CN112710728A - Method for measuring content of aluminum, magnesium and other impurity elements in silicon carbide composite material - Google Patents
Method for measuring content of aluminum, magnesium and other impurity elements in silicon carbide composite material Download PDFInfo
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Abstract
The invention belongs to the technical field of chemical detection, and particularly relates to a method for determining the content of impurity elements such as aluminum, magnesium and the like in a silicon carbide composite material. The method adopts a plasma mass spectrometry method to determine the content of 18 impurity elements in the silicon carbide. The leaching condition, detection limit, matrix concentration condition, acidity condition, atomizer flow and internal standard element of the silicon carbide sample are researched, and matrix interference and coexisting element interference conditions are investigated. The correlation coefficient of each element is not less than 0.999. The precision of the method is better than 10 percent, and the average recovery rate is between 90 and 110 percent.
Description
Technical Field
The invention belongs to the technical field of chemical detection, and particularly relates to a method for determining the content of impurity elements such as aluminum, magnesium and the like in a silicon carbide composite material.
Background
Silicon carbide has high hardness, good wear resistance and grinding performance, and uranium has high stability against thermal shock, oxidation, chemical agents, molten salts and molten metals. In recent years, a lot of reports about the detection of chemical elements are provided, and the national standard GB/T3045 and 2003 ordinary abrasive silicon carbide analysis method are published. However, GB/T3045 and 2003 stipulate analysis methods for 9 detection items including total carbon content, free carbon content, silicon dioxide content, free silicon content, silicon carbide content, ferric oxide content, aluminum oxide content, calcium oxide content and magnesium oxide content in common abrasive silicon carbide materials. The method cannot comprise the analysis of other multiple impurity elements and cannot meet the current technical development.
Disclosure of Invention
In view of the above disadvantages, the present invention aims to provide a method for measuring the content of impurity elements such as aluminum, magnesium, etc. in a silicon carbide composite material, which establishes sample treatment according to the application requirements of the silicon carbide composite material, selects appropriate analysis conditions for each element, and completes the detection method for measuring the content of 18 impurity elements such as aluminum, magnesium, iron, calcium, cadmium, cobalt, copper, lead, manganese, molybdenum, nickel, titanium, vanadium, boron, tungsten, chromium, tin, yttrium in the silicon carbide material.
The technical scheme of the invention is as follows:
a method for measuring the content of impurity elements such as aluminum, magnesium and the like in a silicon carbide composite material comprises the steps of firstly, sample treatment, secondly, determining the analysis mass number, and thirdly, measuring;
step one, sample processing;
the content of manganese, nickel, cobalt, chromium, tungsten, calcium, titanium and yttrium is 5-2000 mu g/g; the content of boron, vanadium, copper, tin and lead is 1-400 mu g/g; the cadmium content is 0.1-40 mu g/g; the content of aluminum, iron and magnesium is 10-4000 mug/g; detecting a silicon carbide sample with the molybdenum content of 0.5-200 mug/g;
the powder sample is directly used for analysis; crushing the samples in other states, and then analyzing the crushed samples by using powder;
taking a powdery sample, accurately measuring the powdery sample to 0.1mg, placing the sample in a quartz beaker, adding 5 times of high-grade pure nitric acid by volume, placing the sample in an ultrasonic cleaner, and ultrasonically leaching the sample for 30min at 100% power;
after the ultrasonic treatment is stopped, taking out the beaker and cooling to room temperature;
then filtering on a funnel by using medium-speed qualitative filter paper, washing the beaker for 3 times by using water, and washing filter residues for 3 times;
the filtrate is received into a volumetric flask, diluted to a scale by water and used as a sample solution for measuring 18 elements of aluminum, magnesium, iron, calcium, cadmium, cobalt, copper, lead, manganese, molybdenum, nickel, titanium, vanadium, boron, tungsten, chromium, tin and yttrium;
carrying out a blank experiment along with the sample, and using the blank experiment as a blank solution to be tested;
step two, determining the analysis mass number;
selecting a detection method of a silicon carbide sample on an inductively coupled plasma mass spectrometer, and determining the analysis mass number of 18 elements of aluminum, magnesium, iron, calcium, cadmium, cobalt, copper, lead, manganese, molybdenum, nickel, titanium, vanadium, boron, tungsten, chromium, tin and yttrium;
finally determining the analysis mass number of each element to be detected as boron-11, tin-118, nickel-60, aluminum-27, titanium-47, lead-208, calcium-44, vanadium-51, tungsten-186, cadmium-111, magnesium-24, cobalt-59, iron-57, chromium-52, molybdenum-98, manganese-55, copper-63 and yttrium-89;
step three, determination;
diluting 17 elements of national standard solution of aluminum, magnesium, iron, calcium, cadmium, cobalt, copper, lead, manganese, molybdenum, nickel, titanium, vanadium, boron, tungsten, chromium and yttrium and 17 elements of tin into mixed working standard solution according to the detection range of a sample; diluting rhodium national standard solution with the concentration of 1000 mug/mL into internal standard solution;
and sequentially measuring the working standard solution, the blank solution and the sample solution on an inductively coupled plasma mass spectrometer, continuously introducing an internal standard solution during measurement, and measuring the content of each element to be measured by using a standard curve method, wherein the unit is nanogram per milliliter (ng/mL).
