CN114544818B - Method and system for detecting concentration of formamide in triazole production recycling matter - Google Patents
Method and system for detecting concentration of formamide in triazole production recycling matter Download PDFInfo
- Publication number
- CN114544818B CN114544818B CN202210222156.9A CN202210222156A CN114544818B CN 114544818 B CN114544818 B CN 114544818B CN 202210222156 A CN202210222156 A CN 202210222156A CN 114544818 B CN114544818 B CN 114544818B
- Authority
- CN
- China
- Prior art keywords
- peak
- formamide
- target
- triazole
- determining
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid chromatography
Abstract
The invention provides an online detection method and system for formamide concentration in a triazole production recovery product, which comprises the following steps: quantitatively extracting the triazole production recovery product obtained by production at preset time intervals, and transmitting the triazole production recovery product to a detection pool; heating the triazole production recovered substance to a preset temperature to obtain a liquid to be detected, and injecting the liquid to be detected into a liquid chromatograph to obtain a chromatogram; performing comparative analysis on peak signals in the chromatogram based on preset formamide peak signals to determine the content of formamide in the liquid to be detected; determining the concentration of formamide in the triazole production recovery product according to the content of formamide in the liquid to be detected based on the drying proportion of the triazole production recovery product; the invention provides an online detection method and system for formamide concentration in a triazole production recovery product, which can realize online real-time detection of the formamide concentration in the triazole production recovery product and have the advantages of high detection speed, high detection precision and high data real-time property.
Description
Technical Field
The invention relates to the technical field of formamide concentration detection, in particular to an online detection method and system for formamide concentration in a triazole production recycling substance.
Background
Triazole is an organic matter, has a chemical formula of C2H3N3, is widely applied to synthesis of pesticides such as triadimefon, paclobutrazol, uniconazole and diniconazole, is a white needle crystal, is a light yellow or brown needle crystal as an industrial product, and has strong water absorption.
The production and manufacture of the triazole are carried out in the presence of formamide, ammonia, hydrogen peroxide and butanone react, a certain amount of formamide exists in a production and manufacture triazole production recovered substance, and the lower the concentration of the formamide in the triazole production recovered substance is, the higher the purity of the prepared triazole is, so that in a production line for continuously producing the triazole, the online detection on the concentration of the formamide in the triazole production recovered substance is required to ensure the purity of the produced triazole.
The traditional detection method for detecting the concentration of formamide is to detect the concentration of formamide in a triazole production recovery product after triazole is completely produced, so that the adjustment and control of the triazole production process are not convenient, the production process is adjusted in time, and the purity of triazole is ensured.
Disclosure of Invention
The invention provides an online detection method and system for formamide concentration in a triazole production recycled substance, which can realize online real-time detection of the formamide concentration in the triazole production recycled substance and have the advantages of quick detection, high detection precision and high data real-time property.
An online detection method for formamide concentration in a triazole production recovery product comprises the following steps:
step 1: quantitatively extracting the triazole production recovery product obtained by production at preset time intervals, and transmitting the triazole production recovery product to a detection pool;
step 2: heating the triazole production recovered substance to a preset temperature to obtain a liquid to be detected, and injecting the liquid to be detected into a liquid chromatograph to obtain a chromatogram;
and 3, step 3: performing comparative analysis on peak signals in the chromatogram based on preset formamide peak signals to determine the content of formamide in the liquid to be detected;
and 4, step 4: and determining the concentration of formamide in the triazole production recovery product according to the content of formamide in the liquid to be detected based on the drying ratio of the triazole production recovery product.
In one possible way of realisation,
step 1, quantitatively extracting triazole production recovery products obtained by production at intervals of preset time, and transmitting the triazole production recovery products to a detection pool comprises the following steps:
establishing a dynamic model of the triazole production recycling material in the production process based on the operation parameters of the extraction device and a historical production database;
inputting quantitative values into the dynamic model, and determining target operating parameters of the extraction device;
and extracting the triazole production recycled material based on the target operation parameters, and conveying the extracted triazole production recycled material to the detection pool through a conveyor belt.
In one possible way of realisation,
in the step 2, heating the triazole production recovered material to a preset temperature to obtain a liquid to be detected comprises the following steps:
heating the detection pool according to a first temperature and a first heating time, and monitoring to obtain the state of a triazole production recycling object in the detection pool when the heating in the first time is completed;
and setting a second temperature to heat the triazole production recovered substance based on the state until the triazole production recovered substance is completely melted into liquid, so as to obtain the liquid to be detected.
In one possible way of realisation,
in step 2, injecting the liquid to be detected into a liquid chromatograph, and obtaining a chromatogram comprises:
injecting the liquid to be detected into a detection channel of the liquid chromatograph after being processed in advance to realize the separation of various substances in the liquid to be detected;
and acquiring the chromatogram of the liquid to be detected after a preset detection time.
In one possible way of realisation,
before step 3, the method further comprises the following steps: determining the peak signals of formamide in the chromatogram by the following steps:
injecting the obtained formamide solution into a detection channel of the liquid chromatograph in the same way as the triazole production recovered substance to obtain a contrast chromatogram;
recording the retention time, peak signal intensity and peak area of a contrast chromatogram peak in the contrast chromatogram;
determining the proportional relation between the formamide solution content and the peak area based on the peak area;
and based on the retention time of the contrast chromatographic peak and the peak signal intensity, taking the contrast chromatographic peak as a preset formamide peak signal.
