KR20240036813A - Apparatus for measuring aging of measuring film of XRF analyzer - Google Patents

Abstract

The present invention is a device for monitoring the aging of a measurement film provided for the transmission of X-rays to a flow cell through which a sample passes in an XRF analyzer, comprising: a valve control unit that selectively supplies either a sample or pure water to the flow cell; a camera that acquires an image of the measurement film as a first measurement image while pure water is supplied to the flow cell by the valve control unit; a measurement image storage unit that stores the first measurement image obtained from the camera; a reference image storage unit that stores a first reference image that serves as a standard for monitoring aging of the measurement film; an image comparison unit that compares the first measurement image stored in the measurement image storage unit with the first reference image stored in the reference image storage unit; a determination unit that determines aging of the measurement film by comparing the first measurement image and the first reference image by the image comparison unit; and an output unit that outputs the results of the determination unit to the outside. It relates to a measurement film aging monitoring device of an XRF analyzer. According to the present invention, it is possible to easily check the replacement period for the measuring film of the XRF analyzer, thereby reducing the manpower and time required for maintenance and management of the By reading the surface of the film, sample inflow defects such as sample blockage, sample pump failure, and reduced transport ability are detected, which has the effect of preventing inaccurate analysis results in advance.

Description

XRF analyzer measuring film aging monitoring device {Apparatus for measuring aging of measuring film of XRF analyzer}

The present invention relates to an aging monitoring device for the measurement film of an It relates to a device for monitoring the aging of the measuring film of an analyzer.

Generally, XRF (X-Ray Fluorescence) analyzer is used for qualitative and quantitative analysis of organic and inorganic elements using Non-destructive analysis can be performed.

Figure 1 is a configuration diagram showing an XRF analyzer according to conventional technology.

Referring to Figure 1, in a conventional XRF analyzer, a measuring film (2) is provided to expose the sample to the side of the flow cell (1) through which the sample passes, and an X-ray tube (4) is supplied from the high voltage supply unit (3). When a high voltage is applied to the sample, the supplied high voltage is irradiated to the sample in the flow cell (1) through the collimator and filter (5) and the measurement film (2) through the X-ray tube (4). The detector 6 detects the intensity of the fluorescent (secondary) X-rays generated by the reaction, and the intensity of the The concentration of metal ions is displayed on the display unit 9 under the control of the display controller 8. Here, the measuring film 2 serves to transmit X-rays while isolating the sample from the outside because the XRF analyzer must continuously flow the sample and irradiate the sample with X-rays.

Such conventional It is widely used in the water quality field. In particular, due to these advantages, XRF analyzers are operated unmanned and continuously 24 hours a day at various industrial sites.

The measurement film used in a conventional XRF analyzer cannot be used permanently, and its replacement cycle must be determined by a certain period of time or empirically, and this period is bound to be flexible depending on the condition of the sample. This inevitably reduces the meaning of the unmanned automatic process system. The reason is that in order to replace the measuring film, you must visit the installation location of the do.

In this way, although the process XRF analyzer operates unmanned, enabling efficient operation of manpower and time, the continuous monitoring of the measurement film eliminates the advantages of such unmanned operation. In addition, because there is no way to check the smooth transfer of the sample, an unmanned XRF analyzer causes the inconvenience of having to periodically replace the measuring film and check the smooth transfer of the sample. At this time, since the exact replacement cycle of the measurement film is not known, it is usually replaced without reason at a certain interval of 1 to 20 days. This is because the replacement of the measuring film is not simply proportional to the usage time of the There was also the problem of having to spend a considerable amount of time.

Korean Patent Publication No. 10-2022-0116471, XRF system and method for identifying samples (published on August 23, 2022)

In order to solve the problems of the prior art as described above, the present invention makes it easy to check the replacement time for the measurement film of the XRF analyzer, thereby reducing the manpower and time required for maintenance and management of the XRF analyzer. This improves the efficiency of equipment operation, and post-verification of results is possible with the sample inflow judgment algorithm, which allows selection of defective results, contributing to improving the accuracy of the The purpose is to prevent inaccurate analysis results in advance by detecting sample inflow defects such as pump failure and reduced transport capacity.

Other objects of the present invention may be easily understood through the description of the examples below.

In order to achieve the above-described object, according to one aspect of the present invention, there is provided a device for monitoring the aging of a measurement film provided for the transmission of X-rays to a flow cell through which a sample passes in an XRF analyzer, the flow cell A valve control unit that selectively supplies either a sample or pure water; a camera that acquires an image of the measurement film while pure water is supplied to the flow cell by the valve control unit; a measurement image storage unit that stores the image acquired from the camera as a first measurement image; a reference image storage unit that stores a first reference image that serves as a standard for monitoring aging of the measurement film; an image comparison unit that compares the first measurement image stored in the measurement image storage unit with the first reference image stored in the reference image storage unit; a determination unit that determines aging of the measurement film by comparing the first measurement image and the first reference image by the image comparison unit; and an output unit that outputs the results of the determination unit to the outside. An apparatus for monitoring the aging of a measurement film of an XRF analyzer is provided.

The measurement image storage unit stores an image of the measurement film acquired by the camera while the sample is supplied to the flow cell by the valve control unit as a second measurement image, and the reference image storage unit stores the measurement image. A second reference image that serves as a standard for sample transfer to the film is stored, and the image comparison unit compares the second measurement image stored in the measurement image storage unit with the second reference image stored in the reference image storage unit. The determination unit may determine whether the sample transport within the flow cell is defective by comparing the second measurement image and the second reference image by the image comparison unit.

The first reference image is an image obtained by shooting a normal measurement film in advance and editing the surface of the measurement film using an image editing program while increasing the wrinkle ratio to the first set ratio of the total area. Produced as an image for the wrinkle standard, the wrinkle area compared to the total area captured is set to the resolution of the second setting ratio up to the first setting ratio, so that it can be quantified when judging wrinkles, and a normal measurement film is photographed in advance. Using an image editing program, the surface of the measurement film in the acquired image was used to produce multiple edited images while increasing the color density of the discolored part to the third set ratio, and the discolored part captured as an image for the discoloration standard was used. By setting the color density to the resolution of the fourth setting ratio up to the third setting ratio, it can be quantified when judging discoloration.

In the comparison of the first reference image and the first measurement image, the determination unit resolves the first setting ratio to a second setting ratio and resolves the wrinkles determined by comparison and the third setting ratio to a fourth setting ratio. By adding up the values for discoloration determined by comparison, the aging of the measurement film can be quantified.

The first reference image consists of an image obtained by shooting a plurality of new measurement films in the process of performing sample analysis, and the replacement time of the measurement films is set as the end point, and the transformation process before the end point is set as the fifth. The ratio is set to the resolution of the sixth set ratio, so that the judgment unit can quantify it when judging aging, and the process of performing the sample analysis is performed under the same conditions as the actual sample analysis conditions by inserting a rest time and a washing time. You can acquire images.

The second reference image is the image of the measurement film edited to black using an image editing program while the sample is normally supplied and inputted at the fifth setting ratio, and the difference between the film boundaries is adjusted from the fifth setting ratio to the sixth setting ratio. By inputting and storing the ratio, the degree to which the sample has not flowed is indicated by black and the border, so that when the determination unit compares with the second measurement image, the ratio is less than or equal to the ratio set from the fifth set ratio to the sixth set ratio. It can be judged that the sample inflow is defective.

The second reference image consists of images obtained for each of the measurement films by artificially generating a sample inflow defect state step by step, and when the determination unit compares the second measurement image, the matched step image is quantified. You can do it.

According to the measuring film aging monitoring device of the XRF analyzer according to the present invention, it is possible to easily check the replacement time for the measuring film of the XRF analyzer, thereby reducing the manpower and time required for maintenance and management of the The efficiency of equipment operation can be increased, and post-verification of results is possible with the sample inflow judgment algorithm, which can filter out defective results, contributing to improving the accuracy of the , it has the effect of detecting sample inflow defects such as sample pump failure and reduced transport capacity, and preventing inaccurate analysis results in advance.

Figure 1 is a configuration diagram showing an XRF analysis device according to conventional technology.
Figure 2 is a configuration diagram showing a measurement film aging monitoring device of an XRF analyzer according to the present invention.

Since the present invention can be subject to various changes and can have various embodiments, specific embodiments will be illustrated in the drawings and described in detail. However, this is not intended to limit the present invention to specific embodiments, but should be understood to include all changes, equivalents, and substitutes included in the technical idea and scope of the present invention, and may be modified into various other forms. The scope of the present invention is not limited to the following examples.

Hereinafter, embodiments according to the present invention will be described in detail with reference to the attached drawings, and identical or corresponding components will be assigned the same reference numerals regardless of reference numerals, and redundant description thereof will be omitted.

Figure 2 is a configuration diagram showing a measurement film aging monitoring device of an XRF analyzer according to the present invention.

Referring to FIG. 2, the measuring film aging monitoring device 100 of an XRF analyzer according to an embodiment of the present invention includes a measuring film 11 provided for the transmission of ) as a device for monitoring aging, comprising a valve control unit 110, a camera 120, a measurement image storage unit 130, a reference image storage unit 140, an image comparison unit 150, a judgment unit 160, and It may include an output unit 170.

The valve control unit 110 selectively supplies either a sample or pure water to the flow cell 10. For example, in order to monitor the surface aging of the measurement film 11, which is provided to expose the sample to the flow cell 10, Open the pure water valve 111 to allow pure water to pass through the flow cell 10. To monitor whether the sample inflow is normal, block the pure water valve 111 and then open the sample valve 112 to allow the sample to flow. Let it pass through the cell (10).

The camera 120 acquires an image of the measurement film 11 while pure water is supplied to the flow cell 10 by the valve control unit 110. This camera 120 may be used for monitoring in an

The measured image storage unit 130 stores the image acquired from the camera 120 as the first measured image. At this time, the measurement image storage unit 130 may compress and store the first measurement image. The measurement image storage unit 130 stores the image of the measurement film 11 acquired by the camera 120 as a second measurement image while the sample is supplied to the flow cell 10 by the valve control unit 110. You can.

The reference image storage unit 140 stores a first reference image that serves as a standard for monitoring aging of the measurement film 11. Additionally, the reference image storage unit 140 may store a second reference image that serves as a standard for sample transfer to the measurement film 11.

For example, the first reference image is an image obtained by pre-photographing a normal measurement film 11, and the surface of the measurement film 11 is edited using an image editing program while increasing the wrinkle ratio up to the first set ratio of the total area. Produce a large number of images for the wrinkle standard, and set the wrinkle area compared to the total area captured as the image for the wrinkle standard at the resolution of the second setting ratio up to the first setting ratio, so that it can be quantified when judging wrinkles, and it is a normal measurement film. From the image obtained by shooting (11) in advance, use an image editing program to change the surface of the measurement film (11) to produce a number of edited images while increasing the color density of the discolored portion to the third set ratio. The color density of the discolored part captured as an image for is set to the resolution of the fourth setting ratio up to the third setting ratio, so that it can be quantified when judging the discoloration. For example, the first reference image uses an image editing program, for example, Photoshop, to embody the typical symptoms of wrinkles occurring when the measurement film 11 ages and discoloration by a colored sample, which is a normal measurement film 11. After filming, use an image editing program such as Photoshop on the surface of the measurement film (11) on a PC to produce an edited image while increasing the wrinkle ratio to 10 to 90% of the total area, and capture it to measure the wrinkles compared to the total area. Compare the area and quantify it from 10 to 90% at 5% resolution. Here, the numerical value may be, for example, a ratio of increase or decrease in 5% units of the wrinkle area compared to the area, or it may be a value converted to an arbitrary range of this ratio. In addition, in the first reference image, the discoloration part is measured using pure water, and then the color contaminated by the sample on the background color is arbitrarily reproduced using an image editing program such as Photoshop, and the color density is adjusted in 5% increments from 10 to 90%. It can be quantified. Here, the value may be, for example, an increase/decrease ratio of the color density in units of 5%, or it may be a value converted to an arbitrary range. When applied in practice, the determination unit 160, which will be described later, can determine the aging of the measurement film 11 by adding the above two variables to a certain value.

In addition, as another example, the first reference image consists of an image obtained by shooting a number of new measurement films 11 in the process of performing sample analysis, and the replacement point of the measurement films 11 is set as the end point, and the end point is set as the end point. Previously, the transformation process was performed at a resolution of the sixth setting ratio up to the fifth setting ratio, so that the judgment unit 16 could quantify it when judging aging, and the process of performing sample analysis included a pause time and a washing time. This allows images to be acquired under the same conditions as the actual sample analysis conditions. That is, in this embodiment, the first reference image is used by directly shooting the actually contaminated measurement film 11 (see FIG. 3). In cases where it is difficult to implement the actual phenomenon with software, the measurement film 11 in the direct sample analysis process is used. ) as a method of filming and recording the aging process while measuring the measuring film (11), while analyzing the actual sample after replacing the new measuring film (11), filming and recording the aging process of the measuring film (11), and then recording the aging process of the measuring film (11). The replacement point can be set as the end point and the transformation process can be quantified, for example, from 10 to 90% with a resolution of 5%. At this time, the sample should not be measured continuously, and images should be acquired and stored under conditions similar to actual conditions by inserting pauses, washing times, etc. during sample measurement. This is because the degree of contamination for each sample is affected by many variables, such as the number of times the analysis was performed, the time the analysis was stopped, and the degree of cleaning.

The second reference image is, for example, in a state where the sample is normally supplied, the image of the measurement film 11 is edited to black using an image editing program and inputted at the fifth setting ratio, and the film boundary difference is calculated from the fifth setting ratio. By entering and storing up to 6 set ratios, the degree to which the sample has not flowed is indicated by black and the border, so that when comparing with the second measurement image, the determination unit 160 determines the ratio from the 5th set ratio to the 6th set ratio. If the ratio is below, it can be judged as a sample inflow defect. This second reference image is produced using an image editing program. If the sample does not flow into the flow cell 10, it appears in black on the camera 120, or a boundary surface appears depending on the water level (see FIG. 4). ). Therefore, the second reference image is input at 10% by adding black parts to the image of the measurement film 11, into which the sample normally flows, using an image editing program such as Photoshop, and is adjusted to 10 to 90% depending on the difference in the boundary of the measurement film 11. After entering and saving the information, it can be compared and used during actual measurement. At this time, the determination unit 160 may determine that the sample inflow is defective when 50% or less occurs.

As another example, the second reference image may be composed of images obtained for each measurement film 11 by artificially generating a sample inflow defect state step by step, and when the judgment unit 160 compares it with the second measurement image, The matching step-by-step images can be quantified. The second reference image according to this other example is to be used by directly filming the actual sample inflow defect state, and the actual sample inflow defect state can be artificially generated and quantified after measuring the measurement film 11 step by step. there is. Here, the number may be the ratio of the step being located within the minimum and maximum values.

The image comparison unit 150 compares the first measurement image stored in the measurement image storage unit 130 with the first reference image stored in the reference image storage unit 140, thereby determining the degree of aging of the measurement film 11. Allows matching. Additionally, the image comparison unit 150 may compare the second measurement image stored in the measurement image storage unit 130 with the second reference image stored in the reference image storage unit 140, thereby allowing the measurement film 11 to be compared. This allows the movement of the sample to be confirmed.

The determination unit 160 determines the aging of the measurement film 11 by comparing the first measurement image and the first reference image by the image comparison unit 150. The determination unit 160 may be configured to logically compare the first measurement image and the first reference image and use the results to numerically calculate the lifespan of the measurement film 11 and the normal and abnormal state of sample inflow. As an example, the normal state of the measurement film 11 is photographed and saved as a reference image, and as described above, this reference image is distorted with an image editing program to create various deformed states, and then the saved image is used, or the normal state is used. It is possible to make several measurement films (11) of the contamination state and to demonstrate them, and then save them individually to use them as a reading standard.

The determination unit 160 may determine whether the sample transfer within the flow cell 10 is defective by comparing the second measurement image and the second reference image by the image comparison unit 150.

In the comparison of the first reference image and the first measurement image, the determination unit 160 resolves the first setting ratio at the second setting ratio, and resolves the value of the wrinkles determined by comparison at the fourth setting ratio up to the third setting ratio. By adding up the comparatively determined discoloration values, the aging of the measurement film 11 can be quantified. Accordingly, when the numerical result is higher than the reference value set by the user, replacement of the measuring film 11 is notified. Of course, this can be similarly applied when determining a defect in sample inflow.

The output unit 170 outputs the results of the determination unit 160 to the outside. The results calculated in numbers by the judgment algorithm can be directly monitored through a monitor or transmitted to a separate operating PC for record management. You can do it. For example, the output unit 170 can display the contamination level of the measurement film 11 as a numerical value such as 75% to an external device, and in the case of sample inflow, it can display it as normal or abnormal.

The operation of the measurement film aging monitoring device of the XRF analyzer according to the present invention will be described by way of example.

First, in order to monitor the aging of the measurement film, the camera 120 can acquire images using a CCD camera in operation for monitoring the flow cell 10, etc., and a number of contaminated measurement films 11 are removed before proceeding. The process of arbitrarily manufacturing the image and storing it in the reference image storage unit 140 as the first reference image is performed.

Then, to start the comparison, the sample valve 112 through which the sample is being introduced is blocked by the valve control unit 110 and the pure water valve 111 is opened. Then, the images acquired for the measurement film 11 through the camera 120 are stored in seconds in the measurement image storage unit 130, and the 10 most recent images are captured for comparison from these images and used as the first standard. After noise removal and color and contrast correction are performed in the same way as the image, the file name is named and saved as the first measurement image. The image comparison unit 150 uses an image processing algorithm or an image comparison algorithm to select a first reference image that has the greatest similarity to the first measurement image in terms of wrinkles, contrast ratio, foreign matter counter, etc. of the measurement film 11. Extract and make a decision as a numerical value for the ratio of the first reference image extracted by the judgment unit 160, or determine the difference as a numerical value using a judgment algorithm that recalculates the coincidence rate with the extracted first reference image. You can get off. The output unit 170 can display the decision result of the determination unit 160 through the display unit of the PC or store it in the memory unit, and output an alarm sound by the alarm unit 180 when a predetermined value is satisfied. It may be configured to flash an alarm light.

In addition, in order to determine the smooth transfer of the sample through the flow cell 10, the camera 120 can acquire images using a CCD camera in operation for monitoring the flow cell 10, etc., and the sample is transferred before proceeding. A plurality of measurement films (11) in a state in which light is normally introduced are arbitrarily manufactured and stored in the reference image storage unit (140) as a second reference image.

And, at the start of the comparison, the sample is already supplied to the flow cell 10 by the valve control unit 110 with the sample valve 112 opened. Then, the images acquired for the measurement film 11 through the camera 120 are stored in seconds in the measurement image storage unit 130, and the 10 most recent images are captured for comparison from these images and used as a second standard. After noise removal and color and contrast correction are performed in the same way as the image, the file name is named and saved as the second measurement image. The image comparison unit 150 uses an image processing algorithm or an image comparison algorithm to recognize the two-tone ratio and boundary occurrence height in the measurement film 11 with respect to the second measurement image and extract a second reference image with the greatest similarity. And, the determination unit 160 determines whether the difference ratio of the boundary surface from the second reference image is 50% or less. The output unit 170 can display the decision result of the determination unit 160 through the display unit of the PC or store it in the memory unit, and is configured to output an alarm sound or flash an alarm light by the alarm unit 180. It can be.

According to the measuring film aging monitoring device of the XRF analyzer according to the present invention, it is possible to easily check the replacement period for the measuring film of the XRF analyzer, thereby reducing the manpower and time required for maintenance and management of the By doing this, the efficiency of equipment operation can be increased, and the sample inflow judgment algorithm allows post-verification of results, allowing defective results to be selected, contributing to improving the accuracy of the XRF analyzer.

In addition, according to the present invention, sample inflow defects such as sample blockage, sample pump failure, and reduced transport capacity can be detected through reading the surface of the measurement film, and inaccurate analysis results can be prevented in advance.

