CN113390808A - Water quality analyzer and water quality analyzing method - Google Patents

Water quality analyzer and water quality analyzing method Download PDF

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Publication number
CN113390808A
CN113390808A CN202110672009.7A CN202110672009A CN113390808A CN 113390808 A CN113390808 A CN 113390808A CN 202110672009 A CN202110672009 A CN 202110672009A CN 113390808 A CN113390808 A CN 113390808A
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sample liquid
cell
data
light
reagent
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CN113390808B (en
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俣野芳朗
河野忠司
石井章夫
田中弘子
北村巧
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Horiba Ltd
Horiba Advanced Techno Co Ltd
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Horiba Ltd
Horiba Advanced Techno Co Ltd
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Abstract

The invention provides a water quality analysis device and a water quality analysis method capable of simply and rapidly determining the error of the device. Sequentially executing: a sample liquid injection step; injecting a reagent; a reaction step; and a measurement step of measuring a predetermined measurement target component contained in the sample liquid having undergone the reaction step in the cell, wherein light is continuously irradiated to the cell using the same light source from the sample liquid injection step to the measurement step and the light emitted from the cell is detected by the light detection section, wherein the water quality analyzer includes a data storage section and a display section, the data storage section stores continuous reference data obtained by using the same light source from the sample liquid injection step to the measurement step and continuous light detection data obtained by using the same light source from the sample liquid injection step to the measurement step or calculation data calculated using the light detection data obtained by the light detection section, and the display section displays the reference data and the light detection data or the calculation data as actual data in a broken line diagram.

