JPH02251760A - Automatic analyzer - Google Patents

Abstract

PURPOSE:To enhance the reproducibility of data by perfectly automating measurement and to also enhance safety by controlling a non-volatile component (NV) measuring apparatus by a computer unit and substituting the air in said apparatus with inert gas. CONSTITUTION:An NV measuring apparatus 5 sets the tray taken out of a tray container by the analytical robot controlled by a computer unit to measure the non-volatile component of a liquid resin. In this apparatus 5, a lid 502 is mounted to the upper part of the apparatus main body 501 in a freely openable and closable manner through a hinge and automatically opened and closed by a lid opening and closing mechanism at each time when the tray 503 goes in and out or a sample to be inspected is dripped. A balance 506 is arranged in the apparatus main body 501 and the non-volatile component of the liquid resin is measured from the difference between the wts. before and after measurement of the tray 53 having the sample to be inspected received therein placed on a tray receiving stand 507. At each time when NV is measured, the air in the NV measuring apparatus 5 is substituted with inert gas by an inert gas substitution apparatus 539 to hold the interior of the apparatus 5 to an explosion limit value or less.

Description

[Detailed description of the invention]

[Industrial Field of Application] 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), p)l, and non-volatility, which are indicators for specifying the quality of liquid resin. Minutes (
Also called evaporation residue, solid content, and resin content. The present invention relates to an apparatus for automatically analyzing rNVJ (hereinafter abbreviated as rNVJ if necessary). [Prior Art] In general, manufacturers of liquid resins adopt Via value, pH, and NVfi as indicators to specify the quality of the liquid resin, and the manufacturers themselves analyze the values to determine the index values and evaluate the quality. Often specified. As an analysis method for determining the above index value, there is the JIS method. For example, the general test method for adhesives is Jl';883
3, in which p) I is JIS K1
18338.2, and the viscosity is JIS K f18336.
3. Non-volatile content is JIS K E! 8338.4. However, since the quality of the liquid resin only needs to be determined regularly, some users may accept an indicator obtained by a simple analysis method. Index values obtained using a simple analysis method are acceptable. However, when we look at the individual analyzes of the three index values, Via value, pH, and +4V value, which have been conventionally performed in the field of liquid resin production, it is the JIS method. 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 Via, PH, and NV values. The measurement is described in JP-A-81-28801.

[Problem to be solved by the invention]

