CN111257097A - Vanadium carbide sample to be tested manufacturing method and impurity content analysis method thereof - Google Patents
Vanadium carbide sample to be tested manufacturing method and impurity content analysis method thereof Download PDFInfo
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- CN111257097A CN111257097A CN202010067058.3A CN202010067058A CN111257097A CN 111257097 A CN111257097 A CN 111257097A CN 202010067058 A CN202010067058 A CN 202010067058A CN 111257097 A CN111257097 A CN 111257097A
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- 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
- G01N1/38—Diluting, dispersing or mixing samples
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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
Abstract
The invention relates to a method for manufacturing a vanadium carbide sample to be tested and an analysis method of impurity content of the vanadium carbide sample to be tested, and belongs to the technical field of analytical chemistry. The method for manufacturing the vanadium carbide sample to be tested comprises the following steps: a. mixing vanadium carbide and aqua regia, decomposing at 80-90 ℃, filtering to obtain filter residue and filtrate, washing the filter residue to obtain washing liquid and filter residue A, and combining the filtrate and the washing liquid to obtain solution A; b. ashing the filter residue A at 900-950 ℃, adding a mixed flux, preserving the temperature for 15min at 950-1000 ℃, and cooling to obtain a filter residue B; c. mixing the filter residue B with a hydrochloric acid aqueous solution, and completely dissolving at 70-80 ℃ to obtain a solution B; d. and combining the solution A and the solution B to obtain a sample to be detected. According to the method for manufacturing the vanadium carbide sample to be tested, the solid sample is processed into liquid, the loss amount of elements to be tested is less, and the contents of iron, phosphorus and titanium in vanadium carbide can be rapidly and accurately determined.
Description
Technical Field
The invention relates to a method for manufacturing a vanadium carbide sample to be tested and an analysis method of impurity content of the vanadium carbide sample to be tested, and belongs to the technical field of analytical chemistry.
Background
Vanadium carbide is often used as an important alloy additive due to its excellent properties, and is widely applied in the field of hard alloys, such as smelting high-strength low alloy steel and the like, and the addition of vanadium carbide can improve the comprehensive mechanical properties of steel, such as wear resistance, toughness and the like. However, the existence of impurity elements in vanadium carbide affects the performance of the hard alloy, and further affects the quality of the hard alloy product. Therefore, it is very important to detect and analyze impurity elements such as iron, phosphorus, titanium and the like in vanadium carbide as a hard alloy additive.
The existing standards GB/T20255.2-2006, GB/T20255.3-2006 and GB/T20255.4-2006 disclose chemical analysis methods of hard alloy iron and titanium, namely flame atomic absorption spectrometry, but the methods additionally need cesium chloride and ammonium chloride reagents, additional analysis errors are brought, and the analysis precision is influenced.
The currently disclosed method for analyzing iron in vanadium carbide mainly comprises the following steps: method 1: in patent application No. 2019108599517, hydrofluoric acid and nitric acid are used to react with vanadium carbide, and inductively coupled plasma emission spectrometry is used to rapidly determine trace amounts of iron, aluminum, silicon, and calcium in vanadium carbide. The 2 nd method: the application No. 2012104377192 discloses a method for analyzing and detecting iron element in vanadium carbide, which comprises dissolving a sample in nitric acid aqueous solution under heating, removing the obtained insoluble free carbon by filtration, and measuring the content of iron by atomic absorption spectrometry. The vanadium carbide contains free carbon, the content of the free carbon is high, about 0.24%, the free carbon can adsorb certain impurity elements such as iron, and if the samples are decomposed according to the two methods, insoluble free carbon in the vanadium carbide is removed without being digested, so that the measurement result is low, and the measurement precision is influenced.
Disclosure of Invention
The first technical problem to be solved by the invention is to provide a method for manufacturing a vanadium carbide sample to be tested, and the loss amount of elements to be tested in the prepared solution sample is less.
In order to solve the first technical problem of the present invention, the method for manufacturing the vanadium carbide sample to be tested includes:
a. mixing vanadium carbide and aqua regia, decomposing at 80-90 ℃, filtering to obtain filter residue and filtrate, washing the filter residue to obtain washing liquid and filter residue A, and combining the filtrate and the washing liquid to obtain solution A;
b. ashing the filter residue A at 900-950 ℃, adding a mixed flux, preserving the heat at 950-1000 ℃ for 15-20 min, and cooling to obtain a filter residue B, wherein the mixed flux is a mixture of sodium carbonate and boric acid;
c. mixing the filter residue B with a hydrochloric acid aqueous solution, and completely dissolving at 70-80 ℃ to obtain a solution B;
d. and combining the solution A and the solution B to obtain a sample to be detected.
