KR101903013B1 - Apparatus and method for measuring concentration of chemical solutions - Google Patents
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- KR101903013B1 KR101903013B1 KR1020160060239A KR20160060239A KR101903013B1 KR 101903013 B1 KR101903013 B1 KR 101903013B1 KR 1020160060239 A KR1020160060239 A KR 1020160060239A KR 20160060239 A KR20160060239 A KR 20160060239A KR 101903013 B1 KR101903013 B1 KR 101903013B1
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- 239000000126 substance Substances 0.000 title claims abstract description 59
- 238000000034 method Methods 0.000 title claims abstract description 56
- 238000012545 processing Methods 0.000 claims abstract description 3
- 238000005259 measurement Methods 0.000 claims description 69
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 37
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- 229920002449 FKM Polymers 0.000 description 1
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
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- ZRBROGSAUIUIJE-UHFFFAOYSA-N azanium;azane;chloride Chemical compound N.[NH4+].[Cl-] ZRBROGSAUIUIJE-UHFFFAOYSA-N 0.000 description 1
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/3103—Atomic absorption analysis
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
- G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
- G01J3/46—Measurement of colour; Colour measuring devices, e.g. colorimeters
- G01J3/50—Measurement of colour; Colour measuring devices, e.g. colorimeters using electric radiation detectors
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
- G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
- G01J3/46—Measurement of colour; Colour measuring devices, e.g. colorimeters
- G01J3/50—Measurement of colour; Colour measuring devices, e.g. colorimeters using electric radiation detectors
- G01J3/502—Measurement of colour; Colour measuring devices, e.g. colorimeters using electric radiation detectors using a dispersive element, e.g. grating, prism
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
- G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
- G01J3/46—Measurement of colour; Colour measuring devices, e.g. colorimeters
- G01J3/50—Measurement of colour; Colour measuring devices, e.g. colorimeters using electric radiation detectors
- G01J2003/503—Densitometric colour measurements
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Abstract
The present invention relates to an apparatus and method for analyzing the concentration of a chemical solution capable of quickly and accurately measuring the concentration of a specific component in a solution composition in a process using the RGB color sensor in real time from a processing apparatus .
Description
The present invention relates to an apparatus and method for analyzing the concentration of a chemical solution, and more particularly, to a method and apparatus for analyzing the concentration of a specific component in a chemical solution in a process using the chemical solution, And an apparatus and method for analyzing the concentration of a solution.
The composition and the concentration of the etching liquid in the liquid crystal substrate manufacturing process must be strictly controlled in accordance with the high definition of the pattern. The analysis of the concentration of a specific component of a chemical solution such as an etching solution was generally performed by a user directly taking a drug and analyzing it using a wet analysis or an analyzer in an analytical room and measuring the concentration of a specific component in the chemical solution accurately in real time It was impossible to do.
For example, as a conventional method for analyzing the concentration of phosphoric acid, ascorbic acid reduction method is used. For example, a sample pretreated in a laboratory is diluted, a coloring is performed by mixing ascorbic acid and molybdic acid, and a spectrophotometer a method of analyzing the concentration of phosphoric acid by measuring the absorbance using an analyzer such as a spectrophotometer is known.
As a method for analyzing the copper concentration, for example, in the case of the chelate titration method, the concentration of copper should be calculated by diluting the sample, titrating with a predetermined amount of ammonia ammonium chloride buffer, methanol and pan indicator, and EDTA standard solution. There is a limit to the accuracy of the wet analysis method.
As a method for analyzing iron concentration, for example, atomic absorption spectrophotometry, an ionized sample is taken in an appropriate amount of beaker, and nitric acid is added and boiled to form a precipitate. The precipitate is dissolved in hydrochloric acid at a predetermined concentration, The concentration of iron should be analyzed by measuring the absorbance using an absorption analyzer.
As described above, in order to accurately analyze the concentration of a specific component in a chemical solution, expensive analytical instruments are indispensable, the analysis method is complicated, and a considerable amount of time is required for analysis. Therefore, in various processes using a chemical solution, It is difficult to analyze and manage concentrations of necessary components in real time.
SUMMARY OF THE INVENTION It is an object of the present invention to provide a chemical solution capable of quickly and accurately measuring in-line the concentration of a specific component in a chemical solution in various processes using a chemical solution. And to provide a concentration analyzing apparatus and method.
It is a further object of the present invention to provide a method of automatically and accurately controlling the process of transferring, supplying, and mixing a reagent required for pretreatment such as color development by taking a part of a chemical solution as a sample and measuring it from a sample using an RGB color sensor And an apparatus and method for analyzing the concentration of a chemical solution capable of analyzing the concentration of a specific component in real time using the RGB values.
According to one aspect of the present invention for achieving the above object,
A storage part for storing the additive solution; A transfer unit for transferring the sample to be analyzed to the mixing unit; A mixing part for mixing the sample to be analyzed and the additive solution; A measuring unit for measuring the concentration of the specific component from the mixed solution; A control unit receiving a measurement value of a specific component from the measurement unit and controlling the transfer unit; And a user operation unit for displaying an operation signal input by the user and a concentration measurement value,
The measurement unit includes an RGB color sensor for measuring the concentration of the sample, measures the RGB color sensor measurement value of the RGB color sensor measurement value of the deionized water and the concentration of the RGB color sensor measurement value of the sample, (Rx), I (Gx) and I (B0) of the deionized water and the RGB color sensor measurement values I (Rx), I Bx) is calculated and the corrected R ', G' and B 'values are calculated for the deionized water color with respect to the known concentration of the component to be measured by the following equation, (Rx), I (Gx), and I (Bx) of an unknown object to be measured in the sample are converted into numerical values, The density value corresponding to the reference data is compared with the reference data on the calibration line, It relates to a chemical solution of a concentration analysis device being configured to calculate a concentration of the substance.
[Equation]
Another aspect of the present invention is a method of measuring colorimetric data comprising: measuring RGB color sensor measurements I (R0), I (G0), I (Bo) of deionized water;
Measuring RGB color sensor measurement values I (Rx), I (Gx), and I (Bx) by adding and coloring an additive solution containing a coloring reagent to a plurality of samples having known concentrations;
Calculating RGB color sensor measurement values R ', G', B 'of a sample whose concentration is corrected for deionized water color using the following equation:
[Equation]
G ', and B' values measured using an RGB color sensor for a sample of known concentration, corrected for deionized water color, to calculate the relationship of the color change according to the concentration change of the sample, ;
(Rx), I (Gx), and I (Bx) of an unknown object to be measured in the sample are measured in numerical values by selecting one of R ', G' To the reference data on the calibration line, and calculating the concentration value corresponding to the reference data as the concentration of the measurement target substance.
According to the present invention, since the chemical solution extracted in real time can be measured by measuring the RGB color sensor measurement value by the RGB color sensor of the measurement unit, the concentration can be analyzed, so that a relatively low-priced apparatus configuration becomes possible, It is possible to quickly and accurately measure the concentration in real time in-line, which makes it easy to analyze and manage the concentrations of necessary components of the process chemicals.
In addition, according to the present invention, it is possible to measure the concentration of all the process chemicals which can change color or develop color by color change.
According to the method of the present invention, deionized water is put into a measuring unit to measure I (Rx), I (G0), and I (B0) of the measured RGB color sensor I (R0) It is possible to measure the values of I (Gx) and I (Bx) by measuring the values of I (Bx) and I (Bx) Even if a change occurs due to a change in the condition, the concentration can be accurately measured and analyzed without error in the concentration measurement.
1 is a schematic block diagram of an apparatus for analyzing a chemical solution concentration according to an embodiment of the present invention.
2 is a detailed block diagram of a measuring unit of the chemical solution concentration analyzing apparatus according to the present invention.
3 is a graph showing a calibration curve showing changes in R ', B' and G 'values according to the change in the concentration of phosphoric acid calculated in Example 1 of the present invention.
4 is a graph showing a calibration curve showing changes in R ', B' and G 'values according to the concentration change of copper in Example 2 of the present invention.
FIG. 5 is a graph showing a calibration curve showing changes in the values of R ', B' and G 'according to the concentration of iron ions in Example 3 of the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, the present invention will be described in detail with reference to the accompanying drawings.
In the present invention, the " ± RGB color sensor measurement value " means a value obtained by quantifying the energy spectrum intensity of the received light after passing through the sample in the analysis container.
"° RGB color sensor values of deionized water I (R 0 ), I (G 0 ), I (B 0 )" ± indicate the color of deionized water in R, G and B wavelength ranges Means an electrical signal value.
FIG. 1 is a schematic block diagram of a chemical solution concentration analyzing apparatus according to an embodiment of the present invention, and FIG. 2 is a detailed block diagram of a measuring unit of the chemical solution concentration analyzing apparatus according to the present invention.
Referring to FIGS. 1 and 2, the apparatus for analyzing the concentration of a chemical solution of the present invention includes a
The
[Equation]
As for the calibration curve, the highest value of the slope of RGB can be selected as the calibration curve.
The concentration analyzing apparatus according to the present invention can be used alone, but it can be used particularly as a concentration analyzing apparatus that can be installed in addition to a process apparatus using a chemical solution. The concentration apparatus of the present invention may further include means for directly transferring the chemical solution from the processing apparatus.
2, when the mixed solution is transferred from the
2, the
The
The front portion of the
The
The
RGB color sensor To calculate the concentration of the measurement target component in the sample using the measurement values I (R), I (G), and I (B) but to correspond to the change in value due to the deterioration of the light source and other parts In the present invention, measured values of I (R), I (G) and I (B) (hereinafter referred to as I (R0), I (G0) and I (B0) I (R), I (Gx), and I (Bx) values of the developed samples were measured and the values of R ', G ', And B', respectively.
[Equation]
When the absorbance value of the measurement target material is measured using such a method, the measured values of I (R0), I (G0), and I (B0) (Rx), I (Gx) and I (Bx) values of the R, B 'and G' values of the light source can be obtained. Accordingly, the concentration measurement error due to the change in the condition of the light source does not occur, and more accurate concentration measurement can be performed.
The apparatus for analyzing a chemical solution concentration of the present invention may include a cleaning function including a cleaning agent for cleaning the mixing section and the measurement unit. The mixed liquid in which the measurement is completed in the measuring
As shown in FIG. 1, the process chemicals are subjected to the process while being accommodated in the
The
Herein, the
On the other hand, the quantitative sampling means and the feeding and feeding means applied to the
The
In the mixing
The mixed liquid of the mixing
Valves can use all valves operated by electrical signals or air pressure, such as solenoid valves, electrically operated valves. The control of the valve can be configured to be operable on the user's operating unit.
Based on the I (R), I (G), and I (B) values received from the
Another aspect of the present invention relates to a method for analyzing the concentration of a chemical solution. According to the method of the present invention, RGB color sensor measurement values I (R0), I (G0) and I (B0) of deionized water are first measured, and then an additive solution (Rx), I (Gx) and I (Bx) of the RGB color sensor are measured. Next, the RGB color sensor measurement values R ', G' and B 'of the sample whose concentration is corrected for the deionized water color are calculated using the following equation.
[Equation]
G ', and B' values measured using an RGB color sensor for a sample of known concentration, corrected for deionized water color, to calculate the relationship of the color change according to the concentration change of the sample, do. (Rx), I (Gx), and I (Bx) of an unknown object to be measured in the sample are measured in numerical values by selecting one of R ', G' Is compared with the reference data on the calibration line, and the concentration value corresponding to the reference data is calculated as the concentration of the measurement target substance. When the intensity of the measurement target substance in the chemical solution is measured by the color sensor, these measured values can be converted into numerical values and the concentration can be calculated in comparison with the reference data. The data derived by the chemical solution with known deionized water and concentration can be made into linear data in the form of a linear function. Here, the calibration curve can select the largest value of the slope of the RGB as the calibration curve.
In the method of the present invention, deionized water is put into the measuring unit, and the measured value of the RGB color sensor of the color developed sample, which is known by the measured value and concentration, is measured and corrected by the equation, It is possible to obtain a constant value of R ', G', and B 'even when the change occurs. Thus, concentration measurement error due to the change in the condition of the light source does not occur, and the concentration can be measured more accurately.
Hereinafter, the present invention will be described in more detail with reference to examples. However, these examples are for illustrative purposes only, and the present invention is not limited to the following examples.
Example 1. Phosphoric acid concentration measurement
Phosphoric acid concentrations in process chemicals containing phosphoric acid were measured using the method and apparatus of the present invention. First, the deionized water in the storage part is transferred to the mixing part in the transfer part, and then transferred to the measuring unit to measure and drain the deionized water I (R0), I (G0), I (B0). I (R0), I (G0), and I (B0) of the measured deionized water are sent to the control unit. Again, the transfer section transfers the process chemicals from the circulation piping and the additive solution from the storage section to the mixing section. Where the additive solution is deionized water, ascorbic acid, molybdic acid, deionized water is transferred in an amount that dilutes the process drug 1500 times, and ascorbic acid and molybdic acid are delivered in a ratio of 1: 5. A syringe pump was used to transfer the drug. In the mixing part, the process chemicals and the additive solution are mixed and developed for 10 minutes. At this time, air is injected to generate bubbles, thereby achieving sufficient mixing. After this process, the phosphoric acid-containing solution develops blue color, and the mixed solution that has undergone color development is transferred to the measurement unit, and the values of I (Rx), I (Gx) and I (Bx) are measured and transmitted to the control unit. The control unit calculates the values of R ', B' and G 'from I (R0), I (G0) and I (B0) and I (Rx) .
[Equation 1]
In Table 1 and FIG. 3, R 'and G', depending on the concentration of phosphoric acid. B 'values were calculated. As shown in FIG. 3, R ', G'. B 'value linearly increased with the concentration of phosphoric acid, and linear data of one - dimensional function form was obtained.
In this embodiment, the R 'value having the largest slope was used for analyzing the phosphoric acid concentration of the unknown sample. From the analysis of the sample with known concentration, the calibration curve consisted of linear data in the form of a linear function expressed as the concentration of phosphoric acid (g / L) = 156.84816 * R'-0.06428. In the above equation, Y 'may be defined as a standard conversion value, and x' may be defined as a density value corresponding to the standard conversion value. From the thus obtained basic data, the R 'value of an unknown concentration sample was measured to obtain a phosphoric acid concentration calculation result. Pearson 's coefficient of linearity was 0.99982.
Example 2. Measurement of copper concentration in an aqueous solution containing copper
The copper concentration of the microetching solution containing copper ions was measured using the method and apparatus of the present invention. First, the deionized water in the storage section is transferred to the mixing section and then transferred to the measurement unit to measure and drain the RGB color sensor measurement values I (R0), I (G0) and I (B0) of the deionized water. The values of R (0), I (G0) and I (B0) and I (Rx), I (Gx) and I (Bx) are transmitted to the controller. The transfer part again transfers the process chemicals from the circulation pipe to the mixing part. No dilution was used, and a syringe pump was used for the transfer. The process chemicals in the mixing section are transferred to the measurement unit again, and the measurement unit measures the I (Rx), I (Gx) and I (Bx) RGB values and transmits them to the control section. B ', and G' by Equation 1 using the values of I (R0), I (G0) and I (B0) and I (Rx), I (Gx) Calculate the value.
Table 1 and FIG. 3 show the results of measuring R ', B' and G 'values according to the copper concentration. It was confirmed that R ', B', and G 'values change very linearly according to the copper concentration. For the measurement of the unknown concentration, the R' value, which has the greatest slope, Respectively.
