JP5492833B2 - Automatic analyzer and control method thereof - Google Patents

Description

  The present invention relates to an automatic analyzer technology, and in particular, is effective when applied to an electrolyte measurement device used for ion analysis in biological fluid, a biochemical automatic analysis device including the electrolyte measurement device, and these control methods. It is about technology.

  In the quantitative measurement of various ions such as Na ion, K ion, Cl ion, etc. present in blood, the mainstream method is to perform electromotive force measurement using an ion selective electrode (ISE). .

  Measurement methods using an ion selective electrode include a dilution method in which a sample solution is diluted with a diluent, and a non-dilution method in which the sample solution is measured without dilution. The dilution method is used in the electrolyte measuring devices installed in most automatic analyzers except for small emergency testing devices. In the dilution method, a sample solution is diluted with a diluent in a container such as a dilution cup or a reaction cell (hereinafter referred to as a dilution container), and this diluted sample solution (hereinafter referred to as a diluted sample solution) is supplied to an ion selective electrode. Measure electrolyte concentration.

  In general, a dilution container used in an electrolyte measuring apparatus employing a dilution method is repeatedly used. An electrolyte measuring device employing such a dilution method is described in Patent Document 1, for example.

JP 2007-57367 A

  By the way, in the dilution method adopted in the conventional electrolyte measuring device including Patent Document 1 described above, all sample solutions are diluted in a dilution container and then measured. Therefore, if the previously measured sample solution remains in the dilution container, it may cause erroneous measurement. On the other hand, the dilution container is cleaned by having an inspection engineer periodically clean it using a cotton swab or the like.

  Ideally, a mechanism for automatically cleaning the dilution container should be provided. However, when the dilution container is cleaned with a cleaning liquid such as pure water, it is necessary to clean the entire dilution container without overflowing from the dilution container. . For this purpose, it is necessary to monitor how much cleaning water has entered the dilution container. For monitoring, for example, a method of measuring the liquid level height by using a water level sensor or a pressure sensor as the liquid level detection sensor can be considered.

  However, when a water level sensor is installed, there is a problem that measurement failure (carry over) is likely to occur due to contamination between sample solutions. In addition, there is a method of measuring the liquid level height by installing a pressure sensor or the like, but there is a problem that the apparatus configuration becomes complicated.

  Therefore, the present invention has been made in view of the problems as described above, and a typical purpose thereof is to install the liquid level height of the solution in the dilution container without installing a mechanism such as a water level sensor or a pressure sensor. Another object of the present invention is to provide an automatic analyzer capable of measuring the flow rate per unit time of a solution discharged into a dilution container.

  The above and other objects and novel features of the present invention will be apparent from the description of this specification and the accompanying drawings.

  Of the inventions disclosed in the present application, the outline of typical ones will be briefly described as follows.

  That is, a typical automatic analyzer includes an electrolyte measurement unit that measures an electrolyte in a liquid by an electrode method, a storage unit that stores an electromotive force measured by the electrolyte measurement unit, a container that holds a liquid, A control unit that controls a dispensing unit that dispenses a liquid into the container, a sipper nozzle that sucks the liquid in the container and supplies the liquid to the electrolyte measurement unit, and a process for detecting the liquid level of the liquid in the container A part. In particular, the control unit stores the electromotive force (E0) measured by the electrolyte measurement unit in a state where the sipper nozzle is not in contact with the liquid in the container, and the sipper nozzle is stored in the container. Based on the electromotive force (En) obtained by the electrolyte measuring unit and the electromotive force (E0) stored in the storage unit in the process up to the state in contact with the liquid inside, the liquid liquid in the container It is characterized by controlling the process for detecting the surface height.

  Further, as a control method of a typical automatic analyzer, as the control of the control unit, the liquid in the container is sucked using the sipper nozzle, and the liquid between the flow path between the electrolyte measurement unit and the sipper nozzle is liquid. And detecting that the liquid in the container is contained up to a predetermined amount or a predetermined liquid level based on the electromotive force generated between the electrolyte measurement unit and the sipper nozzle. And obtaining a reference electromotive force (E0).

  Among the inventions disclosed in the present application, effects obtained by typical ones will be briefly described as follows.

  That is, the typical effect is to measure the liquid level of the solution in the dilution container and the flow rate per unit time of the solution discharged into the dilution container without installing a mechanism such as a water level sensor or a pressure sensor. Can do. As a result, it is possible to provide an automatic analyzer including an electrolyte measuring device having a simple structure and high reliability.

It is a schematic block diagram which shows an example of the whole structure of the automatic analyzer which concerns on one embodiment of this invention. It is a schematic block diagram which shows an example of a structure of the electrolyte measuring device contained in the automatic analyzer which concerns on one embodiment of this invention. In the electrolyte measuring device included in the automatic analyzer according to one embodiment of the present invention, the relationship between the potential of the measured electromotive force and the liquid level of the solution in the dilution container when the measuring system of the electrolyte measuring device is changed It is explanatory drawing which shows an example. It is a flowchart which shows an example of the liquid level height detection processing flow of the solution in a dilution container in the electrolyte measuring device contained in the automatic analyzer which concerns on one embodiment of this invention. It is a flowchart which shows another example of the liquid level height detection processing flow of the solution in a dilution container in the electrolyte measuring device contained in the automatic analyzer which concerns on one embodiment of this invention. It is a flowchart which shows an example of the flow volume measurement processing flow of the solution in a dilution container in the electrolyte measuring device contained in the automatic analyzer which concerns on one embodiment of this invention.

  In the following embodiments, when it is necessary for the sake of convenience, the description will be divided into a plurality of embodiments or sections. However, unless otherwise specified, they are not irrelevant and one is the other. There are some or all of the modifications, details, supplementary explanations, and the like. Further, in the following embodiments, when referring to the number of elements (including the number, numerical value, quantity, range, etc.), especially when clearly indicated and when clearly limited to a specific number in principle, etc. Except, it is not limited to the specific number, and may be more or less than the specific number.

