CN112304903A - Method for detecting concentration of chloride ions in turbid formed liquid - Google Patents
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Abstract
The invention relates to a method for detecting the concentration of chloride ions in turbid formed liquid. A method for detecting the concentration of chloride ions in a turbid formed liquid comprises the following steps: (1) taking the turbid formed solution as a test solution for centrifugation, and layering the solution; (2) adding the reagent 1 into the layered upper layer solution, shaking up, heating in a water bath, and cooling to room temperature; (3) adding the reagent 2 into the cooled reaction solution, uniformly mixing, fixing the volume and standing; (4) preparing a chloride ion standard solution with known concentration, and treating by adopting the method of the steps (1) to (3); (5) and comparing the turbidity of the treated test solution with that of the chloride ion standard solution to obtain the concentration of the chloride ions in the turbid formed solution. According to the method for detecting the concentration of the chloride ions in the turbid forming solution, the traditional visual turbidimetry is improved, the suspended matters in the forming solution are eliminated, the interference of the suspended matters in the forming solution on the detection of the concentration of the chloride ions is reduced, and the accuracy of the detection of the concentration of the chloride ions in the forming solution is improved.
Description
Technical Field
The invention particularly relates to a method for detecting the concentration of chloride ions in a turbid formed liquid.
Background
An anode foil for an aluminum electrolytic capacitor (hereinafter, referred to as an anode foil) is a main material for producing a capacitor, and the properties of the anode foil are deteriorated by surface chloride ions thereof. If the chloride ion content in the anode foil is too high, anode corrosion may occur. The concentration of chloride ions in the formation solution is a main factor influencing the content of chloride ions in the anode foil, so that the concentration of chloride ions in the formation solution needs to be regularly detected and controlled in the production process, and the risk of overhigh content of chloride ions in the anode foil is reduced.
The currently common methods for detecting the concentration of chloride ions include: turbidimetry, silver titration, ion chromatography, and the like. In consideration of detection cost and detection timeliness, a turbidimetry method is often selected to detect the concentration of chloride ions in the formation liquid in actual production. The turbidimetry is based on the principle that chloride ions react with silver ions to generate white silver chloride precipitates, excess silver nitrate is added into a solution to react with the chloride ions in the solution, and the amount of the generated precipitates is judged by naked eyes, so that the concentration of the chloride ions in the solution is obtained. The method mainly comprises the following steps: firstly adding nitric acid into the formation liquid for acidification to eliminate impurity ion interference, then adding a silver nitrate solution to form silver chloride precipitate, standing for a while, and then comparing the turbidity of the formation liquid with a standard liquid to obtain the concentration of chloride ions in the formation liquid. In the case of detection by a turbidimetric method, a standard solution containing a fixed amount of chloride ions (hereinafter, referred to simply as a standard solution) is usually prepared, the standard solution is treated in the same manner, the turbidity of the solution to be detected and the standard solution is compared, and the concentration of the standard solution having a similar turbidity is taken as the chloride ion concentration of the solution to be detected.
The turbidimetry is to judge the concentration of chloride ions according to silver nitrate precipitate generated by the reaction. However, when the solution itself is turbid, that is, when suspended matters exist in the solution to be detected, the detection accuracy of the method is greatly reduced. In the production process of the anode foil, the formation solution often contains more impurity ions, and a part of the formation solution contains more white suspended aluminum hydroxide, so that the concentration of chloride ions in the formation solution is difficult to obtain by a traditional turbidimetric method.
In view of the above, the invention provides a novel method for detecting the concentration of chloride ions in a turbid formed solution, which is simple and feasible and can be used in a large-scale production process to determine the concentration of chloride ions in the turbid formed solution.
Disclosure of Invention
The invention aims to provide a method for detecting the concentration of chloride ions in a turbid formed liquid, which eliminates the influence of white aluminum hydroxide suspended matters in the formed liquid on a turbid result on the premise of not influencing the solubility of silver chloride, improves the accuracy of the determination of the concentration of the chloride ions in the formed liquid by a turbidimetric method, and provides a high-reliability detection method for the detection of the concentration of the chloride ions in the turbid formed liquid.
