CN110658098A - Method for determining heavy metal elements in polymer coating - Google Patents
Method for determining heavy metal elements in polymer coating Download PDFInfo
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- CN110658098A CN110658098A CN201810686132.2A CN201810686132A CN110658098A CN 110658098 A CN110658098 A CN 110658098A CN 201810686132 A CN201810686132 A CN 201810686132A CN 110658098 A CN110658098 A CN 110658098A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
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Abstract
The invention relates to the field of detection, and discloses a method for determining heavy metal elements in a high polymer material coating, which is characterized by comprising the following steps of a, taking a plurality of grams of substrate coating samples with initial mass, putting the substrate coating samples into a container, b, adding dilute sulfuric acid solution with the volume ratio of dilute sulfuric acid to pure water being 3 ~ 8: 2 ~ 7 into the container, starting timing when the substrate coating samples are completely immersed by the dilute sulfuric acid solution, continuously and slightly oscillating or leaching for a plurality of minutes to dissolve a coating in the dilute sulfuric acid solution so as to separate the coating from a substrate, c, immediately separating the substrate coating samples from the dilute sulfuric acid solution, cleaning residual dilute sulfuric acid solution on the substrate for a plurality of times by using pure water, combining the solutions cleaned for a plurality of times, fixing the volume to a certain volume by using water to be determined, d, putting the cleaned substrate into an oven for constant temperature for a period of time, taking out, cooling to room temperature, drying for a period of time, e, transferring the mass of the weighed substrate to the coating, wherein the difference between the mass of the substrate and the initial mass of the coating samples is the coating dissolved by the dilute sulfuric acid solution, and the calculated.
Description
Technical Field
The invention relates to the field of detection, in particular to a method for determining heavy metal elements in a high polymer material coating.
Background
At present, metal or plastic elements or products of electronic and electric products are generally coated with high polymer materials, so that the metal or plastic elements or products have the effects of moisture resistance, rust prevention, corrosion prevention, easy cleaning and beautiful appearance. Since some metals in the polymer coating are harmful substances harmful to human health, regulations and instructions for limiting the harmful substances, such as ROHS directive in european union and CPSIA regulation in the united states, are issued in various countries, and thus it is necessary to separate the coating from the substrate and perform a separate analysis test. Because the base materials and the coatings of the coatings are classified more, the adhesion performance and the coating thickness of the coatings are greatly different, and a hand scraping method is adopted when the heavy metal in the coatings is generally measured, such as the measuring method of the heavy metal elements of the paint coatings disclosed in the application number 201010607630.7.
However, the above-described hand-scraping method often works inefficiently and sometimes is difficult to scrape off or mix into the substrate, which causes a decrease in measurement accuracy. Therefore, there is a need for a method for measuring a polymer coating that can maximally elute the polymer coating and maximally retain the substrate.
Disclosure of Invention
The invention provides a method for measuring heavy metal elements in a polymer material coating, which can ensure that the polymer material coating is dissolved out to the maximum extent and a matrix is reserved to the maximum extent.
In order to achieve the above object, the present invention provides a method for determining heavy metal elements in a polymer material coating, comprising:
firstly, taking a plurality of grams of matrix coating samples with initial mass and placing the samples into a container;
adding a dilute sulfuric acid solution with the volume ratio of dilute sulfuric acid to pure water being 3 ~ 8: 2 ~ 7 into a container, starting timing when the substrate coating sample is completely immersed by the dilute sulfuric acid solution, and continuously and slightly oscillating or leaching for several minutes to dissolve the coating into the dilute sulfuric acid solution so as to separate the coating from the substrate;
step three, immediately separating the substrate coating sample from the dilute sulfuric acid solution, washing residual dilute sulfuric acid solution on the substrate for multiple times by using pure water, combining the solutions washed for multiple times, and fixing the volume to a certain volume by using water to be measured;
step four, putting the cleaned substrate into an oven, keeping the temperature for a period of time, taking out the substrate, cooling the substrate to room temperature, and transferring the substrate into a dryer for constant-temperature drying for a period of time;
and step five, weighing the mass of the substrate, wherein the difference between the mass of the substrate and the initial mass of the substrate coating sample is the mass of the coating dissolved in the dilute sulfuric acid solution, and calculating the mass of the coating, namely the mass of the heavy metal element.