Description

Water quality analyzer and water quality analyzing method
The present application is a divisional application of patent application No. 201410310958.0 entitled "water quality analyzing apparatus and water quality analyzing method" filed on 2014/07/01.
Technical Field
The present invention relates to a water quality analyzer and a water quality analyzing method for analyzing water quality.
Background
As a water quality analyzer for analyzing nitrogen, phosphorus, and the like contained in a liquid sample (sample liquid) such as sewage and sewage, for example, there is an apparatus disclosed in patent document 1.
The water quality analyzer measures the amount of nitrogen contained in a sample liquid by injecting a predetermined reagent into the sample liquid, reacting the reagent with the sample liquid, irradiating the sample liquid with light, and performing light absorption measurement using ultraviolet spectroscopy.
Documents of the prior art
Patent document 1: japanese patent laid-open publication No. Hei 10-142216
However, in the conventional water quality analyzing apparatus, when an error occurs, it is necessary to identify an error occurrence step (step) in which the error occurs by, for example, trial and error and to confirm the error occurrence step, thereby finding the cause of the error.
Even if the error occurrence process is determined, there are many elements that may cause an error in the error occurrence process, and these elements need to be checked one by one, which is a problem in that the work of determining the specific cause is extremely complicated and takes much time.
Disclosure of Invention
In view of the above-described problems, a main object of the present invention is to provide a water quality analyzer and a water quality analyzing method, which can easily and quickly identify an error occurrence process of the analyzer or an error cause thereof.
That is, the present invention provides a water quality analyzer which sequentially executes: a sample liquid injection step of injecting a sample liquid into the cell; a reagent injection step of injecting a reagent into the cell; a reaction step of reacting the sample solution and the reagent in the cell; and a measuring step of measuring a predetermined measurement target component contained in the sample liquid having undergone the reaction step in the cell, wherein the same light source is used to continuously irradiate the cell with light and a light detection unit is used to detect the light emitted from the cell from the sample liquid injecting step to the measuring step, the water quality analyzer includes a data storage unit for storing continuous reference data obtained by using the same light source from the sample liquid injection step to the measurement step, and continuous light detection data obtained by using the same light source from the sample liquid injection step to the measurement step or calculation data calculated by using the light detection data, the display unit displays the reference data and the light detection data or the calculation data as actual data in a line graph.
Furthermore, the present invention provides a water quality analysis method, which sequentially comprises: a sample liquid injection step of injecting a sample liquid into the cell; a reagent injection step of injecting a reagent into the cell; a reaction step of reacting the sample solution and the reagent in the cell; and a measurement step of measuring a predetermined measurement target component contained in the sample liquid having undergone the reaction step in the cell, wherein light is continuously irradiated to the cell using the same light source and light emitted from the cell is detected by a light detection unit from the sample liquid injection step to the measurement step, continuous reference data obtained by using the same light source from the sample liquid injection step to the measurement step, and continuous light detection data obtained by using the same light source from the sample liquid injection step to the measurement step or calculation data calculated using the light detection data are stored in a data storage unit, and the reference data and the light detection data or the calculation data as actual data are displayed in a broken line diagram.
Further, the present invention provides a water quality analyzing apparatus which performs: a sample liquid injection step of injecting a sample liquid into the cell; a reagent injection step of injecting a reagent into the cell; a reaction step of reacting the sample solution and the reagent in the cell; and a measurement step of measuring a predetermined measurement target component contained in the sample liquid that has undergone the reaction step in the cell, wherein the water quality analyzer includes a data storage unit, and in the sample liquid injection step, the reagent injection step, the reaction step, and the measurement step, light is irradiated to the cell and light emitted from the cell is detected by a light detection unit, and the data storage unit stores light detection data obtained by the light detection unit or calculation data calculated using the light detection data.
According to the water quality analyzer described above, since the light detection data or the calculation data obtained by irradiating the cell with light is stored in the data storage unit in the sample liquid injection step, the reagent injection step, the reaction step, and the measurement step, the error generation step and the error cause can be specified in all the steps by displaying and checking the stored data on, for example, a display. Examples of the error generation step and the error cause include deterioration of a reagent, deterioration and failure of peripheral devices used in the respective steps, and an injection error of a sample solution and a reagent.
In the measurement step, it is preferable that the light irradiated to the cell in the sample liquid injection step, the reagent injection step, and the reaction step and the light irradiated to the sample liquid in the measurement step are emitted from the same light source.
According to the above configuration, in the sample solution injecting step, the reagent injecting step, and the reaction step, since the cell can be irradiated with light from the light source used in the measurement step, it is not necessary to separately prepare a light source, and the apparatus configuration can be further simplified. In addition, the structure can be easily realized just because the reaction step and the measurement step are performed using the same cell.
A water quality analysis method using a water quality analyzer according to the present invention includes: a sample liquid injection step of injecting a sample liquid into the cell; a reagent injection step of injecting a reagent into the cell; a reaction step of reacting the sample solution and the reagent in the cell; and a measuring step of measuring a predetermined measurement target component contained in the sample liquid having undergone the reaction step in the cell, wherein in the sample liquid injecting step, the reagent injecting step, the reaction step, and the measuring step, light is irradiated to the cell, light emitted from the cell is detected by a light detecting unit, and light detection data or calculation data calculated using the light detection data is stored in a data storage unit.
According to the present invention, an error generation process of a device or an error cause thereof can be easily and quickly specified.
Drawings
Fig. 1 is a schematic diagram showing a water quality analyzer according to the present embodiment.
Fig. 2 is a flowchart showing a nitrogen component analysis method of the water quality analyzer according to the same embodiment as that shown in fig. 1.
FIG. 3 is a diagram showing nitrogen component analysis performed by using a water quality analyzer according to the same embodiment as that of FIG. 1.
Fig. 4 is a diagram showing nitrogen component analysis performed by using a water quality analyzer according to the same embodiment as that of fig. 1.
