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Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N13/00Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
    • G01N13/02Investigating surface tension of liquids
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N13/00Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
    • G01N13/02Investigating surface tension of liquids
    • G01N2013/0241Investigating surface tension of liquids bubble, pendant drop, sessile drop methods

Definitions

  • the present invention relates to various body fluids such as saliva, blood, lymph fluid, synovial fluid, and urine in the medical field, inks, paints, oils, greases, and the like in the industrial field, soy sauce, sauces, mayonnaise, ketchup, dressing, dairy products, and kneaded products in the food field.
  • the present invention relates to an apparatus and a method for measuring spinnability as a viscosity parameter of a liquid material or a viscous fluid (hereinafter, referred to as a liquid material) including various gels, colloids, and slurries such as soups. n.
  • a sample of saliva at 25 ° C is used to measure the shear stress value (viscosity: mPa ⁇ s unit) after a certain period of rotation.
  • viscosity viscosity: mPa ⁇ s unit
  • viscosity measurement method using a slope plate. In this method, a certain amount of saliva is dropped on the slope plate, and the angle of the saliva starts to flow by gradually increasing the angle of the slope plate, or the saliva is kept constant and the saliva is inclined.
  • Another object of the present invention is to provide various body fluids such as saliva, blood, lymph, synovial fluid, and urine, inks, paints, oils, greases, and the like in the industrial field, soy sauce, sauces, mayonnaise, kechiap, dressing, and the like in the food field.
  • body fluids such as saliva, blood, lymph, synovial fluid, and urine, inks, paints, oils, greases, and the like in the industrial field, soy sauce, sauces, mayonnaise, kechiap, dressing, and the like in the food field.
  • the spinning parameters of liquids containing various gels, colloids, and slurries such as dairy products, pastes, and slurries
  • the chemical composition of the test liquid the chemical conditions such as pH, and the temperature
  • An object of the present invention is to provide an apparatus for measuring the physical properties of a liquid under test conditions that specify physical conditions and a method using the same. Disclosure of the invention
  • the invention according to claim 1 for solving the above-mentioned problem is characterized in that a sample pan for accommodating a test liquid, a lower end portion of the sample pan in contact with the test liquid in the sample pan, and the liquid rises. Therefore, a stringing rod that functions to detect the stringing length of the test liquid, a stringer raising / lowering means that moves the stringing rod up and down at a predetermined speed, and a measurement of the stringing length of the sample liquid.
  • the invention according to claim 2 is characterized in that the optical means for confirming the position at the time of starting the measurement of the thread length of the test liquid and the time of cutting the spine-like test liquid are based on the vertical direction of the stringing rod.
  • the invention is a liquid material spinnability measuring device according to claim 1, which is a light projector that emits light in a crossing direction and at least one optical sensor that receives light from the light projector. 3.
  • the spinnability of a liquid material according to claim 1 or claim 2 wherein a position adjusting means in the elevating direction of the stringing rod is attached to one or both of the sample pan and the optical sensor. It is a measuring device.
  • the ridge of the sample (test liquid) in the sample pan can be detected with high accuracy at every measurement, so that the spinning property of the liquid is measured with higher accuracy. be able to.
  • the optical means for confirming the positions of the start of the measurement of the thread length of the test liquid and the cutting time of the test liquid in the form of a string is provided by an error sensor or an image processing device.
  • a device for measuring the spinnability of a liquid material according to claim 1. there is provided a sample pan for accommodating a test liquid, and a lower end portion of the sample pan in contact with the test liquid in the sample pan, and the rise of the lower end detects the thread length of the test liquid.
  • a stringer which functions smoothly, a stringer raising / lowering means for raising and lowering the stringer at a predetermined speed, a time point at which the measurement of the string length of the test liquid is started, and a cutting of the string-like test liquid
  • This is a device for measuring the spinnability of liquids, provided with a load measuring device that detects a change in the force applied to the stringing rod or the sample pan at the time.
  • the lower end of the stringing rod has a flat shape and a convex spherical surface.
  • the spinnability measuring device for a liquid material according to any one of claims 1 to 5, wherein the device is any one of a ridge or a groove extending radially in a cross shape.
  • the lowering of the stringing rod lower end part can be prevented from lowering the measuring accuracy of the liquid material's stringing property due to the deviation from the center of the cross section of the stringing rod at the top of the test liquid.
  • the invention according to claim 7 is the apparatus for measuring the spinnability of a liquid material according to any one of claims 1 to 6, wherein the sample pan is a cylindrical strip having an upper flat surface.
  • the invention according to claim 8 is the one in which the stringing rod is provided with a scooping hook at the lower end thereof, the scooping hook having a function of scooping up and raising the test liquid in the sample pan.
  • the sample pan is provided with a sample holder that functions to prevent the whole of the test liquid from being lifted. Is a spinnability measuring device.
  • a sample pan for accommodating a test liquid, and any one of a tube, a slit, and an orifice formed at a lower end thereof, and the tube, the slit, And a orifice, which has a sample pot that allows the liquid to flow down from the orifice and functions to detect the thread length of the liquid to be tested.
  • the sample is relatively viscous and elastic, the surface tension is large, the sample is difficult to adhere to the sample pan with constant strength, and the adhesiveness is poor, and the liquid with high fluidity It is possible to accurately measure the spinnability of an object.
  • the invention according to claim 11 has a sample pan for containing a test liquid, and an outflow hole for allowing the test liquid to flow down from a lower end of the sample pan by rising from the sample pan.
  • a threading bar that functions to detect the length of the thread and is slidably and vertically slidably inserted into a holder having an insertion hole, and a thread that grips the holder and moves the threading bar up and down at a predetermined speed.
  • It is a device for measuring the spinnability of a liquid material comprising a towbar elevating means and optical means for confirming the position of the start of the measurement of the length of the thread of the test liquid and the cutting time of the test liquid. .
  • the stringer is lowered at a given speed toward the test liquid in the sample pan, and the light passing just above the top of the test liquid in the sample pan.
  • the threading rod interrupts the shaft, the lowering of the threading rod is stopped, and the lower end of the threading rod is brought into contact with the liquid to be tested. Thereafter, the threading rod is raised.
  • the test liquid is put into a spinning state, the test liquid in the spinning state is cut, the test liquid returns to the sample pan, and the optical axis passing just above the top of the test liquid in the sample pan is
  • the stringer is lowered at a given speed in a direction directed toward the test liquid in the sample pan, and the light passing directly above the top of the test liquid in the sample pan is received.
  • the threading rod interrupts the shaft, the lowering of the threading rod is stopped, and the lower end of the threading rod is brought into contact with the liquid to be tested. Thereafter, the threading rod is raised.
  • the test liquid is set in a spinning state, the test liquid in the spinning state is cut, and one of the optical axes of the upper optical sensors arranged in a plurality of upper and lower directions is detected by a light receiver. This is a method of measuring the spinnability of a liquid material, which measures the amount of upward displacement of a stringing rod until it is detected.
  • the holder on which the stringing rod is mounted prior to the measurement of the spinnability of the test liquid, is lowered for a certain distance, and then is raised for a certain distance, and then the position is increased.
  • the invention according to claim 15 is characterized in that, prior to the measurement of the spinnability of the test liquid, the stringing rod is lowered to bring the lower end portion into contact with the test liquid to be in a wet state.
  • a fixed amount of the test liquid is stored in the sample pot while any one of the tube, slit, and orifice at the lower end of the sample pot is in contact with the sample pan.
  • raise the stringing rod provided with the sample jar to let the sample liquid flow down from one of the tube, slit, and orifice at the lower end of the sample jar, and the tip of the sample liquid flowing down is interrupted.
  • the invention according to claim 17 is to store a fixed amount of the test liquid in the sample container while any one of the tube, slit, and orifice at the lower end of the sample container is in contact with the sample pan. Then, raise the stringing rod provided with the sample jar and let the sample liquid flow down from one of the tube, slit, and orifice at the lower end of the sample jar, and the sample liquid in the sample jar is removed. This is a method for measuring the spinnability of a liquid material, which measures the time until the spill is completed.
  • the invention according to claim 18 is characterized in that the spinning length of the test liquid in the first measurement is a reference value, and the time or the number of measurements until the spinning length reaches a certain ratio of the reference value is determined.
  • This is a method for measuring the spinnability of a liquid material to be detected. According to the present invention, it is possible to measure the coagulability of the liquid material with the spinnability of the test liquid material as a parameter.
  • the invention according to claim 19 is characterized in that the threading property of the test liquid in the sample pan is repeatedly measured by setting the rising distance of the stringing rod to a constant value within a limit at which the test liquid does not cut, and This is a method for measuring the spinnability of a liquid material in which the time or the number of measurements until the test liquid material is cut within the lifting distance of the stringing rod is detected. Also in the case of this invention, it is possible to measure the coagulability of the liquid material by setting the spinnability of the test liquid material as a parameter.
  • the invention according to claim 20 is a spinning line for a liquid material, wherein the stringing rod is lifted up from the sample pan for a fixed distance and held in that state, and a change with time in the electrical conductivity of the test liquid material is detected. It is a method of measuring sex. According to the present invention, the volatility of the liquid material can be measured with the spinnability of the test liquid material as a parameter.
  • FIG. 1 is a schematic view showing an apparatus for measuring the spinnability of a liquid material according to one embodiment of the present invention.
  • FIG. 2 shows a sample tray, a sample, a stringer, and a light at the start of measurement when measuring the spinning length of a liquid using the liquid spinnability measuring device according to one embodiment of the present invention. It is a front view showing the position of axis oa.
  • FIG. 3 is a front view showing a state in which the stringer has descended and its lower end has come into contact with the sample.
  • FIG. 4 is a front view showing the spinning state of the test liquid (sample).
  • Fig. 5 is a front view showing the state at the moment when the sample in the spinning state is cut.o
  • FIG. 6 is a front view showing a state in which the sample has been restored to the sample pan after cutting.
  • FIG. 7 is a front view showing an example of the arrangement of the optical sensor according to another embodiment of the present invention.
  • FIG. 8 is a front view showing another example of the shape of the lower end portion of the stringing rod in the liquid matter stringiness measuring device of the present invention.
  • FIG. 9 is a front view showing another embodiment of the sample tray in the liquid spinnability measuring device of the present invention.
  • FIG. 10 is a front view showing an embodiment of a sample scooping hook portion attached to the lower end of a stringing rod in the liquid matter spinnability measuring device of the present invention.
  • FIG. 11 is a front view showing an embodiment of a sample pot attached to the lower end of a stringing rod in the liquid matter stringiness measuring device of the present invention.
  • FIG. 12 shows a sample flow-through type yarn in the liquid matter spinnability measuring device of the present invention. It is a front view which shows one Example of a tow bar.
  • FIG. 13 is a graph showing the correspondence between the measurement results obtained by the liquid material spinnability measuring device and spinnability measuring method of the present invention and the measured values measured by a single cylinder gauge.
  • the present invention defines the chemical composition of the test liquid, the chemical conditions such as pH, and physical conditions such as temperature, and determines the spinnability of the test liquid by measuring the spinning length, load, and measurement. It measures the time or the number of measurements in the change of the value over time, the electrical conductivity, and the measurement parameter.
  • the physical properties of the test liquid such as saliva and the coagulable test liquid such as blood are measured for spinnability.
  • the spinnability of the test liquid is measured as the development of viscosity, elasticity, and viscoelasticity.
  • FIG. 1 shows an apparatus for measuring the spinnability of a liquid material according to one embodiment of the present invention.
  • 2 to 6 show a spinnability measuring process according to an embodiment of the present invention.
  • reference numeral 1 denotes a motor for rotating a vertically moving screw shaft 3 through a gear train 2.
  • Reference numeral 4 denotes an elevating table, in which an internal female screw is screwed with the elevating screw shaft 3, and the elevating table is moved up and down by forward and reverse rotation of the elevating screw shaft 3.
  • the lifting table 4 moves up and down within a speed range of 5 mm / s to 2 Omm / s.
  • Reference numeral 5 denotes a holder, which is fixed to the elevating table 4 and has a stringer 6 detachably fitted thereto.
  • the motor 1, the gear train 2, the lifting screw shaft 3, the lifting table 4, the holder 5, and the rotation speed control system of the motor 1 constitute lifting means of the stringing rod 6.
  • the lower end of the stringing rod 6 comes into contact with the test liquid (sample) 8, and functions to detect the stringing length until the sample comes into a stringing state and is cut.
  • the lower end of the stringing rod 6 is preferably wetted with the sample prior to the measurement of the stringing length of the test liquid (sample) 8. It is preferable for a high-precision measurement of the spinnability that the peak of the swelling due to the surface tension of the sample in a wet state exists in the center of the cross section of the lower end of the stringing rod 6.
  • the lower end of the stringing rod 6 can be flat, convex spherical, convex conical, convex pyramid, convex pyramid having a spherical tip, concave spherical, concave cone, concave pyramid.
  • Reference numeral 7 denotes a sample receiving tray, which is formed with a shallow cylindrical or inverted truncated cone-shaped concave portion, into which a predetermined amount of a test liquid (sample) 8 is charged.
  • the sample pan 7 is made of, for example, stainless steel.
  • Reference numeral 9 denotes a light emitter and 10 denotes a light receiver.
  • the pair of signal processing systems constitute a transmission type optical sensor.
  • a pair of a projector 9 and a receiver are arranged so that an optical axis oa (optical axis) passes directly above a test liquid (sample) 8 in a sample pan 7.
  • 10 is provided.
  • a transmission type optical sensor having a sensing ability capable of detecting an object of 0.01 mm (10 zm) is used.
  • Reference numeral 1 denotes an emitter / receiver mounting base, which supports the emitter 9 and the receiver 10.
  • the transmitter / receiver mounting base 11 is screwed into the optical axis position fine adjustment screw 12, and the transmission type optical sensor is highly precisely controlled by the rotation of the optical axis position fine adjustment screw 12.
  • the sensor is raised and lowered, and the position of the optical axis oa in the height direction is adjusted.
  • the position adjustment of the optical axis oa in the height direction can be performed by means for raising and lowering one or both of the emitter / receiver mounting base 11 supporting the optical sensor unit and the sample tray 7.
  • Reference numeral 13 denotes a motor drive circuit, which receives an output signal from the operation circuit 14 and drives the lift table 4 to which the holder 5 is fixed in the motor direction 1 in the ascending or descending direction. Turn on the power.
  • the motor 13 and the drive circuit 13 are also operated via the operation circuit 14 by a signal from the towing length measuring circuit 15 and cut off the power to the motor 11. Further, the motor drive circuit 13 is activated by signals from the upper limiter 18 and the lower limit 19 to cut off the power to the motor 11.
  • the operation circuit 14 is provided with a drive switch for driving the elevating table 4 to which the holder 5 is fixed in an ascending or descending direction.