Step a is operated in a container, and if residues exist on the wall of the container in the operation process, the residues are washed off by water and filtered together in order to reduce errors.
Preferably, the ratio of the vanadium carbide to the aqua regia is 0.5g: 20-30 mL.
Preferably, the mass ratio of the vanadium carbide to the flux is 0.5: 0.3-0.4, and the flux is preferably a mixture of sodium carbonate and boric acid according to the mass ratio of 2-2.1: 1.
Preferably, the ratio of the vanadium carbide to the hydrochloric acid aqueous solution is 0.5g: 20-25 mL; the aqueous hydrochloric acid solution is preferably: the hydrochloric acid and the water are mixed according to the volume ratio of 1: 5-10.
Preferably, the filter paper is adopted for filtration, and after filtration, the filter paper and the filter residue A are subjected to ashing treatment; preferably, the filter paper is a slow-speed quantitative filter paper.
The second technical problem to be solved by the invention is to provide a method for determining the content of impurity elements such as iron, phosphorus and titanium in vanadium carbide.
In order to solve the second technical problem, the method comprises the step of processing vanadium carbide by using the method for preparing the vanadium carbide sample to be tested to obtain a solution to be tested.
Preferably, the method further comprises:
a. fixing the volume of the solution to be detected;
b. preparing a standard substance of impurity elements of iron, phosphorus and titanium;
c. measuring the element spectral line intensity of a standard substance of impurity elements of iron, phosphorus and titanium by using an inductively coupled plasma emission spectrometer, and drawing a standard working curve; and measuring the element spectral line intensity of the solution to be measured after constant volume by using an inductively coupled plasma emission spectrometer, obtaining the concentrations of the impurity elements of iron, phosphorus and titanium in the solution to be measured according to the standard working curve, and calculating according to a formula to obtain the content of the impurity elements of iron, phosphorus and titanium in the vanadium carbide.
And introducing the solution to be measured into an inductively coupled plasma emission spectrometer, measuring the spectral line intensity of the element to be measured, obtaining the mass concentration of iron, phosphorus and titanium in the solution to be measured according to the spectral line intensity measured by the standard solution with known concentration, and calculating the content of iron, phosphorus and titanium in the vanadium carbide sample according to the following formula (1).
In the formula:
x represents the element to be detected (iron, phosphorus and titanium);
ρ represents the mass concentration of the element to be detected in the sample solution measured by the instrument, (μ g/mL );
v represents the volume of the test sample solution, (mL, mL);
m represents the mass of the sample, (g, g).
Preferably, the preparation method of the standard substance of impurity elements of iron, phosphorus and titanium in the step b comprises the following steps:
transferring and mixing the iron standard solution, the phosphorus standard solution and the titanium standard solution, and performing constant volume to obtain a mixed standard solution mother solution; mixing the mixed standard solution mother liquor with the vanadium matrix solution, and performing constant volume to obtain a mixed standard solution;
preferably, the concentrations of iron, phosphorus and titanium in the mother liquor of the mixed standard solution are respectively 100 mug/mL, 15 mug/mL and 40 mug/mL; the concentration of the vanadium matrix solution is 20.23 g/L.
Preferably, the method comprises the steps of mixing the mixed standard solution mother liquor with a vanadium matrix solution and aqua regia; the volume ratio of the aqua regia to the vanadium matrix solution is 12-18: 10.
Preferably, the preparation method of the standard substance of impurity elements of iron, phosphorus and titanium in the step b comprises the following steps:
respectively taking 0, 2.00mL, 4.00mL, 6.00mL, 8.00mL and 10.00mL of mixed standard solution mother liquor with iron, phosphorus and titanium concentrations of 100 mu g/mL, 15 mu g/mL and 40 mu g/mL, respectively, putting 10mL and 12mL of vanadium matrix solution with mass concentration of 20.23g/L into 6 100mL volumetric flasks, and adding 12mL of aqua regia; diluting with water to scale and shaking to obtain mixed standard solution.