  Further, in the following embodiments, the constituent elements (including element steps and the like) are not necessarily indispensable unless otherwise specified and apparently essential in principle. Needless to say. Similarly, in the following embodiments, when referring to the shapes, positional relationships, etc. of the components, etc., the shapes are substantially the same unless otherwise specified, or otherwise apparent in principle. And the like are included. The same applies to the above numerical values and ranges.

  Hereinafter, embodiments of the present invention will be described in detail with reference to the drawings. Note that components having the same function are denoted by the same reference symbols throughout the drawings for describing the embodiment, and the repetitive description thereof will be omitted.

<Outline of Embodiment of the Present Invention>
An automatic analyzer according to an embodiment of the present invention (for example, a corresponding component in FIG. 2 or the like is added in parentheses) is an electrolyte measurement unit (ion-selective electrode 204) that measures an electrolyte in a liquid by an electrode method. ˜206, comparative electrode 207, etc.), a storage unit (storage device 12) for storing the electromotive force measured by the electrolyte measurement unit, a container for holding liquid (dilution container 203), and dispensing the liquid into the container Dispensing part (probe 202, syringes 209 and 210, solenoid valves 215 to 218, etc.), a sipper nozzle (sipper nozzle 222) for sucking the liquid in the container and supplying it to the electrolyte measuring part, and liquid liquid in the container And a control unit (control unit 13) for controlling processing for detecting the surface height. In particular, the control unit stores the electromotive force (E0) measured by the electrolyte measurement unit in a state where the sipper nozzle is not in contact with the liquid in the container, and repeats dispensing of the liquid into the container. Controlling the process of detecting the liquid level of the liquid in the container based on the electromotive force (En) obtained by the electrolyte measurement unit in the process and the electromotive force (E0) stored in the storage unit Features.

  Further, the control method of the automatic analyzer according to the embodiment of the present invention (for example, the corresponding steps in FIG. 4 are added in parentheses) is a liquid in the container using a sipper nozzle as control of the control unit. And filling the space between the electrolyte measurement unit and the sipper nozzle with a liquid (S1), and based on the electromotive force generated between the electrolyte measurement unit and the sipper nozzle, a predetermined amount of liquid in the container, Or it has the step (S3) of obtaining the electromotive force (E0) used as the reference | standard for detecting having accommodated to the predetermined | prescribed liquid level height.

  The embodiment based on the outline of the embodiment of the present invention described above will be specifically described below. The embodiment described below is an example using the present invention, and the present invention is not limited to the following embodiment.

<Embodiment>
<< Overall configuration and operation of automatic analyzer >>
The overall configuration and operation of the automatic analyzer according to the present embodiment will be described with reference to FIG. FIG. 1 is a schematic configuration diagram showing an example of the overall configuration of the automatic analyzer. Here, a biochemical automatic analyzer will be described as an example.

  In FIG. 1, 1 is a sample disk, 2 is a reagent disk, 3 is a reaction disk, 4 is a reaction tank, 5 is a sampling mechanism, 6 is a reagent dispensing mechanism, 7 is a stirring mechanism, 8 is a photometric mechanism, and 9 is a cleaning mechanism. 10 is a computer (PC), 11 is an electrolyte measurement unit, 12 is a storage device, 13 is a control unit, 14 is a piezoelectric element driver, 15 is a stirring mechanism controller, 16 is a sample container, 17 is a circular sample disk, and 18 is a reagent. Bottle, 19 is a circular reagent disk, 20 is a cold storage, 21 is a reaction vessel, 22 is a reaction vessel holder, 23 is a drive mechanism, 24 is a sample probe, 25 is a sample probe support shaft, 26 is a sample probe arm, 27 is a reagent Probe, 28 is a reagent probe support shaft, 29 is a reagent probe arm, 30 is a sampling mechanism for electrolyte measurement, 31 is a fixed part, and 33 is a nose , The vertical drive mechanism 34, 35 is the electrolyte measurement sample probe, 36 sample probe support shaft for electrolyte measurement, 37 is a sample probe arm electrolyte measurement.

  The automatic analyzer according to the present embodiment mainly includes a sample disk 1 on which a plurality of sample containers 16 are placed, a reagent disk 2 on which a plurality of reagent bottles 18 are placed, and a plurality of reaction containers 21. A reaction disk 3 to be placed; a sampling mechanism 5 installed in the vicinity of the sample disk 1 and the reaction disk 3; a reagent dispensing mechanism 6 installed in the vicinity of the reagent disk 2 and the reaction disk 3; A stirring mechanism 7, a photometric mechanism 8, a cleaning mechanism 9, an electrolyte measuring unit 11, an electrolyte measuring sampling mechanism 30, and the like installed in the vicinity of the disk 3 are configured.

  In the sample disk 1, a plurality of sample containers 16 for storing a sample to be analyzed (also referred to as a sample) are placed on a circular sample disk 17 side by side on the circumference. A sampling mechanism 5 is installed in the vicinity of the sample disk 1. The sampling mechanism 5 is attached to a sample probe arm 26 fixed to a sample probe support shaft 25, in which a sample probe 24 sucks a sample from the corresponding sample container 16 and discharges the sample to the corresponding reaction container 21. .

  In the reagent disk 2, a plurality of reagent bottles 18 for storing reagents are placed side by side on a circle on a circular reagent disk 19. The reagent disk 2 is provided with a cool box 20. A reagent dispensing mechanism 6 is installed in the vicinity of the reagent disk 2. The reagent dispensing mechanism 6 is attached to a reagent probe arm 29 fixed to a reagent probe support shaft 28. The reagent probe 27 sucks a reagent from the corresponding reagent bottle 18 and discharges the reagent to the corresponding reaction container 21. ing.

  A plurality of reaction vessel holders 22 holding a plurality of reaction vessels 21 are placed side by side on the circumference of the reaction disk 3. A reaction tank 4 is installed on the reaction disk 3. The reaction disk 3 can be intermittently rotated by the drive mechanism 23. In the vicinity of the reaction disk 3, a stirring mechanism 7, a photometric mechanism 8, a cleaning mechanism 9, an electrolyte measuring unit 11, an electrolyte measuring sampling mechanism 30, and the like are installed.