  • Reference numeral 16 denotes an arithmetic circuit.
  • a feedback (feedback) control system for controlling the rotation speed of the motor 1 is formed, and a signal from the thread length measuring circuit 15 is used. Calculates the amount of displacement of the stringing rod 6 from when the stringing rod 6 starts to rise and the sample 8 in the stringing state is cut, and functions to display it on the digital display 17 .
  • the feedback (feed knock) control system for controlling the rotation speed of the motor 11 is incorporated in the liquid material spinnability measuring device.
  • This feedback control system is configured as follows in this embodiment. That is, an infrared ray is projected from a retroreflective photoinjector onto a reflecting disk 20 having black-and-white contrast formed at predetermined intervals in the circumferential direction of the outer peripheral surface, and reflected infrared light from a white portion of the reflecting disk 20 is reflected.
  • This pulse is regarded as an idle-back pulse, and the number of pulses per time is input to the arithmetic circuit 16, and if there is a deviation from the rotation speed target value of the motor 1 which gives the given lifting speed to the holder 5, the deviation is detected To change the ON-OFF width ratio in the input pulse to motor 1 Leakage 44
  • Pulse 23 is input to the motor 1 via the motor drive circuit 13. That is, the speed control of the pulse width modulation method is performed.
  • the rotation speed control of each of the individual spinnability measuring devices is performed by the feedback control system described above, so that the holder 5 Is calibrated to be displaced at a given lifting speed.
  • test liquid (sample) 8 is charged in the sample receiving tray 7 in advance, the holder 5 is lowered until the lower end of the stringing rod 6 comes into contact with the sample 8, and then the constant displacement Increase the amount. In this process, the feedback control is performed to make the elevating speed of the holder 5 converge to a given target value. After carrying out calibration for each spinnability measuring device, the spinnability of the test liquid (sample) 8 is measured.
  • the lower end of the stringing rod 6 becomes wet because the lower end of the stringing rod 6 is in the sample pan 7 when measuring the actual stringiness. When it comes into contact with 8, it becomes a fusion state, and it is possible to eliminate the dispersion of measured values caused by the surface properties of the lower end of the stringing rod 6.
  • the sample pan 7 or the transmission type optical sensor 1 is moved up and down to determine whether or not the optical axis oa is transmitted.
  • the optical sensor is set by the optical axis position adjusting screw 12 so that the optical axis oa passes horizontally at a position about 10 zm higher than that position in the height direction.
  • the stretched sample 8 is cut when the string length corresponding to the viscosity is reached, as shown in FIG. After cutting, the sample 8 returns to the sample pan 7 instantaneously as shown in FIG. 6, and the optical axis o a is again transmitted.
  • the amount of upward displacement of the stringing rod 6 from the interruption of the optical axis oa to the moment when the photodetector 10 outputs a light detection signal again depends on the stringing length of the test liquid (sample) 8 (viscosity parameter). Overnight).
  • An N-OFF signal is input to the arithmetic circuit 16 via the motor drive circuit 13 via the motor drive circuit 13 and the motor from when the light sensor 1 detects light blocking to when the light receiver 10 detects the optical axis oa again.
  • the number of rotations (number of pulses) per night is counted, and this is converted (calculated) into the amount of upward displacement of the stringing rod 6 and output to the digital display 17.
  • test liquid (sample) 8 is a gel-like highly viscous material
  • a plurality of optical sensors 1 are arranged in the elongating (height) direction of the sample 8, and the cutting position ( Height) can be detected directly.
  • Initial state of spinnability measurement After confirming the position of the top of liquid sample (sample) 8 in sample pan 7, the optical sensor (base point optical sensor) is set so that optical axis oa passes about one part above.
  • the distance between the upper optical sensor that detected the optical axis oa of the plurality of optical sensors installed and the base optical sensor after ascending the stringer 6 from the light blocking detection of the base optical sensor Is the spinning length of Sample 8.
  • the number of optical sensors disposed above the base optical sensor and the position in the height direction may be determined in accordance with the physical properties of the target liquid material (sample) 8 to be measured.
  • the liquid material (sample) 8 at the top of the sample 8 at the start of the measurement of the string length and the height direction at the time of cutting of the sample 8 in the state of the string are measured.
  • the optical detection means for confirming the position is a transmission type optical sensor.
  • the present invention is not limited to this, and the cutting of the sample 8 in the state at the start of the spinning property measurement of the liquid material and the spinning state using an area sensor, for example, a CCD camera, a laser, and a sensor, is performed.
  • Optical detection means for confirming the position in the height direction at the time can also be employed.
  • an optical detection means for confirming the position in the height direction at the time of the start of the measurement of the spinnability of the liquid material and the time of the cutting of the sample 8 in the spinning state, using an image processing means may be employed.
  • the optical detection means detects the start time and the spinning state of the liquid material spinnability measurement.
  • the position of the sample 8 in the height direction at the time of cutting was confirmed.
  • a load measuring device that senses a small load variation on the sample pan 7 or the stringing rod 6 is described.
  • a load measuring device with a high resolution such as an electronic balance, is installed, and the load change at the moment the stringer 6 comes into contact with the sample 8 and the cutting time of the sample 8 in the stringing state is 0.1 mg unit.
  • the detection signal can be used as a digital processing signal.
  • the method for measuring the spinnability of a liquid material in the above-described embodiment is as follows.
  • the lower end of the stringing rod 6 is wetted in advance, and the spinning length up to the cutting of the test liquid material (sample) 8 in the spinning state.
  • Wet measurement is repeated several times to extract the average value and distribution state in the sample group, etc., and the stringing rod 6 is dry without wetting the lower end with the test liquid (sample) 8.
  • the gate test method is suitable for measuring a test liquid (sample) 8 having viscosity, elasticity, surface tension, and adhesive strength to some extent.
  • the dry test method is suitable for measuring test liquids (samples) 8 having high adhesive strength and low elasticity.
  • FIG. 10 shows an apparatus for measuring the spinnability of a liquid material according to another embodiment of the present invention.
  • the stringer 26 in this embodiment has a scooping hook 36 at the lower end thereof.
  • the tip of the scooping hook portion 36 is inserted into the test liquid (sample) 8 in the sample pan 7, and a predetermined amount of the sample 8 is scooped up by the raising of the stringing rod 26 to form a string. It functions to measure the length of the string until the cutting of a certain sample 8.
  • the device for measuring the spinnability of a liquid material according to this embodiment is suitable for measuring a liquid material (sample) 8 having low viscosity, elasticity, viscoelasticity, surface tension, and tackiness and high fluidity. ing.
  • reference numeral 101 denotes a sample holder, which has a forked flat shape and is fixed to the sample pan 7.
  • the sample holder 101 prevents the entire amount of the test liquid (sample) 8 from being lifted by the scooping hook 36.
  • the cross-sectional shape of the tip of the scooping hook 3 6 can be appropriately selected according to the physical properties of the test liquid (sample) 8 such as an inverted triangle, a square, a circle, and a spun shape.
  • FIG. 11 shows an apparatus for measuring the spinnability of a liquid material according to another embodiment of the present invention.
  • the test liquid (sample) 8 flows down from one of the tube 481, the slit 482, and the orifice 483 formed at the lower end of the sample # 48.
  • one of the tube 481, the slit 482, and the orifice 483 at the lower end of the sample pot 48 is brought into contact with the bottom surface of the sample pan 7 in advance. Inject a predetermined amount of the test liquid (sample) 8 into the sample jar 48, or close one of the tube 481, slit 482, and orifice 483 with a thin rod.
  • test liquid (sample) 8 A predetermined amount of the test liquid (sample) 8 is injected into the sample pot 48, and opened at the same time as the measurement is started, and the stringer 6 is lifted to raise the string 8 in the height direction at the time of cutting.
  • the position is detected by optical detection means.
  • the apparatus for measuring the spinnability of a liquid material according to this embodiment and the method for measuring the spinnability include a test liquid (sample) 8 having low viscosity, elasticity, viscoelasticity, surface tension, and low adhesiveness and high fluidity. Suitable for measurement. This test method is called a flow test method.
  • FIG. 12 shows an apparatus for measuring the spinnability of a liquid material according to another embodiment of the present invention.
  • 1 to 7 are the same components.
  • the test liquid (sample) 8 flows down from an outflow hole 361 formed at the center of the cross section of the stringing rod 6 and having an opening at the lower end.
  • the test liquid (sample) 8 is stored by the syringe 48 or the spike 48.
  • the method of measuring the spinnability in this example is as follows. A predetermined amount of the test liquid (sample) 8 is stored by bringing the opening of the outflow hole 36 1 into contact with the inner bottom surface of the sample pan 7 in advance.
  • the piston or spoiler of the syringe is opened, the stringing rod 6 is raised, and the position of the sample 8 in the stringing state in the height direction at the time of cutting is detected by optical detection means.
  • the liquid material spinnability measuring device and the spinnability measuring method according to this embodiment are also low in viscosity, elasticity, viscoelasticity, surface tension, and tackiness, and have high fluidity. 8 is suitable for measurement.
  • This test method is also an embodiment of the Fuchi-one test method.
  • the measurement of the stringing length of the test liquid (sample) 8 is repeated a plurality of times, and the amount of change in the stringing length is measured.
  • the time until the stringing length reaches a certain percentage of the reference value, for example, 50% or the number of measurements is determined as the coagulation parameter of the test liquid (sample) 8. I do.
  • a certain length is set within the limit where the test liquid (sample) 8 is not cut, and the stringer 6 is repeatedly moved up and down within that range. Then, the time until cutting of the sample 8 in the spinning state or the number of repetitions of ascending and descending is detected, and this is regarded as a parameter of the coagulability of the test liquid (sample) 8.
  • a certain length is set within the limit where the test liquid (sample) 8 is not cut, and the stringing rod 6 is raised and held within that range. Then, the electrical conductivity of the test liquid (sample) 8 is measured with time. This measured value is used as the volatile parameter of the test liquid (sample) 8.
  • the apparatus for measuring the spinnability of a liquid material of the present invention and the method for measuring the spinnability using the same are carried out as described above. Temperature, humidity, temperature of the test liquid (sample), surface properties (surface roughness, etc.) of the portion of the stringer in contact with the sample, size and shape of the stringer, speed of stringer rise, etc. It is. It is necessary to comprehensively judge and standardize these factors corresponding to the test liquid (sample).
  • FIG. 13 shows the measurement of the liquid material according to the present invention by the spinnability measuring apparatus and spinnability measuring method. 6544
  • the liquid substances which can be targeted by the spinnability measuring device and spinnability measuring method of the present invention include liquid substances in the medical field such as saliva, urine, nasal discharge, and sputum, as well as oils, fats, inks, and paints in addition to saliva.
  • liquid substances in the food field such as liquids, dressings, milk, etc., which are handled in Japan, as well as liquids and pastes that have a drawstring, such as gels and emulsions, can be targeted.
  • the viscosity of the liquid having spinnability is determined regardless of whether the liquid has conductivity. Measurement can be performed with high accuracy without causing individual differences among the measurers. Further, according to the spinnability measuring device and spinnability measuring method for a liquid material of the present invention, an automatic measurement can be performed with as small a sample as possible, and the measurement result is digitally displayed. Factors that tend to cause measurement errors, such as reading the position, can be eliminated. Furthermore, the stringer is detachably fitted to the holder, so that the assembly of the device is simple and the stringer can be easily cleaned.
  • the swelling of the test liquid (sample) in the sample pan can be detected with high accuracy at every measurement, so that the spinnability of the liquid can be measured more accurately. Can be done higher.
  • an error sensor such as a CCD camera, a laser sensor, or the like, or an image processing technique.
  • the spinning property of the liquid material can be measured by attaching a load measuring device such as a load cell to the stringing rod and Z or the sample pan.
  • the viscosity and elasticity of the sample are relatively high, and In cases where the surface tension is large and the sample is difficult to adhere to the sample pan with a certain strength and the adhesiveness is poor, the spinnability of a liquid material with high fluidity can be accurately measured.
  • the viscosity and elasticity of the sample are relatively high, the surface tension is large, and the sample is fixed on the sample pan. It is possible to measure the spinnability of a liquid material with high fluidity even when it is difficult to adhere with low strength and has poor adhesion.
  • the spinnability of the liquid material can be measured as a parameter to measure the coagulability of the liquid material.
  • the volatility of the liquid material can be measured by setting the spinnability of the liquid material as a parameter.

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Abstract

A device for measuring the stringiness of a liquid material capable of measuring the stringiness of a sample in an amount as small as possible, digital measuring, automatic measuring, eliminating individual differences in measurements that might be caused by measuring persons, and measuring independently of whether a sample is electrically conductive or not; and a stringiness measuring method using the device. The device for measuring the stringiness of a liquid material comprises a sample receiving dish for accommodating a liquid to be detected, a stringing rod being in contact at the lower end thereof with the liquid to be detected in the receiving dish to function to detect the stringing length of the liquid to be detected when lifted, a stringing rod lifting means for vertically moving the rod at a specified speed, and an optical detection means for detecting the measurement starting point of the liquid to be detected and the height-direction position at breaking of the liquid to be detected in a stringy condition; and a stringiness measuring method using the device.

Description

PC翻襄 544 PC Jojo 544
- 1 - 明細書 液状物の曳糸性測定装置及び曳糸性測定方法 技術分野  -1-Description Liquid string spinnability measuring device and spinnability measuring method
本発明は、 医療分野における唾液、 血液、 リンパ液、 関節液、 尿といった 各種体液、 産業分野におけるインク、 塗料、 オイル、 グリース等、 食品分野 における醤油、 ソース、 マヨネーズ、 ケチャップ、 ドレッシング、 乳製品、 練り物、 スープ等種々のゲル、 コロイド、 スラリーを含む液状物又は粘稠性 を有する流動状物 (以下、 液状物と称する。 ) の粘性のパラメータとしての 曳糸性を測定する装置及び方法に関する。 n.  The present invention relates to various body fluids such as saliva, blood, lymph fluid, synovial fluid, and urine in the medical field, inks, paints, oils, greases, and the like in the industrial field, soy sauce, sauces, mayonnaise, ketchup, dressing, dairy products, and kneaded products in the food field. The present invention relates to an apparatus and a method for measuring spinnability as a viscosity parameter of a liquid material or a viscous fluid (hereinafter, referred to as a liquid material) including various gels, colloids, and slurries such as soups. n.
