CN112683611B - Digestion solution and method for determining element content in refined aluminum ingot for remelting - Google Patents
Digestion solution and method for determining element content in refined aluminum ingot for remelting Download PDFInfo
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Abstract
The invention relates to a digestion solution and a method for determining the content of elements in a refined aluminum ingot for remelting, belongs to the field of alloy element analysis, and solves the problem of low efficiency in determining the content of elements in the refined aluminum ingot for remelting in the prior art. The digestion solution comprises a lead standard solution and a mixed acid solution. The method comprises the following steps: pretreating a sample; digesting the sample by using a digestion solution, transferring the digested sample to a volumetric flask, diluting and shaking up to obtain a sample solution; carrying out a blank test along with the sample, adding a certain amount of liquid standard substance into a blank test solution, preparing not less than 3 standard solutions in a volumetric flask, fixing the volume, and shaking up to form a series of standard solutions; sequentially carrying out spectral intensity measurement on each element in the series of standard solutions by using ICP-OES, selecting a proper characteristic spectral line, and establishing a working curve; and (4) measuring the sample solution to obtain the spectral intensity of the related elements in the sample, and calculating the content of the related elements in the sample according to the working curve. The method of the invention accelerates the dissolution rate and improves the efficiency.
Description
Technical Field
The invention relates to the technical field of alloy element component detection, in particular to a digestion solution and a method for determining element content in a refined aluminum ingot for remelting.
Background
The aluminum content of the refined aluminum ingot for remelting is generally 99.95% -99.998%. The composition requirement of the refined aluminum ingot for remelting according to the national standard GB/T8644-2000 is (wt%): designation al99.996: not less than 99.996% of Al, not more than 0.001% of Fe, not more than 0.001% of Si, not more than 0.0015% of Cu, not more than 0.001% of Zn and not more than 0.001% of Ti; designation al99.993: not less than 99.993% of Al, not more than 0.0015% of Fe, not more than 0.0013% of Si, not more than 0.003% of Cu, not more than 0.001% of Zn and not more than 0.001% of Ti; trade mark al99.99: not less than 99.99% of Al, not more than 0.003% of Fe, not more than 0.003% of Si, not more than 0.005% of Cu, not more than 0.002% of Zn and not more than 0.002% of Ti; trade mark al99.95: not less than 99.95% of Al, not more than 0.02% of Fe, not more than 0.02% of Si, not more than 0.01% of Cu, not more than 0.005% of Zn and not more than 0.002% of Ti; the contents of Fe, si, cu, zn, ti and other elements in the refined aluminum ingot for remelting play an important role in the final content composition of a remelting product, and are important indexes for checking and accepting the chemical components of the refined aluminum ingot material for remelting. At present, the detection of the element content in the refined aluminum ingot for remelting is generally carried out by methods of GB/T7999 and GB/T20975. GB/T7999 utilizes the photoemission spectrometer to detect aluminium and aluminum alloy multielement content, and this method easy operation, detection speed is fast, but can only detect to the bulk material of specific specification. GB/T20975 is a series of chemical analysis methods for aluminum and aluminum alloys, including the classical method and the ICP-OES method. The ICP-OES method is a method for detecting the content of material elements by using an inductively coupled plasma atomic emission spectrometer (ICP-OES), and is high in detection speed and high in detection precision. The lower limit of the detection range of elements in GB/T20975.25-2008 < aluminum and aluminum alloy chemical analysis method part 25 of inductively coupled plasma atomic emission spectrometry > is 0.002% -2% of Fe and 0.5% -10% of Si, the detection requirements of Fe and Si element contents in refined aluminum cannot be met, and the detection method cannot be used for detecting Fe, si, cu, zn, ti and other element contents in refined aluminum ingots for remelting.
In addition, the rate of sample dissolution in GB/T20975.25-2008 is slow, the detection time is greatly prolonged, and the detection efficiency is low.
Disclosure of Invention
In view of the above analysis, the present invention aims to provide a digestion solution and a method for determining the content of elements in a refined aluminum ingot for remelting, so as to solve the problems of long time and low efficiency of the determination process of the content of elements in the existing refined aluminum ingot for remelting.
On one hand, the invention provides a digestion solution for measuring the element content in a refined aluminum ingot for remelting, which comprises a lead standard solution and a mixed acid solution.
Further, the medium type in the lead standard solution is HNO 3 。
Further, the mixed acid solution is hydrochloric acid: nitric acid: the volume ratio of water is 4-7.