In one possible way of realisation,
in step 3, based on a preset formamide peak signal, performing comparative analysis on the peak signal in the chromatogram, and determining the content of formamide in the liquid to be detected comprises the following steps:
extracting peak signals in the chromatogram to obtain a peak signal sequence, and acquiring a target peak signal sequence consistent with the preset formamide peak signal from the peak signal sequence;
extracting a chromatographic peak in the target peak signal sequence, and performing denoising processing on the chromatographic peak to obtain a denoised chromatographic peak;
comparing the peak signal intensity of the denoising chromatographic peak with the peak signal intensity of the preset formamide peak signal to obtain an intensity difference value, and judging whether the intensity difference value is within a preset difference value range;
if so, determining that the de-noised chromatographic peak is a pure peak and the corresponding substance is formamide, and acquiring a target signal curve corresponding to the de-noised chromatographic peak;
otherwise, determining the denoised chromatographic peak as a mixed peak;
when the denoised chromatographic peak is determined to be a mixed peak, obtaining the retention time of the denoised chromatographic peak, and comparing the retention time with the retention time of a contrast chromatographic peak to obtain a time difference value;
determining a formamide purity value determined by the denoising chromatographic peak based on the intensity difference value and the time difference value;
detecting the denoising chromatographic peak to obtain a signal curve of the denoising chromatographic peak, and marking a peak point in the signal curve to obtain a peak point label;
based on the formamide purity value determined by the denoising chromatographic peak, an adjusting scheme is obtained, and according to the adjusting scheme and based on the peak point label, the peak point in the signal curve is adjusted to obtain a target signal curve;
standardizing the target signal curve according to a contrast signal curve of a contrast chromatographic peak to obtain a standard signal curve;
and calculating the peak area of the region surrounded by the target signal curve, and determining the content of formamide in the liquid to be detected based on the proportional relation between the content of formamide solution and the peak area.
In one possible way of realisation,
determining the formamide purity value determined by the denoising chromatographic peak based on the intensity difference value and the time difference value comprises:
determining possible components of other substances in the mixed peak based on the intensity difference, and acquiring retention time of the possible components;
comparing the time difference with the retention time of the possible components, and selecting a target component in the possible components corresponding to the minimum time difference;
analyzing the de-noised chromatographic peak based on the standard peak signal intensity and the standard retention time of the target component to determine the ratio of the target component;
analyzing the de-noised chromatographic peak based on the peak signal intensity and retention time of formamide, and determining the purity value of the formamide;
and verifying the purity value based on the ratio, wherein if the verification is successful, the purity value is the purity value of the formamide determined by the denoising chromatographic peak, otherwise, the purity value of the formamide is adjusted based on the ratio.
In one possible way of realisation,
in the step 4, based on the drying ratio of the triazole production recovery product, determining the formamide concentration in the triazole production recovery product according to the formamide content in the liquid to be detected comprises:
analyzing the triazole production recovery product obtained by extraction and production, and determining the initial state of the triazole production recovery product;
determining the final state of the triazole production recycled material based on a preset process, and determining the process flow from the initial state to the final state;
acquiring a process example related to the process flow from a process database, and determining the change information of each component in the triazole production recovery before and after the process based on the process example;
determining content changes of the components before and after the process based on the change information, and setting a first weight value based on the weight change;
determining the state change of formamide in the triazole production recycled material based on the change information, and setting a second weight value based on the state change;
determining a first total value of the triazole production recovered material in a final state based on the quantitative value of the triazole production recovered material obtained by extraction and production and the drying ratio of the triazole production recovered material;
based on the first weight value and the second weight value, carrying out weighted calculation on the first weight value to obtain a second total value;
determining a first content value of formamide corresponding to the content of formamide in the liquid to be detected, and performing weighted calculation on the first content value based on the second weight value to obtain a second content value;
and calculating to obtain the concentration of formamide in the triazole production recycling material based on the second total value and the second content value.
In one possible way of realisation,
the method is characterized in that the step of calculating the peak area of the region surrounded by the target signal curve comprises the following steps:
inputting the target signal curve into a slope detection system, determining the slope corresponding to each peak in the target signal curve, eliminating the peak corresponding to the slope which is not in a first preset range, correcting the slope of the peak corresponding to the slope which is in a second preset range, and outputting a new target signal curve according to the elimination and correction results;
sampling the new target signal curve to obtain n acquisition graphs, and obtaining the peak area of the new target signal curve based on the n acquisition graphs;
generating a first target pattern spot based on the target signal curve, generating a second target pattern spot based on the new target signal curve, and superposing the first target pattern spot and the second target pattern spot to obtain a third target pattern spot;
acquiring the peak area reliability of the region surrounded by the standard signal curve based on the first target pattern spot area, the second target pattern spot area and the third target pattern spot area;
judging whether the peak area reliability is greater than a preset reliability;
if so, determining that the peak area of the new target signal curve can represent the content of formamide in the liquid to be detected;
otherwise, correcting the new target curve again until the peak area reliability is greater than the preset reliability.
An online detection system for formamide concentration in a triazole production recovery product comprises:
the extraction and transmission module is used for quantitatively extracting the triazole production recovery substances obtained by production at intervals of preset time and transmitting the triazole production recovery substances to the detection pool;
the detection module is used for heating the triazole production recovered substance to a preset temperature to obtain liquid to be detected, and injecting the liquid to be detected into a liquid chromatograph to obtain a chromatogram;
the analysis module is used for carrying out comparison analysis on the peak signals in the chromatogram based on preset formamide peak signals to determine the content of formamide in the liquid to be detected;
and the determining module is used for determining the concentration of formamide in the triazole production recovery product according to the content of formamide in the liquid to be detected based on the drying ratio of the triazole production recovery product.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The objectives and other advantages of the invention will be realized and attained by the structure particularly pointed out in the written description and claims hereof as well as the appended drawings.
The technical solution of the present invention is further described in detail by the accompanying drawings and embodiments.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is a flow chart of an online detection method for formamide concentration in a triazole production recycling substance in the embodiment of the invention;
FIG. 2 is another flow chart of the online detection method for formamide concentration in a recycle product in triazole production in the embodiment of the invention;
FIG. 3 is a structural diagram of an online detection system for formamide concentration in a triazole production recycling substance in an embodiment of the invention.
