CN102313690B - Rotating disk electrode method for quantitative testing of porosity of tinned steel plate - Google Patents
Rotating disk electrode method for quantitative testing of porosity of tinned steel plate Download PDFInfo
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Abstract
The invention relates to a rotating disk electrode method for quantitative testing of porosity of a tinned steel plate, which comprises the following steps: (1) drawing of a standard straight line: preparing standard solution with different iron ion contents, transferring the standard solution to a three-electrode system with rotating disc electrodes with the rotating speed alpha being 500-2000r/min, linearly scanning the cathode potential of the standard solution, and carrying out linear fitting of the current density under the potential beta, wherein beta is ranged from minus 0.45 to minus 0.10V; (2) packaging of a test piece: fixing the test pipe at the opening of a wild-mouth bottle filled with corrosive solution, and making the wild-mouth bottle inverted; (3) linear scanning of the cathode potential: transferring the corrosive solution in (2) into the three-electrode system with the rotating disc electrodes, and determining the current density at the potential beta; and (4) data processing. The invention has the advantages that the operation is easy, the use cost is low, and changes in the porosity of the tinned steel plate can be tested promptly, rapidly and accurately.
Description
Technical field
The present invention relates to the tin plate sheet surface detection technique, relate in particular to a kind of electrochemical method of testing the tin plate porosity.
Background technology
Ferrostan refers to that the two sides is coated with Low carbon cold rolling steel sheet or the steel band of pure tin.It is incorporated into the intensity of steel and mouldability among a kind of material with corrosion stability, tin-welding and the aesthetic property of tin.Because characteristics such as tin are nontoxic, ductility good, corrosion stability is good, ferrostan is widely applied in industries such as food industry, carrier loader, electron devices.
The tin plate structure of processing through soft heat is broadly divided into three layers: steel matrix, Fe-Sn alloy-layer and tin layer, and ideal tin layer is densification and atresia, and in fact tin coating always exists pin hole.Pin hole divides two classes, a class be the pin hole that reaches the iron layer, another kind of be the pin hole that reaches the tin iron alloy layer.Tin plate in use, there is " current potential counter-rotating " phenomenon in the tin layer under organic acid and oxygen free condition, tin is anodic coating with respect to iron, the tin layer is corroded, iron is protected.When the amount of pin hole and area reach certain value when above, the tin layer is rapidly dissolving just.In aqueous solution, tin coating but is cathodic electrodeposition coating with respect to iron, and this moment, iron was corroded.And in tank process processed, when having hole on the tin layer, the corrosion that the tin layer will be accelerated substrate produces the some rust, greatly reduces the corrosion stability of tin plate.In addition, along with the rising of metallic tin price and from saving the angle of metals resources, the tin coating forward slimming development of tin plate.Yet the result of tin plate slimming development has also increased it, and possibility of spot corrosion occurs, and therefore the life-span of tank also has been subject to seriously influencing.
The method of the porosity of existing test tin plate mainly is to analyze the iron solution value of tin plate by spectrophotometric method, and the size of iron solution value has characterized the size of the porosity of tin plate.Existing sample of the every detection of spectrophotometric method approximately needs 1 hour, and there is certain hysteresis quality in the detection of tin plate porosity, can not instruct timely the adjustment of production technology.
Summary of the invention
The object of the present invention is to provide a kind of rotating disk electrode (r.d.e) method of quantitative test tin plate porosity, the method can shorten the time that detection tin plate porosity spends, and can instruct timely the adjustment of production technology, in addition, the method is simple to operate, measures accurately.
