JPH0812143B2 - Method for making constant immersion depth of rotor and viscosity measuring device having the function - Google Patents

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a viscosity measuring method and a measuring device, in which a cylindrical measuring rotor of a rotary viscometer is inserted into a sample liquid sampled in a sample container such as a beaker. The present invention relates to an apparatus for continuously and automatically measuring the viscosity of a plurality of samples while keeping the immersion depth of the rotor in the sample solution constant.

[0002]

2. Description of the Related Art When handling liquid raw materials or products in all industrial fields including the petrochemical industry, synthetic chemical industry, pharmaceutical industry, food industry, paint and ink industry, the viscosity of the liquid is measured. By doing so, it is often the case that the suitability of raw materials, the suitability of processing steps, the quality of products, and the defects are judged. That is, quality control of materials, intermediate processes, and products is performed according to the viscosity of the liquids.

Conventionally, the sample liquid sampled is placed in a sample liquid container such as a beaker, and the height of the rotary viscometer is manually operated to adjust the immersion depth of the rotor in the liquid and the viscosity. Viscosity is measured by manually operating a meter.

First, the operating principle and structure of the rotary viscometer will be outlined. FIG. 3 is a diagram showing the operating principle of a single cylinder rotor type rotary viscometer which is currently most widely used.

In the figure, 1 is a motor with a reducer, 2 is an output shaft of the motor with a reducer 1, and a scale disk 3 is attached to the output shaft 2. An upper end of a spring 4 is fixedly attached to a shaft end 2'of an output shaft 2 extending below the scale disk 3, and a stem 5 of a rotor 7 is fixedly attached to a lower end of the spring 4. Further, a U-shaped pointer 8 extends laterally from the rotor stem 5 so that the scale engraved on the scale disk 3 can be read by the tip 8'of the pointer.

When the viscometer has stopped rotating, the fingertip 8'pointing finger indicates zero scale. On the other hand, when the rotor 7 is immersed in the sample liquid 6 and rotated, viscous resistance torque due to the viscosity of the sample liquid is generated in the rotor 7, and the spring 4 is twisted to an angle balanced with this viscous resistance torque. The torsion angle of the spring at this time can be read as the scale index on the scale disk 3.

Since the spring torsion angle balanced with the viscous resistance torque is measured in this manner, the viscosity of the sample liquid to be measured depends on the scale index, rotor size, viscometer rotation speed,
And the spring constant of the spring 4 can be calculated. That is, the rotary viscometer can be regarded as a measuring instrument that obtains the viscosity of the sample liquid by measuring the viscous resistance torque generated in the rotor.

[0008] At present, a viscometer is used, in which the torsion angle of the spring is converted into an electric signal and transmitted, and is digitally displayed and recorded, instead of visually reading the graduation index of the graduation plate. Has become.

When the viscosity of the sample liquid sampled in the sample container is measured using such a rotary viscometer, it is mounted on a viscometer lifting stand 100 as shown in FIG. As shown in FIG. 5, this is done after the liquid viscosity of the sample container 151 is measured and the next sample container 15
This is because the viscometer 90 is pulled up to a high level when shifting to the measurement of the viscosity of the second liquid. This is because unless the viscometer 90 is pulled up high, the rotor 80 is caught on the edge of the sample container 151 and the sample container cannot be replaced. In addition, the operation of raising the viscometer to a high level is performed by the rotor 8 in the sample container 151.
It is also necessary for the work of wiping off the sample liquid adhering to 0. That is, in order to remove the sample liquid adhering to the rotor 80, it is necessary for the operation of removing the rotor 80 from the viscometer body 90, wiping it well with a cleaning paper or the like, and then reattaching it to the viscometer body 90 again. However, recently, there has been considered a viscometer in which the internal mechanism of the viscometer is improved so that the rotor can be wiped off with a cleaning paper without removing the rotor from the viscometer body.

An outline of the structure of the lifting stand will be described with reference to FIG. In FIG. 4, the viscometer 90 is attached to the mounting portion 101 of the viscometer lift stand 100. A lifting handle 102 is provided on the mounting portion 101. Although not shown, a pinion is provided on the shaft 103 of the lifting handle 102, and the pinion meshes with a rack 106 provided on the stand guide rod 105.

With such a structure, the lifting handle 10
By turning 2 by hand, the handle shaft 103 rotates,
The mounting portion 101 can be moved to an arbitrary height position by being guided by the stand guide rod 105. That is, the height of the viscometer 90 can be arbitrarily set by operating the elevating handle 102. Further, in order to prevent the viscometer 90 from sliding down due to gravity at the height position, the mounting portion 101 is provided with a clamp handle 107, and the mounting portion 101 can be fixed at that position.

As described above, it is necessary to pull up the viscometer for operations such as replacement of the sample container and cleaning of the rotor. On the other hand, conversely, when lowering the viscometer and immersing the rotor in the liquid in the sample container, for the reasons described below, immerse the rotor to the predetermined depth with respect to the liquid surface of the sample liquid. First, it is necessary to lower the viscometer.