On the other hand, the invention also provides a method for measuring the element content in the refined aluminum ingot for remelting, and the digestion solution is adopted to digest a sample of the refined aluminum ingot for remelting.
Further, the method comprises:
s1, sample pretreatment;
s2, digesting the sample by using a digestion solution, transferring the digested sample to a volumetric flask, diluting and shaking up to obtain a sample solution;
s3, preparing a series of standard solutions: carrying out a blank test along with a sample, adding a certain amount of liquid standard substance into blank test solution according to the content range of elements to be tested, preparing not less than 3 standard solutions in a volumetric flask, and carrying out constant volume and shaking up to form a series of standard solutions;
s4, using ICP-OES to sequentially perform spectral intensity measurement on each element in the series of standard solutions, selecting a proper characteristic spectral line, and establishing a working curve;
and S5, measuring the sample solution by using ICP-OES to obtain the spectral intensity of the related elements in the sample, and calculating the content of the related elements in the sample according to the working curve.
Further, the S1 includes:
and (3) placing the refined aluminum ingot sample for remelting in a hydrochloric acid solution, heating and boiling, cooling, washing with deionized water, and drying.
Further, the S2 includes:
s21, weighing a preprocessed refined aluminum ingot sample for remelting and placing the sample into a conical flask;
s22, sequentially adding the diluted lead standard solution and the mixed acid solution into a conical flask, and heating at low temperature to enable a refined aluminum ingot sample for remelting to be digested;
s23, after digestion is completed, adding deionized water to wash the bottle wall, continuously heating to boil, immediately cooling, transferring to a volumetric flask, diluting to a constant volume, and shaking up to be measured.
Further, in S21 and S22, the ratio of the refined aluminum ingot sample for remelting, the diluted lead standard solution, and the mixed acid solution is 0.5 g.
Further, in the step S22, the temperature of the low-temperature heating process is 50 to 60 ℃.
Further, the linear correlation coefficient γ of the operation curve established in S4 is equal to or greater than 0.999.
Compared with the prior art, the invention can realize at least one of the following beneficial effects:
1. according to the invention, a lead standard solution and an inorganic mixed acid system are adopted in the process of dissolving the refined aluminum ingot for remelting, lead ions are replaced by impurity elements such as Fe, cu, zn and the like in the refined aluminum ingot for remelting to obtain metallic lead, the metallic lead and other metals form a primary battery to form the anode and the cathode of the primary battery, so that an electrolytic reaction generated in the dissolving process is a primary battery process, the dissolving speed is greatly accelerated, the sample digestion is reduced, the efficiency is improved, and all components in the refined aluminum ingot for remelting are completely digested to obtain a clear solution.
2. The lead standard solution is added into the digestion solution, so that the influence of other impurities on the detection result is avoided, and the detection result is more accurate.
3. The digestion solution does not adopt hydrofluoric acid with extremely strong corrosivity, avoids using hydrofluoric acid in the process of digesting the refined aluminum ingot for remelting, has relatively low requirements on equipment, utensils and the like, and can be universally used in a laboratory.
In the invention, the technical schemes can be combined with each other to realize more preferable combination schemes. Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The objectives and other advantages of the invention will be realized and attained by the structure particularly pointed out in the written description.
Detailed Description
The following detailed description is of the preferred embodiments of the invention, which are intended to be illustrative of the principles of the invention and not limiting in scope.
The aluminum content of the refined aluminum ingot for remelting is generally 99.95% -99.998%. Although the contents of Fe, si, cu, zn, ti and other elements in the refined aluminum ingot for remelting are low, the contents of the elements play an important role in the final content composition of a remelted product and are important indexes for the acceptance of chemical components of the refined aluminum ingot material for remelting. At present, the ICP-OES method in GB/T20975 is often adopted to detect the element content in the refined aluminum ingot for remelting, and the following problems exist: the rate of dissolving the sample is slow and the detection efficiency is low.
Based on the above problems, the present invention provides a digestion solution for determining the element content in a refined aluminum ingot for remelting, the digestion solution comprising: lead standard solutions and mixed acid solutions.
Specifically, the sample number of the lead standard solution is GSB 04-1742-2004, the mass concentration of lead in the lead standard solution is 1000 mu g/mL, and the medium type is HNO 3 The concentration of the nitric acid is as follows: 1.0mol/L. Specifically, in the present invention, the lead standard solution is diluted so that the lead mass concentration is 100. Mu.g/mL.