The present invention is achieved in that a kind of rotating disk electrode (r.d.e) method of quantitative test tin plate porosity, and the method comprises the steps:
Step 1, the drafting of standard straight-line: at first prepare by dilute sulfuric acid, the corrosive liquid that hydrogen peroxide and distilled water evenly mix, then corrosive liquid is divided into some parts, the iron sulfate that adds different quality in every part of corrosive liquid, make the standard solution of different iron ion contents, standard solution is transferred in the three-electrode system that rotating disk electrode (r.d.e) is installed, connect electrochemical workstation, the rotating speed of setting rotating disk electrode (r.d.e) is α, α is 500～2000r/min, by using rotating disk electrode (r.d.e) standard solution is carried out cathode potential linear sweep, the current density value of standard solution under the β current potential of different iron concentrations carried out fitting a straight line, obtaining the straight-line equation of standard straight-line and this standard straight-line, β is-0.45～-0.10V;
The encapsulation of step 2, test pieces: tin plate to be measured is cut out a slice test pieces, then test pieces is fixed in bottle mouth position and the sealing of the wide-necked bottle that corrosive liquid is housed, subsequently wide-necked bottle is inverted, the inversion time is 5～30min;
Step 3, cathode potential linear sweep: open wide-necked bottle, solution in the wide-necked bottle is transferred in the three-electrode system that rotating disk electrode (r.d.e) is installed, connect electrochemical workstation, the rotating speed of setting rotating disk electrode (r.d.e) is α, by using rotating disk electrode (r.d.e) that solution is carried out cathode potential linear sweep, determine the current density value at β current potential place;
Step 4, data are processed: with the standard straight-line equation that obtains in the current density value substitution step 1 that records in the step 3, obtain iron concentration in the solution
, obtain the iron solution value of test pieces according to formula [1],
[1]
In the formula:
Iron solution value for test pieces;
Contain mass percentage concentration in the described corrosive liquid and be dilute sulfuric acid 18～26mL of 10～15%, mass percentage concentration is hydrogen peroxide 1～3mL of 30～36%, distilled water 20～30mL; Dilute sulfuric acid is slowly joined in the solution that is comprised of hydrogen peroxide and distilled water, mix and be mixed with corrosive liquid.
Corrosive liquid is divided into 5 parts, adds iron sulfate 5 parts of corrosive liquids are made the standard solution that iron concentration is respectively 20mg/L, 40mg/L, 60mg/L, 80mg/L and 100mg/L.
Described test pieces is circular, and the area of test pieces is 20～40cm
2
The present invention utilizes the characteristics of place, tin plate surface pore and corrosive liquid reaction meeting stripping ferric ion, combined with electrochemical analytical approach, the porosity of mensuration tin plate.The present invention tests in the tin plate porosity process and need not corrosive liquid is diluted, and has effectively avoided in using the spectrophotometric method process because iron ion content is too high, must dilute and the error brought corrosive liquid.The present invention is simple to operate, and use cost is low, and test result can directly show the height of tin plate porosity, is fit to very much on-the-spot fast detecting, can test out accurately real-time the variation of tin plate porosity.
Description of drawings
Fig. 1 is that the standard solution of different iron ion contents among the embodiment 1 is in the current density fitting a straight line at-0.45V current potential place;
Fig. 2 is that the standard solution of different iron ion contents among the embodiment 2 is in the current density fitting a straight line at-0.30V current potential place;
Fig. 3 is that the standard solution of different iron ion contents among the embodiment 3 is in the current density fitting a straight line at-0.10V current potential place.
Among the figure:---■---measures curve,---standard straight-line.
Embodiment
The invention will be further described below in conjunction with the drawings and specific embodiments.
Embodiment 1
A kind of rotating disk electrode (r.d.e) method of quantitative test tin plate porosity, the method comprises the steps:
The drafting of step 1, standard straight-line: at first get mass percentage concentration and be 10% dilute sulfuric acid 18mL, mass percentage concentration is 30% hydrogen peroxide 1mL, distilled water 20mL; Dilute sulfuric acid is slowly joined in the solution that is comprised of hydrogen peroxide and distilled water, mix and be mixed with corrosive liquid.Corrosive liquid is divided into 5 parts, adding iron sulfate is made iron concentration with 5 parts of corrosive liquids and is respectively 20mg/L, 40mg/L, 60mg/L, the standard solution of 80mg/L and 100mg/L, standard solution is transferred in the three-electrode system that rotating disk electrode (r.d.e) is installed, connect electrochemical workstation, described three-electrode system and electrochemical workstation are prior art, the rotating speed of setting rotating disk electrode (r.d.e) is α, α is 2000r/min, by using rotating disk electrode (r.d.e) standard solution is carried out cathode potential linear sweep, 5 parts of standard solution that obtain different iron concentrations equal at β-current density value under the 0.45V current potential, and referring to table 1.