When lowering the viscometer, the rotor 80 mounted on the viscometer 90 is immersed in the working liquid at a certain depth. For this purpose, the rotor 80 mounted on the viscometer 90 is provided with a marked line 82 at a fixed position on the rotor stem 81 as shown in FIG. The marked line 82 indicates the position where the correct viscometer index can be obtained by immersing the rotor in the sample surface to this depth. That is, as described above, since the principle of viscosity measurement is to detect the viscous torque of the sample liquid generated in the rotor when the rotor rotates, the depth at which the rotor is immersed in the liquid is a constant depth. This is because it is necessary. If it is deeper than this, the length of the rotor stem 81 in the liquid becomes long, so a slightly higher measured value is measured. Conversely, if it is shallower than this, in the liquid of the rotor stem 81. Since the length is shortened, a slightly smaller measurement value can be obtained as the length is reduced.

The fact that the viscometer index is influenced by the immersion depth of the rotor as described above is explained as the end face effect of the rotor. For the end face effect, diameter 1.5
Using a 6 cm, 3.53 cm long cylindrical rotor, C.
Detailed research by H. Lindslay and EK Fischer “CHLindslay
and EKFischer, End… Effect in Rotational Viscome
ters. J. Appl, Phys., Vol.18.November.1974. ”
This is summarized as follows.

The smaller the distance between the lower end surface of the rotor and the bottom surface of the cup, the greater the end surface effect, but it becomes a constant value when the distance is 1 cm or more.

The upper end surface of the rotor has a constant value if it is submerged by 5 mm or more from the free surface of the liquid.

The end surface effect is larger at the lower end surface of the rotor than at the upper end surface. The effect of the upper end surface is small because the liquid above the rotor has a relatively large degree of freedom.

Regarding the effect of the end surface effect due to the viscosity, the effect is almost constant when the viscosity of the liquid is 0.1 Pa · s or more. However, when the viscosity is low, the end face effect increases rapidly. Further, as the clearance between the rotor and the cup increases, the degree of increase in the end surface effect due to the phenomenon of viscosity becomes sharper.

That is, according to this study, it can be understood that the lower the viscosity of the sample liquid is, the larger the error due to the end face effect with the measured value becomes, which cannot be ignored.

As described above, in order to improve the reproducibility of the measurement so that the error due to the influence of the end face effect due to the difference in the immersion depth of the rotor does not occur, a deep cup is used as the sample liquid container, and the bottom face of the rotor and the cup are used. It is necessary to make the space between the bottom surface of the rotor and the bottom of the rotor sufficiently large and to match the sample liquid level with the mark of the rotor stem. Therefore, when measuring the viscosity, it is necessary to operate the elevating handle 102 of the viscometer elevating stand 100 described above to set the height of the viscometer according to the height of the sample liquid level in the sample container.

[0021]

In the conventional manual measurement operation in which an operator manually raises and lowers the viscometer as described above, the operator checks the rotor dipping depth with the marked line. Since all that is required is to lower the meter, only the liquid level and the position of the marked line should be taken into consideration each time the descent operation was performed, and no special operational problems occurred.

However, the number of sample liquids may be very large in the viscosity measurement work, and automation of the measurement is desired for such work. At present, a so-called multi-sample continuous automatic viscosity measuring device is practically used, in which a sample container containing a large number of sample liquids is automatically subjected to a measurement operation equivalent to the manual operation by the operator as described above. The reality is that there are few that can withstand. The reason for this is that the inventors of the present application filed Japanese Patent Application No. 3-26658.
A viscometer itself suitable for performing automatic viscosity measurement, such as the rotary viscometer filed as No. 6, was not present before this application.

The invention according to the above application is a viscometer having a function of transmitting a viscosity measurement result as an electric signal, and in particular, a rubber seal is provided at a rotor attaching / detaching portion so as to be suitable for automatic cleaning of a cylindrical rotor, and the viscometer is stopped. Even if the seal sometimes works and the cleaning water is sprayed to the rotor, a protective function is added to prevent splash invasion into the internal machine. This is a viscometer that can be used for automatic viscosity measurement.

However, even if a viscometer suitable for the automatic viscosity measurement as described above is supplied, when the viscometer is actually installed in the automatic viscosity measuring device to perform the measurement, the viscometer functions separately from the viscometer function. There remains a major problem that must be solved as a system as to how the viscometer is brought into contact with the sample liquid to be processed.

The problem of how to bring the viscometer into contact with the sample liquid to be measured has hitherto been the same even when an operator manually measures the viscosity. Nonetheless, the reason why it did not cause a problem is that it is processed so that this problem does not occur by proper work and operation at the operator's discretion.

