JPH01229974A - Automatic analyzer and reaction container - Google Patents

Abstract

PURPOSE:To make it possible to perform stirring of liquid in a reaction container efficiently without carry-over, by arranging the reaction containers wherein stirring balls are contained in a reaction disk, and reciprocating and vibrating the reaction disk in an arc pattern at a high speed. CONSTITUTION:A reaction disk 1 is reciprocated and vibrated in an arc pattern under the adequate conditions. Then, kinetic energy is imparted to stirring balls 4 in liquid in reaction containers 2 which are arranged in the disk 1. The ball 4 starts movement. The direction of the movement is restricted by the inner wall of the container 2. Therefore, the ball 2 is turned in the container 2, and the liquid to be stirred is agitated. In order to obtain efficient stirring, the disk 1 is reciprocated at a high speed under the vibrating conditions wherein the amplitude is 0.8-3.0mm and the frequency is 10-40Hz. The diameter of the ball is made to be one half or less the inner diameter of the container 2. The specific gravity of the ball 4 with respect to the liquid to be stirred is made to be 4 or more. Thus, the adequate stirring without splashing of the liquid out of the container 2 can be carried out.

Description

DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to an analytical device and a reaction vessel, and more particularly to an automatic analysis device and a reaction vessel suitable for stirring a liquid within the reaction vessel.

[Conventional technology]

In conventional clinical automatic analyzers, when stirring the sample and reagent added to the reaction container, for example,
As shown in No. 69, mixing was generally carried out by inserting the same stirring body into the reaction vessels that were sequentially positioned at the stirring position and stirring. However, with such a stirring method, it is difficult to completely remove carryover between the reaction solutions. This led to the idea of non-contact stirring of the reaction solution.

JP-A No. 57-42325 discloses that a disk is provided on the inner circumferential side of a row of reaction vessels arranged on a turntable and contacts the outer walls of a plurality of reaction vessels, and the reaction vessels are moved by reciprocating the disk. This shows a mixing method using driven rotation.

On the other hand, although the stirring device does not have the function of an analyzer, JP-A No. 52-143551 uses
This shows a method in which a large number of diluent chambers are formed in the direction and the Y direction, and the liquid is stirred by applying horizontal vibration to the plate. In this example, considering that complete stirring cannot be achieved by mere vibration, one end of the plate is supported by a support, and an electromagnet or the like is activated to give the plate arc-shaped vibration.

In addition, Japanese Patent Application Laid-open No. 61-56972 discloses a spectrophotometer in which a cell holder with a plurality of sample cells is linearly transferred, each sample cell is sequentially moved to a measurement position, and the cell holder is returned after measurement. , it is shown that forward and reverse rotation signals are alternately applied to the drive source of the cell holder to swing the sample cell in the front and back direction and stir the sample.

[Problem that the invention attempts to solve]

In an automatic analyzer, since a large number of samples must be efficiently processed, a stirring operation must be performed in a short time without carryover between the stirred liquids.

In Japanese Patent Application Laid-Open No. 57-42325, the liquid inside can be stirred by rotating the reaction vessel itself, but the mechanism of the stirring device is complicated. Japanese Patent Publication No. 52-143551
In this method, dilution rods are inserted one after another into each diluent chamber to dilute the sample one after another, and the influence of carryover during stirring is not considered. In Japanese Patent Application Laid-Open No. 61-56972, since the rectangular cell is simply swung back and forth, it takes a relatively long time for the liquid in the sample cell to be sufficiently mixed.

An object of the present invention is to provide an automatic analyzer that has a simple configuration and can efficiently stir the liquid in a reaction container.

Another object of the present invention is to provide an automatic analyzer that can promote the reaction between the sample and reagent by repeatedly stirring the sample and reagent during the period from addition of the sample to measurement of the reaction solution. It is in.

Another object of the present invention is to provide an automatic analyzer that can easily perform stirring without carryover between reaction solutions.

Another object of the present invention is to provide a reaction vessel that can enhance the liquid stirring effect and is easy to handle.