Detailed Description
The preferred embodiments of the present invention will be described in conjunction with the accompanying drawings, and it will be understood that they are described herein for the purpose of illustration and explanation and not limitation.
Example 1
An online detection method for formamide concentration in a triazole production recovery product is shown in figure 1 and comprises the following steps:
step 1: quantitatively extracting the triazole production recovery product obtained by production at preset time intervals, and transmitting the triazole production recovery product to a detection pool;
step 2: heating the triazole production recovered substance to a preset temperature to obtain a liquid to be detected, and injecting the liquid to be detected into a liquid chromatograph to obtain a chromatogram;
and step 3: performing comparative analysis on peak signals in the chromatogram based on preset formamide peak signals to determine the content of formamide in the liquid to be detected;
and 4, step 4: and determining the concentration of formamide in the triazole production recovery product according to the content of formamide in the liquid to be detected based on the drying ratio of the triazole production recovery product.
In this embodiment, the detection cell is used for heating the recovered triazole production product and injecting the liquid to be detected into the liquid chromatograph.
In this example, different species present different peak signals after injection into the liquid chromatograph.
In this embodiment, the preset temperature is an optimal temperature for ensuring that the triazole production recycling material is in a liquid state.
In this embodiment, the determination of the formamide content in the liquid to be detected is determined by the area of a peak signal in the chromatogram which is the same as the preset formamide peak signal.
In this embodiment, after the triazole production recovery product is manufactured, the triazole production recovery product needs to be further dried, and the concentration of formamide in the dried triazole production recovery product is determined to determine the concentration of formamide in the triazole production recovery product.
The beneficial effect of above-mentioned design is: the convenience for detecting the concentration of formamide in the triazole production recovery substances is improved through quantitative extraction of the triazole production recovery substances on the production line at preset time intervals, the detection pool is used for heating the triazole production recovered substance, so that liquidization of the triazole production recovered substance is ensured, a foundation is provided for amide concentration detection, comparing and analyzing peak signals in the chromatogram to determine the content of formamide in the liquid to be detected, having the characteristics of quick detection and high data real-time performance, improving the efficiency of formamide concentration detection, and finally, producing the drying proportion of the recovered substances through triazole, and determining the concentration of formamide in the triazole production recovery product according to the content of formamide in the liquid to be detected, so that the accuracy of formamide concentration determination is ensured, and an accurate data basis is provided for adjustment and control in the triazole production process.
Example 2
Based on embodiment 1, the embodiment of the invention provides an online detection method for formamide concentration in a triazole production recovery product, which is characterized in that step 1, the triazole production recovery product obtained by production is quantitatively extracted every preset time and transmitted to a detection pool, and the method comprises the following steps:
step 11, establishing a dynamic model of the triazole production recycling material in the production process based on the operation parameters of the extraction device and a historical production database;
step 12, inputting quantitative values into the dynamic model, and determining target operating parameters of the extraction device;
and step 13, extracting the triazole production recycled material based on the target operation parameters, and conveying the extracted triazole production recycled material to the detection pool through a conveyor belt.
In the embodiment, the extraction device is specially used for the intelligent extraction device for the triazole production recovered substances, and quantitative extraction of the triazole production recovered substances can be realized by setting the operation parameters.
The beneficial effect of above-mentioned design is: the dynamic model is determined according to the operating parameters of the extraction device and the historical production database, so that appropriate target operating parameters are set, the quantitative extraction of the triazole production recovery substances is realized, the quantitative analysis of the triazole production recovery substances in the formamide concentration detection process is not required, and the convenience of formamide concentration detection in the triazole production recovery substances is improved.
Example 3
Based on embodiment 1, the embodiment of the invention provides an online detection method for formamide concentration in a triazole production recovery product, and in step 2, heating the triazole production recovery product to a preset temperature to obtain a liquid to be detected comprises the following steps:
heating the detection pool according to a first temperature and a first heating time, and monitoring to obtain the state of a triazole production recycling object in the detection pool when the heating in the first time is completed;
and setting a second temperature to heat the triazole production recovered substance based on the state until the triazole production recovered substance is completely melted into liquid, so as to obtain the liquid to be detected.
In this embodiment, the first temperature is greater than the second temperature.
In the embodiment, the approximately melting of the triazole production recycling material is realized by heating according to the first temperature, the complete melting of the triazole production recycling material is realized by heating according to the second temperature, and the melting can be realized without the temperature as high as the first temperature when the triazole production recycling material is melted in the later stage.
The beneficial effect of above-mentioned design is: the first temperature and the second temperature are used for melting the triazole production recycled material in sequence, so that the melting efficiency is guaranteed, the waste of resources is reduced, and the realization of liquidization of the triazole production recycled material in the maximum benefit is guaranteed.
Example 4
Based on embodiment 1, the embodiment of the invention provides an online detection method for formamide concentration in a triazole production recovery product, and in step 2, the liquid to be detected is injected into a liquid chromatograph, and the obtained chromatogram comprises the following steps:
injecting the liquid to be detected into a detection channel of the liquid chromatograph after being processed in advance to realize the separation of various substances in the liquid to be detected;
and acquiring the chromatogram of the liquid to be detected after a preset detection time.
In the embodiment, the liquid chromatograph has an online analysis processing function, so that the liquid to be detected does not need to be processed before being injected into the detection channel, and the detection efficiency is improved.
In this embodiment, the liquid to be detected may be diluted in proportion and then injected in a proper amount.
The beneficial effect of above-mentioned design is: the chromatogram is obtained by directly injecting the liquid to be detected into the detection channel of the liquid chromatograph, so that the liquid to be detected is not required to be treated before being injected into the detection channel, the detection efficiency is improved, and the rapidity of formamide concentration detection is ensured.