Specifically, considering that the excessive concentration of the nitric acid can oxidize an ICP-OES sample injection system and further shorten the service life of the ICP-OES sample injection system, the mixed acid solution is controlled to be hydrochloric acid: nitric acid: the volume ratio of water is 4-7. Exemplary, hydrochloric acid: nitric acid: the volume ratio of water is 6. Wherein, the concentration of the hydrochloric acid is 5.2mol/L, and the concentration of the nitric acid is 1.2mol/L.
The invention provides a method for determining the content of elements in a refined aluminum ingot for remelting.
The method comprises the following steps:
s1, preprocessing a sample;
s2, digesting the sample by using a digestion solution comprising a lead standard solution and a mixed acid solution, transferring the digested sample to a volumetric flask, diluting and shaking up to obtain a sample solution;
s3, preparing a series of standard solutions: carrying out a blank test along with a sample, adding a certain amount of liquid standard substance into blank test solution according to the content range of elements to be tested, preparing not less than 3 standard solutions into a 100mL volumetric flask, and carrying out constant volume and shaking up to form a series of standard solutions;
the content of elements to be detected in the series of standard solutions forms a gradient from low to high, and the linear range contains the content of the elements to be detected;
s4, using ICP-OES to sequentially perform spectral intensity measurement on each element in the series of standard solutions, selecting a proper characteristic spectral line, and establishing a working curve;
and S5, measuring the sample solution by using ICP-OES to obtain the spectral intensity of the related elements in the sample, and calculating the content of the related elements in the sample according to the working curve.
Specifically, in S1, considering that a trace amount of impurities such as iron may be introduced during the machining process, in order to remove the impurities on the surface of the sample, the sample pretreatment includes the following steps: placing a refined aluminum ingot sample for remelting in a hydrochloric acid solution (the volume ratio of hydrochloric acid to water is 1).
Specifically, in S2, the mass concentration of lead in the lead standard solution is 1000 mug/mL, and the type of the medium is HNO 3 The concentration of the nitric acid is as follows: 1.0mol/L. When in use, the lead standard solution is required to be diluted, the mass concentration of lead in the diluted lead standard solution is 100 mu g/mL, and the medium type is HNO 3 The concentration of the nitric acid is as follows: 0.1mol/L.
Specifically, S2 includes:
s21, weighing a preprocessed refined aluminum ingot sample for remelting and placing the sample in a conical flask;
s22, adding the diluted lead standard solution and the mixed acid solution into the conical flask in sequence, and heating at low temperature to digest the refined aluminum ingot sample for remelting;
s23, after digestion is completed, deionized water is added to wash the bottle wall, heating is continued until boiling, then cooling is carried out immediately, the solution is transferred to a volumetric flask, dilution and volume fixing are carried out, and shaking is carried out uniformly to be detected.
Specifically, in S21 and S22, the lead standard solution is added in an excessively small amount, so that the solubilizing effect is poor; the addition amount is excessive, the background is complex, the impurity elements are more, and the dissolution assisting effect is not obviously improved; therefore, the proportion of the refined aluminum ingot sample for remelting, the diluted lead standard solution and the mixed acid solution is controlled to be 0.5g; preferably, the ratio of the refined aluminum ingot sample for remelting, the diluted lead standard solution and the mixed acid solution is 0.5g.
Specifically, in S22, the dissolution rate is too slow in consideration of too low temperature during digestion; the corrosion speed of the digestion liquid to the conical flask is higher when the temperature is too high; therefore, the temperature of the low-temperature heating process is controlled to be 50-60 ℃. Wherein the digestion process time is 20-30min.
Specifically, in S23, the excess acid can be distilled off by continuing heating to boiling after digestion is completed, and the acid is immediately cooled after distillation, considering that the conical flask is corroded by an excessively high temperature.
Specifically, in S3, the concentration of the series of standard solutions is in gradient distribution from low to high. The concentration of the standard solution with gradient distribution can effectively eliminate the error of individual samples, and is favorable for obtaining a more accurate working curve, and the accurate working curve is the premise of accurately measuring the content of each element in the refined aluminum ingot for remelting.
Specifically, the linear correlation coefficient γ of the operating curve established in S4 is equal to or greater than 0.999. Otherwise the calibration curve needs to be re-established after finding the cause and eliminating.
The present invention provides a digestion solution and a method for determining the element content in a refined aluminum ingot for remelting, which are illustrated by the following examples.
