CN111272602A - Method for measuring Al content of zinc-aluminum coating - Google Patents
Method for measuring Al content of zinc-aluminum coating Download PDFInfo
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Abstract
The invention relates to the technical field of zinc alloy, and discloses a method for measuring the Al content of a zinc-aluminum coating, which comprises the following specific measurement steps: preparing 100g/L zinc matrix solution, weighing 10.0g collective zinc particles, placing the collective zinc particles in a 100mL beaker, adding a small amount of nitric acid to slowly dissolve the collective zinc particles, transferring the collective zinc particles into a 100mL volumetric flask, and fixing the volume; preparing 1000mg/L of aluminum standard stock solution, weighing 0.2500g of aluminum sheet, placing the aluminum sheet in a 100mL beaker, adding 20mL of hydrochloric acid and 15mL of nitric acid, dissolving, transferring the aluminum sheet into a 250mL volumetric flask, and fixing the volume. The test result of the determination method provided by the invention is basically consistent with the process design, meanwhile, the repeatability of the test result is high, the result is stable and credible, the significance to the actual detection is larger, the detection process is mature, the error is smaller, and the problem that the error is larger when the aluminum content of the steel wire coating of the bridge cable wire is determined intelligently according to the standard of the EDTA titration method can be solved.
Description
Technical Field
The invention relates to the technical field of zinc alloy, in particular to a method for measuring the Al content of a zinc-aluminum coating.
Background
In recent years, the rapid development of bridge construction in China, the performance of a bridge cable steel wire gradually evolves towards high strength and high anti-corrosion performance, an anti-corrosion coating is a first choice of a bridge steel wire coating by replacing an original zinc-aluminum alloy with the existing zinc-aluminum alloy, the aluminum content of the coating needs to be measured in the construction process, and the existing common detection methods include an EDTA titration method, an inductive coupling plasma emission spectrometry method and the like.
EDTA titration method belongs to manual titration, no instrument is needed, because manual titration is completely adopted, human factor interference is large, especially in the last step, titration is carried out by using lead nitrate standard titration solution to reach a red end point, how to define the red color, the observation time of each person is possibly different, and the detection result error is large, while the inductively coupled plasma emission spectrometry adopts an instrument for detection, the steel wire coating is required to be deplated in the early stage, the difference is that the EDTA titration method is used for carrying out manual titration on the deplated solution, the inductively coupled plasma emission spectrometry is used for analyzing the solution in a spectrometer, but the existing detection process for detecting the aluminum content of the steel wire by the inductively coupled plasma emission spectrometry is not mature, the steel wire immersion mode, the immersion time and the aluminum content in a zinc-aluminum pot have influence on the aluminum content of the steel wire coating, therefore, a method for measuring the Al content of the zinc-aluminum coating is needed to solve the problem that the error is large when the aluminum content of the steel wire coating of the bridge cable is measured by intelligently referring to the standard of an EDTA titration method.
Disclosure of Invention
Solves the technical problem
Aiming at the defects of the prior art, the invention provides a method for measuring the Al content of a zinc-aluminum coating, which solves the problem that the error is larger when the aluminum content of a bridge cable steel wire coating is measured intelligently according to the standard of an EDTA titration method.
Technical scheme
In order to achieve the purpose, the invention provides the following technical scheme:
a method for measuring the Al content of a zinc-aluminum coating comprises the following specific measurement steps:
preparation of the Primary solution
S1 Zinc matrix solution 100g/L
Weighing 10.0g of collective zinc particles, placing the collective zinc particles in a 100mL beaker, adding a small amount of nitric acid to slowly dissolve the collective zinc particles, transferring the collective zinc particles into a 100mL volumetric flask, and fixing the volume;
s2 preparing 1000mg/L standard aluminum stock solution
Weighing 0.2500g of aluminum sheet, placing the aluminum sheet in a 100mL beaker, adding 20mL of hydrochloric acid and 15mL of nitric acid, dissolving, transferring the aluminum sheet into a 250mL volumetric flask, and fixing the volume;
s3 preparing iron standard stock solution 1000mg/L
Weighing 0.2500g of metallic iron, placing the metallic iron in a 100mL beaker, adding 30mL of nitric acid, covering a watch glass, heating until the metallic iron is completely dissolved, boiling to remove nitrogen oxides, respectively transferring the metallic iron into 250mL volumetric flasks, and fixing the volume;
s4 preparing deplating solution
3.5g of analytically pure hexamethylenetetramine C6H12N4 were dissolved in 500mL of concentrated hydrochloric acid and diluted to 1000mL with ultrapure water.
