Intelligent control method for detecting organic chlorine in industrial hydrochloric acid
Patent Information
- Application Number
- CN202411644973.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-18
- Publication Date
- 2025-03-14
AI Technical Summary
The existing organic chlorine detection methods in industrial hydrochloric acid have the problem of artificially distinguishing the chromatograms produced before and after ultraviolet photolysis, and electrodialysis and ultraviolet photolysis devices require artificial judgment on whether they can continue to be used or whether the conditions are set appropriately, and the pre-processing stability cannot be ensured.
By installing resistivity sensors and pressure sensors, combined with the control system to monitor the membrane performance, ensure stability of electrodialysis pre-processing; use light intensity sensors to automatically adjust the power output of the ultraviolet light source to ensure stability of the ultraviolet light pre-processing; realize automatic control of electrodialysis and ultraviolet light solution devices, reduce manual operation, and improve work efficiency.
It realizes intelligent distinction of chromatograms generated before and after ultraviolet photolysis, reduces manual operation errors, ensures the stability of electrodialysis and ultraviolet photolysis pretreatment, and improves detection work efficiency.
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Figure CN119619386A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of ion chromatography detection, and in particular to an intelligent control method for detecting organic chlorine in industrial hydrochloric acid. Background Art
[0002] Industrial hydrochloric acid is usually used as the regeneration agent for cationic resins in the desalted water system and condensate purification system of nuclear power plants. When the cationic resin reaches saturation, the concentrated acid solution is passed through the resin bed through reverse flow, so that the cations on the resin are replaced by hydrogen ions, thereby achieving resin regeneration. This process not only removes the impurities accumulated on the resin, but also restores the resin's selective adsorption capacity for cations. Therefore, the quality of hydrochloric acid will affect the purification effect of the resin bed. However, due to reasons such as the production process of hydrochloric acid, it contains a large amount of organic chlorine.
[0003] After the cation bed is regenerated using this hydrochloric acid, the flushing process cannot completely flush out the residual regeneration liquid. After commissioning, the hydrochloric acid chloride ions in the residual regeneration liquid are adsorbed by the mixed bed, and the organic chlorine is adsorbed by the mixed bed and then quickly desorbed, entering the condensate and feed water, and then degraded at high temperature in the steam generator, releasing chloride ions, causing the steam generator wastewater quality to deviate. The chloride ions exceeding the control requirements will increase the risk of stress corrosion cracking of the steam generator heat transfer tubes, indirectly increasing potential safety risks.
[0004] As an efficient, rapid and highly automated separation and detection technology, ion chromatography has been widely used in the analysis of inorganic anions and cations. However, it is not common to directly use ion chromatography to determine organochlorine in hydrochloric acid, because most organochlorine compounds are not easy to ionize and need to be converted into a detectable form through derivatization or other conversion methods.
[0005] Patent CN202311224870.2 discloses a method for detecting organic chlorine in industrial hydrochloric acid, which includes: step one: using an electrodialysis method to remove inorganic chlorine contained in an industrial hydrochloric acid sample to obtain an industrial hydrochloric acid sample from which inorganic chlorine has been removed; then using an ion chromatography detection method to detect the inorganic chlorine content of the industrial hydrochloric acid sample from which inorganic chlorine has been removed to obtain a first chloride ion content value; step two: using an ultraviolet photolysis method to degrade the organic chlorine components in the industrial hydrochloric acid into inorganic chloride ions using the industrial hydrochloric acid sample from which inorganic chlorine has been removed to obtain a degraded industrial hydrochloric acid sample; step three: using an ion chromatography detection method to detect the inorganic chlorine content of the degraded industrial hydrochloric acid sample to obtain a second chloride ion content value; and converting the difference between the second chloride ion content value and the first chloride ion content value to obtain the content of the organic chlorine components in the industrial hydrochloric acid. However, on the one hand, when using the existing chromatography workstation, it is impossible to distinguish which spectra are produced before ultraviolet photolysis and which are produced after ultraviolet photolysis. It is easy to make mistakes when distinguishing them manually and performing spectrum calculations. On the other hand, electrodialysis devices and ultraviolet photolysis devices require manual judgment whether they can continue to be used or whether the setting conditions are appropriate. Summary of the invention
[0006] One of the purposes of the present invention is to provide an intelligent control method for detecting organochlorine in industrial hydrochloric acid, so as to solve the problems of artificially distinguishing the chromatograms produced before and after ultraviolet photolysis and prone to errors in chromatogram calculation in the existing method for detecting organochlorine in industrial hydrochloric acid, and to realize intelligent distinction of the chromatograms produced before and after ultraviolet photolysis.