たとえば医療分野において、 人の唾液の粘性と精神的 ·肉体的疲労度が相 関関係にあり、 疲労度が増すにつれて唾液の粘性が高くなることが知られて いる処から、 唾液の粘性をはじめとする唾液の物性を検査することの必要性 が認識されてきている。 その際、 口腔乾燥を来している患者からの多量の唾 液の採取は困難であつた。  For example, in the medical field, there is a correlation between the viscosity of human saliva and the degree of mental and physical fatigue, and it is known that the viscosity of saliva increases as the degree of fatigue increases. The necessity of examining the physical properties of saliva has been recognized. At that time, it was difficult to collect large amounts of saliva from patients with dry mouth.
唾液の粘性測定手段として、 たとえばコーンプレート式回転粘度計によつ て、 2 5 °Cの唾液を試料として、 一定時間回転後のずり応力値 (粘度: mP a · s単位) を測定値とする方法がある。 しかしながら、 試料の温度管理や 測定機器の価格の問題で一般には普及していない。 一方、 斜面板を用いる粘 性計測方法もある。 この方法は、 一定量の唾液を斜面板上に垂らし、 斜面板 の角度を徐々に大きくして唾液が流れ始めるときの角度を測定するか或いは 斜面板の角度を一定に保って唾液を斜面板上に垂らしてその流動長さを測定 するものであるが、 斜面板の表面性状や角度の評価や唾液を多量に必要とす る問題があり、 一般化されていない。 唾液の物性測定に限らず、 医療分野、 産業分野、 食品分野等で取り扱われる各種液状物の粘性を、 簡便かつ精確に 測定する手段が強く望まれていた。 As a means of measuring the viscosity of saliva, for example, using a cone-plate rotary viscometer, a sample of saliva at 25 ° C is used to measure the shear stress value (viscosity: mPa · s unit) after a certain period of rotation. There is a way to do that. However, it is not widely used due to problems such as temperature control of samples and price of measuring equipment. On the other hand, there is also a viscosity measurement method using a slope plate. In this method, a certain amount of saliva is dropped on the slope plate, and the angle of the saliva starts to flow by gradually increasing the angle of the slope plate, or the saliva is kept constant and the saliva is inclined. It measures the flow length by hanging it up, but it has not been generalized due to the problem of evaluating the surface properties and angle of the slope plate and requiring a large amount of saliva. Easy and accurate measurement of the viscosity of various liquids handled in the medical, industrial, and food fields, as well as in the measurement of physical properties of saliva A means of measuring was strongly desired.
【発明が解決しょうとする課題】  [Problems to be solved by the invention]
液状物の粘性を測定する手段として液状物の曳糸性を利用し、 液状物の糸 曳き長さを測定してこの測定値を粘性のパラメ一夕として用いる方法がある 。 この方法は、 目視で液状物に棒の先端を接触させ、 この棒を上方向に引き 上げてそのときの液状物の糸曳き長さを測定するものである。 しかしながら 、 被検体である液状物に棒が接触したか否かは、 人間の目視による判断に頼 つていた。 また、 液状物の糸曳きが切れた瞬間の判定も人間に頼っていたた め、 測定値にかなり個人差および誤差を生じる問題があった。 そこで発明者 らは、 特願 2 0 0 1— 1 1 9 4 7 4にて、 液状物の導電性を利用し、 液状物 の糸曳きが切れた瞬間の、 試料受皿と糸曳き棒間に印加した電圧の変ィ匕を検 出しこの検出信号によって液状物の曳糸長さを測定する装置及び方法を提案 した。 しかし、 導電性を有しない液状物を対象とできない問題があった。 本発明は、 ①可及的に少ない量の試料で液状物の曳糸性を測定することが できる。 ②ディジタルな計測ができる。 ③自動計測ができ、 測定結果の個人 差を排除できる。④試料である液状物が導電性を有すると否とに拘わらず液 状物の曳糸性を測定することができる。 液状物の曳糸性測定手段を提供 することを目的とする。 本発明の他の目的は、 唾液、 血液、 リンパ液、 関節 液、 尿といった各種体液、 産業分野におけるインク、 塗料、 オイル、 グリ一 ス等、 食品分野における醤油、 ソース、 マヨネーズ、 ケチヤヅプ、 ドレッシ ング、 乳製品、 練り物、 ス一プ等種々のゲル、 コロイド、 スラリ一を含む液 状物の曳糸性パラメ一夕として、 被検液状物の化学的組成、 p Hといった化 学的条件や温度といつた物理的条件を規定した試験条件下での液状物の物性 を測定するための装置及びそれを用いる方法を提供することである。 発明の開示  As a means for measuring the viscosity of a liquid material, there is a method that utilizes the spinnability of the liquid material, measures the stringing length of the liquid material, and uses the measured value as a parameter of the viscosity. In this method, the tip of a rod is visually brought into contact with a liquid material, and the rod is pulled upward to measure the stringing length of the liquid material at that time. However, whether or not the rod came into contact with the liquid material as the subject relied on human visual judgment. In addition, since the determination of the moment when the stringing of the liquid material was broken also relied on humans, there was a problem that the measured values had considerable individual differences and errors. Therefore, the present inventors, in Japanese Patent Application No. 2001-114, use the conductivity of a liquid material, and apply a force between the sample pan and the stringing rod at the moment when the stringing of the liquid material is broken. An apparatus and method for detecting a change in the applied voltage and for measuring the length of the thread of the liquid material based on the detection signal were proposed. However, there has been a problem that liquid materials having no conductivity cannot be targeted. According to the present invention, (1) the spinnability of a liquid material can be measured with a sample as small as possible. ② Digital measurement is possible. (3) Automatic measurement is possible, and individual differences in measurement results can be eliminated. (4) The spinnability of a liquid material can be measured regardless of whether the liquid material as a sample has conductivity. It is intended to provide a means for measuring the spinnability of a liquid material. Another object of the present invention is to provide various body fluids such as saliva, blood, lymph, synovial fluid, and urine, inks, paints, oils, greases, and the like in the industrial field, soy sauce, sauces, mayonnaise, kechiap, dressing, and the like in the food field. As the spinning parameters of liquids containing various gels, colloids, and slurries such as dairy products, pastes, and slurries, the chemical composition of the test liquid, the chemical conditions such as pH, and the temperature An object of the present invention is to provide an apparatus for measuring the physical properties of a liquid under test conditions that specify physical conditions and a method using the same. Disclosure of the invention
上記課題を解決するための請求項 1に記載の発明は、 被検液状物を収容す る試料受皿と、 該試料受皿内の被検液状物にその下端部が接触しその上昇に よって被検液状物の曳糸長さを検出すべく機能する糸曳き棒と、 該糸曳き棒 を所定の速度で昇降せしめる糸曳き棒昇降手段と、 被検液状物の曳糸長さ測 定開始時点および曳糸状被検液状物の切断時点の位置を確認する光学的手段 とを有する液状物の曳糸性測定装置である。 この発明によれば、 試料である 液状物が導電性を有すると否とに拘わらず液状物の曳糸性を測定することが できる。 The invention according to claim 1 for solving the above-mentioned problem is characterized in that a sample pan for accommodating a test liquid, a lower end portion of the sample pan in contact with the test liquid in the sample pan, and the liquid rises. Therefore, a stringing rod that functions to detect the stringing length of the test liquid, a stringer raising / lowering means that moves the stringing rod up and down at a predetermined speed, and a measurement of the stringing length of the sample liquid. An optical means for confirming the position at the start time and at the time of cutting of the spinning test liquid material. According to the present invention, the spinnability of a liquid material can be measured regardless of whether or not the liquid material as a sample has conductivity.
請求項 2に記載の発明は、 被検液状物の曳糸長さ測定開始時点および曳糸 状被検液状物の切断時点の位置を確認する光学的手段が、 糸曳き棒の昇降方 向と交叉する方向に光を発する投光器と該投光器からの光を受光する少なく とも一の光センサ一である請求項 1に記載の液状物の曳糸性測定装置である 請求項 3に記載の発明は、 試料受皿及び光センサ一の何れか一方または双 方に、 糸曳き棒の昇降方向における位置調整手段が付設されたものである請 求項 1又は請求項 2に記載の液状物の曳糸性測定装置である。 この発明によ るときは、 測定の度毎に試料受皿内の試料 (被検液状物) の盛り上がり頂部 を高精度下に検出することができるから、 液状物の曳糸性測定より精度高く 行うことができる。  The invention according to claim 2 is characterized in that the optical means for confirming the position at the time of starting the measurement of the thread length of the test liquid and the time of cutting the spine-like test liquid are based on the vertical direction of the stringing rod. The invention is a liquid material spinnability measuring device according to claim 1, which is a light projector that emits light in a crossing direction and at least one optical sensor that receives light from the light projector. 3. The spinnability of a liquid material according to claim 1 or claim 2, wherein a position adjusting means in the elevating direction of the stringing rod is attached to one or both of the sample pan and the optical sensor. It is a measuring device. According to the present invention, the ridge of the sample (test liquid) in the sample pan can be detected with high accuracy at every measurement, so that the spinning property of the liquid is measured with higher accuracy. be able to.
請求項 4に記載の発明は、 被検液状物の曳糸長さ測定開始時点および曳糸 状被検液状物の切断時点の位置を確認する光学的手段が、 ェリァセンサ一又 は画像処理装置である請求項 1に記載の液状物の曳糸性測定装置である。 請求項 5に記載の発明は、 被検液状物を収容する試料受皿と、 該試料受皿 内の被検液状物にその下端部が接触しその上昇によって被検液状物の曳糸長 さを検出すベく機能する糸曳き棒と、 該糸曳き棒を所定の速度で昇降せしめ る糸曳き棒昇降手段と、 被検液状物の曳糸長さ測定開始時点および曳糸状被 検液状物の切断時点に糸曳き棒又は試料受皿に負荷される力の変化を検出す る荷重測定器を糸曳き棒又は試料受皿に設けた液状物の曳糸性測定装置であ る。  In the invention according to claim 4, the optical means for confirming the positions of the start of the measurement of the thread length of the test liquid and the cutting time of the test liquid in the form of a string is provided by an error sensor or an image processing device. 2. A device for measuring the spinnability of a liquid material according to claim 1. According to a fifth aspect of the present invention, there is provided a sample pan for accommodating a test liquid, and a lower end portion of the sample pan in contact with the test liquid in the sample pan, and the rise of the lower end detects the thread length of the test liquid. A stringer which functions smoothly, a stringer raising / lowering means for raising and lowering the stringer at a predetermined speed, a time point at which the measurement of the string length of the test liquid is started, and a cutting of the string-like test liquid This is a device for measuring the spinnability of liquids, provided with a load measuring device that detects a change in the force applied to the stringing rod or the sample pan at the time.
請求項 6に記載の発明は、 糸曳き棒の下端部形状が、 フラット状、 凸球面 状、 凸円錐状、 凸角錐状、 球面状先端部を有する凸角錐状、 凹球面状、 凹円 錐状、 凹角錐状、 直径方向に一文字状に延在する凸条または凹溝、 および直 径方向に十文字状に延在する凸条または凹溝の何れかである請求項 1乃至請 求項 5何れかに記載の液状物の曳糸性測定装置である。 この発明によれば、 糸曳き棒下端部を湿潤状態とした被検液状物頭頂部位置の、 糸曳き棒横断面 中心からのずれに起因する液状物の曳糸性測定精度の低下を防止できる。 請求項 7に記載の発明は、 試料受皿が、 上部平面を有する円柱条体である 請求項 1乃至請求項 6何れかに記載の液状物の曳糸性測定装置である。 請求項 8に記載の発明は、 糸曳き棒が、 その下端部に試料受皿内の被検液 状物を掬い取り上昇すベく機能する掬い取りフヅク部をその下端部に付設し たものである請求項 1乃至請求項 7何れかに記載の液状物の曳糸性測定装置 である。 この発明によるときは、 試料の粘性や弾性が比較的高く、 表面張力 が大きくて試料受皿に試料が一定の強度で付着し難く粘着性が劣る場合であ つてかつ、 流動性が高い液状物の曳糸性を精度よく測定することができる。 請求項 9に記載の発明は、 試料受皿が、 被検液状物の全体が持ち上がらな いように機能する試料押さえ具を付設したものである請求項 1乃至請求項 8 何れかに記載の液状物の曳糸性測定装置である。 In the invention according to claim 6, the lower end of the stringing rod has a flat shape and a convex spherical surface. Shape, convex cone shape, convex pyramid shape, convex pyramid shape with spherical tip, concave spherical shape, concave circular cone shape, concave pyramid shape, convex stripe or groove extending in a straight line in the diameter direction, and straight The spinnability measuring device for a liquid material according to any one of claims 1 to 5, wherein the device is any one of a ridge or a groove extending radially in a cross shape. ADVANTAGE OF THE INVENTION According to this invention, the lowering of the stringing rod lower end part can be prevented from lowering the measuring accuracy of the liquid material's stringing property due to the deviation from the center of the cross section of the stringing rod at the top of the test liquid. . The invention according to claim 7 is the apparatus for measuring the spinnability of a liquid material according to any one of claims 1 to 6, wherein the sample pan is a cylindrical strip having an upper flat surface. The invention according to claim 8 is the one in which the stringing rod is provided with a scooping hook at the lower end thereof, the scooping hook having a function of scooping up and raising the test liquid in the sample pan. An apparatus for measuring the spinnability of a liquid material according to any one of claims 1 to 7. According to the present invention, when the viscosity and elasticity of the sample are relatively high, the surface tension is large, the sample is difficult to adhere to the sample pan with a certain strength, and the adhesiveness is poor, and the liquid material having high fluidity is used. The spinnability can be accurately measured. The invention according to claim 9 is characterized in that the sample pan is provided with a sample holder that functions to prevent the whole of the test liquid from being lifted. Is a spinnability measuring device.
