CN111024682A - Method for measuring tantalum content in nickel-based alloy - Google Patents
Method for measuring tantalum content in nickel-based alloy Download PDFInfo
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Abstract
The invention discloses a method for measuring the content of tantalum in nickel-based alloy, which comprises the following steps: (1) preparing standard solution of standard Ta element; (2) establishing an interference correction model according to the actual content range of Cr, V and other elements in the nickel-based alloy; (3) measuring the Ta element standard solution on an inductively coupled plasma emission spectrometer, and drawing a standard curve; (4) accurately weighing a nickel-based alloy sample, and preparing a sample solution; (5) and measuring the emission intensity of the Ta element in the sample solution, calculating the content of the Ta element in the sample solution according to a standard curve, and then correcting by an interference correction formula to obtain the actual content of the Ta element in the nickel-based alloy. The method can accurately measure the actual content of the tantalum element in the nickel-based alloy and has good test precision.
Description
Technical Field
The invention relates to a method for measuring the content of a tantalum element in a nickel-based alloy, and belongs to the field of metallurgical analysis and detection.
Background
The nickel-based alloy is a highly complex alloy containing a plurality of alloying elements by taking nickel as a matrix (the mass fraction is generally more than 50%), and the chromium, the cobalt, the molybdenum, the copper and the like are common alloying elements, has excellent performances of small density, high strength, oxidation resistance, high temperature resistance and the like, and is widely applied to the fields of aviation, aerospace, nuclear reactors, petrochemical industry, energy conversion equipment and the like. In recent years, with the implementation of a 'big airplane' project, China continuously promotes the independent research and development of high-end aviation engines, and meanwhile, the requirements for research, development, production and detection of nickel-based alloys in China are continuously increased. Research shows that the types and contents of elements in the alloy have great influence on the mechanical properties of the nickel-based single crystal superalloy. Because of the high degree of saturation of nickel-based alloys, it is necessary to control the content of each element (especially the main strengthening elements and trace elements) severely, otherwise harmful phases are precipitated during use, and the strength and toughness of the alloy are damaged. Therefore, research on an accurate detection method for the element content in the nickel-based alloy is urgent.
The effect of tantalum on improving the material quality of metal functional materials is considered as an element beneficial to the high-temperature strength, oxidation resistance and hot corrosion resistance of nickel-based alloys, and people are attracted more and more attention, and a certain amount of tantalum is added into the nickel-based alloys, so that the high-temperature hot corrosion resistance of the alloys can be improved, and the alloy structure is stabilized. Therefore, the accuracy of measuring high-content tantalum and trace tantalum is required. Since tantalum is an element that is very susceptible to hydrolysis, separation and measurement have been difficult in analytical chemistry. With the continuous development of instrument analysis in recent years, the difficult problem of separation of tantalum can be solved by adopting a spectral analysis technology, and particularly, the ICP-AES method is more favorable for determination. Because the inductively coupled plasma emission spectrometry (ICP-AES) has the characteristics of high analysis precision, small matrix effect, wide linear range, low detection limit and the like, the ICP-AES can be used for measuring the content range of the tantalum element in the nickel-based alloy from 0.0X% to X.0%, and the analysis is rapid.
Generally, recommended sensitive analysis lines of tantalum are 268.517nm, 263.558nm, 226.230nm and 240.063nm, and when the practical resolution of ICP-AES is larger than 0.010nm, Ta268.517nm has the highest sensitivity but is greatly interfered by the contents of Cr and V elements, while the relative sensitivities of Ta263.558nm, Ta226.230nm, Ta240.063nm and other wavelengths are low, and the relative sensitivities of the elements are simultaneously interfered by the wavelengths of Fe, Ni, Cr, W and the like. Therefore, the invention aims to adopt the most sensitive analysis line of Ta268.517nm and correct the wavelength interference among elements by adopting an interference correction calculation mode, and aims to provide a method for measuring the content of the tantalum element in the nickel-based alloy with low detection limit.
