JPH02251757A - Automatic analyzer - Google Patents

Abstract

PURPOSE:To enhance analytical accuracy and to enhance the reproducibility of measured data by providing a universal joint preventing the eccentric rotation of a rotor between the rotary shaft and rotor of a viscosity measuring apparatus. CONSTITUTION:The viscosity measuring apparatus controlled by a computer unit has the rotary shaft 23 downwardly protruding from the main body of this apparatus. A universal joint 24 is attached to said rotary shaft 23 and a rotor 26 is attached to the universal joint 24 through an automatic joint 25 detachable by one-action operation. When viscosity is measured using the rotor 26 mounted through the universal joint 24, the rotary shaft 23 is rotated in such a state that the rotor 26 is immersed in the sample to be inspected in a container 42. Whereupon, the rotation of the rotary shaft 23 is transmitted to the rotor 26 through the universal joint 24 and, even when the rotary shaft 23 is rotated in a state inclined in an oblique external direction with respect to a vertical line, the rotor 26 is not rotated eccentrically and always rotated on the same vertical line.

Description

[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to an automatic analyzer for liquid resin, and more specifically, the present invention relates to an automatic analyzer for liquid resin, and more specifically, viscosity (hereinafter abbreviated as rVisJ, as necessary), which is an index for specifying the quality of liquid resin. ), p)l and nonvolatile content (also referred to as evaporation residue, solid content, and resin content; hereinafter abbreviated as rNVJ as necessary).

[Prior Art] In general, manufacturers of liquid resins adopt the Vis value, p)l, and MV values as indicators to specify the quality of the liquid resin, and the manufacturers themselves analyze and determine the index values. 1 quality is often specified.

As an analytical method for determining the above index value, there is the JIS method.For example, the general test method for 1L adhesive is JISKs83.
3, in which p)l is JISK88
338.2, the viscosity is JIS K 88336.3,
The non-volatile content is defined as Ei833 B, 4 in JISt. However, since the quality of the liquid resin only needs to be determined on a regular basis, index values obtained using a simple analysis method may be acceptable depending on the user. Index values obtained using a simple analysis method are acceptable.

However, when looking at individual analyzes of the three index values, Vis value, pH, and NV value, which have been conventionally performed in the field of liquid resin production, the JIS method is the best.

Even if it is a simple method, most of it is done manually.
There were not many attempts at automation.

In recent years, attempts have been made to automate devices that independently analyze each of the Vis value, pH, and NV value (for example, P)! The measurement is described in Japanese Unexamined Patent Publication No. 1111-2H4a.

[Problem to be solved by the invention] As mentioned above, in the field of liquid resin production, Vis.
value, p)! (and) automatic analysis of index values such as IV values is extremely slow, and most of them rely on complicated manual operations, and although some index values have been automatically analyzed, they still require manual operation. Many parts are required, and it is difficult to say that the problems of complicated work and high costs have been solved that much.

In view of the above, the present inventors attempted to introduce an analytical robot for the purpose of completely automating liquid resin analysis.

However, after conducting various experiments, we found that several measurement items, especially the Vis value, p)! If you try to automatically analyze the NV value during a series of movements of an analysis robot, simply combining commercially available analyzers and known analysis methods will require additional analysis time due to the specificity of the analysis target and analysis items. It was found that there were problems such as unexpected troubles, requiring additional manual operations, and the inability to obtain data reproducibility.

One example of a viscosity measuring device is one in which a rotor is directly screwed onto a rotating shaft. This rotor was rotated while immersed in the sample in the cup, and the elastic twist was measured as the viscosity of the sample.

However, in the configuration of conventional viscosity measuring devices, the rotor is directly attached to the rotating shaft, so in the case of long objects such as rotors, the minute eccentric rotation of the rotating shaft is multiplied by several times. As a result, the rotor rotates largely eccentrically. As a result, accurate viscosity measurement cannot be performed, resulting in a problem of poor analytical accuracy and reduced reproducibility of measured data.

SUMMARY OF THE INVENTION Therefore, an object of the present invention is to provide an automatic analyzer that can prevent eccentric rotation of the rotor, improve analysis accuracy, and improve reproducibility of measurement data.

[Means to solve the problem] The automatic analyzer of the present invention achieves the above object.