Although the present invention has been described with reference to the accompanying drawings, it goes without saying that various modifications and variations can be made without departing from the technical spirit of the present invention. Therefore, the scope of the present invention should not be limited to the described embodiments, but should be determined by the claims described below as well as equivalents to these claims.

10: Flow cell 11: Measurement film
110: valve control unit 111: pure water valve
112: sample valve 120: camera
130: measurement image storage unit 140: reference image storage unit
150: Image comparison unit 160: Judgment unit
170: output unit 180: alarm unit

Claims (6)

It is a device that monitors the aging of the measurement film provided for the transmission of X-rays to the flow cell through which the sample passes in the XRF analyzer,
a valve control unit that selectively supplies either a sample or pure water to the flow cell;
a camera that acquires an image of the measurement film while pure water is supplied to the flow cell by the valve control unit;
a measurement image storage unit that stores the image acquired from the camera as a first measurement image;
a reference image storage unit that stores a first reference image that serves as a standard for monitoring aging of the measurement film;
an image comparison unit that compares the first measurement image stored in the measurement image storage unit with the first reference image stored in the reference image storage unit;
a determination unit that determines aging of the measurement film by comparing the first measurement image and the first reference image by the image comparison unit; and
an output unit that outputs the results of the determination unit to the outside;
Including, a measuring film aging monitoring device of an XRF analyzer. In claim 1,
The measured image storage unit,
Saving the image of the measurement film acquired by the camera while the sample is supplied to the flow cell by the valve control unit as a second measurement image,
The reference image storage unit,
Storing a second reference image that serves as a standard for sample transfer to the measurement film,
The video comparison section,
Compare the second measurement image stored in the measurement image storage unit with the second reference image stored in the reference image storage unit,
The judgment department,
A measurement film aging monitoring device of an XRF analyzer that determines whether the sample transfer within the flow cell is defective by comparing the second measurement image and the second reference image by the image comparison unit. In claim 1 or claim 2,
The first reference image is,
Using an image editing program, the surface of the measurement film is obtained from an image obtained by shooting a normal measurement film in advance, and a plurality of edited images are produced while increasing the wrinkle ratio up to the first set ratio of the total area, using a wrinkle standard for wrinkles. The wrinkle area compared to the total area captured as an image is set to the resolution of the second setting ratio up to the first setting ratio, so that wrinkles can be quantified when judging,
From the image obtained by shooting a normal measurement film in advance, use an image editing program on the surface of the measurement film to produce a number of edited images while increasing the color density of the discolored portion up to the third set ratio, using a discoloration standard for the discoloration standard. A measuring film aging monitoring device for an
The judgment department,
In the comparison of the first reference image and the first measurement image, the value for wrinkles determined by comparison by resolving at a second setting ratio up to the first setting ratio and the value for wrinkles determined by comparing and determining by resolving at a fourth setting ratio up to the third setting ratio A measurement film aging monitoring device of an XRF analyzer that adds up the values for discoloration and quantifies the aging of the measurement film. In claim 1 or claim 2,
The first reference image is,
In the process of performing sample analysis, it consists of an image obtained by shooting a large number of new measurement films, and the replacement point of the measurement film is set as the end point, and the transformation process before the end point is continued up to the 5th set ratio and the 6th set ratio. XRF, which allows the determination unit to quantify aging when judging aging, and allows the sample analysis process to acquire the image under the same conditions as the actual sample analysis conditions by inserting rest time and washing time. Analyzer's measurement film aging monitoring device. In claim 2,
The second reference image is,
In a state where the sample is normally supplied, the image of the measurement film is edited to black using an image editing program and inputted at the fifth setting ratio, and the film boundary difference is input and stored from the fifth setting ratio to the sixth setting ratio, The extent to which the sample has not flowed is indicated by a black border, so that when comparing with the second measurement image, the determination unit determines that the sample inflow is defective when the ratio is less than the ratio set from the fifth set ratio to the sixth set ratio. A device that monitors the aging of the measuring film of an XRF analyzer. In claim 2,
The second reference image is,
Measurement of an Film aging monitoring device.