Online analyzer for sulfite in electrogilding bath solution

Abstract

The embodiment of the invention provides an online analyzer for sulfite in an electrogilding bath solution, and relates to the field of chemical detection equipment. The online analyzer comprises a case, a multi-channel valve group, a reaction cup, an injection pump, a dual-wavelength colorimetric sensor, a peristaltic pump and a two-position three-way electromagnetic valve are mounted in the case, a stirring mechanism is arranged in the reaction cup, the reaction cup is connected with the multi-channel valve group through a pipeline, the injection pump is connected to the reaction cup through an independent pipeline, and the dual-wavelength colorimetric sensor is connected with the two-position three-way electromagnetic valve. The method is used for controlling and adding the iodine titration solution into the reaction cup. Through the integrated application of the multi-channel valve group, the reaction cup, the injection pump, the dual-wavelength colorimetric sensor, the peristaltic pump and the two-position three-way electromagnetic valve, the full-process automatic operation from automatic sampling to analysis is realized, so that the labor cost is greatly saved, the personal error is reduced, the consistency and reliability of an analysis result are ensured, and the working efficiency is improved. And the sulfite concentration can be monitored and adjusted in real time, so that the process stability and the resource utilization efficiency are optimized.

Description

Technical Field

[0001] The present application relates to the technical field of chemical detection equipment, and in particular to an online sulfite analyzer for gold electroplating bath liquid. Background Art

[0002] Cyanide-free gold plating technology is widely used in aerospace, PCB, electronic products, industrial equipment, communication equipment, semiconductor laser devices and wafer packaging. Gold plating modification of metal, non-metal and composite surfaces can improve the corrosion resistance, wear resistance, conductivity, solderability, heat resistance and other properties of the product. The sulfite system gold plating performance is superior, efficient and environmentally friendly, and has significant economic benefits. As an important component in the gold plating solution, sulfite has a significant effect on the uniformity, glossiness and adhesion of the electroplated layer. However, during the electroplating process, sulfite will be continuously consumed due to oxidation or the use of the plating solution, resulting in an imbalance in the composition of the plating solution. If it is not added and maintained in time, the quality of the coating will decline, affecting the qualified rate of the product.

[0003] The sulfite content is analyzed manually by chemical titration method regularly, and the consumption is directly supplemented according to the analysis results to control it within the process range. This depends on the operator's experience and manual operation, which will cause large fluctuations in the sulfite concentration in the electroplating gold solution, affect the electroplating quality, and increase the difficulty of operation and labor costs. Summary of the invention

[0004] The present application aims to at least solve the technical problem that the existing technology relies on manual and regular chemical titration to analyze the sulfite content, and directly adds the consumption according to the analysis results to control it within the process range, which depends on the experience and manual operation of the operator, resulting in large fluctuations in the sulfite concentration in the electroplating gold solution, affecting the electroplating quality, and increasing the difficulty of operation and labor costs. To this end, the present application proposes an online sulfite analyzer for electroplating gold bath solution.

[0005] According to an embodiment of the present application, an online analyzer for sulfite in a gold plating bath liquid includes a chassis, wherein a multi-channel valve group, a reaction cup, a syringe pump, a dual-wavelength colorimetric sensor, a peristaltic pump, and a two-position three-way solenoid valve are installed inside the chassis, the reaction cup is equipped with a built-in magnetic stirrer and is connected to the multi-channel valve group through a pipeline, the syringe pump is connected to the reaction cup via an independent pipeline for controlling and adding iodine titration solution to the reaction cup, the dual-wavelength colorimetric sensor forms a closed loop with the reaction cup through a circulation pipeline, the peristaltic pump is installed on the circulation pipeline between the reaction cup and the dual-wavelength colorimetric sensor, and the two-position three-way solenoid valve is arranged on the pipeline between the reaction cup and the peristaltic pump.

[0006] Furthermore, a touch screen interface is installed on one side of the chassis.