However, in a multi-sample continuous automatic viscosity measuring apparatus for automatically measuring the viscosity while automatically transporting a large number of sample containers one after another, in order to perform operations corresponding to these operations automatically, It is necessary to control the height of the rotor with respect to the level. However, regarding the problem of the height control with respect to the liquid surface level of the rotor, there has been no actual example of a full-scale multi-sample continuous automatic viscosity measuring device in the past, and therefore no technical proposal related thereto. That is, the height control of the rotor with respect to the liquid level is a problem to be solved.

Note that it is necessary for the operator to sample the amount of the sample liquid sampled in the sample container at a constant level, that is, to sample the liquid level of the sample liquid to be contained in the container at a constant level for all sample containers. Since it takes extra time to perform the work, it is practically difficult to execute.

On the other hand, if the liquid level is different for each sample container in this way, the liquid level in the sample container is detected and the immersion depth of the rotor is made to coincide with the liquid level and the marked line. It is possible to automatically adjust the descending height of the viscometer. However, in this case, the detector for detecting the liquid surface level is preferably a detector based on optical detection or other non-contact detection principle in order to avoid contamination of the liquid.
However, in optical detection, the possibility of detection differs depending on the properties of the target liquid such as whether the sample liquid is transparent or opaque. Further, if the refractive index is used, the optical conditions are not uniform such that the refractive index varies depending on the target liquid, and it is difficult to always deal with all the target liquids with the same detector. In addition, a method of utilizing a change in capacitance is considered as a non-contact detection method, but a definitive detection means has not been found so far.

Therefore, even with this method, the above problem cannot be solved.

An object of the present invention is to provide a method for making constant the immersion depth of the rotor, that is, the immersion depth of the rotor capable of optimally adjusting the liquid level of the sample liquid with respect to the rotor, and the viscosity measurement having the function. To provide a device.

[0031]

In the present invention, there is provided a means for solving], in order to solve the problem of the viscosity automatically measured, by detecting the liquid level, is the even that automatically adjust the falling height of the viscometer . In particular, the torque detecting function of the viscometer itself is used as a liquid level detector.

That is, according to one aspect of the present invention, the torque attached to the viscometer main body through the rotor stem is immersed in the sample solution in the container and rotated to generate the torque generated in the rotor. Is a method for making the immersion depth of the rotor constant when measuring the viscosity, and the rotor mounted on the viscometer main body is set so that the rotor does not come into contact with the sample liquid in the container. A state where the rotor is properly immersed by detecting the abrupt change in the torque generated in the rotor at the moment when the lower end of the rotor comes into contact with the liquid surface while rotating from the position above
From the length from the lower end of the rotor at the time when the rotor was properly immersed, a sudden change in the above torque was detected by the length obtained by subtracting the amount of rise in the liquid level determined by the inner dimensions of the container. When the rotor further descends from the above position, the descending of the rotor is stopped, and a method for making the immersion depth of the rotor constant during viscosity measurement is provided.

[0033] b in a state in which the rotor is properly immersed
The length from the lower end of the rotor is the portion of the rotor stem where the liquid surface of the sample liquid is located when the rotor is properly immersed.
A marked line that is provided Me pre, may be the distance between the rotor bottom.

According to another aspect of the present invention, a rotor and a rotor stem are provided, and a viscometer body for measuring the viscosity by attaching the rotor and the stem is provided, and the viscometer body drives the rotor to rotate. It has a mechanism and a torque detector that detects the rotation torque of the rotor.The rotor is rotated while the rotor is immersed in the sample liquid in the container, and the torque generated at that time is detected to determine the viscosity. In a viscosity measuring device for measuring, a lifting device for lifting and lowering a rotor attached to a viscometer body relative to a sample liquid, and a control device for controlling rotational driving of the rotor, lifting and lowering of the rotor, and viscosity measurement are provided. The control device is provided with the rotor attached to the viscometer main body while rotating the rotor from a position on the liquid level where the rotor does not come into contact with the sample liquid in the container. To control the rotor rotation drive mechanism and the lifting device, and the torque generated in the rotor at the moment when the lower end of the rotor comes into contact with the liquid surface by taking in the detected value from the torque detector. From the lower end of the rotor when the rotor is properly immersed, and the amount of increase in the liquid level determined by the inner dimensions of the container when the rotor is properly immersed. There is provided a viscosity measuring device, characterized in that it has means for stopping the descending of the rotor when the rotor further descends from the position where a rapid change in the torque is detected by the subtracted length.

The present invention further comprises an up / down amount detector for detecting the up / down amount of the rotor, and the means for stopping the lowering of the rotor is an up / down amount when a rapid change in the torque generated in the rotor is detected. It is possible to adopt a configuration in which the lift amount is read from the detector and the position where the lowering of the rotor should be stopped is detected with reference to this.

According to another aspect of the present invention, as a device suitable for automatic viscosity measurement of multiple samples, a sample liquid transfer device for sequentially transferring a plurality of containers containing sample liquid, and a cleaning process for cleaning the rotor. The control device further includes a device, and the control device performs control for sequentially measuring the viscosity of a plurality of sample liquids, and the elevating device automatically includes a viscometer in response to an elevating command from the control device. Provided is a viscosity measuring device, characterized in that a main body is moved up and down.