請求項 1 0に記載の発明は、 被検液状物を収容する試料受皿と、 その下端 部にチューブ、 スリット、 およびォリフィスの何れかが形成され前記試料受 皿からの上昇によって該チューブ、 スリヅト、 およびオリフィスの何れかか ら被検液状物を流下せしめる試料壷を有し被検液状物の曳糸長さ検出すベく 機能する、 揷通孔を有する保持具に上下摺動自在に遊嵌される糸曳き棒と、 前記保持具を把持して該糸曳き棒を所定の速度で昇降せしめる糸引き棒昇降 手段と、 被検液状物の曳糸長さ測定開始時点および曳糸状被検液状物の切断 時点の位置を確認する光学的手段とを有する液状物の曳糸性測定装置である 。 この発明によるときは、 試料の粘性や弾性が比較的高く、 表面張力が大き くて試料受皿に試料が一定の強度で付着し難く粘着性が劣る場合であってか つ、 流動性が高い液状物の曳糸性を精度よく測定することができる。 請求項 1 1に記載の発明は、 被検液状物を収容する試料受皿と、 該試料受 皿からの上昇によってその下端部から被検液状物を流下せしめる流出孔を有 し被検液状物の曳糸長さ検出すべく機能する、 挿通孔を有する保持具に上下 摺動自在に遊嵌される糸曳き棒と、 前記保持具を把持して該糸曳き棒を所定 の速度で昇降せしめる糸曳き棒昇降手段と、 被検液状物の曳糸長さ測定開始 時点および曳糸状被検液状物の切断時点の位置を確認する光学的手段とを有 する液状物の曳糸性測定装置である。 According to a tenth aspect of the present invention, there is provided a sample pan for accommodating a test liquid, and any one of a tube, a slit, and an orifice formed at a lower end thereof, and the tube, the slit, And a orifice, which has a sample pot that allows the liquid to flow down from the orifice and functions to detect the thread length of the liquid to be tested. A stringing rod to be measured; a stringing rod elevating means for gripping the holder and moving the stringing rod up and down at a predetermined speed; and It is an apparatus for measuring the spinnability of a liquid material, comprising an optical means for confirming the position at the time of cutting the material. According to this invention, the sample is relatively viscous and elastic, the surface tension is large, the sample is difficult to adhere to the sample pan with constant strength, and the adhesiveness is poor, and the liquid with high fluidity It is possible to accurately measure the spinnability of an object. The invention according to claim 11 has a sample pan for containing a test liquid, and an outflow hole for allowing the test liquid to flow down from a lower end of the sample pan by rising from the sample pan. A threading bar that functions to detect the length of the thread and is slidably and vertically slidably inserted into a holder having an insertion hole, and a thread that grips the holder and moves the threading bar up and down at a predetermined speed. It is a device for measuring the spinnability of a liquid material, comprising a towbar elevating means and optical means for confirming the position of the start of the measurement of the length of the thread of the test liquid and the cutting time of the test liquid. .
請求項 1 2に記載の発明は、 試料受皿内の被検液状物に指向して所与の速 度で糸曳き棒を降下せしめ、 試料受皿内の被検液状物の頂部の直上を通る光 軸を糸曳き棒下端部が遮断したときに前記糸曳き棒の降下を停止させるとと もに糸曳き棒下端部を被検液状物に接触させ、 然る後、 糸曳き棒を上昇させ て被検液状物を曳糸状態とし、 曳糸状態にある被検液状物が切断し被検液状 物が試料受皿内に戻つて試料受皿内の被検液状物の頂部の直上を通る光軸が 受光器によって検知されるまでの糸曳き棒の上昇変位量を測定する液状物の 曳糸性測定方法である。  According to the invention described in claim 12, the stringer is lowered at a given speed toward the test liquid in the sample pan, and the light passing just above the top of the test liquid in the sample pan. When the lower end of the threading rod interrupts the shaft, the lowering of the threading rod is stopped, and the lower end of the threading rod is brought into contact with the liquid to be tested. Thereafter, the threading rod is raised. The test liquid is put into a spinning state, the test liquid in the spinning state is cut, the test liquid returns to the sample pan, and the optical axis passing just above the top of the test liquid in the sample pan is This is a method for measuring the spinnability of a liquid material, which measures the amount of upward displacement of a stringer until it is detected by a light receiver.
請求項 1 3に記載の発明は、 試料受皿内の被検液状物に指向して所与の速 度で糸曳き棒を降下せしめ、 試料受皿内の被検液状物の頂部の直上を通る光 軸を糸曳き棒下端部が遮断したときに前記糸曳き棒の降下を停止させるとと もに糸曳き棒下端部を被検液状物に接触させ、 然る後、 糸曳き棒を上昇させ て被検液状物を曳糸状態とし、 曳糸状態にある被検液状物が切断し、 上下方 向において複数箇配設された上方の光センサ一の何れかの光軸が受光器によ つて検知されたときまでの糸引き棒の上昇変位量を測定する液状物の曳糸性 測定方法である。  According to the invention described in claim 13, the stringer is lowered at a given speed in a direction directed toward the test liquid in the sample pan, and the light passing directly above the top of the test liquid in the sample pan is received. When the lower end of the threading rod interrupts the shaft, the lowering of the threading rod is stopped, and the lower end of the threading rod is brought into contact with the liquid to be tested. Thereafter, the threading rod is raised. The test liquid is set in a spinning state, the test liquid in the spinning state is cut, and one of the optical axes of the upper optical sensors arranged in a plurality of upper and lower directions is detected by a light receiver. This is a method of measuring the spinnability of a liquid material, which measures the amount of upward displacement of a stringing rod until it is detected.
請求項 1 4に記載の発明は、 被検液状物の曳糸性測定に先立ち、 糸曳き棒 を搭載している保持具を一定の距離降下せしめ、 次いで、 一定の距離上昇せ しめてその間に所与の下降、 上昇速度となるようフィードバック制御を行う ようにした請求項 1 2又は請求項 1 3に記載の液状物の曳糸性測定方法であ る。 請求項 1 5に記載の発明は、 被検液状物の曳糸性測定に先立ち、 糸曳き棒 を降下させてその下端部を被検液状物に接触させて湿潤状態としておく、 請 求項 1 2乃至請求項 1 4何れかに記載の液状物の曳糸性測定方法である。 こ の発明によれば、 繰り返し測定を行うときに、 糸曳き棒下端部の表面性状に 起因する測定値のばらっきをなくすことができる。 In the invention according to claim 14, prior to the measurement of the spinnability of the test liquid, the holder on which the stringing rod is mounted is lowered for a certain distance, and then is raised for a certain distance, and then the position is increased. The spinnability measurement method for a liquid material according to claim 12 or claim 13, wherein feedback control is performed so as to attain a lowering and increasing speed of the application. The invention according to claim 15 is characterized in that, prior to the measurement of the spinnability of the test liquid, the stringing rod is lowered to bring the lower end portion into contact with the test liquid to be in a wet state. A method for measuring the spinnability of a liquid material according to any one of claims 2 to 14. According to the present invention, it is possible to eliminate the dispersion of measured values due to the surface properties of the lower end of the stringing rod when performing repeated measurements.
請求項 1 6に記載の発明は、 試料受皿に、 試料壷下端部のチューブ、 スリ ヅト、 およびオリフィスの何れかを接触させた状態で一定量の被検液状物を 試料壷に貯留し、 次いで、 試料壷が付設されている糸曳き棒を上昇せしめて 試料壷下端部のチューブ、 スリット、 およびォリフィスの何れかから被検液 状物を流下させ、 流下する被検液状物の先端が途切れ液滴状態となるまでの 曳糸長さを測定するようにした液状物の曳糸性測定方法である。  In the invention according to claim 16, a fixed amount of the test liquid is stored in the sample pot while any one of the tube, slit, and orifice at the lower end of the sample pot is in contact with the sample pan. Next, raise the stringing rod provided with the sample jar to let the sample liquid flow down from one of the tube, slit, and orifice at the lower end of the sample jar, and the tip of the sample liquid flowing down is interrupted. This is a method for measuring the spinnability of a liquid material, which measures the spinning length until a droplet is formed.
請求項 1 7に記載の発明は、 試料受皿に、 試料壷下端部の 'チューブ、 スリ ヅト、 およびオリフィスの何れかを接触させた状態で一定量の被検液状物を 試料壷に貯留し、 次いで、 試料壷が付設されている糸曳き棒を上昇せしめて 試料壷下端部のチューブ、 スリヅト、 およびォリフィスの何れかから被検液 状物を流下させ、 試料壷内の被検液状物が流出し終わるまでの時間を測定す るようにした液状物の曳糸性測定方法である。  The invention according to claim 17 is to store a fixed amount of the test liquid in the sample container while any one of the tube, slit, and orifice at the lower end of the sample container is in contact with the sample pan. Then, raise the stringing rod provided with the sample jar and let the sample liquid flow down from one of the tube, slit, and orifice at the lower end of the sample jar, and the sample liquid in the sample jar is removed. This is a method for measuring the spinnability of a liquid material, which measures the time until the spill is completed.
請求項 1 8に記載の発明は、 1回目の測定における被検液状物の曳糸長さ を基準値とし、 曳糸長さが該基準値のある割合となるまでの時間又は測定回 数を検出するようにした液状物の曳糸性測定方法である。 この発明によると きは、 被検液状物の曳糸性をパラメ一夕として液状物の凝固性を測定するこ とができる。  The invention according to claim 18 is characterized in that the spinning length of the test liquid in the first measurement is a reference value, and the time or the number of measurements until the spinning length reaches a certain ratio of the reference value is determined. This is a method for measuring the spinnability of a liquid material to be detected. According to the present invention, it is possible to measure the coagulability of the liquid material with the spinnability of the test liquid material as a parameter.
請求項 1 9に記載の発明は、 糸曳き棒の上昇距離を、 被検液状物が切断し ない際限内の一定値として試料受皿における被検液状物の曳糸性測定を繰り 返し、 前記一定の糸曳き棒上昇距離内において被検液状物が切断するまでの 時間又は測定回数を検出するようにした液状物の曳糸性測定方法である。 こ の発明による場合も、 被検液状物の曳糸性をパラメ一夕として液状物の凝固 性を測定することができる。 請求項 2 0に記載の発明は、 糸曳き棒を一定距離試料受皿から上昇させて その状態で保持し、 被検液状物の電気伝導度の経時変化を検出するようにし た液状物の曳糸性測定方法である。 この発明によるときは、 被検液状物の曳 糸性をパラメ一夕として液状物の揮発性を測定することができる。 図面の簡単な説明 The invention according to claim 19 is characterized in that the threading property of the test liquid in the sample pan is repeatedly measured by setting the rising distance of the stringing rod to a constant value within a limit at which the test liquid does not cut, and This is a method for measuring the spinnability of a liquid material in which the time or the number of measurements until the test liquid material is cut within the lifting distance of the stringing rod is detected. Also in the case of this invention, it is possible to measure the coagulability of the liquid material by setting the spinnability of the test liquid material as a parameter. The invention according to claim 20 is a spinning line for a liquid material, wherein the stringing rod is lifted up from the sample pan for a fixed distance and held in that state, and a change with time in the electrical conductivity of the test liquid material is detected. It is a method of measuring sex. According to the present invention, the volatility of the liquid material can be measured with the spinnability of the test liquid material as a parameter. BRIEF DESCRIPTION OF THE FIGURES
図 1は、 本発明の一実施例に係る液状物の曳糸性測定装置を示す模式図で ある。  FIG. 1 is a schematic view showing an apparatus for measuring the spinnability of a liquid material according to one embodiment of the present invention.
図 2は、 本発明の一実施例に係る液状物の曳糸性測定装置を用いて液状物 の曳糸長さを測定するときの、 測定開始時点の試料受皿、 試料、 糸曳き棒、 光軸 o aの位置を示す正面図である。  FIG. 2 shows a sample tray, a sample, a stringer, and a light at the start of measurement when measuring the spinning length of a liquid using the liquid spinnability measuring device according to one embodiment of the present invention. It is a front view showing the position of axis oa.
図 3は、 糸曳き棒が下降してきて、 その下端部が試料に接触したときの状 態を示す正面図である。  FIG. 3 is a front view showing a state in which the stringer has descended and its lower end has come into contact with the sample.
図 4は、 被検液状物 (試料) の曳糸状態を示す正面図である。  FIG. 4 is a front view showing the spinning state of the test liquid (sample).
図 5は、 曳糸状態にある試料が切断された瞬間の状態を示す正面図である o  Fig. 5 is a front view showing the state at the moment when the sample in the spinning state is cut.o
図 6は、 切断後、 試料が試料受皿に復元した状態を示す正面図である。 図 7は、 本発明の他の実施形態における光センサ一の配置の一例を示す正 面図である。  FIG. 6 is a front view showing a state in which the sample has been restored to the sample pan after cutting. FIG. 7 is a front view showing an example of the arrangement of the optical sensor according to another embodiment of the present invention.
図 8は、 本発明の液状物の曳糸性測定装置における糸曳き棒下端部形状の 他の実施例を示す正面図である。  FIG. 8 is a front view showing another example of the shape of the lower end portion of the stringing rod in the liquid matter stringiness measuring device of the present invention.
図 9は、 本発明の液状物の曳糸性測定装置における試料受皿の他の実施例 を示す正面図である。  FIG. 9 is a front view showing another embodiment of the sample tray in the liquid spinnability measuring device of the present invention.
図 1 0は、 本発明の液状物の曳糸性測定装置における、 糸曳き棒下端部に 付設される試料掬い取りフック部の一実施例を示す正面図である。  FIG. 10 is a front view showing an embodiment of a sample scooping hook portion attached to the lower end of a stringing rod in the liquid matter spinnability measuring device of the present invention.
図 1 1は、 本発明の液状物の曳糸性測定装置における、 糸曳き棒下端部に 付設される試料壷の一実施例を示す正面図である。  FIG. 11 is a front view showing an embodiment of a sample pot attached to the lower end of a stringing rod in the liquid matter stringiness measuring device of the present invention.
図 1 2は、 本発明の液状物の曳糸性測定装置における、 試料流下方式用糸 曳き棒の一実施例を示す正面図である。 FIG. 12 shows a sample flow-through type yarn in the liquid matter spinnability measuring device of the present invention. It is a front view which shows one Example of a tow bar.
図 1 3は、 本発明の液状物の曳糸性測定装置及び曳糸性測定方法による測 定結果と、 シリンダ一ゲージによる実測値との対応関係を示すグラフである  FIG. 13 is a graph showing the correspondence between the measurement results obtained by the liquid material spinnability measuring device and spinnability measuring method of the present invention and the measured values measured by a single cylinder gauge.
発明を実施するための最良の形態 BEST MODE FOR CARRYING OUT THE INVENTION
以下、 本発明をその好ましい実施形態に則して説明する。  Hereinafter, the present invention will be described based on preferred embodiments.
本発明は、 被検液状物の化学的組成、 p Hといった化学的条件や温度とい つた物理的条件を規定した上で、 被検液状物の曳糸性を、 曳糸長さ、 荷重、 測定値の経時変化における時間又は測定回数、 電気伝導度といつた測定ノ ラ メータを以て計測するものである。 また、 たとえば唾液がねばねばするとい うような患者から感覚的に表現されるときの唾液といった被検液状物や、 血 液といった凝固性を有する被検液状物の物性をそれに適した曳糸性測定手段 で測定し、 被検液状物 (試料) 間の相対比較を行うことによって、 たとえば 人の健康状態の診断や産業分野、 食品分野等における品質管理、 新製品の開 発のためのデ一夕とすることができる。 さらに、 被検液状物の粘性、 弾性、 粘弾性の発現としての曳糸性を測定する。  The present invention defines the chemical composition of the test liquid, the chemical conditions such as pH, and physical conditions such as temperature, and determines the spinnability of the test liquid by measuring the spinning length, load, and measurement. It measures the time or the number of measurements in the change of the value over time, the electrical conductivity, and the measurement parameter. In addition, for example, when the patient feels that the saliva is sticky, the physical properties of the test liquid such as saliva and the coagulable test liquid such as blood are measured for spinnability. By performing relative measurements between test liquids (samples), it can be used for diagnosis of human health, quality control in the industrial and food fields, and development of new products for development. It can be. In addition, the spinnability of the test liquid is measured as the development of viscosity, elasticity, and viscoelasticity.