Description of the reference numerals
1. water quality analysis device
6. pool (measuring pool)
8. light detecting section
Detailed Description
An embodiment of the water quality analyzer of the present invention will be described below.
The water quality analyzer 1 of the present embodiment measures the concentration of a predetermined measurement target component such as nitrogen and phosphorus contained in a liquid sample (sample liquid) such as sewage and sewage by using an ultraviolet spectrophotometry, and as shown in fig. 1, the water quality analyzer 1 includes: an analysis device 2 for analyzing the sample liquid; and a control device 3 that controls the analysis device 2.
As shown in fig. 1, the analysis apparatus 2 includes: a sample liquid metering mechanism 4 for metering a sample liquid; a reagent metering mechanism 5 for metering a reagent; a measuring cell 6 into which the sample liquid measured by the sample liquid measuring mechanism 4 and the reagent measured by the reagent measuring mechanism 5 are injected; a light source 7 that irradiates light to the measuring cell 6; and a light detection unit 8 for detecting light emitted from the measuring cell 6.
The sample liquid measuring mechanism 4 measures a predetermined amount of sample liquid, and includes: a sample liquid container (not shown) for containing a sample liquid; a measuring section 4 a; and a sample liquid pipe 4b for introducing the sample liquid measured by the measuring section 4a into the measuring cell 6. The sample liquid pipe 4b is provided with a first on-off valve 4c for opening and closing the inside of the pipe.
The reagent measuring mechanism 5 measures a predetermined constant amount of reagent, and includes: a reagent container (not shown) for storing a reagent; a measuring section 5 a; and a reagent pipe 5a for introducing the reagent measured by the measuring section 5a into the measuring cell 6. The reagent pipe 5b is provided with a second on-off valve 5c for opening and closing the inside of the pipe.
The reagent of the present embodiment is a reagent for analyzing a nitrogen component contained in a sample solution, and sodium hydroxide, potassium peroxodisulfate, and hydrochloric acid are used, for example. Further, a metering mechanism 5 is provided for each reagent.
The measuring cell 6 is filled with a predetermined amount of the sample liquid measured by the sample liquid measuring mechanism 4 and a predetermined amount of the reagent measured by the reagent measuring mechanism 5, and the sample liquid filling step, the reagent filling step, the reaction step, the pH adjustment step, the measurement step, and the waste liquid step, which will be described later, are performed in the measuring cell 6.
The light source 7 irradiates the measuring cell 6 with light having a predetermined wavelength (for example, light having an ultraviolet wavelength band such as 220 nm). As the light source, for example, a UV lamp such as a xenon lamp, an ultraviolet LED, or the like can be used.
The light detection unit 8 detects light that is emitted from the light source 7 to the measurement cell 6 and transmitted through the measurement cell 6. As the light detection unit 8, for example, a photomultiplier tube (PMT) that converts light of a predetermined wavelength (light having an ultraviolet wavelength band) transmitted through the measuring cell 6 into an electric signal (light detection data) corresponding to the light intensity of the transmitted light can be used.
The analysis device 2 of the structure is controlled by a control device 3.
The control device 3 is a dedicated or general-purpose computer having a CPU, an internal memory, an I/O buffer circuit, an AD converter, and the like, and performs information processing by operating according to a program stored in a predetermined area of the internal memory, and as shown in fig. 1, the control device 3 functions as an analysis control unit 10, a data management unit 11, a data storage unit 12, a display unit 13, and a density calculation unit 14.
Specifically, as shown in fig. 2, the control device 3 sequentially controls the analysis device 2, and specifically, the control device 3 performs a series of analysis processes including a sample liquid injection step, a reagent injection step, a reaction step, a pH adjustment step, a measurement step, and a waste liquid step.
In the sample liquid pouring step, the analysis controller 10 controls the sample liquid measuring mechanism 4 to pour the measured sample liquid into the measuring cell 6.
In the reagent injection step, the analysis controller 10 controls the reagent metering mechanism 5 to inject the metered reagents (sodium hydroxide and potassium peroxodisulfate) into the measuring cell 6.
In the reaction step, the analysis control unit 10 controls the heater 15 to heat a solution composed of the sample solution and the reagent mixed in the measuring cell 6, and controls the ultraviolet light source 9 to irradiate the solution with ultraviolet light to hydrolyze the sample solution contained in the solution with the reagent. The ultraviolet light source 9 may be a UV lamp, an LED, or the like, for example, and a mercury lamp is used in the present embodiment, as the light having a wavelength necessary for the hydrolysis reaction.
In the pH adjustment step, the analysis controller 10 controls the reagent measuring mechanism 5 to add a measured reagent (hydrochloric acid) to the solution to neutralize the solution.
In the measurement step, the analysis control unit 10 controls the light source 7 to irradiate the measuring cell 6 with light, and the light detection unit 8 detects transmitted light emitted from the measuring cell 6. The light detection data obtained by the light detection unit 8 is output to the concentration calculation unit 14, and the concentration calculation unit 14 measures the concentration of nitrogen contained in the sample liquid using the light detection data.
In the waste liquid step, the solution in the measuring cell 6 having passed through the measuring step is discharged.
The control device 3 of the present embodiment has a cause specifying function for specifying an error that may occur in a series of analysis processes including a sample liquid injection step, a reagent injection step, a reaction step, a pH adjustment step, a measurement step, and a waste liquid step, or a cause of the error, by the analysis control unit 10, the data management unit 11, the data storage unit 12, and the display unit 13.
Specifically, for example, when a certain error occurs in the water quality analyzer 1, the analysis controller 10 of the control device 3 controls the light source 7 to continuously irradiate the measuring cell 6 with light in a series of analysis processes from the sample liquid injection step to the waste liquid step. The light transmitted through the measuring cell 6 is detected as light detection data by the light detection section 8 and transmitted to the data management section 11. The data management unit 11 stores the light detection data or calculation data indicating the absorbance calculated using the light detection data in the data storage unit 12. The data management unit 11 may acquire calculation data indicating the absorbance calculated by the concentration calculation unit 14 and store the calculation data in the data storage unit 12.
The data storage unit 12 is constituted by an internal memory built in the device, and includes: a reference data storage unit 12a that stores data (reference data) obtained when the nitrogen analysis is normally performed; and an actual data storage unit 12b that stores data (actual data) detected by the light detection unit 8. The actual data transmitted from the data management unit 11 is stored in the actual data storage unit 12 b.
The data management unit 11 acquires the reference data stored in the reference data storage unit 12a and the actual data stored in the actual data storage unit 12b, and transmits them to the display unit 13. The display unit 13 displays these data as a line graph on a display. The user and the manager can confirm the line graph to determine which step has an error or the cause of the error in a series of analysis processes from the sample liquid injection step to the waste liquid step.