[0037]

In the structure of the present invention, when measuring the viscosity, the main body of the viscometer is lowered to immerse the rotor in the sample liquid.
At this time, the rotor is lowered in a rotated state immediately above the liquid level of the sample container. At this time, since the rotor is not in contact with the sample liquid, no resistance torque is generated in the rotor. That is, the detection index of the viscometer shows a state of zero. When the viscometer main body descends and the lower end of the rotor comes into contact with the liquid surface of the sample liquid, a resistance torque is generated in the rotor at the moment of contact, so that the detection finger of the viscometer rapidly rises from zero.

In the present invention, the viscometer itself is thus used as a liquid level detector for the sample liquid. That is,
The rise of the resistance torque generated in the rotor is detected to detect the position of the liquid level, which is used as a reference. Also, from the difference between the length from the marked line of the rotor to the lower end and the increase in the liquid level due to the rotor volume and the inner size of the sample container,
The immersion depth is obtained, and the rotor is lowered from the reference position by the depth. As a result, the rotor is immersed in the depth where the marked line and the liquid surface level match.

[0039]

Embodiments of the present invention will be described below with reference to the drawings.

FIG. 7 shows an outline of the constitution of an embodiment of the viscometer of the present invention. The viscometer according to the present embodiment shown in FIG. 7 includes an automatic lifting device 500 that automatically moves the viscometer main body 90 up and down, a lift amount detector 800 that detects the lift amount of the rotor (that is, the viscometer main body), and the viscometer main body. It has a control device 900 for controlling the ascending / descending operation and the viscosity measuring operation, and a data processing device 1000 for processing the measurement data. The rest of the configuration is basically the same as that of the viscometer shown in FIG.
That is, the viscometer of the present embodiment includes a viscometer main body 90, a rotor stem 81 protruding from the lower part 90a of the main body,
Rotor 80 attached to this rotor stem 81
And a stand 100 that supports the viscometer main body 90. The rotor stem 81 has a liquid level mark (immersion mark) 82 engraved to indicate the depth of the rotor. The marked line 82 is not limited to engraving, and does not take any display form as long as the display is clear.

The viscometer main body 90 has a rotor rotation drive mechanism 91 for rotationally driving the rotor, and a torque detector 92 for detecting torque generated in the rotor. The rotor rotation drive mechanism 91 is composed of, for example, a motor with a speed reducer. The torque detector 92 is constructed in principle as shown in FIG. 3, but in the present embodiment, instead of the scale disk and the pointer,
It has a converter that electrically detects the torsion angle of the spring and outputs the magnitude of the torque by an electric signal. For example, a differential transformer is used as the converter.

The automatic elevating device 500 meshes with the rack 106 provided on the stand 100, and the viscometer main body 90
And a clamp mechanism 502 that clamps the viscometer main body 90 when reaching a target position. The lifting mechanism 501 is not shown in the drawing, but is not shown in the rack 1.
It has a pinion that meshes with 06, a driving device including a motor that drives the pinion, and a control device that performs positioning.

Although not shown, the lift amount detector 800 is provided with an encoder for detecting the lift amount, a counter for counting the pulses transmitted from the encoder, etc. in association with the lifting operation of the lift mechanism 501. When the driving device of the lifting mechanism 501 uses a pulse motor as a driving source, the amount of lifting may be detected by counting the pulses for driving the pulse motor.

The control device 900 controls the operations of the viscometer main body 90, the automatic lifting device 500, and the lift amount detector 800 by adjusting the timing and the like. Basically, it executes a pre-programmed sequential operation. The control device 900 can be configured by, for example, a computer system. That is, a central processing unit (CPU) 9 that executes various controls according to a program
01, a memory 902 for storing an operation program of the CPU 901, and data, and an input / output interface 903.
Have and.

As a program stored in the memory 902, for example, there is a program for executing the procedure shown in FIG. The data stored in the memory 902 include the length h from the marked line 82 to the lower end 80 'and the volume below the marked line 82, the inner size data of the sample container, and the sample for various rotors used in the viscometer. Data and the like indicating the position where the rotor is temporarily stopped immediately above the liquid surface are stored. These data are stored in advance. Note that these data may be input from the outside. For example, a device for data input, for example, a keyboard, a disk type storage device, a communication control device, or the like is connected to the input / output interface of the control device, and manually input, input via a storage medium, or input by communication. And so on.

In addition to this, the control device 900 may have a function of calculating and outputting the viscosity of the sample liquid based on the measurement result. In this case, the data processing device 100
0 may be omitted. Further, the control device 900 may be configured by a hardware logic circuit such as a programmable logic array, for example.