As mentioned above, in the field of liquid resin production, Via
Automatic analysis of index values such as pH, pH and NV values is extremely slow, and most rely on complicated manual operations.
In addition, although some of the index values have been automatically analyzed, there are still many parts that require manual operations, and it cannot be said that the problems of the complexity of two operations and the high cost have been solved to a great extent. 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 if we tried to automatically analyze multiple measurement items, especially Vf value, P)l, and NV value during a series of movements of the analysis robot, commercially available analyzers and Simply combining known analysis methods may require additional analysis time due to the specificity of the analysis target or analysis items, unexpected troubles may occur, requiring additional manual operations, or data reproducibility may not be achieved. It turned out that there was a problem. To measure the nonvolatile content of a test sample, an NV measurement device was used, and operations such as opening and closing the lid, setting the tray, and dropping the sample were performed manually. However, with conventional NY measuring devices, opening and closing the lid, setting the tray, dropping the sample, etc. must be done manually.
It was a hassle. In addition, there was a problem that there was a risk of explosion due to the volatile gas generated during the measurement, resulting in a lack of safety. Therefore, the present invention aims to completely automate NV measurement. It is an object of the present invention to provide an automatic analyzer equipped with an NV measurement device that can improve data reproducibility and maintain volatile gas below the explosion limit value to improve safety. [Means for Solving the Problems] The automatic analyzer of the present invention that achieves the above object is an automatic analyzer that automatically analyzes the viscosity, pH, and nonvolatile content of a liquid resin using an analytical robot. NV measurement device. It is equipped with an analytical robot that takes out the tray from the tray container via a suction tool, sets it in the NV measuring device, and takes it out after measurement, and a computer unit that controls the analytical robot and the NV measuring device. It is characterized by being equipped with an inert gas replacement device that replaces air with an inert gas. [Operation] When measuring the volatile content of liquid resin, first open the lid using the lid opening/closing mechanism.Next, the analytical robot takes out the tray from the tray container via the suction tool, sets it on the balance, and then closes the lid. Closed. When the analytical robot takes a test sample and drops it onto the filter paper in the tray, the lid is opened again and there is a pause after dropping. The test sample is radiated with heat by the heater, and NV measurement is started. In this way, complete automation of NV determination is achieved, the performance of one analysis is good, and the reproducibility of measurement data is improved. Furthermore, the inert gas replacement device eliminates the risk of explosion due to the filling of volatile gas, improving safety. Therefore, the above-mentioned problem can be eliminated. The analysis items by the automatic analyzer of the present invention are viscosity (Via
), pH1 non-volatile content (NV) (7) Although it is a preferable embodiment to include all three items, analysis of only two of these items is also effective in determining the quality of liquid resin, so it is also included in the present invention. included in the device. [Examples] The present invention will be explained below using examples shown in the drawings. Kasa 1J and Type 1 Figure 1 is a plan view showing an automatic analyzer according to an embodiment of the present invention, Figure 2 is an explanatory diagram showing the control system of the equipment, and Figure 3
FIG. 2 is a flowchart showing the automatic analysis system. FIG. 4 is a perspective view showing the analysis robot and turntable device. In FIG. 1, l is an analysis robot placed approximately at the center of the analysis stage 2. As shown in FIG. The operating range around the analytical robot 1 includes a turntable device 3, an analytical robot hand stage, an NV measuring device 5, a vacuum device 6. Vij measuring device 7.9H measuring device 8.
A cleaning device 9, a storage device IO, and a barcode reader 11 are arranged. Also, outside the operating range of the analysis robot 1. A computer unit H2 is arranged. The computer unit 12 mainly includes a CPU (central processing unit) 121, a CRT (screen) 122, a keyboard 123, a printer 124. Floppy disk device 1
25, and barcode management 1 as described below.
It performs important functions such as public analysis robot management, sequencer communication, real-time data check management, and analysis data reanalysis management. In this embodiment, as means for realizing the control system of the computer unit 12, there are five analytical robot controllers 13, a power event controller, and the like, as shown in FIG. 4, a network controller 15 and a sequencer 18 are provided. The analysis robot 1 has cylindrical coordinates. There are polar coordinates, rectangular coordinates, articulated 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 3201■, maximum vertical operating distance 340mm
mm, maximum operating speed is 78 mm/see, 80 degree rotation 1
It is 3 seconds. As shown in FIG. 4, the analytical robot 1 of this embodiment mainly consists of a platform 101. It is composed of two vertical shafts 102, an arm 103, a grip hand 104, and a finger portion 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 position setting is a teaching method, and the speed is 0.1 to 1. It is variable in 10 steps of .0, and has 8 inputs and 8 outputs. The analysis stage 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.) thereon.
In order to simplify the task of accurately arranging various devices in accordance with the operating range of the analysis robot, it is preferable that the analysis table is provided with set positions for the various devices in advance. It is also preferable to process the surface of the analysis table to have irregularities, etc., so that the equipment can be set in a detachable manner.It is also preferable to set the entire system in the analysis station 2 so that it can be treated as a system product. 1st
It goes without saying that it is not necessary to arrange the computer units 12 separately as shown in the figure. 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 304 further has a set position (direction) of the container 303.
A positioning groove 305 is provided for determining the position. When the container 303 is set on the lower turntable, the corresponding container @
The turntable 302 functions as a support plate to prevent the turntable 303 from falling, and is preferably provided with a small hole (not shown) at a position in contact with the turntable 303.
The direction of rotation is not particularly limited, but in this embodiment, it is rotated clockwise. The NVil determination device 5 is a device for measuring non-volatile content.
The NV 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 the main body and a heater on the inner surface of the lid. It also has an automatic opening/closing mechanism to automatically open and close the lid. The vacuum device 6 includes a suction machine (for example, a vacuum cleaner), a suction hose, and unused and used trays for mounting a tray (aluminum plate) for holding a test sample into the NV measurement device during NV measurement. 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 Via measuring device 7 measures the Vis 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 and attachment/detachment are performed automatically. 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 devices, 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, the temperature should be adjusted 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 via 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 IO is a device for storing the Vis rotor and the pH electrode, and the pH electrode is preferably stored immersed in water at a predetermined temperature, and the rotor is preferably stored in an environment at a predetermined temperature. 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 during subsequent Wig measurements. The automatic analysis system of the present invention will be explained based on the drawings. When the number n of test samples is input into the computer 121, the program of the automatic system is started. (Selection of robot hand for analysis) Robot hand for analysis (r below as necessary) IAND