Example 5
Based on embodiment 1, the embodiment of the invention provides an online detection method for formamide concentration in a triazole production recovery product, which comprises the following steps before step 3: determining the peak signals of formamide in the chromatogram by the following steps:
injecting the obtained formamide solution into a detection channel of the liquid chromatograph in the same way as the triazole production recovered substance to obtain a contrast chromatogram;
recording retention time, peak signal intensity and peak area of chromatographic peaks in the contrast chromatogram;
determining the proportional relation between the formamide solution content and the peak area based on the peak area;
and based on the retention time of the chromatographic peak and the peak signal intensity, the formamide peak signal is used as a preset formamide peak signal.
The beneficial effect of above-mentioned design is: the formamide solution is detected in advance in the same way as the triazole production recovery to obtain the retention time of a chromatographic peak, the peak signal intensity and the peak area, and a basis is provided for determining the content of formamide in the liquid to be detected.
Example 6
Based on embodiment 1, the embodiment of the invention provides an online detection method for formamide concentration in a triazole production recovery product, and in step 3, based on a preset formamide peak signal, comparison analysis is performed on the peak signal in a chromatogram, and the determination of formamide content in a liquid to be detected comprises the following steps:
extracting peak signals in the chromatogram to obtain a peak signal sequence, and acquiring a target peak signal sequence consistent with the preset formamide peak signal from the peak signal sequence;
extracting a chromatographic peak in the target peak signal sequence, and performing denoising processing on the chromatographic peak to obtain a denoised chromatographic peak;
comparing the peak signal intensity of the denoising chromatographic peak with the peak signal intensity of the preset formamide peak signal to obtain an intensity difference value, and judging whether the intensity difference value is within a preset difference value range;
if so, determining that the de-noised chromatographic peak is a pure peak and the corresponding substance is formamide, and acquiring a target signal curve corresponding to the de-noised chromatographic peak;
otherwise, determining the denoised chromatographic peak as a mixed peak;
when the denoised chromatographic peak is determined to be a mixed peak, obtaining the retention time of the denoised chromatographic peak, and comparing the retention time with the retention time of a contrast chromatographic peak to obtain a time difference value;
determining a formamide purity value determined by the denoising chromatographic peak based on the intensity difference value and the time difference value;
detecting the denoising chromatographic peak to obtain a signal curve of the denoising chromatographic peak, and marking a peak point in the signal curve to obtain a peak point label;
based on the formamide purity value determined by the denoising chromatographic peak, an adjusting scheme is obtained, and according to the adjusting scheme and based on the peak point label, the peak point in the signal curve is adjusted to obtain a target signal curve;
standardizing the target signal curve according to a contrast signal curve of a contrast chromatographic peak to obtain a standard signal curve;
and calculating the peak area of the region surrounded by the target signal curve, and determining the content of formamide in the detection liquid based on the proportional relation between the content of formamide solution and the peak area.
In this embodiment, the peak signal sequence consists of a plurality of peak signals in chronological order.
In this embodiment, after the denoising processing is performed on the chromatographic peak, noise interference can be removed, and the accuracy of the peak signal is ensured.
In this embodiment, due to reasons such as improper operation of the liquid chromatograph, complete separation of each substance in the liquid to be detected may not be achieved, and a mixed peak may occur, and at this time, the purity of formamide in the mixed peak needs to be determined according to the retention time of the mixed peak, so as to ensure the accuracy of determining the content of formamide.
In this embodiment, the adjustment scheme is to adjust the position of the peak point in the signal curve according to the purity value of formamide, so as to ensure that the obtained target signal curve can represent the characteristic of formamide.
In this embodiment, the target signal curve is normalized to ensure the consistency of the standard signal curve and the comparison signal curve in format, so as to facilitate the analysis of the standard signal curve according to the comparison signal curve.
The beneficial effect of above-mentioned design is: the peak signal in the chromatogram is adjusted from the peak signal intensity and retention time, and is subjected to standardization treatment, and is analyzed and compared with a comparison chromatographic peak, so that the accuracy of finally determining the content of formamide in the liquid to be detected is ensured, and an accurate data basis is provided for determining the concentration of formamide in a triazole production recovery product.
Example 7
Based on embodiment 6, the embodiment of the invention provides an online detection method for formamide concentration in a triazole production recycled product, and the determination of the purity value of formamide determined by the de-noising chromatographic peak based on the intensity difference value and the time difference value comprises the following steps:
determining possible components of other substances in the mixed peak based on the intensity difference, and acquiring retention time of the possible components;
comparing the time difference with the retention time of the possible components, and selecting a target component in the possible components corresponding to the minimum time difference;
analyzing the de-noised chromatographic peak based on the standard peak signal intensity and the standard retention time of the target component to determine the ratio of the target component;
analyzing the de-noised chromatographic peak based on the peak signal intensity and retention time of formamide, and determining the purity value of the formamide;
and verifying the purity value based on the ratio, wherein if the verification is successful, the purity value is the purity value of the formamide determined by the de-noised chromatographic peak, otherwise, the purity value of the formamide is adjusted based on the ratio.
In this embodiment, the possible components are various and are all the substances of the triazole production recycling matter.
In this embodiment, based on the ratio, verifying the purity value is to determine whether the sum of the purity value and the ratio is 1, if so, indicating that the verification is successful, otherwise, indicating that the verification is failed, and after the verification fails, adjusting the value of the purity value based on the ratio.
The beneficial effect of above-mentioned design is: the components determined by the de-noising chromatographic peak are judged based on the intensity difference value and the time difference value, and the determined components are utilized to verify the determined formamide purity value, so that the reliability of the determined formamide purity value is ensured.