The data processing apparatus 1000 is composed of, for example, a computer system, and executes recording of measured values, calculation based on measured values, output of measured values and calculation results, and the like. Therefore, the data processing device 1000 has a central processing unit (CPU), a memory, an interface, etc., and also has an external storage device, an output device, etc. For example, a printer is connected as the output device.

Next, the viscosity measuring operation by the viscometer of this embodiment will be described with reference to FIGS. 1 and 8 together with FIG. 1a shows a state where the lower end of the rotor is located at a position just above the liquid level of the sample liquid, FIG. 1b shows a state where the viscometer descends and the lower end of the rotor is in contact with the liquid surface of the sample liquid, and FIG. 1c shows a viscometer. Indicates a state where the marked line 82 and the liquid level of the sample liquid finally match. FIG. 8 shows a control device 900.
3 is a flowchart showing a rotor dipping treatment procedure, in particular, of the control procedures in the viscosity measurement performed by the above.

In FIG. 1a, a sample container 151 contains a sample liquid 6 whose viscosity is to be measured. The viscometer main body 90 and the rotor 80 are located directly above the sample container 151. Viscometer main body 90, that is, rotor 8
The initial position of the lower end 80 ′ of 0 is at a high position so as not to hinder the loading of the sample container 151, as shown in FIG.

When the sample container 151 is loaded and the viscometer is activated (step S1), the control device 900 sends an instruction to the elevating mechanism 501 of the automatic elevating device 500,
As shown in FIG. 1a, the viscometer 90 is rapidly lowered to a height g where the rotor lower end 80 ′ has a margin in a range where the liquid level 6 ′ can fluctuate in the sample container 151 (step S2). . The descending amount is detected by reading the descending amount detection value from the ascending / descending amount detector 800. Here, after temporarily stopping, a command is sent to the rotor rotation drive mechanism 91 of the viscometer main body 90 to rotate the rotor 80 (step S3). Further, a command is sent to the lifting mechanism 501 to slowly lower the viscometer main body 90 (step S
4). The detection of the liquid level 6'of the sample liquid starts from this position. When the rotor 80 is rotationally driven, the output signal of the torque detector 92 may have a transient fluctuation due to the start of rotation. Therefore, wait a time until the fluctuation is stopped and the steady state is reached, and then the viscometer. The lowering operation of the main body 90 may be started.

When the lower end 80 'of the rotor 80 is not in contact with the liquid surface when the viscometer 90 descends at a slow speed while the rotor 80 is rotationally driven, no torque is generated in the rotor 80. The torque detected by the detector 92 is zero. However, as shown in FIG. 1b, when the rotor lower end 80 'comes into contact with the liquid surface 67 of the sample liquid, torque is suddenly generated in the rotor 80 at the moment of contact, and the magnitude of the torque rises sharply. The torque detector 92 is
The rising of the torque is converted into an electric signal and output. The control device 900 monitors the signal from the torque detector 92 (step S4). The signal from the torque detector 92 is
When it exceeds a predetermined threshold value (threshold value), the rotor rotation drive mechanism 901 is instructed to stop the rotation of the rotor (step S6). In addition, the lift detector 8
The descending amount detection value is read from 00 (step S7). This value represents the position (reference position) where the rotor lower end 80 'comes into contact with the liquid surface 6'of the sample liquid 6.

In this state, the descending operation of the viscometer 90 is continued. The control device 900 determines whether or not the descending amount detection value has reached the target descending amount (step S8). This determination is made by determining the difference between the currently detected descent amount detection value and the descent amount detection value representing the reference position, and determining whether this value is the target descent amount. Until the target descending amount is reached, the descending amount detection value is read from the ascending / descending amount detector 800 in a constant cycle, and this determination is repeated (steps S7 and S8). The target descent amount from this reference position is determined as shown in FIGS. 1b and 1c. When the rotor 80 is immersed in the sample solution, the sample solution corresponding to the immersed volume of the rotor is removed. The liquid level rises due to the removed sample liquid. The rise is determined by the inner diameter of the sample container 151. If a fixed container is used as the sample container 151,
The rising level is a constant determined by the volume of the rotor 80. Therefore, the length from the lower end 80 'of the rotor to the marked line 82 is set to i, and the increase in the liquid level determined by the inner diameter of the sample container 151 and the volume of the rotor 80 below the marked line 82 is h. Then, the target descending amount of the viscometer from the reference position can be determined by i-h.

Here, in order to improve the sensitivity of the torque detector 92 when the lower end 80 'of the rotor comes into contact with the liquid surface 6'of the sample liquid, the rotor is driven to rotate at the maximum rotation speed of the viscometer. Is effective. As shown in FIG. 2, when the rotor lower end 80 'comes into contact with the liquid surface 6', bubbles 6 "are generated at the rotor lower end 80 'as shown in FIG.
In case such as adhered, the rotation speed of the rotor is high, so that there is a secondary effect that the bubbles 6 ″ are easily discharged.