In the first step, the sample is sieved by a sieve of 60 meshes to 100 meshes;
in the second step, in the mass number analysis, the mass number is determined by selecting isotopes which have large abundance and high sensitivity and can be free of interference or subjected to interference elimination and correction; selecting and comparing the mass number of each element to be detected, and comparing the mass number with a detection limit according to the interference factors of the coexisting elements;
in the second step, the selected mass numbers require that the linear correlation coefficients are all greater than 0.999.
In the third step, indium national standard solution with the concentration of 1000 mug/mL is adopted to be diluted into internal standard solution.
And in the third step, cesium national standard solution with the concentration of 1000 mug/mL is adopted to be diluted into internal standard solution.
The concentration of the national standard solution of the 17 elements in the third step is 1000 mug/mL.
The concentration of the national standard solution of tin in the third step is 500 mug/mL.
The invention has the beneficial effects that:
the method for detecting the content of 18 impurity elements in the silicon carbide is successfully established, the content of the impurity elements in the silicon carbide can be accurately determined by using the experimental conditions listed in the invention content (the range is shown in table 1), the problem of determination of the content of the impurity elements in the silicon carbide which is urgently needed in production is solved, and the requirement for detecting the content of the impurity elements in the silicon carbide is met. The correlation coefficient of each element is not less than 0.999 by using the method. The precision of the method is better than 10 percent, and the average recovery rate is between 90 and 110 percent.
TABLE 1 determination of impurity elements in silicon carbide
| Element(s) | Range (μ g/g) | Element(s) | Range (μ g/g) |
| Mn、Ni、Co、Cr、W、Ca、Ti、Y | 5～2000 | B、V、Cu、Sn、Pb | 1～400 |
| Cd | 0.1～40 | Al、Fe、Mg | 10～4000 |
| Mo | 0.5～200 | — | — |
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
A method for measuring the content of impurity elements such as aluminum, magnesium and the like in a silicon carbide composite material comprises the steps of firstly, sample treatment, secondly, determining the analysis mass number, and thirdly, measuring;
step one, sample processing;
the content of manganese, nickel, cobalt, chromium, tungsten, calcium, titanium and yttrium is (5-2000) mu g/g; the content of boron, vanadium, copper, tin and lead is (1-400) mu g/g; the cadmium content is (0.1-40) mu g/g; the content of aluminum, iron and magnesium is 10-4000 mu g/g; and (3) detecting the silicon carbide sample with the molybdenum content in the range of (0.5-200) mu g/g.
The sample is sieved by a sieve of 60 meshes to 100 meshes, and the powder sample is directly used for analysis; the samples in other states were crushed and analyzed with powder.
Taking a powdery sample, accurately measuring to 0.1mg, placing in a quartz beaker, adding 5 times of high-grade pure nitric acid, placing in an ultrasonic cleaner, and ultrasonically leaching for 30min at 100% power.
After the ultrasonic treatment is stopped, taking out the beaker and cooling to room temperature;
then, the mixture was filtered on a funnel with medium speed qualitative filter paper, the beaker was washed with water 3 times, and the residue was washed 3 times.
And (3) receiving the filtrate into a volumetric flask, diluting the filtrate to a scale with water, and taking the diluted filtrate as a sample solution for measuring 18 elements of aluminum, magnesium, iron, calcium, cadmium, cobalt, copper, lead, manganese, molybdenum, nickel, titanium, vanadium, boron, tungsten, chromium, tin and yttrium.
And carrying out a blank experiment along with the sample, and using the blank experiment as a blank solution to be tested.
Step two, determining the analysis mass number;
a detection method for selecting a silicon carbide sample on an inductively coupled plasma mass spectrometer (ICP-MS) determines the analysis mass number of 18 elements of aluminum, magnesium, iron, calcium, cadmium, cobalt, copper, lead, manganese, molybdenum, nickel, titanium, vanadium, boron, tungsten, chromium, tin and yttrium.