  The stirring mechanism 7 is a mechanism for stirring the contents (sample and reagent) in the reaction vessel 21, and includes a piezoelectric element driver 14, a stirring mechanism controller 15, and the like. The photometric mechanism 8 is a mechanism for measuring transmitted light that has been transmitted through the contents in the reaction vessel 21 and scattered light that has been scattered by the contents, and includes a light source, a detector, and the like (not shown). The cleaning mechanism 9 is a mechanism for cleaning the inside of the reaction vessel 21 and includes a nozzle 33, a vertical drive mechanism 34, and the like.

  The electrolyte measurement unit 11 is an apparatus for measuring the electrolyte of the sample, and is configured by an ion selection electrode, a comparison electrode, and the like which will be described later with reference to FIG. The electrolyte measurement sampling mechanism 30 is a mechanism for dispensing a sample to the electrolyte measurement unit 11. The electrolyte measurement sample probe 35 for inhaling the sample is fixed to the electrolyte measurement sample probe support shaft 36. A sample probe arm 37 is attached.

  These sample disk 1, reagent disk 2, reaction disk 3, sampling mechanism 5, reagent dispensing mechanism 6, stirring mechanism 7, photometric mechanism 8, washing mechanism 9, electrolyte measuring unit 11, and electrolyte measuring sampling mechanism 30 are Each operation is controlled by being connected to the control unit 13 and further connected to the computer 10. The control unit 13 is connected to the storage device 12.

  The computer 10 includes, for example, a main body including an arithmetic processing function and a storage function, an input unit such as a keyboard and a mouse, and a display unit such as a liquid crystal and a CRT. The computer 10 stores measurement sample information, measurement item registration, analysis parameters, and the like. Set. The storage device 12 stores analysis parameters, the number of times each reagent bottle can be analyzed, the maximum number of times that analysis can be performed, a calibration result, an analysis result, a determination process for evaluating a dispensing operation, and data necessary for a determination to be held in advance. Is retained. The information stored and held in the storage device 12 may be stored in a storage medium attached to the computer 10, or may exist alone as the storage device 12 as an individual storage database.

  In the automatic analyzer configured as described above, the colorimetric analysis of the sample is performed in the order of data processing such as sampling, reagent dispensing, stirring, photometry, reaction vessel cleaning, concentration conversion and the like as follows. .

  Sample disk 1, reagent disk 2, reaction disk 3, sampling mechanism 5, reagent dispensing mechanism 6, stirring mechanism 7, photometric mechanism 8, cleaning mechanism 9, electrolyte measuring unit 11, and electrolyte measuring sampling mechanism 30 are controlled by a control unit 13 through the computer 10.

  First, a plurality of sample containers 16 containing samples to be analyzed are installed on the sample disk 1 side by side on the circumference. Under the sample probe 24 of the sampling mechanism 5 according to the order of the samples to be analyzed. Move up. A predetermined amount of the sample in the sample container 16 is dispensed into the reaction container 21 on the reaction disk 3 by a sample pump (not shown) connected to the sampling mechanism 5.

  Furthermore, the reaction container 21 into which the sample has been dispensed moves through the reaction tank 4 to the first reagent addition position. A predetermined amount of reagent sucked from the reagent bottle 18 on the reagent disk 2 is added to the moved reaction container 21 by a reagent pump (not shown) connected to the reagent probe 27 of the reagent dispensing mechanism 6. The reaction vessel 21 after the addition of the first reagent moves to the position of the stirring mechanism 7 and the first stirring is performed. Such reagent addition-stirring is performed on the first to fourth reagents, for example.

  Subsequently, the reaction vessel 21 in which the contents are agitated passes through the light beam emitted from the light source in the photometric mechanism 8, and the absorbance at this time is detected by a multiwavelength photometer. The detected absorbance signal enters the control unit 13 and is converted into a sample concentration. Further, the control unit 13 simultaneously determines abnormality based on the absorbance.

  Further, the electrolyte measurement of the sample is performed by dispensing the sample to the electrolyte measurement unit 11 by the electrolyte measurement sampling mechanism 30. The dispensing to the electrolyte measurement unit 11 may be performed by the sampling mechanism 5.

  The density-converted data is stored in the storage device 12 and displayed on a display device attached to the computer 10. After completion of photometry, the reaction vessel 21 moves to the position of the cleaning mechanism 9, is cleaned, and is used for the next analysis.

  As described above, in the automatic analyzer according to the present embodiment, data processing such as sampling, reagent dispensing, stirring, photometry, reaction vessel washing, concentration conversion, etc. is performed in order, and colorimetric analysis of the sample is performed. It can be performed.

<< Configuration and operation of electrolyte measuring device >>
With reference to FIG. 2, the configuration and operation of an electrolyte measurement device (a portion including the electrolyte measurement unit 11 and a mechanism part such as a solenoid valve and a syringe in the vicinity thereof) included in the automatic analyzer described above will be described. FIG. 2 is a schematic configuration diagram showing an example of the electrolyte measuring apparatus.

  In FIG. 2, 201 is a sample container, 202 is a probe, 203 is a dilution container, 204 is a Na ion selection electrode, 205 is a K ion selection electrode, 206 is a Cl ion selection electrode, 207 is a comparison electrode, 208 is a sipper syringe, 209 Is an internal standard solution syringe, 210 is a diluent syringe, 211 is a pinch valve, 212 is a two-way solenoid valve for reference electrode, 213 is a two-way solenoid valve for sucking a sipper syringe, 214 is a two-way solenoid valve for discharging waste fluid, and 215 is Two-way solenoid valve for discharging internal standard solution, 216 is a two-way solenoid valve for sucking internal standard solution, 217 is a two-way solenoid valve for discharging diluent, 218 is a two-way solenoid valve for sucking diluent, and 219 is a reference electrode solution bottle , 220 is an internal standard solution bottle, 221 is a dilution solution bottle, 222 is a sipper nozzle, 223 is a heater for dilution solution, 224 is a heater for internal standard solution, 225 Dilution container heater, the ion selective electrode heater 226, 227 reference electrode heater, 228 is a vacuum nozzle.

