CN112268893A - Method for measuring molybdenum content and titanium content in molybdenum-titanium alloy by using inductively coupled plasma emission spectrometer - Google Patents
Method for measuring molybdenum content and titanium content in molybdenum-titanium alloy by using inductively coupled plasma emission spectrometer Download PDFInfo
- Publication number
- CN112268893A CN112268893A CN202011099155.7A CN202011099155A CN112268893A CN 112268893 A CN112268893 A CN 112268893A CN 202011099155 A CN202011099155 A CN 202011099155A CN 112268893 A CN112268893 A CN 112268893A
- Authority
- CN
- China
- Prior art keywords
- molybdenum
- titanium
- sample
- content
- solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Engineering & Computer Science (AREA)
- Plasma & Fusion (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention relates to a method for determining molybdenum content and titanium content in molybdenum-titanium alloy by using an inductively coupled plasma emission spectrometer, which comprises the steps of adding a molybdenum-titanium alloy sample into a mixed solution of concentrated nitric acid and hydrofluoric acid, heating at 90-110 ℃ to completely dissolve the molybdenum-titanium alloy sample, adding water to dilute and fix the volume to obtain a sample solution; and then, measuring the molybdenum content and the titanium content in the sample solution by using the inductively coupled plasma emission spectrometer, thereby obtaining the molybdenum content and the titanium content in the molybdenum-titanium alloy sample. The method provided by the invention develops an effective acid solution capable of dissolving the molybdenum-titanium alloy, so that a sample solution capable of being used for an inductively coupled plasma emission spectrometer is prepared, and the requirement of simultaneously measuring the molybdenum content and the titanium content in the molybdenum-titanium alloy by using the inductively coupled plasma emission spectrometer is met.
Description
Technical Field
The invention relates to the technical field of analytical chemistry, in particular to a method for measuring molybdenum content and titanium content in molybdenum-titanium alloy by using an inductively coupled plasma emission spectrometer.
Background
The molybdenum-titanium alloy is an alloy formed by adding minimum titanium element into molybdenum phase as a basic element, the nominal component of the general alloy is Mo-0.5 Ti, the mass fraction of titanium in the molybdenum-titanium alloy is generally 0.4-0.55%, on one hand, the titanium is dissolved in the molybdenum in a solid solution manner and can play a role in solid solution strengthening, and on the other hand, the titanium can improve the low-temperature plasticity of the molybdenum and the recrystallization temperature of the molybdenum. At present, most molybdenum-titanium alloys are prepared into alloy ingots by powder mixing, pressing and sintering, and then are processed into materials.
One of the important uses of molybdenum-titanium alloy is as a molybdenum-titanium alloy target material, and then a molybdenum-titanium film is formed on a substrate through magnetron sputtering. For example, CN106148903A discloses a method for manufacturing a molybdenum-titanium alloy target, which includes: providing molybdenum powder and titanium powder; mixing the molybdenum powder and the titanium powder to form mixed powder; preparing the mixed powder into a molybdenum-titanium alloy target blank by adopting a vacuum hot pressing process with the heat preservation temperature of 1200-1300 ℃; and preparing the molybdenum-titanium alloy target blank into a molybdenum-titanium alloy target. The manufacturing method can obtain the high-density molybdenum-titanium alloy target with the density of more than or equal to 99 percent, and the obtained molybdenum-titanium alloy target has a uniform microstructure and can meet the requirements of magnetron sputtering on the purity and the density of the target. The molybdenum-titanium thin film formed by magnetron sputtering using a molybdenum-titanium alloy target can be used as a base film or a cover film required for a wiring electrode film of Al, Cu or the like.
Because the purity of the molybdenum-titanium alloy target material has an important influence on the molybdenum-titanium film generated by magnetron sputtering, once the molybdenum-titanium alloy target material with the purity not up to the standard is adopted for magnetron sputtering, the generated molybdenum-titanium film is not up to the standard, the waste of energy and materials is caused, the substrate is scrapped, and the irreparable loss is caused. Therefore, after the molybdenum-titanium alloy target material is synthesized, purity detection is required to judge whether the molybdenum-titanium alloy target material can be used for subsequent magnetron sputtering. At present, an inductively coupled plasma emission spectrometer (ICP-OES for short) is generally adopted to detect components of a metal material, and the inductively coupled plasma emission spectrometer not only can detect most of metal elements and part of non-metal elements, but also has the advantages of less interference, stable signal, simplicity in operation and the like.