J) has GP HANDS and syringe HANDS, and GP 11ANDs have size r large" and "
There are ``medium'' and ``small,'' but in this example, ``medium'' is used.
- "Small" OP HAND and "Syringe HANDJ. First, select the "Medium" (iP HAND). In Fig. 2, 401 is the tip rack to hold the tips upright. (Checking the number of samples) Computer If the number of samples is greater than the number input from 121, the process ends. If it is within the input number, proceed to the next step. (Barcode reading) Barcode (hereinafter referred to as rBCJ as necessary) reader 11 and BC sensor At step 110, the barcode information of the test sample is read.The turntable automatically rotates for one test sample.If the BC reading is normal, proceed to the next step shown below.If it is abnormal, set 1 to n. Add and return. (Open the lid of the NV measuring device 5 and use the vacuum device 6 to set the tray (aluminum plate) 503. Close the lid of the NY device (delete the tare of the aluminum tray. do)
. Next, open the lid of the test sample container 303 and open the GP HAND.
Change ``Medium'' to ``Syringe'' and select Syringe HAN.
Tip at the end of D (dropper-like thing for aspirating the test sample)
Attach the test sample to the tip from the test sample container 303. Next, open the lid of the N'/measuring device 5, and place eight tubes on the glass fiber filter paper in the aluminum pan, one in the center and at equal intervals around it. Drop in a total of 9 locations. In this embodiment, the amount of test sample sucked is 1.2 g. Next, close the lid of the +IV measurement device 5, start the NV measurement, and then discard the tip at the tip of the syringe. In addition, in FIG. 2, M2 is a motor. (Via measurement) Change the HAND from "Syringe" to "Small" and select the rotor that matches the test sample from the storage device IO based on the instructions from the computer unit. Next, in order to dry the water droplets adhering to the rotor, the rotor is immersed in a methanol container 101 and dried at room temperature in a dryer 102 kept at room temperature for 1 hour.
g [fixed? auto-join to the rotation axis of the position. The temperature sensor is set near the viscometer included in the Via measuring device 7. Next, change GP HAND from "small" to "medium". The test sample container in the turntable device 3 is set in a viscometer and the viscosity is measured. 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) p) I The pH sensor included in the measuring device 8 is set in the test sample container, and the measured results are displayed graphically (pH and temperature) on the CR7 screen 122, at the same time data processing (data acquisition comparison) is performed. (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. OP) Change IAND from "medium" to "small" and use Vig
The rotor is removed from the measuring device 7, and the rotor is
While operating the cleaning liquid automatic supply and drainage system in the same way as the sensor, the cleaning device 9 cleans the test sample and removes the attached test sample, then the storage device! Return to 110 0 Next, the temperature sensor is cleaned in the cleaning device 9 while operating the cleaning liquid automatic supply and drainage system in the same way as the PH sensor, and returned to the storage device IO. Then change GP)IAND from "small" to "r medium". Process data and check NV completion 0 then NV
The lid of the measuring device 5 is opened, and the tray (aluminum plate) inside the NV measuring device M5 is taken out and processed using the vacuum device 6. FIG. 5 is a perspective view showing the external configuration of the NV measuring device according to the embodiment of the present invention, FIG. 6 is a sectional view taken along the line ■-■ in FIG. 5, and FIG. 7 is a block diagram showing the lid opening/closing mechanism. . The NV measuring device 5 has a device main body 501 having a substantially rectangular parallelepiped shape, and the device main body 50! 41502 is attached to the upper side via a hinge so as to be openable and closable, and a lid opening/closing mechanism 504 is provided which automatically opens and closes the lid 502 each time a tray 503 is taken in and out or a test sample is dropped. Specifically, the tip of the lid 502 is tied with something like a reel 525, pulled from behind using a pulley 52B as shown in FIG. 7, and tied to the next pulley 527 in the same way. The pulley 527 is connected to a motor shaft 528, and the lid 502 is opened and closed by rotating the motor 529 in the forward and reverse directions. Limit switches 530 and 53 for close and ozone to prevent the motor 528 from rotating too much.
1 is installed in each. The motor 528, limit switches 530, 531 and manual switch 532 are electrically connected to the sequencer 16, and the sequencer IB is electrically connected to the computer 121.
The lid 502 is opened and closed according to instructions from the program. Further, a data display and operation panel 505 is integrally provided on the entire surface of the apparatus main body 501, and a balance 50B is arranged inside the apparatus main body 521. The balance 50B has a tray 503 containing a test sample placed on its tray holder 507.
The non-volatile content can be measured from the difference in weight before and after measurement. A spiral heater 508 is attached to the back of the lid 502 so as to face the tray holder 507 of the balance 50B, so that heat is radiated toward the tray 503 containing the test sample. Furthermore, an inert gas replacement device 538 is provided for replacing the internal air with inert gas for NV measurement. Specifically, an N2 cylinder 543 is connected to the side wall of the device main body 501 via a hose 540, and a solenoid valve 542 is used to seal in NZ gas in an amount equivalent to or more than the volatile gas, so that the volatile gas reaches its explosive limit. It is possible to keep it below the value. Next, the operation of the NV measuring device 5 having the above configuration will be explained. 8 and 9 are explanatory diagrams showing the operation of the NV measuring device 5. FIG. When measuring the nonvolatile content of the liquid resin, the nonvolatile content is measured through a series of operations according to a program of the computer 121. That is, the lid 502 is opened by the lid opening/closing mechanism 5'o4, and then the tray 503 is removed from the tray container by the analysis robot 1 via the suction tool 534.
0 analysis robot that takes out the sample, sets it on the balance 50B, and then closes the lid 502! When taking a test sample and dropping it onto the filter paper 509 in the tray 5H, open the lid 502 again.
After opening, a test sample is dropped onto the filter paper 503 via the chip 50 by the analytical robot 1, and a period of time is left after dropping. Then, the test sample is radiated with heat by the heater 50B and N
V measurement is started and the measurement data is sent to the computer 121
The measured data is sent to the computer 121 for processing and displayed in real time, and the measured data after a predetermined period of time is stored in the memory in the computer 121 as NV measured values. During measurement, the volatile components in the test sample gasify and become filled with volatile gas, but since the inert gas replacement device 538 has filled in H2 gas in an amount equivalent to or more than the volatile gas, The toxic gas can be kept below its explosive limit, thus eliminating the risk of explosion. Note that the present invention is not limited to the above embodiments.
For example, in this embodiment, a case has been described in which the lid is closed by its own weight, but the present invention is not limited to this, and the lid may be closed by a weight or a tension spring. [Effects of the Invention] According to the present invention, there is provided an NV measuring device that measures the nonvolatile content of liquid resin, an analytical robot that takes out a tray from a tray container via a suction tool, and sets it in the NV measuring device, and this analytical robot. and a computer unit that controls the NV measurement device, as well as an inert gas purge device, which enables complete automation of NV measurement, improves the performance of one analysis, and improves the reproducibility of measurement data. The effect of eliminating the risk of explosion due to volatile gas and improving safety can be obtained.