  The electrolyte measurement apparatus in the present embodiment mainly includes an electrolyte measurement unit that measures an electrolyte in a liquid by an electrode method, a storage unit that stores an electromotive force measured by the electrolyte measurement unit, and a dilution container that holds the liquid 203, a dispensing unit that dispenses liquid into the dilution container 203, a sipper nozzle 222 that sucks the liquid in the dilution container 203 and supplies it to the electrolyte measurement unit, and the liquid level height of the liquid in the dilution container 203 A control unit for controlling the processing to be detected is provided.

  The electrolyte measurement unit includes a Na ion selection electrode 204, a K ion selection electrode 205, a Cl ion selection electrode 206, a comparison electrode 207, and the like. In the vicinity of the electrolyte measurement unit, the diluted sample solution (the sample solution is diluted with the diluent) in the flow path from the sipper nozzle 222 to the Na ion selection electrode 204, the K ion selection electrode 205, and the Cl ion selection electrode 206. A sipper syringe 208 for sucking and filling the internal standard solution and a two-way solenoid valve 213 for sucking the sipper syringe, and a flow path from the comparison electrode solution bottle 219 to the comparison electrode 207 is provided. A reference electrode two-way solenoid valve 212 for filling the reference electrode solution of the reference electrode solution bottle 219 is provided.

  The dispensing unit sucks the sample solution in the sample container 201 and discharges it to the dilution container 203, and the two-way electromagnetic valve for dilution liquid suction that sucks the dilution liquid in the dilution bottle 221 and discharges it to the dilution container 203 218, diluent syringe 210, two-way solenoid valve 217 for discharging diluent, and two-way solenoid valve 216 for sucking internal standard solution for sucking and discharging the internal standard solution in internal standard solution bottle 220 to dilution container 203, It comprises a standard solution syringe 209, an internal standard solution discharge two-way solenoid valve 215, and the like.

  The sipper nozzle 222 is a nozzle that sucks the diluted sample solution or the internal standard solution in the dilution container 203. Further, the sipper nozzle 222 can be driven in the vertical direction, and has a structure capable of descending from the upper limit point by a certain amount with respect to the dilution container 203.

  In this electrolyte measuring apparatus, for example, the dilution container 203 corresponds to the reaction container 21 shown in FIG. 1, and the sipper nozzle 222 corresponds to the electrolyte measurement sample probe 35 of the electrolyte measurement sampling mechanism 30 shown in FIG. To do. Furthermore, although not limited thereto, the ion selection electrodes 204 to 206, the comparison electrode 207, and the like are included in the electrolyte measurement unit 11 shown in FIG. Further, the storage unit constituting the electrolyte measuring device corresponds to the storage device 12 (or a storage area in the computer 10 or an attached storage medium) shown in FIG. 1, and the control unit is the control unit 13 shown in FIG. (Or including the computer 10). The control unit 13 controls a flow level detection process flow of the solution in the dilution container 203 and a flow rate measurement process flow of the solution in the dilution container 203, which will be described later with reference to FIGS.

  In the electrolyte measuring apparatus configured as described above, the operation of the electrolyte measuring apparatus will be described with reference to FIG. The operation of the electrolyte measuring device is controlled by the control unit 13 via the computer 10.

  In FIG. 2, the sample solution in the sample container 201 is aspirated by a set amount by the probe 202 and discharged to the dilution container 203. Then, the diluent in the diluent bottle 221 is discharged to the dilution container 203 by the operations of the two-way electromagnetic valve 218 for sucking the diluent, the diluent syringe 210, and the two-way solenoid valve 217 for discharging the diluent, and is diluted from the sample container 201. The sample solution discharged into the container 203 is diluted.

  With the pinch valve 211 closed, the comparison electrode liquid in the comparison electrode liquid bottle 219 is compared via the comparison electrode two-way electromagnetic valve 212 by the operation of the sipper syringe 208 and the two-way electromagnetic valve 213 for sucking the sipper syringe. The electrode 207 is sucked. Next, the diluted sample solution diluted in the dilution container 203 is moved from the sipper nozzle 222 to the Na ion selection electrode by the operation of the sipper syringe 208 and the sipper syringe suction two-way electromagnetic valve 213 with the pinch valve 211 opened. 204, the K ion selection electrode 205, and the Cl ion selection electrode 206 are attracted. Then, the electromotive force generated between the comparison electrode 207 and the ion selection electrodes 204, 205, 206 is measured. The diluted sample solution remaining in the dilution container 203 is removed by the vacuum nozzle 228.

  On the other hand, the internal standard solution in the internal standard solution bottle 220 is discharged into the dilution container 203 by the operations of the internal standard solution suction two-way solenoid valve 216, the internal standard solution syringe 209, and the internal standard solution discharge two-way solenoid valve 215. The The diluted sample solution and the internal standard solution are alternately sucked from the sipper nozzle 222 to the ion selection electrodes 204, 205, 206, and the electromotive force generated between the comparison electrode 207 and the ion selection electrodes 204, 205, 206 is measured. . The internal standard solution remaining in the dilution container 203 is removed by the vacuum nozzle 228.

In an ideal state, an electromotive force generated between the comparison electrode 207 and the ion selection electrodes 204, 205, 206 is
E = E ′ + 2.3303 × RT / nF × log (f × Ci) (1)
E: Electromotive force
E ′: Constant electromotive force determined by the measurement system
R: Gas constant
T: Absolute temperature
F: Faraday constant
f: Activity coefficient
Ci: concentration of ion (i)
n: Expressed by a calculation formula equal to or greater than the number of charges of ion (i).

  From equation (1), since the electromotive force depends on the absolute temperature, the dilution container 203 of the electrolyte measurement device, the solution in the dilution container 203, and the electrolyte measurement unit are controlled at a constant temperature. The sample concentration is calculated from the difference in electromotive force between the internal standard solution and the sample solution and a calibration curve prepared in advance. The sample and the internal standard solution for which the measurement has been completed are discharged out of the apparatus from the waste liquid flow path by opening and closing the two-way solenoid valve 214 for discharging the waste liquid.

  The internal standard solution and the diluting solution are heated by the internal standard solution heater 224 and the diluting solution heater 223 after passing through the internal standard solution discharging two-way electromagnetic valve 215 and the diluting solution discharging two-way electromagnetic valve 217. The temperature of the dilution container 203, the ion selection electrodes 204, 205, 206, and the comparison electrode 207 is controlled by the dilution container heater 225, the ion selection electrode heater 226, and the comparison electrode heater 227, respectively.