When the descending amount of the viscometer main body 90 reaches the target descending amount, the control device 900 instructs the elevating mechanism 501 to
The lowering of the viscometer main body 90 is stopped (step S9).
Then, from this state, the viscosity is measured (step S10), and a series of operations is ended. The viscosity is measured by rotating the rotor 80 by the rotor rotation drive mechanism 91 and detecting the torque generated in the rotor at that time by the torque detector 92. The detected torque value is sent to the data processing device 1000. The data processing device 1000 calculates the viscosity by processing such as calculation, records the value, and outputs it.

Next, an example of applying the present invention to a multi-sample continuous automatic viscosity measuring apparatus will be described.

The present embodiment is an example of a multi-sample continuous automatic viscosity measuring device provided with a device capable of washing the sample liquid adhering to the rotor with an easily handleable solvent such as warm water. FIG. 9 shows the configuration.

In FIG. 9, the present embodiment is the same as the viscometer main body 90 and the sample liquid up / down amount detector 800, the automatic elevating device 500, the constant temperature water tank 200, the sample container transfer mechanism 201, and the sample container transfer device. A transport mechanism driving device 202 that drives the mechanism 201, a cleaning device 300, a viscometer main body moving mechanism 700, a lift amount detector 800, a control device 900 that controls these operations, and data that processes measurement data. And a processing device 1000.

The constant temperature water tank 200 is a water tank for keeping the sample liquid at a constant temperature, and is filled with a liquid kept at a constant temperature, for example, hot water. The sample container transport mechanism 201 is arranged in this. Sample container transport mechanism 20
1 is composed of, for example, a belt conveyer, and a sample container 150 containing the sample liquid 6 is placed on the belt 201a in order. Here, the sample liquid 6 is bathed in warm water for a sufficient time for constant temperature.

The cleaning device 300 is for cleaning the rotor, and includes a cleaning pot 301 and a cleaning pot 301.
Motor 302 for rotating and driving the cleaning pot 30
1, a cleaning liquid supply device 303 for supplying the cleaning liquid, a rotor drying device 304 for blowing dry air for drying the rotor 80 after cleaning, and a cleaning liquid discharge portion (not shown). The cleaning device 300 is arranged at an appropriate position above the sample container transport mechanism 201 and cleans the rotor 80. The cleaning liquid supplier 303 supplies hot water as the cleaning liquid in this embodiment.

Although not shown, the viscometer main body moving mechanism 700 includes, for example, a rail provided along the sample container transport mechanism 201, and a stand placed on the rail to movably support the viscometer main body. And a drive unit that is provided below the stand to move the stand. Although not shown in the drawings, the drive unit has wheels, a drive motor, a brake, and a lock mechanism.
The viscometer main body 90 is moved along the sample container transporting mechanism 201 in accordance with the command.

The viscometer main body 90 is not limited to the parallel movement.
May be configured to be horizontally rotated. In this case, the rail and the wheel are unnecessary, and a rotatable stand,
A drive unit and a control unit are used.

The controller 900 controls the operations of the viscometer main body 90, the automatic elevating device 500, the viscometer main body moving mechanism 700, the transport mechanism driving device 202, and the cleaning device 300 by adjusting the timing and the like. Basically, it is configured similarly to the one shown in FIG. 7 described above, and executes a pre-programmed sequential operation. In addition to this, the control device 900 may have a function of calculating and outputting the viscosity of the sample liquid based on the measurement result. In this case, the data processing device 1000 may be omitted.

The data processing apparatus 1000 is shown in FIG.
Similar to the one shown, for example, it is configured by a computer system and executes recording of measured values, calculation based on measured values, output of measured values and calculation results, and the like. Further, the configuration of the lift amount detector 800 and other components are also the same as those shown in FIG.

The sequential operation of the multi-sample continuous automatic viscosity measuring apparatus of this embodiment having such a structure will be described. As for the state of each part before the operation is started, the viscometer main body 90 is in the rotor cleaning completed state and is located at the upper retracted position P1 of the measurement position P0, and the sample container transport mechanism 201 determines that the first sample container NO. It is assumed that it is in the state immediately before the loading of one container.

First, an operator pushes a measurement start switch (not shown) of the control device 900 to instruct the start. In response to this, the control device 900 controls the transport mechanism driving device 202.
To operate the sample container transport mechanism 201,
First sample container No. 1 is loaded into the viscosity measurement position P0. At this time, the viscometer main body 90 is placed at the initial position (retracted position P1). Further, the control device 900 instructs the rotor rotation drive mechanism 91 of the main body of the viscometer to rotate the rotor. After that, the rotor 80 is set to the sample liquid 6
The operation until it is immersed in the desired depth in FIG.
Since it is the same as the procedure shown in, the description will not be repeated here.