In the process of detecting the components of the metal material by using the inductively coupled plasma emission spectrometer, the metal material to be detected needs to be dissolved by acid liquor, and then the sample solution is obtained by constant volume dilution. Although the chemical properties of pure molybdenum metal and pure titanium metal are relatively stable and are not easy to dissolve in acid liquor, for example, pure molybdenum metal is not corroded by air at normal temperature and does not react with hydrochloric acid or hydrofluoric acid, and pure titanium metal does not react with nitric acid and aqua regia at normal temperature. However, the prior art still develops an acid solution formula for dissolving pure molybdenum metal and pure titanium metal, the pure molybdenum metal can be dissolved by aqua regia, and the pure titanium metal can react with 27% hydrochloric acid at normal temperature, react with dilute hydrochloric acid in a boiling state, and can also react with hydrofluoric acid. However, molybdenum-titanium alloy is an alloy formed by adding a minimum amount of titanium element into molybdenum phase as a basic element, and the titanium element not only plays a role in solid solution strengthening, but also increases the recrystallization temperature of molybdenum, so that the chemical properties of the molybdenum-titanium alloy are more stable, and an effective acid solution capable of dissolving the molybdenum-titanium alloy is not developed so far.
In summary, there is a need to develop an effective acid solution capable of dissolving a molybdenum-titanium alloy to prepare a sample solution for an inductively coupled plasma emission spectrometer, i.e., a method for determining the molybdenum content and the titanium content in the molybdenum-titanium alloy by using the inductively coupled plasma emission spectrometer.
Disclosure of Invention
In view of the problems in the prior art, the invention provides a method for measuring the molybdenum content and the titanium content in a molybdenum-titanium alloy by using an inductively coupled plasma emission spectrometer, and the method develops an effective acid solution capable of dissolving the molybdenum-titanium alloy, namely, a molybdenum-titanium alloy sample is added into a mixed solution of concentrated nitric acid and hydrofluoric acid and heated at 90-110 ℃ to completely dissolve the molybdenum-titanium alloy sample, then water is added to dilute the mixed solution to a constant volume to obtain a sample solution, and the sample solution which can be used for the inductively coupled plasma emission spectrometer is further prepared, so that the requirement for simultaneously measuring the molybdenum content and the titanium content in the molybdenum-titanium alloy by using the inductively coupled plasma emission spectrometer is met.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a method for measuring molybdenum content and titanium content in molybdenum-titanium alloy by using an inductively coupled plasma emission spectrometer, which comprises the following steps:
firstly, adding a molybdenum-titanium alloy sample into a mixed solution of concentrated nitric acid and hydrofluoric acid, heating at 90-110 ℃ to completely dissolve the molybdenum-titanium alloy sample, and then adding water to dilute to a constant volume to obtain a sample solution; and then, measuring the molybdenum content and the titanium content in the sample solution by using the inductively coupled plasma emission spectrometer, thereby obtaining the molybdenum content and the titanium content in the molybdenum-titanium alloy sample.
According to the method, a molybdenum-titanium alloy sample is added into a mixed solution of concentrated nitric acid and hydrofluoric acid, the mixed solution is heated at 90-110 ℃, the specific ratio of the concentrated nitric acid to the hydrofluoric acid is limited, the dissolving rate is further accelerated by heating, the molybdenum-titanium alloy sample can be effectively and completely dissolved, then the sample solution is obtained by adding water to dilute and fix the volume, and then the sample solution which can be used for an inductively coupled plasma emission spectrometer is prepared, so that the requirement of simultaneously measuring the molybdenum content and the titanium content in the molybdenum-titanium alloy by using the inductively coupled plasma emission spectrometer is met.
The inductively coupled plasma emission spectrometer used in the invention is an iCAP6300Radial full-spectrum direct-reading inductively coupled plasma emission spectrometer of Seimer Feishale, USA.
The concentrated nitric acid and hydrofluoric acid used in the invention are both high-grade pure reagents, and the experimental water is first-grade water meeting the regulation in GB/T6682.
The heating temperature in the process of the invention is 90-110 ℃, for example 90 ℃, 95 ℃, 100 ℃, 105 ℃ or 110 ℃ and the like, but is not limited to the recited values, and other values not recited in the range of values are equally applicable.