<< State change when the measurement system of the electrolyte measuring device changes >>
Next, a case where the measurement system of the electrolyte measuring device is changed in the operation of the electrolyte measuring device described above will be described with reference to FIG. FIG. 3 is an explanatory diagram showing an example of the relationship between the potential of the measured electromotive force and the liquid level of the solution in the dilution container when the measurement system of the electrolyte measuring device is changed.

  When the measurement system of the electrolyte measuring device changes, the constant electromotive force E ′ determined by the measurement system of the above-described equation (1) changes, and the obtained electromotive force E also changes. For example, the sipper nozzle 222 that is electrically connected to the ion selective electrodes 204, 205, and 206 is not in contact with the solution in the dilution vessel 203 (state 1 shown in FIG. 3) and in contact (state shown in FIG. 3). Since the measurement system differs from 2), even if the same sample is filled in the electrode, the electromotive force obtained is different.

  In normal electrolyte measurement, a sample is measured so that the electromotive force E ′ determined by the measurement system is constant, and the sample concentration is calculated from the obtained electromotive force. On the other hand, in the present embodiment, the same electrolyte solution is measured so that there is no change in electromotive force due to concentration. In this case, if the measurement system does not change (if the solution in the dilution container 203 and the sipper nozzle 222 are not in contact with each other (state 1)), the electromotive force obtained is constant, and if the measurement system changes (dilution container) If the solution in 203 comes into contact with the sipper nozzle 222 (state 2)), the electromotive force E ′ determined by the measurement system changes, and the obtained electromotive force E also changes.

  Therefore, in the electrolyte measuring device according to the present embodiment, the state in which the solution in the dilution container 203 and the sipper nozzle 222 are not in contact with each other, and the state in which the solution in the dilution container 203 and the sipper nozzle 222 are in contact with each other Focusing on the change, as described in detail below, the liquid level detection processing of the solution in the dilution container 203 and the flow rate measurement processing of the solution in the dilution container 203 are performed.

<< Flow level detection processing flow (1) of the solution in the dilution container >>
With reference to FIG. 2 described above, the flow level detection processing flow of the solution in the dilution container in the above-described electrolyte measuring device will be described with reference to FIG. FIG. 4 is a flowchart showing an example of a processing flow for detecting the liquid level of the solution in the dilution container.

  The liquid level detection processing flow of the solution in the dilution container is controlled by the control unit 13 via the computer 10. That is, the control unit 13 is based on a control program at the time of starting up the apparatus that operates on the computer 10, for example, and the measurement is performed by the electrolyte measurement unit in a state where the sipper nozzle 222 is not in contact with the solution in the dilution container 203. The electric power E0 is stored in the storage unit, and the electromotive force En obtained by the electrolyte measurement unit and the electromotive force E0 stored in the storage unit until the sipper nozzle 222 comes into contact with the solution in the dilution container 203. Based on this, the process for detecting the liquid level of the solution in the dilution container 203 is controlled.

  Further, the control unit 13 repeats the dispensing of the solution into the dilution container 203 based on the control program at the time of starting up the apparatus that operates on the computer 10, and the electromotive force En and the electromotive force E0. A function for determining that the difference is equal to or greater than the specified value is also realized. The specified value storage unit that stores the specified value that is the threshold value ΔE of the function to be determined is provided in the storage area in the storage device 12 or the computer 10 or an attached storage medium.

  First, as a preparation for detecting the liquid level of the solution in the dilution container 203, the old internal standard solution in the flow path is discharged out of the apparatus from the waste liquid flow path by opening and closing the two-way electromagnetic valve 214 for discharging the waste liquid. . Further, the internal standard solution in the internal standard solution bottle 220 is discharged into the dilution container 203 by the operations of the internal standard solution suction two-way solenoid valve 216, the internal standard solution syringe 209, and the internal standard solution discharge two-way solenoid valve 215.

  In the electrolyte solution suction in step S1, the internal standard solution discharged into the dilution container 203 is transferred from the sipper nozzle 222 to the ion selective electrodes 204, 205, by the sipper syringe 208, the sipper syringe suction two-way electromagnetic valve 213, and the pinch valve 211. Aspirate to 206. This operation is performed a plurality of times so that the sipper nozzle 222 to the ion selection electrodes 204, 205, 206 are filled with a new internal standard solution, and the ion selection electrodes 204, 205, 206 and the tip of the sipper nozzle 222 are in a conductive state. .

  Next, in the sipper nozzle tip position control in step S2, the sipper nozzle 222 is driven to a liquid level to be detected and stopped. And in the electromotive force E0 measurement of step S3, after removing the residual liquid in the dilution container 203 with the vacuum nozzle 228, the electromotive force E0 is measured in a state where the height of the sipper nozzle 222 is maintained, and the obtained electromotive force is obtained. E0 is recorded in the storage unit (the storage device 12 or a storage area in the computer 10 or an attached storage medium).

  Furthermore, in discharging the solution to the dilution container in step S4, a certain amount of solution is discharged to the dilution container 203. For this solution, pure water, detergent, diluent, internal standard solution or the like is used. In this state, the electromotive force En of the internal standard solution measured in step S3 is measured again in the electromotive force En (first time n = 1) measurement in step S5.

  Subsequently, in step S6, determination of | En−E0 |> ΔE is performed based on the electromotive force E0 recorded in the storage unit in step S3 and the electromotive force En measured in step S5. For example, when the solution reaches the sipper nozzle 222, the electromotive force En obtained in step S5 is different from the electromotive force E0 obtained in step S3. Therefore, the difference between En and E0 (| En−E0 |) is measured, and this difference is compared with a predetermined threshold value (ΔE).

  As a result of the comparison in step S6, when the difference between En and E0 is larger than the threshold (| En−E0 |> ΔE) (Yes), the liquid level in the dilution container 203 has reached the tip of the sipper nozzle 222. Become. In this case, in the liquid level detection of step S7, the liquid level of the solution in the dilution container 203 is detected.