Next, the control device 900 includes the viscometer main body 90.
Is instructed to start measurement. In response to this, the viscometer main body 90 starts the measurement rotation operation. With the rotation of the viscometer, the measurement signal from the torque detector 92 is sent to the data processing device 1000, where it is stored in a memory or the like.
Also, it is output from an output device or the like. Further, the calculation for obtaining the viscosity is performed based on the measured value. Here, the recording is performed, for example, with respect to the measured value of the viscometer, the sample liquid number and the like.

When the viscometer rotation measurement operation continues for a predetermined measurement time, the measurement is terminated and the rotation is stopped.

When the measurement is completed, the control device 900 activates the automatic elevating device 500 to move the viscometer main body 90 upward to the retreat position P1. Then, the control device 900
A movement command is sent to the viscometer main body movement mechanism 700. In response to this, the viscometer main body moving mechanism 700 operates to move the viscometer main body 90 to the retracted position P2 above the rotor cleaning position P3. These positionings are performed by the control device 900 based on the detection value of the lift amount detector 800.

Next, in the same manner as described above, the control device 900
Activates the automatic elevating device 500, lowers the viscometer main body 90, and inserts the rotor 80 into the cleaning pot 301 located at the cleaning position P3 based on the detection value of the vertical movement amount detector 800. Subsequently, the control device 900 instructs the cleaning liquid supplier 303 to supply hot water as the cleaning liquid to the cleaning pot 301, and also instructs the motor 302 to rotate. As a result, the motor 302 rotationally drives the cleaning pot 301. In addition, the cleaning liquid supply device 303
Supplies hot water for cleaning to the cleaning pot 301. Therefore, the NO. 1 Sample solution is washed.

When the preset cleaning time has elapsed, the control device 900 stops the rotation of the cleaning pot 301 and the supply of the warm water for cleaning, and terminates the cleaning. And
The control device 900 activates the automatic elevating device 500, raises the viscometer main body 90, and retracts it to the retreat position P2 above the cleaning position P3. Then, the rotor drying device 304 is activated. At the retracted position P2, the rotor drying device 304 blows dry air onto the rotor from an air nozzle (not shown) to dry the rotor. At this time, the temperature of the dry air should be as close to the temperature of the constant temperature water bath as possible.

When a predetermined time has passed, the control device 900 stops the rotor drying device 304, then activates the automatic elevating mechanism 500 to move the viscometer main body 90 to the measuring position P.
It is moved to the retracted position P1 above 0. At the same time, the transport mechanism driving device 202 is activated to activate the sample container transport mechanism 201.
To move to the next NO. 2 The sample is tact-transported to the measurement position. After that, the above NO. The operation performed for sample 1 is repeated.

By sequentially performing such an operation for all sample liquids, viscosity measurement can be performed automatically even for multiple samples. In this case, the constant immersion depth of the rotor can be automatically executed. Moreover, since the rotor can be washed, the sample can be prevented from being contaminated and the viscosity can be measured accurately. If all the sample liquids are contained in the sample container 151 having the same inner diameter, the descending amount from the reference position is constant.

According to the embodiments of the present invention described above, for example, even if the liquid level varies depending on the sample liquid amount in the sample container, the lower end of the rotor comes into contact with the liquid surface of the sample liquid. Since the position to be moved is detected and the descending amount of the rotor is determined with this position as the reference position, the liquid level can be automatically corrected only by adding the control program of the control device. This makes it possible to automatically maintain a high viscosity measurement accuracy.

Further, in the embodiment of the multi-sample continuous automatic viscosity measuring apparatus for automatically measuring the viscosity of the sample liquid in the sample container conveyed by the tact feeding, the stability of the measurement is ensured by the above effect. You can

For cleaning the rotor in the above embodiment,
An ultrasonic cleaning bath can also be used.

In the above embodiment, the rotor is cleaned and the same rotor is used to measure different sample liquids. However, the present invention is not limited to this. For example, a large number of rotors may be replaced for each measurement without cleaning the rotors. In such a case, if a large number of rotors are stored in a magazine rack and a new rotor is taken out from the magazine rack and replaced with a used rotor every time the sample solution is measured. Good. This is because if the rotor cleaning cannot be performed easily due to the nature of the sample solution,
Especially effective.

Further, in the above embodiment, the rotor / stem having the marked line showing the optimum liquid surface level is used, but the marked line may not be provided. That is, the immersion amount of the rotor can be controlled if the volume in which the rotor is immersed and the inner size of the sample container are determined.

Further, in the above-mentioned embodiment, an example in which a sample container whose inner size is known in advance is used is shown, but the present invention can be applied even when the inner size of the sample container is unknown. In this case, first, for the container to be used, the rotor is immersed in the sample liquid up to the marked line according to the procedure up to step S7 shown in FIG. Step S
The judgment of 8 is made by the operator's observation. The operator also manually gives an affirmative instruction in step S9. In this way, the descending amount is obtained for the rotor and sample container used. By storing this descending amount in the memory 902, when the same sample container and rotor are used thereafter, the liquid level can be automatically set to a constant level.