[Means to solve the problem]

In the present invention, reaction vessels containing stirring balls are arranged on a reaction disk, the reaction disk is vibrated by reciprocating at high speed in an arc, and this vibration rotates the stirring ball in the reaction vessel, causing the liquid in the reaction vessel to flow. It was configured to stir.

[Effect]

When the reaction disk is reciprocated in an arc under appropriate conditions, kinetic energy is imparted to the stirring balls submerged in the liquid in the reaction vessels arranged on the reaction disk.

Along with this, the stirring ball starts to move, but the direction of movement is restricted by the inner wall of the reaction container, so the stirring ball rotates inside the reaction container and stirs the liquid to be stirred.

In a preferred embodiment of the present invention, the amplitude is 0.8 to 3.0 mm and the frequency is 10 to 4 mm to obtain efficient stirring.
The reaction disk is reciprocated at high speed under vibration conditions of 0 Hz.

By setting the diameter of the stirring ball to be less than half the inner diameter of the reaction vessel, and by setting the specific gravity of the stirring ball to the liquid to be stirred to be 4 or more, suitable stirring without splashing out of the liquid from the reaction vessel can be carried out.

Furthermore, since a stirring ball is placed in each of the reaction vessels of the first reaction disk and the second reaction vessel, carryover between reaction liquids does not occur through the stirring balls.

When the present invention is practically applied to an automatic analyzer, high photometric accuracy must be obtained.

By forming a pair of smooth light-transmitting windows in the reaction vessel whose inner wall side surface is curved, stable photometric values can be obtained even if the position of the reaction vessel in the optical path of the photometer is slightly shifted. It is also possible to suitably perform the rotational movement of. By forming the stirrer from a ferromagnetic material and arranging the magnet near the photometry position, it is possible to prevent the stirrer from interfering with the optical path when selling the DL.

Since the entire reaction disk is vibrated, the liquids in multiple reaction containers on the reaction disk are stirred all at once.

Since this stirring is performed each time a sample and reagent are added to a new reaction vessel, the result is 1fJ11 from the start of the reaction.
The reaction solution will be frequently stirred for a certain period of time. When the reaction vessel contains an insoluble reagent having a specific gravity different from that of the liquid, the reaction is promoted by such repeated stirring.

〔Example〕

An embodiment of the present invention will be described with reference to FIGS. 1 to 4.

A plurality of reaction vessels 2 are arranged on the circumference of a rotating disk-shaped reaction disk 1, and the reaction disk 1 is rotated by a drive mechanism 3. The drive mechanism 3 enables the reaction container 2 to be rotated intermittently one pitch at a time or to reciprocate in short periods. The reaction disk 1 is reciprocated at high speed with minute amplitude to stir the liquid in one reaction container.

As shown in FIG. 3, a stirring ball 4 made of permalloy is placed in the reaction container 2 mounted on the reaction disk 1 in advance. The reaction vessel shown in FIG. 3 is for fluorescence photometry. The upper end of the reaction vessel 2 is sealed with an aluminum membrane 5, so that the stirring ball 4 will not jump out of the reaction vessel 2 during transportation. It has a smooth entrance window 24 on the bottom and a smooth exit window 25 on the side. This reaction vessel 2 is made of a transparent material such as glass or acrylic resin.

When the reaction container 2 is set on the reaction disk 1, a hole 5a of a desired size is made in the seal membrane 5 by a seal breaker device (not shown). Therefore, after that, the dispensing mechanism 1
The sample and/or reagent dispensing operation performed by the probe 15 of No. 4 is as follows.

unobstructed by sealing membrane 5.

Inside the reaction constant temperature bath 6, a permanent magnet or electromagnet 7 is arranged near the photometry position of the photometer 19, as shown in FIG.

Since the magnet 7 attracts the stirring ball 4 in the reaction vessel that has come to the photometry position to the side wall opposite to the exit window 25, the stirring ball 4 does not obstruct the passage of the light beam 22.

On the other hand, a rotating disk-shaped sample disk 8 and a rotating disk-shaped reagent disk 9 are arranged concentrically, and the sample disk 8 and the reagent disk 9 are simultaneously and integrally driven to rotate by a central drive shaft 10. do. In addition, although the sample disk 8 is provided on the center side and the reagent disk 9 is provided on the outer circumferential side in the illustration, it is also possible to provide the sample disk 8 in the opposite direction.