S5 preparing Al standard stock solution and Fe standard stock solution 1000mg/L, diluting into working solution with different concentrations according to the national standard method [8] according to the requirement.
(II) preparation of sample solution
(1) Taking a straight galvanized steel wire, respectively cutting out samples with the length of about 100mm (3 samples with the length being more than 300mm) at two ends and the middle to be used as a parallel test sample A, cutting out a parallel test sample B by the same method, degreasing and drying the test sample by absolute ethyl alcohol, and respectively weighing the mass m (A)1 and the mass m (B) 1;
(2) accurately adding 200mL of deplating solution into two beakers, respectively placing the parallel test samples A and B into 2 beakers, completely immersing the test samples, making the test samples overhead by using a glass rod, enabling 3 test samples not to be in contact with each other, and turning over the test samples;
(3) observing the reaction condition of the surface of the sample, when hydrogen evolution (violent bubbling) obviously stops, finishing the deplating test, clamping the sample out by using tweezers, washing the sample for 3 times by using a small amount of water, wherein the total amount of the washed water is less than 30mL, the washed water is also kept in a corresponding beaker, washing the parallel test samples A and B by using ethanol, quickly absorbing water by using absorbent paper, and quickly drying by using hot air;
(4) respectively weighing mass m (A)2 and mass m (B)2 again, completely transferring the solution in the beaker into a 250mL volumetric flask, performing constant volume, respectively transferring 10mL of sample solution into a 100mL volumetric flask, performing constant volume, wherein the obtained solution is an upper machine to-be-tested solution for parallelly testing the samples A and B, and calculating the content of Al in the plating layer according to the percentage of the tested Al mass in the mass loss of the samples;
(5) and (3) testing the wire diameter of the steel wire after deplating so as to check the relevance between the quality of the coating and the content of elements in the coating by a national standard method [5 ].
(III) drawing of Standard Curve
According to the quality of the coating and the approximate aluminum content, roughly estimating that the Al concentration of the solution to be tested on the machine of the parallel test sample AB is 30-80 mg/L, the Zn concentration is 600-1500 mg/L, a small amount of Fe is contained, and a zinc matrix solution with the median of 1000mg/L is added into the standard curve.
(IV) results of sample testing
6 samples were taken: three aluminum-plated zinc wires with the diameter of 5.0mm and the diameter of 6.2mm are respectively used as test objects, a solution to be tested is prepared according to the preparation of the sample solution of the test, and the test is carried out according to the working curve.
Preferably, the mass fraction of the collective zinc particles is more than 99.9999%.
Preferably, the mass fraction of the aluminum sheet is more than 99.99%.
Preferably, the mass fraction of the metallic iron is more than 99.99%.
Preferably, the hydrochloric acid and the nitric acid are both priorities, and the experimental water is 18.2M omega cm deionized water.
Preferably, the standard stock solutions of Al and Fe can be selected from standard solutions with corresponding concentrations.
Preferably, the experimental instrument can be selected from an inductively coupled plasma emission spectrometer, a pure water generator and an electronic balance.
Advantageous effects
The invention provides a method for measuring the Al content of a zinc-aluminum coating, which has the following beneficial effects:
the test result of the determination method provided by the invention is basically consistent with the process design, meanwhile, the repeatability of the test result is high, the result is stable and credible, the significance to the actual detection is larger, the detection process is mature, the error is smaller, and the problem that the error is larger when the aluminum content of the steel wire coating of the bridge cable wire is determined intelligently according to the standard of the EDTA titration method can be solved.
Detailed Description
All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Further explaining a technical scheme provided by the invention:
a method for measuring the Al content of a zinc-aluminum coating comprises the following specific measurement steps:
preparation of the Primary solution
S1 Zinc matrix solution 100g/L
Weighing 10.0g of collective zinc particles, placing the collective zinc particles in a 100mL beaker, adding a small amount of nitric acid to slowly dissolve the collective zinc particles, transferring the collective zinc particles into a 100mL volumetric flask, and fixing the volume;
s2 preparing 1000mg/L standard aluminum stock solution
Weighing 0.2500g of aluminum sheet, placing the aluminum sheet in a 100mL beaker, adding 20mL of hydrochloric acid and 15mL of nitric acid into the beaker when the mass fraction of the aluminum sheet is more than 99.99%, dissolving the aluminum sheet, transferring the aluminum sheet into a 250mL volumetric flask, and fixing the volume;
s3 preparing iron standard stock solution 1000mg/L
Weighing 0.2500g of metallic iron, placing the metallic iron in a 100mL beaker, adding 30mL of nitric acid, covering a watch glass, heating until the metallic iron is completely dissolved, boiling to remove nitrogen oxides, respectively transferring the metallic iron into a 250mL volumetric flask, and fixing the volume;
s4 preparing deplating solution
3.5g of analytically pure hexamethylenetetramine C6H12N4 were dissolved in 500mL of concentrated hydrochloric acid and diluted to 1000mL with ultrapure water.
The hydrochloric acid and the nitric acid are both priorities, and the experimental water is 18.2M omega cm deionized water.
S5 preparing Al standard stock solution and Fe standard stock solution 1000mg/L, diluting into working solution with different concentrations according to the national standard method [8] according to the requirement.
(II) preparation of sample solution
(1) Taking a straight galvanized steel wire, respectively cutting out samples with the length of about 100mm (3 samples with the length being more than 300mm) at two ends and the middle to be used as a parallel test sample A, cutting out a parallel test sample B by the same method, degreasing and drying the test sample by absolute ethyl alcohol, and respectively weighing the mass m (A)1 and the mass m (B) 1;
(2) accurately adding 200mL of deplating solution into two beakers, respectively placing the parallel test samples A and B into 2 beakers, completely immersing the test samples, making the test samples overhead by using a glass rod, enabling 3 test samples not to be in contact with each other, and turning over the test samples;
(3) observing the reaction condition of the surface of the sample, when hydrogen evolution (violent bubbling) obviously stops, finishing the deplating test, clamping the sample out by using tweezers, washing the sample for 3 times by using a small amount of water, wherein the total amount of the washed water is less than 30mL, the washed water is also kept in a corresponding beaker, washing the parallel test samples A and B by using ethanol, quickly absorbing water by using absorbent paper, and quickly drying by using hot air;
(4) respectively weighing mass m (A)2 and mass m (B)2 again, completely transferring the solution in the beaker into a 250mL volumetric flask, performing constant volume, respectively transferring 10mL of sample solution into a 100mL volumetric flask, performing constant volume, wherein the obtained solution is an upper machine to-be-tested solution for parallelly testing the samples A and B, and calculating the content of Al in the plating layer according to the percentage of the tested Al mass in the mass loss of the samples;
(5) and (3) testing the wire diameter of the steel wire after deplating so as to check the relevance between the quality of the coating and the content of elements in the coating by a national standard method [5 ].
(III) drawing of Standard Curve
According to the quality of a coating and the approximate aluminum content, roughly estimating the Al concentration of an on-machine solution to be tested of a parallel test sample AB to be 30-80 mg/L, the Zn concentration to be 600-1500 mg/L and a small amount of Fe, adding a zinc matrix solution with the median value of 1000mg/L into a standard curve to keep the matching of matrixes so as to eliminate the influence of the matrixes on results, then adding an Al and Fe mixed standard solution, wherein the concentration of elements in the Al and Fe mixed standard series solution is shown in a table 1, and the Al and Fe standard storage solution can be a standard solution with corresponding concentration.
TABLE 1 concentration of elements/(mg. L) in Al and Fe mixed standard series solution-1)
(IV) results of sample testing
6 samples were taken: three aluminum-zinc plated steel wires with the diameter of 5.0mm and the diameter of 6.2mm are respectively used as test objects, a solution to be tested is prepared according to the preparation of a sample solution of the test, the test is carried out according to the working curve (refer to the table 1), the measured result is shown in the table 2, the calculation formula of the coating content is shown in the formula, and X is the actually measured concentration of the solution to be tested.
The formula:
TABLE 2 measurement results of Al and Fe in various samples
The experimental instrument can be selected from an inductively coupled plasma emission spectrometer, a pure water generator and an electronic balance.
The analytical wavelengths of the elements to be measured are shown in Table 3
Table 3 analytical line wavelength of elements
The spectrometer used in the experiment has the function of synchronous background correction, background interference and overlapping interference in the experiment are eliminated or reduced by adjusting and buckling background points and selecting analysis lines, the solution has high zinc content, the interference situation between spectral lines needs to be verified, an aluminum and iron standard solution series is configured, meanwhile, 1000mg/L zinc matrix solution is added, and the analysis lines selected according to the table 2 detect that the baseline separation and the interference-free situation between elements are achieved.
11 blank solutions were measured successively, the standard deviation of the measurement results was calculated, and the detection limit of the method was calculated as 3 times the standard deviation. Table 3 shows that the working curves of the elements have good linear relationship, and the linear coefficients and the detection limits of the element method are shown in table 4.
TABLE 4 detection limits and Linear Range of the method
The aluminum-zinc-plated steel wires with two specifications are independently detected for 11 times according to the processing method and the instrument conditions, and the calculated relative standard deviation (RSD, n is 11) is respectively 1.0-1.4% of aluminum and 2.1-4.8% of iron, which shows that the method has higher accuracy and precision.
The final plating solution contains a small amount of iron, the small amount of iron may be from the plating raw material or the steel wire itself, if the small amount of iron is from the steel wire itself, the part should be subtracted in the denominator when calculating the aluminum content, the small amount of steel wire itself is supposed to be corroded, the mass of iron is subtracted in the denominator of the formula, the result after recalculation is unchanged, and the source is uncertain, so the influence can be ignored in the calculation. The iron content does not affect the accuracy of the results.
The experimental result is mainly the detection result of the galvanized steel wire, the chemical component detection method of the galvanized steel wire can refer to the above method, but the general galvanized steel wire is mostly pure zinc as the raw material, aluminum, iron and the like are impurity elements, the content is less, so the linear range of the standard curve should be reduced, and the deplating solution should not be diluted. Because the content is too low after dilution, the detection is not easy.
From Table 4 we can see that there is no direct connection between the aluminium content of the coating and the quality of the coating, but only
The larger the quality of the plating layer is, the larger the quality difference before and after deplating is, and the larger the concentration of the matrix and the element to be tested in the solution tested on the computer is. The direct influence factors of the aluminum content in the coating are the aluminum content of the raw materials (zinc ingot and zinc aluminum ingot) and the hot-dip coating process. The low iron content of the experiment indicates that the deplating liquid has good protection on the matrix and basically does not affect the iron matrix, the process design range value of the aluminum content in the plating layer of the selected sample is 4.2-7.2%, the iron content is less than 0.03%, and the experimental values of the experiment are 4.71-7.05% of the aluminum content and 0.01-0.02% of the iron content. The test result is basically consistent with the process design, meanwhile, the repeatability of the test result is high, the result is stable and credible, the significance to actual detection is large, the detection process is mature, the error is small, and the problem that the error is large when the aluminum content of the steel wire coating of the bridge cable intelligently refers to the standard of an EDTA titration method can be solved.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. A method for measuring the Al content of a zinc-aluminum coating is characterized by comprising the following specific measuring steps:
preparation of the Primary solution
S1 Zinc matrix solution 100g/L
Weighing 10.0g of collective zinc particles, placing the collective zinc particles in a 100mL beaker, adding a small amount of nitric acid to slowly dissolve the collective zinc particles, transferring the collective zinc particles into a 100mL volumetric flask, and fixing the volume;
s2 preparing 1000mg/L standard aluminum stock solution
Weighing 0.2500g of aluminum sheet, placing the aluminum sheet in a 100mL beaker, adding 20mL of hydrochloric acid and 15mL of nitric acid, dissolving, transferring the aluminum sheet into a 250mL volumetric flask, and fixing the volume;
s3 preparing iron standard stock solution 1000mg/L
Weighing 0.2500g of metallic iron, placing the metallic iron in a 100mL beaker, adding 30mL of nitric acid, covering a watch glass, heating until the metallic iron is completely dissolved, boiling to remove nitrogen oxides, respectively transferring the metallic iron into 250mL volumetric flasks, and fixing the volume;
s4 preparing deplating solution
3.5g of analytically pure hexamethylenetetramine C6H12N4 were dissolved in 500mL of concentrated hydrochloric acid and diluted to 1000mL with ultrapure water.