[0007] The second object of the present invention is to provide an intelligent control method for detecting organochlorine in industrial hydrochloric acid, so as to solve the problem that the electrodialysis device and the ultraviolet photolysis device in the existing method for detecting organochlorine in industrial hydrochloric acid need manual judgment on whether they can continue to be used or whether the setting conditions are appropriate, and the stability of the electrodialysis and ultraviolet photolysis pretreatment cannot be ensured, and the automatic control of the electrodialysis device and the ultraviolet photolysis device is realized to ensure the stability of the electrodialysis and ultraviolet photolysis pretreatment.
[0008] In order to achieve the above object, the present invention provides the following technical solutions:
[0009] An intelligent control method for detecting organochlorine in industrial hydrochloric acid comprises the following steps:
[0010] Step 1: Electrodialysis pretreatment: Use sensor technology to monitor membrane performance, warn of membrane contamination or failure, and automatically trigger cleaning procedures or replace membrane components when membrane flux drops to a certain level;
[0011] Step 2, UV photolysis pre-treatment: automatically adjust the power output of the UV light source according to the preset photolysis efficiency target and the current organic chlorine concentration;
[0012] Step 3: Ion chromatography detection: standard sample injection and unknown sample injection.
[0013] As one possible approach, in step 1, the membrane performance is monitored using sensing technology, including:
[0014] Install a resistivity sensor at the inlet, outlet or inside the membrane stack of the electrodialysis device;
[0015] The resistivity sensor measures the resistance of the solution in real time based on the conductive properties of the solution and converts it into an electrical signal for transmission to the control system;
[0016] The control system compares the resistance value of the solution with a preset standard value or historical trend; when the resistance value of the solution is higher than the set standard value or historical trend, the control system automatically triggers an alarm mechanism and the operator performs inspection or maintenance.
[0017] As one possible implementation, the resistivity sensor is a contact resistivity sensor or a non-contact resistivity sensor.
[0018] As one possible approach, in step 1, the membrane performance is monitored using sensing technology, including:
[0019] Install pressure sensors at the water inlet and outlet ends of the membrane stack of the electrodialysis device;
[0020] The pressure sensor measures the pressure drop of the solution before and after passing through the membrane stack in real time and converts it into an electrical signal to be transmitted to the control system;
[0021] When the pressure drop of the solution before and after passing through the membrane stack exceeds the set threshold, the control system automatically triggers an alarm, prompting the operator to check the operating status of the electrodialysis device and perform cleaning or maintenance in a timely manner.
[0022] As one of the achievable methods, step 2, automatically adjusting the power output of the ultraviolet light source, includes:
[0023] Install a light intensity sensor inside or near the UV photolysis device;
[0024] The light intensity sensor monitors the UV intensity of the UV light source in real time and transmits it to the control system;
[0025] When the ultraviolet intensity of the ultraviolet light source is lower than the set threshold, the control system increases the power supply through closed-loop control to improve the power output of the ultraviolet light source; when the ultraviolet intensity of the ultraviolet light source is higher than the set threshold, the control system reduces the power supply through closed-loop control to reduce the power output of the ultraviolet light source.
[0026] As one possible implementation method, in step 3, the standard sample injection includes the following steps:
[0027] (1) Method editing: chromatographic methods and processing methods;
[0028] (2) Sample Editing: Set the standard sample name, select the standard sample chromatographic method, set the standard sample injection well position information, standard sample calibration level and standard sample injection volume;
[0029] (3) Checking the instrument status: When starting the sequence, check whether the current status of the instrument is in an operational state or in an abnormal state;
[0030] (4) Sending the chromatography method: sending the pre-processing module setting parameters and the ion chromatograph setting parameters to the lower computer, setting the analysis parameters, and the electrodialysis device and the ultraviolet photolysis device executing the standard sample injection mode;
[0031] (5) Waiting for acquisition: When the valve state is switched after the injection is completed, a valve cut signal is transmitted, and the system starts to acquire spectra after detecting the trigger signal;
[0032] (6) Start acquisition: After receiving the trigger signal, the instrument starts timing the acquisition signal to generate a spectrum. When the acquisition time is up, the acquisition ends.
