CN116359309A - Method and device for detecting chloride ion content - Google Patents
Method and device for detecting chloride ion content Download PDFInfo
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Abstract
The application discloses a method and a device for detecting chloride ion content. The method for detecting the chloride ion content comprises the following steps: preparing a first volume of liquid to be detected; adding a second volume of phosphoric acid solution into the to-be-detected liquid to form a to-be-detected sample; and (3) dropwise adding a silver nitrate solution into the sample to be detected, and determining the chloride ion content in the sample to be detected according to the potential change in the sample to be detected. By the scheme, the accuracy and the stability of detecting the content of chloride ions in the brown oxide liquid can be improved.
Description
Technical Field
The application belongs to the technical field of printed circuit board production, and particularly relates to a method and a device for detecting chloride ion content.
Background
In the production process of the printed circuit board, the surface copper layer of the core board is generally required to be browned by adopting a browned liquid, so that an organic browned film is formed on the copper surface, the binding force between the surface copper layer and resin is improved, and the manufacturing of the multilayer board is realized. Among them, organic browning films are key to the production of multilayer boards, and the composition of the browning liquid directly affects the quality of the organic browning films, wherein chloride ions are key factors affecting the organic browning films.
However, copper ions, sulfate ions and the like contained in the conventional brown oxide liquid generally interfere with the test of chloride ions, so that the accurate content of the chloride ions in the brown oxide liquid is difficult to determine by adopting the conventional test method.
Disclosure of Invention
The application provides a method and a device for detecting the content of chloride ions, which are used for solving the technical problem that the content of chloride ions in the brown oxide liquid is difficult to accurately detect due to the fact that the existing brown oxide liquid contains copper ions, sulfate ions and the like and generally interferes with the test of the chloride ions.
In order to solve the technical problems, one technical scheme adopted by the application is as follows: the method for detecting the chloride ion content comprises the following steps:
preparing a first volume of liquid to be detected;
adding a second volume of phosphoric acid solution into the to-be-detected liquid to form a to-be-detected sample;
and (3) dropwise adding a silver nitrate solution into the sample to be detected, and determining the chloride ion content in the sample to be detected by detecting the potential change in the sample to be detected.
Optionally, the concentration of the phosphoric acid solution is not less than 85%, and the volume ratio of the first volume to the second volume is 5:1.5-5:2.5.
Optionally, the first volume is not less than 50ml.
Optionally, the liquid to be detected is brown liquid.
Optionally, the step of dropping a silver nitrate solution into the sample to be detected, and determining the chloride ion content in the sample to be detected by detecting the potential change in the sample to be detected includes:
inserting a detection electrode into the sample to be detected;
dripping an equal amount of silver nitrate solution into the sample to be detected at preset time intervals;
determining the total amount of the silver nitrate solution in the sample to be detected after each dripping of the silver nitrate solution and the potential of the sample to be detected after each dripping of the silver nitrate solution;
determining a chemical metering point of the silver nitrate solution for titrating the sample to be detected according to the total dripping amount and the potential;
and determining the chloride ion content in the liquid to be detected according to the dropping amount of the silver nitrate solution at the stoichiometric point.
Optionally, the determining the stoichiometric point of the silver nitrate solution for titrating the sample to be detected according to the total dropping amount and the electric potential includes:
setting up a change curve of the potential of the sample to be detected along with the total dripping amount of the silver nitrate solution by taking the total dripping amount as a horizontal axis and the potential as a vertical axis;
and determining the stoichiometric point according to the change mutation point of the change curve.
Optionally, the surface of the detection electrode is plated with a sulfur-containing plating layer, and the inserting the detection electrode to the sample to be detected includes:
inserting the part of the detection electrode with the sulfur-containing plating layer into the sample to be detected.
Optionally, the adding a phosphoric acid solution to the solution to be detected to form a sample to be detected includes:
and adding a phosphoric acid solution into the detection liquid, and uniformly stirring to form a sample to be detected.