[0007] Furthermore, the multi-channel valve group introduces the precisely determined volume of sample, starch indicator and pure water into the reaction cup in sequence according to a predetermined order, and uniformly mixes all the components through the stirring mechanism.

[0008] Furthermore, the chassis has a height of 600 mm, a width of 450 mm, and a depth of 1750 mm.

[0009] Furthermore, the chassis supports Ethernet TCP / IP network communication and uploads analysis data, dosing records and alarm information according to the Modbus protocol.

[0010] The beneficial effects of the present application are: through the use of a multi-channel valve group, a reaction cup, a syringe pump, a dual-wavelength colorimetric sensor, a peristaltic pump and a two-position three-way solenoid valve, the full process from automatic sampling to automatic analysis is realized, and the entire analysis process can be completed without human intervention. This not only greatly saves labor costs, but also reduces the impact of human factors on the analysis results, improves work efficiency and stability, and the sample analysis is carried out according to the preset program, and the concentration analysis results are automatically determined by a high-precision colorimetric sensor. Compared with the traditional manual analysis method, this method reduces operating errors, ensures the consistency and reliability of the analysis results, and helps to maintain the stability of the production process parameters. Since it can realize high-frequency automatic analysis, the device can monitor the concentration changes of sulfite in the production process in real time, and quickly adjust the dosage accordingly, avoiding the waste caused by excessive addition and preventing the process instability caused by insufficient addition.

[0011] Additional aspects and advantages of the present application will be given in part in the description below, and in part will become apparent from the description below, or will be learned through the practice of the present application. BRIEF DESCRIPTION OF THE DRAWINGS

[0012] In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings required for use in the embodiments of the present application will be briefly introduced below. It should be understood that the following drawings only show certain embodiments of the present application and therefore should not be regarded as limiting the scope. For ordinary technicians in this field, other related drawings can be obtained based on these drawings without paying creative work.

[0013] Figure 1 is an overall front view of an online analyzer for sulfite in a gold electroplating bath according to an embodiment of the present application;

[0014] Figure 2 is a side view schematic diagram of the overall structure according to an embodiment of the present application;

[0015] Figure 3 is a schematic diagram of a detection process according to an embodiment of the present application;

[0016] Figure 4 The colorimetric probe according to the embodiment of the present application adopts the post-spectral technology. Figure 1 ;

[0017] Figure 5 The colorimetric probe according to the embodiment of the present application adopts the post-spectral technology. Figure 2 .

[0018] Icons: 1. Chassis; 2. Touch screen interface; 3. Multi-channel valve group; 4. Reaction cup; 5. Syringe pump; 6. Dual-wavelength colorimetric sensor; 7. Peristaltic pump; 8. Two-position three-way solenoid valve. DETAILED DESCRIPTION

[0019] The technical solutions in the embodiments of the present application will be described below in conjunction with the drawings in the embodiments of the present application.

[0020] In order to make the purpose, technical solutions and advantages of the implementation methods of this application clearer, the technical solutions in the implementation methods of this application will be clearly and completely described below in conjunction with the drawings in the implementation methods of this application. Obviously, the described implementation methods are part of the implementation methods of this application, not all of the implementation methods. Based on the implementation methods in this application, all other implementation methods obtained by ordinary technicians in this field without creative work are within the scope of protection of this application.

[0021] Therefore, the following detailed description of the embodiments of the present application provided in the accompanying drawings is not intended to limit the scope of the present application for protection, but merely represents selected embodiments of the present application. Based on the embodiments in the present application, all other embodiments obtained by ordinary technicians in the field without creative work are within the scope of protection of the present application.

[0022] It should be noted that similar reference numerals and letters denote similar items in the following drawings, and therefore, once an item is defined in one drawing, further definition and explanation thereof is not required in subsequent drawings.

[0023] In the description of the present application, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside", "clockwise", "counterclockwise" and the like indicating orientations or positional relationships are based on the orientations or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present application and simplifying the description, and do not indicate or imply that the referred device or element must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be understood as a limitation on the present application.