  On the other hand, when the difference between En and E0 is smaller than the threshold value (| En−E0 | <ΔE) (No) as a result of the comparison in step S6, the liquid level in the dilution container 203 has not reached the tip of the sipper nozzle 222. become. In this case, from the solution discharge to the dilution container in step S4, the electromotive force En in step S5 (n = 2 for the second time, n = 3 for the third time in the following order) is measured, and | En-E0 | > ΔE is repeated until the difference between En and E0 becomes larger than the threshold, and when the difference between En and E0 becomes larger than the threshold, the liquid level of the solution in the dilution container 203 is detected in step S7. To do.

  As described above, in the example of the flow level detection processing flow of the solution in the dilution container 203 shown in FIG. 4, the solution is discharged into the dilution container 203 by a certain amount, and the determination condition of | En−E0 |> ΔE is By repeating the operation until it is established, the liquid level of the solution in the dilution container 203 can be detected.

<< Liquid surface height detection processing flow (2) of the solution in the dilution container >>
An example different from the liquid level detection processing flow of the solution in the dilution container shown in FIG. 4 will be described with reference to FIG. FIG. 5 is a flowchart showing an example of the processing flow for detecting the liquid level of the solution in the other dilution container. Here, a different part from FIG. 4 is mainly demonstrated.

  In the liquid level detection processing flow of the solution in the dilution container, the control unit 13 lowers the sipper nozzle 222 to the dilution container 203 based on, for example, a control program when starting up the apparatus operating on the computer 10. A function of determining that the difference between the electromotive force En and the electromotive force E0 is equal to or greater than a specified value (threshold value ΔE) in the process of iterating is realized.

  First, in the electrolyte solution suction in step S11, the internal standard solution discharged to the dilution container 203 is sucked, and the sipper nozzle 222 to the ion selection electrodes 204, 205, 206 are filled with new internal standard solution, and the ion selection electrode 204, 205 and 206 are connected to the tip of the sipper nozzle 222.

  Next, in the sipper nozzle upper limit movement in step S12, the sipper nozzle 222 is driven to the upper limit and stopped. And in the electromotive force E0 measurement of step S13, after removing the residual liquid in the dilution container 203 with the vacuum nozzle 228, the electromotive force E0 is measured in the state which maintained the height of the sipper nozzle 222, and the obtained electromotive force was obtained. E0 is recorded in the storage unit.

  Further, in the solution discharge to the dilution container in step S14, solutions such as pure water, detergent, dilution liquid, and internal standard solution are discharged to the dilution container 203. Then, in the recording of the sipper nozzle constant amount descending / decreasing amount in step S15, the sipper nozzle 222 is descended by a certain amount, and this descending amount is recorded in the storage unit (storage device 12 or storage area in the computer 10 or an attached storage medium). To do. In this state, in the electromotive force En measurement in step S16, the electromotive force En of the internal standard solution measured in step S13 is measured again.

  Subsequently, in the determination of | En−E0 |> ΔE in step S17, the difference between En and E0 (| En−E0 |) and the threshold value (ΔE) are compared. As a result of this comparison, if the difference between En and E0 is larger than the threshold value (| En−E0 |> ΔE) (Yes), in the liquid level detection in step S18, the solution in the dilution container 203 is determined from the height of the sipper nozzle 222. Detects the liquid level height.

  On the other hand, if the difference between En and E0 is smaller than the threshold value (| En−E0 | <ΔE) as a result of the comparison in step S17 (No), the liquid level cannot be detected and output to the monitor (monitor of the computer 10). Then, from the recording of the sipper nozzle constant amount descending / decreasing amount in step S15 to the electromotive force En measurement in step S16 and the determination of | En−E0 |> ΔE in step S17 are repeated until the difference between En and E0 becomes larger than the threshold value. When the difference between En and E0 becomes larger than the threshold value, the liquid level of the solution in the dilution container 203 is detected in step S18.

  As described above, in the example of the flow level detection processing flow of the solution in the dilution container 203 shown in FIG. 5, the sipper nozzle 222 is lowered by a certain amount, and the determination condition of | En−E0 |> ΔE is satisfied. By repeating the operation until the liquid level height of the solution in the dilution container 203 can be detected.

<< Flow measurement processing flow of the solution in the dilution container >>
With reference to FIG. 6, the flow rate measurement of the solution in the dilution container in the above-described electrolyte measurement device from a viewpoint different from the process for detecting the liquid level of the solution in the dilution container shown in FIGS. 4 and 5 described above. A processing flow will be described. FIG. 6 is a flowchart showing an example of a flow measurement process flow of the solution in the dilution container. Here, a different part from FIG. 4 and FIG. 5 is mainly demonstrated.

  The flow rate measurement processing flow of the solution in the dilution container is controlled by the control unit 13 via the computer 10. That is, the control unit 13 repeats the dispensing of the solution into the dilution container 203 based on, for example, a control program at the time of starting the apparatus that operates on the computer 10, and the solution is dispensed at the dilution container 203 by the dispensing unit. Measure the time from the start of dispensing until the difference between the electromotive force (En) and the electromotive force (E0) exceeds the specified value (threshold value ΔE), and dilute at the dispensing unit from this measured time. The function of calculating the flow rate of the solution dispensed into the container 203 is also realized.

  First, in the electrolyte solution suction in step S21, the internal standard solution discharged to the dilution container 203 is sucked, and the sipper nozzle 222 to the ion selection electrodes 204, 205, 206 are filled with new internal standard solution, and the ion selection electrode 204, 205 and 206 are connected to the tip of the sipper nozzle 222.

  Next, in the sipper nozzle tip position control in step S22, the sipper nozzle 222 is driven to a desired liquid level and stopped so that the amount of solution required to reach the tip of the sipper nozzle 222 becomes a set value. And in the electromotive force E0 measurement of step S23, after removing the residual liquid in the dilution container 203 with the vacuum nozzle 228, the electromotive force E0 is measured in the state which maintained the height of the sipper nozzle 222, and the obtained electromotive force was obtained. E0 is recorded in the storage unit.