S5 preparing Al standard stock solution and Fe standard stock solution 1000mg/L, diluting into working solution with different concentrations according to the national standard method [8] according to the requirement.
(II) preparation of sample solution
(1) Taking a straight galvanized steel wire, respectively cutting out samples with the length of about 100mm (3 samples with the length being more than 300mm) at two ends and the middle to be used as a parallel test sample A, cutting out a parallel test sample B by the same method, degreasing and drying the test sample by absolute ethyl alcohol, and respectively weighing the mass m (A)1 and the mass m (B) 1;
(2) accurately adding 200mL of deplating solution into two beakers, respectively placing the parallel test samples A and B into 2 beakers, completely immersing the test samples, making the test samples overhead by using a glass rod, enabling 3 test samples not to be in contact with each other, and turning over the test samples;
(3) observing the reaction condition of the surface of the sample, when hydrogen evolution (violent bubbling) obviously stops, finishing the deplating test, clamping the sample out by using tweezers, washing the sample for 3 times by using a small amount of water, wherein the total amount of the washed water is less than 30mL, the washed water is also kept in a corresponding beaker, washing the parallel test samples A and B by using ethanol, quickly absorbing water by using absorbent paper, and quickly drying by using hot air;
(4) respectively weighing mass m (A)2 and mass m (B)2 again, completely transferring the solution in the beaker into a 250mL volumetric flask, performing constant volume, respectively transferring 10mL of sample solution into a 100mL volumetric flask, performing constant volume, wherein the obtained solution is an upper machine to-be-tested solution for parallelly testing the samples A and B, and calculating the content of Al in the plating layer according to the percentage of the tested Al mass in the mass loss of the samples;
(5) and (3) testing the wire diameter of the steel wire after deplating so as to check the relevance between the quality of the coating and the content of elements in the coating by a national standard method [5 ].
(III) drawing of Standard Curve
According to the quality of the coating and the approximate aluminum content, roughly estimating that the Al concentration of the solution to be tested on the machine of the parallel test sample AB is 30-80 mg/L, the Zn concentration is 600-1500 mg/L, a small amount of Fe is contained, and a zinc matrix solution with the median of 1000mg/L is added into the standard curve.
(IV) results of sample testing
6 samples were taken: three aluminum-plated zinc wires with the diameter of 5.0mm and the diameter of 6.2mm are respectively used as test objects, a solution to be tested is prepared according to the preparation of the sample solution of the test, and the test is carried out according to the working curve.
2. The method for measuring the Al content in the zinc-aluminum coating according to claim 1, which is characterized in that: the mass fraction of the collective zinc particles is more than 99.9999 percent.
3. The method for measuring the Al content in the zinc-aluminum coating according to claim 1, which is characterized in that: the mass fraction of the aluminum sheet is more than 99.99%.
4. The method for measuring the Al content in the zinc-aluminum coating according to claim 1, which is characterized in that: the mass fraction of the metallic iron is more than 99.99%.
5. The method for measuring the Al content in the zinc-aluminum coating according to claim 1, which is characterized in that: the hydrochloric acid and the nitric acid are both priorities, and the experimental water is 18.2M omega cm deionized water.
6. The method for measuring the Al content in the zinc-aluminum coating according to claim 1, which is characterized in that: the standard stock solution of Al and Fe can be selected from standard solutions with corresponding concentrations.
7. The method for measuring the Al content in the zinc-aluminum coating according to claim 1, which is characterized in that: the experimental instrument can be selected from an inductively coupled plasma emission spectrometer, a pure water generator and an electronic balance.
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Application publication date: 20200612 |