[0079]

According to the present invention, the rotor can be automatically immersed so that the immersion depth of the rotor, that is, the liquid level of the sample liquid with respect to the rotor is optimized. As a result, when the viscosity is automatically measured while automatically transporting a large number of sample containers in sequence, control can be performed to optimize the height of the rotor with respect to the liquid level.

[Brief description of drawings]

FIG. 1 is an explanatory view showing a method for making a rotor immersion depth constant in a viscometer of the present invention.

FIG. 2 is an explanatory diagram showing an effect when a rotor is rotated at a high speed.

FIG. 3 is an explanatory diagram showing the operating principle of a single cylinder rotor type rotary viscometer.

FIG. 4 is a front view showing the outline of the configuration of a rotor rotation type viscometer.

FIG. 5 is an explanatory diagram showing a procedure of viscosity measurement when there are a plurality of sample liquids.

FIG. 6 is a front view showing a rotor stem on which a marked line indicating the reference of the immersion depth of the rotor is engraved.

FIG. 7 is a front view showing the main part of the configuration of an example of the viscometer of the present invention.

FIG. 8 is a flowchart showing an operation procedure of the control device for the viscometer of the present invention.

FIG. 9 is a block diagram showing an example of the configuration of a multi-sample continuous automatic viscosity measuring device according to another embodiment of the present invention.

[Explanation of symbols]

6 ... Sample solution, 80 ... Rotor, 81 ... Rotor stem, 8
2 ... Mark line, 90 ... Viscometer body, 100 ... Stand, 15
0 ... Container, 200 ... Water tank, 201 ... Sample container transport mechanism,
202 ... Conveyance mechanism driving device, 300 ... Cleaning device, 301
... Washing pot, 302 ... Motor, 303 ... Washing liquid feeder, 304 ... Rotor drying device, 500 ... Automatic lifting device,
700 ... Viscometer main body moving mechanism, 800 ... Lift amount detector,
900 ... Control device, 1000 ... Data processing device.

Claims (5)

[Claims] 1. A rotor attached to a main body of a viscometer via a rotor stem is immersed in a sample solution in a container,
A method of detecting the torque generated in the rotor by rotating the rotor to make the immersion depth of the rotor constant when the viscosity is measured. From the position on the liquid level that does not come into contact with the sample liquid inside,
The rotor lower end in the state where the rotor is properly immersed is detected by detecting the abrupt change of the torque generated in the rotor at the moment when the rotor lower end comes into contact with the liquid surface while rotating.
From the length of the rotor, the rotor further descends from the position where a rapid change in the torque is detected by the length obtained by subtracting the increase in the liquid level determined by the inner dimensions of the container when the rotor is properly immersed. At this time, the method for keeping the immersion depth of the rotor constant when measuring the viscosity is characterized in that the descending of the rotor is stopped. 2. The length from the lower end of the rotor in a state where the rotor is properly immersed is such that, when the rotor is properly immersed, the liquid surface of the sample liquid of the rotor stem is located. A method of making constant the immersion depth of the rotor in the viscosity measuring device, which is the distance between the marked line previously provided on the part and the lower end of the rotor. 3. A rotor and a rotor stem, and a viscometer main body for mounting them to measure viscosity, the viscometer main body detecting a rotor rotation drive mechanism for rotationally driving the rotor, and rotational torque of the rotor. A viscometer that has a torque detector and measures the viscosity by rotating the rotor while the rotor is immersed in the sample liquid in the container and detecting the torque generated in the rotor at that time. And a controller for controlling the rotation of the rotor, the rotor ascent and descent, and the viscosity measurement. The controller is a viscometer main body. From the position where the rotor is on the liquid level not contacting the sample liquid in the container,
A means for controlling to approach the sample liquid while rotating, a means for controlling the rotor rotation drive mechanism and the elevating device, and a detection value taken from the torque detector, and the lower end of the rotor came into contact with the liquid surface. Means for detecting sudden changes in torque generated in the rotor at the moment, and rotor lower end when the rotor is properly immersed
From the length of the rotor, the rotor further descends from the position where a sudden change in the torque is detected by the length obtained by subtracting the increase in the liquid level determined by the inner dimensions of the container when the rotor is properly immersed. And a means for stopping the descending of the rotor. 4. The lift amount detector for detecting the lift amount of the rotor according to claim 3, further comprising means for stopping the lowering of the rotor when a rapid change in the torque generated in the rotor is detected. A viscosity measuring device for reading the amount of elevation from the amount of elevation detector and detecting the position where the lowering of the rotor should be stopped based on this reading. 5. The sample liquid carrier according to claim 3, further comprising a sample liquid carrier for sequentially carrying a plurality of containers containing the sample liquid, and a cleaning device for cleaning the rotor, wherein the control device has a plurality of sample liquids. With respect to the above, the viscosity measuring device is for sequentially performing control for viscosity measurement, and the elevating device automatically elevates the viscometer main body in response to an elevating command from the control device. .