Example 8
On the basis of embodiment 1, the embodiment of the invention provides an online detection method for formamide concentration in a triazole production recovery product, and in step 4, determining the formamide concentration in the triazole production recovery product according to the formamide content in the liquid to be detected based on the drying ratio of the triazole production recovery product comprises the following steps:
analyzing the triazole production recovery product obtained by extraction and production, and determining the initial state of the triazole production recovery product;
determining the final state of the triazole production recycled material based on a preset process, and determining the process flow from the initial state to the final state;
acquiring a process example related to the process flow from a process database, and determining the change information of each component in the triazole production recovery before and after the process based on the process example;
determining content changes of the components before and after the process based on the change information, and setting a first weight value based on the weight change;
determining the state change of formamide in the triazole production recycled material based on the change information, and setting a second weight value based on the state change;
determining a first total value of the triazole production recovered matter in a final state based on the quantitative value of the triazole production recovered matter obtained by extraction and production and the drying ratio of the triazole production recovered matter;
based on the first weight value and the second weight value, carrying out weighted calculation on the first weight value to obtain a second total value;
determining a first content value of formamide corresponding to the content of formamide in the liquid to be detected, and performing weighted calculation on the first content value based on the second weight value to obtain a second content value;
and calculating to obtain the concentration of formamide in the triazole production recycling material based on the second total value and the second content value.
In this embodiment, the process flow may be, for example, drying the triazole production recycle.
In this embodiment, the change information includes, for example, changes in the form and weight of each component.
In this embodiment, the first weight value is weighted and calculated based on the first weight value and the second weight value to obtain a second total value, so that the influence on the total amount caused by the operation of producing the recycle product from triazole in the process can be reduced, and the accuracy of the second total value is ensured.
In this embodiment, the drying ratio is set in advance.
In this embodiment, based on the second weight value, the first content value is subjected to weighted calculation to obtain a second content value, so that the influence on the formamide content caused by the operation of producing the recycle product from triazole in the process is reduced, and the accuracy of the second content value is ensured.
The beneficial effect of above-mentioned design is: the method comprises the steps of determining the change information of each component of the triazole production recovered product before and after the process flow according to the process flow of the triazole production recovered product, performing weighted calculation on the total amount of the triazole production recovered product and the content of formamide according to the change information, ensuring the real-time performance of data, and enabling the obtained numerical value to be more accurate, thereby ensuring the accuracy of formamide concentration determination, determining the formamide concentration before the processing technology of the triazole production recovered product, and providing an accurate data base for the adjustment and control of the triazole production process on the premise of no stop of production.
Example 9
Based on embodiment 6, the invention provides an online detection method for formamide concentration in a triazole production recovery product, and the calculation of the peak area of the region surrounded by the target signal curve comprises the following steps:
inputting the target signal curve into a slope detection system, determining the slope corresponding to each peak in the target signal curve, eliminating the peak corresponding to the slope which is not in a first preset range, correcting the slope of the peak corresponding to the slope which is in a second preset range, and outputting a new target signal curve according to the elimination and correction results;
sampling the new target signal curve to obtain n acquisition graphs, and obtaining the peak area of the new target signal curve based on the n acquisition graphs;
the calculation formula of the peak area is as follows:
wherein A represents the peak area, ω represents the sampling frequency, n represents the number of sampling times and the number of acquisition patterns, s i The length of the side of the ith collection graph is shown, tau represents the error coefficient determined by the sampling frequency value to the peak area, the value is (0.1, 0.5), A 1 Denotes the area of the 1 st acquisition pattern, A n Representing the area of the nth acquisition pattern;
generating a first target pattern spot based on the target signal curve, generating a second target pattern spot based on the new target signal curve, and superposing the first target pattern spot and the second target pattern spot to obtain a third target pattern spot;
acquiring the peak area reliability of the new target signal curve based on the areas of the first target pattern spot, the second target pattern spot and the third target pattern spot;
the calculation formula of the peak area reliability is as follows:
wherein δ represents the peak area reliability of the new target signal curve, D a Representing the first target spot area, D b Representing the second target spot area, D c Representing the second target spot area, wherein D c >D a ，D c >D b ；
Judging whether the peak area reliability is greater than a preset reliability;
if so, determining that the peak area of the new target signal curve can represent the content of formamide in the liquid to be detected;
and if not, correcting the new target curve again until the peak area reliability is greater than the preset reliability.
In this embodiment, the peak whose slope is not within the first preset range is removed to eliminate interference of an interference peak in the target signal curve, the slope of the peak whose slope is within the second preset range is corrected to avoid interference of peak noise, and the slope of the peak is corrected to change the shape of the peak, so that the peak area is also changed, and the accuracy of the peak area is ensured.
In this embodiment, the peak area reliability of the new target signal curve is calculated by the first target pattern area, the second target pattern area, and the third target pattern area, and the reasonability of the new target signal curve can be ensured, thereby ensuring the peak area reliability of the new target signal curve.
In this embodiment, for the formula
It may be for example that,
A 1 ＝0.4，A n when ω is 0.6, ω is 0.5, τ is 0.2, a is 15.3.
In this embodiment, for maleFormula (II)
For example, can be D c ＝16.0，D a ＝15.3，D b When δ is 15.0, δ can be 0.5.
The beneficial effect of above-mentioned design is: the accuracy of the peak area is guaranteed by adjusting the target signal curve, and the reliability of the peak area is judged according to the area difference between the new target curve and the target signal curve, so that the peak area of the obtained new target signal curve can represent the content of formamide in the liquid to be detected, and a reliable data base is extracted for determining the concentration of formamide.