As a preferred technical scheme of the invention, the method comprises the following steps:
(1) preparation of a sample solution: firstly, adding a molybdenum-titanium alloy sample into a mixed solution of concentrated nitric acid and hydrofluoric acid, heating at 90-110 ℃ to completely dissolve the molybdenum-titanium alloy sample, 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 molybdenum and titanium;
(3) drawing a standard curve: preparing a mixed standard solution of molybdenum and titanium, measuring the emission light intensity of the molybdenum and the titanium 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: and (3) measuring the emission intensity of the molybdenum element and the titanium element in the sample solution under the analysis spectral line in the step (2) by using the inductively coupled plasma emission spectrometer, and determining the contents of the molybdenum element and the titanium element in the sample solution according to the standard curve drawn in the step (3) so as to obtain the molybdenum content and the titanium content in the molybdenum-titanium alloy sample.
As a preferred embodiment of the present invention, the concentration of the concentrated nitric acid in step (1) is 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 range of the recited values are also applicable.
Preferably, the concentration of hydrofluoric acid in step (1) is 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 not recited within the range of values are equally applicable.
Preferably, the volume ratio of the concentrated nitric acid to the hydrofluoric acid in the step (1) is 1 (1-3), such as 1:1, 1:1.5, 1:2, 1:2.5 or 1:3, but not limited to the recited values, and other values not recited in the range of the values are also applicable.
As a preferred embodiment of the present invention, the ratio of the mass of the molybdenum-titanium alloy sample to the volume of the mixed solution in step (1) is 1g (40-80) mL, for example, 1g:40mL, 1g:45mL, 1g:50mL, 1g:55mL, 1g:60mL, 1g:65mL, 1g:70mL, 1g:75mL, or 1g:80mL, but the present invention is not limited to the above-mentioned values, and other values not listed in the above-mentioned value range are also applicable.
Preferably, the heating time in step (1) is 20-50min, such as 20min, 25min, 30min, 35min, 40min, 45min or 50min, but not limited to the recited values, and other values not recited in the range of values are also applicable.
In a preferred embodiment of the present invention, in the step (2), the analytical line of the molybdenum element is 202.032nm, and the analytical line of the titanium element is 336.122 nm.
As is well known to those skilled in the art, an inductively coupled plasma emission spectrometer provides dozens of spectral lines, different spectral lines are adopted, the measured results are far from each other, and great interference exists among the spectral lines, so that not only is interference among different spectral lines of the same element exist, but also coexisting ions in a solution can cause serious interference on the selection of the spectral lines, and the intensities of different spectral lines are different, therefore, according to the composition of coexisting ions in the sample solution, the method screens the analysis spectral lines of molybdenum element and titanium element, finally selects the analysis spectral line of the molybdenum element to be 202.032nm, and the analysis spectral line of the titanium element to be 336.122 nm.
As a preferable technical solution of the present invention, the step of preparing the mixed standard solution of molybdenum and titanium in step (3) includes:
weighing molybdenum and titanium, and preparing a mixed standard solution with gradient molybdenum and titanium content according to the method in the step (1).
As a preferable technical scheme of the invention, the mass percent of the molybdenum is more than or equal to 99.999%.
Preferably, the mass percent of the titanium 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 molybdenum titanium content gradient of 90:10, 85:15, 80:20, 75:25, 70:30, 65:35 and 60: 40.
Preferably, the mixed standard solution is sequentially introduced into the inductively coupled plasma emission spectrometer from low to high according to the concentration of the titanium element, the emission light intensity of the molybdenum element and the titanium 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 molybdenum and titanium 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 molybdenum element and titanium 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 introduction system, can meet the purpose of measuring the contents of molybdenum and titanium in the molybdenum-titanium 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 independently: 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: adding a molybdenum-titanium alloy sample into a mixed solution of concentrated nitric acid and hydrofluoric acid with a volume ratio of 1 (1-3), controlling the ratio of the mass of the molybdenum-titanium alloy sample to the volume of the mixed solution to be 1g (40-80) mL, heating at 90-110 ℃ for 20-50min to completely dissolve the molybdenum-titanium alloy sample, 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 molybdenum and titanium, wherein the analysis spectral line of the molybdenum is 202.032nm, and the analysis spectral line of the titanium is 336.122 nm;
(3) drawing a standard curve: weighing molybdenum with the mass percent of more than or equal to 99.999% and titanium with the mass percent of more than or equal to 99.999%, and preparing at least five mixed standard solutions with the molybdenum and titanium contents changing in a gradient manner according to the method in the step (1), wherein the molybdenum and titanium contents of the mixed standard solutions are 90:10, 85:15, 80:20, 75:25, 70:30, 65:35 and 60:40 in a gradient manner;
introducing the mixed standard solution into the inductively coupled plasma emission spectrometer sequentially from low concentration to high concentration of the titanium element through a hydrofluoric acid-resistant sample introduction system, measuring the emission light intensity of the molybdenum element and the titanium element under the analysis spectral line in the step (2), and drawing a standard curve;
(4) detecting a sample: and (3) introducing the sample solution prepared in the step (1) into the inductively coupled plasma emission spectrometer through a hydrofluoric acid-resistant sample introduction system, measuring the emission light intensity of molybdenum and titanium under the analysis spectral line in the step (2), and determining the contents of the molybdenum and the titanium in the sample solution according to the standard curve drawn in the step (3) so as to obtain the molybdenum content and the titanium content in the molybdenum-titanium alloy sample.