[0033] (7) Chromatographic peak identification: Chromatographic peaks are identified by setting integration parameters and peaks are judged by calculating slope curvature algorithm;
[0034] (8) Qualitative and quantitative calculations: The compound retention time set in the calibration method is compared with the retention time of the identified chromatographic peak to qualitatively identify the chromatographic peak. When the last standard sample is injected, the grade information set in the series is associated with the compound concentration level table to automatically calculate the calibration curve.
[0035] As one of the feasible ways, in the standard sample injection, the chromatographic method includes basic information setting, pre-treatment module setting and ion chromatograph setting;
[0036] Basic information settings include setting the chromatographic column model and analysis time;
[0037] The pre-treatment module includes an electrodialysis device pre-treatment module and an ultraviolet photolysis device pre-treatment module. The electrodialysis device pre-treatment module settings include setting sample type, electrodialysis pump speed, electrodialysis pump volume and electrodialysis time. The ultraviolet photolysis device pre-treatment module settings include setting sample type, ultraviolet photolysis pump speed, ultraviolet photolysis pump volume, metering pump flow, constant current source current, photolysis time, injection pump speed, injection volume and cleaning parameters.
[0038] Ion chromatograph settings include setting the pump flow rate, suppressor current, eluent concentration, and column oven temperature;
[0039] The processing methods include setting integration parameters, editing compound information, making calibration curves and editing print templates.
[0040] As one of the feasible methods, unknown sample injection includes the following steps:
[0041] (1) Method editing: chromatographic methods and processing methods;
[0042] (2) Sample editing: set the unknown sample name, select the unknown sample chromatographic method, set the unknown sample injection well information, unknown sample calibration level and unknown sample injection volume;
[0043] (3) Checking the instrument status: When starting the running sequence, first check whether the current status of the instrument is in an operational state or in an abnormal state;
[0044] (4) Sending the chromatography method: sending the pre-processing module setting parameters, cleaning parameters and ion chromatograph setting parameters to the lower computer, setting the analysis parameters, and the electrodialysis device and the ultraviolet photolysis device to execute the unknown sample injection mode;
[0045] (5) Waiting for acquisition: When the valve state is switched after the injection is completed, a valve cut signal is transmitted, and the system starts to acquire spectra after detecting the trigger signal;
[0046] (6) Start acquisition: After receiving the trigger signal, the instrument starts timing the acquisition signal to generate a spectrum. When the acquisition time is up, the acquisition ends.
[0047] (7) Cleaning: After the two injections are completed, the electrodialysis device and the UV photolysis device begin to perform the cleaning process, and the default is one empty position cleaning;
[0048] (8) Chromatographic peak identification: Chromatographic peaks are identified by setting integration parameters and peaks are judged by calculating slope curvature algorithm;
[0049] (9) Qualitative and quantitative calculation: In the calibration method, the compound retention time is set to compare with the retention time of the identified chromatographic peak, the chromatographic peak is qualitatively analyzed, and the calibration curve is called to perform quantitative calculation on the chromatographic peak. After calculating the chloride ion concentration, the second calculated concentration minus the first calculated concentration is the organic chlorine concentration.
[0050] As one of the feasible ways, in the unknown sample injection, the chromatographic method includes basic information setting, pre-treatment module setting and ion chromatograph setting;
[0051] Basic information settings include setting the chromatographic column model and analysis time;
[0052] The pre-treatment module includes an electrodialysis device pre-treatment module and an ultraviolet photolysis device pre-treatment module. The electrodialysis device pre-treatment module settings include setting sample type, electrodialysis pump speed, electrodialysis pump volume and electrodialysis time. The ultraviolet photolysis device pre-treatment module settings include setting sample type, ultraviolet photolysis pump speed, ultraviolet photolysis pump volume, metering pump flow, constant current source current, photolysis time, injection pump speed, injection volume and cleaning parameters.