A plurality of sample containers 11 are arranged on the sample disk 8. Further, on the reagent disk 9, a reagent container group 12, which is a group of several types of reagent containers, is arranged.

In the reagent container 12, a first reagent, a second reagent, etc. for a specific analysis item are arranged as a group. The reagent disk 9 and sample disk 8 are configured to rotate around a drive shaft 10, and the reagent container 12 and sample container 11 are rotated by one pitch or a specified number of pitches. Further, the reagent container 12 and the sample container 11 are set so that they can be attached and removed separately depending on the object to be analyzed. Also, sample container 1
1 in a sample constant temperature bath, and the reagent container 12 in a reagent cold storage bath] 3 to maintain a predetermined temperature.

A pipetting mechanism 14 is provided for dispensing the sample, target substance, or reagent described above from the sample container 11 or the reagent container 12 into the reaction container 2, respectively. The pipetting mechanism 14 includes a probe 15 at the tip of a rotary arm 14a, sucks up a sample or reagent with the probe 5, rotates the probe 15, and discharges it into the reaction container 2 located at a sample and reagent dispensing position 16. . At this time, the sample container 11 or reagent container 12 to be dispensed once is arranged in the movement trajectory of the probe 15 of the pipetting mechanism L 11, and the sample disk 8 or reagent disk 9 is rotated and moved by the drive shaft 10. Make it stop on the trajectory.

Further, a probe cleaning device 17 is provided, and cleaning water is pumped to the inside and outside of the probe 15 to thoroughly clean it.

A predetermined amount of sample is aspirated by the probe 15 from the sample container 11 on the sample disk 8 by the pipetting mechanism 14, weighed, and transferred to the reaction container 2 at a designated position on the reaction disk 1 and discharged.

After discharging, the probe 15 of the pipetting mechanism 14 is thoroughly cleaned by the cleaning device 17 to prevent contamination due to sample liquid carryover. Next, move the reaction disk 1 back and forth at high speed! The frequency of the II drive mechanism 31 is 33 Hz.

After reciprocating for 3 seconds with an amplitude of 1.2+nm, it is rotated so as to advance by 1 pinch.

As shown in FIG. 1, the high-speed reciprocating drive mechanism 3 uses a step motor 3a as a power source, and is connected to the rotation of the reaction disk 1 @3C by a gear or a connecting belt 3b. Of course, it is also possible to integrate the rotational shaft of the step motor 3a and the rotational shaft 3C of the reaction disk, and in that case, neither a gear nor a connecting belt is necessary. The operation of the step motor 3a is controlled by a central processing unit 18.
It rotates by 5 pulses each in the forward and reverse directions in m seconds,
By repeating this for 3 seconds, one reaction disk is reciprocated at high speed at a frequency of about 33 Hz. As a result, the reaction vessel also reciprocates at high speed at about 33 Hz, and by using a reaction disk with a diameter of about 300+nn+, an amplitude of about several Ill Il+ can be obtained depending on the gears. This high-speed reciprocating drive mechanism 3 is also used to rotate one reaction disk for step feeding and move the reaction container 2 to the target position, while moving the sample disk 8 to the pipetting position for the next aspiration. Rotate to. By sequentially repeating this operation, a required number of sample liquids are first transferred and dispensed into the reaction container 2. Next, the reagent solution is similarly aspirated from the reagent container 12 by the pipetting mechanism 14 and dispensed into the reaction container 2 at the sample and reagent dispensing position 16.

Next, the reaction liquid in the reaction container 2 is stirred by reciprocating the reaction disk 1 for 3 seconds by the high-speed reciprocating drive mechanism 3, and then transferred one pitch rotation.

The reagents are sequentially transferred and dispensed starting from the first reagent in the reagent series of the reagent container group. In this manner, the reaction disk 1 is rotated in a specified manner, and the sample and reagent are dispensed into the reaction container 2 in batches. A biological fluid such as serum, plasma, or urine is used as the sample.

As the reagent, the same reagent that is commonly used can be used.