The current density value of 5 parts of standard solution of the different iron concentrations of table 1 under-0.45V current potential
| Iron concentration (mg/L) | 20 | 40 | 60 | 80 | 100 |
| Current density (mA/cm 2) | 0.0517 | 0.0853 | 0.1064 | 0.1339 | 0.1740 |
5 parts of standard solution of different iron concentrations are carried out fitting a straight line at the current density value the under-0.45V current potential, obtain standard straight-line, referring to shown in Figure 1, the standard straight-line equation is:
In the formula,
Be iron concentration value (mg/L);
Step 2, zinc-plated encapsulation: freshly prepd No. 1 tin plate sample and No. 2 tin plate samples are cut out respectively a slice test pieces, and described test pieces is circular, and the area of test pieces is 20cm
2, then 2 test pieces being fixed in 2 bottle mouth positions that the wide-necked bottle of 39ml corrosive liquid is housed, the composition of this corrosive liquid is identical with corrosive liquid composition in the step 1, is sealed with rubber cushion and bottle cap, subsequently wide-necked bottle is inverted, and the inversion time is 30min;
Step 3, negative electrode linear sweep: open wide-necked bottle, solution in the wide-necked bottle is transferred in the three-electrode system that rotating disk electrode (r.d.e) is installed, connect electrochemical workstation, the setting rotating speed is 2000r/min, by using rotating disk electrode (r.d.e) that solution is carried out cathode potential linear sweep, determine the current density value at-0.45V current potential place.
Step 4, data are processed: with the standard straight-line equation that obtains in the current density value substitution step 1 that records in the step 3:
Obtain iron concentration in the solution
, obtain again the iron solution value of test pieces according to formula [1],
In the formula:
Iron solution value for test pieces;
Volume for corrosive liquid in the wide-necked bottle;
According to the method for step 1 in the present embodiment to step 4, the test result of No. 1 and No. 2 test pieces and prior art spectrophotometric method iron solution value are as shown in table 2.
The rotating disk electrode (r.d.e) method is analyzed iron solution value result and prior art spectrophotometric method iron solution value among table 2 embodiment 1
| Sample | Current density (mA/cm 2) | Iron concentration (mg/L) | Iron solution value (g/m 2) | Spectrophotometric method iron solution value (g/m 2) |
| No. 1 | 0.1658 | 97.62 | 1.9036 | 1.9704 |
| No. 2 | 0.1573 | 91.84 | 1.7909 | 1.8570 |
Can find out from table 2 test result, the iron solution value that uses the analysis of rotating disk electrode (r.d.e) method to obtain is very little with the numerical value difference of using spectrophotometric method to obtain, degree of accuracy is higher, and the very wide 10～100mg/L of ferric ion test concentrations of the present invention, can avoid in the spectrophotometric method because the error that the corrosive liquid dilution brings.
Embodiment 2
A kind of rotating disk electrode (r.d.e) method of quantitative test tin plate porosity, the method comprises the steps:
The drafting of step 1, standard straight-line: at first get mass percentage concentration and be 12% dilute sulfuric acid 22mL, mass percentage concentration is 33% hydrogen peroxide 2mL, distilled water 25mL; Dilute sulfuric acid is slowly joined in the solution that is comprised of hydrogen peroxide and distilled water, mix and be mixed with corrosive liquid.Corrosive liquid is divided into 5 parts, adding iron sulfate is made iron concentration with 5 parts of corrosive liquids and is respectively 20mg/L, 40mg/L, 60mg/L, the standard solution of 80mg/L and 100mg/L, standard solution is transferred in the three-electrode system that rotating disk electrode (r.d.e) is installed, connect electrochemical workstation, described three-electrode system and electrochemical workstation are prior art, the rotating speed of setting rotating disk electrode (r.d.e) is α, α is 1200r/min, by using rotating disk electrode (r.d.e) standard solution is carried out cathode potential linear sweep, 5 parts of standard solution that obtain different iron concentrations equal at β-current density value under the 0.30V current potential, and referring to table 3.
The current density value of 5 parts of standard solution of the different iron concentrations of table 3 under-0.30V current potential
| Iron concentration (mg/L) | 20 | 40 | 60 | 80 | 100 |
| Current density (mA/cm 2) | 0.0392 | 0.0668 | 0.0898 | 0.1094 | 0.1450 |
5 parts of standard solution of different iron concentrations are carried out fitting a straight line at the current density value the under-0.30V current potential, obtain standard straight-line, referring to shown in Figure 2, the standard straight-line equation is:
In the formula,
Be iron concentration value (mg/L);
Step 2, zinc-plated encapsulation: freshly prepd No. 3 tin plate samples and No. 4 tin plate samples are cut out respectively a slice test pieces, and described test pieces is circular, and the area of test pieces is 30cm
2, then 2 test pieces being fixed in 2 bottle mouth positions that the special wide-necked bottle of 49ml corrosive liquid is housed, the composition of this corrosive liquid is identical with corrosive liquid composition in the step 1, is sealed with rubber cushion and bottle cap, subsequently wide-necked bottle is inverted, and the inversion time is 20min;
Step 3, negative electrode linear sweep: open wide-necked bottle, solution in the wide-necked bottle is transferred in the three-electrode system, connect electrochemical workstation, the rotating speed of setting rotating disk electrode (r.d.e) is 1200r/min, by using rotating disk electrode (r.d.e) that solution is carried out negative electrode linear sweep, determine the current density value at-0.30V current potential place.