Example 1
The embodiment provides a digestion solution for measuring the element content in a refined aluminum ingot for remelting, which comprises the following components: lead standard solutions and mixed acid solutions.
Specifically, the sample number of the lead standard solution is GSB 04-1742-2004, the mass concentration of lead in the lead standard solution is 1000 mu g/mL, and the medium type is HNO 3 (ii) a Hydrochloric acid in mixed acid solution: nitric acid: the volume ratio of water is 6. Wherein, the concentration of the hydrochloric acid is 5.2mol/L, and the concentration of the nitric acid is 1.2mol/L.
The method for measuring the element content in the refined aluminum ingot for remelting comprises the following steps:
s1, preprocessing a sample;
placing a refined aluminum ingot sample for remelting into a 250mL conical flask, adding a hydrochloric acid solution (the volume ratio of hydrochloric acid to water is 1).
S2, preparing a sample solution;
weighing 0.5g (accurate to 0.0001 g) of the pretreated refined aluminum ingot sample for remelting, placing the sample in a 150mL conical flask, sequentially adding 5mL of diluted lead standard solution (the concentration of lead in the diluted lead standard solution is 100 mug/mL) and 20mL of mixed acid solution (hydrochloric acid: nitric acid: water volume ratio is 6.
S3, preparing a series of standard solutions;
a blank test was carried out with the sample, and the blank test solution was transferred to a 100mL volumetric flask having a serial number of 0# -3 #. According to the table 1, the national standard solution of the single element (used after being diluted to 10 mug/mL) is respectively added into a 0# -3# volumetric flask, and is diluted to the scale with water and shaken up to prepare a series of standard solutions.
TABLE 1 series of standard solutions
S4, using ICP-OES to sequentially perform spectral intensity measurement on each element in the series of standard solutions, selecting a proper characteristic spectral line, and establishing a working curve;
A. setting instrument parameters
The method adopts an ARCOS type inductively coupled plasma atomic emission spectrometer of German Scheker analytical instrument company, and the working parameters of the instrument are shown in table 2.
TABLE 2 Instrument operating parameters
Selecting a plurality of sensitive lines of Fe, si, cu, zn and Ti elements, and scanning the prepared series of standard solutions and sample solutions at a selected wavelength to investigate the interference condition of the spectral lines of the elements to be detected. By selecting and comparing, the analysis spectral line of the element to be measured is finally determined, as shown in the following table 3.
TABLE 3 analysis lines of the elements
| Element(s) | Fe | Si | Cu | Zn | Ti |
| Line/nm | 259.941 | 251.612 | 324.754 | 213.856 | 334.941 |
B. Drawing of working curve
And (3) sequentially measuring a series of standard solutions at the selected wavelength of each element according to an ICP-OES analysis program according to the sequence from low content to high content of each element in the standard solutions, and controlling software to automatically perform unary linear regression analysis to establish a working curve. The linear correlation coefficient gamma of the working curve should not be less than 0.999, otherwise the calibration curve should be re-established after finding the cause and eliminating.
S5, determining each element in sample solution
The prepared sample solution was introduced into ICP-OES, and the measurement of the sample solution was independently performed twice, and the average value thereof was taken.
Measurement precision of this example:
the method is adopted to carry out the standard recovery rate test on the blank sample, and the recovery rate of each element of the detected 3 parts of sample is between 80% and 120% from the experimental result, which shows that the measurement result of the method is accurate and reliable, the precision level meets the requirement of GB/T20975.25-2008, and the method can be used for detecting the refined aluminum ingot product for remelting. The results are shown in Table 4.
TABLE 4 results of the precision test
Comparative example 1
The comparative example adopts the existing national standard detection method and comprises the following steps:
step 1, preparing a sample solution;
weighing 0.50g (accurate to 0.0001 g) of a refined aluminum ingot sample for remelting, placing the sample in a 100mL beaker, adding 25mL of a mixed acid solution (the volume ratio of hydrochloric acid to nitric acid to water is 3.
Steps 2 to 4 are the same as S3 to S5 in embodiment 1, and are not described in detail here.
Measurement precision of comparative example:
the method is adopted to carry out the standard recovery rate test on the blank sample, and the recovery rate of each element of the detected 3 samples is between 80 and 220 percent from the test result. The results are shown in Table 5.
TABLE 5 results of precision test of comparative example 1
As can be seen by comparing Table 4 and Table 5, the method of the invention is equivalent to the existing national standard method in the precision level within the range specified by the national standard method, wherein the detection lower limit and the precision level of Si and Fe are obviously superior to those of the national standard method. According to the digestion process of the sample, a lead standard solution and an inorganic mixed acid system are adopted, lead ions are remelted and replaced by impurity elements such as Fe, cu, zn and the like in a refined aluminum ingot to obtain metal lead, the metal lead and other metals form a primary battery to form the anode and the cathode of the primary battery, so that the electrolytic reaction generated in the dissolution process is the primary battery process, the dissolution rate is greatly accelerated, the sample dissolution time is reduced, only 20-30min is needed, the time is far lower than 125-150min in the prior art, the efficiency is obviously improved, the time is saved, and the applicability is wide.
While the invention has been described with reference to specific preferred embodiments, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention as defined in the following claims.
Claims (7)
1. A digestion solution for measuring the element content in a refined aluminum ingot for remelting is characterized in that the elements in the refined aluminum ingot for remelting are Fe, si, cu, zn and Ti elements; the digestion solution comprises a lead standard solution and a mixed acid solution; the mass concentration of lead in the lead standard solution is 1000 mug/mL, and the type of the medium is HNO 3 The concentration of the nitric acid is as follows:1.0mol/L; when in use, the lead standard solution needs to be diluted, the mass concentration of lead in the diluted lead standard solution is 100 mug/mL, and the concentration of nitric acid is as follows: 0.1mol/L; controlling the mixed acid solution to be hydrochloric acid: nitric acid: the volume ratio of water is 4-7; the proportion of the refined aluminum ingot sample for remelting, the diluted lead standard solution and the mixed acid solution is 0.5g.
2. The digestion solution for determining the element content in a refined aluminum ingot for remelting according to claim 1, wherein the mixed acid solution is hydrochloric acid: nitric acid: the volume ratio of water is 4-6.
3. A method for measuring the content of an element in a refined aluminum ingot for remelting, characterized by digesting a sample of a refined aluminum ingot for remelting with the digestion liquid according to claim 1 or 2; the method specifically comprises the following steps:
s21, weighing a preprocessed refined aluminum ingot sample for remelting and placing the sample in a conical flask;
s22, sequentially adding the diluted lead standard solution and the mixed acid solution into a conical flask, and heating at low temperature to enable a refined aluminum ingot sample for remelting to be digested; wherein the temperature of the low-temperature heating process is controlled to be 50-60 ℃, and the time of the digestion process is 20-30min;
s23, after digestion is completed, adding deionized water to wash the wall of the flask, continuously heating to boil, immediately cooling, transferring to a volumetric flask, diluting to a constant volume, and shaking up to be tested;
the ratio of the refined aluminum ingot sample for remelting, the diluted lead standard solution and the mixed acid solution is controlled to be 0.5g.
4. A method according to claim 3, including the steps of:
s1, sample pretreatment: placing a refined aluminum ingot sample for remelting in a hydrochloric acid solution, heating and boiling, cooling, washing with deionized water, and drying;
s2, digesting the sample by using a digestion solution, transferring the digested sample to a volumetric flask, diluting and shaking up to obtain a sample solution; said S2 includes S21-S23;
s3, preparing a series of standard solutions: carrying out a blank test along with the sample, adding a certain amount of liquid standard substance into the blank test solution according to the content range of the element to be tested, preparing not less than 3 standard solutions into a volumetric flask, fixing the volume, and shaking up to form a series of standard solutions;
s4, using ICP-OES to sequentially perform spectral intensity measurement on each element in the series of standard solutions, selecting a proper characteristic spectral line, and establishing a working curve;
and S5, measuring the sample solution by using ICP-OES to obtain the spectral intensity of the related elements in the sample, and calculating the content of the related elements in the sample according to the working curve.
5. The method for measuring the element content in the refined aluminum ingot for remelting according to claim 4, wherein in S21 and S22, the proportion of the refined aluminum ingot for remelting sample, the diluted lead standard solution and the mixed acid solution is 0.5g.
6. The method for measuring the content of an element in a fine aluminum ingot for remelting according to claim 4, wherein the temperature of the low-temperature heating process in S22 is 60 ℃.
7. A method for determining the content of an element in a fine aluminum ingot for remelting according to any one of claims 4 to 6, wherein a linear correlation coefficient γ of the operation curve created in S4 is 0.999 or more.
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