Has the advantages that:
1. according to the method for manufacturing the vanadium carbide sample to be detected, the solid sample is processed into liquid, the sample is dissolved by aqua regia, the filtered residue is processed by the mixed solvent of sodium carbonate and boric acid and then extracted by hydrochloric acid, and the two solutions are combined.
2. By utilizing the technical scheme of the invention, the contents of iron, phosphorus and titanium in vanadium carbide can be rapidly and accurately measured; and the element content can be accurately measured when being lower.
3. The environment is protected; the invention only needs a small amount of hydrochloric acid, nitric acid and mixed flux, and has less reagent consumption and environmental protection.
Detailed Description
In order to solve the first technical problem of the present invention, the method for manufacturing the vanadium carbide sample to be tested includes:
a. mixing vanadium carbide and aqua regia, decomposing at 80-90 ℃, filtering to obtain filter residue and filtrate, washing the filter residue to obtain washing liquid and filter residue A, and combining the filtrate and the washing liquid to obtain solution A;
b. ashing the filter residue A at 900-950 ℃, adding a mixed flux, preserving the heat at 950-1000 ℃ for 15-20 min, and cooling to obtain a filter residue B, wherein the mixed flux is a mixture of sodium carbonate and boric acid;
c. mixing the filter residue B with a hydrochloric acid aqueous solution, and completely dissolving at 70-80 ℃ to obtain a solution B;
d. and combining the solution A and the solution B to obtain a sample to be detected.
Step a is operated in a container, and if residues exist on the wall of the container in the operation process, the residues are washed off by water and filtered together in order to reduce errors.
Preferably, the ratio of the vanadium carbide to the aqua regia is 0.5g: 20-30 mL.
Preferably, the mass ratio of the vanadium carbide to the flux is 0.5: 0.3-0.4, and the flux is preferably a mixture of sodium carbonate and boric acid according to the mass ratio of 2-2.1: 1.
Preferably, the ratio of the vanadium carbide to the hydrochloric acid aqueous solution is 0.5g: 20-25 mL; the aqueous hydrochloric acid solution is preferably: the hydrochloric acid and the water are mixed according to the volume ratio of 1: 5-10.
Preferably, the filter paper is adopted for filtration, and after filtration, the filter paper and the filter residue A are subjected to ashing treatment; preferably, the filter paper is a slow-speed quantitative filter paper.
In order to solve the second technical problem, the method comprises the step of processing vanadium carbide by using the method for preparing the vanadium carbide sample to be tested to obtain a solution to be tested.
Preferably, the method further comprises:
a. fixing the volume of the solution to be detected;
b. preparing a standard substance of impurity elements of iron, phosphorus and titanium;
c. measuring the element spectral line intensity of a standard substance of impurity elements of iron, phosphorus and titanium by using an inductively coupled plasma emission spectrometer, and drawing a standard working curve; and measuring the element spectral line intensity of the solution to be measured after constant volume by using an inductively coupled plasma emission spectrometer, obtaining the concentrations of the impurity elements of iron, phosphorus and titanium in the solution to be measured according to the standard working curve, and calculating according to a formula to obtain the content of the impurity elements of iron, phosphorus and titanium in the vanadium carbide.
And introducing the solution to be measured into an inductively coupled plasma emission spectrometer, measuring the spectral line intensity of the element to be measured, obtaining the mass concentration of iron, phosphorus and titanium in the solution to be measured according to the spectral line intensity measured by the standard solution with known concentration, and calculating the content of iron, phosphorus and titanium in the vanadium carbide sample according to the following formula (1).
In the formula:
x represents the element to be detected (iron, phosphorus and titanium);
ρ represents the mass concentration of the element to be detected in the sample solution measured by the instrument, (μ g/mL );
v represents the volume of the test sample solution, (mL, mL);
m represents the mass of the sample, (g, g).
Preferably, the preparation method of the standard substance of impurity elements of iron, phosphorus and titanium in the step b comprises the following steps:
transferring and mixing the iron standard solution, the phosphorus standard solution and the titanium standard solution, and performing constant volume to obtain a mixed standard solution mother solution; mixing the mixed standard solution mother liquor with the vanadium matrix solution, and performing constant volume to obtain a mixed standard solution;
preferably, the concentrations of iron, phosphorus and titanium in the mother liquor of the mixed standard solution are respectively 100 mug/mL, 15 mug/mL and 40 mug/mL; the concentration of the vanadium matrix solution is 20.23 g/L.