  Furthermore, in the solution discharge / discharge time recording to the dilution container in step S24, solutions such as pure water, detergent, dilution liquid, and internal standard solution are discharged to the dilution container 203 for a fixed time, and this discharge time is stored in the storage unit ( In the storage device 12 or a storage area in the computer 10 or an attached storage medium). In this state, in the electromotive force En measurement in step S25, the electromotive force En of the internal standard solution measured in step S23 is measured again.

  Subsequently, in the determination of | En−E0 |> ΔE in step S26, the difference between En and E0 (| En−E0 |) is compared with a threshold value (ΔE). As a result of this comparison, if the difference between En and E0 is larger than the threshold (| En−E0 |> ΔE) (Yes), in the flow rate calculation from the discharge time in step S27, the total discharge time of the discharge time recorded in step S24. Then, from the amount of solution (set value) required to reach the tip of the sipper nozzle 222, the average flow rate discharged to the dilution container 203 and the flow rate per unit time are calculated.

  On the other hand, if the difference between En and E0 is smaller than the threshold value (| En−E0 | <ΔE) as a result of the comparison in step S26 (No), the flow rate measurement is impossible and a solution is supplied to the dilution container in step S24 for a certain period of time. The process from the discharge / discharge time recording to the electromotive force En measurement in step S25 and the determination of | En−E0 |> ΔE in step S26 is repeated until the difference between En and E0 becomes larger than the threshold, and the difference between En and E0 is the threshold. When it becomes larger, the average flow rate discharged to the dilution container 203 and the flow rate per unit time are calculated in step S27.

  As described above, in the example of the flow measurement processing flow of the solution in the dilution container 203 shown in FIG. 6, the solution is discharged into the dilution container 203 for a certain period of time until the determination condition of | En−E0 |> ΔE is satisfied. By repeating the operation, the average flow rate of the solution discharged to the dilution container 203 and the flow rate per unit time can be measured.

<< Effects of Embodiment >>
According to the electrolyte measurement device included in the automatic analyzer according to the present embodiment described above, the electrolyte measurement unit including the ion selective electrodes 204 to 206 and the comparison electrode 207, the storage unit such as the storage device 12, and the dilution The following effects can be obtained by providing the container 203, the dispensing unit including the probe 202, the syringes 209 and 210, the electromagnetic valves 215 to 218, the sipper nozzle 222, the control unit 13, and the like.

  (1) The electromotive force E0 is measured by the electrolyte measurement unit in a state where the sipper nozzle 222 is not in contact with the solution in the dilution container 203, and the process until the sipper nozzle 222 comes into contact with the solution in the dilution container 203. The electromotive force En is measured by the electrolyte measurement unit, and the liquid level of the solution in the dilution container 203 can be detected based on the electromotive force En and the electromotive force E0.

  (2) In the process until the sipper nozzle 222 comes into contact with the solution in the dilution container 203, the dispensing of the solution into the dilution container 203 is repeated, and the difference between the electromotive force En and the electromotive force E0 becomes greater than or equal to the threshold ΔE. By detecting that the solution in the dilution container 203 is stored up to a predetermined amount or a predetermined liquid level, it is possible to dilute without installing a mechanism such as a water level sensor or a pressure sensor. The liquid level of the solution in the container 203 can be measured.

  (3) In the process until the sipper nozzle 222 comes into contact with the solution in the dilution container 203, the sipper nozzle 222 is repeatedly lowered to the dilution container 203, and the difference between the electromotive force En and the electromotive force E0 is greater than or equal to the threshold ΔE. By determining that the solution in the dilution container 203 is stored up to a predetermined amount or a predetermined liquid level, without installing a mechanism such as a water level sensor or a pressure sensor, The liquid level of the solution in the dilution container 203 can be measured.

  (4) The time until the difference between the electromotive force En and the electromotive force E0 becomes equal to or greater than the threshold value ΔE after the dispensing of the solution to the dilution container 203 is measured by the dispensing unit is measured. By calculating the flow rate of the solution dispensed to the dilution container 203 by the injection section, the average flow rate of the solution discharged to the dilution container 203 and the unit time per unit time can be obtained without installing a mechanism such as a water level sensor or a pressure sensor. The flow rate can be measured.

  (5) According to the above (1) to (4), it is possible to provide an electrolyte measuring device having a simple structure and high reliability.

  (6) According to the above (1) to (4), it is not necessary to clean the dilution container 203 by a conventional inspection engineer, which can contribute to reducing the burden on the inspection engineer.

  As mentioned above, the invention made by the present inventor has been specifically described based on the embodiment. However, the present invention is not limited to the embodiment, and various modifications can be made without departing from the scope of the invention. Needless to say.

  The automatic analyzer of the present invention is particularly effective when applied to an electrolyte measuring device used for analyzing ions in biological fluid, a biochemical automatic analyzer including this electrolyte measuring device, and these control methods.

DESCRIPTION OF SYMBOLS 1 ... Sample disk, 2 ... Reagent disk, 3 ... Reaction disk, 4 ... Reaction tank, 5 ... Sampling mechanism, 6 ... Reagent dispensing mechanism, 7 ... Agitation mechanism, 8 ... Photometry mechanism, 9 ... Cleaning mechanism, 10 ... Computer DESCRIPTION OF SYMBOLS 11 ... Electrolyte measurement part, 12 ... Memory | storage device, 13 ... Control part, 14 ... Piezoelectric element driver, 15 ... Stirring mechanism controller, 16 ... Sample container, 17 ... Circular sample disk, 18 ... Reagent bottle, 19 ... Circular reagent disk , 20 ... Cold storage, 21 ... Reaction vessel, 22 ... Reaction vessel holder, 23 ... Drive mechanism, 24 ... Sample probe, 25 ... Sample probe support shaft, 26 ... Sample probe arm, 27 ... Reagent probe, 28 ... Reagent probe support Axis 29 ... Reagent probe arm 30 ... Sampling mechanism for electrolyte measurement 31 ... Fixing part 33 ... Nozzle 34 ... Vertical drive mechanism 35 ... electrolyte measurement sample probe, 36 ... sample probe supporting shaft for electrolyte measurement, 37 ... electrolyte measurement sample probe arm,
201 ... Sample container 202 ... Probe 203 ... Dilution container 204 ... Na ion selection electrode 205 ... K ion selection electrode 206 ... Cl ion selection electrode 207 ... Comparative electrode 208 ... Sipper syringe 209 ... Internal standard solution Syringe, 210 ... Diluent syringe, 211 ... Pinch valve, 212 ... Two-way solenoid valve for reference electrode, 213 ... Two-way solenoid valve for sucking sipper syringe, 214 ... Two-way solenoid valve for discharging waste liquid, 215 ... Discharging internal standard solution Two-way solenoid valve for use, 216 ... Two-way solenoid valve for suction of internal standard solution, 217 ... Two-way solenoid valve for discharge of diluent, 218 ... Two-way solenoid valve for suction of dilution solution, 219 ... Comparison electrode solution bottle, 220 ... Inside Standard solution bottle, 221 ... Dilution solution bottle, 222 ... Sipper nozzle, 223 ... Dilution solution heater, 224 ... Internal standard solution heater, 225 ... Dilution container heater Tha, 226 ... ion selective electrode heater, 227 ... reference electrode heater, 228 ... vacuum nozzle.

