Method for measuring nickel and vanadium content in NiV alloy by using inductively coupled plasma emission spectrometer
Technical Field
The invention relates to the technical field of analytical chemistry, relates to a method for measuring nickel and vanadium content in NiV alloy by using an inductively coupled plasma emission spectrometer, and particularly relates to an effective acid solution capable of dissolving the NiV alloy.
Background
At present, sputtering target materials are intensively used in industries such as information storage, integrated circuits, displays, automobile rearview mirrors and the like, and are mainly used for magnetron sputtering of various thin film materials. Magnetron sputtering is a method for preparing a film material, ions generated by an ion source are accelerated and gathered into high-speed ion flow in vacuum, the accelerated particle flow bombards the surface of an object of the film to be deposited, kinetic energy exchange is carried out between the ions and atoms on the surface of the object of the film to be deposited, and a nano or micron film is deposited on the surface of the object of the film to be deposited. While the bombarded solid is the starting material for depositing thin films by sputtering, known as the sputtering target.
In the fabrication of integrated circuits, pure gold is generally used as the surface conductive layer, but gold and silicon wafers tend to generate AuSi low-melting-point compounds, which results in weak bonding between gold and silicon interfaces. The barrier layer needs to be made of metal with high melting point and also needs to bear larger current density, and high-purity metal vanadium can meet the requirement. Therefore, nickel sputtering targets, vanadium sputtering targets, gold sputtering targets, etc. are used in integrated circuit fabrication.
The nickel-vanadium sputtering target material is prepared by adding vanadium into a nickel melt in the process of preparing nickel-vanadium and gold, so that the prepared alloy is more beneficial to magnetron sputtering, combines the advantages of the nickel sputtering target material and the vanadium sputtering target material, and can finish sputtering a nickel layer (bonding layer) and a vanadium layer (barrier layer) at one time. The nickel-vanadium alloy is nonmagnetic and is beneficial to magnetron sputtering. In the electronics and information industry, pure nickel sputtering targets have been completely replaced. The nickel-vanadium sputtering target is mainly used in the solar industry, flat panel display coating, electronics and semiconductor fields; such as integrated circuits, backplane metallization, optoelectronics, and the like.
CN111004985A discloses a preparation method of a nickel-vanadium sputtering target, which comprises the steps of (1) hot forging, (2) annealing, (3) cold deformation and (4) secondary annealing of a nickel-vanadium cast ingot in sequence. The content of V in the nickel-vanadium sputtering target material is 7 +/-0.7%, and the purity of the nickel-vanadium cast ingot is 99.9-99.995%. The grain size of the obtained nickel-vanadium sputtering target material is less than or equal to 150 mu m, and the crystal grains are fine and uniformly distributed.
CN111304606A discloses a preparation method of a defect-free high-purity nickel-vanadium target blank and a target prepared by using the same, wherein the method comprises the following steps: (1) carrying out hot isostatic pressing treatment on the high-purity nickel-vanadium cast ingot, and then forging to obtain a forged cast ingot; (2) and (3) sequentially carrying out primary annealing, rolling-furnace returning heating and secondary annealing on the forged cast ingot obtained in the step (1) to obtain a defect-free high-purity nickel-vanadium target blank. In the invention, by utilizing the synergistic coupling effect of the processes such as hot isostatic pressing treatment, forging, annealing, rolling and the like, the obtained blank has a uniform internal structure, fine grains and no defect inside, and conforms to the nickel-vanadium target blank for semiconductors.
However, regardless of the preparation method adopted to obtain the nickel-vanadium alloy sputtering target material, component determination, particularly determination of nickel content and vanadium content, is required. At present, an inductively coupled plasma emission spectrometer (ICP-OES) is generally used for component testing, because the ICP-OES can detect most of metal elements and some of non-metal elements, and has the advantages of less interference, stable signal, simple operation, and the like. In the actual process of component determination, the metal material to be detected needs to be dissolved by acid liquor, and then the sample solution is obtained by constant volume dilution, so that the detection can be carried out on a machine. Pure nickel is insoluble in water, and is loaded into humid air at normal temperature to form a compact oxide film on the lower surface, and is slowly dissolved in dilute acid, and nickel is slowly dissolved in dilute nitric acid. Pure vanadium has the performance of resisting hydrochloric acid and sulfuric acid, is not oxidized in the air, and can be dissolved in hydrofluoric acid, nitric acid and aqua regia. However, at present, only a dissolving method of pure nickel and pure vanadium single metal is available, and a dissolving method of the NiV alloy is not available, so that a dissolving method of the NiV alloy needs to be found, a test sample for an inductively coupled plasma emission spectrometer can be obtained, and the contents of two main elements, namely Ni and V, can be detected simultaneously.
In summary, there is a need to develop an effective acid solution capable of dissolving NiV alloy to prepare a test sample for an inductively coupled plasma emission spectrometer, that is, to develop a method for determining the nickel and vanadium content in NiV alloy by using an inductively coupled plasma emission spectrometer.
Disclosure of Invention
In order to solve the technical problems, the invention provides a method for determining nickel and vanadium content in NiV alloy by using an inductively coupled plasma emission spectrometer, and the method develops an effective acid solution capable of dissolving the NiV alloy, namely, the NiV alloy is added into a mixed solution of concentrated nitric acid, hydrofluoric acid and deionized water, the mixed solution is heated at 90-110 ℃ to completely dissolve the NiV alloy, then water is added for diluting and fixing the volume to obtain a sample solution, and further the nickel content and the vanadium content in the NiV alloy can be obtained by using the inductively coupled plasma emission spectrometer. The mixed solution of concentrated nitric acid, hydrofluoric acid and deionized water developed by the invention can effectively dissolve the NiV alloy to obtain a sample solution which can be used for an inductively coupled plasma emission spectrometer, and meets the requirement of simultaneously determining the nickel content and the vanadium content in the NiV alloy by using the inductively coupled plasma emission spectrometer.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a method for measuring nickel and vanadium content in NiV alloy by using an inductively coupled plasma emission spectrometer, which comprises the following steps:
adding an NiV alloy into a mixed solution of concentrated nitric acid, hydrofluoric acid and deionized water, heating at 90-110 ℃ to completely dissolve the NiV alloy, and adding water to dilute and fix the volume to obtain a sample solution; and then, measuring the nickel content and the vanadium content in the sample solution by using the inductively coupled plasma emission spectrometer, thereby obtaining the nickel content and the vanadium content in the NiV alloy.
The method provided by the invention develops a mixed solution of concentrated nitric acid, hydrofluoric acid and deionized water, and limits the specific ratio of the concentrated nitric acid to the hydrofluoric acid, so that the NiV alloy can be effectively dissolved, the dissolution rate can be accelerated by heating at 90-110 ℃, and after the NiV alloy is completely dissolved, water is added to dilute and fix the volume to obtain a sample solution, thereby meeting the requirements of simultaneously measuring the nickel content and the vanadium content in the NiV alloy by using an inductively coupled plasma emission spectrometer.
It is worth to say that the heating in the method of the invention can also play a role in dispelling acid, and the nitric acid and the hydrofluoric acid are removed as much as possible, thereby avoiding the interference in the subsequent determination process.
The inductively coupled plasma emission spectrometer used in the invention is a 5110 type full-spectrum direct-reading inductively coupled plasma emission spectrometer of Agilent in America.
The concentrated nitric acid and hydrofluoric acid used in the invention are both super-grade pure, and the deionized water and the experimental water are first-grade water meeting the regulation in GB/T6682.
As a preferred technical scheme of the invention, the method comprises the following steps:
(1) preparation of a sample solution: adding an NiV alloy into a mixed solution of concentrated nitric acid, hydrofluoric acid and deionized water, heating at 90-110 ℃ to completely dissolve the NiV alloy, and adding water to dilute and fix the volume to obtain a sample solution;
(2) selecting an element spectral line: selecting analysis spectral lines of nickel elements and vanadium elements;
(3) drawing a standard curve: preparing a mixed standard solution of nickel elements and vanadium elements, measuring the emission light intensity of the nickel elements and the vanadium elements in the mixed standard solution under an analysis spectral line by using an inductively coupled plasma emission spectrometer, and drawing a standard curve;
(4) detecting a sample: measuring the emission light intensity of the nickel element and the vanadium element in the sample solution in the step (1) under the analysis spectral line in the step (2) by using the inductively coupled plasma emission spectrometer in the step (3), and determining the content of the nickel element and the vanadium element in the sample solution in the step (1) according to the standard curve drawn in the step (3) so as to obtain the content of nickel and vanadium in the NiV alloy;
wherein, the step (1), the step (2) and the step (3) have no sequence.
As a preferred embodiment of the present invention, the concentrated nitric acid of step (1) has a concentration of 65 to 68 wt%, for example, 65 wt%, 65.5 wt%, 66 wt%, 66.5 wt%, 67 wt%, or 68 wt%, but is not limited to the recited values, and other values not recited within the above-mentioned range of values are also applicable.
Preferably, the hydrofluoric acid of step (1) has a concentration of 30-40 wt%, such as 30 wt%, 32 wt%, 35 wt%, 38 wt% or 40 wt%, etc., but is not limited to the recited values, and other values within the above range are equally applicable.
Preferably, the volume ratio of the concentrated nitric acid, the hydrofluoric acid and the deionized water in the step (1) is 1 (0.8-1.2): (1.8-2.2), such as 1:0.8:1.8, 1:1:1.8, 1:1.2:1.8, 1:0.8:2, 1:1:2, 1:1.2:2, 1:0.8:2.2, 1:1:2.2 or 1:1.2:2.2, but not limited to the enumerated values, and other non-enumerated values in the above numerical range are also applicable.
Preferably, the mixed solution of step (1) is prepared in a polytetrafluoroethylene tube.
As a preferred embodiment of the present invention, the ratio of the mass of the NiV alloy in step (1) to the volume of the mixed solution is 1g (70-100) mL, for example, 1g:70mL, 1g:75mL, 1g:80mL, 1g:85mL, 1g:90mL, 1g:95mL, or 1g:100mL, but is not limited to the values listed above, and other values not listed in the above-mentioned numerical ranges are also applicable.
Preferably, the heating time in step (1) is 60-80min, such as 60min, 65min, 70min, 75min or 80min, but not limited to the recited values, and other values not recited in the above range are also applicable.
Preferably, the heating in step (1) is performed by using a graphite heater.
In a preferred embodiment of the present invention, in the step (2), the analytical line of the nickel element is 231.604nm, and the analytical line of the vanadium element is 292.401 nm.
As is well known to those skilled in the art, an inductively coupled plasma emission spectrometer provides dozens of spectral lines, and different spectral lines are used for analysis, the measured results are often very different, and there is great interference among the spectral lines, not only there is interference among different spectral lines of the same element, but also there is serious interference on the selection of the spectral lines due to ions coexisting in a solution, and the intensities of different spectral lines are also different, so that the method screens the analysis spectral lines of nickel element and vanadium element according to the composition of ions coexisting in the sample solution, and finally selects the analysis spectral line of nickel element to be 231.604nm, and the analysis spectral line of vanadium element to be 292.401 nm.
As a preferable technical solution of the present invention, the step of preparing the mixed standard solution of the nickel element and the vanadium element in the step (3) includes:
weighing nickel and vanadium, and preparing a mixed standard solution with gradient change of nickel and vanadium content according to the method for preparing the sample solution in the step (1).
As a preferable technical scheme of the invention, the mass percent of the nickel is more than or equal to 99.999%.
Preferably, the mass percent of the vanadium is more than or equal to 99.999 percent.
As a preferred technical scheme of the invention, the amount of the mixed standard solution is at least five parts.
The quantity of the mixed standard solution in the method is at least five parts, and the parts of the mixed standard solution can be properly increased according to the content of the element to be measured, so that the measured standard curve can better cover the concentration range of the element to be measured, and the accuracy of content measurement is improved.
Preferably, the mixed standard solution has a nickel vanadium content gradient of 0ppm, 2ppm, 4ppm, 8ppm and 16 ppm.
It is worth noting that the concentration of the standard solution in the invention refers to the concentration value of both nickel and vanadium, and taking the mixed standard solution with the nickel and vanadium content of 16ppm as an example, the nickel content is 16ppm, and the vanadium content is also 16 ppm.
Preferably, the mixed standard solution is sequentially introduced into the inductively coupled plasma emission spectrometer from low to high according to the concentration of vanadium element, the emission light intensity of nickel element and vanadium element under the analysis spectral line is measured, and a standard curve is drawn.
As a preferable technical scheme of the invention, the mixed standard solution in the step (3) is introduced into the inductively coupled plasma emission spectrometer through a sample introduction system, and the emission light intensity of the nickel element and the vanadium element under the analysis spectral line is measured.
Preferably, the sample solution in the step (4) is introduced into the inductively coupled plasma emission spectrometer through a sample introduction system, and the emission light intensity of the nickel element and the vanadium element under the analysis spectral line is measured.
Preferably, the sample injection system in the step (3) and the step (4) is a hydrofluoric acid resistant sample injection system.
The method provided by the invention uses an unconventional hydrofluoric acid-resistant sample injection system, can meet the purpose of measuring the contents of nickel and vanadium in the NiV alloy sample, and ensures the accuracy of the measurement result.
Preferably, the operating conditions of the inductively coupled plasma emission spectrometer in step (3) and step (4) are the same, and are both: the RF power is 1200W, the pump speed is 12r/min, the auxiliary gas flow is 1L/min, the atomizer flow is 0.70L/min, the observation height is 8cm, the reading time is 10s, and the stabilization time is 10 s.
As a preferred technical scheme of the invention, the method comprises the following steps:
(1) preparation of a sample solution: preparing a mixed solution of concentrated nitric acid, hydrofluoric acid and deionized water with a volume ratio of 1 (0.8-1.2) to 1.8-2.2 in a polytetrafluoroethylene tube, adding an NiV alloy, controlling the ratio of the mass of the NiV alloy to the volume of the mixed solution to be 1g (70-100) mL, heating for 60-80min at 90-110 ℃ by using a graphite heater to completely dissolve the NiV alloy, and then adding water to dilute and fix the volume to obtain a sample solution;
wherein the concentration of the concentrated nitric acid is 65-68 wt%, and the concentration of the hydrofluoric acid is 30-40 wt%;
(2) selecting an element spectral line: selecting analysis spectral lines of a nickel element and a vanadium element, wherein the analysis spectral line of the nickel element is 231.604nm, and the analysis spectral line of the vanadium element is 292.401 nm;
(3) drawing a standard curve: weighing nickel with the mass percent of more than or equal to 99.999 percent and vanadium with the mass percent of more than or equal to 99.999 percent, and preparing at least five parts of mixed standard solutions with the nickel and vanadium content gradient changed according to the method for preparing the sample solution in the step (1), wherein the nickel and vanadium content gradient of the mixed standard solutions is 0ppm, 2ppm, 4ppm, 8ppm and 16 ppm;
introducing the mixed standard solution into the inductively coupled plasma emission spectrometer sequentially from low concentration to high concentration of vanadium element through a hydrofluoric acid-resistant sample introduction system, measuring the emission light intensity of the nickel element and the vanadium element under the analysis spectral line, and drawing a standard curve;
(4) detecting a sample: introducing the sample solution obtained in the step (1) into the inductively coupled plasma emission spectrometer obtained in the step (3) through a hydrofluoric acid-resistant sample introduction system, measuring the emission light intensity of the nickel element and the vanadium element under the analysis spectral line obtained in the step (2), and determining the content of the nickel element and the vanadium element in the sample solution obtained in the step (1) according to a standard curve drawn in the step (3) so as to obtain the content of nickel and vanadium in the NiV alloy;
wherein, the step (1), the step (2) and the step (3) have no sequence.
Compared with the prior art, the invention has at least the following beneficial effects:
the invention provides a method for determining nickel and vanadium content in NiV alloy by using an inductively coupled plasma emission spectrometer, and particularly develops a mixed solution of concentrated nitric acid, hydrofluoric acid and deionized water, so that the NiV alloy can be effectively dissolved to obtain a sample solution for the inductively coupled plasma emission spectrometer, and the requirement for simultaneously determining the nickel content and the vanadium content in the NiV alloy by using the inductively coupled plasma emission spectrometer is met.
Detailed Description
For the purpose of facilitating an understanding of the present invention, the present invention will now be described by way of examples. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Apparatus and operating conditions
Using an instrument: a5110 full-spectrum direct-reading inductively coupled plasma emission spectrometer of Agilent, USA.
The working conditions of the instrument are as follows: the RF power is 1200W, the pump speed is 12r/min, the auxiliary gas flow is 1L/min, the atomizer flow is 0.70L/min, the observation height is 8cm, the reading time is 10s, and the stabilization time is 10 s.
It is worth noting that the NiV alloys described in the examples and comparative examples are both machined scrap of nickel vanadium alloy sputtering target materials, suitable for NiV alloys of any composition.
Example 1
The embodiment provides a method for measuring the content of nickel and vanadium in NiV alloy by using an inductively coupled plasma emission spectrometer, which comprises the following steps:
(1) preparation of a sample solution: adding 2mL of concentrated nitric acid with the concentration of 68 wt%, 2mL of hydrofluoric acid with the concentration of 36 wt% and 4mL of deionized water into a polytetrafluoroethylene tube, namely preparing a mixed solution of the concentrated nitric acid, the hydrofluoric acid and the deionized water with the volume ratio of 1:1:2, adding 0.1g of NiV alloy, controlling the ratio of the mass of the NiV alloy to the volume of the mixed solution to be 1g:80mL, heating for 60min at 100 ℃ by using a graphite heater to completely dissolve the NiV alloy, removing acid until the residual volume of the solution is 4mL, and then adding water to dilute and fix the volume to obtain a sample solution;
(2) selecting an element spectral line: selecting analysis spectral lines of a nickel element and a vanadium element, wherein the analysis spectral line of the nickel element is 231.604nm, and the analysis spectral line of the vanadium element is 292.401 nm;
(3) drawing a standard curve: weighing nickel with the mass percent of more than or equal to 99.999 percent and vanadium with the mass percent of more than or equal to 99.999 percent, and preparing five mixed standard solutions with the nickel and vanadium content gradient change according to the method for preparing the sample solution in the step (1), wherein the nickel and vanadium content gradient of the mixed standard solutions is 0ppm, 2ppm, 4ppm, 8ppm and 16 ppm;
introducing the mixed standard solution into the inductively coupled plasma emission spectrometer sequentially from low concentration to high concentration of vanadium element through a hydrofluoric acid-resistant sample introduction system, measuring the emission light intensity of the nickel element and the vanadium element under the analysis spectral line, and drawing a standard curve;
(4) detecting a sample: introducing the sample solution obtained in the step (1) into the inductively coupled plasma emission spectrometer obtained in the step (3) through a hydrofluoric acid-resistant sample introduction system, measuring the emission light intensity of the nickel element and the vanadium element under the analysis spectral line obtained in the step (2), and determining the content of the nickel element and the vanadium element in the sample solution obtained in the step (1) according to a standard curve drawn in the step (3) so as to obtain the content of nickel and vanadium in the NiV alloy;
wherein, the step (1), the step (2) and the step (3) have no sequence.
The NiV alloy can be completely dissolved, the content of the nickel element obtained by measurement is 95.05 wt%, and the content of the vanadium element is 4.94 wt%, so that the NiV alloy has the advantages of simplicity in operation and high accuracy.
Example 2
The embodiment provides a method for measuring the content of nickel and vanadium in NiV alloy by using an inductively coupled plasma emission spectrometer, which comprises the following steps:
(1) preparation of a sample solution: adding 2mL of concentrated nitric acid with the concentration of 68 wt%, 1.6mL of hydrofluoric acid with the concentration of 36 wt% and 4mL of deionized water into a polytetrafluoroethylene tube, namely preparing a mixed solution of the concentrated nitric acid, the hydrofluoric acid and the deionized water with the volume ratio of 1:0.8:2, adding 0.1g of NiV alloy, controlling the ratio of the mass of the NiV alloy to the volume of the mixed solution to be 1g:76mL, heating for 60min at 100 ℃ by adopting a graphite heater to completely dissolve the NiV alloy, removing acid until the residual volume of the solution is 4mL, and then adding water to dilute to a constant volume to obtain a sample solution;
(2) selecting an element spectral line: selecting analysis spectral lines of a nickel element and a vanadium element, wherein the analysis spectral line of the nickel element is 231.604nm, and the analysis spectral line of the vanadium element is 292.401 nm;
(3) drawing a standard curve: weighing nickel with the mass percent of more than or equal to 99.999 percent and vanadium with the mass percent of more than or equal to 99.999 percent, and preparing five mixed standard solutions with the nickel and vanadium content gradient change according to the method for preparing the sample solution in the step (1), wherein the nickel and vanadium content gradient of the mixed standard solutions is 0ppm, 2ppm, 4ppm, 8ppm and 16 ppm;
introducing the mixed standard solution into the inductively coupled plasma emission spectrometer sequentially from low concentration to high concentration of vanadium element through a hydrofluoric acid-resistant sample introduction system, measuring the emission light intensity of the nickel element and the vanadium element under the analysis spectral line, and drawing a standard curve;
(4) detecting a sample: introducing the sample solution obtained in the step (1) into the inductively coupled plasma emission spectrometer obtained in the step (3) through a hydrofluoric acid-resistant sample introduction system, measuring the emission light intensity of the nickel element and the vanadium element under the analysis spectral line obtained in the step (2), and determining the content of the nickel element and the vanadium element in the sample solution obtained in the step (1) according to a standard curve drawn in the step (3) so as to obtain the content of nickel and vanadium in the NiV alloy;
wherein, the step (1), the step (2) and the step (3) have no sequence.
The NiV alloy can be completely dissolved, the content of the nickel element obtained by measurement is 95.31 wt%, the content of the vanadium element is 5.10 wt%, and the NiV alloy has the advantages of simplicity in operation and high accuracy.
Example 3
The embodiment provides a method for measuring the content of nickel and vanadium in NiV alloy by using an inductively coupled plasma emission spectrometer, which comprises the following steps:
(1) preparation of a sample solution: adding 2mL of concentrated nitric acid with the concentration of 68 wt%, 2.4mL of hydrofluoric acid with the concentration of 36 wt% and 4.4mL of deionized water into a polytetrafluoroethylene tube, namely preparing a mixed solution of the concentrated nitric acid, the hydrofluoric acid and the deionized water with the volume ratio of 1:1:2, adding 0.1g of NiV alloy, controlling the ratio of the mass of the NiV alloy to the volume of the mixed solution to be 1g:88mL, heating for 60min at 100 ℃ by adopting a graphite heater to completely dissolve the NiV alloy, removing acid until the residual volume of the solution is 4.4mL, and then adding water to dilute and fix the volume to obtain a sample solution;
(2) selecting an element spectral line: selecting analysis spectral lines of a nickel element and a vanadium element, wherein the analysis spectral line of the nickel element is 231.604nm, and the analysis spectral line of the vanadium element is 292.401 nm;
(3) drawing a standard curve: weighing nickel with the mass percent of more than or equal to 99.999 percent and vanadium with the mass percent of more than or equal to 99.999 percent, and preparing five mixed standard solutions with the nickel and vanadium content gradient change according to the method for preparing the sample solution in the step (1), wherein the nickel and vanadium content gradient of the mixed standard solutions is 0ppm, 2ppm, 4ppm, 8ppm and 16 ppm;
introducing the mixed standard solution into the inductively coupled plasma emission spectrometer sequentially from low concentration to high concentration of vanadium element through a hydrofluoric acid-resistant sample introduction system, measuring the emission light intensity of the nickel element and the vanadium element under the analysis spectral line, and drawing a standard curve;
(4) detecting a sample: introducing the sample solution obtained in the step (1) into the inductively coupled plasma emission spectrometer obtained in the step (3) through a hydrofluoric acid-resistant sample introduction system, measuring the emission light intensity of the nickel element and the vanadium element under the analysis spectral line obtained in the step (2), and determining the content of the nickel element and the vanadium element in the sample solution obtained in the step (1) according to a standard curve drawn in the step (3) so as to obtain the content of nickel and vanadium in the NiV alloy;
wherein, the step (1), the step (2) and the step (3) have no sequence.
The NiV alloy can be completely dissolved, the content of the nickel element obtained by measurement is 95.21 wt%, and the content of the vanadium element is 4.92 wt%, so that the NiV alloy has the advantages of simplicity in operation and high accuracy.
It is worth noting that for NiV alloys, the detection accuracy of the method of the present invention is + -1 wt%, i.e., the sum of the contents of nickel and vanadium elements is 100 + -1 wt%.
Comparative example 1
This comparative example provides a method for determining nickel and vanadium content in NiV alloys using an inductively coupled plasma emission spectrometer, based on the method described in example 1, with the only difference that: replacing the step (1) of adding 2mL of concentrated nitric acid with the concentration of 68 wt%, 2mL of hydrofluoric acid with the concentration of 36 wt% and 4mL of deionized water into a polytetrafluoroethylene tube, namely preparing the mixed solution of the concentrated nitric acid, the hydrofluoric acid and the deionized water with the volume ratio of 1:1:2 with the step of adding 3mL of concentrated hydrochloric acid with the concentration of 38 wt% and 1mL of concentrated nitric acid with the concentration of 68 wt% into the polytetrafluoroethylene tube, namely preparing the aqua regia according to the volume ratio of 3: 1.
The NiV alloy in the comparative example is basically not dissolved, can not be prepared into a sample solution which can be used for an inductively coupled plasma emission spectrometer, and can not meet the requirement of simultaneously measuring the nickel content and the vanadium content in the NiV alloy by using the inductively coupled plasma emission spectrometer.
Comparative example 2
This comparative example provides a method for determining nickel and vanadium content in NiV alloys using an inductively coupled plasma emission spectrometer, based on the method described in example 1, with the only difference that: replacing the step (1) of heating for 60min at 100 ℃ by a graphite heater with the step (1) of heating for 60min at 80 ℃.
The NiV alloy cannot be completely dissolved, cannot be prepared into a sample solution which can be used for an inductively coupled plasma emission spectrometer, and cannot meet the requirement for simultaneously measuring the nickel content and the vanadium content in the NiV alloy by using the inductively coupled plasma emission spectrometer.
In summary, the invention provides a method for determining nickel and vanadium content in NiV alloy by using an inductively coupled plasma emission spectrometer, and particularly develops an effective acid solution capable of dissolving NiV alloy, namely, a mixed solution of concentrated nitric acid, hydrofluoric acid and deionized water is prepared, NiV alloy is added, heating is carried out at 90-110 ℃, so that the NiV alloy is completely dissolved, then water is added to dilute and fix volume to obtain a sample solution, and the requirement for simultaneously determining nickel content and vanadium content in NiV alloy by using an inductively coupled plasma emission spectrometer is met.
The present invention is illustrated by the above-mentioned examples, but the present invention is not limited to the above-mentioned detailed process equipment and process flow, i.e. it is not meant to imply that the present invention must rely on the above-mentioned detailed process equipment and process flow to be practiced. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.