Analytical mass numbers general mass numbers are determined by selecting isotopes which have large abundance, high sensitivity, no interference, or can be subjected to interference elimination and correction. And under the working condition of the instrument, selecting and comparing the mass number of each element to be detected, and comparing the mass number with the detection limit according to the interference factors of the coexisting elements. The selected mass number requires a good linear relation of a determination standard curve, and the linear correlation coefficients are all larger than 0.999.
Finally determining the analysis mass number of each element to be detected to be boron-11, tin-118, nickel-60, aluminum-27, titanium-47, lead-208, calcium-44, vanadium-51, tungsten-186, cadmium-111, magnesium-24, cobalt-59, iron-57, chromium-52, molybdenum-98, manganese-55, copper-63 and yttrium-89.
Step three, determination;
the method is characterized in that 17 elements of aluminum, magnesium, iron, calcium, cadmium, cobalt, copper, lead, manganese, molybdenum, nickel, titanium, vanadium, boron, tungsten, chromium and yttrium are adopted, the national standard solution with the concentration of 1000 mu g/mL and the national standard solution with the concentration of 500 mu g/mL of tin are adopted to be diluted into the mixed working standard solution according to the detection range of the sample. And (3) diluting the obtained product into an internal standard solution by using a national standard rhodium (or indium or cesium) solution with the concentration of 1000 mu g/mL.
And sequentially measuring the working standard solution, the blank solution and the sample solution on an inductively coupled plasma mass spectrometer, continuously introducing an internal standard solution during measurement, and measuring the content of each element to be measured by using a standard curve method, wherein the unit is nanogram per milliliter (ng/mL).
Precision and recovery after using the method
Under the analysis conditions determined by the method, 6 samples are parallelly measured, and the content of 18 impurity elements is measured. And (3) placing the impurity element standard solution in a beaker, adding 0.1g of sample, performing precision and addition recovery test of the method according to the operation steps determined by the method, adding the recovery test to the lower limit of 5 times of impurity detection, and parallelly measuring 6 data, wherein the results are shown in table 2.
TABLE 2 precision and recovery Experimental results
| Element(s) | Al | Ca | B | Cd | Fe | Mg | Mn | Sn | Ti |
| Background of the invention | 11.4 | 0.0 | 3.4 | 0.1 | 82.4 | 40.2 | 4.3 | 0.4 | 35.9 |
| Adding quantity of scalar | 25 | 5 | 5 | 1 | 50 | 50 | 25 | 5 | 25 |
| Determination of the mean value | 36.1 | 4.7 | 8.2 | 1.1 | 135.7 | 92.2 | 29.0 | 5.4 | 62.0 |
| RSD％ | 1.4 | 2.1 | 0.9 | 4.1 | 3.2 | 1.9 | 6.2 | 5.2 | 2.9 |
| Recovery rate | 98.9 | 94.3 | 96.7 | 96.0 | 106.5 | 104.0 | 98.8 | 100.4 | 104.5 |
| Element(s) | V | Cr | Cu | Ni | Pb | W | Co | Mo | Y |
| Background of the invention | 29.1 | 1.3 | 3.8 | 1.0 | 1.7 | 0.3 | 0.1 | 0.2 | 2.6 |
| Adding quantity of scalar | 25 | 25 | 25 | 25 | 5 | 5 | 5 | 5 | 25 |
| Determination of the mean value | 52.3 | 25.3 | 27.6 | 25.8 | 6.6 | 5.3 | 5.2 | 5.3 | 27 |
| RSD％ | 2.9 | 2.7 | 4.2 | 2.9 | 4.6 | 3.5 | 3.3 | 2.6 | 4.3 |
| Recovery rate | 93.1 | 95.9 | 95.1 | 99.4 | 98.6 | 101.1 | 102.2 | 101.9 | 98.3 |
The precision of the method is better than 10 percent, and the average recovery rate is between 90 and 110 percent.
In the disclosed embodiments of the present invention, only methods related to the disclosed embodiments are referred to, and other methods may refer to general designs, and under the condition of no conflict, the same embodiment and different embodiments of the present invention may be combined with each other;
the above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that are within the spirit and principle of the present invention are intended to be included in the scope of the present invention.