[0053] Ion chromatograph settings include setting the pump flow rate, suppressor current, eluent concentration, and column oven temperature;
[0054] The processing methods include setting integration parameters, editing compound information, making calibration curves and editing print templates.
[0055] As one feasible method, during the injection of an unknown sample, in step (6), during the start of collection, one sample analysis will trigger two collection signals, namely, the sample injection collection signal before ultraviolet photolysis, and the sample injection collection signal after the ultraviolet photolysis is completed. After receiving the trigger collection signal, the electrodialysis device and the ultraviolet photolysis device record the number of triggering times.
[0056] Beneficial technical effects of the present invention:
[0057] The intelligent control method for detecting organic chlorine in industrial hydrochloric acid of the present invention uses a resistivity sensor and a pressure sensor in conjunction with a control system to monitor membrane performance, thereby ensuring that the electrodialysis pretreatment process is stable; uses a light intensity sensor in conjunction with a control system to automatically adjust the power output of an ultraviolet light source, thereby ensuring that the ultraviolet photolysis pretreatment is stable; automatically completes sample processing, detection and data analysis, thereby greatly reducing manual operation links and improving work efficiency; one sample analysis triggers two acquisition signals, namely, a sample injection acquisition signal before ultraviolet photolysis and a sample injection acquisition signal after ultraviolet photolysis is completed; after receiving the trigger acquisition signal, an electrodialysis device and an ultraviolet photolysis device record the number of triggers, and intelligent acquisition replaces manual distinction, thereby further improving work efficiency. BRIEF DESCRIPTION OF THE DRAWINGS
[0058] Figure 1 It is a flow chart of an embodiment of the intelligent control method for detecting organic chlorine in industrial hydrochloric acid of the present invention;
[0059] Figure 2 Schematic diagram of the process for standard sample injection;
[0060] Figure 3 Schematic diagram of the process for injecting an unknown sample. DETAILED DESCRIPTION
[0061] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by technicians in the technical field to which this application belongs; the terms used in the specification of the application are only for the purpose of describing specific embodiments and are not intended to limit this application; the terms "including" and "having" and any variations thereof in the specification and claims of this application and the above-mentioned figure descriptions are intended to cover non-exclusive inclusions.
[0062] Reference to "embodiments" herein means that a particular feature, structure, or characteristic described in conjunction with the embodiments may be included in at least one embodiment of the present application. The appearance of the phrase in various locations in the specification does not necessarily refer to the same embodiment, nor is it an independent or alternative embodiment that is mutually exclusive with other embodiments. It is explicitly and implicitly understood by those skilled in the art that the embodiments described herein may be combined with other embodiments.
[0063] The technical solution of the present invention is clearly and completely described below in conjunction with the accompanying drawings and specific embodiments.
[0064] The existing method for detecting organochlorine in industrial hydrochloric acid includes the following steps:
[0065] Step 1: removing inorganic chlorine contained in the industrial hydrochloric acid sample by an electrodialysis device to obtain an industrial hydrochloric acid sample from which inorganic chlorine is removed; then detecting the inorganic chlorine content of the industrial hydrochloric acid sample from which inorganic chlorine is removed by an ion chromatograph to obtain a first chloride ion content value;
[0066] Step 2: degrading the organic chlorine in the industrial hydrochloric acid sample from which the inorganic chlorine has been removed into inorganic chloride ions by a UV photolysis device to obtain a degraded industrial hydrochloric acid sample;
[0067] Step three: Detect the inorganic chlorine content of the degraded industrial hydrochloric acid sample by ion chromatography to obtain a second chloride ion content value; and convert the content of organic chlorine components in the industrial hydrochloric acid according to the difference between the second chloride ion content value and the first chloride ion content value.
[0068] The existing methods for detecting organochlorine in industrial hydrochloric acid have the following problems: However, on the one hand, when using an ion chromatograph, it is impossible to distinguish which spectra are produced before ultraviolet photolysis and which are produced after ultraviolet photolysis. It is easy to make mistakes when distinguishing them manually and performing spectrum calculations; on the other hand, electrodialysis devices and ultraviolet photolysis devices require manual judgment on whether they can continue to be used or whether the setting conditions are appropriate.