[0024] In addition, the terms "first" and "second" are used for descriptive purposes only and should not be understood as indicating or implying relative importance or implicitly indicating the number of the indicated technical features. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of the features. In the description of this application, the meaning of "plurality" is two or more, unless otherwise clearly and specifically defined.

[0025] In this application, unless otherwise clearly specified and limited, the terms "installed", "connected", "connected", "fixed" and the like should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be directly connected or indirectly connected through an intermediate medium, it can be the internal connection of two elements or the interaction relationship between two elements. For ordinary technicians in this field, the specific meanings of the above terms in this application can be understood according to specific circumstances.

[0026] In the present application, unless otherwise clearly specified and limited, a first feature being "above" or "below" a second feature may include that the first and second features are in direct contact, or may include that the first and second features are not in direct contact but are in contact through another feature between them. Moreover, a first feature being "above", "above" and "above" a second feature includes that the first feature is directly above and obliquely above the second feature, or simply indicates that the first feature is higher in level than the second feature. A first feature being "below", "below" and "below" a second feature includes that the first feature is directly below and obliquely below the second feature, or simply indicates that the first feature is lower in level than the second feature.

[0027] An online sulfite analyzer for gold electroplating bath solution according to an embodiment of the present application is described below with reference to the accompanying drawings.

[0028] like Figure 1-Figure 3 As shown, an online analyzer for sulfite in a gold electroplating bath according to an embodiment of the present application includes a chassis 1, which is a sheet metal painted chassis with a height of 600 mm, a width of 450 mm, and a depth of 1750 mm.

[0029] A touch screen interface 2 is installed on the front of the chassis 1, and the touch screen interface 2 provides an intuitive platform for users to interact with the sulfite online analyzer. Through the touch screen interface 2, users can easily set analysis parameters, start or stop the analysis process, adjust system settings, etc., and view the status and results of the analysis process in real time, including the current analysis steps, solution concentration change trends, system operation status and other information. This helps to understand the working status of the equipment in a timely manner and make quick responses when necessary.

[0030] like Figure 3As shown, a multi-channel valve group 3, a reaction cup 4, a syringe pump 5, a dual-wavelength colorimetric sensor 6, a peristaltic pump 7 and a two-position three-way solenoid valve 8 are installed inside the chassis 1. The multi-channel valve group 3 is a seven-input and one-output structure for tank liquid, reagent, pure water, and standard sample injection for switching sampling. The reaction cup 4 is equipped with a magnetic stirrer and is connected to the multi-channel valve group 3 through a pipeline. The reaction cup 4 is a container for the titration reaction of the tank liquid and the reagent. The syringe pump 5 is connected to the reaction cup 4 via an independent pipeline, and is used to control and add iodine titrant to the reaction cup 4, and accurately add the titrant;

[0031] The dual-wavelength colorimetric sensor 6 forms a closed loop with the reaction cup 4 through a circulation pipeline, continuously measures the solution undergoing a titration reaction in the reaction cup 4, and outputs the actual result in the form of an electrical signal. The peristaltic pump 7 is installed on the circulation pipeline between the reaction cup 4 and the dual-wavelength colorimetric sensor 6. It continuously runs during the titration reaction to provide real-time solution to the dual-wavelength colorimetric sensor 6, and can discharge waste at the end of the titration. A two-position three-way solenoid valve 8 is arranged on the pipeline between the reaction cup 4 and the peristaltic pump 7. During titration, the normally open end is enabled to circulate the dual-wavelength colorimetric sensor 6, and the normally closed end is switched to discharge the waste liquid in the reaction cup 4 at the end of the titration.

