JPS6064256A - Degassing equipment for automatic analyzers - Google Patents

Abstract

(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

[Detailed Description of the Invention] [Field of Application of the Invention] The present invention relates to an automatic analyzer, and in particular to a degassing device for degassing cleaning water for cleaning a dispenser that dispenses a reagent to a sample in a reaction container. The present invention relates to an automatic analyzer equipped with a device.

[Background of the invention]

FIG. 1 is a block diagram of a conventional reagent pipetting type automatic analyzer. Which device is suitable for handling multiple samples in small quantities, and employs a reagent pipetting method in which different reagents are dispensed one after another using a small number of dispensers.

Next, an overview of its configuration and operation will be explained.

A combination table 2 on which a large number of sample containers 1 are arranged on a concentric circle and a reaction table 4 on which a large number of reaction containers 3 are arranged on a concentric circle are installed adjacent to each other. They rotate intermittently in relation to each other. A sample sampling nozzle 5 is installed on the side between these two tables 2 and 4, and a pipetter 6
The suction and discharge operations are repeated by the operation of a, but during this time the sampling nozzle 5 rotates according to the command from the computer 19, sucking a certain amount of the sample in the sample container 1 of the sample table 2 (reaction table 4). Upper reaction vessel 3
Discharge to. After the dispensing operation is finished, the inside and outside of the sampling nozzle 5 are cleaned by a cleaning device (not shown).

The reaction table 4 rotates intermittently by a predetermined angle,
During this time, the 1 inch moving mechanism Ba, 13b attached to the reagent nozzle 7 moves from side to side, extracts a predetermined amount of reagent from the reagent bottle 10 housed in the cold storage 1, and adds it to the reaction container 3. . Note that the reaction table 4 is equipped with a constant temperature water circulator 11.
Since the reaction container 3 is connected to the thermostat 12 and rotates in a constant temperature bath 12, the reaction container 3 is incubated (warmed) for a predetermined period of time, and finally stirred by the agitator 13 to complete the reaction. .

When the reaction container 3 is rotated to a predetermined measurement position, the light from the light source 14 is transmitted through the multi-wavelength photometer 15.
to be introduced. The light is dispersed by the concave diffraction grating 16 of the multi-wavelength photometer 15, and the amount of bright line light is detected by a plurality of light receiving elements 17 installed on the spectrum coupling surface. This light receiving element 17 detects the absorbance proportional to the amount of the test component in the sample liquid, and the detected value is transmitted to the A-D converter 1.
8, it is converted into a digital quantity, sent to the computer 19, and displayed on an output device such as a printer 20a or a cathode ray tube 20b. Note that the pipetter 6b operates and the reagent nozzle 7
After inhaling the reagent, the reagent nozzle 7 moves to the moving mechanism 8a'
, 8b between the reaction vessel 3 and the washer 21, and is cleaned after applying the partial pressure of the reagent.

In such a pipetting type automatic analyzer, the pipetter 8b operates to aspirate and dispense the required number of reagents, so the entire amount of the inhaled reagent can be added to the reaction container 3, and there is no waste. In addition, the reagent nozzle 7 can be easily cleaned with the washer 21, and since the rotating disk type reaction table 4 is used, there is an advantage that the entire apparatus can be made compact. However, on the other hand, the reagent nozzle 7 is moved to the reagent bottle 1 by the moving mechanisms 88 and 8b.
0. It is necessary to reciprocate between the reaction container 3 and the washer 21 in a timely manner, and the moving mechanism 8a.

As the number of simultaneous analysis items increases, that is, as the number of reagents increases, the operation time becomes longer and the dispensing processing speed decreases. However, since there is a limit to the operating speed of the reagent nozzle 7, it is not possible to increase the number of measurement items within a unit time, and the cleaning time of the reagent nozzle 7 is limited. There are disadvantages such as the shortening of the time period, which may cause cross-contamination, and furthermore, the carryover between the washing water and each reagent may cause the concentration of the reagent to decrease.