At the sample and reagent dispensing position 16, the sample and reagent sequentially dispensed into the reaction vessel 2 start reacting within the reaction vessel 2. For example, the interval at which one reaction container is transferred is 18
If the reciprocating drive time of the reaction disk 1 is 3 seconds, all the reaction vessels on one reaction disk 1 will move 3 seconds every 18 seconds.
It will repeat the reciprocating motion for seconds. As a result, the reaction liquid in all reaction vessels is stirred for 3 seconds every 18 seconds during the entire reaction process. Reagent dispensing position 1
When a coloring reagent is added to the reaction vessel in step 6, a magenta reaction proceeds.

The photometer 19 is a multi-wavelength simultaneous J1 light type having a plurality of detectors, and the reaction vessel facing the reaction vessel 2 and located at the photometry position 20 on the reaction disk 1 passes the light beam 22 from the light source lamp 21. is configured to do so.

In FIG. 1, the light from the light source lamp 21 is transmitted through the lens 2.
3a and 23b, and enters the reaction liquid in the reaction vessel 2 through the entrance window 24 on the bottom of the reaction vessel 2 as excitation light. The fluorescence emitted from the reaction solution is emitted through the exit window 25 of the reaction container.
The fluorescence intensity is detected by the first multiplier 26 after passing through the lens 23c. By the movement of the reaction disk 1, reaction vessels are positioned one after another at the optical position 20, and the fluorescence intensity based on each sample is measured by the photometer 19. For the output of the photometer 19, a signal of the currently required measurement wavelength is selected by a multiplexer.
The data is taken into the central processing unit 18 by the A/D converter 27 and stored in the RAM.

The series of operations from dispensing the sample and reagent to the end of the measurement is shown in a flowchart in FIG. 4, including the stirring operation by high-speed reciprocating motion.

The central processing unit 18 is a microcomputer that controls the entire dosage including the mechanical system and performs general data processing such as concentration calculation.

The effect of stirring the reaction solution on the progress of the chemical reaction is shown in FIG. Total stirring time during the entire reaction process from addition of the first reagent to itl'l light and reaction progress results when the theophylline measurement reagent similar to Experimental Example 1 and theophylline standard solution 30 μg / m Q were reacted. The relationship between the resulting fluorescence intensities is shown. In FIG. 5, data A shows the data when the reaction solution was stirred for 3 seconds every time the reaction container was transferred by one pinch using the automatic analyzer of this example, and the sample and reagent were mixed. The reaction solution is continuously and thoroughly stirred during the entire reaction process from the time the reaction is initiated to photometry. Data B corresponds to the case where a conventional automatic analyzer is used, but the reaction solution is stirred only once per reaction step.

As is clear from Figure 5, the reaction solution was stirred frequently (
That is, as the total stirring time was increased (longer), the reaction was accelerated and the fluorescence intensity generated as a result of the reaction increased significantly. However, even if attempts were made to stir more frequently than the stirring conditions (conditions of data A) adopted by the automatic analyzer of the present invention.

In FIG. 5, the fluorescence intensity obtained as shown in data C was almost the same as data A, and no further promotion of the reaction was observed. This revealed that data A was the point at which the reaction proceeded most efficiently due to frequent stirring. Based on the above results, stirring the reaction solution during the reaction process has a great influence on promoting the reaction, and it is important to continuously stir the reaction solution throughout the reaction process as in the automatic analyzer of this example. It is clear that the progress of the reaction is significantly accelerated.

In addition, if the reaction solution contains components that are insoluble and have poor dispersibility, it is necessary to prevent sedimentation and accelerate the reaction by stirring frequently. , the stirring method described above is useful.

When using the reaction vessel 2 containing a stirrer in advance, various materials such as an aluminum film, a polyethylene film, and a silicone film can be used as the sealing material. In order to prevent the seal 5 from interfering with the dispensing of the sample or reagent using the dispensing probe 15, a seal breaker is provided separately from the dispensing probe to easily break the seal 5, so that the reaction of the sample or reagent is prevented. The seal 5 may be broken prior to dispensing into the container, or the seal may be broken with the dispensing probe 15.