実施例 1  Example 1
図 1に、 本発明の一実施例に係る液状物の曳糸性測定装置を示す。 図 2乃 至図 6に、 本発明の一実施形態に係る曳糸性測定プロセスを示す。  FIG. 1 shows an apparatus for measuring the spinnability of a liquid material according to one embodiment of the present invention. 2 to 6 show a spinnability measuring process according to an embodiment of the present invention.
図 1において、 1はモ一夕一であって、 歯車列 2を介して昇降用ねじ軸 3 を正逆回転させる。 4は昇降テーブルであり、 内設されている雌ねじが昇降 用ねじ軸 3と螺合して、 昇降用ねじ軸 3の正逆回転によって昇降する。 この 実施例においては、 昇降テ一ブル 4は 5 mm/ s〜2 O mm/ sの速度範囲 内で昇降する。 5は保持具であって、 昇降テーブル 4に固定されるとともに 糸曳き棒 6を着脱自在に嵌装している。 これらモー夕一 1、 歯車列 2、 昇降 用ねじ軸 3、 昇降テーブル 4、 保持具 5、 およびモ一夕一 1の回転速度制御 系によって、 糸曳き棒 6の昇降手段が構成される。 糸曳き棒 6は、 その下端部が被検液状物 (試料) 8に接し、 上昇して試料 が糸曳き状態となり切断するまでの曳糸長さを検出すべく機能する。 糸曳き 棒 6の下端部は、 発明者らの知見によれば、 被検液状物 (試料) 8の曳糸長 さ測定に先立って、 試料によって湿潤状態にしておくことが好ましくまた、 下端部を湿潤状態にした試料の表面張力による盛り上がり頂点が糸曳き棒 6 下端部横断面中心に存在することが、 高精度の曳糸性測定にとって好ましい 。 而して、 糸曳き棒 6下端部形状を、 フラット状、 凸球面状、 凸円錐状、 凸 角錐状、 球面状先端部を有する凸角錐状、 凹球面状、 凹円錐状、 凹角錐状ま たは、 図 8に示す、 直径方向に一文字状に延在する凸条または凹溝、 および 直径方向に十文字状に延在する凸条または凹溝の何れかの形状とすることが 好ましい。 In FIG. 1, reference numeral 1 denotes a motor for rotating a vertically moving screw shaft 3 through a gear train 2. Reference numeral 4 denotes an elevating table, in which an internal female screw is screwed with the elevating screw shaft 3, and the elevating table is moved up and down by forward and reverse rotation of the elevating screw shaft 3. In this embodiment, the lifting table 4 moves up and down within a speed range of 5 mm / s to 2 Omm / s. Reference numeral 5 denotes a holder, which is fixed to the elevating table 4 and has a stringer 6 detachably fitted thereto. The motor 1, the gear train 2, the lifting screw shaft 3, the lifting table 4, the holder 5, and the rotation speed control system of the motor 1 constitute lifting means of the stringing rod 6. The lower end of the stringing rod 6 comes into contact with the test liquid (sample) 8, and functions to detect the stringing length until the sample comes into a stringing state and is cut. According to the knowledge of the inventors, the lower end of the stringing rod 6 is preferably wetted with the sample prior to the measurement of the stringing length of the test liquid (sample) 8. It is preferable for a high-precision measurement of the spinnability that the peak of the swelling due to the surface tension of the sample in a wet state exists in the center of the cross section of the lower end of the stringing rod 6. Thus, the lower end of the stringing rod 6 can be flat, convex spherical, convex conical, convex pyramid, convex pyramid having a spherical tip, concave spherical, concave cone, concave pyramid. Alternatively, as shown in FIG. 8, it is preferable to use any one of a convex ridge or a concave groove extending in a diametrical direction and a convex ridge or a concave groove extending in a diametrical direction.
7は試料受皿であって、 浅い円筒状或いは逆円錐台状凹部が形成され、 こ の凹部に被検液状物 (試料) 8が、 所定量装入される。 試料受皿 7は、 たと えばステンレス鋼製である。 試料受皿 7の縦断面形状を浅い円筒状或いは逆 円錐台状凹部とすることによって、 試料 8の試料受皿 7の平面上における位 置の偏りを防止し得て試料 8の表面張力による盛り上がりの頂点が平面中心 に位置し、 高精度の測定を可能にするとともに、 試料 8収容量の目視判断を 容易にすることができる。 試料受皿 7として、 図 9に示すように、 上部平面 を有する円柱形のものを用いることもできる。  Reference numeral 7 denotes a sample receiving tray, which is formed with a shallow cylindrical or inverted truncated cone-shaped concave portion, into which a predetermined amount of a test liquid (sample) 8 is charged. The sample pan 7 is made of, for example, stainless steel. By making the vertical cross-sectional shape of the sample pan 7 a shallow cylindrical or inverted truncated conical recess, the position of the sample 8 on the plane of the sample pan 7 can be prevented from shifting, and the peak of the bulge due to the surface tension of the sample 8 can be prevented. Is located at the center of the plane, enabling high-precision measurement and facilitating visual judgment of the sample 8 capacity. As the sample pan 7, as shown in FIG. 9, a columnar shape having an upper flat surface can be used.
9は投光器、 1 0は受光器であり、 この一対の信号処理システムで透過型 光センサ一を構成する。 この実施形態にあっては、 図 2に示すように、 試料 受皿 7内の被検液状物 (試料) 8の直上を光軸 o a (optical axis) が水平 に通る如く一対の投光器 9と受光器 1 0が配設される。 この実施例において は、 0 . 0 1 mm ( 1 0 zm) の物体を検出し得る感知能力をもつ透過型光 センサ一を用いている。  Reference numeral 9 denotes a light emitter and 10 denotes a light receiver. The pair of signal processing systems constitute a transmission type optical sensor. In this embodiment, as shown in FIG. 2, a pair of a projector 9 and a receiver are arranged so that an optical axis oa (optical axis) passes directly above a test liquid (sample) 8 in a sample pan 7. 10 is provided. In this embodiment, a transmission type optical sensor having a sensing ability capable of detecting an object of 0.01 mm (10 zm) is used.
1 1は投受光器取付台であって、 投光器 9と受光器 1 0を支承している。 この実施形態にあっては、 投受光器取付台 1 1は光軸位置微調整ねじ 1 2に 螺合され、 光軸位置微調整ねじ 1 2の回転によって高精度下に透過型光セン サ一が昇降せしめられ、 光軸 o aの高さ方向における位置が調整される。 光 軸 o aの高さ方向における位置調整は、 光センサ一ュニットを支承している 投受光器取付台 1 1および試料受皿 7の何れか一方または双方を昇降せしめ る手段によって行うことができる。 Reference numeral 1 denotes an emitter / receiver mounting base, which supports the emitter 9 and the receiver 10. In this embodiment, the transmitter / receiver mounting base 11 is screwed into the optical axis position fine adjustment screw 12, and the transmission type optical sensor is highly precisely controlled by the rotation of the optical axis position fine adjustment screw 12. The sensor is raised and lowered, and the position of the optical axis oa in the height direction is adjusted. The position adjustment of the optical axis oa in the height direction can be performed by means for raising and lowering one or both of the emitter / receiver mounting base 11 supporting the optical sensor unit and the sample tray 7.
1 3はモーター駆動回路であり、 操作回路 1 4からの出力信号を入力され てモー夕一 1に、 保持具 5が固定されている昇降テーブル 4を上昇方向或い は下降方向へ駆動すべく電力を投入する。 モー夕一,駆動回路 1 3はまた、 曳 糸長さ測定回路 1 5からの信号によって操作回路 1 4を介して作動し、 モ一 夕一 1への電力を遮断する。 さらに、 モーター駆動回路 1 3は上限リミッタ 1 8および下限リミヅ夕 1 9からの信号によって作動し、 モ一夕一 1への電 力を遮断する。操作回路 1 4には、 保持具 5が固定されている昇降テーブル 4を上昇方向或いは下降方向へ駆動する駆動スィツチが設けられている。  Reference numeral 13 denotes a motor drive circuit, which receives an output signal from the operation circuit 14 and drives the lift table 4 to which the holder 5 is fixed in the motor direction 1 in the ascending or descending direction. Turn on the power. The motor 13 and the drive circuit 13 are also operated via the operation circuit 14 by a signal from the towing length measuring circuit 15 and cut off the power to the motor 11. Further, the motor drive circuit 13 is activated by signals from the upper limiter 18 and the lower limit 19 to cut off the power to the motor 11. The operation circuit 14 is provided with a drive switch for driving the elevating table 4 to which the holder 5 is fixed in an ascending or descending direction.
1 6は演算回路であり、 この実施形態においては、 モー夕一 1の回転速度 を制 Pする帰還 (フィードバック) 制御系を構成するとともに、 曳糸長さ測 定回路 1 5からの信号に基づいて、 糸曳き棒 6が上昇を開始して曳糸状態に ある試料 8が切断するまでの糸曳き棒 6の上昇変位量を演算算出し、 デイジ 夕ル表示器 1 7に表示すべく機能する。  Reference numeral 16 denotes an arithmetic circuit. In this embodiment, a feedback (feedback) control system for controlling the rotation speed of the motor 1 is formed, and a signal from the thread length measuring circuit 15 is used. Calculates the amount of displacement of the stringing rod 6 from when the stringing rod 6 starts to rise and the sample 8 in the stringing state is cut, and functions to display it on the digital display 17 .
発明者らの知見によれば、 試料 8の曳糸性測定においては、 糸曳き棒 6の 上昇速度が測定精度に大きく影響する。 そこで本発明においては、 上記のよ うに、 モータ一 1の回転速度を制御する帰還 (フィードノ ヅク)制御系を、 液状物の曳糸性測定装置に組み込んでいる。 この帰還制御系は、 この実施例 においては、 次のように構成されている。 即ち、 外周面の周方向に所定間隔 で黒白のコントラストが形成された反射円盤 2 0に回帰反射型フォトイン夕 ラブ夕から赤外線を投射し、 反射円盤 2 0の白色部分からの反射赤外線をフ イードバヅクパルスとして捉え、 この時間当たりパルス数を演算回路 1 6に 入力し、 所与の昇降速度を保持具 5に与えるモー夕一 1の回転速度目標値と 比較して偏差があればそれを消去すべく、 モー夕一 1への投入パルスにおけ る O N— O F Fの幅比率を変化させる操作量、 即ち PWM (pulse width mo 漏雇 44 According to the findings of the inventors, in the measurement of the spinnability of the sample 8, the ascending speed of the stringing rod 6 greatly affects the measurement accuracy. Therefore, in the present invention, as described above, the feedback (feed knock) control system for controlling the rotation speed of the motor 11 is incorporated in the liquid material spinnability measuring device. This feedback control system is configured as follows in this embodiment. That is, an infrared ray is projected from a retroreflective photoinjector onto a reflecting disk 20 having black-and-white contrast formed at predetermined intervals in the circumferential direction of the outer peripheral surface, and reflected infrared light from a white portion of the reflecting disk 20 is reflected. This pulse is regarded as an idle-back pulse, and the number of pulses per time is input to the arithmetic circuit 16, and if there is a deviation from the rotation speed target value of the motor 1 which gives the given lifting speed to the holder 5, the deviation is detected To change the ON-OFF width ratio in the input pulse to motor 1 Leakage 44
- 11 - dulation) パルス 2 3をモ一夕一駆動回路 1 3を介してモー夕一 1へ入力す る。 即ち、 パルス幅変調方式の速度制御を行っている。  -11-dulation) Pulse 23 is input to the motor 1 via the motor drive circuit 13. That is, the speed control of the pulse width modulation method is performed.
次に、 実施例 1の液状物の曳糸性測定装置の動作を説明する。 本発明にお いては、 試料 8の曳糸性測定に先立って、 個々の曳糸性測定装置について先 に説明した帰還制御系によるモ一夕一 1の回転速度制御を行って、 保持具 5 を所与の昇降速度で変位せしめるようにキャリブレーションしている。 これ は、 電圧の変動、 モ一夕一の個体差、 回転部分の摺動抵抗等に起因して、 保 持具 5の昇降速度が所与の値に安定するまでの時間がばらつく問題を解決す るためである。  Next, the operation of the liquid matter spinnability measuring device of the first embodiment will be described. In the present invention, prior to the measurement of the spinnability of the sample 8, the rotation speed control of each of the individual spinnability measuring devices is performed by the feedback control system described above, so that the holder 5 Is calibrated to be displaced at a given lifting speed. This solves the problem that the time required for the lifting / lowering speed of the holder 5 to stabilize to a given value varies due to voltage fluctuations, individual differences between motors, sliding resistance of rotating parts, etc. To do so.
即ち、 予め試料受皿 7内に被検液状物 (試料) 8を装入しておき、 糸曳き 棒 6の下端部が試料 8に接するまで一定変位量保持具 5を降下させ、 次いで 、 一定変位量上昇させる。 この過程で、 前記帰還制御を実施して保持具 5の 昇降速度を所与の目標値に収束させておく。個々の曳糸性測定装置について キヤリブレーシヨンを行った後に、 被検液状物 (試料) 8の曳糸性測定を実 施する。  That is, the test liquid (sample) 8 is charged in the sample receiving tray 7 in advance, the holder 5 is lowered until the lower end of the stringing rod 6 comes into contact with the sample 8, and then the constant displacement Increase the amount. In this process, the feedback control is performed to make the elevating speed of the holder 5 converge to a given target value. After carrying out calibration for each spinnability measuring device, the spinnability of the test liquid (sample) 8 is measured.
このキヤリブレ一シヨンの過程で糸曳き棒 6の下端部が湿潤状態となるの で、 実際の曳糸性測定に際して、 糸曳き棒 6の下端部が試料受皿 7内の被検 液状物 (試料) 8に接触したときに融合状態となり、 糸曳き棒 6下端部の表 面性状に起因する測定値のばらっきをなくすことができる。  During the calibration process, the lower end of the stringing rod 6 becomes wet because the lower end of the stringing rod 6 is in the sample pan 7 when measuring the actual stringiness. When it comes into contact with 8, it becomes a fusion state, and it is possible to eliminate the dispersion of measured values caused by the surface properties of the lower end of the stringing rod 6.