When the substrate coating is an iron-based coating, the volume ratio of dilute sulfuric acid to pure water in the dilute sulfuric acid solution added in the step two is 8: 2, the time of continuous gentle shaking was 2 minutes.
When the substrate plating layer is a copper-based nickel plating layer: and the volume ratio of the dilute sulfuric acid to the pure water in the dilute sulfuric acid solution added in the step two is 1: 1, the time of continuous gentle shaking was 1 minute.
And when the substrate coating is a zinc alloy substrate coating, the volume ratio of dilute sulfuric acid to pure water in the dilute sulfuric acid solution added in the step two is 1: 1, and the time of continuous slight oscillation is 1 ~ 2 minutes.
When the substrate plating layer is a copper-based nickel plating layer buckle: and the volume ratio of the dilute sulfuric acid to the pure water in the dilute sulfuric acid solution added in the step two is 3: 7, the time of continuous gentle shaking was 2 minutes.
When the base plating layer is a copper-based belt buckle plating layer: and the volume ratio of the dilute sulfuric acid to the pure water in the dilute sulfuric acid solution added in the step two is 3: 7, leaching time is 6 minutes.
When the matrix coating is a copper-based porous and small round buckle coating with gaps: and the volume ratio of the dilute sulfuric acid to the pure water in the dilute sulfuric acid solution added in the step two is 3: 7, the time of continuous gentle shaking was 3 minutes.
When the matrix plating layer is copper alloy sand-plated nickel: and the volume ratio of the dilute sulfuric acid to the pure water in the dilute sulfuric acid solution added in the step two is 1: 1, leaching time is 1 minute.
When the matrix coating is a polymer substrate coating: the dilute sulfuric acid solution added in the second step is concentrated dilute sulfuric acid, and is vibrated or placed on an oscillator from time to time until the coating is completely removed; in the fourth step, the polymer matrix is placed on a filter paper to suck water before the cleaned matrix is placed in an oven for a period of time under constant temperature.
The invention has the beneficial effects that: the method for determining the heavy metal elements in the high polymer material coating can rapidly remove the high polymer material coating, so that the high polymer material coating is dissolved out to the maximum extent, the matrix is reserved to the maximum extent, matrix interference can be introduced as little as possible, and the accuracy of determining the high polymer material coating is improved.
Detailed Description
In order to explain technical contents, structural features, and objects and effects of the present invention in detail, the following description is given in detail with reference to the embodiments.
The method for determining the heavy metal elements in the high polymer material coating comprises the following steps:
firstly, taking a plurality of grams of matrix coating samples with initial mass and placing the samples into a container; in this embodiment, the container is a beaker, but other suitable containers may be selected;
adding dilute sulfuric acid solution into the container, timing when the substrate coating sample is completely immersed by the dilute sulfuric acid solution, and continuously slightly oscillating or leaching for several minutes to dissolve the coating in the dilute sulfuric acid solution so as to separate the coating from the substrate;
step three, immediately separating the substrate coating sample from the dilute sulfuric acid solution, washing residual dilute sulfuric acid solution on the substrate for multiple times by using pure water, combining the solutions washed for multiple times, and fixing the volume to a certain volume by using water to be measured;
step four, putting the cleaned substrate into an oven, keeping the temperature for a period of time, taking out the substrate, cooling the substrate to room temperature, and transferring the substrate into a dryer for constant-temperature drying for a period of time;
and step five, weighing the mass of the substrate, wherein the difference between the mass of the substrate and the initial mass of the substrate coating sample is the mass of the coating dissolved in the dilute sulfuric acid solution, and calculating the mass of the coating, namely the mass of the heavy metal elements.
The concentration of the dilute sulfuric acid solution is different according to different characteristics of different substrate coatings, and the method for determining heavy metal elements in the polymer material coating is illustrated in detail in the invention.
The treatment steps of the metal-based coating (different treatments are carried out according to different coating matrixes):
example 1 (treatment of iron-based plating):
firstly, putting an iron-based plating layer sample with the initial mass of 1 ~ 10g into a beaker, wherein the iron-based plating layer sample is preferably dried by a dryer when the iron-based plating layer sample is properly sampled according to the size of a plating piece during sampling so that the mass of the iron-based plating layer sample is within 1-10 g;
adding a dilute sulfuric acid solution into the beaker, wherein the volume ratio of dilute sulfuric acid to pure water in the dilute sulfuric acid solution is 8: 2, pressing a stopwatch to start timing when the iron-based plating layer sample is completely immersed by the dilute sulfuric acid solution, and continuously and slightly oscillating for 2 minutes to dissolve the plating layer in the dilute sulfuric acid solution so as to separate the plating layer from the iron base;
step three, immediately separating the iron-based coating sample from the dilute sulfuric acid solution, immediately washing residual dilute sulfuric acid solution on the iron base for multiple times with a small amount of pure water, combining the solutions washed for multiple times, and fixing the volume to a certain volume with water to be measured;
step four, putting the cleaned iron base into a 105 ℃ oven, keeping the temperature for 1 hour, taking out, cooling to room temperature, and transferring into a dryer for constant-temperature drying for 30 minutes;
and step five, weighing the mass of the iron base dried in the step four, wherein the difference between the mass and the initial mass of the iron base coating sample is the mass of the coating dissolved in the dilute sulfuric acid solution, and the mass of the coating is calculated to be the mass of the heavy metal elements of the coating.
Example 2 (treatment of copper-based nickel plating layer):
firstly, putting a copper-based nickel-plating layer sample with the initial mass of 1 ~ 10g into a beaker, wherein the sample is properly sampled according to the size of a plated part during sampling, so that the mass of the plated part is within 1-10g, and the copper-based nickel-plating layer sample is preferably a sample dried by a dryer;
adding a dilute sulfuric acid solution into the beaker, wherein the volume ratio of dilute sulfuric acid to pure water in the dilute sulfuric acid solution is 1: 1, pressing a stopwatch to start timing when the copper-based nickel-plated layer sample is completely immersed by the dilute sulfuric acid solution, and continuously slightly oscillating for 1 minute to dissolve a plating layer in the dilute sulfuric acid solution so as to separate the plating layer from the copper base;
step three, immediately separating the copper-based nickel-plating layer sample from the dilute sulfuric acid solution, immediately washing the residual dilute sulfuric acid solution on the copper base by using pure water for a small amount of times, combining the solutions washed for a plurality of times, and using water to fix the volume to a certain volume for determination;
step four, putting the cleaned copper base into a 105 ℃ oven, keeping the temperature for 1 hour, taking out, cooling to room temperature, and transferring into a dryer for constant-temperature drying for 30 minutes;
and step five, weighing the mass of the copper base after drying in the step four, wherein the difference between the mass and the initial mass of the copper base nickel plating layer sample is the mass of the plating layer dissolved by the dilute sulfuric acid solution, and calculating the mass of the plating layer, namely the mass of the nickel metal element of the plating layer.
Example 3 (treatment of zinc alloy based coating):
firstly, taking a zinc alloy base coating sample with the initial mass of 1 ~ 10g and placing the zinc alloy base coating sample into a beaker, wherein the sample is properly taken according to the size of a coated piece during sampling, so that the mass of the zinc alloy base coating sample is within 1-10g, and the zinc alloy base coating sample is preferably a sample dried by a dryer;
adding a dilute sulfuric acid solution into the beaker, wherein the volume ratio of dilute sulfuric acid to pure water in the dilute sulfuric acid solution is 1: 1, pressing a stopwatch to start timing when the zinc alloy base coating sample is completely immersed by the dilute sulfuric acid solution, and continuously slightly oscillating for 1 minute to dissolve the coating in the dilute sulfuric acid solution so as to separate the coating from the zinc alloy base;
separating the zinc alloy base coating sample from the dilute sulfuric acid solution immediately, washing residual dilute sulfuric acid solution on the zinc alloy base with a small amount of pure water for multiple times immediately, combining the solutions washed for multiple times, and fixing the volume to a certain volume with water to be measured;
step four, putting the cleaned zinc alloy base into a 105 ℃ oven, keeping the temperature for 1 hour, taking out, cooling to room temperature, and transferring into a dryer for constant-temperature drying for 30 minutes;
step five, the mass of the zinc alloy base after drying in the step four is weighed, the difference between the mass and the initial mass of the zinc alloy base coating sample is the coating mass dissolved by the dilute sulfuric acid solution, and the calculated coating mass is the mass of the heavy metal elements of the coating.
Example 4 (treatment of copper-based button (shrimp button, small round button) with nickel plating):
taking a copper-based button nickel-plating layer sample with initial mass (the number of the shrimp buttons and the small round buttons is 3 ~ 5) and putting the copper-based button nickel-plating layer sample into a beaker, wherein the copper-based button nickel-plating layer sample is preferably dried by a dryer;
adding a dilute sulfuric acid solution into the beaker, wherein the volume ratio of dilute sulfuric acid to pure water in the dilute sulfuric acid solution is 3: 7, pressing a stopwatch to start timing when the copper-based button nickel-plated layer sample is completely immersed by the dilute sulfuric acid solution, and continuously and slightly oscillating for 2 minutes to dissolve the plating layer in the dilute sulfuric acid solution so as to separate the plating layer from the copper base;
separating the copper-based button nickel-plating layer sample from the dilute sulfuric acid solution immediately, washing residual dilute sulfuric acid solution on the copper base with a small amount of pure water for multiple times immediately, combining the solutions washed for multiple times, and metering the volume to a certain volume with water to be measured;
step four, putting the cleaned copper base into a 105 ℃ oven, keeping the temperature for 1 hour, taking out, cooling to room temperature, and transferring into a dryer for constant-temperature drying for 30 minutes;
and step five, weighing the mass of the copper base after drying in the step four, wherein the difference between the mass and the initial mass of the sample of the nickel-plated layer of the copper base button is the mass of the plated layer dissolved in the dilute sulfuric acid solution, and calculating the mass of the plated layer, namely the mass of the nickel metal element of the plated layer.
Example 5 (treatment of copper-based belt buckle plating):
taking a sample of an initial mass of copper-based belt fastener plating layer (the number of belt fasteners is 1) and putting the sample into a beaker; the copper-based belt buckle coating sample is preferably dried by a dryer;
adding a dilute sulfuric acid solution into the beaker, wherein the volume ratio of dilute sulfuric acid to pure water in the dilute sulfuric acid solution is 3: 7, when the copper-based belt buckle coating sample is completely immersed by the dilute sulfuric acid solution, pressing a stopwatch to start timing, and leaching for 6 minutes to enable the coating to be dissolved in the dilute sulfuric acid solution so as to be separated from the copper base;
step three, immediately separating a copper-based belt buckle coating sample from a dilute sulfuric acid solution, immediately washing residual dilute sulfuric acid solution on the copper base for multiple times with a small amount of pure water, combining the solutions washed for multiple times, and adding water to a constant volume to be determined;
step four, putting the cleaned copper base into a 105 ℃ oven, keeping the temperature for 1 hour, taking out, cooling to room temperature, and transferring into a dryer for constant-temperature drying for 30 minutes;
step five, weighing the mass of the copper base after drying in the step four, wherein the difference between the mass and the initial mass of the sample of the coating of the copper base belt buckle is the mass of the coating dissolved in the dilute sulfuric acid solution, and calculating the mass of the coating, namely the mass of the heavy metal elements of the coating.
Example 6 (treatment of copper-based small button plating with holes and gaps):
firstly, putting an initial mass sample of the copper-based small round button plating layer with holes and gaps (the number is 3 ~ 5) into a beaker, wherein the sample of the copper-based small round button plating layer with holes and gaps is preferably dried by a dryer;
adding a dilute sulfuric acid solution into the beaker, wherein the volume ratio of dilute sulfuric acid to pure water in the dilute sulfuric acid solution is 3: 7, pressing a stopwatch to start timing when the copper-based porous and small round buckle plating layer sample with the gap is completely immersed by the dilute sulfuric acid solution, and continuously slightly oscillating for 3 minutes to dissolve the plating layer in the dilute sulfuric acid solution so as to separate the plating layer from the copper base;
immediately separating a small button plating layer sample with holes and gaps on the copper base from a dilute sulfuric acid solution, immediately washing residual dilute sulfuric acid solution on the copper base for multiple times by using a small amount of pure water, combining the solutions washed for multiple times, and fixing the volume to a certain volume by using water to be measured;
step four, putting the cleaned copper base into a 105 ℃ oven, keeping the temperature for 1 hour, taking out, cooling to room temperature, and transferring into a dryer for constant-temperature drying for 30 minutes;
step five, the mass of the copper base after drying in the step four is weighed, the difference between the mass and the initial mass of the copper base small button plating layer sample with holes and gaps is the plating layer mass dissolved by the dilute sulfuric acid solution, and the calculated plating layer mass is the mass of the plating layer heavy metal elements.
Example 7 (treatment of copper alloy with sand nickel plating):
taking an initial mass of copper alloy sand-plated nickel (the number of the samples is 1) and placing the samples into a beaker; wherein, the copper alloy sand-plated nickel sample is preferably dried by a dryer;
adding a dilute sulfuric acid solution into the beaker, wherein the volume ratio of dilute sulfuric acid to pure water in the dilute sulfuric acid solution is 1: 1, when the copper alloy sand-plated nickel sample is completely immersed by the dilute sulfuric acid solution, pressing a stopwatch to start timing, and leaching for 1 minute to dissolve a plating layer in the dilute sulfuric acid solution so as to separate the plating layer from a copper base;
step three, immediately separating the copper alloy sand-plated nickel sample from the dilute sulfuric acid solution, immediately washing the residual dilute sulfuric acid solution on the copper base for multiple times with a small amount of pure water, combining the solutions washed for multiple times, and metering the volume to a certain volume with water to be measured;
step four, putting the cleaned copper base into a 105 ℃ oven, keeping the temperature for 1 hour, taking out, cooling to room temperature, and transferring into a dryer for constant-temperature drying for 30 minutes;
and step five, weighing the mass of the copper base after drying in the step four, wherein the difference between the mass and the initial mass of the copper alloy sand-plated nickel sample is the mass of the plating layer dissolved by the dilute sulfuric acid solution, and calculating the mass of the plating layer, namely the mass of the heavy metal elements of the plating layer.
Treatment step of polymer substrate coating
Example 8 (treatment of polymer substrate coating):
step one, taking 0.5-5.0 g of complete polymer substrate plating (plating piece) and putting the complete polymer substrate plating into a 50mL beaker;
step two, adding concentrated and dilute sulfuric acid into a beaker, completely immersing the polymer substrate coating (plated part) sample into the concentrated and dilute sulfuric acid as a standard, and vibrating the beaker or placing the beaker on an oscillator from time to time until the coating is completely removed;
step three, taking out the polymer matrix, putting the polymer matrix into another beaker, washing residual concentrated dilute sulfuric acid on the polymer matrix for multiple times by using a small amount of pure water, and completely combining the washing liquid and the extraction liquid and then fixing the volume to be measured;
placing the polymer matrix on filter paper to suck the residual water, placing the filter paper in an electric oven at 60 ℃ for 1 hour, taking out the polymer matrix, placing the polymer matrix to room temperature, and immediately transferring the polymer matrix into a silica gel dryer for 30 minutes;
step five, the quality of the polymer matrix after drying in the step four is weighed, the difference between the quality and the initial quality of a sample of the coating (plated part) of the polymer substrate is the quality of the coating dissolved by concentrated and diluted sulfuric acid, and the calculated quality of the coating is the quality of the heavy metal elements of the coating.
In conclusion, the method for determining heavy metal elements in the high polymer material coating can rapidly remove the high polymer material coating, so that the high polymer material coating is dissolved out to the maximum extent, the matrix is retained to the maximum extent, matrix interference can be introduced as little as possible, the determination accuracy of the high polymer material coating is improved, and the method is favorable for analyzing the high polymer material coating independently.
The present invention is not limited to the above-described embodiments, and various changes may be made by those skilled in the art, which changes are equivalent or similar to the present invention and are intended to be included within the scope of the appended claims.
Claims (9)
1. A method for measuring heavy metal elements in a high polymer material coating is characterized by comprising the following steps:
a. taking a matrix coating sample with the initial mass of a plurality of grams and placing the matrix coating sample into a container;
b. adding a dilute sulfuric acid solution with the volume ratio of dilute sulfuric acid to pure water being 3 ~ 8: 2 ~ 7 into the container, starting timing when the substrate coating sample is completely immersed by the dilute sulfuric acid solution, and continuously slightly shaking or leaching for several minutes to dissolve the coating in the dilute sulfuric acid solution so as to separate the coating from the substrate;
c. immediately separating the substrate coating sample from the dilute sulfuric acid solution, washing residual dilute sulfuric acid solution on the substrate for multiple times by using pure water, combining the solutions washed for multiple times, and metering the volume to a certain volume by using water to be measured;
d. putting the cleaned substrate into an oven, keeping the temperature constant for a period of time, taking out the substrate, cooling the substrate to room temperature, and transferring the substrate into a dryer for constant-temperature drying for a period of time;
e. weighing the mass of the substrate, wherein the difference between the mass of the substrate and the initial mass of the substrate coating sample is the mass of the coating dissolved in the dilute sulfuric acid solution, and calculating the mass of the coating, namely the mass of the heavy metal element.
2. The method for determining heavy metal elements in a polymer material coating according to claim 1, wherein: the matrix coating is an iron-based coating, and the volume ratio of dilute sulfuric acid to pure water in the dilute sulfuric acid solution added in the step two is 8: 2, the time of continuous gentle shaking was 2 minutes.
3. The method for determining heavy metal elements in a polymer material coating according to claim 1, wherein: the substrate plating layer is a copper-based nickel plating layer, and the volume ratio of dilute sulfuric acid to pure water in the dilute sulfuric acid solution added in the second step is 1: 1, the time of continuous gentle shaking was 1 minute.
4. The method for determining heavy metal elements in a polymer material coating according to claim 1, wherein the base coating is a zinc alloy base coating, the volume ratio of dilute sulfuric acid to pure water in the dilute sulfuric acid solution added in the second step is 1: 1, and the time for continuous slight oscillation is 1 ~ 2 minutes.
5. The method for determining heavy metal elements in a polymer material coating according to claim 1, wherein: the substrate plating layer is a copper-based button nickel plating layer, and the volume ratio of dilute sulfuric acid to pure water in the dilute sulfuric acid solution added in the second step is 3: 7, the time of continuous gentle shaking was 2 minutes.
6. The method for determining heavy metal elements in a polymer material coating according to claim 1, wherein: the base coating is a copper-based belt buckle coating, and the volume ratio of dilute sulfuric acid to pure water in the dilute sulfuric acid solution added in the step two is 3: 7, leaching time is 6 minutes.
7. The method for determining heavy metal elements in a polymer material coating according to claim 1, wherein: the matrix coating is a copper-based porous small-button coating with gaps, and the volume ratio of dilute sulfuric acid to pure water in the dilute sulfuric acid solution added in the step two is 3: 7, the time of continuous gentle shaking was 3 minutes.
8. The method for determining heavy metal elements in a polymer material coating according to claim 1, wherein: the matrix coating is copper alloy sand-plated nickel, and the volume ratio of dilute sulfuric acid to pure water in the dilute sulfuric acid solution added in the second step is 1: 1, leaching time is 1 minute.
9. The method for determining heavy metal elements in a polymer material coating according to claim 1, wherein: the matrix coating is a polymer substrate coating; the dilute sulfuric acid solution added in the second step is concentrated dilute sulfuric acid, and is vibrated or placed on an oscillator from time to time until the coating is completely removed; in the fourth step, the polymer matrix is placed on a filter paper to suck water before the cleaned matrix is placed in an oven for a period of time under constant temperature.
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