Compared with the prior art, the invention has at least the following beneficial effects:
according to the method, the molybdenum-titanium alloy sample is added into the mixed solution of concentrated nitric acid and hydrofluoric acid and heated at 90-110 ℃, so that the molybdenum-titanium alloy sample can be effectively and completely dissolved, and then the sample solution is obtained by diluting with water and fixing the volume, so that the sample solution which can be used for the inductively coupled plasma emission spectrometer is prepared, and the requirements of simultaneously measuring the molybdenum content and the titanium content in the molybdenum-titanium alloy by using the inductively coupled plasma emission spectrometer are 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: iCAP6300Radial full-spectrum direct-reading inductively coupled plasma emission spectrometer of Seimer Feishale, 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.
Example 1
The embodiment provides a method for measuring molybdenum content and titanium content in a molybdenum-titanium alloy by using an inductively coupled plasma emission spectrometer, which comprises the following steps:
(1) preparation of a sample solution: firstly, adding a molybdenum-titanium alloy sample into a mixed solution of concentrated nitric acid and hydrofluoric acid in a volume ratio of 1:2, controlling the ratio of the mass of the molybdenum-titanium alloy sample to the volume of the mixed solution to be 1g:60mL, heating at 100 ℃ for 30min to completely dissolve the molybdenum-titanium alloy sample, and then adding water to dilute to a constant volume to obtain a sample solution;
wherein the concentration of the concentrated nitric acid is 68 wt%, and the concentration of the hydrofluoric acid is 36 wt%;
(2) selecting an element spectral line: selecting analysis spectral lines of molybdenum and titanium, wherein the analysis spectral line of the molybdenum is 202.032nm, and the analysis spectral line of the titanium is 336.122 nm;
(3) drawing a standard curve: weighing molybdenum with the mass percent of more than or equal to 99.999% and titanium with the mass percent of more than or equal to 99.999%, and preparing seven mixed standard solutions with the molybdenum and titanium contents changing in a gradient manner according to the method in the step (1), wherein the molybdenum and titanium contents of the mixed standard solutions are 90:10, 85:15, 80:20, 75:25, 70:30, 65:35 and 60:40 in a gradient manner;
introducing the mixed standard solution into the inductively coupled plasma emission spectrometer sequentially from low concentration to high concentration of the titanium element through a hydrofluoric acid-resistant sample introduction system, measuring the emission light intensity of the molybdenum element and the titanium element under the analysis spectral line in the step (2), and drawing a standard curve;
(4) detecting a sample: and (3) introducing the sample solution prepared in the step (1) into the inductively coupled plasma emission spectrometer through a hydrofluoric acid-resistant sample introduction system, measuring the emission light intensity of molybdenum and titanium under the analysis spectral line in the step (2), and determining the contents of the molybdenum and the titanium in the sample solution according to the standard curve drawn in the step (3) so as to obtain the molybdenum content and the titanium content in the molybdenum-titanium alloy sample.
The molybdenum-titanium alloy sample can be completely dissolved, the content of molybdenum element obtained by measurement is 66.38 wt%, the content of titanium element is 33.62 wt%, and the molybdenum-titanium alloy sample has the advantages of simple operation and high accuracy.