Step 4, data are processed: with the standard straight-line equation that obtains in the current density value substitution step 1 that records in the step 3:
Obtain iron concentration in the solution
, obtain again the iron solution value of test pieces according to formula [1],
In the formula:
Iron solution value for test pieces;
Area for test pieces.
According to the method for step 1 in the present embodiment to step 4, the test result of No. 3 and No. 4 test pieces and prior art spectrophotometric method iron solution value are as shown in table 4.
The rotating disk electrode (r.d.e) method is analyzed iron solution value result and prior art spectrophotometric method iron solution value among table 4 embodiment 2
| Sample | Current density (mA/cm 2) | Iron concentration (mg/L) | Iron solution value (g/m 2) | Spectrophotometric method iron solution value (g/m 2) |
| No. 3 | 2.75E-02 | 10.65 | 0.1740 | 0.1801 |
| No. 4 | 3.51E-02 | 16.64 | 0.2718 | 0.2793 |
Can find out from table 4 test result, the iron solution value that uses the analysis of rotating disk electrode (r.d.e) method to obtain is very little with the numerical value difference of using spectrophotometric method to obtain, degree of accuracy is higher, and the very wide 10～100mg/L of ferric ion test concentrations of the present invention, can avoid in the spectrophotometric method because the error that the corrosive liquid dilution brings.
Embodiment 3
A kind of rotating disk electrode (r.d.e) method of quantitative test tin plate porosity, the method comprises the steps:
The drafting of step 1, standard straight-line: at first get mass percentage concentration and be 15% dilute sulfuric acid 26mL, mass percentage concentration is 36% hydrogen peroxide 3mL, distilled water 30mL; Dilute sulfuric acid is slowly joined in the solution that is comprised of hydrogen peroxide and distilled water, mix and be mixed with corrosive liquid.Corrosive liquid is divided into 5 parts, adding iron sulfate is made iron concentration with 5 parts of corrosive liquids and is respectively 20mg/L, 40mg/L, 60mg/L, the standard solution of 80mg/L and 100mg/L, standard solution is transferred in the three-electrode system that rotating disk electrode (r.d.e) is installed, connect electrochemical workstation, described three-electrode system and electrochemical workstation are prior art, the rotating speed of setting rotating disk electrode (r.d.e) is α, α is 500r/min, by using rotating disk electrode (r.d.e) standard solution is carried out cathode potential linear sweep, 5 parts of standard solution that obtain different iron concentrations equal at β-current density value under the 0.10V current potential, and referring to table 5.
The current density value of 5 parts of standard solution of the different iron concentrations of table 5 under-0.10V current potential
| Iron concentration (mg/L) | 20 | 40 | 60 | 80 | 100 |
| Current density (mA/cm 2) | 0.0278 | 0.0471 | 0.0649 | 0.0755 | 0.0952 |
5 parts of standard solution of different iron concentrations are carried out fitting a straight line at the current density value the under-0.10V current potential, obtain standard straight-line, referring to shown in Figure 3, the standard straight-line equation is:
In the formula,
Be iron concentration value (mg/L);
Step 2, zinc-plated encapsulation: freshly prepd No. 5 tin plate samples and No. 6 tin plate samples are cut out respectively a slice test pieces, and described test pieces is circular, and the area of test pieces is 40cm
2, then 2 test pieces being fixed in 2 bottle mouth positions that the special wide-necked bottle of 59ml corrosive liquid is housed, the composition of this corrosive liquid is identical with corrosive liquid composition in the step 1, is sealed with rubber cushion and bottle cap, subsequently wide-necked bottle is inverted, and the inversion time is 5min;
Step 3, negative electrode linear sweep: open wide-necked bottle, solution in the wide-necked bottle is transferred in the three-electrode system, connect electrochemical workstation, the rotating speed of setting rotating disk electrode (r.d.e) is 500r/min, by using rotating disk electrode (r.d.e) that solution is carried out negative electrode linear sweep, determine the current density value at-0.10V current potential place.