[0032] Specifically, the precisely determined sample enters the reaction cup 4 from the multichannel valve group 3, the starch indicator enters the reaction cup 4 from the multichannel valve group 3, and the pure water enters the reaction cup 4 from the multichannel valve group 3, and the residual sample or indicator of the entire multichannel valve group 3 is added to the reaction cup 4, the stirring mechanism works to make the tank liquid constant and stir it evenly, the peristaltic pump 7 is turned on, and the solution color in the reaction cup 4 and the solution color in the dual-wavelength colorimetric sensor 6 are kept to change synchronously, the injection pump 5 starts to work, and iodine titration solution is slowly added until the signal of the dual-wavelength colorimetric sensor 6 shows that the color change stops, and the sulfite concentration is calculated according to the volume recorded by the injection pump 5, the normally closed end of the two-position three-way solenoid valve 8 is opened, the peristaltic pump 7 is turned on, the waste liquid in the reaction cup 4 is discharged, and the multichannel valve group 3 is washed with water, The two-position three-way solenoid valve 8 is switched to normally open, and the peristaltic pump 7 is turned on to clean the reaction cup 4 and the dual-wavelength colorimetric sensor 6. The normally closed end of the two-position three-way solenoid valve 8 is opened, and the peristaltic pump 7 is turned on to drain the waste liquid in the reaction cup 4. The number of cleaning times can be set.

[0033] The device uses a titration method to determine whether the titration endpoint has been reached based on the developed colorimetric probe, and then accurately calculates the concentration of sulfite ions. Automatic sampling, automatic analysis and automatic dosing control of the entire system are achieved through a PLC program.

[0034] Specifically, the main principle of titration is:

[0035] The principle of iodine titration of sulfite is based on a redox reaction, in which elemental iodine ( ) as an oxidizing agent to convert sulfite ions ( ) is oxidized to sulfate ions ( ), while iodine itself is reduced to iodide ions ( ). At the end of the reaction, the excess iodine combines with the starch indicator to form a dark blue complex, indicating that the titration is complete. The specific analysis is as follows:

[0036] Reaction mechanism and equation

[0037] Main reaction: In acidic or neutral solution, sulfite ion ( ) and iodine ( ) undergoes a redox reaction.

[0038] Oxidation process: Loses 2 electrons and is oxidized to .

[0039] Restore process: Gaining 2 electrons is reduced to .

[0040] The balanced ionic equation is:

[0041]

[0042] The corresponding molecular equation is:

[0043]

[0044] The core of this reaction is the interaction between the reducing property of sulfite and the oxidizing property of iodine.

[0045] End point indication principle:

[0046] The starch indicator is added near the end point. When the sulfite in the solution is completely oxidized, a slightly excess of iodine will combine with starch to form a dark blue starch-iodine complex with a sensitivity of up to .

[0047] This instrument uses a visible light wavelength (400-700nm) sensor, which can convert the starch-iodine complex concentration signal into an electrical signal after being transmitted through the titration solution, and then determine the reaction endpoint.

[0048] Dual wavelength colorimetric sensor 6 endpoint judgment principle:

[0049] Dual wavelength spectrophotometry

[0050] The main principle is: the same incident light (composite light source) passes through the sample to be tested with a concentration of C and a liquid tank width of B. After the light beam passes through two different filters, the two receivers receive two monochromatic lights of different wavelengths respectively. (Primary Wavelength, also called measurement wavelength) and (second Wavelength, reference wavelength), if and If the selection is appropriate, light scattering and background absorption can be ignored, improving measurement accuracy, and interference can be eliminated by selecting filters, thereby improving selectivity. Lambert-Beer's law can be derived:

[0051] (1)

[0052] (2)

[0053] (3)

[0054] , are the incident light intensity and the outgoing light intensity of the sample to be tested, , is the incident light intensity and the outgoing light intensity of the reference sample. From formula (3), we can get: the ion concentration in the sample to be tested is related to the two wavelengths. or lg( ) has a linear relationship.

[0055] By choosing the appropriate reference wavelength and measurement wavelength, it is possible to accurately determine the drop of the titrant that reaches the endpoint, thereby obtaining the titration volume and calculating the concentration of the analyte.

[0056] Figure 4 and Figure 5 In the composite light source, it can be any light source that can provide white light, such as LED, tungsten lamp, etc.