Disclosure of Invention
The invention aims to provide an ICP-AES (inductively coupled plasma-atomic emission spectrometry) method for measuring tantalum element in nickel-based alloy with low detection limit.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a method for measuring the content of tantalum element in a nickel-based alloy comprises the following steps:
(1) preparing a standard solution: weighing high-purity nickel, and adding a mixed acid prepared from hydrochloric acid, nitric acid and a small amount of hydrofluoric acid for digestion; after digestion is finished, preparing a series of Ta element standard solutions with different concentrations;
(2) establishing an interference correction model: establishing a plurality of interference correction values of Cr and V to Ta according to the actual content ranges of elements such as Cr, V and the like in the nickel-based alloy, and obtaining an interference correction equation of Cr and V to Ta by adopting weighted regression iteration, wherein the content range of Cr is 1.0-30%, the content range of V is 0.1-5%, and the content range of Ta is 0.02-5%;
(3) establishing a standard curve: measuring the Ta element standard solution prepared in the step (1) on an inductively coupled plasma emission spectrometer, and drawing a standard curve by taking the Ta element content as a horizontal coordinate and the emission intensity as a vertical coordinate;
(4) preparing a sample solution: accurately weighing a nickel-based alloy sample, adding mixed acid prepared from hydrochloric acid, nitric acid and a small amount of hydrofluoric acid, and placing the mixture in a microwave digestion instrument for digestion; after digestion, cooling and fixing the volume to obtain a sample solution;
(5) testing and data processing: measuring emission intensity of Ta element in the sample solution by using the same measuring conditions as those in the step (3), and establishing the standard curve according to the step (3)Calculating in line to obtain the content omega of the Ta element in the sample solution0(Ta), the actual content of the Ta element in the nickel-based alloy can be obtained through calculation of an interference correction formula (1):
ω(Ta)＝ω0(Ta)-ω(Ta/Cr)-ω(Ta/V) (1)
wherein omega (Ta) is the actual content of Ta element in the nickel-based alloy,%; omega0(Ta) calculating the content of the Ta element according to the standard curve established in the step (2); omega (Ta/Cr) is a correction value of a Cr element to a Ta element,%; omega (Ta/V) is a corrected value of the V element to the Ta element,%; and omega (Ta/Cr) and omega (Ta/V) can be calculated by the interference correction equation in the step (2) in percentage.
The content of the Ta element in the nickel-base alloy refers to the mass percentage of the element in the sample, for example, the actual content omega (Ta) of the Ta element refers to the mass percentage of the Ta element in the nickel-base alloy.
The mixed acid in the step (1) and the step (4) is prepared from high-purity hydrochloric acid, high-purity nitric acid and 0.5-1 ml of hydrofluoric acid in a volume ratio of 1: 1-4: 1.
In the step (4), the digestion power of microwave digestion is 800 w-1600 w, the pressure is 300-600 psi, the temperature is raised to the target temperature of 170-190 ℃, and the temperature is kept until complete digestion.
The detection range of the tantalum element in the nickel-based alloy measured by the method is 0.002% -5%.
Adopt the produced beneficial effect of above-mentioned technical scheme to lie in: (1) the method can be used for measuring the content of the lower-content tantalum element in the nickel-based alloy, and has good measuring precision.
(2) In the sample dissolving process, the microwave digestion instrument is used for sample digestion, so that the elements to be detected in the sample can be completely digested, the hydrolysis condition does not exist, the operation is simple and convenient, and the detection efficiency is improved.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
Example 1: the tantalum element in the nickel-based alloy is exemplified by a certain nickel-based alloy sample, and is specifically described as follows.
(1) Preparing a standard solution: accurately weighing 6 parts of 0.2500g of high-purity nickel, adding mixed acid prepared from 6ml of high-purity hydrochloric acid, 3ml of high-purity nitric acid and 0.5ml of hydrofluoric acid for digestion, and transferring the mixture into 6 volumetric flasks of 100ml after digestion; accurately transferring the tantalum element standard diluent with different volumes and concentrations of 10 mug/L into the 6 100mL volumetric flasks, shaking uniformly with ultrapure water with the resistivity of 18.2M omega cm in a constant volume manner to prepare a series of Ta element standard solutions with different concentrations, wherein the mass percentage of the Ta element in the standard solutions to the high-purity nickel, namely the tantalum element content, is shown in Table 1.
Table 1: content of tantalum element in standard solution
| Standard solution | Standard 1 | Standard 2 | Standard 3 | Standard 4 | Standard 5 | Standard 6 |
| Tantalum content (wt%) | 0 | 0.02 | 0.05 | 0.1 | 0.2 | 0.5 |
(2) Establishing an interference correction model: according to the actual content range of Cr, V and other elements in the nickel-based alloy, a plurality of interference correction values of Cr and V to Ta are established, and an interference correction equation of Cr and V to Ta is obtained by adopting weighted regression iteration, and is shown in Table 2.
Wherein omega (Cr) is the content of Cr element,%; omega (Ta/Cr) is a correction value of a Cr element to a Ta element,%; omega (V) is the content percent of the V element; omega (Ta/V) is the corrected value of V element to Ta element,%.
In the present embodiment, the sample # 1 is taken as an example, in which the content ω (Cr) of the Cr element is 10.43%, the content of the V element is 0.257%, and according to the disturbance correction equation, the corrected value ω (Ta/Cr) of the Cr element to the Ta element is 0.0391%, and the corrected value ω (Ta/V) of the V element to the Ta element is 0.0024%.
(3) Establishing a standard curve: setting instrument parameters on an inductively coupled plasma spectrometer according to table 3, sequentially measuring the spectral intensity of the Ta element in the standard solution prepared in the step (1), and taking the content omega of the Ta element0(Ta) is an abscissa, the spectral intensity is an ordinate, and a standard curve of a Ta element is drawn, wherein the standard curve equation is as follows: 467.28 omega for y0(Ta) +3.09, linearity coefficient 0.9998, good linearity.
Table 3: conditions of measuring apparatus
| Parameters of the instrument | Set value |
| ICP power | 1150W |
| Flow of cooling gas | 15.0L/min |
| Auxiliary gas flow | 0.75L/min |
| Flow rate of atomized gas | 0.85L/min |
| Speed of sample pump | 15r/min |
| Integration time | 15s |
(4) Preparing a sample solution: weighing 0.4000g of nickel-based alloy (accurate to 0.0001g), wetting the nickel-based alloy with 5ml of ultrapure water in a TFM digestion tank, adding a mixed acid solution, wherein the mixed acid solution is prepared from 6ml of high-grade pure hydrochloric acid, 3ml of high-grade pure nitric acid and 0.5ml of high-grade pure hydrofluoric acid, the concentration of the high-grade pure hydrochloric acid is 36-38%, the concentration of the high-grade pure nitric acid is 60-68%, and the concentration of the high-grade pure hydrofluoric acid is not less than 40%, after the severe reaction is finished, covering a TFM cover, putting the TFM cover into a safety shield, tightening the cover with a torque wrench, putting the TFM cover into a microwave cavity, connecting a temperature sensor, and putting a prepared blank sample into a microwave digestion instrument. The microwave digestion instrument parameters are as follows: digestion power is 1600w, pressure is 600psi, temperature rise time is 30min, target temperature is 180 ℃, and heat preservation time is 25 min. After the digestion procedure was completed, the reaction mixture was cooled to 30 ℃ or below, the digestion solution was transferred to a 100ml volumetric flask, and a sample solution was prepared by fixing the volume to a scale with ultrapure water having a resistivity of 18.2 M.OMEGA.cm, shaking up, and standing.
(5) Testing and data processing: measuring the emission intensity of the Ta element in the sample solution by adopting the measuring conditions of the table 3, wherein the result is 113.13c/s, and the content omega of the Ta element in the sample solution is calculated according to the standard curve established in the step (3)0(Ta), the result was 0.2355%, and the fact of the Ta element in the nickel-base alloy was calculated by the interference correction formula (1)The content of the active carbon is the same as the content of the active carbon,
ω(Ta)＝ω0(Ta)-ω(Ta/Cr)-ω(Ta/V) (1)
wherein omega (Ta) is the actual content of Ta element in the nickel-based alloy,%; omega0(Ta) calculating the content of the Ta element according to the standard curve established in the step (2); omega (Ta/Cr) is a correction value of a Cr element to a Ta element,%; omega (Ta/V) is the corrected value of V element to Ta element,%.
The actual content of Ta element in the nickel base alloy sample No. 1 was calculated to be 0.194%.
To verify the accuracy of the method, spiking recovery and precision tests were performed with the results shown in table 4.
Table 4: measurement result (wt)
Example 2: the tantalum element in the nickel-based alloy is exemplified by a certain nickel-based alloy sample, and is specifically described as follows.
(1) Preparing a standard solution: accurately weighing 6 parts of 0.2500g of high-purity nickel, adding mixed acid prepared from 5ml of high-purity hydrochloric acid, 5ml of high-purity nitric acid and 0.5ml of hydrofluoric acid for digestion, and transferring the mixture into 6 volumetric flasks of 100ml after digestion; accurately transferring the tantalum element standard diluent with different volumes and concentrations of 10 mug/L into the 6 100mL volumetric flasks, shaking uniformly with ultrapure water with the resistivity of 18.2M omega cm in a constant volume manner to prepare a series of Ta element standard solutions with different concentrations, wherein the mass percentage of the Ta element in the standard solutions to the high-purity nickel, namely the tantalum element content, is shown in Table 1.
(2) Establishing an interference correction model: establishing a plurality of interference correction values of Cr and V to Ta according to the actual content ranges of elements such as Cr, V and the like in the nickel-based alloy, and obtaining an interference correction equation of Cr and V to Ta by adopting weighted regression iteration, wherein the interference correction equation is shown in a table 2; wherein the content range of Cr is 1.0-30%, the content range of V is 0.1-5%, and the content range of Ta is 0.02-5%.
In the present embodiment, the nickel-based alloy is obtained by taking a sample # 3 as an example, wherein the content of the Cr element is 23.59%, the content of the V element is 0.937%, and according to the interference correction equation, the corrected value ω (Ta/Cr) of the Cr element to the Ta element is 0.0891%, and the corrected value ω (Ta/V) of the V element to the Ta element is 0.0105%.
(3) Establishing a standard curve: setting instrument parameters on an inductively coupled plasma spectrometer according to table 3, sequentially measuring the spectral intensity of the Ta element in the standard solution prepared in the step (1), and taking the content omega of the Ta element0(Ta) is an abscissa, and the spectral intensity is an ordinate to draw a standard curve equation: 467.28 omega for y0(Ta) +3.09, linearity coefficient 0.9998, good linearity.
(4) Preparing a sample solution: weighing 0.3000 nickel-based alloy (accurate to 0.0001g), wetting with 5ml of ultrapure water in a TFM digestion tank, adding a mixed acid solution, wherein the mixed acid solution is prepared from 5ml of high-grade pure hydrochloric acid, 5ml of high-grade pure nitric acid and 0.5ml of high-grade pure hydrofluoric acid, the concentration of the high-grade pure hydrochloric acid is 36-38%, the concentration of the high-grade pure nitric acid is 60-68%, and the concentration of the high-grade pure hydrofluoric acid is not less than 40%, after the severe reaction is finished, covering a TFM cover, putting the TFM cover into a safety cover, tightening the cover with a torque wrench, putting the TFM cover into a microwave cavity, connecting a temperature sensor, and putting the TFM cover into a microwave digestion instrument along with a prepared blank sample. The microwave digestion instrument parameters are as follows: digestion power is 1600w, pressure is 500psi, heating time is 25min, target temperature is 170 ℃, and heat preservation time is 25 min. After the digestion procedure was completed, the reaction mixture was cooled to 30 ℃ or below, the digestion solution was transferred to a 100ml volumetric flask, and a sample solution was prepared by fixing the volume to a scale with ultrapure water having a resistivity of 18.2 M.OMEGA.cm, shaking up, and standing.
(5) Testing and data processing: measuring the emission intensity of the Ta element in the sample solution by adopting the measuring conditions of the table 3, wherein the result is 923.44c/s, and the content omega of the Ta element in the sample solution is calculated according to the standard curve established in the step (3)0(Ta), the result was 1.970%, the actual content of Ta element in the nickel-base alloy was calculated by the interference correction formula (1),
ω(Ta)＝ω0(Ta)-ω(Ta/Cr)-ω(Ta/V) (1)
wherein omega (Ta) is the actual content of Ta element in the nickel-based alloy; omega0(Ta) is the content of Ta element calculated according to the standard curve established in the step (2)An amount; omega (Ta/Cr) is a correction value of a Cr element to a Ta element; and omega (Ta/V) is a correction value of the V element to the Ta element.
The actual content of Ta element in the ni-based alloy No. 3 sample was calculated to be 1.87%.
To verify the accuracy of the method, spiking recovery and precision tests were performed with the results shown in table 5.
TABLE 5 results of recovery and precision test with standard addition
The experimental results show that the method provided by the invention can accurately measure the actual content of the tantalum element in the nickel-based alloy, and has good test precision and accuracy.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (4)
1. A method for measuring the content of tantalum element in nickel-based alloy is characterized by comprising the following steps:
(1) preparing a standard solution: weighing high-purity nickel, and adding a mixed acid prepared from hydrochloric acid, nitric acid and a small amount of hydrofluoric acid for digestion; after digestion is finished, preparing a series of Ta element standard solutions with different concentrations;
establishing an interference correction model: establishing a plurality of interference correction values of Cr and V to Ta according to the actual content ranges of elements such as Cr, V and the like in the nickel-based alloy, and obtaining an interference correction equation of Cr and V to Ta by adopting weighted regression iteration, wherein the content range of Cr is 1.0-30%, the content range of V is 0.1-5%, the content range of Ta is 0.02-5%, and the nickel-based alloy is used as a basis;
establishing a standard curve: measuring the Ta element standard solution prepared in the step (1) on an inductively coupled plasma emission spectrometer, and determining the content omega of the Ta element0(Ta) is an abscissa, and the emission intensity is an ordinate to draw a standard curve;
(4) preparing a sample solution: accurately weighing a nickel-based alloy sample, adding mixed acid prepared from hydrochloric acid, nitric acid and a small amount of hydrofluoric acid, and placing the mixture in a microwave digestion instrument for digestion; after digestion, cooling and fixing the volume to obtain a sample solution;
(5) testing and data processing: measuring the emission intensity of the Ta element in the sample solution by adopting the same measuring conditions as the step (3), and calculating the content omega of the Ta element in the sample solution according to the standard curve established in the step (3)0(Ta), the actual content of the Ta element in the nickel-based alloy can be obtained through calculation of an interference correction formula (1):
wherein omega (Ta) is the actual content of Ta element in the nickel-based alloy,%; omega0(Ta) calculating the content of the Ta element according to the standard curve established in the step (2); omega (Ta/Cr) is a correction value of a Cr element to a Ta element,%; omega (Ta/V) is a corrected value of the V element to the Ta element,%; and omega (Ta/Cr) and omega (Ta/V) can be calculated by the interference correction equation in the step (2) in percentage.
2. The method for determining the tantalum content in a nickel-based alloy according to claim 1, wherein the method comprises the following steps: the mixed acid in the step (1) and the step (4) is prepared from high-purity hydrochloric acid, high-purity nitric acid and 0.5-1 ml of hydrofluoric acid in a volume ratio of 1: 1-4: 1.
3. The method for determining the tantalum content in a nickel-based alloy according to claim 1, wherein the method comprises the following steps: in the step (4), the digestion power of microwave digestion is 800 w-1600 w, the pressure is 300-600 psi, the temperature is raised to the target temperature of 170-190 ℃, and then the temperature is maintained until complete digestion is achieved.
4. The method for determining the tantalum content in the nickel-based alloy according to claim 1, wherein the method comprises the following steps: the detection range of tantalum element in the nickel-based alloy is 0.002% -5%.
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| CN111426679A (en) * | 2020-04-22 | 2020-07-17 | 河钢股份有限公司 | Method for measuring content of tungsten element in nickel-based alloy |
| CN112834486A (en) * | 2020-12-29 | 2021-05-25 | 河钢股份有限公司 | Method for measuring chromium content in nickel-based alloy |
| CN112834486B (en) * | 2020-12-29 | 2022-09-30 | 河钢股份有限公司 | Method for measuring chromium content in nickel-based alloy |
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Application publication date: 20200417 |