In order to solve the technical problems, one technical scheme adopted by the application is as follows: there is provided a detection apparatus including: the device comprises a detection container, a feeding device and a detection device;
the feeding device is used for sequentially injecting a first volume of to-be-detected liquid and a second volume of phosphoric acid solution into the detection container to form a to-be-detected sample;
the detection device comprises a titration mechanism, a detection electrode and a potential detection device electrically connected with the detection electrode, wherein the detection electrode is inserted into the sample to be detected, the titration mechanism is used for dripping silver nitrate solution into the sample to be detected, the potential detection device detects potential change in the sample to be detected, and the chloride ion content in the liquid to be detected is determined according to the potential change.
Optionally, the detection device further comprises a stirring mechanism, wherein the stirring mechanism is used for extending into the detection container so as to stir the solution in the detection container.
The beneficial effects of this application are: in the scheme of the application, through directly selecting the first volume wait to detect the liquid to add the phosphoric acid solution of second volume into the wait to detect the liquid of first volume and form to wait to detect the sample, and need not adopt DI water to carry out the constant volume dilution, consequently, compare current detection method in the wait to detect the sample, acidity is stronger, thereby can make the silver sulfate deposit that partial sulfate radical ion formed with silver ion can redissolve ionization and form sulfate radical ion and silver ion, consequently can reduce the sulfate radical and silver ion reaction and form the deposit and wait to detect the influence of ion concentration in the sample, consequently can improve the accuracy that silver nitrate solution titrated chloride ion.
In addition, since the solution of the embodiment does not need to use DI water for constant volume dilution in the sample to be detected, the concentration of the organic matters in the sample to be detected can be higher, so that the solubility of inorganic salt (silver chloride) in the sample to be detected can be reduced, the formed silver chloride precipitate can be further reduced to electrolyze in the solution, so that chloride ions can tend to be completely reacted, and the accuracy of titration of chloride ions by the silver nitrate solution can be further improved.
Drawings
For a clearer description of the technical solutions in the embodiments of the present application, the drawings that are needed in the description of the embodiments will be briefly introduced below, it being obvious that the drawings in the following description are only some embodiments of the present application, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art, wherein:
FIG. 1 is a schematic flow chart of an embodiment of a method for detecting chloride ion content according to the present application;
FIG. 2 is a schematic diagram showing the potential of a sample to be tested according to the total amount of silver nitrate solution dropped.
Detailed Description
The following description of the embodiments of the present application will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all, of the embodiments of the present application. All other embodiments, which can be made by one of ordinary skill in the art without undue burden from the present disclosure, are within the scope of the present disclosure.
It should be noted that, in the embodiment of the present application, directional indications (such as up, down, left, right, front, and rear … …) are referred to, and the directional indications are merely used to explain the relative positional relationship, movement conditions, and the like between the components in a specific posture (as shown in the drawings), and if the specific posture is changed, the directional indications are correspondingly changed.
In addition, if there is a description of "first", "second", etc. in the embodiments of the present application, the description of "first", "second", etc. is for descriptive purposes only and is not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include at least one such feature. In addition, the technical solutions of the embodiments may be combined with each other, but it is necessary to base that the technical solutions can be realized by those skilled in the art, and when the technical solutions are contradictory or cannot be realized, the combination of the technical solutions should be regarded as not exist and not within the protection scope of the present application.
In the process of manufacturing a printed circuit board, it is generally required to fixedly connect a metal conductive layer with an insulation base layer, for example, to fix a metal conductive layer (generally, copper foil) on a surface of an insulation substrate to form a core board or to place a prepreg between two adjacent core boards, and to fixedly connect the metal conductive layer on the surface of the core board with the prepreg by hot pressing.
Among them, in order to improve the connection stability of the metal conductive layer and the insulation base layer, it is generally necessary to brown-oxide the metal conductive layer. The browning treatment is to react with the metal conducting layer with the browning liquid to form one organic browning film on the metal conducting layer to raise the binding force between the metal conducting layer and the insulating base layer.