In an automatic analyzer that automatically analyzes the viscosity, pl+, and nonvolatile content of a liquid resin using an analytical robot.

A viscosity measuring device that measures the viscosity of liquid resin, and an analysis device that takes out the rotor from the storage device and sets it in the viscosity measuring device, and also takes out the test sample container from the turntable device and holds the set rotor in an immersed state. A robot, a computer unit for controlling the analytical robot and the viscosity measuring device, and a universal joint for preventing eccentric rotation of the rotor is provided between the rotating shaft of the viscosity measuring device and the rotor. do.

According to two preferred embodiments of the present invention, the universal joint includes a pair of universal joints extending in the direction of the rotation axis;
It is characterized by comprising an elastic sleeve fitted around the outer periphery of the universal joint.

[Operation] When measuring viscosity using a rotor attached via a universal joint, if the rotor is immersed in the test sample in a container and the rotating shaft is rotated, the rotation of the rotating shaft will cause the universal joint to rotate. Even if there is a minute eccentric rotation on the rotating shaft, the rotation is absorbed by the pair of universal joints, and the rotor will not rotate eccentrically.

In this way, eccentric rotation of the rotor is prevented, and therefore accurate viscosity measurement can be obtained, analytical accuracy is good, and reproducibility of 21M constant data is improved.

Therefore, the above-mentioned problem can be eliminated.

The analysis items by the automatic analyzer of the present invention are viscosity (Vis
), pH, and non-volatile content (NV) (7) Although it is preferable to include all three items, analysis of only two of these items is also important for determining the quality of liquid resin, so we do not recommend it here. Included in the device of the invention.

[Example] The present invention will be explained below with reference to embodiments shown in the drawings.

FIG. 1 is a plan view showing an automatic analyzer according to an embodiment of the present invention, FIG. 2 is an explanatory diagram showing a control system of the device, and FIG.
The figure is a flowchart showing the automatic analysis system, and FIG. 4 is a perspective view showing the analysis robot and turntable device.

In FIG. 1, reference numeral 1 denotes an analysis robot placed approximately at the center of an analysis stage 2. As shown in FIG. In the operating range around the analysis robot 1, there are a turntable device 3, an analysis robot hand stage plate 4, an NV measurement device 5, a vacuum device 16. Vi5 measuring device7. pH measuring device 8
．． Cleaning device9. A storage device 10 and a barcode reader 11 are arranged.

Further, a computer unit 12 is arranged outside the operating range of the analysis robot 1.

The computer unit 12 mainly includes a CPU (central processing unit) 121. CRT (screen) 122, keyboard! 23, printer 124, floppy disk device 12
5, and performs important functions such as barcode management, analysis robot management, sequencer communication, real-time data check management, analysis data pass reanalysis management, etc., which will be described later.

In this embodiment, as means for realizing the control system of the computer unit 12, as shown in FIG. A network controller 15 and a sequencer 16 are provided.

The analysis robot 1 has cylindrical coordinates.

There are polar coordinates, blood angle coordinates, multi-jointed robots, etc.

In this example, cylindrical coordinates are used.The analytical robot 1 used in this example has an arm length of 800 mm.
mm, operating radius 320 layers, maximum vertical operating distance 340 mm
++v, maximum operating speed is 7t3yam/sea, 80 degree rotation/3 seconds.

As shown in FIG. 4, the analytical robot 1 of this embodiment is mainly composed of a base 101, two vertical shafts 102, an arm 103, a grip hand 104, and a part of a finger 105.

The analytical robot l is an analytical robot controller 13.
The analytical robot controller 13
The specifications are that the maximum number of control axes is 3 at the same time, the path control method is a servo motor method, the control method is a semi-closed loop method using a rotary encoder, the 5 position setting is a teaching method, and the speed is 0.1 to 1. .0 lθ step variable, input/output is input 8.0. The output is 8.

The analysis station 2 may be a commonly used laboratory analysis table, and is preferably configured such that the analysis robot 1 and various peripheral devices can be set (fixed, etc.) therein.
In order to simplify the task of accurately arranging various instruments in accordance with the operating range of the analysis robot, it is preferable to set the various instruments in advance on the analysis table, and to It is also preferable to apply processing such as unevenness so that the device can be set in a removable manner.It is also preferable to set the entire system in the analysis station 2 and treat it as a system product.Therefore, as shown in Fig. 1 Needless to say, there is no need to locate the computer unit H2 separately.