[0057] Sample pool: A container for placing samples, with a width of 2~10mm. Quartz is the preferred material, but glass is also acceptable.

[0058] Monochromatic filter 1: obtain monochromatic light of reference wavelength .

[0059] Monochromatic filter 2: Obtain monochromatic light of reference wavelength .

[0060] Photoelectric signal converter 1: Receives from Signal and convert it into an electrical signal Output.

[0061] Photoelectric signal converter 2: Receives from Signal and convert it into an electrical signal Output.

[0062] Sample flow inlet: The sample enters the sample cell from here.

[0063] Sample flow outlet: Sample flows out of the sample cell from here.

[0064] Signal output interface: measured signal.

[0065] Chassis 1 supports Ethernet TCP / IP network communication and uploads analysis data, dosing records and alarm information according to the Modbus protocol. Through the built-in Ethernet interface, chassis 1 can access the existing local area network or wide area network to achieve connection with the enterprise's internal network or other external systems. This networking function allows remote access and control of the device, allowing operators to monitor and manage the device away from the device. The TCP / IP protocol is an Internet protocol family used to achieve data exchange in the network. The use of the TCP / IP protocol can ensure that data packets are accurately transmitted in a complex network environment and provide stable and reliable network communication. Modbus is a serial communication protocol widely used in the field of industrial automation. It is simple, open and easy to implement. The use of the Modbus protocol can enable the sulfite online analyzer to seamlessly connect with other devices or systems that support the protocol (such as PLC, SCADA system, etc.), making it easy to integrate into a larger industrial control system.

[0066] The above are only embodiments of the present application and are not intended to limit the scope of protection of the present application. For those skilled in the art, the present application may have various changes and variations. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present application should be included in the scope of protection of the present application. It should be noted that similar numbers and letters represent similar items in the following drawings, so once an item is defined in one drawing, it does not need to be further defined and explained in the subsequent drawings.

[0067] The above are only specific implementations of the present application, but the protection scope of the present application is not limited thereto. Any technician familiar with the technical field can easily think of changes or substitutions within the technical scope disclosed in the present application, which should be included in the protection scope of the present application. Therefore, the protection scope of the present application should be based on the protection scope of the claims.

Claims

1. An online analyzer for sulfite in electroplating gold bath, characterized in that: The invention comprises a chassis (1), wherein a multi-channel valve group (3), a reaction cup (4), a syringe pump (5), a dual-wavelength colorimetric sensor (6), a peristaltic pump (7) and a two-position three-way solenoid valve (8) are installed inside the chassis (1); the reaction cup (4) is equipped with a magnetic stirrer and is connected to the multi-channel valve group (3) through a pipeline; the syringe pump (5) is connected to the reaction cup (4) through an independent pipeline and is used to control and add iodine titration solution to the reaction cup (4); the dual-wavelength colorimetric sensor (6) forms a closed loop with the reaction cup (4) through a circulation pipeline; the peristaltic pump (7) is installed on the circulation pipeline between the reaction cup (4) and the dual-wavelength colorimetric sensor (6); and the two-position three-way solenoid valve (8) is arranged on the pipeline between the reaction cup (4) and the peristaltic pump (7).

2. The gold electroplating bath sulfite online analyzer according to claim 1, characterized in that: A touch screen interface (2) is installed on one side of the chassis (1).

3. The gold electroplating bath sulfite online analyzer according to claim 2, characterized in that: The multi-channel valve group (3) sequentially introduces precisely determined volumes of sample, starch indicator and pure water into the reaction cup (4) in a predetermined order, and uniformly mixes all the components through a stirring mechanism.

4. The gold electroplating bath sulfite online analyzer according to claim 3, characterized in that: The chassis (1) has a height of 600 mm, a width of 450 mm and a depth of 1750 mm.

5. The gold electroplating bath sulfite online analyzer according to claim 4, characterized in that: The chassis (1) supports Ethernet TCP / IP network communication and uploads analysis data, drug addition records and alarm information according to the Modbus protocol.

Images