Among them, since chloride ions in the brown oxide liquid are key factors affecting the mechanical brown oxide film, accurate determination of the chloride ion concentration in the brown oxide liquid is required for subsequent production evaluation of the brown oxide liquid.
In the existing scheme, the method for measuring the concentration of chloride ions in the brown oxide liquid specifically comprises the following steps:
1. preparing a calibration solution.
The calibration solution can be prepared by using a standard solution of 1000ppm chloride ion, for example, 2ml of a standard solution of 1000ppm chloride ion concentration can be selected, 20ml of concentrated phosphoric acid can be added to the standard solution, and DI water (deionized water or ultrapure water) can be added to fix the volume to 100ml, thereby obtaining 100ml of calibration solution. The chloride ion concentration value L1 of the calibration solution is then detected by titration with a silver chloride solution.
2. A sample solution was prepared.
In the sample solution, 10ml of brown oxide solution can be taken, 2ml of standard solution with chloride ion concentration of 1000ppm is added into the 10ml of brown oxide solution, then 20ml of concentrated phosphoric acid is added, and DI water is added to fix the volume to 100ml, so that 100ml of sample solution can be obtained. The chloride ion concentration value L2 of the sample solution was then detected by titration with a silver chloride solution.
Further, the chloride ion concentration (in ppm) in the raw brown oxide solution can be determined by the formula (L2-L1) ×10.
Among them, the detection results of the sample detected by the conventional detection method are shown in the following table 1.
TABLE 1
Wherein, the expression of 2ml of standard solution is that 2ml of standard solution with chloride ion concentration of 1000ppm is adopted for the sample solution, 20ml of concentrated phosphoric acid is added, and DI water is added to fix the volume to 100ml, so that 100ml of sample solution can be obtained; "2ml of standard solution+brown oxide" means that the sample solution is obtained by mixing 2ml of standard solution with chloride ion concentration of 1000ppm and 10ml of brown oxide solution, adding 20ml of concentrated phosphoric acid, and then adding DI water to a volume of 100ml, thereby obtaining 100ml of sample solution; "3ml of the standard solution+brown oxide" means that the sample solution was obtained by mixing 3ml of a standard solution having a chloride ion concentration of 1000ppm with 10ml of brown oxide, adding 20ml of concentrated phosphoric acid, and then adding DI water to a volume of 100 ml.
In the existing detection scheme, the detection method is complex; in addition, the brown oxide liquid usually contains sulfate ions, and sulfate ions are combined with silver ions to form precipitates when the brown oxide liquid is subjected to titration detection by a silver chloride solution, so that the titration result is influenced, and the accuracy of the concentration detection result of chloride ions in the brown oxide liquid is influenced.
Referring to fig. 1, fig. 1 is a flow chart of an embodiment of a method for detecting chloride ion content provided in the present application.
The method for detecting the content of chloride ions specifically comprises the following steps:
s110: a first volume of liquid to be tested is prepared.
In this step, a liquid to be detected having a first volume may be prepared, wherein the liquid to be detected may be brown liquid to be detected. The brown oxide liquid contains chloride ions (Cl) - ) Nitric acid (HNO) 3 ) Sulfuric acid (H) 2 SO 4 )、H 2 O 2 Copper ion (Cu) 2+ ) And a preset organic matter.
Wherein the first volume may be not less than 50ml, for example, the first volume may be selected to be 50, 60 or 70ml.
S120: and adding a second volume of phosphoric acid solution to the to-be-detected liquid to form a to-be-detected sample.
When the preparation of the liquid to be detected is completed, a second volume of phosphoric acid solution can be added to the liquid to be detected to form a sample to be detected.
In the step, the phosphoric acid solution can be a concentrated phosphoric acid solution with the concentration of not less than 85%, and the concentrated phosphoric acid solution can form a reaction environment for subsequent titration detection. Wherein the concentration of the concentrated phosphoric acid solution is not less than 85% expressed as: in the concentrated phosphoric acid solution, the volume ratio of phosphoric acid is not less than 85% of the volume of the phosphoric acid solution. Wherein the concentration of the phosphoric acid solution may be 85%, 90% or 95%.