Example 2
The embodiment provides a method for measuring molybdenum content and titanium content in a molybdenum-titanium alloy by using an inductively coupled plasma emission spectrometer, which comprises the following steps:
(1) preparation of a sample solution: firstly, adding a molybdenum-titanium alloy sample into a mixed solution of concentrated nitric acid and hydrofluoric acid in a volume ratio of 1:1, controlling the ratio of the mass of the molybdenum-titanium alloy sample to the volume of the mixed solution to be 1g:80mL, heating at 90 ℃ for 50min to completely dissolve the molybdenum-titanium alloy sample, and then adding water to dilute to a constant volume to obtain a sample solution;
wherein the concentration of the concentrated nitric acid is 65 wt%, and the concentration of the hydrofluoric acid is 40 wt%;
(2) selecting an element spectral line: selecting analysis spectral lines of molybdenum and titanium, wherein the analysis spectral line of the molybdenum is 202.032nm, and the analysis spectral line of the titanium is 336.122 nm;
(3) drawing a standard curve: weighing molybdenum with the mass percent of more than or equal to 99.999% and titanium with the mass percent of more than or equal to 99.999%, and preparing seven mixed standard solutions with the molybdenum and titanium contents changing in a gradient manner according to the method in the step (1), wherein the molybdenum and titanium contents of the mixed standard solutions are 90:10, 85:15, 80:20, 75:25, 70:30, 65:35 and 60:40 in a gradient manner;
introducing the mixed standard solution into the inductively coupled plasma emission spectrometer sequentially from low concentration to high concentration of the titanium element through a hydrofluoric acid-resistant sample introduction system, measuring the emission light intensity of the molybdenum element and the titanium element under the analysis spectral line in the step (2), and drawing a standard curve;
(4) detecting a sample: and (3) introducing the sample solution prepared in the step (1) into the inductively coupled plasma emission spectrometer through a hydrofluoric acid-resistant sample introduction system, measuring the emission light intensity of molybdenum and titanium under the analysis spectral line in the step (2), and determining the contents of the molybdenum and the titanium in the sample solution according to the standard curve drawn in the step (3) so as to obtain the molybdenum content and the titanium content in the molybdenum-titanium alloy sample.
The molybdenum-titanium alloy sample can be completely dissolved, the content of molybdenum element obtained by measurement is 66.34 wt%, the content of titanium element is 33.66 wt%, and the molybdenum-titanium alloy sample has the advantages of simple operation and high accuracy.
Example 3
The embodiment provides a method for measuring molybdenum content and titanium content in a molybdenum-titanium alloy by using an inductively coupled plasma emission spectrometer, which comprises the following steps:
(1) preparation of a sample solution: firstly, adding a molybdenum-titanium alloy sample into a mixed solution of concentrated nitric acid and hydrofluoric acid in a volume ratio of 1:3, controlling the ratio of the mass of the molybdenum-titanium alloy sample to the volume of the mixed solution to be 1g:40mL, heating at 110 ℃ for 20min to completely dissolve the molybdenum-titanium alloy sample, and then adding water to dilute to a constant volume to obtain a sample solution;
wherein the concentration of the concentrated nitric acid is 68 wt%, and the concentration of the hydrofluoric acid is 30 wt%;
(2) selecting an element spectral line: selecting analysis spectral lines of molybdenum and titanium, wherein the analysis spectral line of the molybdenum is 202.032nm, and the analysis spectral line of the titanium is 336.122 nm;
(3) drawing a standard curve: weighing molybdenum with the mass percent of more than or equal to 99.999% and titanium with the mass percent of more than or equal to 99.999%, and preparing seven mixed standard solutions with the molybdenum and titanium contents changing in a gradient manner according to the method in the step (1), wherein the molybdenum and titanium contents of the mixed standard solutions are 90:10, 85:15, 80:20, 75:25, 70:30, 65:35 and 60:40 in a gradient manner;
introducing the mixed standard solution into the inductively coupled plasma emission spectrometer sequentially from low concentration to high concentration of the titanium element through a hydrofluoric acid-resistant sample introduction system, measuring the emission light intensity of the molybdenum element and the titanium element under the analysis spectral line in the step (2), and drawing a standard curve;
(4) detecting a sample: and (3) introducing the sample solution prepared in the step (1) into the inductively coupled plasma emission spectrometer through a hydrofluoric acid-resistant sample introduction system, measuring the emission light intensity of molybdenum and titanium under the analysis spectral line in the step (2), and determining the contents of the molybdenum and the titanium in the sample solution according to the standard curve drawn in the step (3) so as to obtain the molybdenum content and the titanium content in the molybdenum-titanium alloy sample.