[0069] refer to Figure 1 , shows a flow chart of an embodiment of an intelligent control method for detecting organochlorine in industrial hydrochloric acid, the intelligent control method for detecting organochlorine in industrial hydrochloric acid comprising the following steps:
[0070] Step 1: Electrodialysis pretreatment: Use sensor technology to monitor membrane performance, warn of membrane contamination or failure, and automatically trigger cleaning procedures or replace membrane components when membrane flux drops to a certain level;
[0071] Step 2, UV photolysis pre-treatment: according to the preset photolysis efficiency target and the current organic chlorine concentration, the power output of the UV light source is automatically adjusted to ensure that sufficient photolysis energy is used to convert the organic chlorine into detectable inorganic chlorine;
[0072] Step 3: Ion chromatography detection: standard sample injection and unknown sample injection.
[0073] In this embodiment, as one of the achievable methods, in step 1, the membrane performance is monitored using sensing technology, including:
[0074] Install a resistivity sensor at the inlet, outlet or inside the membrane stack of the electrodialysis device;
[0075] The resistivity sensor measures the resistance of the solution in real time based on the conductive properties of the solution and converts it into an electrical signal for transmission to the control system;
[0076] The control system compares the resistance value of the solution with a preset standard value or historical trend; when the resistance value of the solution is higher than the set standard value or historical trend, the control system automatically triggers an alarm mechanism and the operator performs inspection or maintenance.
[0077] In this embodiment, as one of the achievable ways, the resistivity sensor is a contact resistivity sensor or a non-contact resistivity sensor.
[0078] In this embodiment, as one of the achievable methods, in step 1, the membrane performance is monitored using sensing technology, including:
[0079] Install pressure sensors at the water inlet and outlet ends of the membrane stack of the electrodialysis device;
[0080] The pressure sensor measures the pressure drop of the solution before and after passing through the membrane stack in real time and converts it into an electrical signal to be transmitted to the control system;
[0081] When the pressure drop of the solution before and after passing through the membrane stack exceeds the set threshold, the control system automatically triggers an alarm, prompting the operator to check the operating status of the electrodialysis device and perform cleaning or maintenance in a timely manner.
[0082] In this embodiment, as one of the achievable methods, step 2, automatically adjusting the power output of the ultraviolet light source, includes:
[0083] Install a light intensity sensor inside or near the UV photolysis device;
[0084] The light intensity sensor monitors the UV intensity of the UV light source in real time and transmits it to the control system;
[0085] When the ultraviolet intensity of the ultraviolet light source is lower than the set threshold, the control system increases the power supply through closed-loop control to improve the power output of the ultraviolet light source; when the ultraviolet intensity of the ultraviolet light source is higher than the set threshold, the control system reduces the power supply through closed-loop control to reduce the power output of the ultraviolet light source.
[0086] See also Figure 2 In this embodiment, as one of the achievable methods, in step 3, the standard sample injection includes the following steps:
[0087] (1) Method editing: chromatographic methods and processing methods;
[0088] (2) Sample Editing: Set the standard sample name, select the standard sample chromatographic method, set the standard sample injection well position information, standard sample calibration level and standard sample injection volume;
[0089] (3) Checking the instrument status: When starting the sequence, check whether the current status of the instrument is in an operational state or in an abnormal state;
[0090] (4) Sending the chromatography method: sending the pre-processing module setting parameters and the ion chromatograph setting parameters to the lower computer, setting the analysis parameters, and the electrodialysis device and the ultraviolet photolysis device executing the standard sample injection mode;
[0091] (5) Waiting for acquisition: When the valve state is switched after the injection is completed, a valve cut signal is transmitted, and the system starts to acquire spectra after detecting the trigger signal;
[0092] (6) Start acquisition: After receiving the trigger signal, the instrument starts timing the acquisition signal to generate a spectrum. When the acquisition time is up, the acquisition ends.
[0093] (7) Chromatographic peak identification: Chromatographic peaks are identified by setting integration parameters and peaks are judged by calculating slope curvature algorithm;
[0094] (8) Qualitative and quantitative calculations: The compound retention time set in the calibration method is compared with the retention time of the identified chromatographic peak to qualitatively identify the chromatographic peak. When the last standard sample is injected, the grade information set in the series is associated with the compound concentration level table to automatically calculate the calibration curve.