Claims (8)
1. A method for measuring the content of impurity elements such as aluminum, magnesium and the like in a silicon carbide composite material comprises the steps of firstly, sample treatment, secondly, determining the analysis mass number, and thirdly, measuring; the method is characterized in that:
step one, sample processing;
the content of manganese, nickel, cobalt, chromium, tungsten, calcium, titanium and yttrium is 5-2000 mu g/g; the content of boron, vanadium, copper, tin and lead is 1-400 mu g/g; the cadmium content is 0.1-40 mu g/g; the content of aluminum, iron and magnesium is 10-4000 mu g/g; detecting a silicon carbide sample with the molybdenum content of 0.5-200 mug/g;
the powder sample is directly used for analysis; crushing the samples in other states, and then analyzing the crushed samples by using powder;
taking a powdery sample, accurately measuring the powdery sample to 0.1mg, placing the sample in a quartz beaker, adding 5 times of high-grade pure nitric acid by volume, placing the sample in an ultrasonic cleaner, and ultrasonically leaching the sample for 30min at 100% power;
after the ultrasonic treatment is stopped, taking out the beaker and cooling to room temperature;
then filtering on a funnel by using medium-speed qualitative filter paper, washing the beaker for 3 times by using water, and washing filter residues for 3 times;
the filtrate is received into a volumetric flask, diluted to a scale by water and used as a sample solution for measuring 18 elements of aluminum, magnesium, iron, calcium, cadmium, cobalt, copper, lead, manganese, molybdenum, nickel, titanium, vanadium, boron, tungsten, chromium, tin and yttrium;
carrying out a blank experiment along with the sample, and using the blank experiment as a blank solution to be tested;
step two, determining the analysis mass number;
selecting a detection method of a silicon carbide sample on an inductively coupled plasma mass spectrometer, and determining the analysis mass number of 18 elements of aluminum, magnesium, iron, calcium, cadmium, cobalt, copper, lead, manganese, molybdenum, nickel, titanium, vanadium, boron, tungsten, chromium, tin and yttrium;
finally determining the analysis mass number of each element to be detected as boron-11, tin-118, nickel-60, aluminum-27, titanium-47, lead-208, calcium-44, vanadium-51, tungsten-186, cadmium-111, magnesium-24, cobalt-59, iron-57, chromium-52, molybdenum-98, manganese-55, copper-63 and yttrium-89;
step three, determination;
diluting 17 elements of national standard solution of aluminum, magnesium, iron, calcium, cadmium, cobalt, copper, lead, manganese, molybdenum, nickel, titanium, vanadium, boron, tungsten, chromium and yttrium and 17 elements of tin into mixed working standard solution according to the detection range of a sample; diluting rhodium national standard solution with the concentration of 1000 mug/mL into internal standard solution;
and sequentially measuring the working standard solution, the blank solution and the sample solution on an inductively coupled plasma mass spectrometer, continuously introducing an internal standard solution during measurement, and measuring the content of each element to be measured by using a standard curve method, wherein the unit is nanogram per milliliter (ng/mL).
2. The method for determining the content of the impurity elements such as aluminum and magnesium in the silicon carbide composite material according to claim 1, wherein the method comprises the following steps: in the first step, the sample is sieved by a sieve of 60 meshes to 100 meshes.
3. The method for determining the content of the impurity elements such as aluminum and magnesium in the silicon carbide composite material according to claim 1, wherein the method comprises the following steps: in the second step, in the mass number analysis, the mass number is determined by selecting isotopes which have large abundance and high sensitivity and can be free of interference or subjected to interference elimination and correction; and selecting and comparing the mass number of each element to be detected, and comparing the mass number with a detection limit according to the interference factors of the coexisting elements.
4. The method for determining the content of the impurity elements such as aluminum and magnesium in the silicon carbide composite material according to claim 1, wherein the method comprises the following steps: in the second step, the selected mass numbers require that the linear correlation coefficients are all greater than 0.999.
5. The method for determining the content of the impurity elements such as aluminum and magnesium in the silicon carbide composite material according to claim 1, wherein the method comprises the following steps: in the third step, indium national standard solution with the concentration of 1000 mug/mL is adopted to be diluted into internal standard solution.
6. The method for determining the content of the impurity elements such as aluminum and magnesium in the silicon carbide composite material according to claim 1, wherein the method comprises the following steps: and in the third step, cesium national standard solution with the concentration of 1000 mug/mL is adopted to be diluted into internal standard solution.
7. The method for determining the content of the impurity elements such as aluminum and magnesium in the silicon carbide composite material according to claim 1, wherein the method comprises the following steps: the concentration of the national standard solution of the 17 elements in the third step is 1000 mug/mL.
8. The method for determining the content of the impurity elements such as aluminum and magnesium in the silicon carbide composite material according to claim 1, wherein the method comprises the following steps: the concentration of the national standard solution of tin in the third step is 500 mug/mL.
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