In order to realize the purpose, the adopted technical scheme is as follows:
a method for detecting the concentration of chloride ions in a turbid formed liquid comprises the following steps:
(1) taking the turbid formed solution as a test solution, carrying out centrifugal treatment, and layering the solution;
(2) adding reagent 1 into the layered upper layer solution, shaking, heating in water bath at 90-100 deg.C for 4-6min, and cooling to room temperature; the reagent 1 is a nitric acid solution with the mass fraction of 34%;
(3) adding the reagent 2 into the cooled reaction solution, uniformly mixing, fixing the volume, and standing for 10-20 min;
the reagent 2 is a silver nitrate solution with the mass fraction of 0.5%;
(4) preparing at least 3 chloride ion standard solutions with known concentrations and different concentrations, and treating by adopting the method of the steps (1) to (3);
(5) and (3) comparison: and (3) placing the treated test solution and the chloride ion standard solution in a dark box, comparing the turbidity, and taking the chloride ion standard solution with the concentration similar to the turbidity of the treated test solution as the concentration of chloride ions in the turbid formed solution.
Further, the conditions of the centrifugal treatment in the step (1) are as follows: the rotating speed is 2000-3000r/min, and the centrifugation is 15-20 min.
Further, in the step (2), the volume ratio of the upper layer solution to the reagent 1 is 20-30: 2-5;
in the step (3), the volume ratio of the reagent 1 to the reagent 2 is 2-5: 2-5.
Still further, in the step (3), the volume ratio of the reagent 1 to the reagent 2 is 1: 1.
Further, in the step (2), the temperature of the water bath heating is 95 ℃.
Further, in the step (3), the volume after constant volume is the same as the volume of the test solution obtained in the step (1).
Further, in the step (4), not less than 5 chloride ion standard solutions with known concentrations and different concentrations are prepared.
Still further, in the step (4), a chloride ion standard solution with an equal concentration difference is prepared.
Compared with the prior art, the invention has the beneficial effects that:
1. the method is improved on the basis of the traditional turbidimetry, introduces centrifugal treatment, simultaneously promotes the reaction of nitric acid and suspended aluminum hydroxide in the formed liquid by adopting heating treatment, and adds a cooling step at a proper position, namely, under the premise of not influencing the solubility of silver chloride, the influence of white suspended aluminum hydroxide in the formed liquid on the turbidity result is eliminated, and the turbidity accuracy of the turbidimetry for measuring the concentration of chloride ions in the formed liquid is improved.
2. The method is simple in operation method, easy in process control and short in flow, and is suitable for detecting the concentration of the chloride ions in the solution in batches.
3. The invention improves the detection accuracy on the basis of ensuring the detection efficiency, and is suitable for detecting the concentration of the formed liquid chloride ions in the production of the anode foil.
Detailed Description
In order to further illustrate the method for detecting the concentration of chloride ions in the turbid chemical solution of the present invention to achieve the intended purpose of the invention, the following embodiments are combined to describe the method for detecting the concentration of chloride ions in the turbid chemical solution according to the present invention, and the detailed implementation, structure, characteristics and efficacy thereof are as follows. In the following description, different "one embodiment" or "an embodiment" refers to not necessarily the same embodiment. Furthermore, the particular features, structures, or characteristics may be combined in any suitable manner in one or more embodiments.
Before describing the method for detecting the concentration of chloride ions in the turbid formed liquid in detail, it is necessary to further describe the related method mentioned in the present invention to achieve better effect.
The invention improves the traditional turbidimetry, firstly removes suspended large particles by centrifugal treatment, then takes 20-30ml of centrifuged supernatant liquid to be put in a turbidimetric tube, and adds 2-5ml of nitric acid for acidification. Heating the acidified solution in water bath at 90-100 deg.C for 4-6min to promote the reaction between nitric acid and aluminum hydroxide, and dissolving suspended aluminum hydroxide. After the formed solution is clarified, the formed solution is taken out and cooled to room temperature, so that the problem that the original solution containing chloride ions does not generate white flocculent precipitate or less precipitate due to the fact that the solubility of silver chloride is increased at high temperature, and the turbidimetric result is influenced is avoided. At this time, the suspended aluminum hydroxide in the stock solution is reacted with aluminum ions and hydroxide ions, and is difficult to precipitate under acidic conditions. Then 2-5ml of silver nitrate solution is added into the clarified chemical liquid to generate silver chloride sediment, and the sediment is kept stand for 10-20min and then turbidity is compared.