Claims (8)

An electrolyte measurement unit for measuring an electrolyte in a liquid by an electrode method;
A storage unit for storing an electromotive force measured by the electrolyte measurement unit;
A container for holding a liquid;
A dispensing unit for dispensing a liquid into the container;
A sipper nozzle that sucks the liquid in the container and supplies the liquid to the electrolyte measurement unit;
The electromotive force (E0) measured by the electrolyte measurement unit in a state where the sipper nozzle is not in contact with the liquid in the container is stored in the storage unit, and the sipper nozzle is in contact with the liquid in the container The process of detecting the liquid level of the liquid in the container based on the electromotive force (En) obtained by the electrolyte measurement unit in the process up to and the electromotive force (E0) stored in the storage unit And an automatic analyzer characterized by comprising a control unit for controlling the operation. The automatic analyzer according to claim 1, further comprising:
A specified value storage unit for storing a specified value for determining a difference between the electromotive force (En) and the electromotive force (E0);
The controller is configured to repeat the dispensing of the liquid into the container until the sipper nozzle is in contact with the liquid in the container, and the electromotive force (En) and the electromotive force (E0). An automatic analyzer characterized by determining that the difference is equal to or greater than the specified value and detecting the liquid level of the liquid in the container. The automatic analyzer according to claim 1, further comprising:
A specified value storage unit for storing a specified value for determining a difference between the electromotive force (En) and the electromotive force (E0);
In the process of repeatedly lowering the sipper nozzle to the container until the sipper nozzle is in contact with the liquid in the container, the controller is configured to generate the electromotive force (En) and the electromotive force (E0). An automatic analyzer characterized by determining that the difference is equal to or greater than the specified value and detecting the liquid level of the liquid in the container. The automatic analyzer according to claim 1, further comprising:
A specified value storage unit for storing a specified value for determining a difference between the electromotive force (En) and the electromotive force (E0);
The control unit starts dispensing the liquid into the container at the dispensing unit in the process of repeating the dispensing of the liquid into the container until the sipper nozzle is in contact with the liquid in the container. Then, the time until the difference between the electromotive force (En) and the electromotive force (E0) becomes equal to or greater than the specified value is measured, and from the measured time, the dispensing unit dispenses the container. An automatic analyzer that calculates a flow rate of the liquid. An electrolyte measurement unit for measuring an electrolyte in a liquid by an electrode method;
A container for holding a liquid;
A dispensing unit for dispensing a liquid into the container;
A sipper nozzle that sucks the liquid in the container and supplies the liquid to the electrolyte measurement unit;
In a control method of an automatic analyzer comprising a control unit for controlling processing for detecting the liquid level of the liquid in the container,
As control of the control unit,
Sucking the liquid in the container using the sipper nozzle and filling the space between the electrolyte measuring unit and the sipper nozzle with the liquid;
Based on an electromotive force generated between the electrolyte measurement unit and the sipper nozzle, an electromotive force serving as a reference for detecting that the liquid in the container is contained up to a predetermined amount or a predetermined liquid level. And (E0) obtaining step. A method for controlling an automatic analyzer. In the control method of the automatic analyzer according to claim 5,
The step of obtaining the electromotive force (E0) is a step of measuring the electromotive force (E0) in the electrolyte measurement unit in a state where the sipper nozzle is not in contact with the liquid in the container,
As control of the control unit,
Measuring the electromotive force (En) by the electrolyte measurement unit in the process of repeating the dispensing of the liquid into the container until the sipper nozzle is in contact with the liquid in the container;
It is determined that the difference between the electromotive force (En) and the electromotive force (E0) is equal to or greater than a specified value, and the liquid in the container is accommodated to a predetermined amount or a predetermined liquid level. And a step of detecting the automatic analyzer. In the control method of the automatic analyzer according to claim 5,
The step of obtaining the electromotive force (E0) is a step of measuring the electromotive force (E0) in the electrolyte measurement unit in a state where the sipper nozzle is not in contact with the liquid in the container,
As control of the control unit,
Measuring the electromotive force (En) by the electrolyte measurement unit in the process of repeatedly lowering the sipper nozzle to the container until the sipper nozzle is in contact with the liquid in the container;
It is determined that the difference between the electromotive force (En) and the electromotive force (E0) is equal to or greater than a specified value, and the liquid in the container is accommodated to a predetermined amount or a predetermined liquid level. And a step of detecting the automatic analyzer. In the control method of the automatic analyzer according to claim 5,
The step of obtaining the electromotive force (E0) is a step of measuring the electromotive force (E0) in the electrolyte measurement unit in a state where the sipper nozzle is not in contact with the liquid in the container,
As control of the control unit,
In the process of repeating the dispensing of the liquid into the container until the sipper nozzle is in contact with the liquid in the container, the dispensing of the liquid into the container at the dispensing unit, Measuring a time until a difference between an electromotive force (En) and the electromotive force (E0) becomes a specified value or more;
And a step of calculating a flow rate of the liquid dispensed into the container by the dispensing unit from the measured time.

Images