The turntable device 3 has a constant temperature bath 30 as shown in FIG.
1 and a turntable 302 rotatably provided within the constant temperature bath 301. Water is filled in the constant temperature bath 301, and the temperature is controlled at approximately 25°C.

Although the temperature control means is not particularly limited, it is convenient to use circulating hot water. The turntable 302 may have one stage, but it is preferable to have three stages separated by a predetermined interval. In that case, the upper and middle turntables have through holes 304 for setting the test sample containers 303. established,
The through hole 3G4 is further provided with a positioning groove 305 for determining the position (direction) of the container 303. When the lower turntable is set with container 3H,
The turntable 302 functions as a support plate to prevent the container 303 from falling, and it is preferable that a small hole (not shown) is provided at a position in contact with the container 303.The direction of rotation of the turntable 302 is not particularly limited; In this embodiment, it is rotated clockwise.

The MV measurement device t5 is a device that measures nonvolatile components.
The MV value is determined by heating and drying the test sample at a predetermined temperature with a heater until it reaches a constant weight.

In this embodiment, two measuring devices are provided in order to improve the reliability of the analysis values. The device 5 has a weighing table in its main body and a heater on its inner surface. It also has an automatic opening/closing mechanism to automatically open and close the lid.

The vacuum device 6 includes a suction machine (such as a vacuum cleaner) for mounting a tray (aluminum plate) containing a test sample into the MV measurement device during NY measurement, a suction hose, and unused and used trays. It consists of a tray mounting section that is housed in a container. A filter paper is placed on the tray to uniformly diffuse the test sample.

The Vig measuring device 7 measures the Via value based on the viscosity of the test sample by rotating a rotor, and consists of a device main body and a rotor for rotating the rotor. Since the viscosity varies depending on the type of test sample, it is desirable to select an appropriate rotor, and for this reason, rotor selection 1 attachment/detachment is automatically performed. A one-touch coupling (auto joint) is preferable because the rotor is attached and detached by an analytical robot.It is preferable to interpose a universal joint between the rotor and the device body to prevent rotor eccentricity. For some large-sized products, it is preferable to make the rotor hollow inside to reduce weight in order to prevent it from falling off when transferred to an analytical robot.Since viscosity changes depending on temperature, when the rotor rotates, it is recommended to reduce the humidity at the same time. Although it is necessary to also measure the temperature, a temperature sensor such as a thermocouple or a thermistor is preferable as such temperature measuring means.

A commercially available pH sensor can be used as the pH measuring device 8.

The cleaning device 9 is a device for washing off test samples adhering to the surfaces of the pH electrode, the Vis measurement rotor, and the temperature sensor. The cleaning means is not particularly limited, but if the viscosity of the test sample is high, a configuration using a pair of rotating brushes is preferred.

The storage device 10 is a device for storing a via rotor and a pH electrode, and the pH electrode is preferably stored immersed in water at a predetermined temperature, and the rotor may be stored in an environment at a predetermined temperature, more preferably. is to be stored together with the pH electrode. The storage temperature may be room temperature, but is preferably controlled to be equal to the analysis temperature (for example, 25°C). The configuration of the storage device is not particularly limited, but it is preferable to have a rotor suspension mechanism and a pH electrode immersion part in a constant temperature water bath.The rotor suspension mechanism is a one-touch coupling so that it can be easily attached and detached by an analytical robot. (auto joint) is preferred.

When the rotor is stored immersed in water, it is preferable to provide a device that can clean the rotor with methanol in order to remove water droplets that have adhered to the rotor in advance for subsequent ViS measurements.

252 mutual 11 The automatic analysis system of the present invention will be explained based on the drawings.

When the number n of test samples is entered into the computer 121, the program of the automatic system is started.

(Selection of robot hand for analysis) Robot hand for analysis (rHANDJ as necessary)
There are GP HAN[l] and syringe HAND, and GP HAN comes in sizes "large" and "medium".
・There is "Small", but in this example, "Medium" and "
``Small'' GP HANDS and ``Syringe HANDJ.'' First, select ``Medium'' GP HANDS. Furthermore, the second
- In the figure, 401 is a chip rack for holding chips.