[Brief explanation of drawings]

15th! i is a plan view showing an automatic analysis device according to an embodiment of the present invention, FIG. 2 is an explanatory diagram showing a control system of the device,
Figure 3 is a flowchart showing the automatic analysis system;
The figure is a perspective view showing the robot and turntable device,
FIG. 5 is a perspective view showing the external configuration of an NV measuring device according to another embodiment of the present invention, FIG. 6 is a sectional view taken along the line ■-■ in FIG.
FIG. 7 is a block diagram showing the lid opening/closing mechanism, and FIGS. 8 and 9 are explanatory diagrams showing the operation of the NV measuring device. robot 2: analysis station 3: turntable device 4; robot hunt station 5: NV measurement device 5: vacuum device 7: viscosity measurement device 8: pH measurement device 9: washing device 1G = storage device 11: bar coat reader computer Unit tray lid opening/closing mechanism suction tool 506: Balance 538: Inert gas replacement device

Claims (1)

[Claims] In an automatic analyzer that automatically analyzes the viscosity, pH, and non-volatile content of liquid resin using an analytical robot, there is an NV measurement device that measures the non-volatile content of liquid resin, and a tray that is removed from the tray container via an adsorption device and then transferred to the NV measurement device. It is equipped with an analytical robot for setting and taking out after measurement, and a computer unit for controlling the analytical robot and the NV measuring device, and the NV measuring device is equipped with an inert gas replacement device for replacing the internal air with an inert gas. An automatic analyzer characterized by: