Method for measuring the dissolution rate of deposits by cleaning agents

Abstract

The present application discloses a method for measuring the dissolution rate of sediment by a cleaning agent. Specifically, a sediment sample of a first preset mass and a cleaning agent solution of a first preset volume are mixed, so that the sediment and the cleaning agent solution undergo a dissolution reaction under preset cleaning conditions to obtain a dissolved mixture; supernatants of different reaction times are extracted from the dissolved mixture; the maximum concentration value of each target element in each supernatant and the target extraction time corresponding to the maximum concentration value are determined; the dissolution rate of the sediment by the cleaning agent solution is calculated based on the first preset volume, the maximum concentration value corresponding to each target element, the target extraction time corresponding to each target element, and the mass relationship coefficient between each target element and the phase composition. By measuring the peak concentration of the target element and the time point when the peak is reached, the dissolution rate of the cleaning agent solution is calculated, which helps to select the most effective cleaning agent to meet actual needs.

Description

Technical Field

[0001] The present application relates to the field of cleaning technology, and in particular to a method for measuring the dissolution rate of a cleaning agent on sediments. Background Art

[0002] Currently, cleaning agents are often selected based on their performance data. However, this approach doesn't guarantee the suitability of the selected cleaning agents for the steam generator secondary side deposit samples being cleaned, and thus, their effectiveness in actual applications. Summary of the Invention

[0003] In view of this, the present application provides a method for measuring the dissolution rate of deposits by a cleaning agent. The main purpose is to solve the technical problem that the existing method of selecting cleaning agents based on their product performance data cannot ensure the cleaning effect of the cleaning agent solution in actual application.

[0004] According to the first aspect of the present application, a method for measuring the dissolution rate of a cleaning agent on a sediment is provided, the method comprising:

[0005] Obtaining multiple elements contained in the sediment sample to be cleaned, the phase composition corresponding to each element, and the mass content of each phase composition in the sediment sample;

[0006] Sort the multiple mass contents in descending order, add up each mass content in sequence starting from the mass content in the first position, and when the sum of the mass contents reaches a preset threshold, obtain at least one target element corresponding to at least one phase composition contained in the sum of the mass contents;

[0007] Mixing a sediment sample of a first preset mass and a cleaning solution of a first preset volume, so that the sediment and the cleaning solution undergo a dissolution reaction under preset cleaning conditions to obtain a dissolved mixture, wherein the dissolved mixture includes a supernatant and undissolved sediment;

[0008] extracting a plurality of supernatants from the lysis mixture at predetermined time intervals and a second predetermined volume;

[0009] Diluting the plurality of supernatants with a detergent solution according to a preset dilution multiple to obtain a plurality of dissolved solutions;

[0010] Based on the quantitative standard curve of each target element, a preset dilution factor, and multiple dissolution solutions, the maximum concentration value of each target element in each supernatant and the target extraction time corresponding to the maximum concentration value are determined. The quantitative standard curve shows the corresponding relationship between the signal intensity measured by the quantitative instrument and the concentration of the target element;

[0011] The dissolution rate of the deposit by the cleaning solution is calculated according to the first preset volume, the maximum concentration value corresponding to each target element, the target extraction time corresponding to each target element, and the mass relationship coefficient between each target element and the phase composition.

[0012] Optionally, the step of obtaining multiple elements contained in the sediment sample to be cleaned, the phase composition corresponding to each element, and the mass content of each phase composition in the sediment sample specifically includes:

[0013] Obtain sediment samples from the equipment to be cleaned;

[0014] Utilize element quantitative analysis technology to conduct element quantitative analysis on sediment samples and obtain multiple mass contents of multiple elements in sediment samples;

[0015] X-ray diffraction (XRD) was used to analyze the phase of sediment samples and determine the phase composition corresponding to each element.

[0016] Calculate the mass relationship coefficient between each element and its corresponding phase composition;

[0017] The mass content of each element is multiplied by the mass relationship coefficient to obtain the mass content of the phase composition corresponding to each element in the sediment sample.

[0018] Optionally, the step of mixing a sediment sample of a first preset mass and a cleaning solution of a first preset volume, so that the sediment and the cleaning solution undergo a dissolution reaction under preset cleaning conditions to obtain a dissolved mixture, specifically includes:

[0019] Add a first preset volume of cleaning solution into a three-necked flask of preset specifications, and immerse the bottom of the three-necked flask in the silicone oil;

[0020] Heat the silicone oil to obtain the temperature of the cleaning solution in the three-necked flask;

[0021] When the temperature reaches and maintains the preset temperature value of the preset cleaning condition of the cleaning agent, a first preset mass of sediment sample is added to the three-necked flask and stirred, so that the cleaning agent solution dissolves the sediment sample to obtain a dissolved mixture.

[0022] Optionally, the step of extracting a plurality of supernatants from the dissolved mixture according to a preset time interval and a second preset volume specifically includes:

[0023] Determining multiple extraction moments according to preset time intervals;

[0024] When the sediment sample is added to the three-necked flask, the timer is started to obtain the dissolution time;

[0025] When the dissolution time reaches each extraction moment, a second preset volume of supernatant is extracted from the dissolution mixture into a centrifuge tube, and a second preset volume of detergent solution is added into the three-necked flask.

[0026] Optionally, the step of diluting each supernatant with a detergent solution according to a preset dilution multiple to obtain a plurality of dissolved solutions specifically includes:

[0027] According to the preset dilution multiple, a detergent solution is added to each centrifuge tube to dilute the supernatant in each centrifuge tube to obtain a dissolved solution.

[0028] Optionally, the method further includes determining the maximum concentration value of each target element in each supernatant according to a quantitative standard curve of the target element, a preset dilution factor, and a plurality of dissolving solutions, and determining the maximum concentration value before the target extraction time corresponding to the maximum concentration value.

[0029] Obtaining a standard solution of a target element with a first preset concentration;

[0030] diluting the standard solution with a detergent solution to obtain a plurality of diluted solutions with a second preset concentration;

[0031] Measuring a first signal intensity value of each diluted solution using a quantitative detection method;

[0032] A quantitative standard curve of the target element is drawn according to the plurality of second preset concentrations and the plurality of first signal intensity values.

[0033] Optionally, the step of determining the maximum concentration value of each target element in each supernatant and the target extraction time corresponding to the maximum concentration value based on the quantitative standard curve of the target element, a preset dilution factor, and a plurality of dissolution solutions specifically includes:

[0034] Measuring the second signal intensity value of each dissolved solution using a quantitative detection method;

[0035] Determining the first concentration value corresponding to each second signal intensity value according to the quantitative standard curve;

[0036] Multiplying each first concentration value by the preset dilution factor to obtain a second concentration value of the target element in the supernatant;

[0037] Obtain the maximum concentration value of the target element in the supernatant and the target extraction time corresponding to the maximum concentration value.

[0038] Optionally, the method further includes:

[0039] Obtain the relative atomic mass of each element and the molar mass of its corresponding phase composition;

[0040] The mass relationship coefficient between each element and its corresponding phase composition is calculated through molar mass and relative atomic mass.

[0041] Optionally, the step of calculating the dissolution rate of the deposit by the cleaning solution based on the first preset volume, the maximum concentration value corresponding to each target element, the target extraction time corresponding to each target element, and the mass relationship coefficient between each target element and the phase composition specifically includes:

[0042] Multiplying the mass relationship coefficient and the maximum concentration value of each target element by the first preset volume, and dividing the multiplied value by the target extraction time to obtain the dissolution rate of the cleaning solution for the phase composition corresponding to each target element;

[0043] In the case where there are multiple at least one target element, multiple dissolution rates of multiple phase compositions corresponding to the multiple target elements are added together to obtain the dissolution rate of the deposit by the cleaning solution.

[0044] Optionally, the element quantitative analysis technique includes any one of the following: X-ray fluorescence analysis and inductively coupled plasma optical emission spectrometry.

[0045] Based on the above technical solution, this application provides a method for measuring the sediment dissolution rate of a cleaning agent. Specifically, a sediment sample from the secondary side of a steam generator is dissolved using a cleaning agent solution to be evaluated. The supernatant is collected as a measurement sample solution at a preset time interval and a second preset volume. After determining the primary elements and their phase composition in the sediment sample, the concentration changes of the primary elements in the measurement sample solution are monitored. The peak concentration of the target element and the time when the peak is reached are measured. The dissolution rate of the cleaning agent solution is then calculated. This serves as a reference for measuring the cleaning efficiency of the cleaning agent for cleaning sediment. This allows the suitability of the evaluated cleaning agent for real-time application scenarios to be determined, facilitating the selection of the most effective cleaning agent to meet actual needs.

[0046] The above description is only an overview of the technical solution of the present application. In order to more clearly understand the technical means of the present application, it can be implemented in accordance with the contents of the specification. In order to make the above and other purposes, features and advantages of the present application more obvious and easy to understand, the specific implementation methods of the present application are listed below. BRIEF DESCRIPTION OF THE DRAWINGS

[0047] Various other advantages and benefits will become apparent to those skilled in the art upon reading the detailed description of the preferred embodiment below. The accompanying drawings are for illustration purposes only and are not to be considered as limiting the present application. The same reference symbols are used throughout the drawings to represent the same components. In the drawings:

[0048] Figure 1A schematic flow chart of a method for measuring the dissolution rate of a deposit by a cleaning agent provided in an embodiment of the present application is shown;

[0049] Figure 2 A schematic flow chart of another method for measuring the dissolution rate of sediment by a cleaning agent provided in an embodiment of the present application is shown;

[0050] Figure 3 A comparison chart showing the XRD spectrum of the sediment sample provided in the examples of the present application and the standard XRD data of Fe3O4 is shown;

[0051] Figure 4 The figure shows the quantitative standard curve of Fe element provided in the examples of the present application;

[0052] Figure 5 A curve diagram showing the relationship between Fe concentration and extraction time during the cleaning process of the cleaning solution provided in the embodiment of the present application is shown. DETAILED DESCRIPTION

[0053] The following describes exemplary embodiments of the present application in more detail with reference to the accompanying drawings. Although exemplary embodiments of the present application are shown in the accompanying drawings, it should be understood that the present application can be implemented in various forms and should not be limited by the embodiments set forth herein. Rather, these embodiments are provided to enable a more thorough understanding of the present application and to fully convey the scope of the present application to those skilled in the art.

[0054] The present application embodiment provides a method for measuring the dissolution rate of a cleaning agent on a sediment, such as Figure 1 As shown, the method includes:

[0055] S101. Obtain multiple elements contained in a sediment sample to be cleaned, the phase composition corresponding to each element, and the mass content of each phase composition in the sediment sample.

[0056] The method for measuring the dissolution rate of deposits by a cleaning agent provided in the embodiment of the present application is mainly used in the test scenario of the cleaning efficiency of the cleaning agent for cleaning deposits. Among them, the sediment sample to be cleaned can be the sediment extracted from the equipment to be cleaned. In the actual application scenario, the equipment to be cleaned can be the secondary side of the steam generator. During the operation of the reactor, the sediment in the secondary side of the steam generator will affect the heat transfer efficiency of the heat transfer tube, endanger the integrity of the heat transfer tube, and threaten the safe operation of the reactor. Therefore, when the sediment on the secondary side of the steam generator reaches a certain amount (such as 100 g / m 2), cleaning work needs to be carried out. At present, cleaning agents are usually selected based on their product performance data, including cleaning efficiency, dissolution ability, scope of application, etc. However, the deposits on the secondary side of different steam generators contain different materials, and their reactions and tolerances to different cleaning agents are different. The product performance data may not be able to fully and objectively and truly reflect the performance of the cleaning agent under various actual conditions. In order to ensure the effectiveness of the selected cleaning agent in cleaning deposits, this application proposes measuring the dissolution rate of the cleaning agent to measure the cleaning efficiency of the cleaning agent, providing a reference basis for selecting a suitable cleaning agent.

[0057] Specifically, different elements and their compounds in the sediment sample have different solubility and reactivity requirements for different cleaning agents. Analytical methods are used to determine which elements are contained in the sediment sample, and X-ray diffraction technology is used to determine the phase composition corresponding to each element. Subsequently, the mass content of each element in the sediment sample is measured. The relative atomic mass of each element and the molar mass of its corresponding phase composition are obtained. Using the relative atomic mass and molar mass, the mass relationship coefficient between the element and the phase composition is calculated. The mass content of each element is then multiplied by the mass relationship coefficient to obtain the mass content of its corresponding phase composition in the sediment sample.

[0058] S102. Sort the multiple mass contents in descending order, and add up each mass content in sequence starting from the mass content in the first position. When the sum of the mass contents reaches a preset threshold, obtain at least one target element corresponding to at least one phase composition contained in the sum of the mass contents.

[0059] In this step, in order to measure the main elements in the sediment sample, the multiple mass contents of the various phases are sorted in descending order, and starting from the mass content of the first position, each mass content is added in turn to calculate the sum of the mass contents. When the sum of the mass contents reaches a preset threshold, it can be determined that at least one target element in the sum of the mass contents is the main element in the sediment sample.

[0060] Optionally, the preset threshold can be 90%. After calculating the mass contents of multiple phase compositions, the mass contents are added sequentially, starting from the largest mass content. When the sum of the mass contents reaches 90%, the calculation stops. At this point, the one or more phase compositions included in the sum of the mass contents are the main components of the sediment, and the corresponding target element is the main element of the sediment. If the maximum mass content is already greater than 90%, the target element corresponding to this mass content is determined to be the main element in the sediment, and no further summation calculation is required.

[0061] S103 , mixing a sediment sample of a first preset mass and a cleaning solution of a first preset volume, so that the sediment and the cleaning solution undergo a dissolution reaction under preset cleaning conditions to obtain a dissolved mixture, wherein the dissolved mixture includes a supernatant and undissolved sediment.

[0062] In this step, a first preset mass of a sediment sample and a first preset volume of a cleaning solution are weighed, the weighed cleaning solution is added to a three-necked flask, and then the sediment sample is added to the three-necked flask containing the cleaning solution. A dissolution reaction is performed under preset cleaning conditions to obtain a dissolved mixture, wherein the dissolved mixture includes a liquid portion (i.e., a supernatant) produced when the sediment and the cleaning agent are mixed during the cleaning process and the cleaning agent dissolves the metal oxides in the sediment, and an undissolved solid portion (i.e., undissolved sediment).

[0063] Alternatively, based on experience, the sediment sample is accurately weighed. The amount of cleaning solution to be added is then determined based on the sediment sample mass and the solubility of the cleaning solution selected for measurement. In a practical application scenario, if a 5g (first preset mass) sediment sample is selected and the solubility of the cleaning solution to be evaluated is 200ml, which can dissolve 5g of sediment, then the first preset volume of the cleaning solution is determined to be 200ml.

[0064] Furthermore, the preset cleaning conditions refer to presetting the cleaning temperature and stirring speed in the three-necked flask.

[0065] S104 , extracting a plurality of supernatants from the dissolved mixture according to a preset time interval and a second preset volume.

[0066] S105 , diluting the plurality of supernatants with a detergent solution according to a preset dilution multiple to obtain a plurality of dissolved solutions.

[0067] In steps S104 and S105, during the cleaning process, the dissolution of the sediment requires a certain amount of time. When the concentration of the target element in the dissolving solution reaches a peak over time, the cleaning agent exhibits its maximum dissolving power and activity, which means that the cleaning agent has reached its highest efficiency and can effectively dissolve the chemical components indicated by the sediment. In order to measure the dissolution rate of the main elements in the sediment by the cleaning agent, it is necessary to detect the change trend of the concentration of the main elements over time and measure the time point when the concentration peaks. Therefore, during the test process, according to the preset time interval and the second preset volume, supernatants of different reaction times are extracted from the dissolving mixture in turn and placed in centrifuge tubes to measure the concentration of the target element corresponding to different extraction times.

[0068] Furthermore, due to the high number of extractions, the supernatant volume is limited, resulting in a small amount of supernatant sample available at each extraction time. To ensure the accuracy of the measurement results, the extracted supernatant is diluted with a detergent solution according to a preset dilution factor to prepare a dissolving solution. This increases the volume of the extracted dissolving solution and the stability of the measurement, reducing errors introduced by uneven sampling or limited sensitivity of the measuring equipment. It also reduces the amount of reagents used and saves measurement costs.

[0069] Optionally, when monitoring changes in the concentration of the target element, the value ranges of the second preset volume, the preset time interval, and the preset dilution factor can be specifically set according to the experimental design and are not specifically limited here.

[0070] S106. Determine the maximum concentration value of each target element in each supernatant and the target extraction time corresponding to the maximum concentration value based on the quantitative standard curve of each target element, a preset dilution factor, and multiple dissolution solutions, wherein the quantitative standard curve shows the corresponding relationship between the signal intensity measured by the quantitative instrument and the concentration of the target element.

[0071] In this step, the quantitative standard curve provides a quantitative tool that shows the correspondence between signal intensity and concentration. The quantitative standard curve can be used to accurately measure the concentration of the target element contained in different dissolved solutions. After the dissolved solutions are prepared in sequence according to the preset dilution multiples, for any target element, the concentration of the target element in each dissolved solution is measured using the quantitative standard curve. Since the dissolved solution is a diluted solution, in order to obtain the concentration of the target element in the supernatant, it is also necessary to multiply the measured concentration value by the preset dilution multiple to obtain the concentration value of the target element in the supernatant at different extraction time points.

[0072] Furthermore, the peak concentration (i.e., the maximum concentration) is determined from the multiple measured concentration values. This peak concentration reflects the critical point at which the cleaning agent reacts and dissolves with the sediment sample, indicating that the cleaning agent's solubility has reached its limit. Obtaining the target extraction time of the peak concentration indicates the time when the cleaning agent achieves its maximum cleaning effect. This provides quantitative data for calculating the cleaning agent's dissolution rate, which is crucial for evaluating the cleaning agent's efficiency in cleaning sediments.

[0073] S107 , calculating the dissolution rate of the deposit by the cleaning solution according to the first preset volume, the maximum concentration value corresponding to each target element, the target extraction time corresponding to each target element, and the mass relationship coefficient between each target element and the phase composition.

[0074] In this step, for each target element, the mass of dissolved sediment is calculated using the target element concentration at the point where the cleaning solution reaches its solubility limit and the cleaning solution volume. Combined with the peak concentration moment and the proportional relationship between the mass of the phase composition and the mass of the target element, the dissolution rate of the cleaning solution for each phase composition corresponding to the target element is calculated as the primary basis for measuring the cleaning effectiveness of the cleaning solution on the sediment sample. If there are multiple target elements, the dissolution rates for the multiple phase compositions corresponding to the multiple target elements are summed to obtain the cleaning rate of the cleaning solution for the sediment.

[0075] The method for measuring the sediment dissolution rate of a cleaning agent provided in an embodiment of the present application uses a cleaning agent solution to dissolve a sediment sample from the secondary side of a steam generator, preparing a dissolved solution as the measurement sample solution. After determining the primary elements and their phase composition in the sediment sample, the concentration changes of the primary elements in the measurement sample solution are monitored, and the peak concentration of the target element and the time point at which the peak is reached are measured. The dissolution rate of the cleaning agent solution is then calculated, which serves as a reference for measuring the cleaning efficiency of the cleaning agent for cleaning sediment. This allows the suitability of the cleaning agent being evaluated for real-time application scenarios to be determined, facilitating the selection of the most effective cleaning agent to meet actual needs.

[0076] This application further refines and expands the specific implementation of the above embodiment. In order to fully illustrate the specific implementation process of this embodiment, this application embodiment provides another method for measuring the dissolution rate of the sediment by the cleaning agent, such as Figure 2 As shown, the method includes:

[0077] S201. Obtain a sediment sample from the equipment to be cleaned.

[0078] In this step, an appropriate amount of sediment from the equipment to be cleaned is collected to evaluate the cleaning efficiency of the cleaning agent.

[0079] In practical applications, the equipment to be cleaned might be the secondary side of a steam generator. During a nuclear power plant shutdown, high-pressure water jets are used to flush out sediment from the secondary side. The slurry is then collected and dried. A certain amount of sediment is then sampled as the cleaning sample.

[0080] S202. Perform element quantitative analysis on the sediment sample using element quantitative analysis technology to obtain multiple mass contents of multiple elements in the sediment sample.

[0081] S203. Use X-ray diffraction (XRD) technology to perform phase analysis on the sediment sample to determine the phase composition corresponding to each element.

[0082] S204. Calculate the mass relationship coefficient between each element and its corresponding phase composition.

[0083] S205. Multiply the mass content of each element by the mass relationship coefficient to obtain the mass content of the phase composition corresponding to each element in the sediment sample.

[0084] S206. Sort the multiple mass contents in descending order, and add each mass content in sequence starting from the mass content in the first position. When the sum of the mass contents reaches a preset threshold, obtain at least one target element corresponding to at least one phase composition contained in the sum of the mass contents.

[0085] In steps S202 to S206, the content of the constituent elements in the sediment sample is quantitatively analyzed using elemental quantitative analysis technology to obtain multiple mass contents of multiple elements in the sediment sample. Optionally, the elemental quantitative analysis technology can be X-ray fluorescence analysis or inductively coupled plasma optical emission spectrometry.

[0086] Furthermore, X-ray diffraction analysis can identify the various crystalline phases present in the sediment, including oxides, sulfides, salts, and more. By comparing the diffraction pattern of each element with the standard data of various crystalline phases in the database, the phase composition corresponding to each element in the sediment can be accurately determined.

[0087] Furthermore, the relative atomic mass of each element and the molar mass of its corresponding phase composition are obtained, and the mass relationship coefficient between the element and the phase composition is calculated using the relative atomic mass and molar mass. Then, the mass content of each element is multiplied by the mass relationship coefficient to obtain the mass content of its corresponding phase composition in the sediment sample. Thereafter, in order to measure the main elements in the sediment sample, the multiple mass contents of the various phase compositions are sorted in descending order, starting from the mass content of the first position, each mass content is added in sequence, and the sum of the mass contents is calculated. When the sum of the mass contents reaches a preset threshold, it can be determined that at least one target element in the sum of the mass contents is the main element in the sediment sample.

[0088] In actual application scenarios, a certain mass of sediment sample from the secondary side of a steam generator is weighed using an analytical balance. Instrumental analytical techniques (such as X-ray fluorescence spectroscopy and inductively coupled plasma optical emission spectroscopy) are then used to quantitatively analyze the content of the main component elements in the sediment sample. Table 1 shows the elemental content analysis results for the sediment sample, with iron accounting for 70.11% by weight.

[0089]

[0090] Table 1

[0091] Furthermore, elements in sediments may exist in various forms. Taking iron as an example, iron oxides (such as FeO, Fe2O3, Fe3O4, etc.) are the most common forms. They may also be iron carbonates, iron sulfides, and other forms. The physical properties of sediment samples are analyzed using an X-ray diffractometer to obtain the XRD spectrum of iron in the sediment samples to display the physical phase information of iron in the sediment samples. Subsequently, the standard XRD data of various possible forms of iron are compared with the sample XRD spectrum one by one, and the position and intensity of the diffraction peaks are compared to find the standard data that matches the XRD spectrum. Figure 3 The following is a comparison chart of the XRD spectrum of the sediment sample and the standard XRD data of Fe3O4. Figure 3 It can be seen that the experimental data is very consistent with the standard XRD data of Fe3O4, which further indicates that the iron element in the sediment sample exists in the form of Fe3O4.

[0092] Furthermore, the mass correlation coefficient between iron and Fe₃O₄ was calculated to be 1.378. Multiplying the iron mass content of 70.11% by 1.378 yields a Fe₃O₄ mass content of 96.61% in the sediment. Since the Fe₃O₄ mass content exceeds the preset threshold, it can be determined that iron is the primary component of the sediment. Therefore, the iron dissolution rate can be used to measure the cleaning efficiency of the sediment sample.

[0093] S207: Add a first preset volume of cleaning solution into a three-necked flask of preset specifications, and immerse the liquid portion of the three-necked flask below the silicone oil level.

[0094] S208. Heat the silicone oil to obtain the temperature of the cleaning solution in the three-necked flask.

[0095] S209 . When the temperature reaches and maintains the preset temperature value of the preset cleaning condition of the cleaning agent, a first preset mass of the sediment sample is added into the three-necked flask and stirred, so that the cleaning agent solution dissolves the sediment sample to obtain a dissolved mixture.

[0096] In steps S207 to S209, a first preset volume of cleaning solution is weighed and added to a three-necked flask of preset specifications. The solution at the bottom of the flask is submerged below the level of silicone oil. The silicone oil is heated to a preset temperature, ensuring that the cleaning solution reaches and maintains the required cleaning process temperature. Subsequently, a first preset mass of sediment sample is added to the three-necked flask, allowing the cleaning solution in the flask to dissolve the sediment sample. Dissolution of the sediment takes time, and during this process, the flask contains a supernatant resulting from the mixture of the cleaning solution and sediment sample, as well as undissolved sediment at the bottom of the supernatant.

[0097] In actual application scenarios, the three-necked flask is 500 ml in size. The top opening is used to accommodate the stirring shaft and impeller of the mechanical stirrer, while the other two openings are used to insert a thermometer and take analytical samples. Preset cleaning conditions include the stirring shaft speed and the cleaning agent temperature. When the temperature inside the three-necked flask reaches and maintains the cleaning agent temperature, the sediment sample is placed in the flask and the stirring shaft is controlled to stir at the set speed to ensure thorough mixing of the sediment and cleaning agent.

[0098] S210, determining multiple extraction moments according to a preset time interval;

[0099] S211. When the sediment sample is added to the three-necked flask, start timing to obtain the dissolution time;

[0100] S212. When the dissolution time reaches each extraction moment, extract a second preset volume of supernatant from the dissolution mixture into a centrifuge tube, and add a second preset volume of detergent solution into the three-necked flask.

[0101] In steps S210 through S212, to measure the peak concentration and its arrival time during the dissolution process, multiple extraction times are determined based on pre-set time intervals. When the sediment sample is added to the three-necked flask, the detergent solution begins dissolving the sediment sample, and the dissolution time of the detergent solution is measured. When the dissolution time reaches any extraction time, a second preset volume of supernatant is extracted from the dissolved mixture to measure the ion concentration at each extraction time. After each supernatant extraction, the three-necked flask is replenished with the second preset volume of detergent solution to prevent a reduction in supernatant volume from affecting the dissolution reaction rate.

[0102] Optionally, the value range of the preset time interval can be set according to the experimental design and the reference time range of the cleaning agent dissolution. For example, under normal circumstances, the cleaning process of the cleaning agent may need to be maintained for 8 to 12 hours. The initial dissolution reaction is faster, so the range of the preset time interval can be set shorter in the initial stage. For example, the extraction time intervals for the first three times are 10 minutes apart, that is, when the dissolution time is 10 minutes, 20 minutes and 30 minutes, the dissolved solution is extracted once respectively. Thereafter, the dissolution reaction tends to stabilize, and the extraction time interval can be stabilized at 30 minutes. That is, the dissolved solution is extracted every 30 minutes thereafter until 8.5 hours.

[0103] S213. Add a detergent solution into each centrifuge tube according to a preset dilution multiple to dilute the supernatant in each centrifuge tube to obtain a dissolved solution.