(Checking the number of specimens) If the number of specimens exceeds the number input from the computer 121, the process ends. If it is within the input number, proceed to the next step.

(Barcode Reading) The barcode (hereinafter referred to as rBcJ as necessary) reader 11 and BC sensor 110 read the barcode information of the test sample. The turntable automatically rotates by one test sample amount. If the BC reading is normal, proceed to the next step shown below; if it is abnormal, add 1 to n and return.

(Open the lid of the MV measurement device 5 for NV measurement, and set the tray (aluminum plate) 800 using the vacuum device 6.

Close the lid of the NVJtg measuring device 5 (delete the tare on the aluminum plate).

Next, open the lid of the test sample container 303, change the HAND from "Medium" to "Syringe," attach a tip (dropper-like thing for aspirating the test sample) to the tip of the syringe (syringe) IAND, and insert the tip from the test sample container 303 into the tip. 8. Next, the lid of the MV measuring device 5 is opened, and the sample is dropped onto the glass fiber filter paper in the aluminum pan at 9 locations in total, 1 location in the center and 8 locations equally spaced around it. In this embodiment, the amount of test sample sucked is 1.2 g.

Next, close the lid of the MV measuring device 5, start the NV measurement, and then discard the tip at the tip of the syringe. In addition, in FIG. 2, Ml and M2 are motors.

(Via measurement)) Change the IAND from "syringe" to "small" and select the rotor that matches the test sample from the storage device 10 based on the instructions from the computer unit.

Next, the rotor is immersed in a container 101 containing methanol to dry water droplets attached to the rotor, and dried at room temperature in a dryer 102 maintained at room temperature.Then, the rotor is automatically inserted into the rotating shaft of a Via measuring device.

The temperature sensor is set near the viscometer included in the Vis measuring device 7.

Next, change the OP HAND from "small" to "r medium".

The test sample container in the turntable device 3 is set in a viscometer and the viscosity is measured. In addition, in FIG. 2, 700 is a viscometer controller.

This viscosity and temperature are displayed graphically on the CR7 screen 122. At this time, data processing (data acquisition comparison) is performed.

(pH measurement) The p) I sensor included in the pH measuring device 8 is set in the test sample container, and it is measured (graphed (pH and temperature) on the R sub-screen 122), and at the same time data processing (data acquisition) is performed. comparison).

(Cleaning/Storage/End) The pH sensor is cleaned with the cleaning device 9. pH in cleaning device 9
After setting the sensor, the cleaning device will automatically operate. That is, the rotating brush rotates and the cleaning liquid automatic supply and drainage system starts.

Next, the test sample container 303 is returned to the turntable device 3, and the test sample container 303 is covered.

Change GP HAND from “Medium” to “Small” and set Vis
The rotor is removed from the measuring device 7, and the rotor is cleaned in the cleaning device 9 while operating the cleaning liquid automatic supply and drainage system in the same way as the PO sensor, and after removing the attached test sample, it is returned to the storage device 10. Next, the temperature sensor The above pH
While operating the cleaning liquid automatic supply and drainage system in the same way as the sensor, it is cleaned by the cleaning device 9 and returned to the storage device 10.

Next, change GP HAND from "small" to "medium".

Process data and check NV completion 0 then MV
The lid of the measuring device is opened, and the tray (aluminum plate) inside the MV measuring device 5 is taken out and processed using the vacuum device 6.

FIG. 5 is a front view showing a viscosity measuring device according to an embodiment of the present invention, and FIG. 6 is an explanatory diagram showing the operation of the device.

The viscosity measuring device 7 has a rotating shaft 23 that projects downward from the device body 22. A universal joint 24 is attached to this rotary shaft 23, and the rotor 2B is attached to this 22 versalge 24 via an autojoint 25 which can be attached and detached with one touch.