[0095] In this embodiment, as one of the achievable methods, in the standard sample injection, the chromatographic method includes basic information setting, pre-processing module setting and ion chromatograph setting;
[0096] Basic information settings include setting the chromatographic column model and analysis time;
[0097] The pre-treatment module includes an electrodialysis device pre-treatment module and an ultraviolet photolysis device pre-treatment module. The electrodialysis device pre-treatment module settings include setting sample type, electrodialysis pump speed, electrodialysis pump volume and electrodialysis time. The ultraviolet photolysis device pre-treatment module settings include setting sample type, ultraviolet photolysis pump speed, ultraviolet photolysis pump volume, metering pump flow, constant current source current, photolysis time, injection pump speed, injection volume and cleaning parameters.
[0098] Ion chromatograph settings include setting the pump flow rate, suppressor current, eluent concentration, and column oven temperature;
[0099] The processing methods include setting integration parameters, editing compound information, making calibration curves and editing print templates.
[0100] See also Figure 3 In this embodiment, as one of the feasible methods, unknown sample injection includes the following steps:
[0101] (1) Method editing: chromatographic methods and processing methods;
[0102] (2) Sample editing: set the unknown sample name, select the unknown sample chromatographic method, set the unknown sample injection well information, unknown sample calibration level and unknown sample injection volume;
[0103] (3) Checking the instrument status: When starting the running sequence, first check whether the current status of the instrument is in an operational state or in an abnormal state;
[0104] (4) Sending the chromatography method: sending the pre-processing module setting parameters, cleaning parameters and ion chromatograph setting parameters to the lower computer, setting the analysis parameters, and the electrodialysis device and the ultraviolet photolysis device to execute the unknown sample injection mode;
[0105] (5) Waiting for acquisition: When the valve state is switched after the injection is completed, a valve cut signal is transmitted, and the system starts to acquire spectra after detecting the trigger signal;
[0106] (6) Start acquisition: After receiving the trigger signal, the instrument starts timing the acquisition signal to generate a spectrum. When the acquisition time is up, the acquisition ends.
[0107] (7) Cleaning: After the two injections are completed, the electrodialysis device and the UV photolysis device begin to perform the cleaning process, and the default is one empty position cleaning;
[0108] (8) Chromatographic peak identification: Chromatographic peaks are identified by setting integration parameters and peaks are judged by calculating slope curvature algorithm;
[0109] (9) Qualitative and quantitative calculation: In the calibration method, the compound retention time is set to compare with the retention time of the identified chromatographic peak, the chromatographic peak is qualitatively analyzed, and the calibration curve is called to perform quantitative calculation on the chromatographic peak. After calculating the chloride ion concentration, the second calculated concentration minus the first calculated concentration is the organic chlorine concentration.
[0110] In this embodiment, as one of the achievable methods, in the unknown sample injection, the chromatographic method includes basic information setting, pre-processing module setting and ion chromatograph setting;
[0111] Basic information settings include setting the chromatographic column model and analysis time;
[0112] The pre-treatment module includes an electrodialysis device pre-treatment module and an ultraviolet photolysis device pre-treatment module. The electrodialysis device pre-treatment module settings include setting sample type, electrodialysis pump speed, electrodialysis pump volume and electrodialysis time. The ultraviolet photolysis device pre-treatment module settings include setting sample type, ultraviolet photolysis pump speed, ultraviolet photolysis pump volume, metering pump flow, constant current source current, photolysis time, injection pump speed, injection volume and cleaning parameters.
[0113] Ion chromatograph settings include setting the pump flow rate, suppressor current, eluent concentration, and column oven temperature;
[0114] The processing methods include setting integration parameters, editing compound information, making calibration curves and editing print templates.
[0115] In this embodiment, as one of the feasible methods, during the injection of an unknown sample, in step (6), during the start of collection, one sample analysis will trigger two collection signals, namely, the sample injection collection signal before ultraviolet photolysis, and the sample injection collection signal after the ultraviolet photolysis is completed. After receiving the trigger collection signal, the electrodialysis device and the ultraviolet photolysis device record the number of triggering times.
[0116] The above-mentioned embodiments only express several implementation methods of the present invention, and the description thereof is relatively specific and detailed, but it cannot be understood as limiting the scope of the patent of the present invention. It should be pointed out that, for ordinary technicians in this field, several variations and improvements can be made without departing from the concept of the present invention, which all belong to the protection scope of the present invention. Therefore, the protection scope of the patent of the present invention shall be subject to the attached claims.
