CN102169074A - Method for detecting heavy metal elements in metal coating - Google Patents
Method for detecting heavy metal elements in metal coating Download PDFInfo
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- CN102169074A CN102169074A CN 201010607634 CN201010607634A CN102169074A CN 102169074 A CN102169074 A CN 102169074A CN 201010607634 CN201010607634 CN 201010607634 CN 201010607634 A CN201010607634 A CN 201010607634A CN 102169074 A CN102169074 A CN 102169074A
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Abstract
The invention discloses a method for detecting heavy metal elements in a metal coating. The method comprises the steps of getting a substrate coating sample and putting the sample into a container; adding a nitric acid solution into the container; starting to time when the substrate coating sample is completely immersed in the nitric acid solution and keeping slightly shaking or leaching for several minutes so that the coating is dissolved into the nitric acid solution, thereby separating the coating from the substrate; separating the substrate coating sample from the nitric acid solution, washing the residual nitric acid solution left on the substrate with clean water many times, merging the residual solution which are cleaned out many times and adding water for constant volume to a certain volume for later detection; putting the cleaned substrate into a baking oven for a period of time at a constant temperature, then taking out for cooling to a room temperature and placing into a drier for drying for a period of time at a constant temperature; and weighing the mass of the substrate, wherein the difference between the mass of the substrate and the original mass of the substrate coating sample is the mass of the coating with dissolving of the nitric acid solution. The method of the invention enables the metal coating to be rapidly removed and to be dissolved out to a maximum while the substrate is reserved to a maximum, thereby improving accuracy of detecting the metal coating.
Description
Technical field
Patent of the present invention relates to determination of heavy metal elements method in a kind of coat of metal.
Background technology
At present, the metal of electric equipment products or plastics original paper or product generally all are coated with the coat of metal, make it to have protection against the tide, effect antirust, anticorrosion, easy to clean, elegant in appearance.And some coated metal belongs to the disadvantageous hazardous substance of health, therefore, each country has issued that the ROHS of the rules that limit these hazardous substances and instruction as European Union instructs and the CPSIA rules of the U.S. etc., so just need with coating with carry out independent analytical test after matrix separates.Because the classification of the base material of coating and coated metal is many, the adhesion property and the thickness of coating of coating are widely different, the method that all adopts hand to scrape during heavy metal in the general mensuration coating.
Yet the method that above-mentioned hand is scraped usually work efficiency lowly and sometimes is difficult to wipe off or sneak into matrix, and this has caused the reduction of measuring degree of accuracy.Therefore, press for and a kind ofly can make the coat of metal assay method that the coat of metal is dissolved to greatest extent and matrix is retained to greatest extent.
Summary of the invention
The invention provides and a kind ofly can make determination of heavy metal elements method in the coat of metal that the coat of metal is dissolved to greatest extent and matrix is retained to greatest extent.
For achieving the above object, the invention provides determination of heavy metal elements method in a kind of coat of metal, comprising:
Step 1 is got the some gram matrix coatings of initial mass sample and is put into container;
Step 2, the volume ratio that adds nitric acid and pure water in container is the salpeter solution of 3 ~ 8:2 ~ 7, this salpeter solution picks up counting during with the complete submergence of described matrix coating sample, separates with matrix thereby constantly slight vibration or leaching some minutes are dissolved in the salpeter solution coating;
Step 3 is separated described matrix coating sample immediately from described salpeter solution, repeatedly clean remaining salpeter solution on the matrix with pure water, merges the solution that repeatedly cleans, the water constant volume behind certain volume with to be determined;
Step 4 is put into constant temperature a period of time in the baking oven to the matrix of cleaning, and changes freeze-day with constant temperature a period of time in the exsiccator over to behind the taking-up cool to room temperature;
Step 5, the quality of weighing matrix, the difference of the quality of this matrix and matrix coating sample initial mass are the quality of coating under the salpeter solution dissolving, and the quality that calculates coating is the quality of heavy metal element.
When described matrix coating was iron-based coating, the volume ratio of nitric acid and pure water was 8:2 in the salpeter solution that adds in the described step 2, and constantly the time of slight vibration is 2 minutes.
When described matrix coating was copper base nickel coating: the volume ratio of nitric acid and pure water was 1:1 in the salpeter solution that adds in the described step 2, and constantly the time of slight vibration is 1 minute.
When described matrix coating was Zinc alloy based coating: the volume ratio of nitric acid and pure water was 1:1 in the salpeter solution that adds in the described step 2, and constantly the time of slight vibration is 1 ~ 2 minute.
When described matrix coating was copper base nickel coating button: the volume ratio of nitric acid and pure water was 3:7 in the salpeter solution that adds in the described step 2, and constantly the time of slight vibration is 2 minutes.
When described matrix coating was copper base belt hook coating: the volume ratio of nitric acid and pure water was 3:7 in the salpeter solution that adds in the described step 2, and leaching time is 6 minutes.
When described matrix coating was copper base band hole, band space roundlet button coating: the volume ratio of nitric acid and pure water was 3:7 in the salpeter solution that adds in the described step 2, and constantly the time of slight vibration is 3 minutes.
Described matrix coating is an aldary when plating husky nickel: the volume ratio of nitric acid and pure water is 1:1 in the salpeter solution that adds in the described step 2, and leaching time is 1 minute.
When described matrix coating was the polymer-matrix prime coat: the salpeter solution that adds in the described step 2 was a red fuming nitric acid (RFNA), vibrates frequently or places on the oscillator and taken off fully to coating; In the described step 4 matrix of cleaning being put into has polymeric matrix to place before constant temperature a period of time in the baking oven to blot this step of water on the filter paper.
Beneficial effect of the present invention: the determination of heavy metal elements method can be taken off the coat of metal fast in the coat of metal of the present invention, the coat of metal is dissolved to greatest extent, and matrix is retained to greatest extent, introducing matrix that can be the least possible disturbs, and has improved the accurate of coat of metal mensuration.
Embodiment
By describing technology contents of the present invention, structural attitude in detail, realized purpose and effect, give explanation below in conjunction with embodiment is detailed.
Determination of heavy metal elements method in the coat of metal of the present invention may further comprise the steps:
Step 1 is got the some gram matrix coatings of initial mass sample and is put into container; In the present embodiment, container is a beaker, certainly also can be according to selecting other appropriate containers;
Step 2 adds salpeter solution in container, this salpeter solution picks up counting during with the complete submergence of described matrix coating sample, separates with matrix thereby constantly slight vibration or leaching some minutes are dissolved in the salpeter solution coating;
Step 3 is separated described matrix coating sample immediately from described salpeter solution, repeatedly clean remaining salpeter solution on the matrix with pure water, merges the solution that repeatedly cleans, the water constant volume behind certain volume with to be determined;
Step 4 is put into constant temperature a period of time in the baking oven to the matrix of cleaning, and changes freeze-day with constant temperature a period of time in the exsiccator over to behind the taking-up cool to room temperature;
Step 5, the quality of title matrix, the difference of the quality of this matrix and matrix coating sample initial mass are the quality of coating under the salpeter solution dissolving, and the quality that calculates coating is the quality of heavy metal element.
The concentration of salpeter solution is different and different according to the characteristics of different matrix coatings, describes determination of heavy metal elements method in the coat of metal of the present invention below the present invention for example in detail.
The treatment step of Metal Substrate coating (difference according to the coating matrix is carried out different processing):
The processing of embodiment 1(iron-based coating):
Step 1 is got initial mass 1 ~ 10 gram iron-based coating sample and is put into beaker; Wherein, the size by plating piece during sampling is suitably taken a sample, and makes its quality in 1-10g, the dried sample of the preferred drying device of iron-based coating sample;
Step 2, in beaker, add salpeter solution, the volume ratio of nitric acid and pure water is 8:2 in the salpeter solution, and this salpeter solution is pressed stopwatch during with the complete submergence of described iron-based coating sample and picked up counting, and separates with iron-based thereby constantly slight vibration was dissolved in the salpeter solution coating in 2 minutes;
Step 3 is separated iron-based coating sample immediately from salpeter solution, repeatedly clean remaining salpeter solution on the iron-based on a small quantity with pure water immediately, merges the solution that repeatedly cleans, the water constant volume behind certain volume with to be determined;
Step 4 is put in 105 ℃ of baking ovens constant temperature to the iron-based of cleaning after 1 hour, takes out to change in the exsiccator freeze-day with constant temperature behind the cool to room temperature over to 30 minutes;
Step 5, the quality of dry back iron-based in the weighing step 4, the difference of this quality and iron-based coating sample initial mass is the quality of coating under the salpeter solution dissolving, and the quality that calculates coating is the quality of coating heavy metal element.
The processing of embodiment 2(copper base nickel coating):
Step 1 is got initial mass 1 ~ 10 gram copper base nickel coating sample and is put into beaker; Wherein, the size by plating piece during sampling is suitably taken a sample, and makes its quality in 1-10g, the dried sample of the preferred drying device of copper base nickel coating sample;
Step 2, in beaker, add salpeter solution, the volume ratio of nitric acid and pure water is 1:1 in the salpeter solution, and this salpeter solution is pressed stopwatch during with the complete submergence of described copper base nickel coating sample and picked up counting, and separates with the copper base thereby constantly slight vibration was dissolved in the salpeter solution coating in 1 minute;
Step 3 is separated copper base nickel coating sample immediately from salpeter solution, repeatedly clean remaining salpeter solution on the copper base on a small quantity with pure water immediately, merges the solution that repeatedly cleans, the water constant volume behind certain volume with to be determined;
Step 4 is put in 105 ℃ of baking ovens constant temperature to the copper base of cleaning after 1 hour, takes out to change in the exsiccator freeze-day with constant temperature behind the cool to room temperature over to 30 minutes;
Step 5, the quality of dry back copper base in the title step 4, the difference of this quality and copper base nickel coating sample initial mass is the quality of coating under the salpeter solution dissolving, and the quality that calculates coating is the quality of coating nickel metallic element.
The processing of the Zinc alloy based coating of embodiment 3():
Step 1 is got the Zinc alloy based coating sample of initial mass 1 ~ 10 gram and is put into beaker; Wherein, the size by plating piece during sampling is suitably taken a sample, and makes its quality in 1-10g, the dried sample of the preferred drying device of Zinc alloy based coating sample;
Step 2, in beaker, add salpeter solution, the volume ratio of nitric acid and pure water is 1:1 in the salpeter solution, and this salpeter solution is pressed stopwatch during with the complete submergence of described Zinc alloy based coating sample and picked up counting, and separates with Zinc alloy based thereby constantly slight vibration was dissolved in the salpeter solution coating in 1 minute;
Step 3 is separated Zinc alloy based coating sample immediately from salpeter solution, repeatedly clean remaining salpeter solution on Zinc alloy based on a small quantity with pure water immediately, merges the solution that repeatedly cleans, the water constant volume behind certain volume with to be determined;
Step 4 the Zinc alloy based constant temperature of cleaning that is put in 105 ℃ of baking ovens after 1 hour, is taken out and was changed in the exsiccator freeze-day with constant temperature behind the cool to room temperature over to 30 minutes;
Step 5 claims the Zinc alloy based quality in dry back in the step 4, and the difference of this quality and Zinc alloy based coating sample initial mass is the quality of coating under the salpeter solution dissolving, and the quality that calculates coating is the quality of coating heavy metal element.
The processing of embodiment 4(copper base button (shrimp button, roundlet button) nickel coating):
Step 1 is got initial mass (quantity of shrimp button, roundlet button is 3 ~ 5) copper base button nickel coating sample and is put into beaker; Wherein, the dried sample of the preferred drying device of copper base button nickel coating sample;
Step 2, in beaker, add salpeter solution, the volume ratio of nitric acid and pure water is 3:7 in the salpeter solution, and this salpeter solution is pressed stopwatch during with the complete submergence of described copper base button nickel coating sample and picked up counting, and separates with the copper base thereby constantly slight vibration was dissolved in the salpeter solution coating in 2 minutes;
Step 3 is separated copper base button nickel coating sample immediately from salpeter solution, repeatedly clean remaining salpeter solution on the copper base on a small quantity with pure water immediately, merges the solution that repeatedly cleans, the water constant volume behind certain volume with to be determined;
Step 4 is put in 105 ℃ of baking ovens constant temperature to the copper base of cleaning after 1 hour, takes out to change in the exsiccator freeze-day with constant temperature behind the cool to room temperature over to 30 minutes;
Step 5, the quality of dry back copper base in the title step 4, the difference of this quality and copper base button nickel coating sample initial mass is the quality of coating under the salpeter solution dissolving, and the quality that calculates coating is the quality of coating nickel metallic element.
The processing of embodiment 5(copper base belt hook coating):
Step 1 is got initial mass copper base belt hook coating (quantity of belt hook is 1) sample and is put into beaker; Wherein, the dried sample of the preferred drying device of copper base belt hook coating sample;
Step 2, in beaker, add salpeter solution, the volume ratio of nitric acid and pure water is 3:7 in the salpeter solution, and this salpeter solution is pressed stopwatch during with the complete submergence of described copper base belt hook coating sample and picked up counting, and separates with the copper base thereby leaching was dissolved in the salpeter solution coating in 6 minutes;
Step 3 is separated copper base belt hook coating sample immediately from salpeter solution, repeatedly clean remaining salpeter solution on the copper base on a small quantity with pure water immediately, merges the solution that repeatedly cleans, the water constant volume behind certain volume with to be determined;
Step 4 is put in 105 ℃ of baking ovens constant temperature to the copper base of cleaning after 1 hour, takes out to change in the exsiccator freeze-day with constant temperature behind the cool to room temperature over to 30 minutes;
Step 5, the quality of dry back copper base in the title step 4, the difference of this quality and copper base belt hook coating sample initial mass is the quality of coating under the salpeter solution dissolving, and the quality that calculates coating is the quality of coating heavy metal element.
The processing of embodiment 6(copper base band hole, band space roundlet button coating):
Step 1 is got initial mass copper base band hole, is with space roundlet button coating (quantity is 3 ~ 5) sample to put into beaker; Wherein, copper base band hole, the dried sample of the band space preferred drying device of roundlet button coating sample;
Step 2, in beaker, add salpeter solution, the volume ratio of nitric acid and pure water is 3:7 in the salpeter solution, this salpeter solution is pressed stopwatch during with described copper base band hole, band space roundlet button coating sample complete submergence and is picked up counting, and separates with the copper base thereby constantly slight vibration was dissolved in the salpeter solution coating in 3 minutes;
Step 3 is separated copper base band hole, band space roundlet button coating sample immediately from salpeter solution, repeatedly clean remaining salpeter solution on the copper base on a small quantity with pure water immediately, merges the solution that repeatedly cleans, the water constant volume behind certain volume with to be determined;
Step 4 is put in 105 ℃ of baking ovens constant temperature to the copper base of cleaning after 1 hour, takes out to change in the exsiccator freeze-day with constant temperature behind the cool to room temperature over to 30 minutes;
Step 5, the quality of dry back copper base in the title step 4, the difference of this quality and copper base band hole, band space roundlet button coating sample initial mass is the quality of coating under the salpeter solution dissolving, and the quality that calculates coating is the quality of coating heavy metal element.
The processing that embodiment 7(aldary plates husky nickel):
Step 1 is got the initial mass aldary and is plated husky nickel (quantity is 1) sample and put into beaker; Wherein, aldary plates the dried sample of the preferred drying device of husky nickel sample;
Step 2, in beaker, add salpeter solution, the volume ratio of nitric acid and pure water is 1:1 in the salpeter solution, presses stopwatch when this salpeter solution plates the complete submergence of husky nickel sample with described aldary and picks up counting, and separates with the copper base thereby leaching was dissolved in the salpeter solution coating in 1 minute;
Step 3 is plated aldary husky nickel sample immediately and is separated from salpeter solution, repeatedly cleans remaining salpeter solution on the copper base on a small quantity with pure water immediately, merges the solution that repeatedly cleans, the water constant volume behind certain volume with to be determined;
Step 4 is put in 105 ℃ of baking ovens constant temperature to the copper base of cleaning after 1 hour, takes out to change in the exsiccator freeze-day with constant temperature behind the cool to room temperature over to 30 minutes;
Step 5, the difference that claims the quality of dry back copper base in the step 4, this quality and aldary to plate husky nickel sample initial mass are the quality of coating of salpeter solution under dissolving, and the quality that calculates coating is the quality of coating heavy metal element.