キヤリブレーションが終了した液状物の曳糸性測定装置を用いて、 試料受 皿 7内に被検液状物 (試料) 8を装入する。 次いで、 図 2に示すように、 試 料受皿 7或いは透過型光センサ一を昇降させて光軸 o a透過の存否によって 、 試料受皿 7内で表面張力によって盛り上がり状態となっている試料 8の頭 頂部の高さ方向における位置を検出し、 その位置よりも 1 0 zm程度高い位 置を水平に光軸 o aが通るように、 光軸位置調整ねじ 1 2によって光センサ ーをセヅ卜する。  Using the apparatus for measuring the spinnability of a liquid that has been calibrated, load the test liquid (sample) 8 into the sample pan 7. Next, as shown in FIG. 2, the sample pan 7 or the transmission type optical sensor 1 is moved up and down to determine whether or not the optical axis oa is transmitted. The optical sensor is set by the optical axis position adjusting screw 12 so that the optical axis oa passes horizontally at a position about 10 zm higher than that position in the height direction.
この状態で、 図 3に示すように、 糸曳き棒 6を降下させて行きその下端部 が光軸 o aを遮断したとき (遮光検知) に、 糸曳き棒 6の下降停止信号が出 力され、 曳糸長さ測定回路 1 5、 操作回路 1 4、 およびモ一夕一駆動回路 1 3を経てモー夕一 1が停止せしめられる。 糸曳き棒 6は、 光センサ一による 遮光検知後も試料 8に接触するまで降下する。 この状態から糸曳き棒 6が上 昇する方向にモ一夕一 1が回転駆動され、 図 4に示すように、 所与の上昇速 度で糸曳き棒 6が上昇せしめられ、 被検液状物 (試料) 8は曳糸状態となる 。 図 4に示すように、 曳糸状態にある被検液状物 (試料) 8によって、 光軸 o aは遮断された状態となっている。 In this state, as shown in Fig. 3, when the line puller 6 is lowered and its lower end cuts off the optical axis oa (light blocking detection), a lowering stop signal of the line puller 6 is output. Then, the motor 1 is stopped via the thread length measuring circuit 15, the operating circuit 14, and the motor driving circuit 13. The stringing rod 6 descends until it comes into contact with the sample 8 even after the light sensor 1 detects light shielding. In this state, the motor 1 is driven to rotate in the direction in which the stringer 6 rises, and as shown in FIG. 4, the stringer 6 is raised at a given rising speed, and the test liquid (Sample) 8 is in the spinning state. As shown in Fig. 4, the optical axis oa is shut off by the test liquid (sample) 8 in the spinning state.
伸びた試料 8は、 図 5に示すように、 粘性に対応する曳糸長さとなったと きに切断される。 切断後、 試料 8は、 図 6に示すように、 瞬時に試料受皿 7 に戻り再び光軸 o aが透過する状態となる。 光軸 o aの遮断から再び受光器 1 0が光の検出信号を出力した瞬間までの糸曳き棒 6の上昇変位量が、 その 被検液状物 (試料) 8の曳糸長さ (粘性のパラメ一夕) となる。  The stretched sample 8 is cut when the string length corresponding to the viscosity is reached, as shown in FIG. After cutting, the sample 8 returns to the sample pan 7 instantaneously as shown in FIG. 6, and the optical axis o a is again transmitted. The amount of upward displacement of the stringing rod 6 from the interruption of the optical axis oa to the moment when the photodetector 10 outputs a light detection signal again depends on the stringing length of the test liquid (sample) 8 (viscosity parameter). Overnight).
この実施形態においては、 被検液状物 (試料) 8の粘性に対応して、 曳糸 状態が切断された瞬間から、 試料 8が図 6に示すような復元状態となるまで の時間に差違があることを考慮し、 予め実験により、 各種試料の粘性に対応 する、 曳糸状態が切断された瞬間から復元状態となるまでの時間デ一夕を採 取しておき、 差違を被検液状物 (試料) 8の液質、 粘性毎にソフトウェアに よって補正するようにしている。  In this embodiment, according to the viscosity of the test liquid (sample) 8, there is a difference in the time from the moment when the stringing state is cut to the time when the sample 8 returns to the restored state as shown in FIG. In consideration of the fact that there is a certain amount of time from the moment when the threading state is cut to the time when the stringing state returns to the restored state corresponding to the viscosity of various samples by experiments in advance, (Sample) Correction is made by software for each liquid quality and viscosity of 8.
而して、 光センサ一の遮光検出信号および受光器 1 0が再び光軸 o aを検 出した信号が曳糸長さ測定回路 1 5を経て、 それに対応するモ一夕一 1の駆 動〇N— O F F信号としてモー夕一駆動回路 1 3を介して演算回路 1 6に入 力され、 光センサ一が遮光を検知したときから受光器 1 0が再び光軸 o aを 検知したときまでのモ一夕一 1の回転数 (パルス数) をカウントするととも に、 これを糸曳き棒 6の上昇変位量に変換 (演算算出) して、 ディジタル表 示器 1 7に出力する。  Thus, the light-blocking detection signal of the optical sensor 1 and the signal of the optical receiver 10 detecting the optical axis oa again pass through the thread length measuring circuit 15 and the corresponding motor 1 is driven. An N-OFF signal is input to the arithmetic circuit 16 via the motor drive circuit 13 via the motor drive circuit 13 and the motor from when the light sensor 1 detects light blocking to when the light receiver 10 detects the optical axis oa again. The number of rotations (number of pulses) per night is counted, and this is converted (calculated) into the amount of upward displacement of the stringing rod 6 and output to the digital display 17.
実施例 2  Example 2
被検液状物 (試料) 8がゲル状の粘稠性に富むものである場合、 曳糸状態 にある試料 8の切断から、 図 6に示すような測定開始前の状態に復元し難い か或いはばらつきが大きい。 このような場合は、 曳糸状態にある試料 8の切 断の瞬間そのものの位置を直接的に検出する必要がある。 When the test liquid (sample) 8 is a gel-like highly viscous material, it is difficult to recover from the cutting of the sample 8 in the string state to the state before the start of measurement as shown in Fig. 6. Or the variation is large. In such a case, it is necessary to directly detect the position of the moment of cutting of the sample 8 in the spinning state.
そこでこの実施例においては、 図 1および図 7に示すように、 試料 8の延 伸 (高さ) 方向において複数箇の光センサ一を配設し、 曳糸状態にある試料 8の切断位置 (高さ) を直接的に検出できるようにしている。 曳糸性測定の 初期状態 (試料受皿 7内の被検液状物 (試料) 8の頭頂部位置の確認後その 1 程度上部を光軸 o aが通るように光センサー (基点光センサー) が セヅトされた状態) における基点光センサ一の遮光検知から糸曳き棒 6上昇 後、 配設された複数箇の光センサ一のうちの光軸 o aを検出した上方の光セ ンサ一と基点光センサーの間隔が、 その試料 8の曳糸長さとなる。基点光セ ンサ一の上方の光センサ一の配置数およびその高さ方向における位置は、 対 象とする被検液状物 (試料) 8の物性に対応して決めるとよい。  Therefore, in this embodiment, as shown in FIGS. 1 and 7, a plurality of optical sensors 1 are arranged in the elongating (height) direction of the sample 8, and the cutting position ( Height) can be detected directly. Initial state of spinnability measurement (After confirming the position of the top of liquid sample (sample) 8 in sample pan 7, the optical sensor (base point optical sensor) is set so that optical axis oa passes about one part above. The distance between the upper optical sensor that detected the optical axis oa of the plurality of optical sensors installed and the base optical sensor after ascending the stringer 6 from the light blocking detection of the base optical sensor Is the spinning length of Sample 8. The number of optical sensors disposed above the base optical sensor and the position in the height direction may be determined in accordance with the physical properties of the target liquid material (sample) 8 to be measured.
実施例 3  Example 3
これまで説明した実施例は、 被検液状物 (試料) 8の曳糸長さ測定開始時 点における試料 8の頭頂部およぴ曳糸状態にある試料 8の切断時点の高さ方 向における位置を確認する光学的検出手段を透過型光センサ一とする実施例 である。 しかし、 本発明はこれに限るものではなく、 エリアセンサ一、 たと えば C C Dカメラゃレ一ザ一センサ一を用いる、 液状物の曳糸性測定の開始 時点および曳糸状態にある試料 8の切断時点の高さ方向における位置を確認 する光学的検出手段を採ることもできる。 さらに、 画像処理手段を用いる、 液状物の曳糸性測定の開始時点および曳糸状態にある試料 8の切断時点の高 さ方向における位置を確認する光学的検出手段を採ることもできる。  In the embodiments described so far, the liquid material (sample) 8 at the top of the sample 8 at the start of the measurement of the string length and the height direction at the time of cutting of the sample 8 in the state of the string are measured. This is an embodiment in which the optical detection means for confirming the position is a transmission type optical sensor. However, the present invention is not limited to this, and the cutting of the sample 8 in the state at the start of the spinning property measurement of the liquid material and the spinning state using an area sensor, for example, a CCD camera, a laser, and a sensor, is performed. Optical detection means for confirming the position in the height direction at the time can also be employed. Further, an optical detection means for confirming the position in the height direction at the time of the start of the measurement of the spinnability of the liquid material and the time of the cutting of the sample 8 in the spinning state, using an image processing means, may be employed.
実施例 4  Example 4
上記、 本発明の液状物の曳糸性測定装置およびそれを用いる曳糸性測定方 法の実施例においては、 光学的検出手段によって、 液状物の曳糸性測定の開 始時点および曳糸状態にある試料 8の切断時点の高さ方向における位置を確 認するようにしている。 しかし、 本発明においては、 前記確認手段として、 試料受皿 7または糸曳き棒 6に、 微小な荷重変動を感知する荷重測定器たと えば、 電子天秤等高度の分解能をもつ荷重測定器を装着し、 糸曳き棒 6が試 料 8に接触した瞬間および曳糸状態にある試料 8の切断時点の荷重変化を 0 . l mgの単位で検出し、 この検出信号をディジタルな処理信号として用い ることもできる。 In the above-described embodiment of the liquid material spinnability measuring apparatus and the spinnability measuring method using the same according to the present invention, the optical detection means detects the start time and the spinning state of the liquid material spinnability measurement. The position of the sample 8 in the height direction at the time of cutting was confirmed. However, in the present invention, as the confirmation means, a load measuring device that senses a small load variation on the sample pan 7 or the stringing rod 6 is described. For example, a load measuring device with a high resolution, such as an electronic balance, is installed, and the load change at the moment the stringer 6 comes into contact with the sample 8 and the cutting time of the sample 8 in the stringing state is 0.1 mg unit. The detection signal can be used as a digital processing signal.
上に述べた実施例における液状物の曳糸性測定方法は、 予め糸曳き棒 6下 端部を湿潤状態として、 曳糸状態にある被検液状物 (試料) 8の切断までの 曳糸長さを測定することを複数回繰り返し、 試料群内の平均値や分布状態な どを抽出するウエット試験法と、 糸曳き棒 6下端部を被検液状物 (試料) 8 で濡らすことなくドライな状態として曳糸長さを 1回測定するドライ試験法 とがある。 ゥェヅト試験法は、 粘性、 弾性、 表面張力、 粘着力をある程度以 上有する被検液状物 (試料) 8を測定対象とするのに適している。 ドライ試 験法は、 粘着力が強く弾性の低い被検液状物 (試料) 8を測定対象とするの に適している。  The method for measuring the spinnability of a liquid material in the above-described embodiment is as follows. The lower end of the stringing rod 6 is wetted in advance, and the spinning length up to the cutting of the test liquid material (sample) 8 in the spinning state. Wet measurement is repeated several times to extract the average value and distribution state in the sample group, etc., and the stringing rod 6 is dry without wetting the lower end with the test liquid (sample) 8. There is a dry test method in which the thread length is measured once as a condition. The gate test method is suitable for measuring a test liquid (sample) 8 having viscosity, elasticity, surface tension, and adhesive strength to some extent. The dry test method is suitable for measuring test liquids (samples) 8 having high adhesive strength and low elasticity.
実施例 5  Example 5
図 1 0に、 本発明の他の実施例に係る液状物の曳糸性測定装置を示す。 図 1乃至図 7におけると同じ符号は、 同じ構成要素である。 この実施例におけ る糸曳き棒 2 6は、 その下端部に掬い取りフック部 3 6を有している。 掬い 取りフック部 3 6は、 その先端部が試料受皿 7内の被検液状物 (試料) 8に 挿入され、 糸曳き棒 2 6の上昇によって試料 8の所定量を掬い上げ、 曳糸状 態にある試料 8の切断までの曳糸長さを測定すべく機能する。 この実施例に 係る液状物の曳糸性測定装置は、 粘性、 弾性、 粘弾性、 表面張力、 粘着性が ともに低く流動性の高い被検液状物 (試料) 8を測定対象とするのに適して いる。 図 1 0において、 1 0 1は試料押さえであって、 平面二股状であり試 料受皿 7に固定される。 この試料押さえ 1 0 1によって、 被検液状物 (試料 ) 8の全量が掬い取りフック部 3 6によって持ち上げられるのを防止する。 掬い取りフヅク部 3 6先端部の断面形状は、 逆三角形、 方形、 円形、 スプ一 ン形状など被検液状物 (試料) 8の物性に応じて適宜選択することができる 実施例 6 FIG. 10 shows an apparatus for measuring the spinnability of a liquid material according to another embodiment of the present invention. 1 to 7 are the same components. The stringer 26 in this embodiment has a scooping hook 36 at the lower end thereof. The tip of the scooping hook portion 36 is inserted into the test liquid (sample) 8 in the sample pan 7, and a predetermined amount of the sample 8 is scooped up by the raising of the stringing rod 26 to form a string. It functions to measure the length of the string until the cutting of a certain sample 8. The device for measuring the spinnability of a liquid material according to this embodiment is suitable for measuring a liquid material (sample) 8 having low viscosity, elasticity, viscoelasticity, surface tension, and tackiness and high fluidity. ing. In FIG. 10, reference numeral 101 denotes a sample holder, which has a forked flat shape and is fixed to the sample pan 7. The sample holder 101 prevents the entire amount of the test liquid (sample) 8 from being lifted by the scooping hook 36. The cross-sectional shape of the tip of the scooping hook 3 6 can be appropriately selected according to the physical properties of the test liquid (sample) 8 such as an inverted triangle, a square, a circle, and a spun shape. Example 6
図 1 1に、 本発明の他の実施例に係る液状物の曳糸性測定装置を示す。 図 1乃至図 7におけると同じ符号は、 同じ構成要素である。 この実施例におい ては、 被検液状物 (試料) 8は試料壶 4 8下端部に形成されているチューブ 4 8 1、 スリット 4 8 2、 およびオリフィス 4 8 3の何れかから流下する。 この実施例における液状物の曳糸性測定方法は、 予め、 試料壷 4 8下端部の チューブ 4 8 1、 スリット 4 8 2、 およびォリフィス 4 8 3の何れかを試料 受皿 7の底面に接触させておいて被検液状物 (試料) 8の所定量を試料壷 4 8に注入しまたは、 チューブ 4 8 1、 スリット 4 8 2、 およびオリフィス 4 8 3の何れかを細い棒状物で閉止しておいて被検液状物 (試料) 8の所定量 を試料壷 4 8に注入し測定開始と同時に開き、 糸曳き棒 6を上昇させて曳糸 状態にある試料 8の切断時点の高さ方向における位置を光学的検出手段で検 出する。 この実施例に係る液状物の曳糸性測定装置および曳糸性測定方法は 、 粘性、 弾性、 粘弾性、 表面張力、 粘着性がともに低く流動性の高い被検液 状物 (試料) 8を測定対象とするのに適している。 この試験法をフロー試験 法と称する。  FIG. 11 shows an apparatus for measuring the spinnability of a liquid material according to another embodiment of the present invention. 1 to 7 are the same components. In this embodiment, the test liquid (sample) 8 flows down from one of the tube 481, the slit 482, and the orifice 483 formed at the lower end of the sample # 48. In the method for measuring the spinnability of the liquid material in this example, one of the tube 481, the slit 482, and the orifice 483 at the lower end of the sample pot 48 is brought into contact with the bottom surface of the sample pan 7 in advance. Inject a predetermined amount of the test liquid (sample) 8 into the sample jar 48, or close one of the tube 481, slit 482, and orifice 483 with a thin rod. A predetermined amount of the test liquid (sample) 8 is injected into the sample pot 48, and opened at the same time as the measurement is started, and the stringer 6 is lifted to raise the string 8 in the height direction at the time of cutting. The position is detected by optical detection means. The apparatus for measuring the spinnability of a liquid material according to this embodiment and the method for measuring the spinnability include a test liquid (sample) 8 having low viscosity, elasticity, viscoelasticity, surface tension, and low adhesiveness and high fluidity. Suitable for measurement. This test method is called a flow test method.