The invention promotes the reaction of nitric acid and aluminum hydroxide suspended matters in the formed liquid by adding heat treatment, and avoids the precipitation of decomposed aluminum hydroxide by utilizing nitric acid to acidify the solution. After the aluminum hydroxide suspended matter is digested, the formed liquid is cooled to room temperature, and then subsequent operation is carried out, so that the silver chloride precipitation is prevented from being influenced by high temperature.
After understanding the related methods mentioned in the present invention, the following will describe in further detail a method for detecting the concentration of chloride ions in a turbid chemical liquid according to the present invention with reference to specific examples:
the technical scheme of the invention is as follows:
a method for detecting the concentration of chloride ions in a turbid formed liquid comprises the following steps:
(1) taking the turbid formed solution as a test solution, carrying out centrifugal treatment, and layering the solution;
(2) adding reagent 1 into the layered upper layer solution, shaking, heating in water bath at 90-100 deg.C for 4-6min, and cooling to room temperature; the reagent 1 is a nitric acid solution with the mass fraction of 34%;
(3) adding the reagent 2 into the cooled reaction solution, uniformly mixing, fixing the volume, and standing for 10-20 min;
the reagent 2 is a silver nitrate solution with the mass fraction of 0.5%;
(4) preparing at least 3 chloride ion standard solutions with known concentrations and different concentrations, and treating by adopting the method of the steps (1) to (3);
(5) and (3) comparison: and (3) placing the treated test solution and the chloride ion standard solution in a dark box, comparing the turbidity, and taking the chloride ion standard solution with the concentration similar to the turbidity of the treated test solution as the concentration of chloride ions in the turbid formed solution.
Preferably, the conditions of the centrifugal treatment in the step (1) are as follows: the rotating speed is 2000-3000r/min, and the centrifugation is 15-20 min.
Preferably, in the step (2), the volume ratio of the upper solution to the reagent 1 is 20-30: 2-5;
in the step (3), the volume ratio of the reagent 1 to the reagent 2 is 2-5: 2-5.
Further preferably, in the step (3), the volume ratio of the reagent 1 to the reagent 2 is 1: 1.
Preferably, in the step (2), the temperature of the water bath heating is 95 ℃.
Preferably, in the step (3), the volume after constant volume is the same as the volume of the test solution taken in the step (1).
Preferably, in the step (4), not less than 5 chloride ion standard solutions with known concentrations and different concentrations are prepared.
Further preferably, in the step (4), a chloride ion standard solution with an equal concentration difference is prepared. The invention adds centrifugal treatment in the detection process, and the centrifugal treatment is used as the first step for detecting the concentration of the chloride ions in the formed liquid. The specific operation is that the turbid formation solution is centrifuged for 15-20min under the condition of 2000-3000r/min, and the centrifuged upper formation solution is used for detecting chloride ions. The method is used for separating and removing suspended particles in the formed liquid, and the influence of macromolecular impurities on the turbidity of the formed liquid is eliminated.
The invention promotes the reaction of the nitric acid and the aluminum hydroxide suspended matter in the formation solution by using high temperature; meanwhile, the formed liquid is in an acid environment, and the aluminum hydroxide after decomposition is prevented from being separated out. Meanwhile, after the nitric acid is dissolved, the formed solution is cooled to room temperature, and then the subsequent operation is carried out, so that the interference of high temperature on silver chloride precipitation is eliminated. By the method, on the premise of not influencing silver chloride precipitation, aluminum hydroxide suspended matters in the formed liquid are eliminated, and the interference on detection is reduced, so that the accuracy of detecting chloride ions in the formed liquid by a turbidimetric method is improved.
Example 1:
taking the clarified formed liquid without chloride ions, and quantitatively adding sodium chloride to obtain test liquids with chloride ion concentrations of 0.0mg/L, 0.1mg/L, 0.2mg/L, 0.3mg/L and 0.4mg/L respectively. And (3) taking 20mL of test solutions with different concentrations respectively, putting the test solutions into a turbidimetric tube, sequentially adding 2mL of 34% nitric acid solution, shaking up, adding 2mL of 0.5% silver nitrate solution, shaking up, and fixing the volume to 25 mL. Standing for 15min, and then putting the turbidimetric tube into a dark box, and comparing with a standard solution to obtain the concentration of the formed liquid chloride ions.