Wherein the volume ratio of the first volume to the second volume is 5:1.5-5:2.5.
Thus, when the first volume is 50ml, the second volume may be 15 to 25ml. Wherein the second volume may be 15, 20 or 25ml.
In a preferred embodiment, when the first volume is 50ml, the second volume may be 20ml.
When the phosphoric acid solution is added into the detection liquid, the required sample to be detected can be formed after uniform stirring.
S130: and (3) dropwise adding a silver nitrate solution into the sample to be detected, and determining the chloride ion content in the sample to be detected according to the potential change in the sample to be detected.
After the preparation of the sample to be detected in step S120 is completed, the sample to be detected may be subjected to titration detection, so as to determine the chloride ion content in the original solution to be detected.
Specifically, the titration can be performed through the silver nitrate solution with the preset concentration, silver ions in the silver nitrate solution react with chloride ions to generate silver chloride precipitates, so that the ion concentration in the sample to be detected is changed, the conductivity of the sample to be detected is changed, and therefore the potential change in the sample to be detected can be detected, and the chloride ion content can be determined.
Wherein titration may be performed with 0.01 equivalent (0.01 mol/L) of silver nitrate solution.
Therefore, in the solution of this embodiment, the to-be-detected sample is formed by directly selecting the first volume of to-be-detected liquid and adding the second volume of phosphoric acid solution into the first volume of to-be-detected liquid, and the DI water is not required to be used for constant volume dilution.
In addition, since the solution of the embodiment does not need to use DI water for constant volume dilution in the sample to be detected, the concentration of the organic matters in the sample to be detected can be higher, so that the solubility of inorganic salt (silver chloride) in the sample to be detected can be reduced, the formed silver chloride precipitate can be further reduced to electrolyze in the solution, so that chloride ions can tend to be completely reacted, and the accuracy of titration of chloride ions by the silver nitrate solution can be further improved.
Further, in this embodiment, the titration of the chloride ion content in the sample to be detected by using the silver nitrate solution specifically includes the following steps:
a. the detection electrode is inserted into the sample to be detected.
In this step, the detection sample may be electrically connected to an external power source, and the potential change of the sample to be detected may be detected by the detection electrode.
The detection electrode can be an electrode with a sulfur-containing coating, and the potential change of the sample to be detected can be detected by inserting the part of the detection electrode with the sulfur-containing coating into the sample to be detected, so that the interference of copper ions in the sample to be detected can be avoided, the sensitivity of the detection electrode for detecting the potential change of the sample to be detected can be improved, and the accuracy of detecting the content of chloride ions in the sample to be detected can be further ensured.
b. And dripping an equal amount of silver nitrate solution into the sample to be detected at preset intervals.
In the insertion detection electrode, an equal amount of silver nitrate solution may be dropped dropwise into the sample to be detected.
The silver nitrate solution can be added into the sample to be detected in an equal amount after every preset time interval. For example, 1 or more drops of the silver nitrate solution may be dropped into the sample to be detected at a time, and after a predetermined time interval, an equal amount of the silver nitrate solution may be dropped into the sample to be detected.
c. And determining the total dropping amount of the silver nitrate solution in the sample to be detected after each silver nitrate solution dropping and the potential of the sample to be detected after each silver nitrate solution dropping.
Wherein, after each instillation of the silver nitrate solution into the sample to be detected, the total amount of instillation of the silver nitrate solution can be recorded. For example, if 0.1ml of the silver nitrate solution is added each time, the total amount of the silver nitrate solution added by the first addition is 0.1ml, the total amount of the silver nitrate solution added by the second addition is 0.2ml, and so on.
The potential change of the sample to be detected can also be detected by the detection electrode after each dropping of the silver nitrate solution.
After the silver nitrate solution is dripped each time and the potential of the sample to be detected is detected to be stable, the next operation of dripping the silver nitrate solution can be continued, and the potential of the sample to be detected is detected.
d. And determining a chemical metering point for titrating the sample to be detected by the silver nitrate solution according to the total dripping amount and the potential.
And determining a chemical metering point for titrating the sample to be detected by the silver nitrate solution according to the total dripping amount and the potential.
Wherein, when the stoichiometric point is reached, chloride ions in the sample to be detected are completely precipitated (silver chloride precipitation), and even if the silver nitrate solution is added again, no new silver chloride precipitation is further generated. At this time, the total amount of the silver nitrate solution dropped exactly reacts with the chloride ions in the test sample.
e. And determining the chloride ion content in the liquid to be detected according to the dropping amount of the silver nitrate solution at the stoichiometric point.
After the stoichiometric point is determined, the chloride ion content in the liquid to be detected can be converted according to the dropping amount of the silver nitrate solution and the concentration of the dropping amount of the silver nitrate solution.
In this embodiment, the total dropping amount may be taken as the horizontal axis potential and the vertical axis potential, and a change curve of the potential of the sample to be detected along with the total dropping amount of the silver nitrate solution may be established; and determining the stoichiometric point according to the change mutation point of the change curve.
Referring to fig. 2, fig. 2 is a schematic diagram showing the change of the potential of the sample to be detected along with the total amount of the silver nitrate solution dropped.
The slope abrupt change point of the change curve corresponds to the stoichiometric point of the sample to be detected.
The detection results of detecting the sample to be detected by the conventional detection method are shown in the following table 2.
TABLE 2
Wherein, the expression of "1ml of standard solution" in Table 2 indicates that the sample to be detected is 1ml of standard solution with chloride ion concentration of 1000ppm, and the standard solution is fixed to 50ml by DI water; "brown" means that the sample to be detected is 50ml of brown liquid to be detected; "0.5ml of the standard solution and the brown oxide" is expressed as a mixed solution formed by adding 0.5ml of the standard volume solution of the sample to be detected to 49.5ml of the brown oxide solution; "1ml of the standard solution+brown-out" means a mixed solution of 1ml of the sample to be detected and 1000ppm of the standard volume solution added to 49ml of the brown-out solution. The data in "results" are in ppm.
From comparison of the foregoing tables 1 and 2, it can be seen that the results of detecting the concentration of chloride ions in the sample to be detected using the detection method corresponding to table 2 are stable and highly accurate.
Further, based on the same inventive concept, the application also provides a detection device. The detection device can be used for realizing the chloride ion detection method.
The detection device comprises a detection container, a feeding device and a detection device;
the feeding device is used for sequentially injecting a first volume of to-be-detected liquid and a second volume of phosphoric acid solution into the detection container to form a to-be-detected sample;
the detection device comprises a titration mechanism, a detection electrode and a potential detection device electrically connected with the detection electrode, wherein the detection electrode is inserted into a sample to be detected, the titration mechanism is used for dripping silver nitrate solution into the sample to be detected, the potential detection device detects potential change in the sample to be detected, and the chloride ion content in the sample to be detected is determined according to the potential change.
The detection device is used for detecting the content of chloride ions in the liquid to be detected, and the detailed description is omitted herein.
In addition, the detection device further comprises a stirring mechanism, and the stirring mechanism is used for extending into the detection container so as to stir the solution in the detection container.
To sum up, those skilled in the art will readily understand that the beneficial effects of the present application are: in the scheme of the application, through directly selecting the first volume wait to detect liquid to add the phosphoric acid solution of second volume into the wait to detect liquid of first volume and form to wait to detect the sample, and need not adopt DI water to carry out the constant volume dilution, consequently, compare current detection method in the wait to detect the sample of this embodiment acidity stronger, thereby can make the silver sulfate deposit that partial sulfate ion formed with silver ion can redissolve ionization and form sulfate ion and silver ion, consequently can reduce the influence that sulfate and silver ion reaction formed the deposit and wait to detect ion concentration in the sample, consequently can improve the accuracy of titrating chloride ion through silver nitrate solution.