Example 10
An online detection system for formamide concentration in a triazole production recovery product, as shown in fig. 3, comprises:
the extraction and transmission module is used for quantitatively extracting the triazole production recovered material obtained by production at intervals of preset time and transmitting the triazole production recovered material to the detection pool;
the detection module is used for heating the triazole production recovered substance to a preset temperature to obtain a liquid to be detected, and injecting the liquid to be detected into a liquid chromatograph to obtain a chromatogram;
the analysis module is used for carrying out comparison analysis on the peak signals in the chromatogram based on preset formamide peak signals to determine the content of formamide in the liquid to be detected;
and the determining module is used for determining the concentration of formamide in the triazole production recovery product according to the content of formamide in the liquid to be detected based on the drying ratio of the triazole production recovery product.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (8)
1. An online detection method for formamide concentration in a triazole production recovery product is characterized by comprising the following steps:
step 1: quantitatively extracting the triazole production recovery product obtained by production at preset time intervals, and transmitting the triazole production recovery product to a detection pool;
step 2: heating the triazole production recovered substance to a preset temperature to obtain a liquid to be detected, and injecting the liquid to be detected into a liquid chromatograph to obtain a chromatogram;
and step 3: performing comparative analysis on peak signals in the chromatogram based on preset formamide peak signals to determine the content of formamide in the liquid to be detected;
and 4, step 4: determining the concentration of formamide in the triazole production recovery product according to the content of formamide in the liquid to be detected based on the drying proportion of the triazole production recovery product;
in step 3, based on a preset formamide peak signal, performing comparative analysis on the peak signal in the chromatogram, and determining the content of formamide in the liquid to be detected comprises the following steps:
extracting peak signals in the chromatogram to obtain a peak signal sequence, and acquiring a target peak signal sequence consistent with the preset formamide peak signal from the peak signal sequence;
extracting a chromatographic peak in the target peak signal sequence, and performing denoising processing on the chromatographic peak to obtain a denoised chromatographic peak;
comparing the peak signal intensity of the denoising chromatographic peak with the peak signal intensity of the preset formamide peak signal to obtain an intensity difference value, and judging whether the intensity difference value is within a preset difference value range;
if so, determining that the de-noised chromatographic peak is a pure peak and the corresponding substance is formamide, and acquiring a target signal curve corresponding to the de-noised chromatographic peak;
otherwise, determining the denoised chromatographic peak as a mixed peak;
when the denoised chromatographic peak is determined to be a mixed peak, obtaining the retention time of the denoised chromatographic peak, and comparing the retention time with the retention time of a comparison chromatographic peak to obtain a time difference value;
determining a formamide purity value determined by the denoising chromatographic peak based on the intensity difference value and the time difference value;
detecting the denoising chromatographic peak to obtain a signal curve of the denoising chromatographic peak, and marking a peak point in the signal curve to obtain a peak point label;
based on the formamide purity value determined by the denoising chromatographic peak, an adjusting scheme is obtained, and according to the adjusting scheme and based on the peak point label, the peak point in the signal curve is adjusted to obtain a target signal curve;
standardizing the target signal curve according to a contrast signal curve of a contrast chromatographic peak to obtain a standard signal curve;
calculating the peak area of the region surrounded by the target signal curve, and determining the content of formamide in the liquid to be detected based on the proportional relation between the content of formamide solution and the peak area;
calculating the peak area of the region enclosed by the target signal curve comprises:
inputting the target signal curve into a slope detection system, determining the slope corresponding to each peak in the target signal curve, eliminating the peak corresponding to the slope which is not in a first preset range, correcting the slope of the peak corresponding to the slope which is in a second preset range, and outputting a new target signal curve according to the elimination and correction results;
sampling the new target signal curve to obtain n acquisition graphs, and obtaining the peak area of the new target signal curve based on the n acquisition graphs;
the calculation formula of the peak area is as follows:
wherein A represents the peak area, ω represents the sampling frequency, n represents the number of sampling times and the number of acquisition patterns, s i Representing the side length of the ith collection graph, and tau representing the error of the sampling frequency value to the peak area determinationThe difference coefficient is (0.1, 0.5), A 1 Area of the 1 st acquisition pattern, A n Representing the area of the nth acquisition pattern;
generating a first target pattern spot based on the target signal curve, generating a second target pattern spot based on the new target signal curve, and superposing the first target pattern spot and the second target pattern spot to obtain a third target pattern spot;
acquiring the peak area reliability of the new target signal curve based on the areas of the first target pattern spot, the second target pattern spot and the third target pattern spot;
the calculation formula of the peak area reliability is as follows:
wherein δ represents the peak area reliability of the new target signal curve, D a Representing the first target spot area, D b Representing the second target spot area, D c Representing the third target spot area, wherein D c >D a ，D c >D b ；
Judging whether the peak area reliability is greater than a preset reliability;
if so, determining that the peak area of the new target signal curve can represent the content of formamide in the liquid to be detected;
and if not, correcting the new target curve again until the peak area reliability is greater than the preset reliability.
2. The on-line detection method for the concentration of formamide in a triazole production recycle according to claim 1, wherein in step 1, the triazole production recycle obtained by quantitative extraction production at preset time intervals is transmitted to a detection pool, and the method comprises the following steps:
establishing a dynamic model of the triazole production recycling material in the production process based on the operation parameters of the extraction device and a historical production database;
inputting quantitative values into the kinetic model, and determining target operating parameters of the extraction device;
and extracting the triazole production recycled material based on the target operation parameters, and conveying the extracted triazole production recycled material to the detection pool through a conveyor belt.
3. The on-line detection method for the concentration of formamide in the triazole production recycling substances according to claim 1, characterized in that in step 2, heating the triazole production recycling substances to a preset temperature to obtain the liquid to be detected comprises:
heating the detection pool according to a first temperature and a first heating time, and monitoring to obtain the state of a triazole production recycling substance in the detection pool when the heating in the first heating time is completed;
and setting a second temperature to heat the triazole production recovered substance based on the state until the triazole production recovered substance is completely melted into liquid, so as to obtain the liquid to be detected.
4. The on-line detection method for the concentration of formamide in a triazole production recycling substance according to claim 1, characterized in that in step 2, the liquid to be detected is injected into a liquid chromatograph, and the chromatogram obtained comprises:
injecting the liquid to be detected into a detection channel of the liquid chromatograph after being processed in advance to realize the separation of various substances in the liquid to be detected;
and acquiring the chromatogram of the liquid to be detected after a preset detection time.