The treatment step of polymer-matrix prime coat
The processing of embodiment 8(polymer-matrix prime coat):
Step 1 is got complete polymer-matrix prime coat (plating piece) 0.5-5.0 gram and is put into the 50mL beaker;
Step 2 adds red fuming nitric acid (RFNA) in beaker, this red fuming nitric acid (RFNA) is a standard with the complete submergence of described polymer-matrix prime coat (plating piece) sample, vibrates beaker frequently or beaker is placed on the oscillator until till coating taken off fully;
Step 3 is taken out polymeric matrix and is also put into another beaker, repeatedly cleans remaining red fuming nitric acid (RFNA) on this polymeric matrix on a small quantity with pure water, and washing lotion and extract are completely integrated afterwards constant volume with to be determined;
Step 4 places polymeric matrix and blots remaining water on the filter paper, and places in 60 ℃ of electric dry ovens 1 hour, take out be placed into room temperature after, change in the silica gel drier 30 minutes immediately over to;
Step 5, the quality of dry back polymeric matrix in the title step 4, the difference of this quality and polymer-matrix prime coat (plating piece) sample initial mass is the quality of coating under the red fuming nitric acid (RFNA) dissolving, and the quality that calculates coating is the quality of coating heavy metal element.
In sum, the determination of heavy metal elements method can be taken off the coat of metal fast in the coat of metal of the present invention, the coat of metal is dissolved to greatest extent, and matrix is retained to greatest extent, introducing matrix that can be the least possible disturbs, improve the degree of accuracy that the coat of metal is measured, helped the independent coat of metal is analyzed.
The present invention is not limited to above-mentioned embodiment, and those skilled in the art that also can make multiple variation in view of the above, but any and the present invention are equal to or similar variation all should be encompassed in the scope of claim of the present invention.
Claims (9)
1. determination of heavy metal elements method in the coat of metal comprises:
Step 1 is got the some gram matrix coatings of initial mass sample and is put into container;
Step 2, the volume ratio that adds nitric acid and pure water in container is the salpeter solution of 3 ~ 8:2 ~ 7, this salpeter solution picks up counting during with the complete submergence of described matrix coating sample, separates with matrix thereby constantly slight vibration or leaching some minutes are dissolved in the salpeter solution coating;
Step 3 is separated described matrix coating sample immediately from described salpeter solution, repeatedly clean remaining salpeter solution on the matrix with pure water, merges the solution that repeatedly cleans, the water constant volume behind certain volume with to be determined;
Step 4 is put into constant temperature a period of time in the baking oven to the matrix of cleaning, and changes freeze-day with constant temperature a period of time in the exsiccator over to behind the taking-up cool to room temperature;
Step 5, the quality of weighing matrix, the difference of the quality of this matrix and matrix coating sample initial mass are the quality of coating under the salpeter solution dissolving, and the quality that calculates coating is the quality of heavy metal element.
2. determination of heavy metal elements method in the coat of metal according to claim 1, it is characterized in that: described matrix coating is an iron-based coating, the volume ratio of nitric acid and pure water is 8:2 in the salpeter solution that adds in the described step 2, and constantly the time of slight vibration is 2 minutes.
3. determination of heavy metal elements method in the coat of metal according to claim 1, it is characterized in that: described matrix coating is a copper base nickel coating, the volume ratio of nitric acid and pure water is 1:1 in the salpeter solution that adds in the described step 2, and constantly the time of slight vibration is 1 minute.
4. determination of heavy metal elements method in the coat of metal according to claim 1, it is characterized in that: described matrix coating is Zinc alloy based coating, the volume ratio of nitric acid and pure water is 1:1 in the salpeter solution that adds in the described step 2, and constantly the time of slight vibration is 1 ~ 2 minute.
5. determination of heavy metal elements method in the coat of metal according to claim 1, it is characterized in that: described matrix coating is a copper base button nickel coating, the volume ratio of nitric acid and pure water is 3:7 in the salpeter solution that adds in the described step 2, and constantly the time of slight vibration is 2 minutes.
6. determination of heavy metal elements method in the coat of metal according to claim 1, it is characterized in that: described matrix coating is a copper base belt hook coating, the volume ratio of nitric acid and pure water is 3:7 in the salpeter solution that adds in the described step 2, and leaching time is 6 minutes.
7. determination of heavy metal elements method in the coat of metal according to claim 1, it is characterized in that: described matrix coating is copper base band hole, band space roundlet button coating, the volume ratio of nitric acid and pure water is 3:7 in the salpeter solution that adds in the described step 2, and constantly the time of slight vibration is 3 minutes.
8. determination of heavy metal elements method in the coat of metal according to claim 1, it is characterized in that: described matrix coating is that aldary plates husky nickel, the volume ratio of nitric acid and pure water is 1:1 in the salpeter solution that adds in the described step 2, and leaching time is 1 minute.
9. determination of heavy metal elements method in the coat of metal according to claim 1 is characterized in that: described matrix coating is the polymer-matrix prime coat; The salpeter solution that adds in the described step 2 is a red fuming nitric acid (RFNA), vibrates frequently or places on the oscillator and taken off fully to coating; In the described step 4 matrix of cleaning being put into has polymeric matrix to place before constant temperature a period of time in the baking oven to blot this step of water on the filter paper.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102507364A (en) * | 2011-10-27 | 2012-06-20 | 四川中自尾气净化有限公司 | Surface coating deadsorbing and content determining method for catalytic converter |
| CN103353432A (en) * | 2013-06-14 | 2013-10-16 | 江苏法尔胜材料分析测试有限公司 | Detection method of plated layer corrosion rate in steel wire or steel wire rope |
| CN104880378A (en) * | 2015-05-08 | 2015-09-02 | 大禹节水（天津）有限公司 | Method for measuring copper content in copper-containing master batch for copper root removal dripper |
| CN106442065A (en) * | 2016-10-28 | 2017-02-22 | 东莞出入境检验检疫局检验检疫综合技术中心 | Solvent separation method for coating and soft rubber |
| CN110987998A (en) * | 2019-12-12 | 2020-04-10 | 山东东岳高分子材料有限公司 | Method for testing inorganic coating amount on surface of polymer film material |
-
2010
- 2010-12-28 CN CN 201010607634 patent/CN102169074A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 《YB/T 135-1998 镀铜钢丝镀层重量及其组分试验方法》 19981201 朱永刚等 YB/T 135-1998 镀铜钢丝镀层重量及其组分试验方法 , 1 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102507364A (en) * | 2011-10-27 | 2012-06-20 | 四川中自尾气净化有限公司 | Surface coating deadsorbing and content determining method for catalytic converter |
| CN102507364B (en) * | 2011-10-27 | 2014-03-05 | 四川中自尾气净化有限公司 | Surface coating deadsorbing and content determining method for catalytic converter |
| CN103353432A (en) * | 2013-06-14 | 2013-10-16 | 江苏法尔胜材料分析测试有限公司 | Detection method of plated layer corrosion rate in steel wire or steel wire rope |
| CN104880378A (en) * | 2015-05-08 | 2015-09-02 | 大禹节水（天津）有限公司 | Method for measuring copper content in copper-containing master batch for copper root removal dripper |
| CN104880378B (en) * | 2015-05-08 | 2017-11-03 | 大禹节水（天津）有限公司 | A kind of copper that determines is dispelled the method for copper content in root water dropper cupric masterbatch |
| CN106442065A (en) * | 2016-10-28 | 2017-02-22 | 东莞出入境检验检疫局检验检疫综合技术中心 | Solvent separation method for coating and soft rubber |
| CN106442065B (en) * | 2016-10-28 | 2018-11-23 | 东莞出入境检验检疫局检验检疫综合技术中心 | A method of it is separated for coating with flexible glue solvent |
| CN110987998A (en) * | 2019-12-12 | 2020-04-10 | 山东东岳高分子材料有限公司 | Method for testing inorganic coating amount on surface of polymer film material |
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Application publication date: 20110831 |