In addition, since the solution of the embodiment does not need to use DI water for constant volume dilution in the sample to be detected, the concentration of the organic matters in the sample to be detected can be higher, so that the solubility of inorganic salt (silver chloride) in the sample to be detected can be reduced, the formed silver chloride precipitate can be further reduced to electrolyze in the solution, so that chloride ions can tend to be completely reacted, and the accuracy of titration of chloride ions by the silver nitrate solution can be further improved.
The foregoing description is only exemplary embodiments of the present application and is not intended to limit the scope of the present application, and all equivalent structures or equivalent processes using the descriptions and the drawings of the present application, or direct or indirect application in other related technical fields are included in the scope of the present application.
Claims (10)
1. The method for detecting the content of the chloride ions is characterized by comprising the following steps of:
preparing a first volume of liquid to be detected;
adding a second volume of phosphoric acid solution into the to-be-detected liquid to form a to-be-detected sample;
and (3) dropwise adding a silver nitrate solution into the sample to be detected, and determining the chloride ion content in the sample to be detected by detecting the potential change in the sample to be detected.
2. The method for detecting chloride ion content according to claim 1, wherein,
the concentration of the phosphoric acid solution is not less than 85%, and the volume ratio of the first volume to the second volume is 5:1.5-5:2.5.
3. The method for detecting chloride ion content according to claim 1, wherein,
the first volume is not less than 50ml.
4. The method for detecting chloride ion content according to claim 1, wherein,
the liquid to be detected is brown liquid.
5. The method for detecting chloride ion content according to any one of claims 1 to 4, wherein the dropping of the silver nitrate solution into the sample to be detected, by detecting a potential change in the sample to be detected, to determine the chloride ion content in the sample to be detected, comprises:
inserting a detection electrode into the sample to be detected;
dripping an equal amount of silver nitrate solution into the sample to be detected at preset time intervals;
determining the total amount of the silver nitrate solution in the sample to be detected after each dripping of the silver nitrate solution and the potential of the sample to be detected after each dripping of the silver nitrate solution;
determining a chemical metering point of the silver nitrate solution for titrating the sample to be detected according to the total dripping amount and the potential;
and determining the chloride ion content in the liquid to be detected according to the dropping amount of the silver nitrate solution at the stoichiometric point.
6. The method according to claim 5, wherein determining a stoichiometric point at which the silver nitrate solution titrates the sample to be detected based on the total amount of dropwise addition and the potential comprises:
setting up a change curve of the potential of the sample to be detected along with the total dripping amount of the silver nitrate solution by taking the total dripping amount as a horizontal axis and the potential as a vertical axis;
and determining the stoichiometric point according to the change mutation point of the change curve.
7. The method for detecting chloride ion content according to claim 5, wherein the surface of the detection electrode is plated with a sulfur-containing plating layer, and the inserting the detection electrode into the sample to be detected comprises:
inserting the part of the detection electrode with the sulfur-containing plating layer into the sample to be detected.
8. The method for detecting chloride ion content according to claim 1, wherein said adding a phosphoric acid solution to the liquid to be detected to form a sample to be detected comprises:
and adding a phosphoric acid solution into the detection liquid, and uniformly stirring to form a sample to be detected.
9. A detection device, characterized in that the detection device comprises: the device comprises a detection container, a feeding device and a detection device;
the feeding device is used for sequentially injecting a first volume of to-be-detected liquid and a second volume of phosphoric acid solution into the detection container to form a to-be-detected sample;
the detection device comprises a titration mechanism, a detection electrode and a potential detection device electrically connected with the detection electrode, wherein the detection electrode is inserted into the sample to be detected, the titration mechanism is used for dripping silver nitrate solution into the sample to be detected, the potential detection device detects potential change in the sample to be detected, and the chloride ion content in the liquid to be detected is determined according to the potential change.
10. The test device of claim 9, further comprising a stirring mechanism for extending into the test receptacle to stir the solution in the test receptacle.
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