Specifically, errors that may occur in each step and the causes of the errors are exemplified.
In the sample liquid injection step, an error in which the sample liquid is not injected into the measuring cell 6 may be considered, and the cause of the error may be a failure of the sample liquid metering mechanism 4, an injection error of the sample liquid, and the like.
In the reagent injection step, an error in which the reagent is not injected into the measuring cell 6 may be considered, and the cause of the error may be a failure of the reagent metering mechanism 5, an injection error of the reagent (potassium peroxodisulfate and sodium hydroxide), or the like.
In the reaction step, an error in which no reaction occurs, an error in which the reaction rate is slow, and the like are considered, and the causes of the error include deterioration and failure due to deterioration and failure of the heater 15 and the ultraviolet light sources 7 and 9, deterioration of the reagent, and the like.
In the pH adjustment step, an error such as non-neutralization may be considered, and the cause of the error is an injection error of the reagent (hydrochloric acid).
In the measurement step, it is conceivable that an error of a normal measurement value does not occur, and the cause of the error is, for example, deterioration or failure of the light source 7 or the light detection unit 8. In addition, when an error occurs in the measurement step, the cause may be an error generated in any one of the steps, and the measurement step may check an error of the entire preprocessing step before the measurement step.
In the waste liquid step, an error in which waste liquid is not normally discharged may be considered, and the cause of the error may be a failure of a waste liquid mechanism or the like, not shown.
Further, when light is irradiated from the light source 7 to the measuring cell 6, since the reagent in the measuring cell 6 is also irradiated with light, the actual data stored in the actual data storage unit 12b also includes light detection data or calculation data of light transmitted through the reagent. Here, since the characteristics of the absorbance of each reagent are known in advance, the type, amount, and the like of the reagent can be determined from a map showing these actual data.
The data management unit 11 may store the reference data stored in the reference data storage unit 12a and the actual data stored in the actual data storage unit 12b in an external memory such as an SD card or a USB memory, which is detachably provided in the apparatus, and allow the user or the administrator to display and confirm the stored data on the display at an arbitrary place.
Next, a method for identifying the cause of an error using the water quality analyzer 1 of the present embodiment will be described with reference to fig. 3 and 4. Fig. 3 and 4 are graphs of calculation data displayed on the display by the display unit 13, in which the horizontal axis represents time (seconds) and the vertical axis represents the amount of light received by the light detection unit 8. In both fig. 3 and 4, the reference data and the actual data are superimposed on the same drawing.
Fig. 3 shows a waveform a showing reference data and a waveform B showing actual data superimposed from the sample liquid injection step to the measurement step.
In the figure, if comparing the waveform a and the waveform B, the waveform B when an error occurs in the portion r1 enclosed by a circle greatly deviates from the waveform a in the normal state. This is considered to be because the amount of potassium peroxodisulfate contained as a reagent in the solution in the pH adjustment step is not changed. Therefore, it can be understood that an error is generated in the pH adjustment step, and in addition, the reason for the error is that hydrochloric acid is not injected into the measuring cell 6 and the solution is not neutralized.
Fig. 4 shows a waveform a of the reference data and waveforms C, D, and E of the actual data superimposed on each other from the reagent injection step to the pH adjustment step.
When the actual data is the waveform C, if the waveform a and the waveform C are compared, the absorbance of the waveform C is smaller than that of the waveform a in the reagent injection step, and the waveform C sharply decreases to a point on an extension line of a straight portion of the waveform a in the reaction step (when the ultraviolet light source is turned on). Therefore, it can be seen from the actual data of the waveform C that the cause of the error is the possibility that the potassium peroxodisulfate as the reagent is not injected into the sample liquid in the reagent injection step or that the reagent is not operated at all (for example, pure water is injected).
Next, when the actual data is the waveform D, if the waveform a and the waveform D are compared, the absorbance of the waveform D is smaller than that of the waveform a in the reagent injection step, and the inclination angle of the rising speed (rising) of the light amount of the waveform D is steeper than that of the waveform a in the reaction step. Therefore, it can be seen from the data of the waveform D that the cause of the error is the possibility of deterioration of the potassium peroxodisulfate injected into the sample liquid in the reagent injection step.
Finally, if the actual data is the waveform E, if the waveform a and the waveform E are compared, the absorbance of the waveform E becomes larger in the reagent injection step as in the waveform a, but the inclination angle of the rising speed (rise) of the light amount of the waveform E is gentler than that of the waveform a in the reaction step. Therefore, it was found that the cause of the error was the possibility of deterioration of the ultraviolet light source 9 irradiated to the cell in the reaction step.
The water quality analyzer 1 having the above configuration has the following effects.
Since the light detection data or calculation data obtained by irradiating the measuring cell 6 with light from the sample liquid injection step to the waste liquid step is stored in the data storage unit 12, the error generation step and the error cause can be specified in all the steps as long as the stored data is displayed on a display or the like and confirmed.
In the present embodiment, since the steps from the sample liquid injection step to the measurement step are performed in the same measurement cell 6, time for changing the cell or the like in the middle of the step can be saved, and the apparatus configuration can be simplified.
In the sample solution injection step, the reagent injection step, the reaction step, the pH adjustment step, and the waste solution step, since the measuring cell 6 can be irradiated with light from the light source 7 used in the measurement step, it is not necessary to separately prepare a light source, and the apparatus configuration can be further simplified.
In addition, the present invention is not limited to the embodiments.
In the above embodiment, the light detection data or the calculation data is stored in all the steps, but the light detection data or the light calculation data may be stored only in a specific step.
In the above embodiment, the same light source is used in all the steps, but different light sources may be used for the light source for irradiating the cell in the measurement step and the light source for irradiating the measurement cell 6 with light in the sample solution injection step, the reagent injection step, the reaction step, the pH adjustment step, and the waste solution step.
The present invention can be variously modified within a range not departing from the gist of the present invention.
The technical features described in the embodiments of the present invention may be combined with each other to form a new technical solution.