5. The on-line detection method for the concentration of formamide in a triazole production recycle product according to claim 1, characterized in that before step 3, the method further comprises: determining the peak signals of formamide in the chromatogram by the following process:
injecting the obtained formamide solution into a detection channel of the liquid chromatograph in the same way as the triazole production recovered substance to obtain a contrast chromatogram;
recording the retention time, peak signal intensity and peak area of a contrast chromatogram peak in the contrast chromatogram;
determining the proportional relation between the formamide solution content and the peak area based on the peak area;
and taking the retention time and the peak signal intensity of the contrast chromatographic peak as a preset formamide peak signal.
6. The on-line detection method for the concentration of formamide in a triazole production recycle product according to claim 1, wherein the determination of the purity value of formamide determined by the de-noised chromatographic peak based on the intensity difference value and the time difference value comprises:
determining possible components of other substances in the mixed peak based on the intensity difference, and acquiring retention time of the possible components;
comparing the time difference with the retention time of the possible components, and selecting a target component in the possible components corresponding to the minimum time difference;
analyzing the de-noised chromatographic peak based on the standard peak signal intensity and the standard retention time of the target component to determine the ratio of the target component;
analyzing the de-noised chromatographic peak based on the peak signal intensity and retention time of formamide, and determining the purity value of the formamide;
and verifying the purity value based on the ratio, wherein if the verification is successful, the purity value is the purity value of the formamide determined by the de-noised chromatographic peak, otherwise, the purity value of the formamide is adjusted based on the ratio.
7. The on-line detection method for the concentration of formamide in a triazole production recycling product according to claim 1, wherein in step 4, determining the concentration of formamide in the triazole production recycling product according to the content of formamide in the liquid to be detected based on the drying ratio of the triazole production recycling product comprises:
analyzing the triazole production recovery product obtained by extraction and production, and determining the initial state of the triazole production recovery product;
determining the final state of the triazole production recovered material based on a preset process, and determining the process flow from the initial state to the final state;
acquiring a process example related to the process flow from a process database, and determining the change information of each component in the triazole production recovery before and after the process based on the process example;
determining the content change of each component before and after the process based on the change information, and setting a first weight value based on the content change;
determining the state change of formamide in the triazole production recycled material based on the change information, and setting a second weight value based on the state change;
determining a first total value of the triazole production recovered matter in a final state based on the quantitative value of the triazole production recovered matter obtained by extraction and production and the drying ratio of the triazole production recovered matter;
based on the first weight value and the second weight value, carrying out weighted calculation on the first total value to obtain a second total value;
determining a first content value of formamide corresponding to the content of the formamide in the liquid to be detected, and performing weighted calculation on the first content value based on the second weight value to obtain a second content value;
and calculating to obtain the concentration of formamide in the triazole production recycling material based on the second total value and the second content value.
8. An online detection system for formamide concentration in a triazole production recovery product is characterized by comprising:
the extraction and transmission module is used for quantitatively extracting the triazole production recovery substances obtained by production at intervals of preset time and transmitting the triazole production recovery substances to the detection pool;
the detection module is used for heating the triazole production recovered substance to a preset temperature to obtain liquid to be detected, and injecting the liquid to be detected into a liquid chromatograph to obtain a chromatogram;
the analysis module is used for carrying out comparison analysis on the peak signals in the chromatogram based on preset formamide peak signals to determine the content of formamide in the liquid to be detected;
the determining module is used for determining the concentration of formamide in the triazole production recovery product according to the content of formamide in the liquid to be detected based on the drying proportion of the triazole production recovery product;
the specific workflow of the analysis module is as follows:
extracting peak signals in the chromatogram to obtain a peak signal sequence, and acquiring a target peak signal sequence consistent with the preset formamide peak signal from the peak signal sequence;
extracting a chromatographic peak in the target peak signal sequence, and performing denoising processing on the chromatographic peak to obtain a denoised chromatographic peak;
comparing the peak signal intensity of the denoising chromatographic peak with the peak signal intensity of the preset formamide peak signal to obtain an intensity difference value, and judging whether the intensity difference value is within a preset difference value range;
if so, determining that the de-noised chromatographic peak is a pure peak and the corresponding substance is formamide, and acquiring a target signal curve corresponding to the de-noised chromatographic peak;
otherwise, determining the denoised chromatographic peak as a mixed peak;
when the denoised chromatographic peak is determined to be a mixed peak, obtaining the retention time of the denoised chromatographic peak, and comparing the retention time with the retention time of a comparison chromatographic peak to obtain a time difference value;
determining a formamide purity value determined by the denoising chromatographic peak based on the intensity difference value and the time difference value;
detecting the denoising chromatographic peak to obtain a signal curve of the denoising chromatographic peak, and marking a peak point in the signal curve to obtain a peak point label;
based on the formamide purity value determined by the denoising chromatographic peak, an adjusting scheme is obtained, and according to the adjusting scheme and based on the peak point label, the peak point in the signal curve is adjusted to obtain a target signal curve;
standardizing the target signal curve according to a contrast signal curve of a contrast chromatographic peak to obtain a standard signal curve;
calculating the peak area of the region surrounded by the target signal curve, and determining the content of formamide in the liquid to be detected based on the proportional relation between the content of formamide solution and the peak area;