Example 3. Measurement of Iron Concentration
The iron ion concentration of a ferric chloride etching solution containing iron ions (Fe 3 + ) was measured using the method and apparatus of the present invention. First, the deionized water in the storage section is transferred to the mixing section and then transferred to the measurement unit to measure and drain the RGB color sensor measurement values I (R0), I (G0) and I (B0) of the deionized water. The measured RGB color sensor values I (R0), I (G0) and I (B0) of the deionized water are sent to the control unit. Again, the transfer section transfers the process chemicals from the circulation piping and the additive solution from the storage section to the mixing section. Where the additive solution is deionized water and an amount that dilutes the process drug by 1000 times is transferred. The process chemicals and deionized water are mixed and diluted in the mixing section, and the diluted solution is transferred to the measuring unit to measure the values and I (Rx), I (Gx) and I (Bx) values. The measured values and I (Rx), I (Gx), and I (Bx) values are transmitted to the control unit. The control unit calculates R ', B' and G 'values using the values I (R0), I (G0) and I (B0) and I (Rx), I (Gx) and I .
In Table 1 and FIG. 3, R ', B' and G 'values were calculated according to the iron ion concentration. The values of R ', B' and G 'were linearly dependent on the iron ion concentration and the G' value with the highest slope was used to analyze the iron concentration of the unknown solution.
According to the method and apparatus of the present invention, deionized water is introduced into a measuring unit and I (Rx), I (Gx) and I (Bx) ) And I (Bx) are measured together, so that contamination of the light emitting unit and the light receiving sensor unit in the measuring unit, change in light amount, change in current and voltage, and change It is possible to accurately measure and analyze the concentration without any error in the concentration measurement.
The embodiments of the present invention described above are merely illustrative of the technical idea of the present invention, and the scope of protection of the present invention should be interpreted according to the claims. It will be apparent to those skilled in the art that various modifications and variations can be made in the present invention without departing from the spirit and scope of the invention as defined by the appended claims. It should be interpreted that it is included in the scope of right.
100: solution storage tank 200:
300: control unit 400:
500: storage part 600: mixing part
700: measuring unit 710: housing
720: RGB color sensor 730:
740: Analysis vessel 750: Light emitting diode
760: Converter
Claims (12)
The measurement unit includes an RGB color sensor for measuring the concentration of the sample, measures the RGB color sensor measurement value of the RGB color sensor measurement value of the deionized water and the concentration of the RGB color sensor measurement value of the sample, (Rx), I (Gx) and I (B0) of the deionized water and the RGB color sensor measurement values I (Rx), I Bx) is calculated and the corrected R ', G' and B 'values are calculated for the deionized water color with respect to the known concentration of the component to be measured by the following equation, (Rx), I (Gx), and I (Bx) of an unknown object to be measured in the sample are converted into numerical values, In contrast to the reference data on the calibration line, And the concentration of the substance is calculated by the concentration of the substance.
[Equation]
Measuring RGB color sensor measurement values I (Rx), I (Gx), and I (Bx) by adding and coloring an additive solution containing a coloring reagent to a plurality of samples having known concentrations;
Calculating RGB color sensor measurement values R ', G', B 'of a sample whose concentration is corrected for deionized water color using the following equation:
[Equation]
G ', and B' values measured using an RGB color sensor for a sample of known concentration, corrected for deionized water color, to calculate the relationship of the color change according to the concentration change of the sample, ;
Selecting a value having the largest slope as a calibration curve among R ', G', and B 'linear data; And
A value obtained by converting the RGB color sensor measurement values I (Rx), I (Gx), and I (Bx) of the unknown measurement object in the sample into numerical values is compared with the reference data on the calibration line, To the concentration of the substance to be measured.
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| KR1020160060239A KR101903013B1 (en) | 2016-05-17 | 2016-05-17 | Apparatus and method for measuring concentration of chemical solutions |
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| CN111610156A (en) * | 2020-06-05 | 2020-09-01 | 舟山欧莱克新材料科技有限公司 | Red-based KD synthesis decoloration reaction concentration monitoring device and operation method thereof |
| KR102343187B1 (en) * | 2020-09-08 | 2021-12-27 | 주식회사농심 | system of measuring oil acid value using artificial intelligence and the method thereof |
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| JPH11258048A (en) * | 1998-03-09 | 1999-09-24 | Shinko Electric Co Ltd | Coloring degree measuring method for solution |
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