The molybdenum-titanium alloy sample can be completely dissolved, the content of the molybdenum element obtained by measurement is 66.43 wt%, and the content of the titanium element is 33.57 wt%, so that the molybdenum-titanium alloy sample has the advantages of simplicity in operation and high accuracy.
Comparative example 1
This comparative example provides a method for measuring the molybdenum content and the titanium content in a molybdenum-titanium alloy using an inductively coupled plasma emission spectrometer, except that the "mixed solution of concentrated nitric acid and hydrofluoric acid at a volume ratio of 1: 2" described in step (1) was replaced with "aqua regia (prepared from concentrated hydrochloric acid at a concentration of 38 wt% and concentrated nitric acid at a concentration of 68 wt% at a volume ratio of 3: 1)", and the other conditions were completely the same as in example 1.
The molybdenum-titanium alloy sample in the comparative example is basically not dissolved, and cannot be prepared into a sample solution which can be used for an inductively coupled plasma emission spectrometer, so that the requirement for simultaneously measuring the molybdenum content and the titanium content in the molybdenum-titanium alloy by using the inductively coupled plasma emission spectrometer cannot be met.
Comparative example 2
The comparative example provides a method for measuring the molybdenum content and the titanium content in the molybdenum-titanium alloy by using an inductively coupled plasma emission spectrometer, except that the condition of heating at 100 ℃ for 30min in the step (1) is replaced by the condition of heating at 25 ℃ for 30min, and the other conditions are completely the same as the condition of the example 1.
The molybdenum-titanium alloy sample in the comparative example is basically not dissolved, and cannot be prepared into a sample solution which can be used for an inductively coupled plasma emission spectrometer, so that the requirement for simultaneously measuring the molybdenum content and the titanium content in the molybdenum-titanium alloy by using the inductively coupled plasma emission spectrometer cannot be met.
In conclusion, the method of the invention adds the molybdenum-titanium alloy sample into the mixed solution of concentrated nitric acid and hydrofluoric acid, heats the mixed solution at 90-110 ℃, can effectively and completely dissolve the molybdenum-titanium alloy sample, then obtains the sample solution by adding water to dilute and fix the volume, and further prepares the sample solution which can be used for the inductively coupled plasma emission spectrometer, thereby meeting the requirement of simultaneously measuring the molybdenum content and the titanium content in the molybdenum-titanium alloy by using the inductively coupled plasma emission spectrometer.
The applicant states that the present invention is illustrated by the above examples to show the detailed process equipment and process flow of the present invention, but the present invention is not limited to the above detailed process equipment and process flow, i.e. it does not mean that the present invention must rely on the above detailed process equipment and process flow to be implemented. 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 content of molybdenum and the content of titanium in a molybdenum-titanium alloy by using an inductively coupled plasma emission spectrometer is characterized by comprising the following steps of:
firstly, adding a molybdenum-titanium alloy sample into a mixed solution of concentrated nitric acid and hydrofluoric acid, heating at 90-110 ℃ to completely dissolve the molybdenum-titanium alloy sample, and then adding water to dilute to a constant volume to obtain a sample solution; and then, measuring the molybdenum content and the titanium content in the sample solution by using the inductively coupled plasma emission spectrometer, thereby obtaining the molybdenum content and the titanium content in the molybdenum-titanium alloy sample.
2. Method according to claim 1, characterized in that it comprises the following steps:
(1) preparation of a sample solution: firstly, adding a molybdenum-titanium alloy sample into a mixed solution of concentrated nitric acid and hydrofluoric acid, heating at 90-110 ℃ to completely dissolve the molybdenum-titanium alloy sample, 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 molybdenum and titanium;
(3) drawing a standard curve: preparing a mixed standard solution of molybdenum and titanium, measuring the emission light intensity of the molybdenum and the titanium 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: and (3) measuring the emission intensity of the molybdenum element and the titanium element in the sample solution under the analysis spectral line in the step (2) by using the inductively coupled plasma emission spectrometer, and determining the contents of the molybdenum element and the titanium element in the sample solution according to the standard curve drawn in the step (3) so as to obtain the molybdenum content and the titanium content in the molybdenum-titanium alloy sample.
3. The process of claim 2, wherein the concentration of the concentrated nitric acid in 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 to the hydrofluoric acid in the step (1) is 1 (1-3).