Claims
1. An intelligent control method for detecting organochlorine in industrial hydrochloric acid, characterized in that: The steps include: Step 1: Electrodialysis pretreatment: Use sensor technology to monitor membrane performance, warn of membrane contamination or failure, and automatically trigger cleaning procedures or replace membrane components when membrane flux drops to a certain level; Step 2, UV photolysis pre-treatment: automatically adjust the power output of the UV light source according to the preset photolysis efficiency target and the current organic chlorine concentration; Step 3: Ion chromatography detection: standard sample injection and unknown sample injection.
2. The intelligent control method for detecting organic chlorine in industrial hydrochloric acid according to claim 1, characterized in that: In step 1, membrane performance is monitored using sensing technology, including: Install a resistivity sensor at the inlet, outlet or inside the membrane stack of the electrodialysis device; The resistivity sensor measures the resistance of the solution in real time based on the conductive properties of the solution and converts it into an electrical signal for transmission to the control system; The control system compares the resistance value of the solution with a preset standard value or historical trend; when the resistance value of the solution is higher than the set standard value or historical trend, the control system automatically triggers an alarm mechanism and the operator performs inspection or maintenance.
3. The intelligent control method for detecting organic chlorine in industrial hydrochloric acid according to claim 2, characterized in that: The resistivity sensor is a contact resistivity sensor or a non-contact resistivity sensor.
4. The intelligent control method for detecting organic chlorine in industrial hydrochloric acid according to claim 1, characterized in that: In step 1, membrane performance is monitored using sensing technology, including: Install pressure sensors at the water inlet and outlet ends of the membrane stack of the electrodialysis device; The pressure sensor measures the pressure drop of the solution before and after passing through the membrane stack in real time and converts it into an electrical signal to be transmitted to the control system; When the pressure drop of the solution before and after passing through the membrane stack exceeds the set threshold, the control system automatically triggers an alarm, prompting the operator to check the operating status of the electrodialysis device and perform cleaning or maintenance in a timely manner.
5. The intelligent control method for detecting organic chlorine in industrial hydrochloric acid according to claim 1, characterized in that: Step 2, automatically adjusting the power output of the ultraviolet light source, including: Install a light intensity sensor inside or near the UV photolysis device; The light intensity sensor monitors the UV intensity of the UV light source in real time and transmits it to the control system; When the ultraviolet intensity of the ultraviolet light source is lower than the set threshold, the control system increases the power supply through closed-loop control to improve the power output of the ultraviolet light source; when the ultraviolet intensity of the ultraviolet light source is higher than the set threshold, the control system reduces the power supply through closed-loop control to reduce the power output of the ultraviolet light source.
6. The intelligent control method for detecting organic chlorine in industrial hydrochloric acid according to claim 1, characterized in that: In step 3, the standard sample is injected, including the following steps: (1) Method editing: chromatographic methods and processing methods; (2) Sample Editing: Set the standard sample name, select the standard sample chromatographic method, set the standard sample injection well information, standard sample calibration level and standard sample injection volume; (3) Checking the instrument status: When starting the sequence, check whether the current status of the instrument is in an operational state or in an abnormal state; (4) Sending the chromatography method: sending the pre-processing module setting parameters and the ion chromatograph setting parameters to the lower computer, setting the analysis parameters, and the electrodialysis device and the ultraviolet photolysis device executing the standard sample injection mode; (5) Waiting for acquisition: When the valve state is switched after the injection is completed, a valve cut signal is transmitted, and the system starts to acquire spectra after detecting the trigger signal; (6) Start acquisition: After receiving the trigger signal, the instrument starts timing the acquisition signal to generate a spectrum. When the acquisition time is up, the acquisition ends. (7) Chromatographic peak identification: Chromatographic peaks are identified by setting the integral parameters and the peaks are judged by calculating the slope curvature algorithm; (8) Qualitative and quantitative calculations: The compound retention time set in the calibration method is compared with the retention time of the identified chromatographic peak to qualitatively identify the chromatographic peak. When the last standard sample is injected, the grade information set in the series is associated with the compound concentration level table to automatically calculate the calibration curve.