In particular, cross-contamination between reagents occurs when specific components in the reagents are electrically or physically adsorbed to the metal nozzle, and the solution to this problem is extremely internal.

By the way, the following dispenser has been proposed as a solution to this problem. FIG. 2 is a diagram showing the principle of the dispenser.

This dispenser is roughly divided into four elements.

The first is a switchback type dispensing flow path. This dispensing channel includes three-way switching valves 22a to 22h, suction tubes 23a to 23h, and discharge tubes 248 to 2411, respectively.
, discharge nozzles 258 to 25h, and escape tubes 26a to 26h for switches ♂. Each suction tube 23a to 23h and discharge tube 24a to 24h are
Each evacuation tube 26a~
The volume of 26h is larger than the volume of the syringe 27 at full stroke.

In the example of FIG. 2, each suction tube 23a to 23h
and discharge tubes 248 to 241] each have an inner diameter of 0.8
Q. Each retraction tube 26a to 2611 is a Teflon tube with a length of 1000mm (inner volume 500μt) and an inner diameter of 1.5mm and a length of 1500mm (inner volume 2.6mm).
5m1) Teflon tube.

The second component is a multiple flow path switching valve (hereinafter abbreviated as multiple valve) 28, which connects the discharge side flow path of the syringe 27 and any one of the evacuation tubes 268 to 26h. It has the function of selectively conducting the liquid, and the function of waste liquid when cleaning the common flow path from the inlet of the syringe 27 to the sliding surface of the valve before conducting the liquid to each of the evacuation tubes 26a to 26h.

The third component is the syringe mechanism, which is the syringe 271. @The driving rack mechanism 29 and the driving pulse motor 3o are also included.

The fourth component is a cold storage 31, which is indicated by a dashed line in FIG. Most of the reagents are stored and kept cool at 25 to IFI' to prevent deterioration of the reagents.

Next, the operation of the dispenser shown in FIG. 2 will be explained. First, before use, old reagents remaining in all channels other than the tubes 23a to 23h are washed and discarded. That is, all the three-way switching valves 22a to 22h are switched to the discharge side, the wash water supply valve 32 is opened, and the multiple valve 28 is sequentially switched to Q1.
→Qo→Q2→Qo・・・・・・Q7→Qo−+Q8, and pass through the syringe 27 and the multiple valve 28 to the escape tubes 26a to 26h of each switchback type partial pressure flow path
and all discharge tubes 24a to 24h.

Once cleaning is complete, replace all switchback dispensing channels with new reagents by performing the following steps.

(1) Close the wash water supply valve 32, switch the three-way switching valve 22a to the suction side, set the multiple valve 28 to position Q, and make the syringe 27 take a full stroke (3 ml). .

(2) Switch the three-way switching valve 22a to the discharge side to make the syringe 27 full-stroke discharge.

(3) Switch the three-way switching valve 22a to the suction side again to make the syringe 27 full stroke suction.

(4) Set the multiple valve 28 to the intermediate point Qo and use the syringe 2
7 is a full stroke discharge (at this point, the reagent in the reagent bottle 10a for 1 ml is aspirated into the evacuation tube 26 = 2), and this is always retained during subsequent use as a dummy to prevent dilution. ).

(5) Set the multiple valve 28 to Ql again, set the three-way switching valve 22a to the suction side, and set the syringe 27 to a total of 300 μm.
After inhalation at t (maximum discharge in use condition), the three-way switching valve 22a is set to the discharge side and the same amount of 300 μt is discharged.

(6) Repeat the operation in (5) above for one more line.

(7) Set the multiple valve 28 to the intermediate point Qo, open the cleaning water supply valve 32, and clean the common flow path from the syringe 27 to the multiple valve 28 with cleaning water (the cleaning water is supplied to the multiple valve 28). It is discharged from the waste liquid port, and the above-mentioned liquid is in the evacuation tube 26a.
The reagent in the ml reagent bottle 10a is held, and the suction tube 23a, +? I: Output tube 24a1 discharge/X tube 25a
is completely filled with the above reagents).

As a result of the above-mentioned (1) to (force operations), the switchback type dispensing channel at the top of FIG.

Next, the multiple valve 28 is set to the 1.92 position, the three-way cut-off percentage valve 22b and the syringe 27 are operated, and the above (1)
) to (7), the switchback type dispensing channel in the second stage of FIG. 2 is filled with the reagent in the reagent bottle 10b. Furthermore, the multiple valve 28. +1i+ in position 3~Q8
Next, set all the switchback type dispensing flow paths to reagent bottles 10C to 1, respectively, and perform the same operation.
Fill with reagent within 0h. In short, for each reagent 2.
All dispensers are ready for use by only consuming 6 ml f. In use, only the required amount of reagent is inhaled and dispensed at all times, so the amount of loss of each reagent in this dispenser is 2.5 regardless of the number of samples processed.
ml.

FIG. 3 is a block diagram of an automatic analyzer using the dispenser shown in FIG. 2. The same parts as in FIGS. 1 and 2 are denoted by the same reference numerals, and the explanation thereof will be omitted here. In this apparatus, a plurality of switchback type dispensing channels shown in FIG. 2 and a cold storage 31 for holding all reagent bottles are provided above the reaction table 4. The syringe, multiple valve, and wash water supply valve are 27al, 27bl, 28a, and 28b, respectively.

Two lines, 32a and 32b, are provided. In addition, 27G is a syringe for specimen sampling, and 32C and 32d are washing water supply valves for the syringe.

After all the switchback type dispensing channels are filled with new reagents by the preparatory operation described above, the entire measurement operation is started. That is, a certain amount of the sample in the sample container l at a predetermined position on the sample table 2 is collected into the reaction container 3 at a predetermined position on the reaction table 4 by the operation of the sampling nozzle 5 and the sample sampling syringe 27C. Ru. Every time the reaction table 4 rotates one pitch, a necessary sample is collected into the next reaction container 3. When the reaction container 3 in which the specimen was collected reaches a predetermined reagent addition position, the two systems of dispensing systems described above operate to add the necessary amount of the necessary reagent to each reaction container 3. For example, assuming that it is necessary to add 250μ of the reagent in the reagent bottle 10b in FIG. Switch the switch 22b to the discharge side and dispense the same amount of 250μ.
The reagent t is discharged into the reaction container 3b. At this time, the evacuation tube 26b retains the reagent in the reagent bottle 10b for 1 ml, which prevents the 250 μm of reagent that is inhaled and dispensed from being diluted by mixing with the wash water. ing.

When dispensing of the reagent is completed, the three-way switching valve 22b'f - suction side and the multiple valve 28 are set to the Qo position, the wash water supply valve 32 is opened for a certain period of time, and the multiple valve 28 is discharged from the syringe 27.
The common flow path up to the sliding surface is cleaned in preparation for the next necessary reagent intake and discharge.

Cleaning this common flow path is one of the important points of this type of device. However, the evacuation tube 268
~26h of volume 4'R'r No matter how you stir it up, if you repeat the inhalation and ejection operations many times, each reagent will diffuse into the common flow path from the multiple valve 28 to the syringe 27. In addition to causing contamination between reagents, mutual reactions may destroy the partial pressure system.

Note that the flow path from the aforementioned sample sampling cylinder 27C to the sampling nozzle 5 is also cleaned with the cleaning water as required (in the case where the sample is changed).

In this way, the reaction container 3 to which the specimen and reagent have been added as appropriate
When the light beam advances to the optical axis position of the multi-wavelength photometer 15, it is measured using the wavelength and photometry method (end point assay, rate assay, etc.) determined for each measurement item.

After the measurement is completed, the reaction vessel 3 is cleaned by a cleaning mechanism 33, cleaning 1 polishing 2
1 and subjected to measurement of a new specimen.

By the way, in a normal automatic analyzer, deionized water or distilled water is used as washing water, but in the case of the automatic analyzer shown in FIG. Microscopic air bubbles are generated in the common flow path, and as time passes,
This causes the fatal problem of reducing the reproducibility of the amount of each reagent added because it acts as a damper during the suction and discharge operations of the cylinder 27. This is because while the supplied deionized water or distilled water is below room temperature, the temperature inside the automatic analyzer rises to 40-50C due to heat radiation from various electrical components. This is due to the air being released and forming bubbles.

By the way, even if all the deaerated cleaning water is prepared in advance, it is not practical to store or transfer the water completely without contact with air.

[Purpose of the invention]

The present invention has been made in view of the above, and an object of the present invention is to provide an automatic analyzer that can prevent air bubbles from being generated when a dispenser is washed with washing water.

[Summary of the invention]

A feature of the present invention is that the cleaning water used for cleaning the pressure divider for dispensing reagents into reaction vessels is degassed so that dissolved air does not form bubbles in any condition within the operating temperature range of the dispenser. The point is that the structure is equipped with a device.

[Embodiments of the invention]

The present invention will be explained in detail below using the embodiment shown in FIG.

FIG. 4 is a system diagram showing an embodiment of the deaerator for deaerating the washing water of the automatic analyzer of the present invention. The explanation will be omitted here. In FIG. 4, 40 is a circulation joint, 41 is a gas-liquid trap with an inner diameter larger than the supply pipe that deaerates the supplied pressurized cleaning water by a significant drop in pressure, and 42 is the cleaning water exiting the gas-liquid trap 41. A heating water tank that heats water to about 55 centimeters.The heating water tank 42 has an internal heater 43 that heats water and metal.
A coil 44 is provided to allow cleaning water to flow into the coil 44. 45 is the gas-liquid trap 41 where the cleaning water
A separation drag separates air bubbles generated while passing through the heating water tank 42, and one air bubble is collected above the separation trap 45 and discharged from the gas discharge valve 46. Reference numeral 47 is a centrifugal pump, which uses the high speed rotation of the blades of the centrifugal pump 47 to agitate the heated washing water to form all bubbles of supersaturated dissolved air, and the bubbles are collected above the separation trap 45 to be used as described above. Discharge the same. The cleaning water from the thin winding pump 47 is guided to the trap 48, where air bubbles are further separated and air is removed. The washing water from which the packaging has been completely separated is supplied to the conduit 49 and the washing water supply valve 3.
2 to the syringe 27. Also, trap 48
The circulation joint 40 is connected above by the circulation hose 50.
The excess washing water and the washing water when the washing water supply valve 32 is closed are returned to the circulation joint 40 (A), and this heated washing water is used to pressurize cold water. A rapid temperature change is applied to the wash water to facilitate the release of dissolved air.

Note that the gas discharge valve 46 and the wash water supply valve 32 are arranged to operate in the opposite direction, that is, the gas discharge valve 46 is operated so that the wash water supply valve 32 opens and wash water flows into the syringe 27 for washing. It is closed when water is flowing, and the wash water supply valve 3
When 2 is closed, it remains open for a certain period of time to exhaust gas. Although this gas may be exhausted directly to the atmosphere, the gas exhaust valve 46
A vacuum pump may be provided at the tip of the separation trap 45 to reduce the pressure in the separation trap 45 for a certain period of time to promote the generation of bubbles.

Table 1 shows the solubility of nitrogen and oxygen, which are the main components of air, in water. 10r of water is approximately 0.0029
It dissolves 23% (W/W) of air.

If the water temperature rises to 50p, the solubility of air decreases to 0.001504 inches (w/w), so the difference in air, 0.001419 degrees, will be released. Therefore, if the temperature of the supplied deionized water (washing water) is 10C1, the temperature inside the device is 50C5, and the consumption of washing water is 10t/hr, the amount of bubbles generated is approximately 0.1419
g/11 r), 13 at 50C, 1 atm
Bubbles of 1 m1/l+r are continuously generated.

That is, in FIG. 2, in the common flow path from the wash water supply valve 32 to the multiple valve 28, 1317'
As many as ljI air bubbles will be generated. If these continuously generated air bubbles are continuously discharged through the waste liquid port Qo of the multiple valve 28 for each cleaning in a steady state, the damping effect due to the air bubbles will be small and constant, so it will not be a problem. No.

However, the bubbles that are generated are initially extremely fine;
It accumulates on the inner wall of the channel, and when it becomes a certain amount of large bubbles, it flows out together with the initial cleaning water, so the damping effect of the total amount of bubbles remaining in the common channel continues. This causes a decrease in reagent dispensing accuracy due to the switchback method.

Therefore, it is important to prevent air bubbles from forming in the washing water within the apparatus. By the way, in principle,
Considering the change in gas solubility due to temperature, it is considered effective to heat the cleaning water to around 50C immediately before the cleaning water supply valve 32 and separate the generated gas. It has been found that heating only in the flow path is not very effective because the excess dissolved air moves in a supersaturated state and forms bubbles near the multi-delivery valve 28 near the end of the flow path. Therefore, in the present invention, a degassing device such as the embodiment shown in FIG. 4 is provided.

According to the deaeration device shown in FIG. 4, preliminary deaeration is performed in the gas-liquid trap 41, heating deaeration is performed in the heated water 41#42, and final deaeration is performed in the centrifugal pump 49. ,
The dissolved air can be completely degassed to a state where dissolution equilibrium is reached at the water temperature in the heated water tank 42, and the generated air bubbles are separated in the separation trap 45, and some remaining air bubbles are circulated from the trap 48. Geoindo 40
Therefore, if the cleaning water that has passed through the deaerator shown in FIG. 4 is supplied to the syringe 27 and the multiple valve 28 via the cleaning water supply valve 32, the multiple valve 2
No air bubbles are generated in the common flow path up to 8, and a decrease in reagent dispensing accuracy due to damper action can be prevented.

〔Effect of the invention〕

As explained above, according to the present invention, it is possible to prevent air bubbles from being generated when cleaning the reagent dispensing system with cleaning water, thereby eliminating the damping effect caused by air bubbles and improving reagent dispensing accuracy. This has the effect of increasing analysis accuracy.

[Brief explanation of the drawing]

Figure 1 is a configuration diagram of a conventional reagent pipetting type automatic analyzer, Figure 2 is a principle diagram of a switch/vine type dispenser, and Figure 3 is a diagram of the switch/vine type dispenser shown in Figure 2. FIG. 4 is a system diagram showing an embodiment of a deaerator for deaerating the washing water of the automatic analyzer of the present invention.

Claims (1)

[Scope of Claims] 1. Sampling a predetermined amount of a sample into each of a plurality of reaction vessels, applying partial pressure, and dispensing a predetermined amount of reagent using a dispenser to react, and analyzing each sample. The automatic analyzer is equipped with a degassing device that degasses the washing water used for washing the pressure divider so that dissolved air does not form bubbles under any conditions within the operating temperature range of the dispenser. An automatic analyzer characterized by: 2. The deaerator includes a gas-liquid trap that performs preliminary deaeration by changing the pressure of pressurized cleaning water, a constant temperature bath that heats the cleaning water that has passed through the gas-liquid trap to a predetermined temperature, and a constant temperature 2. The automatic analyzer according to claim 1, comprising a thin winding pump that completely foams the supersaturated dissolved air in the wash water heated in the tank, and an external trap that removes the air bubbles by 1 minute.