4. The method according to claim 2 or 3, wherein the ratio between the mass of the molybdenum-titanium alloy sample and the volume of the mixed solution in step (1) is 1g (40-80) mL;
preferably, the heating time in step (1) is 20-50 min.
5. The process according to any one of claims 2 to 4, wherein in step (2) the analytical line for the molybdenum element is 202.032nm and the analytical line for the titanium element is 336.122 nm.
6. The method according to any one of claims 2 to 5, wherein the step of preparing the mixed standard solution of the molybdenum element and the titanium element in the step (3) comprises:
weighing molybdenum and titanium, and preparing a mixed standard solution with gradient molybdenum and titanium content according to the method in the step (1).
7. The method according to claim 6, wherein the mass percent of the molybdenum is more than or equal to 99.999%;
preferably, the mass percent of the titanium 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 molybdenum titanium content gradient of 90:10, 85:15, 80:20, 75:25, 70:30, 65:35 and 60: 40;
preferably, the mixed standard solution is sequentially introduced into the inductively coupled plasma emission spectrometer from low to high according to the concentration of the titanium element, the emission light intensity of the molybdenum element and the titanium 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 emission light intensities of molybdenum element and titanium element under the analysis line are 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 molybdenum element and titanium 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: adding a molybdenum-titanium alloy sample into a mixed solution of concentrated nitric acid and hydrofluoric acid with a volume ratio of 1 (1-3), controlling the ratio of the mass of the molybdenum-titanium alloy sample to the volume of the mixed solution to be 1g (40-80) mL, heating at 90-110 ℃ for 20-50min to completely dissolve the molybdenum-titanium alloy sample, 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 molybdenum and titanium, wherein the analysis spectral line of the molybdenum is 202.032nm, and the analysis spectral line of the titanium is 336.122 nm;
(3) drawing a standard curve: weighing molybdenum with the mass percent of more than or equal to 99.999% and titanium with the mass percent of more than or equal to 99.999%, and preparing at least five mixed standard solutions with the molybdenum and titanium contents changing in a gradient manner according to the method in the step (1), wherein the molybdenum and titanium contents of the mixed standard solutions are 90:10, 85:15, 80:20, 75:25, 70:30, 65:35 and 60:40 in a gradient manner;
introducing the mixed standard solution into the inductively coupled plasma emission spectrometer sequentially from low concentration to high concentration of the titanium element through a hydrofluoric acid-resistant sample introduction system, measuring the emission light intensity of the molybdenum element and the titanium element under the analysis spectral line in the step (2), and drawing a standard curve;
(4) detecting a sample: and (3) introducing the sample solution prepared in the step (1) into the inductively coupled plasma emission spectrometer through a hydrofluoric acid-resistant sample introduction system, measuring the emission light intensity of molybdenum and titanium under the analysis spectral line in the step (2), and determining the contents of the molybdenum and the titanium in the sample solution according to the standard curve drawn in the step (3) so as to obtain the molybdenum content and the titanium content in the molybdenum-titanium alloy sample.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011099155.7A CN112268893A (en) | 2020-10-14 | 2020-10-14 | Method for measuring molybdenum content and titanium content in molybdenum-titanium alloy by using inductively coupled plasma emission spectrometer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011099155.7A CN112268893A (en) | 2020-10-14 | 2020-10-14 | Method for measuring molybdenum content and titanium content in molybdenum-titanium alloy by using inductively coupled plasma emission spectrometer |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112268893A true CN112268893A (en) | 2021-01-26 |
Family
ID=74338079
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011099155.7A Pending CN112268893A (en) | 2020-10-14 | 2020-10-14 | Method for measuring molybdenum content and titanium content in molybdenum-titanium alloy by using inductively coupled plasma emission spectrometer |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112268893A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113237871A (en) * | 2021-05-19 | 2021-08-10 | 宁波江丰电子材料股份有限公司 | Method for detecting AlSc alloy components |
| CN114113044A (en) * | 2021-12-13 | 2022-03-01 | 宁波江丰电子材料股份有限公司 | Method for measuring nickel and iron content in NiFe alloy by using inductively coupled plasma emission spectrometer |
| CN114113043A (en) * | 2021-12-13 | 2022-03-01 | 宁波江丰电子材料股份有限公司 | Method for measuring nickel and vanadium content in NiV alloy by using inductively coupled plasma emission spectrometer |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101303307A (en) * | 2008-07-08 | 2008-11-12 | 株洲硬质合金集团有限公司 | Analyses testing method of aluminum, calcium, iron, molybdenum, niobium, titanium, tungsten impurity elements in chromium carbide |
| 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 |
| CN111024679A (en) * | 2019-12-17 | 2020-04-17 | 中核北方核燃料元件有限公司 | Method for measuring chemical components in Inconel |
| 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 |
-
2020
- 2020-10-14 CN CN202011099155.7A patent/CN112268893A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101303307A (en) * | 2008-07-08 | 2008-11-12 | 株洲硬质合金集团有限公司 | Analyses testing method of aluminum, calcium, iron, molybdenum, niobium, titanium, tungsten impurity elements in chromium carbide |
| 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 |
| CN111024679A (en) * | 2019-12-17 | 2020-04-17 | 中核北方核燃料元件有限公司 | Method for measuring chemical components in Inconel |
| 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 |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113237871A (en) * | 2021-05-19 | 2021-08-10 | 宁波江丰电子材料股份有限公司 | Method for detecting AlSc alloy components |
| CN114113044A (en) * | 2021-12-13 | 2022-03-01 | 宁波江丰电子材料股份有限公司 | Method for measuring nickel and iron content in NiFe alloy by using inductively coupled plasma emission spectrometer |
| CN114113043A (en) * | 2021-12-13 | 2022-03-01 | 宁波江丰电子材料股份有限公司 | Method for measuring nickel and vanadium content in NiV alloy by using inductively coupled plasma emission spectrometer |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN112268893A (en) | Method for measuring molybdenum content and titanium content in molybdenum-titanium alloy by using inductively coupled plasma emission spectrometer | |
| CN102564834B (en) | Digestion method of metallurgical materials and detection method | |
| Ishizuka et al. | Determination of trace inpurities high-purity aluminum oxide by inductively-coupled plasma atomic emission-spectrometry | |
| Hu et al. | Determination of trace elements in super alloy by ICP-MS | |
| CN107632011B (en) | Method for measuring content of impurity elements in high-purity bismuth | |
| Zhen et al. | Matrix-assisted photochemical vapor generation for determination of trace bismuth in FeNi based alloy samples by inductively coupled plasma mass spectrometry | |
| CN105806826A (en) | Method for determining content of elements in potassium-bearing ore by ICP (Inductively Coupled Plasma) internal standard method | |
| CN109030465B (en) | Method for detecting content of strontium, iron, barium, magnesium and calcium in zinc-strontium alloy | |
| CN109324036A (en) | The method that ICP measures lanthanum, cobalt, strontium, barium, calcium content in permanent-magnet ferrite | |
| CN111982890A (en) | Mixed acid for dissolving molybdenum-titanium-nickel alloy and preparation method and application thereof | |
| CN111257097A (en) | Vanadium carbide sample to be tested manufacturing method and impurity content analysis method thereof | |
| CN114739982A (en) | Method for detecting element content in glass | |
| CN109060774B (en) | Method for detecting contents of calcium, iron, aluminum, magnesium and manganese in zinc-calcium alloy | |
| Balaram | Recent developments in analytical techniques for characterization of ultra pure materials—An overview | |
| Coedo et al. | A micro-scale mercury cathode electrolysis procedure for on-line flow injection inductively coupled plasma mass spectrometry trace elements analysis in steel samples | |
| Diegor et al. | Parameter interaction in signal optimization of an ICP mass spectrometer | |
| Hu et al. | Determination of elemental impurities in iron-nickel-based superalloys by glow discharge mass spectrometry | |
| CN114113043A (en) | Method for measuring nickel and vanadium content in NiV alloy by using inductively coupled plasma emission spectrometer | |
| Sun et al. | Evaluation of closed-vessel microwave digestion method for the determination of trace impurities in polymer-based photoresist by inductively coupled plasma mass spectrometry | |
| CN112683611A (en) | Digestion solution and method for determining element content in refined aluminum ingot for remelting | |
| Paama et al. | Optimal conditions for europium and samarium determination in cathodoluminophors by inductively coupled plasma atomic emission spectrometry | |
| Khomyakov et al. | Purity of MoO 3 from different manufacturers | |
| JPH10132801A (en) | Analytical method for composition composed of ceramic and of amphoteric metal | |
| CN110715913A (en) | Method for measuring selenium in geochemical sample by atomic fluorescence spectrometry | |
| CN114113044A (en) | Method for measuring nickel and iron content in NiFe alloy by using inductively coupled plasma emission spectrometer |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210126 |