calculating the peak area of the region enclosed by the target signal curve comprises:
inputting the target signal curve into a slope detection system, determining the slope corresponding to each peak in the target signal curve, eliminating the peak corresponding to the slope which is not in a first preset range, correcting the slope of the peak corresponding to the slope which is in a second preset range, and outputting a new target signal curve according to the elimination and correction results;
sampling the new target signal curve to obtain n acquisition graphs, and obtaining the peak area of the new target signal curve based on the n acquisition graphs;
the calculation formula of the peak area is as follows:
wherein A represents the peak area, ω represents the sampling frequency, n represents the number of sampling times and the number of collection patterns, s i The length of the side of the ith collection graph is shown, tau represents the error coefficient determined by the sampling frequency value to the peak area, the value is (0.1, 0.5), A 1 Denotes the area of the 1 st acquisition pattern, A n Representing the area of the nth acquisition pattern;
generating a first target pattern spot based on the target signal curve, generating a second target pattern spot based on the new target signal curve, and superposing the first target pattern spot and the second target pattern spot to obtain a third target pattern spot;
acquiring the peak area reliability of the new target signal curve based on the first target pattern spot area, the second target pattern spot area and the third target pattern spot area;
the calculation formula of the peak area reliability is as follows:
wherein δ represents the peak area reliability of the new target signal curve, D a Representing the first target spot area, D b Representing the second target spot area, D c Represents the third target spot area, wherein D c >D a ，D c >D b ；
Judging whether the peak area reliability is greater than a preset reliability;
if so, determining that the peak area of the new target signal curve can represent the content of formamide in the liquid to be detected;
otherwise, correcting the new target curve again until the peak area reliability is greater than the preset reliability.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210222156.9A CN114544818B (en) | 2022-03-09 | 2022-03-09 | Method and system for detecting concentration of formamide in triazole production recycling matter |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210222156.9A CN114544818B (en) | 2022-03-09 | 2022-03-09 | Method and system for detecting concentration of formamide in triazole production recycling matter |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114544818A CN114544818A (en) | 2022-05-27 |
| CN114544818B true CN114544818B (en) | 2022-09-13 |
Family
ID=81664254
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210222156.9A Active CN114544818B (en) | 2022-03-09 | 2022-03-09 | Method and system for detecting concentration of formamide in triazole production recycling matter |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114544818B (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3365931A (en) * | 1964-07-21 | 1968-01-30 | Exxon Research Engineering Co | Data processing system for a gas chromatograph |
| CN113516000A (en) * | 2021-01-13 | 2021-10-19 | 腾讯科技（深圳）有限公司 | Method, device and equipment for processing waveform image and storage medium |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2501003C (en) * | 2004-04-23 | 2009-05-19 | F. Hoffmann-La Roche Ag | Sample analysis to provide characterization data |
| CN106596814B (en) * | 2016-11-25 | 2018-01-26 | 大连达硕信息技术有限公司 | A kind of chromatographic peak quantitative analysis method in complicated LC-MS data |
| JP7386234B2 (en) * | 2018-08-31 | 2023-11-24 | ディーエイチ テクノロジーズ デベロップメント プライベート リミテッド | Identification and scoring of related compounds within complex samples |
| CN113552239A (en) * | 2020-04-25 | 2021-10-26 | 江苏天士力帝益药业有限公司 | Method for determining formamide content in temozolomide bulk drug |
| CN111739067A (en) * | 2020-05-28 | 2020-10-02 | 中国国土勘测规划院 | Remote sensing image change detection method and device |
-
2022
- 2022-03-09 CN CN202210222156.9A patent/CN114544818B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3365931A (en) * | 1964-07-21 | 1968-01-30 | Exxon Research Engineering Co | Data processing system for a gas chromatograph |
| CN113516000A (en) * | 2021-01-13 | 2021-10-19 | 腾讯科技（深圳）有限公司 | Method, device and equipment for processing waveform image and storage medium |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114544818A (en) | 2022-05-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US10919791B2 (en) | Intelligent identification method of sludge bulking based on type-2 fuzzy neural network | |
| CN101576956B (en) | On-line character detection method based on machine vision and system thereof | |
| US20140358465A1 (en) | Yield analysis system and method using sensor data of fabrication equipment | |
| CN105334185B (en) | The near-infrared model maintaining method differentiated based on spectrum projection | |
| CN104132967B (en) | A kind of light concentration gas detection method based on dual threshold accidental resonance | |
| Yu et al. | Identification of wine according to grape variety using near-infrared spectroscopy based on radial basis function neural networks and least-squares support vector machines | |
| CN111272686B (en) | Hyperspectral detection method for iron grade of iron ore concentrate powder | |
| CN104680185A (en) | Hyperspectral image classification method based on boundary point reclassification | |
| CN114544818B (en) | Method and system for detecting concentration of formamide in triazole production recycling matter | |
| CN115420707A (en) | Sewage near infrared spectrum chemical oxygen demand assessment method and system | |
| CN112651173B (en) | Agricultural product quality nondestructive testing method based on cross-domain spectral information and generalizable system | |
| CN117193178B (en) | Production process optimization control method and system for glass fiber composite board | |
| CN103234923A (en) | On-line monitoring method of total sugar content during yellow wine fermentation process | |
| CN108376266A (en) | One-class support vector machines Optimization Method of Kernel Parameter based on sample edge point internal point | |
| CN117171655A (en) | Intelligent judging method and device for coal mine production state based on spectrum analysis | |
| CN113406037B (en) | Infrared spectrum online rapid identification analysis method based on sequence forward selection | |
| CN113252641B (en) | Substance identification method based on residual analysis under Raman spectrum | |
| CN114488595A (en) | Substrate cutting method and system | |
| CN112949169B (en) | Coal sample test value prediction method based on spectral analysis | |
| CN115169832A (en) | Sensitivity analysis method and system based on curve form change | |
| CN115436342A (en) | Method and device for reducing LIBS detection uncertainty among multiple batches of samples | |
| CN113791062A (en) | Method for judging fixed substance type based on Raman spectrum | |
| CN113567417A (en) | Method for identifying peanut oil production place based on Raman spectrum fingerprint analysis technology | |
| CN104049624A (en) | Chemical product production mode optimization method and device and continuous type chemical system | |
| CN114611582B (en) | Method and system for analyzing substance concentration based on near infrared spectrum technology |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |