CN114113043A - Method for measuring nickel and vanadium content in NiV alloy by using inductively coupled plasma emission spectrometer - Google Patents
Method for measuring nickel and vanadium content in NiV alloy by using inductively coupled plasma emission spectrometer Download PDFInfo
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 243
- 229910052720 vanadium Inorganic materials 0.000 title claims abstract description 128
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 title claims abstract description 127
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 122
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 89
- 239000000956 alloy Substances 0.000 title claims abstract description 89
- 238000009616 inductively coupled plasma Methods 0.000 title claims abstract description 58
- 238000000034 method Methods 0.000 title claims abstract description 57
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 88
- 239000012488 sample solution Substances 0.000 claims abstract description 53
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 41
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 33
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 33
- 239000011259 mixed solution Substances 0.000 claims abstract description 27
- 239000008367 deionised water Substances 0.000 claims abstract description 24
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 24
- 238000010438 heat treatment Methods 0.000 claims abstract description 20
- 230000003595 spectral effect Effects 0.000 claims description 52
- 238000004458 analytical method Methods 0.000 claims description 41
- 239000012086 standard solution Substances 0.000 claims description 35
- 239000000523 sample Substances 0.000 claims description 29
- HBVFXTAPOLSOPB-UHFFFAOYSA-N nickel vanadium Chemical compound [V].[Ni] HBVFXTAPOLSOPB-UHFFFAOYSA-N 0.000 claims description 17
- 238000002360 preparation method Methods 0.000 claims description 10
- -1 polytetrafluoroethylene Polymers 0.000 claims description 9
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 9
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 9
- 230000008569 process Effects 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 229910002804 graphite Inorganic materials 0.000 claims description 8
- 239000010439 graphite Substances 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 7
- 230000008859 change Effects 0.000 claims description 5
- 238000002347 injection Methods 0.000 claims description 5
- 239000007924 injection Substances 0.000 claims description 5
- 239000002253 acid Substances 0.000 abstract description 11
- 239000000243 solution Substances 0.000 abstract description 10
- 238000005477 sputtering target Methods 0.000 description 15
- 239000013077 target material Substances 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 6
- 239000010408 film Substances 0.000 description 6
- 150000002500 ions Chemical class 0.000 description 6
- 238000000137 annealing Methods 0.000 description 5
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 5
- 229910052737 gold Inorganic materials 0.000 description 5
- 239000010931 gold Substances 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 238000001755 magnetron sputter deposition Methods 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 229910000756 V alloy Inorganic materials 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000005242 forging Methods 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000001513 hot isostatic pressing Methods 0.000 description 2
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- 230000006641 stabilisation Effects 0.000 description 2
- 238000011105 stabilization Methods 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 238000011282 treatment Methods 0.000 description 2
- 230000033228 biological regulation Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000001808 coupling effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000001465 metallisation Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 235000012431 wafers Nutrition 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
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- Chemical & Material Sciences (AREA)
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- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
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Abstract
The invention provides a method for determining nickel and vanadium content in NiV alloy by using an inductively coupled plasma emission spectrometer, which comprises the steps of adding the 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 mainly develops an effective acid solution capable of dissolving the NiV alloy, namely, a mixed solution of concentrated nitric acid, hydrofluoric acid and deionized water is prepared to completely dissolve the NiV alloy, and then water is added to dilute and fix the volume to obtain a sample solution, so that the requirement of simultaneously measuring the nickel content and the vanadium content in the NiV alloy by using an inductively coupled plasma emission spectrometer is met.
Description
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.
Claims (10)
1. A method for measuring the contents of nickel and vanadium in NiV alloy by using an inductively coupled plasma emission spectrometer is characterized by comprising 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.
2. Method according to claim 1, characterized in that it 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.
3. The process of claim 2, wherein the concentration of the concentrated nitric acid of step (1) is 65-68 wt%;
preferably, the concentration of the hydrofluoric acid in the step (1) is 30-40 wt%;
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) to (1.8-2.2);
preferably, the mixed solution of step (1) is prepared in a polytetrafluoroethylene tube.
4. The method according to claim 2 or 3, wherein the ratio between the mass of the NiV alloy of step (1) and the volume of the mixed solution is 1g (70-100) mL;
preferably, the heating time of the step (1) is 60-80 min;
preferably, the heating in step (1) is performed by using a graphite heater.
5. The method according to any one of claims 2 to 4, wherein the analytical line of the nickel element in step (2) is 231.604nm, and the analytical line of the vanadium element is 292.401 nm.
6. The method according to any one of claims 2 to 5, wherein the step of preparing the mixed standard solution of the nickel element and the vanadium element in the step (3) comprises:
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).
7. The method according to claim 6, wherein 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.
8. The method of claim 6, wherein the amount of the mixed standard solution is at least five parts;
preferably, the mixed standard solution has a nickel vanadium content gradient of 0ppm, 2ppm, 4ppm, 8ppm and 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.
9. The method according to any one of claims 2 to 8, wherein the mixed standard solution in step (3) is introduced into the inductively coupled plasma emission spectrometer through a sample introduction system, and the emission light intensity of nickel element and vanadium element under the analysis 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 nickel element and 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.
10. A method according to any of claims 2-9, characterized in that the method comprises the steps of:
(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.
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Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1998020341A1 (en) * | 1996-11-08 | 1998-05-14 | Mountain States Analytical, Inc. | Sample preparation for metals analysis using accelerated acid digestion (aad) |
| JP2008285738A (en) * | 2007-05-21 | 2008-11-27 | Jfe Steel Kk | Surface-treated steel sheet |
| US20080289958A1 (en) * | 2007-04-27 | 2008-11-27 | Janine Kardokus | Novel Manufacturing Design and Processing Methods and Apparatus for Sputtering Targets |
| US20110269311A1 (en) * | 2010-04-29 | 2011-11-03 | Medtronic, Inc. | Gold-tin etch using combination of halogen plasma and wet etch |
| CN104568916A (en) * | 2013-10-29 | 2015-04-29 | 青岛天恒机械有限公司 | Inductive coupling plasma atomic emission spectrometry for determining elements in nuclear-grade zirconium alloy |
| CN105223186A (en) * | 2015-10-28 | 2016-01-06 | 贵州航天精工制造有限公司 | Adopt the method for silicon content in ICP method Fast Measurement titanium or titanium alloy |
| CN105510301A (en) * | 2016-02-14 | 2016-04-20 | 内蒙古包钢钢联股份有限公司 | Method for measuring aluminum, magnesium, calcium, vanadium, titanium, nickel, copper and manganese in rare earth silicon-magnesium alloy |
| CN105823772A (en) * | 2015-01-09 | 2016-08-03 | 自贡硬质合金有限责任公司 | Method for detecting impurity element in tungsten carbide |
| CN111323410A (en) * | 2020-04-24 | 2020-06-23 | 钢研纳克成都检测认证有限公司 | Method for detecting content of multiple elements in stainless steel |
| CN111707513A (en) * | 2020-06-17 | 2020-09-25 | 宁波江丰电子材料股份有限公司 | Preparation method of NiV alloy metallographic specimen |
| CN112268893A (en) * | 2020-10-14 | 2021-01-26 | 宁波江丰电子材料股份有限公司 | Method for measuring molybdenum content and titanium content in molybdenum-titanium alloy by using inductively coupled plasma emission spectrometer |
| CN113390860A (en) * | 2021-06-29 | 2021-09-14 | 洛阳金鹭硬质合金工具有限公司 | Detection method for simultaneously detecting sixteen trace impurity elements in chromium carbide |
-
2021
- 2021-12-13 CN CN202111520994.6A patent/CN114113043A/en active Pending
Patent Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1998020341A1 (en) * | 1996-11-08 | 1998-05-14 | Mountain States Analytical, Inc. | Sample preparation for metals analysis using accelerated acid digestion (aad) |
| US20080289958A1 (en) * | 2007-04-27 | 2008-11-27 | Janine Kardokus | Novel Manufacturing Design and Processing Methods and Apparatus for Sputtering Targets |
| JP2008285738A (en) * | 2007-05-21 | 2008-11-27 | Jfe Steel Kk | Surface-treated steel sheet |
| US20110269311A1 (en) * | 2010-04-29 | 2011-11-03 | Medtronic, Inc. | Gold-tin etch using combination of halogen plasma and wet etch |
| CN104568916A (en) * | 2013-10-29 | 2015-04-29 | 青岛天恒机械有限公司 | Inductive coupling plasma atomic emission spectrometry for determining elements in nuclear-grade zirconium alloy |
| CN105823772A (en) * | 2015-01-09 | 2016-08-03 | 自贡硬质合金有限责任公司 | Method for detecting impurity element in tungsten carbide |
| CN105223186A (en) * | 2015-10-28 | 2016-01-06 | 贵州航天精工制造有限公司 | Adopt the method for silicon content in ICP method Fast Measurement titanium or titanium alloy |
| CN105510301A (en) * | 2016-02-14 | 2016-04-20 | 内蒙古包钢钢联股份有限公司 | Method for measuring aluminum, magnesium, calcium, vanadium, titanium, nickel, copper and manganese in rare earth silicon-magnesium alloy |
| CN111323410A (en) * | 2020-04-24 | 2020-06-23 | 钢研纳克成都检测认证有限公司 | Method for detecting content of multiple elements in stainless steel |
| CN111707513A (en) * | 2020-06-17 | 2020-09-25 | 宁波江丰电子材料股份有限公司 | Preparation method of NiV alloy metallographic specimen |
| CN112268893A (en) * | 2020-10-14 | 2021-01-26 | 宁波江丰电子材料股份有限公司 | Method for measuring molybdenum content and titanium content in molybdenum-titanium alloy by using inductively coupled plasma emission spectrometer |
| CN113390860A (en) * | 2021-06-29 | 2021-09-14 | 洛阳金鹭硬质合金工具有限公司 | Detection method for simultaneously detecting sixteen trace impurity elements in chromium carbide |
Non-Patent Citations (4)
| Title |
|---|
| 向清华，吴杰周，成东: "内标法测定镍钒合金中的钒含量", 《广东化工》, 30 July 2021 (2021-07-30) * |
| 成勇;袁金红;彭慧仙;: "电感耦合等离子体原子发射光谱法(ICP-OES)测定含钒尾渣中钒的含量", 中国无机分析化学, no. 04, 15 December 2013 (2013-12-15) * |
| 赵欢娟;杨军红;刘厚勇;王小静;高明明;: "ICP-AES测定钨镍铜合金中镍、铜含量", 山东化工, no. 15, 8 August 2020 (2020-08-08) * |
| 陈波;陈焱;谷德君;: "凸点下金属层湿法刻蚀与凸点底切的控制", 半导体技术, no. 12, 3 December 2009 (2009-12-03) * |
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