Claims (3)

1. A water quality analyzing apparatus, characterized in that the water quality analyzing apparatus sequentially executes: a sample liquid injection step of injecting a sample liquid into the cell; a reagent injection step of injecting a reagent into the cell; a reaction step of reacting the sample solution and the reagent in the cell; and a measuring step of measuring a predetermined measurement target component contained in the sample liquid subjected to the reaction step in the cell,
the cell is irradiated with light continuously from the sample solution injection step to the measurement step using the same light source and the light emitted from the cell is detected by a light detection unit,
the water quality analysis device comprises a data storage part and a display part,
the data storage unit stores continuous reference data obtained by using the same light source from the sample liquid injection step to the measurement step, and continuous light detection data obtained by using the same light source from the sample liquid injection step to the measurement step obtained by the light detection unit or calculation data calculated by using the light detection data,
the display unit displays the reference data and the light detection data or the calculation data as actual data in a line graph.
2. The water quality analyzing apparatus according to claim 1,
in the measuring step, a predetermined measurement target component contained in the sample liquid is measured by irradiating the sample liquid with light,
the light irradiated to the cell in the sample solution injecting step, the reagent injecting step, and the reaction step and the light irradiated to the sample solution in the measurement step are light emitted from the same light source.
3. A water quality analysis method is characterized by sequentially comprising the following steps: a sample liquid injection step of injecting a sample liquid into the cell; a reagent injection step of injecting a reagent into the cell; a reaction step of reacting the sample solution and the reagent in the cell; and a measuring step of measuring a predetermined measurement target component contained in the sample liquid subjected to the reaction step in the cell,
the sample liquid injection step to the measurement step are performed by irradiating the cell with light continuously using the same light source and detecting the light emitted from the cell by a light detection unit, and continuous reference data obtained by using the same light source from the sample liquid injection step to the measurement step, and continuous light detection data obtained by using the same light source from the sample liquid injection step to the measurement step or calculation data calculated by using the light detection data are stored in a data storage unit,
the reference data and the light detection data or the calculation data as actual data are displayed in a line graph.
CN202110672009.7A 2013-07-29 2014-07-01 Water quality analysis device and water quality analysis method Active CN113390808B (en)