As the material of the reaction container 2, glass or plastics can be used. The container needs to have strength, low adsorption of reaction reagents and samples, low cost, and good translucency especially when directly photometrically measuring the reaction solution, and acrylic resin can be suitably used.

Although permalloy was used here as the material for the stirrer 4, any material having a specific gravity relative to the solution to be stirred greater than 1 can be used as a stirrer without twisting. The stirring effect can be increased by changing the size of the stirring bar depending on the volume and viscosity of the solution to be stirred. However, for materials such as iron that rust easily, or materials that cause chemical reactions with the solution and adversely affect the original reaction, surface treatment such as plastic coating or plating is required for the stirrer.

When performing direct photometry, if a ferromagnetic material such as iron or permalloy is used, the light flux 22 can be easily avoided by the magnetic force of the magnet. In this case, regardless of whether the whites react or not, if a ferromagnetic substance is involved in the reaction, for example in a reaction using an iron catalyst, if residual magnetism remains in the stirrer 4, the ferromagnetic substance in the reaction solution will It is conceivable that the stirring bar 4 may be adsorbed and adversely affect the reaction. In this case, it is necessary to use a material with minute residual magnetism as the stirrer 4. Permalloy has little residual magnetism and is suitable for reactions where residual magnetism is a problem like this. The shape of the stirrer is preferably approximately spherical.

Next, FIG. 6 shows the effects of high-speed reciprocating conditions, the shape of the reaction vessel 2, the shape of the stirrer, etc. on the stirring efficiency.

This will be described with reference to FIG. In FIG. 6, the amplitude of high-speed reciprocating motion is plotted on the vertical axis and the frequency is plotted on the horizontal axis, and the range of high-speed reciprocating motion conditions that provide different stirring efficiencies is divided by A-E.

In the case of a spherical stirrer (hereinafter referred to as a stirring ball), Figure 6A
, B, and E are applied to the cylindrical reaction vessel 35, the stirring ball 4 performs a revolving motion along the inner wall surface of the cylindrical vessel 35, as shown in A of FIG. According to such a revolving movement of the stirring ball 4, stirring is completed within 3 seconds when the liquid depth is within 10 times the diameter of the stirring ball.

This is because a vortex is generated in the solution due to the revolution of the stirring ball 4, and results similar to those obtained with a portex mixer or a magnetic stirrer can be obtained.

Even with the same high-speed reciprocating motion, if the reaction container has a square prism shape and the bottom surface is flat, stirring can only be carried out to a height of 2 to 3 times the diameter of the stirring ball 4 (FIG. 7B). However, if the stirring ball 4 is made to reciprocate at high speed in the diagonal direction of the square prism under the same conditions, the stirring ball 4 will move around two-dimensionally on the bottom surface of the square prism container 36, as shown in FIG. If the liquid depth is within twice the depth, stirring will be completed in about 5 seconds.

When a reciprocating motion having a frequency and amplitude in the range shown in FIG. 6C is applied to a flat-bottomed reaction vessel, the above-mentioned revolving motion of the stirring ball 4 no longer occurs in the cylindrical vessel 35 as shown in FIG. 7. Therefore, when the liquid depth is within 10 times the diameter of the stirring ball 4, a stirring time of 3 to 20 seconds is required. 7th
As shown in Figure E, when the rectangular prism container 36 is reciprocated at high speed in the lateral direction, stirring can only be performed up to a height approximately twice the diameter of the stirring ball 4. However, as shown in FIG. 7F, even when the square columnar container 36 is reciprocated diagonally at high speed, it is possible to obtain a stirring efficiency approximately equal to that of a cylindrical container.

Even if high-speed reciprocating motion having a frequency and amplitude in the range D shown in FIG. 6 is applied to a reaction vessel with a flat bottom, stirring will only be possible to a height approximately twice the diameter of the stirring ball 4. However, as shown in FIGS. 7G and 7H, if a step having a height approximately equal to the radius of the stirring ball 4 is provided on the inner periphery of the bottom surface, vertical movement is added to the horizontal movement of the stirring ball 4, and the stirring efficiency is improved. As an alternative to this step, a recess (I, J in FIG. 7), a horizontal step on the bottom surface (L in FIG. 7), or other bottom shape can be considered. In this case as well, the cylindrical container 35 (FIG. 7 G, I,
K) is better than the square prism container 36 (Fig. 7 H1J, L).
Good stirring efficiency. This means that when the collision angle between the stirring ball 4 and the reaction container is projected onto the bottom surface, it is always 9 in the square prism container 36.
0', whereas in the case of the cylindrical container 35, the angle is O°
This is because the range of movement of the stirring ball 4 is widened since it can take various angles from 90' to 90'. In this case as well, if the rectangular prism container 36 is reciprocated diagonally at high speed, the stirring efficiency will be approximately the same as that of the single cylindrical container 35.