実施例 7  Example 7
図 1 2に、 本発明の他の実施例に係る液状物の曳糸性測定装置を示す。 図 1乃至図 7におけると同じ符号は、 同じ構成要素である。 この実施例におい ては、 被検液状物 (試料) 8は糸曳き棒 6の横断面中心に穿設され下端部に 開口を有する流出孔 3 6 1から流下する。 被検液状物 (試料) 8はシリンジ 4 8或はスポィド 4 8によって貯留される。 この実施例における曳糸性測定 方法は、 予め、 流出孔 3 6 1の開口を試料受皿 7内底面に接触させておいて 被検液状物 (試料) 8の所定量を貯留しておき、 測定開始と同時にシリンジ のピストン或はスポイドを開き、 糸曳き棒 6を上昇させて曳糸状態にある試 料 8の切断時点の高さ方向における位置を光学的検出手段で検出する。 この 実施例に係る液状物の曳糸性測定装置および曳糸性測定方法も、 粘性、 弾性 、 粘弾性、 表面張力、 粘着性がともに低く流動性の高い被検液状物 (試料) 8を測定対象とするのに適している。 この試験法もフ口一試験法の一実施形 態である。 FIG. 12 shows an apparatus for measuring the spinnability of a liquid material according to another embodiment of the present invention. 1 to 7 are the same components. In this embodiment, the test liquid (sample) 8 flows down from an outflow hole 361 formed at the center of the cross section of the stringing rod 6 and having an opening at the lower end. The test liquid (sample) 8 is stored by the syringe 48 or the spike 48. The method of measuring the spinnability in this example is as follows. A predetermined amount of the test liquid (sample) 8 is stored by bringing the opening of the outflow hole 36 1 into contact with the inner bottom surface of the sample pan 7 in advance. Simultaneously with the start, the piston or spoiler of the syringe is opened, the stringing rod 6 is raised, and the position of the sample 8 in the stringing state in the height direction at the time of cutting is detected by optical detection means. The liquid material spinnability measuring device and the spinnability measuring method according to this embodiment are also low in viscosity, elasticity, viscoelasticity, surface tension, and tackiness, and have high fluidity. 8 is suitable for measurement. This test method is also an embodiment of the Fuchi-one test method.
実施例 8  Example 8
図 1乃至図 1 2に示す曳糸性測定装置を用いて被検液状物 (試料) 8の曳 糸長さの測定を複数回繰り返し、 糸曳き長さの変化量を測定する。 1回目の 測定結果を基準値とし、 基準値のある割合たとえば 5 0 %の糸曳き長さとな るまでの時間或は測定回数を被検液状物 (試料) 8の凝固性のパラメ一夕と する。  Using the spinnability measuring apparatus shown in FIGS. 1 to 12, the measurement of the stringing length of the test liquid (sample) 8 is repeated a plurality of times, and the amount of change in the stringing length is measured. Using the result of the first measurement as the reference value, the time until the stringing length reaches a certain percentage of the reference value, for example, 50% or the number of measurements is determined as the coagulation parameter of the test liquid (sample) 8. I do.
実施例 9  Example 9
図 1乃至図 1 2に示す曳糸性測定装置を用いて、 被検液状物 (試料) 8が 切断しない際限内で一定長さを設定しその範囲で糸曳き棒 6の上昇 ·下降を 繰り返し、 曳糸状態にある試料 8の切断時点までの時間或は上昇 ·下降繰り 返し回数を検出し、 これを被検液状物 (試料) 8の凝固性のパラメ一夕とす る。  Using the spinnability measuring device shown in Fig. 1 to Fig. 12, a certain length is set within the limit where the test liquid (sample) 8 is not cut, and the stringer 6 is repeatedly moved up and down within that range. Then, the time until cutting of the sample 8 in the spinning state or the number of repetitions of ascending and descending is detected, and this is regarded as a parameter of the coagulability of the test liquid (sample) 8.
実施例 1 0  Example 10
図 1乃至図 1 2に示す曳糸性測定装置を用いて、 被検液状物 (試料) 8が 切断しない際限内で一定長さを設定しその範囲で糸曳き棒 6を上昇させて保 持し、 被検液状物 (試料) 8の電気伝導度の経時変ィ匕を測定する。 この測定 値を被検液状物 (試料) 8の揮発性のパラメ一夕とする。 この測定を行うと きは、 糸曳き棒 6と試料受皿 7間に電圧を印加する装置を付加する必要があ る。  Using the spinnability measuring device shown in Fig. 1 to Fig. 12, a certain length is set within the limit where the test liquid (sample) 8 is not cut, and the stringing rod 6 is raised and held within that range. Then, the electrical conductivity of the test liquid (sample) 8 is measured with time. This measured value is used as the volatile parameter of the test liquid (sample) 8. When performing this measurement, it is necessary to add a device for applying a voltage between the stringer 6 and the sample pan 7.
本発明の液状物の曳糸性測定装置およびそれを用いる曳糸性測定方法は上 記のように実施されるが、 液状物の曳糸性測定に影響を及ぼす因子は、 測定 時の環境の温度、 湿度、 被検液状物 (試料) の温度、 糸曳き棒の試料に接す る部分の表面性状 (表面粗さなど) 、 糸曳き棒の大きさ、 形状、 糸曳き棒の 上昇速度などである。被検液状物 (試料) に対応してこれら諸因子を総合的 に判断して規格化することが必要である。  The apparatus for measuring the spinnability of a liquid material of the present invention and the method for measuring the spinnability using the same are carried out as described above. Temperature, humidity, temperature of the test liquid (sample), surface properties (surface roughness, etc.) of the portion of the stringer in contact with the sample, size and shape of the stringer, speed of stringer rise, etc. It is. It is necessary to comprehensively judge and standardize these factors corresponding to the test liquid (sample).
図 1 3に、 本発明の液状物の曳糸性測定装置及び曳糸性測定方法による測 6544 FIG. 13 shows the measurement of the liquid material according to the present invention by the spinnability measuring apparatus and spinnability measuring method. 6544
- 17 - 定結果と、 シリンダーゲージによる実測値との対応関係を示す。 図 1 3から 明らかなように、 きわめてよい対応関係を示している。  -17-Shows the correspondence between the measurement result and the actual value measured by the cylinder gauge. As is evident from Figure 13, it shows a very good correspondence.
本発明の液状物の曳糸性測定装置及び曳糸性測定方法が対象とし得る液状 物は、 唾液のほか尿、 鼻汁、 痰など医療分野における液状物のほか、 油脂、 インク、 塗料など産業分野で取り扱われる液状物やドレヅシング、 ミルクな ど食品分野における液状物さらには、 ゲル、 ェマルジヨンなど曳糸 1·生を有す る液状物やペースト状のものを全て対象とし得る。  The liquid substances which can be targeted by the spinnability measuring device and spinnability measuring method of the present invention include liquid substances in the medical field such as saliva, urine, nasal discharge, and sputum, as well as oils, fats, inks, and paints in addition to saliva. Liquids in the food field, such as liquids, dressings, milk, etc., which are handled in Japan, as well as liquids and pastes that have a drawstring, such as gels and emulsions, can be targeted.
請求項 1、 請求項 2、 請求項 1 2、 および請求項 1 3に記載の発明によれ ば、 曳糸性を有する液状物の粘性を、 液状物が導電性を有すると否とに拘ら ず高い精度下に、 測定者の個人差を生じることなく測定することができる。 また、 本発明の液状物の曳糸性測定装置及び曳糸性測定方法によれば、 可及 的に少量の試料での自動測定が可能であり、 測定結果はディジタルに表示さ れるから、 針の位置を読む等の測定誤差を生じやすい因子を排除できる。 さ らに、 糸曳き棒は保持具に着脱自在に嵌装されていて装置の組み立てが簡単 であり、 糸曳き棒の洗浄も容易に行える。  According to the invention described in claim 1, claim 2, claim 12, and claim 13, the viscosity of the liquid having spinnability is determined regardless of whether the liquid has conductivity. Measurement can be performed with high accuracy without causing individual differences among the measurers. Further, according to the spinnability measuring device and spinnability measuring method for a liquid material of the present invention, an automatic measurement can be performed with as small a sample as possible, and the measurement result is digitally displayed. Factors that tend to cause measurement errors, such as reading the position, can be eliminated. Furthermore, the stringer is detachably fitted to the holder, so that the assembly of the device is simple and the stringer can be easily cleaned.
請求項 3に記載の発明によるときは、 測定の度毎に試料受皿内の被検液状 物 (試料) の盛り上がり頭頂部を高精度下に検出できるから、 液状物の曳糸 性測定をより精度高く行うことができる。  According to the third aspect of the present invention, the swelling of the test liquid (sample) in the sample pan can be detected with high accuracy at every measurement, so that the spinnability of the liquid can be measured more accurately. Can be done higher.
請求項 4に記載の発明によれば、 C C Dカメラ、 レーザ一センサ一等のェ リァセンサ一或は画像処理技術を用いて液状物の曳糸性測定を行うことがで ぎる。  According to the invention described in claim 4, it is possible to measure the spinnability of the liquid material by using an error sensor such as a CCD camera, a laser sensor, or the like, or an image processing technique.
請求項 5に記載の発明によるときは、 糸曳き棒および Zまたは試料受皿に ロードセルといつた荷重測定器を装着することによって、 液状物の曳糸性測 定を行うことができる。  According to the invention described in claim 5, the spinning property of the liquid material can be measured by attaching a load measuring device such as a load cell to the stringing rod and Z or the sample pan.
請求項 6に記載の発明によれば、 糸曳き棒下端部を湿潤状態とした試料頭 頂部位置の、 糸曳き棒横断面中心からのずれに起因する液状物の曳糸性測定 精度の低下を防止できる。  According to the invention as set forth in claim 6, it is possible to reduce the accuracy of measuring the spinnability of the liquid material due to the deviation of the top of the sample in which the lower end of the threading rod is in a wet state from the center of the cross section of the threading rod. Can be prevented.
請求項 8に記載の発明によるときは、 試料の粘性や弾性が比較的高く、 表 面張力が大きくて試料受皿に試料が一定の強度で付着し難く粘着性が劣る場 合であってかつ、 流動性が高い液状物の曳糸性を精度よく測定することがで ぎる。 According to the invention of claim 8, the viscosity and elasticity of the sample are relatively high, and In cases where the surface tension is large and the sample is difficult to adhere to the sample pan with a certain strength and the adhesiveness is poor, the spinnability of a liquid material with high fluidity can be accurately measured.
請求項 1 0、 請求項 1 1、 請求項 1 6、 および請求項 1 7に記載の発明に よれば、 試料の粘性や弾性が比較的高く、 表面張力が大きくて試料受皿に試 料が一定の強度で付着し難く粘着性が劣る場合であつてかつ、 流動性が高い 液状物の曳糸性を精度よく測定することができる。  According to the inventions described in Claims 10, 11, 16, and 17, the viscosity and elasticity of the sample are relatively high, the surface tension is large, and the sample is fixed on the sample pan. It is possible to measure the spinnability of a liquid material with high fluidity even when it is difficult to adhere with low strength and has poor adhesion.
請求項 1 4に記載の発明によるときは、 糸曳き棒の上昇速度のばらつきに 起因する液状物の曳糸性測定値のばらつきをなくすことができる。  According to the invention of claim 14, it is possible to eliminate the dispersion of the measured value of the stringiness of the liquid material caused by the dispersion of the lifting speed of the stringing rod.
請求項 1 5に記載の発明によれば、 繰り返し測定を行うときに、 糸曳き棒 下端部の表面性状に起因する液状物の曳糸性測定値のばらつきをなくすこと ができる。  According to the invention as set forth in claim 15, it is possible to eliminate variations in the measured value of the stringiness of the liquid material due to the surface properties of the lower end of the stringing rod when performing repeated measurements.
請求項 1 8および請求項 1 9に記載の発明によるときは、 液状物の曳糸性 をパラメ一夕として液状物の凝固性を測定することができる。  According to the inventions of claims 18 and 19, the spinnability of the liquid material can be measured as a parameter to measure the coagulability of the liquid material.
請求項 2 0に記載の発明によれば、 液状物の曳糸性をパラメ一夕として液 状物の揮発性を測定することができる。  According to the invention described in claim 20, the volatility of the liquid material can be measured by setting the spinnability of the liquid material as a parameter.