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JP2013-157069 2013-07-29
JP2013157069A JP6174411B2 (en) 2013-07-29 2013-07-29 Water quality analyzer and water quality analysis method
CN201410310958.0A CN104345033A (en) 2013-07-29 2014-07-01 Apparatus and method for analyzing water quality

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CN201410310958.0A Division CN104345033A (en) 2013-07-29 2014-07-01 Apparatus and method for analyzing water quality

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CN113390808A true CN113390808A (en) 2021-09-14
CN113390808B CN113390808B (en) 2024-04-26

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JPH06288923A (en) * 1993-04-02 1994-10-18 Japan Organo Co Ltd Analyzer for silica content in water
JPH07243964A (en) * 1994-03-07 1995-09-19 Doriko Kk Water quality measuring device, water quality measuring method, and waste water treating method
CN101865833A (en) * 2009-11-24 2010-10-20 宇星科技发展(深圳)有限公司 Method and system for monitoring total phosphorus and total nitrogen of water quality on line
CN101960294A (en) * 2008-03-19 2011-01-26 小幡彻 Gel particle measuring apparatus
CN102419367A (en) * 2010-09-24 2012-04-18 株式会社堀场制作所 Whole blood immunity measuring device and whole blood immunity measuring method
CN102519887A (en) * 2005-03-29 2012-06-27 希森美康株式会社 Method of analyte analysis and analyte analyzer
CN102985829A (en) * 2010-07-14 2013-03-20 株式会社日立高新技术 Automatic analysis device, analysis method and information processing device

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06288923A (en) * 1993-04-02 1994-10-18 Japan Organo Co Ltd Analyzer for silica content in water
JPH07243964A (en) * 1994-03-07 1995-09-19 Doriko Kk Water quality measuring device, water quality measuring method, and waste water treating method
CN102519887A (en) * 2005-03-29 2012-06-27 希森美康株式会社 Method of analyte analysis and analyte analyzer
CN101960294A (en) * 2008-03-19 2011-01-26 小幡彻 Gel particle measuring apparatus
CN101865833A (en) * 2009-11-24 2010-10-20 宇星科技发展(深圳)有限公司 Method and system for monitoring total phosphorus and total nitrogen of water quality on line
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CN102419367A (en) * 2010-09-24 2012-04-18 株式会社堀场制作所 Whole blood immunity measuring device and whole blood immunity measuring method

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