When a rod-shaped stirring bar 37 is used as shown in FIGS. 7M and 7N, the solution can be moved over a wide range at the same time, so that stirring can still be achieved. When the rod-shaped stirrer 37 is used, the movement range of the rod-shaped stirrer 37 is widened and the stirring efficiency is improved as in the case where the stirring ball 4 is used, but this is not preferable in terms of photometry.

In the case of direct photometry, if steps or depressions are made on the bottom surface as described above to cause the stirring ball 4 to move up and down, or if a rod-shaped stirring bar 37 is used, the translucent surface on the side of the reaction vessel 2 can be used. It is inappropriate as it may damage the person. Furthermore, considering the stirring efficiency, when using a cylindrical container,
The frequency and amplitude ranges of and B are suitable for stirring. However, in the range A, the high-speed reciprocating motion is too intense, and there is a possibility that the solution will scatter from the reaction container. Therefore, B in Figure 6
This means that the range is suitable for practical use.

When actually applying high-speed reciprocating stirring to an automatic analyzer,
For example, when reciprocating with an amplitude larger than one step,
When performing direct Al11 light while reciprocating at high speed, the reaction vessel may be removed from the light beam, making measurement difficult.
Furthermore, when the reaction vessel 2 containing the ferromagnetic stirrer 4 is located next to the il+'1 light section where the magnet 7 is arranged, the reaction vessel 2 reciprocates between the magnet 7 position and the position without the magnet 7. This causes problems such as bubbling and scattering of the solution. Therefore, it is desirable that the amplitude be smaller than one step.

As is clear from FIG. 6, as the frequency increases, the range of the amplitude of B becomes narrower. This is because the amplitude variation in the high-speed reciprocating motion of the reaction vessel caused by variations in gear engagement in the high-speed reciprocating drive mechanism 3 of the reaction disk is 1.
It's a few tenths of a millimeter.

This indicates that the vibration conditions for high-speed reciprocating motion shift from the appropriate range B to inappropriate ranges A, C, and D, and stable stirring cannot be obtained.

Taking these into consideration, it has been found that the range E in FIG. 6 is suitable for the high-speed reciprocating conditions of the reaction vessel that should be applied to the automatic analyzer. That is, the amplitude is 0.8 to 3. Oa
u++, and a frequency of 10 to 40 Hz is appropriate.

FIG. 8 shows the relationship between the liquid depth and the specific gravity of the stirring ball relative to the solution to be stirred (hereinafter referred to as the specific gravity of the solution) necessary to stir the solution at that depth for 3 seconds.

The vertical axis shows the specific gravity of the stirring ball relative to the solution to be stirred, and the horizontal axis shows the ratio of the liquid depth to the diameter of the stirring ball.

The specific gravity of the stirrer material relative to the solution to be stirred, which is necessary to perform sufficient stirring with a stirring time of about 3 seconds, increases as the amount of the liquid to be stirred increases. In the case of the stirring ball 4 in Fig. 1, when the liquid depth is about the diameter of the stirring ball 4, the stirring ball 4
requires a specific gravity to the solution of about 1.5, but when the liquid depth becomes about 15 times as deep, a stirring ball with a specific gravity to the solution of about 4 is required to stir this for 3 seconds.

Further, even if the specific gravity of the stirring ball 4 to the solution is set to 4 or more, the stirring efficiency remains almost the same. From this, stirring ball 4
In general, stirring of a solution by reciprocating the reaction vessel 2 at high speed, not only stirring by A suitable stirrer is suitable.