[0104] In this step, due to the limited volume of the solution sample, the volume of the supernatant extracted each time is small. In order to ensure the concentration measurement result, the supernatant is diluted with a detergent solution according to a preset dilution multiple to obtain a diluted dissolved solution.

[0105] Optionally, the preset dilution multiple can be five times, ten times, etc. According to the preset dilution multiple, the added volume of the cleaning agent is calculated, and the cleaning agent solution is dripped into the centrifuge tube according to the added volume to dilute the supernatant. In an embodiment of the present application, optionally, in order to ensure the accuracy of the concentration value measurement results, the maximum concentration value of each target element in each supernatant is determined according to the quantitative standard curve of the target element, the preset dilution multiple and a plurality of dissolving solutions, as well as the target extraction time corresponding to the maximum concentration value, further comprising: obtaining a standard solution of the target element with a first preset concentration; diluting the standard solution with a cleaning agent solution to obtain a plurality of diluted solutions with a second preset concentration; measuring the first signal intensity value of each diluted solution using a quantitative detection method; and drawing a quantitative standard curve of the target element according to the plurality of second preset concentrations and the plurality of first signal intensity values.

[0106] In this embodiment, in order to accurately measure the concentration change of the target element in the dissolved solution, it is necessary to construct a quantitative standard curve in advance using a standard solution of the target element. Specifically, the first preset concentration is the concentration value of the required standard solution of the target element, and this concentration value needs to be higher than the maximum concentration of the target element in the dissolved solution, so that the concentration in the drawn quantitative standard curve can cover the concentration change range of the target element in the dissolved solution. Thereafter, in order to ensure that the curve has enough data points to characterize the correspondence between concentration and signal intensity, a plurality of different second preset concentration values ​​are selected to prepare a dilution solution, and these concentrations cover three concentration ranges of lower concentration, medium concentration and higher concentration. After selecting a plurality of second preset concentration values, the standard solution is diluted with a detergent solution based on each second preset concentration value to obtain a dilution solution.

[0107] Furthermore, using X-ray fluorescence spectrometry or another appropriate quantitative method, measure the fluorescence intensity (first signal intensity) of each diluted solution. Record the first signal intensity value and the corresponding second predetermined concentration for each diluted solution. Then, plot a quantitative standard curve using the first signal intensity value of the target element in each diluted solution as the y-axis and the corresponding second predetermined concentration as the x-axis, ensuring good linearity across the concentration range.

[0108] In actual application scenarios, the maximum concentration of the target element in the dissolved solution is confirmed through prior analytical data or literature, and the first preset concentration is determined based on the maximum concentration to ensure that the first preset concentration exceeds the maximum concentration of the target element. For example, if the maximum concentration of the target element is 15,000 mg / L, then the first preset concentration of the purchased standard solution can be 20,000 mg / L. Then, based on the first preset concentration and the first preset volume, a standard solution of the target element is purchased. Thereafter, based on the first preset concentration, multiple second preset concentrations are set, such as 2,000 mg / L, 5,000 mg / L, 10,000 mg / L, 15,000 mg / L, and 20,000 mg / L, and the corresponding cleaning agent solutions are weighed according to the multiple second preset concentrations. Through appropriate mixing and dilution steps, the standard solution is adjusted to each second preset concentration to obtain multiple diluted solutions.

[0109] S214. Measure the second signal intensity value of each dissolved solution using a quantitative detection method.

[0110] S215 . Determine the first concentration value corresponding to each second signal intensity value according to the quantitative standard curve.

[0111] S216 , multiplying each first concentration value by the preset dilution factor to obtain a second concentration value of the target element in the supernatant.

[0112] S217 , obtaining the maximum concentration value of the target element in the supernatant and the target extraction time corresponding to the maximum concentration value.

[0113] In steps S214 to S217, the second signal intensity value of each dissolved solution is measured using X-ray fluorescence spectrometry or other appropriate quantitative methods. The first concentration value corresponding to each second signal intensity value is determined in a quantitative standard curve. Since the first concentration value represents the ion concentration in the diluted dissolved solution, to obtain the concentration of the target element in the supernatant before dilution, each second concentration value is multiplied by the preset dilution factor to obtain the concentration of the target element in the supernatant before dilution. Subsequently, the peak concentration and extraction time point at which the detergent solution has the highest dissolving power are determined. The peak concentration and target extraction time are then used to calculate the dissolution rate of the detergent solution on the sediment.

[0114] In an embodiment of the present application, optionally, in order to ensure the accuracy of the dissolution rate calculation, the method also includes: obtaining the relative atomic mass of each element and the molar mass of its corresponding phase composition; and calculating the mass relationship coefficient between each element and its corresponding phase composition through the molar mass and relative atomic mass.

[0115] In this embodiment, the relative atomic mass of the main target element can be determined by the molar mass of the constituent phase, and then the relationship coefficient between the mass of the constituent phase and the mass of the target element in the dissolved solution can be obtained. The dissolved amount of the constituent phase can be inferred from the concentration data of the target element obtained experimentally, thereby achieving quantitative measurement of the dissolution rate.

[0116] S218, multiplying the mass relationship coefficient and the maximum concentration value of each target element by the first preset volume, and dividing the multiplied value by the target extraction time to obtain the dissolution rate of the cleaning solution for the phase composition corresponding to each target element;

[0117] S219. In the case where there are multiple at least one target element, multiple dissolution rates of multiple phase compositions corresponding to the multiple target elements are added together to obtain a dissolution rate of the deposit by the cleaning solution.

[0118] In steps S218 and S219, for any target element, the first preset volume of the cleaning agent is multiplied by the maximum concentration value to obtain the mass of the dissolved sediment. The mass of the sediment is then multiplied by the mass relationship coefficient and divided by the target extraction time (expressed in minutes) corresponding to the maximum concentration value to obtain the dissolution rate of the cleaning agent solution for the phase composition corresponding to the target element.

[0119] Furthermore, if there is only one main target element in the sediment, the dissolution rate of the phase composition corresponding to the main element is directly used as the cleaning efficiency of the cleaning agent for cleaning the sediment; if the main target elements in the sediment contain two or more, after calculating the dissolution rate of the phase composition corresponding to each target element, the multiple dissolution rates are added together as the dissolution rate of the cleaning agent solution for cleaning the sediment.

[0120] This application further refines and expands the above-mentioned specific implementation methods, and in order to fully illustrate the specific implementation process of this embodiment, this embodiment provides another method for measuring the dissolution rate of a cleaning agent on a sediment, which includes the following six steps:

[0121] Step 1: Collection of sediment samples and quantitative analysis of main component elements and phase analysis of sediment samples.

[0122] Step 2: Prepare the cleaning solution.

[0123] Specifically, a chemical cleaning solution for the secondary side of the steam generator can be prepared according to literature, or a cleaning solution commercially available on the market can be directly purchased.

[0124] Step 3: Prepare experimental instruments.

[0125] Specifically, 200 ml of the cleaning solution was added to a 500 ml three-necked flask, with the bottom of the flask submerged below the silicone oil level. The top opening of the flask housed the agitator shaft and impeller of a mechanical stirrer, while the other two openings served as a thermometer and a sampling port for analytical samples. The silicone oil was heated until the cleaning solution reached and maintained the required cleaning temperature.

[0126] Step 4: After the cleaning solution reacts with the sediment sample, the concentration of iron in the supernatant is measured.

[0127] Specifically, 6 grams of dried secondary sediment sample was placed in a three-necked flask. At preset time intervals of 10 minutes, 20 minutes, and 0.5, 1, 1.5, 2, 2.5, 3, 3.5, 4, 4.5, 5, 5.5, 6, 6.5, 7, 7.5, 8, and 8.5 hours, 1 ml of the supernatant in the three-necked flask was placed in a centrifuge tube and diluted. Subsequently, a standard solution of the element Fe was prepared using the detergent solution as the matrix. A quantitative standard curve for the element Fe was established using X-ray fluorescence spectrometry. Figure 4 The figure shows a quantitative standard curve for Fe. Based on eight pre-set second concentrations, the signal intensity corresponding to each second concentration was measured. A standard curve was then plotted based on the corresponding relationship between signal intensity and concentration. Finally, the quantitative standard curve was used to determine the Fe concentration in the centrifuge tube at different extraction time points, thereby determining the Fe concentration in the three-necked flask.

[0128] Step 5: Draw a curve of the relationship between Fe concentration and time in the three-necked flask to determine the peak Fe concentration and its extraction time.

[0129] Specifically, if Figure 5 The figure below shows the relationship between Fe concentration and extraction time during the cleaning process. Plotting the relationship curve using multiple extraction times as the x-axis and multiple Fe concentrations as the y-axis clearly shows the dissolution changes of the cleaning solution, allowing the extraction time when the Fe concentration reaches its peak to be determined.

[0130] Step 6: Calculation of sediment cleaning efficiency.

[0131] Specifically, the mass of the dissolved Fe element is calculated based on the peak concentration when the Fe element in the supernatant no longer increases and the first preset volume extracted by the cleaning agent solution. Then, the dissolution rate of the cleaning agent, that is, the cleaning efficiency of the cleaning agent on Fe3O4, is calculated using the relationship coefficient between the mass of the dissolved Fe element, the mass of Fe3O4 and the mass of the Fe element, and the time point when the dissolving power is the strongest.

[0132] The calculation formula for the cleaning efficiency of the cleaning agent on Fe3O4 is:

[0133]

[0134] Wherein, p is the cleaning efficiency, in mg / min; c is the maximum concentration value, in μg / ml; v is the first preset volume (ignoring the change in cleaning agent volume caused by sampling), in ml; k is the coefficient of the relationship between the mass of dissolved Fe3O4 and the mass of Fe element in the solution, which is a constant of 1.378, in 1; t is the target extraction time when the Fe element concentration reaches its peak, in minutes.

[0135] By the above method, the concentration of relevant ions in the dissolved solution is measured, the relationship between ion concentration and time is established, the dissolution rate of the cleaning agent is calculated, and the cleaning efficiency of the cleaning agent on the secondary side of the steam generator is determined.

[0136] Those skilled in the art will understand that the accompanying drawings are only schematic diagrams of a preferred implementation scenario, and the modules or processes in the accompanying drawings are not necessarily required to implement the present application.

[0137] The above application serial numbers are for description only and do not represent the advantages or disadvantages of the implementation scenarios.

[0138] The above disclosure only describes several specific implementation scenarios of the present application. However, the present application is not limited thereto, and any changes that can be conceived by those skilled in the art should fall within the scope of protection of the present application.

Claims

1. A method for measuring the dissolution rate of a cleaning agent on a sediment, characterized in that: include: Obtaining multiple elements contained in the sediment sample to be cleaned, the phase composition corresponding to each element, and the mass content of each phase composition in the sediment sample; Sort the multiple mass contents in descending order, add up each mass content in sequence starting from the mass content in the first position, and when the sum of the mass contents reaches a preset threshold, obtain at least one target element corresponding to at least one phase composition contained in the sum of the mass contents; Mixing a first preset mass of the sediment sample with a first preset volume of a cleaning solution, so that the sediment and the cleaning solution undergo a dissolution reaction under preset cleaning conditions to obtain a dissolved mixture, wherein the dissolved mixture includes a supernatant and undissolved sediment; extracting a plurality of supernatants from the dissolution mixture according to a preset time interval and a second preset volume; Diluting the plurality of supernatants with the cleaning solution according to a preset dilution multiple to obtain a plurality of dissolved solutions; Determining the maximum concentration of each target element in each supernatant and the target extraction time corresponding to the maximum concentration based on a quantitative standard curve for each target element, the preset dilution factor, and the plurality of dissolving solutions, wherein the quantitative standard curve shows a corresponding relationship between the signal intensity measured by the quantitative instrument and the concentration of the target element; The dissolution rate of the deposit by the cleaning solution is calculated according to the first preset volume, the maximum concentration value corresponding to each target element, the target extraction time corresponding to each target element, and the mass relationship coefficient between each target element and the phase composition.

2. The method according to claim 1, characterized in that The step of obtaining multiple elements contained in the sediment sample to be cleaned, the phase composition corresponding to each element, and the mass content of each phase composition in the sediment sample specifically includes: obtaining the sediment sample in the equipment to be cleaned; Performing element quantitative analysis on the sediment sample using element quantitative analysis technology to obtain multiple mass contents of multiple elements in the sediment sample; Performing phase analysis on the sediment sample using X-ray diffraction (XRD) technology to determine the phase composition corresponding to each element; Calculating the mass relationship coefficient between each element and its corresponding phase composition; The mass content of each element is multiplied by the mass relationship coefficient to obtain the mass content of the phase composition corresponding to each element in the sediment sample.

3. The method according to claim 1, characterized in that The step of mixing the sediment sample of a first preset mass and the cleaning solution of a first preset volume so that the sediment and the cleaning solution undergo a dissolution reaction under preset cleaning conditions to obtain a dissolved mixture specifically includes: Adding the first preset volume of the cleaning solution into a three-necked flask of preset specifications, and immersing the bottom solution portion of the three-necked flask below the silicone oil; Heating the silicone oil to obtain the temperature of the cleaning solution in the three-necked flask; When the temperature reaches and maintains the preset temperature value of the preset cleaning condition of the cleaning agent, the sediment sample of the first preset mass is added to the three-necked flask and stirred, so that the cleaning agent solution dissolves the sediment sample to obtain the dissolved mixture.

4. The method according to claim 3, characterized in that The step of extracting a plurality of supernatants from the dissolved mixture according to a preset time interval and a second preset volume specifically includes: Determining multiple extraction moments according to the preset time interval; When the sediment sample is added to the three-necked flask, the timing is started to obtain the dissolution time; When the dissolution time reaches each extraction moment, the second preset volume of supernatant is extracted from the dissolution mixture into a centrifuge tube, and the second preset volume of the cleaning agent solution is added to the three-necked flask.

5. The method according to claim 4, characterized in that The step of diluting each supernatant with the cleaning solution according to a preset dilution multiple to obtain a plurality of dissolved solutions specifically includes: According to the preset dilution multiple, the detergent solution is added into each centrifuge tube to dilute the supernatant in each centrifuge tube to obtain a dissolved solution.

6. The method according to claim 1, characterized in that The method further comprises determining the maximum concentration value of each target element in each supernatant according to the quantitative standard curve of each target element, the preset dilution factor, and the plurality of dissolving solutions, and determining the target extraction time corresponding to the maximum concentration value. Obtaining a standard solution of a target element with a first preset concentration; diluting the standard solution with the cleaning solution to obtain a plurality of diluted solutions with a second preset concentration; Measuring a first signal intensity value of each diluted solution using a quantitative detection method; The quantitative standard curve of the target element is drawn according to the multiple second preset concentrations and the multiple first signal intensity values.

7. The method according to claim 1, characterized in that The step of determining the maximum concentration value of each target element in each supernatant and the target extraction time corresponding to the maximum concentration value based on the quantitative standard curve of each target element, the preset dilution factor, and the multiple dissolution solutions specifically includes: Measuring the second signal intensity value of each dissolved solution using a quantitative detection method; Determining the first concentration value corresponding to each second signal intensity value according to the quantitative standard curve; Multiplying the preset dilution factor by each first concentration value to obtain a second concentration value of the target element in the supernatant; The maximum concentration value of the target element in the supernatant and the target extraction time corresponding to the maximum concentration value are obtained.

8. The method according to any one of claims 1 to 7, characterized in that Also includes: Obtain the relative atomic mass of each element and the molar mass of its corresponding phase composition; The mass relationship coefficient between each element and its corresponding phase composition is calculated based on the molar mass and the relative atomic mass.

9. The method according to any one of claims 1 to 7, characterized in that The step of calculating the dissolution rate of the sediment by the cleaning solution based on the first preset volume, the maximum concentration value corresponding to each target element, the target extraction time corresponding to each target element, and the mass relationship coefficient between each target element and the phase composition specifically includes: Multiplying the mass relationship coefficient of each target element, the maximum concentration value, and the first preset volume, and dividing the multiplied value by the target extraction time to obtain the dissolution rate of the cleaning solution for the phase composition corresponding to each target element; In the case where there are multiple at least one target element, multiple dissolution rates of multiple phase compositions corresponding to the multiple target elements are added together to obtain the dissolution rate of the deposit by the cleaning solution.

10. The method according to any one of claims 1 to 7, characterized in that Elemental quantitative analysis techniques include any of the following: X-ray fluorescence analysis and inductively coupled plasma optical emission spectrometry.

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