The results of the measurements are shown in the following table:
TABLE 1 results of chloride ion concentration in clarified chemical-synthesis liquor measured by conventional method
As can be seen from the contents in Table 1, the concentration of chloride ions in the clarified test solution can be accurately distinguished by using the conventional silver chloride turbidimetry.
Example 2.
The procedure of example 2 is substantially the same as example 1, except that: the used formation liquid is turbid formation liquid without chloride ions.
The results of the measurements are shown in the following table:
TABLE 2 results of chloride ion concentration in turbid solutions detected by conventional method
As can be seen from the contents in Table 2, the conventional silver chloride turbidimetry cannot accurately distinguish the chloride ion concentration in the turbid test solution due to the influence of the suspended matter in the formation solution.
Example 3.
The procedure of example 3 is substantially the same as example 1, except that: the used formation liquid is upper formation liquid obtained by centrifuging turbid formation liquid without chloride ions. The centrifugation conditions were: the rotating speed is 3000r/min, and the processing time is 15 min.
The results of the measurements are shown in the following table:
TABLE 3 chloride ion concentration results of turbid solutions after centrifugation by conventional methods
As can be seen from the contents in Table 3, the efficacy of the turbidimetric silver chloride method for detecting the chloride ion concentration is slightly enhanced after the addition of the centrifugation treatment, but the chloride ion concentration in the turbid formed liquid can not be accurately distinguished.
Example 4.
The procedure of example 4 is substantially the same as example 3, except that: adding 0.5% silver nitrate solution, heating the turbidimetric tube in a water bath at 95 deg.C for 5min, cooling to room temperature, metering to 25ml, standing for 15min, placing the turbidimetric tube in a dark box, and comparing with standard solution to obtain the formed liquid chloride ion concentration.
The results of the measurements are shown in the following table:
TABLE 4 results of heat treatment and chloride ion concentration detection of turbid solution after centrifugation
As can be seen from table 4, the suspension in the formation liquid was almost disappeared and the formation liquid was clear after the addition of the centrifugation treatment and the heat treatment. However, the heating causes the solubility product of the silver chloride to change, and partial silver chloride precipitates are dissolved, so that the detection result is low.
Example 5.
The procedure of example 5 is substantially the same as example 3, except that: adding a nitric acid solution with the mass fraction of 34%, firstly placing the turbidimetric tube in a water bath kettle at 95 ℃ for heating for 5min, cooling to room temperature, adding 2ml of 0.5% silver nitrate solution, then fixing the volume to 25ml, standing for 15min, then placing the turbidimetric tube in a dark box, and comparing with a standard solution to obtain the concentration of the formed liquid chloride ions.
The results of the measurements are shown in the following table:
table 5 results of detecting chloride ion concentration of turbid centrifuged solution after partial heat treatment
As can be seen from the contents in table 5, the silver chloride turbidimetry can accurately distinguish the chloride ion concentration in the turbid chemical solution after adding centrifugation to remove suspended matters and promoting nitric acid acidification by heat treatment.
According to the invention, after the aluminum hydroxide suspended matter in the formation solution is dissolved by the high-temperature nitric acid, the formation solution is cooled to room temperature and then the subsequent operation is carried out, so that the influence of high temperature on silver chloride precipitation is avoided.
And (3) adding heat treatment in the middle section of the detection process to promote nitric acid digestion, namely adding nitric acid into the formed liquid to acidify the formed liquid, and then placing the formed liquid in a 95 ℃ water bath to carry out constant-temperature heat treatment for 4-6min, so that the decomposition of the aluminum hydroxide suspended solids in the solution by the nitric acid is promoted, and the interference of the aluminum hydroxide suspended solids in the formed liquid on turbidity is eliminated.
Example 6.
(1) 60ml of the test solution (turbid solution) is taken at normal temperature and is placed in a centrifuge tube, and the centrifuge tube is centrifuged for 20min under the condition of 2000r/min of rotation speed. And (3) putting 30ml of centrifuged upper layer test solution into a turbidimetric tube, adding 5ml of 34% nitric acid solution, shaking up, and heating in a water bath at 95 ℃ for 4-6 min.