The upper limit of the specific gravity to the solution is practically about 20, since most of the cheap materials such as iron, copper, and tungsten have a density of 20 g/cm" or less. Therefore, the specific gravity to the solution is practically suitable for the stirring bar 4. It can be seen that the range of is 4 to 20.

It has been found that the relationship between the radius of the stirring ball and the inner radius of the cylindrical container that can be stirred using this ball is expressed by the following equation.

D≦4 (Az+d), D≧1.1d (d<10) D≧d
+ 1 (d≧10) where, A2: both amplitudes (twice the amplitude) (m,,)
.

d: Stirring ball diameter (mm), D: Cylindrical container inner diameter (mm) Considering that the size of the reaction container applied to automatic analyzers is generally 30o+n+ or less, this is the range in which stirring efficiency is excellent. In this case, both amplitudes A2 are 7.5 mm or more.

1.48d≦D≦4.4d (A2≧7.5), when both amplitudes A2 are 7.5mm or less
AZ, 4AZ), (2,73AZ, 4A2),
The interior of the triangle formed by joining the three points (0, O) and (
0,909A2.4A2), (2,73A2.4A2)
.

(22,2-0,25A, 30), (12,5-0,
75A2.30).

((0, 909Ax, 4 A2)) It turns out that the interior of a trapezoid is formed by connecting the four points in this order.

FIG. 9 is a graph showing the relationship between the ability to stir and d when both amplitudes A2 are 2 mm. The vertical axis is the inner diameter D of the cylindrical container.
(am), and the horizontal axis is the stirring ball diameter d (n+m). The range A indicates a range that can be stirred, and the range B indicates a range particularly suitable for automatic analyzers.

FIG. 11 shows the configuration of an example in which the transmitted light characteristics of a reaction solution are measured using the reaction vessel 2a shown in FIG. 12. Components having the same functions as those in the embodiment shown in FIG. 1 are given the same reference numerals. The cylindrical reaction vessel 2a of the 12th UA is formed with an entrance window 24a and an exit window 25'a that are parallel to each other. When measuring transmitted light, the stirring bar 4 sinks to the bottom of the reaction vessel 4 as shown in Figure 11, so by setting the light flux position above the stirring bar, light blocking by the stirring bar can be prevented. can do. In this case, the material of the stirring ball 4 is not limited to ferromagnetic material, but also aluminum,
Metals such as copper, non-metals such as glass, and magnets can also be used.

FIG. 13 shows various shapes of reaction vessels. A plurality of flat transparent windows are formed on the side surface of the cylindrical container. Figure 13A
A substantially cylindrical container having two planar light transmission windows facing each other on the side surface of the cylindrical reaction container 2 can be used for light absorption measurement, as shown in FIG.
The one in which the two light transmitting windows form an angle of 90' to each other, as shown in Figure 13B, can be used for fluorescence measurements;
A structure in which three planar light transmitting windows are arranged at 90° intervals as shown in Figure C can be used to simultaneously measure light absorption and fluorescence.

Experimental Example 1 An example in which theophylline was analyzed using the automatic analyzer shown in the example of FIG. 1 will be described.

As a reagent, Ames TDMT''I theophylline kit (manufactured by Miles Sankyo Co., Ltd.) was used.

Theophylline standard solution (0°10.20
．． 30 and 40 μg/mQ) were placed in the sample container 11 and set. Also, on the reagent disk 9 are reagents for measuring theophylline (first reagent: β-galactosidase and anti-theophylline antibody).

Second reagent: Fluorescently labeled theophylline (β-galacto
syl -umbelliferone-theop
hylline)) was set.

After 50 μQ of the sample and 250 μQ of the first reagent were mixed and reacted for 36 minutes, 50 μQ of the second reagent was added, and 5 minutes later, measurement was performed at an excitation wavelength of 400 nm and a fluorescence wavelength of 450 nm. FIG. 10 shows a standard curve prepared by plotting the theophylline concentration of the measured standard solution on the horizontal axis and the fluorescence intensity of the measured standard solution on the vertical axis.

〔Effect of the invention〕

As explained above, according to the present invention, it is possible to efficiently stir the liquid in the reaction container with a simple configuration, and since there is no need to share a stirring bar, stirring can be performed without carryover. .