7. The intelligent control method for detecting organic chlorine in industrial hydrochloric acid according to claim 6, characterized in that: In standard sample injection, the chromatographic method includes basic information settings, pre-treatment module settings, and ion chromatograph settings; Basic information settings include setting the chromatographic column model and analysis time; The pre-treatment module includes an electrodialysis device pre-treatment module and an ultraviolet photolysis device pre-treatment module. The electrodialysis device pre-treatment module settings include setting sample type, electrodialysis pump speed, electrodialysis pump volume and electrodialysis time. The ultraviolet photolysis device pre-treatment module settings include setting sample type, ultraviolet photolysis pump speed, ultraviolet photolysis pump volume, metering pump flow, constant current source current, photolysis time, injection pump speed, injection volume and cleaning parameters. Ion chromatograph settings include setting the pump flow rate, suppressor current, eluent concentration, and column oven temperature; The processing methods include setting integration parameters, editing compound information, making calibration curves and editing print templates.
8. The intelligent control method for detecting organic chlorine in industrial hydrochloric acid according to claim 1, characterized in that: The injection of unknown samples includes the following steps: (1) Method editing: chromatographic methods and processing methods; (2) Sample editing: set the unknown sample name, select the unknown sample chromatographic method, set the unknown sample injection well information, unknown sample calibration level and unknown sample injection volume; (3) Checking the instrument status: When starting the sequence, first check whether the current status of the instrument is in an operational state or in an abnormal state; (4) Sending the chromatography method: sending the pre-processing module setting parameters, cleaning parameters and ion chromatograph setting parameters to the lower computer, setting the analysis parameters, and the electrodialysis device and the ultraviolet photolysis device to execute the unknown sample injection mode; (5) Waiting for acquisition: When the valve state is switched after the injection is completed, a valve cut signal is transmitted, and the system starts to acquire spectra after detecting the trigger signal; (6) Start acquisition: After receiving the trigger signal, the instrument starts timing the acquisition signal to generate a spectrum. When the acquisition time is up, the acquisition ends. (7) Cleaning: After the two injections are completed, the electrodialysis device and the UV photolysis device begin to perform the cleaning process, and the default is one empty position cleaning; (8) Chromatographic peak identification: Chromatographic peaks are identified by setting integration parameters and peaks are judged by calculating slope curvature algorithm; (9) Qualitative and quantitative calculation: In the calibration method, the compound retention time is set to compare with the retention time of the identified chromatographic peak, the chromatographic peak is qualitatively analyzed, and the calibration curve is called to perform quantitative calculation on the chromatographic peak. After calculating the chloride ion concentration, the second calculated concentration minus the first calculated concentration is the organic chlorine concentration.
9. The intelligent control method for detecting organic chlorine in industrial hydrochloric acid according to claim 8, characterized in that: In the unknown sample injection, the chromatographic method includes basic information settings, pre-treatment module settings and ion chromatograph settings; Basic information settings include setting the chromatographic column model and analysis time; The pre-treatment module includes an electrodialysis device pre-treatment module and an ultraviolet photolysis device pre-treatment module. The electrodialysis device pre-treatment module settings include setting sample type, electrodialysis pump speed, electrodialysis pump volume and electrodialysis time. The ultraviolet photolysis device pre-treatment module settings include setting sample type, ultraviolet photolysis pump speed, ultraviolet photolysis pump volume, metering pump flow, constant current source current, photolysis time, injection pump speed, injection volume and cleaning parameters. Ion chromatograph settings include setting the pump flow rate, suppressor current, eluent concentration, and column oven temperature; The processing methods include setting integration parameters, editing compound information, making calibration curves and editing print templates.
10. The intelligent control method for detecting organic chlorine in industrial hydrochloric acid according to claim 8, characterized in that: During the injection of an unknown sample, step (6), when the collection begins, one sample analysis will trigger two collection signals, namely, the sample injection collection signal before ultraviolet photolysis and the sample injection collection signal after the ultraviolet photolysis is completed. After receiving the trigger collection signal, the electrodialysis device and the ultraviolet photolysis device record the number of triggering times.
Citation Information
Patent Citations
Method for detecting organochlorine in industrial hydrochloric acid
CN117129620A