Heating, taking out the turbidimetric tube, cooling to room temperature, adding 5ml of 0.5% silver nitrate solution, shaking, metering to 60ml, and standing for 20 min.
(2) Preparing 5 chloride ion standard solutions with known concentrations and different concentrations, and treating the standard solutions by using the method in the step (1), wherein the turbidity of the standard solutions is gradually increased along with the increase of the concentration of the contained chloride ions.
(3) And (3) placing the test solution and the standard solution in a dark box, comparing the turbidity of the test solution and the turbidity of the standard solution, and taking the concentration of the standard solution close to the turbidity of the test solution as the concentration of the test solution.
The actual concentration is the same as the detection result through testing.
Example 7.
(1) Taking 50ml of the test solution (turbid solution) at normal temperature, and centrifuging for 15min at the rotation speed of 2500 r/min. And (3) putting 20ml of centrifuged upper layer test solution into a turbidimetric tube, adding 3ml of 34% nitric acid solution, shaking up, and heating in a water bath at 95 ℃ for 4-6 min.
Heating, taking out the turbidimetric tube, cooling to room temperature, adding 3ml of 0.5% silver nitrate solution, shaking, metering to 50ml, and standing for 10 min.
(2) Preparing 5 chloride ion standard solutions with known concentrations and different concentrations, and treating the standard solutions by using the method in the step (1), wherein the turbidity of the standard solutions is gradually increased along with the increase of the concentration of the contained chloride ions.
(3) And (3) placing the test solution and the standard solution in a dark box, comparing the turbidity of the test solution and the turbidity of the standard solution, and taking the concentration of the standard solution close to the turbidity of the test solution as the concentration of the test solution.
The actual concentration is the same as the detection result through testing.
In conclusion, the method for detecting the concentration of chloride ions in the turbid forming solution can eliminate the influence of suspended impurities in the forming solution on the turbidity of the solution on the premise of not influencing the silver chloride precipitation reaction, improves the detection capability of the silver chloride turbidimetry, and provides a reliable and efficient method for large-scale detection of the concentration of chloride ions in the forming solution.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any simple modification, equivalent change and modification made to the above embodiments according to the technical spirit of the present invention are within the scope of the technical solution of the present invention.
Claims (8)
1. A method for detecting the concentration of chloride ions in a turbid formed liquid is characterized by comprising the following steps:
(1) taking the turbid formed solution as a test solution, carrying out centrifugal treatment, and layering the solution;
(2) adding reagent 1 into the layered upper layer solution, shaking, heating in water bath at 90-100 deg.C for 4-6min, and cooling to room temperature; the reagent 1 is a nitric acid solution with the mass fraction of 34%;
(3) adding the reagent 2 into the cooled reaction solution, uniformly mixing, fixing the volume, and standing for 10-20 min;
the reagent 2 is a silver nitrate solution with the mass fraction of 0.5%;
(4) preparing at least 3 chloride ion standard solutions with known concentrations and different concentrations, and treating by adopting the method of the steps (1) to (3);
(5) and (3) comparison: and (3) placing the treated test solution and the chloride ion standard solution in a dark box, comparing the turbidity, and taking the chloride ion standard solution with the concentration similar to the turbidity of the treated test solution as the concentration of chloride ions in the turbid formed solution.
2. The detection method according to claim 1,
the conditions of the centrifugal treatment in the step (1) are as follows: the rotating speed is 2000-3000r/min, and the centrifugation is 15-20 min.
3. The detection method according to claim 1,
in the step (2), the volume ratio of the upper layer solution to the reagent 1 is 20-30: 2-5;
in the step (3), the volume ratio of the reagent 1 to the reagent 2 is 2-5: 2-5.
4. The detection method according to claim 3,
in the step (3), the volume ratio of the reagent 1 to the reagent 2 is 1: 1.
5. The detection method according to claim 1,
in the step (2), the temperature of water bath heating is 95 ℃.
6. The detection method according to claim 1,
in the step (3), the volume after constant volume is the same as the volume of the test solution obtained in the step (1).
7. The detection method according to claim 1,
in the step (4), not less than 5 chloride ion standard solutions with known and different concentrations are prepared.
8. The detection method according to claim 7,
in the step (4), the prepared chloride ion standard solution with the equal differential concentration is used.
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Application publication date: 20210202 |