The universal joint 24 has a cylindrical shape as a whole and is composed of first and second universal joint parts 27 and 28. That is, the first universal joint part 27 is formed between the first and second joint shaft parts 29.30, and the second universal joint part 28 is formed between the second and third joint shaft parts 30.31. has been done. The first universal joint part 27 has first and N42 pins 34.35 which are rotatably provided in the recesses 32.33 of the first and second joint shaft parts 211.30, and are orthogonal to each other in the center and are pin-coupled. Similar to the universal joint part 27 of N41, the universal joint part 28 of 0w42 which is made of 38 and 38 are pin-coupled at right angles to each other at the center.

A transparent elastic sleeve 40 is fitted around the outer periphery of the first and second universal joints 27.28, so that when the rotor 26 is attached or detached, the first and second universal joints 27.28 absorb the horizontal attachment/detachment force. It is designed to prevent people from escaping.

When measuring viscosity using the rotor 2B attached via the universal joint 24 configured as described above.

As shown in FIG. 6, when the rotary shaft 23 is rotated with the rotor 26 immersed in the test sample in the container 42.

The rotation of the rotating shaft 23 is transmitted to the rotor 2B via the universal joint 24. N42 with 2 universal joints 27 and 28
Since the third joint shaft parts 30 and 31 rotate in a state in which they are sequentially bent inward, the rotor 2B always rotates on the same vertical line without eccentric rotation. Therefore, highly accurate viscosity measurement can be performed.

Furthermore, when the rotor 28 is attached or detached, the attachment/detachment force tends to escape to the side due to the first and second universal joints 27, 28, but the restoring force of the elastic sleeve 40 prevents the attachment/detachment force from easily escaping to the side. Therefore, the rotor 28 can be attached and detached smoothly.

It should be noted that the present invention is not limited to the above embodiments8.
For example, in this embodiment, a case has been described in which the universal joint has a cylindrical shape, but the present invention is not limited to this, and the present invention can also be applied to cases in which the universal joint has one of various shapes.

[Effects of the Invention] According to the present invention, there is provided a viscosity measuring device for measuring the viscosity of a liquid resin, and a rotor is taken out from a storage device and set in the viscosity measuring device, and a test sample container is taken out from a turntable device to be placed in the set state. an analytical robot that holds the rotor in an immersed state, and a computer unit that controls the analytical robot and the viscosity measuring device, and the eccentric rotation of the rotor is provided between the rotating shaft of the viscosity measuring device and the rotor. Since the configuration includes a universal joint to prevent eccentric rotation of the rotor, it is possible to prevent eccentric rotation of the rotor, thereby increasing analysis accuracy and improving reproducibility of measurement data.

[Brief explanation of drawings]

FIG. 1 is a plan view showing an automatic analyzer according to an embodiment of the present invention, FIG. 2 is an explanatory diagram showing a control system of the same device, and FIG.
The figure is a flowchart showing the automatic analysis system, and Figure 4 is a perspective view showing the analysis robot and turntable device. 1 to 5 are front views showing the viscosity measuring device, and FIG. 6 is an explanatory diagram showing the operation of the device. 1: Analysis robot 2: Analysis stage 3: Turntable device 4: Analysis robot hand station 5: NV measurement device 6: Vacuum device 7: Viscosity measurement device 8: pH measurement device 9: Cleaning device 10: Storage device ll: barcode league 12: computer unit 2a: rotating shaft 24: universal joint 28: rotor 27: first universal joint 28: second universal joint 29: first joint shaft 30: second joint Shaft portion 31: Third joint Shaft portion 40: Elastic sleeve

Claims (1)

[Scope of Claims] 1. An automatic analyzer that automatically analyzes the viscosity, pH, and nonvolatile content of a liquid resin using an analytical robot, which includes a viscosity measuring device that measures the viscosity of the liquid resin, and a viscosity measuring device that measures the viscosity of the liquid resin by removing the rotor from the storage device. An analytical robot that is set in a measuring device, takes out a test sample container from a turntable device, and holds the set rotor in an immersed state, and a computer unit that controls the analytical robot and the viscosity measuring device. . An automatic analysis device, characterized in that a universal joint is provided between the rotating shaft and the rotor of the viscosity measuring device to prevent eccentric rotation of the rotor. 2. The automatic analyzer according to claim 1, wherein the universal joint comprises a pair of universal joints extending in the direction of the rotation axis, and an elastic sleeve fitted around the outer circumference of the universal joints.