Claims

請求の範囲 The scope of the claims
1 . 被検液状物を収容する試料受皿と、 該試料受皿内の被検液状物にその下 端部が接触しその上昇によつて被検液状物の曳糸長さを検出すベく機能する 糸曳き棒と、 該糸曳き棒を所定の速度で昇降せしめる糸曳き棒昇降手段と、 被検液状物の曳糸長さ測定開始時点および曳糸状被検液状物の切断時点の位 置を確認する光学的手段とを有することを特徴とする液状物の曳糸性測定装 置。  1. A sample pan for containing the test liquid, and a function for detecting the length of the thread of the test liquid by the rise of the lower end of the sample pan in contact with the test liquid in the sample pan. A stringing rod, a stringing rod elevating means for raising and lowering the stringing rod at a predetermined speed, and a position for starting a measurement of a string length of the test liquid and a time for cutting the string-like test liquid. An apparatus for measuring the spinnability of a liquid material, comprising: an optical means for confirming the spinnability.
2 . 被検液状物の曳糸長さ測定開始時点および曳糸状被検液状物の切断時点 の位置を確認する光学的手段が、 糸曳き棒の昇降方向と交叉する方向に光を 発する投光器と該投光器からの光を受光する少なくとも一の光センサーであ る請求項 1に記載の液状物の曳糸性測定装置。  2. The optical means for confirming the position of the start of the measurement of the thread length of the test liquid and the cutting time of the test liquid is a light emitter that emits light in a direction crossing the vertical direction of the stringer. The liquid stringiness measuring device according to claim 1, wherein the device is at least one optical sensor that receives light from the light emitter.
3 . 試料受皿及び光センサ一の何れか一方または双方に、 糸曳き棒の昇降方 向における位置調整手段が付設されたものである請求項 1又は請求項 2に記 載の液状物の曳糸性測定装置。  3. The liquid thread described in claim 1 or claim 2, wherein one or both of the sample pan and the optical sensor is provided with a position adjusting means in a direction in which the stringing rod is raised and lowered. Sex measurement device.
4 . 被検液状物の曳糸長さ測定開始時点および曳糸状被検液状物の切断時点 の位置を確認する光学的手段が、 ェリァセンサ一又は画像処理装置である請 求項 1に記載の液状物の曳糸性測定装置。  4. The optical device according to claim 1, wherein the optical means for confirming the positions of the start of the measurement of the thread length of the test liquid and the cutting time of the spin-like test liquid is an error sensor or an image processing device. Equipment for measuring the spinnability of objects.
■ 5 . 被検液状物を収容する試料受皿と、 該試料受皿内の被検液状物にその下 端部が接触しその上昇によつて被検液状物の曳糸長さを検出すベく機能する 糸曳き棒と、 該糸曳き棒を所定の速度で昇降せしめる糸曳き棒昇降手段と、 被検液状物の曳糸長さ測定開始時点および曳糸状被検液状物の切断時点に糸 曳き棒又は試料受皿に負荷される力の変ィ匕を検出する荷重測定器を糸曳き棒 又は試料受皿に設けたことを特徴とする液状物の曳糸性測定装置。 ■ 5. The sample pan for containing the test liquid, and the lower end of the sample pan in contact with the test liquid in the sample pan. A function of a stringing rod that functions, a stringing rod elevating means for moving the stringing rod up and down at a predetermined speed, and a stringing operation at the start of the measurement of the stringing length of the test liquid and the cutting of the test string. A stringiness measuring device for a liquid material, wherein a load measuring device for detecting a change in a force applied to a rod or a sample pan is provided on the stringing rod or the sample pan.
6 . 糸曳き棒の下端部形状が、 フラット状、 凸球面状、 凸円錐状、 凸角錐状 、 球面状先端部を有する凸角錐状、 凹球面状、 凹円錐状、 凹角錐状、 直径方 向に一文字状に延在する凸条または凹溝、 および直径方向に十文字状に延在 する凸条または凹溝の何れかである請求項 1乃至請求項 5何れかに記載の液 状物の曳糸性測定装置。 6. The lower end of the stringing rod is flat, convex spherical, convex conical, convex pyramid, convex pyramid with spherical tip, concave spherical, concave cone, concave pyramid, diameter square. The liquid according to any one of claims 1 to 5, which is one of a convex ridge or a concave groove extending in a single character direction in the direction and a convex ridge or a concave groove extending in a cross shape in the diameter direction. Spinnability measuring device.
7 . 試料受皿が、 上部平面を有する円柱条体である請求項 1乃至請求項 6何 れかに記載の液状物の曳糸性測定装置。 7. The apparatus for measuring the spinnability of a liquid material according to any one of claims 1 to 6, wherein the sample pan is a cylindrical strip having an upper flat surface.
8 . 糸曳き棒が、 その下端部に試料受皿内の被検液状物を掬い取り上昇すベ く機能する掬い取りフック部をその下端部に付設したものである請求項 1乃 至請求項 7何れかに記載の液状物の曳糸性測定装置。  8. The stringing rod is provided with a scooping hook at the lower end thereof, which functions to scoop up and lift the test liquid in the sample pan at the lower end thereof. The apparatus for measuring the spinnability of a liquid material according to any one of the above.
9 . 試料受皿が、 被検液状物の全体が持ち上がらないように機能する試料押 さえ具を付設したものである請求項 1乃至請求項 8何れかに記載の液状物の 曳糸性測定装置。  9. The apparatus for measuring the spinnability of a liquid material according to any one of claims 1 to 8, wherein the sample pan is provided with a sample retainer that functions so as not to lift the entire test liquid material.
1 0 . 被検液状物を収容する試料受皿と、 その下端部にチューブ、 スリット 、 およびォリフィスの何れかが形成され前記試料受皿からの上昇によって該 チューブ、 スリット、 およびォリフィスの何れかから被検液状物を流下せし める試料壷を有し被検液状物の曳糸長さ検出すベく機能する、 揷通孔を有す る保持具に上下摺動自在に遊嵌される糸曳き棒と、 前記保持具を把持して該 糸曳き棒を所定の速度で昇降せしめる糸曳き棒昇降手段と、 被検液状物の曳 糸長さ測定開始時点および曳糸状被検液状物の切断時点の位置を確認する光 学的手段とを有することを特徴とする液状物の曳糸性測定装置。  10. A sample pan that contains the test liquid and a tube, slit, or orifice formed at the lower end of the sample pan. When the sample pan is lifted from the sample pan, the sample is inspected from any of the tube, slit, and orifice.試 料 A stringer that has a sample pot that allows the liquid to flow down and functions to detect the length of the thread of the test liquid. A rod; a stringing rod elevating means for gripping the holder and elevating and lowering the stringing rod at a predetermined speed; and a point in time at which the measurement of the string length of the test liquid is started and a point in time when the string-like liquid is cut. An optical device for confirming the position of a liquid material, the device for measuring the spinnability of a liquid material.
1 1 . 被検液状物を収容する試料受皿と、 該試料受皿からの上昇によってそ の下端部から被検液状物を流下せしめる流出孔を有し被検液状物の曳糸長さ 検出すべく機能する、 揷通孔を有する保持具に上下摺動自在に遊嵌される糸 曳き棒と、 前記保持具を把持して該糸引き棒を所定の速度で昇降せしめる糸 弓 (き棒昇降手段と、 被検液状物の曳糸長さ測定開始時点および曳糸状被検液 状物の切断時点の位置を確認する光学的手段とを有することを特徴とする液 状物の曳糸性測定装置。  1 1. A sample pan for containing the test liquid, and an outflow hole for letting the test liquid flow down from the lower end of the sample pan by ascending from the sample pan to detect the thread length of the test liquid. A thread puller bar that is slidably fitted up and down slidably in a holder having a through-hole, and a thread bow that grips the holder and raises and lowers the thread puller at a predetermined speed. And an optical means for confirming the positions of the starting point of the measurement of the thread length of the test liquid and the cutting time of the spinning test liquid. .
1 2 . 試料受皿内の被検液状物に指向して所与の速度で糸曳き棒を降下せし め、 試料受皿内の被検液状物の頂部の直上を通る光軸を糸曳き棒下端部が遮 断したときに前記糸曳き棒の降下を停止させるとともに糸曳き棒下端部を被 検液状物に接触させ、 然る後、 糸曳き棒を上昇させて被検液状物を曳糸状態 とし、 曳糸状態にある被検液状物が切断し被検液状物が試料受皿内に戻って 試料受皿内の被検液状物の頂部の直上を通る光軸が受光器によって検知され るまでの糸曳き棒の上昇変位量を測定することを特徴とする液状物の曳糸性 測定方法。 1 2. Lower the stringing rod at a given speed in a direction facing the sample liquid in the sample pan, and move the optical axis passing directly above the top of the sample liquid in the sample pan to the lower end of the stringing rod. When the section is interrupted, the lowering of the stringing rod is stopped, and the lower end of the stringing rod is brought into contact with the test liquid. Thereafter, the stringer is raised to bring the liquid to be tested into a stringy state. When the test liquid in the spinning state is cut and the test liquid returns to the sample pan, A method for measuring the spinnability of a liquid material, comprising measuring an amount of upward displacement of a stringing rod until an optical axis passing directly above a top of a test liquid material in a sample pan is detected by a light receiver.
1 3 . 試料受皿内の被検液状物に指向して所与の速度で糸曳き棒を降下せし め、 試料受皿内の被検液状物の頂部の直上を通る光軸を糸曳き棒下端部が遮 断したときに前記糸曳き棒の降下を停止させるとともに糸曳き棒下端部を被 検液状物に接触させ、 然る後、 糸曳き棒を上昇させて被検液状物を曳糸状態 とし、 曳糸状態にある被検液状物が切断し、 上下方向において複数箇配設さ れた上方の光センサ一の何れかの光軸が受光器によって検知されたときまで の糸曳き棒の上昇変位量を測定することを特徴とする液状物の曳糸性測定方 法。  13. Lower the stringing rod at a given speed in a direction facing the sample liquid in the sample pan, and move the optical axis passing directly above the top of the sample liquid in the sample pan to the lower end of the stringing rod. When the section is interrupted, the lowering of the stringing rod is stopped, and the lower end of the stringing rod is brought into contact with the test liquid. Thereafter, the stringer is raised to bring the liquid to be tested into a stringy state. The test liquid in the stringing state is cut, and the stringing rod is moved until one of the optical axes of the upper plurality of optical sensors arranged in the vertical direction is detected by the light receiver. A method for measuring the spinnability of a liquid material, which comprises measuring the amount of upward displacement.
1 4 . 被検液状物の曳糸性測定に先立ち、 糸曳き棒を搭載している保持具を 一定の距離降下せしめ、 次いで、 一定の距離上昇せしめてその間に所与の下 降、 上昇速度となるようフィードバヅク制御を行うようにした請求項 1 2又 は請求項 1 3に記載の液状物の曳糸性測定方法。  14 4. Prior to the measurement of the spinnability of the test liquid, lower the holder equipped with the stringing rod for a certain distance, and then raise it for a certain distance. 14. The spinnability measurement method for a liquid material according to claim 12, wherein feedback control is performed so as to satisfy the following.
1 5 . 被検液状物の曳糸性測定に先立ち、 糸曳き棒を降下させてその下端部 を被検液状物に接触させて湿潤状態としておく、 請求項 1 2乃至請求項 1 4 何れかに記載の液状物の曳糸性測定方法。  15. Prior to the measurement of the spinnability of the test liquid, the stringing rod is lowered and the lower end thereof is brought into contact with the test liquid to be in a wet state. 3. The method for measuring the spinnability of a liquid material according to item 1.
1 6 . 試料受皿に、 試料壷下端部のチューブ、 スリット、 およびオリフィス の何れかを接触させた状態で一定量の被検液状物を試料壷に貯留し、 次いで 1 6. A certain amount of the test liquid is stored in the sample pan while the tube, slit, or orifice at the lower end of the sample pan is in contact with the sample pan.
、 試料壷が付設されている糸曳き棒を上昇せしめて試料壷下端部のチューブ 、 スリヅト、 およぴォリフィスの何れかから被検液状物を流下させ、 流下す る被検液状物の先端が途切れ液滴状態となるまでの曳糸長さを測定するよう にしたことを特徴とする液状物の曳糸性測定方法。 Then, the stringer provided with the sample pot is raised, and the test liquid is allowed to flow down from one of the tubes, slits, and orifices at the lower end of the sample pot. A method for measuring the spinnability of a liquid material, wherein the spinning length until a broken droplet state is measured.
1 7 . 試料受皿に、 試料壷下端部のチューブ、 スリット、 およびォリフィス の何れかを接触させた状態で一定量の被検液状物を試料壷に貯留し、 次いで 、 試料壷が付設されている糸曳き棒を上昇せしめて試料壷下端部のチューブ 、 スリット、 およびオリフィスの何れかから被検液状物を流下させ、 試料壷 内の被検液状物が流出し終わるまでの時間を測定するようにしたことを特徴 とする液状物の曳糸性測定方法。 17. A fixed amount of the test liquid is stored in the sample pan with one of the tube, slit, and orifice at the lower end of the sample pan in contact with the sample pan, and then the sample pan is attached. Raise the stringing rod and let the test liquid flow down from one of the tube, slit, and orifice at the lower end of the sample pot. A method for measuring the spinnability of a liquid material, characterized in that the time until the liquid material to be tested in the liquid is completely discharged is measured.
1 8 . 1回目の測定における被検液状物の曳糸長さを基準値とし、 曳糸長さ が該基準値のある割合となるまでの時間又は測定回数を検出するようにした ことを特徴とする液状物の曳糸性測定方法。  18. The characteristic is that the thread length of the test liquid in the first measurement is used as a reference value, and the time or the number of measurements until the thread length reaches a certain ratio of the reference value is detected. A method for measuring the spinnability of a liquid material.
1 9 . 糸曳き棒の上昇距離を、 被検液状物が切断しない際限内の一定値とし て試料受皿における被検液状物の曳糸性測定を繰り返し、 前記一定の糸引き 棒上昇距離内において被検液状物が切断するまでの時間又は測定回数を検出 するようにしたことを特徴とする液状物の曳糸性測定方法。  1 9. Repeat the measurement of the stringiness of the test liquid in the sample pan by setting the lifting distance of the stringing rod to a constant value within the limit at which the test liquid does not cut. A method for measuring the spinnability of a liquid material, wherein the time until the test liquid material is cut or the number of measurements is detected.
2 0 . 糸曳き棒を一定距離試料受皿から上昇させてその状態で保持し、 被検 液状物の電気伝導度の経時変ィ匕を検出するようにしたことを特徴とする液状 物の曳糸性測定方法。  20. A stringer for liquids, characterized in that the stringer is lifted from the sample pan for a certain distance and held in that state to detect changes over time in the electrical conductivity of the test liquid. Sex measurement method.
PCT/JP2003/006544 2002-05-24 2003-05-26 Device for measuring stringiness of liquid material and stringiness measuring method WO2003100387A1 (en)

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JP2002071542A (en) * 2000-08-25 2002-03-08 Kao Corp Apparatus for measuring threading quantity

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