Step 4, data are processed: with the standard straight-line equation that obtains in the current density value substitution step 1 that records in the step 3:
Obtain iron concentration in the solution
, obtain again the iron solution value of test pieces according to formula [1],
In the formula:
Iron solution value for test pieces;
Area for test pieces.
According to the method for step 1 in the present embodiment to step 4, the test result of No. 5 and No. 6 test pieces and prior art spectrophotometric method iron solution value are as shown in table 6.
The rotating disk electrode (r.d.e) method is analyzed iron solution value result and prior art spectrophotometric method iron solution value among table 6 embodiment 3
| Sample | Current density (mA/cm 2) | Iron concentration (mg/L) | Iron solution value (g/m 2) | Spectrophotometric method iron solution value (g/m 2) |
| No. 5 | 2.89E-02 | 19.22 | 0.2835 | 0.2971 |
| No. 6 | 8.48E-02 | 87.39 | 1.2890 | 1.3264 |
Can find out from table 6 test result, the iron solution value that uses the analysis of rotating disk electrode (r.d.e) method to obtain is very little with the numerical value difference of using spectrophotometric method to obtain, degree of accuracy is higher, and the very wide 10～100mg/L of ferric ion test concentrations of the present invention, can avoid in the spectrophotometric method because the error that the corrosive liquid dilution brings.
Claims (4)
1. the rotating disk electrode (r.d.e) method of a quantitative test tin plate porosity, it is characterized in that: the method comprises the steps:
Step 1, the drafting of standard straight-line: at first prepare by dilute sulfuric acid, the corrosive liquid that hydrogen peroxide and distilled water evenly mix, then corrosive liquid is divided into some parts, the iron sulfate that adds different quality in every part of corrosive liquid, make the standard solution of different iron ion contents, standard solution is transferred in the three-electrode system that rotating disk electrode (r.d.e) is installed, connect electrochemical workstation, the rotating speed of setting rotating disk electrode (r.d.e) is α, α is 500～2000r/min, by using rotating disk electrode (r.d.e) standard solution is carried out cathode potential linear sweep, the current density value of standard solution under the β current potential of different iron concentrations carried out fitting a straight line, obtaining the straight-line equation of standard straight-line and this standard straight-line, β is-0.45～-0.10V;
The encapsulation of step 2, test pieces: tin plate to be measured is cut out a slice test pieces, then test pieces is fixed in bottle mouth position and the sealing of the wide-necked bottle that corrosive liquid is housed, subsequently wide-necked bottle is inverted, the inversion time is 5～30min;
Step 3, cathode potential linear sweep: open wide-necked bottle, solution in the wide-necked bottle is transferred in the three-electrode system that rotating disk electrode (r.d.e) is installed, connect electrochemical workstation, the rotating speed of setting rotating disk electrode (r.d.e) is α, by using rotating disk electrode (r.d.e) that solution is carried out cathode potential linear sweep, determine the current density value at β current potential place;
Step 4, data are processed: with the standard straight-line equation that obtains in the current density value substitution step 1 that records in the step 3, obtain iron concentration in the solution
, obtain again the iron solution value of test pieces according to formula [1],
[1]
In the formula:
Iron solution value for test pieces;
2. the rotating disk electrode (r.d.e) method of quantitative test tin plate porosity according to claim 1, it is characterized in that: contain mass percentage concentration in the described corrosive liquid and be dilute sulfuric acid 18～26mL of 10～15%, mass percentage concentration is hydrogen peroxide 1～3mL of 30～36%, distilled water 20～30mL; Dilute sulfuric acid is slowly joined in the solution that is comprised of hydrogen peroxide and distilled water, mix and be mixed with corrosive liquid.
3. the rotating disk electrode (r.d.e) method of quantitative test tin plate porosity according to claim 2, it is characterized in that: corrosive liquid is divided into 5 parts, adds iron sulfate 5 parts of corrosive liquids are made the standard solution that iron concentration is respectively 20mg/L, 40mg/L, 60mg/L, 80mg/L and 100mg/L.
4. the rotating disk electrode (r.d.e) method of quantitative test tin plate porosity according to claim 1 is characterized in that: described test pieces is for circular, and the area of test pieces is 20～40cm
2
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