[Brief explanation of the drawing]

Figure 1 is a schematic diagram of the main parts of the embodiment shown in Figure 2;
3 is a partially cutaway sectional view of a reaction vessel for fluorescence photometry, and FIG. 4 is a 11 constant operation process similar to the embodiment of FIG. 2. Flowcharts 1 to 5 are graphs showing the relationship between stirring time and fluorescence intensity, and Figure 6 is a classification diagram of vibration conditions due to high-speed reciprocating motion.
Figure 7 is a diagram showing the movement of the stirrer under the conditions of Figure 6, Figure 8 is a graph showing the relationship between the liquid depth and the amount of liquid that can be stirred with respect to the diameter of the stirring ball, and Figure 9 is a graph showing the relationship between the stirring ball diameter and the amount of liquid that can be stirred. A graph showing the relationship between the inner diameter of the stirrable cylindrical reaction vessel and the diameter of the stirring ball in the case of FIG. 10 is a graph showing the theophylline standard curve measured using the embodiment apparatus of FIG. FIG. 12 is a diagram showing the structure of the reaction vessel for light absorption direct photometry used in the example of FIG. 11, and FIG. 13 is a diagram showing various forms of the reaction vessel. FIG. 2 is a schematic diagram illustrating an example. DESCRIPTION OF SYMBOLS 1... Reaction disk, 2... Reaction container, 3... Drive mechanism, 4... Stirring ball or stirring bar. 5...Seal,
8...sample disk, 9...reagent disk, 14.
... Pipetting mechanism, 15... Probe, 18...
Central processing unit, 19... Photometer, 20... Photometry position, 24... Entrance window, 25... Output window. Y j 口 3rd 4I2I 5th ward rounding paper time (枦wo 4th figure circumference 'l k (ng 8th ward rising q mouth to ED 1 1 ■ O/θ 20 3θ Mukute spear fin feather Naon Koh (11, counterfeit horn ￥11 unillustrated 12-figure)

Claims (1)

[Claims] 1. A plurality of reaction vessels each containing a stirrer made of a ferromagnetic material, a reaction disk in which the plurality of reaction vessels are arranged, and an intermittent transfer motion and short-period reciprocating motion on the reaction disk. a drive device that applies vibration based on motion; a device that supplies a sample and a reagent to the reaction container; a photometer that irradiates the reaction container with light and measures the reaction liquid in the reaction container; An automatic analyzer equipped with a magnet that is disposed near a photometric position and attracts a stirrer in the reaction vessel positioned at the photometric position to a wall surface of the reaction vessel so that the stirrer does not obstruct the optical path of the photometer. 2. Arrange reaction vessels containing stirring balls on a reaction disk, vibrate the reaction disk by reciprocating it in an arc at high speed, and use this vibration to rotate the stirring ball in the reaction vessel, causing the inside of the reaction vessel to rotate. An automatic analyzer characterized by stirring a liquid. 3. In the device according to claim 2, the vibration has an amplitude of 0.8 to 3.0 mm and a frequency of 10
An automatic analyzer characterized in that the frequency is ~40Hz. 4. The automatic analyzer according to claim 2, wherein the specific gravity of the stirring ball relative to the liquid in the reaction container is 4 or more. 5. The automatic analyzer according to claim 2, wherein the inner diameter of the reaction vessel is at least twice the diameter of the stirring ball. 6. Arrange a plurality of reaction vessels containing stirrers on a reaction disk, add samples and reagents to the corresponding reaction vessels at predetermined positions while the reaction disk is stopped, and apply a short cycle to the reaction disk. By vibrating the reaction disk in a continuous reciprocating motion, the liquids in the plurality of reaction vessels are stirred, and by stepping the reaction disk, the reaction vessels to which the sample and reagent have been added are photometered. An automatic analyzer configured to advance toward a location. 7. A reaction vessel in which at least a part of the inner wall side surface is curved and has a pair of smooth light-transmitting windows, and a substantially spherical stirrer is housed inside, and a stirring bar is provided at the upper end to prevent the stirrer from escaping. Reaction vessel with membrane.