Preferably, the method comprises the steps of mixing the mixed standard solution mother liquor with a vanadium matrix solution and aqua regia; the volume ratio of the aqua regia to the vanadium matrix solution is 12-18: 10.
Preferably, the preparation method of the standard substance of impurity elements of iron, phosphorus and titanium in the step b comprises the following steps:
respectively taking 0, 2.00mL, 4.00mL, 6.00mL, 8.00mL and 10.00mL of mixed standard solution mother liquor with iron, phosphorus and titanium concentrations of 100 mu g/mL, 15 mu g/mL and 40 mu g/mL, respectively, putting 10mL and 12mL of vanadium matrix solution with mass concentration of 20.23g/L into 6 100mL volumetric flasks, and adding 12mL of aqua regia; diluting with water to scale and shaking to obtain mixed standard solution.
The following examples are provided to further illustrate the embodiments of the present invention and are not intended to limit the scope of the present invention.
Example 1
Reagent:
hydrochloric acid: the density is 1.19 g/mL;
aqua regia solution: the volume ratio of the hydrochloric acid to the nitric acid is 3: 1;
hydrochloric acid aqueous solution: hydrochloric acid: the water volume ratio is 1: 10;
mixing a fusing agent: sodium carbonate: the mass ratio of boric acid is 2: 1.
1. preparing an atomized solution of a vanadium carbide sample: weighing a vanadium carbide sample with the mass of 0.5000g, placing the sample in a 250mL conical flask, washing the inner wall of the conical flask with about 10mL of water, adding 20mL of aqua regia to perform low-temperature digestion at 80 ℃ on an electric heating plate, and washing the inner wall of the conical flask with water at proper time in the process of heating and decomposing the sample. Taking down the flask after the reaction is stopped, washing the inner wall of the flask with a small amount of water, filtering the flask with slow quantitative filter paper while the flask is hot, washing the filter residue with hot water for 5 times, and collecting the obtained filtrate in a 200mL volumetric flask. Putting the filter paper and the residues into a platinum crucible, putting the platinum crucible into a muffle furnace for ashing treatment at 950 ℃, adding 0.3g of mixed flux, and preserving the heat for 15min at 950 ℃ in the muffle furnace. After cooling, the platinum crucible was taken out and washed with water to clean the outer surface of the crucible, and the crucible was placed in a 200mL beaker, to which hydrochloric acid and water were added in a volume ratio of 1: and (3) after 10mL of mixed hydrochloric acid aqueous solution is mixed, heating at the low temperature of 75 ℃ until the mixed hydrochloric acid aqueous solution is completely dissolved, taking down the mixed hydrochloric acid aqueous solution for slight cooling, combining the cooled mixed hydrochloric acid aqueous solution with the previously collected filtrate, and finally metering the volume to a 200mL volumetric flask and shaking up the volumetric flask to obtain the atomized solution of the vanadium carbide sample.
2. Preparing a vanadium standard solution: 3.6120g of pure vanadium pentoxide with a purity of 99.99% was weighed into a 250mL conical flask, the flask was rinsed with about 10mL of water to wet the inner wall of the flask, hydrochloric acid was added: the volume ratio of the nitric acid is 3: 1 of aqua regia 20mL is heated on an electric hot plate at the low temperature of 80 ℃ until the aqua regia is completely dissolved, taken down and cooled, the inner wall of the bottle is flushed by water, the solution is transferred to a 100mL volumetric flask, diluted to the scale by water and shaken up to prepare a vanadium matrix solution of 20.23 mg/mL.
3. Preparation of standard solution: the standard solutions of iron, phosphorus and titanium used in this example were prepared by the institute of iron and steel, and the mass concentrations were all 1000. mu.g/mL. Preparing mixed standard solutions of iron, phosphorus and titanium with the mass concentrations of 100 mu g/mL, 15 mu g/mL and 40 mu g/mL respectively: 10mL of the iron standard solution, 1.5mL of the phosphorus standard solution and 4mL of the titanium standard solution which are prepared by a steel research institute are respectively transferred and placed in a 100mL volumetric flask, diluted to the scale with deionized water, mixed uniformly and stored in the volumetric flask.
Preparing a mixed standard solution series matched with a vanadium matrix: respectively transferring the prepared mixed standard solutions of iron, phosphorus and titanium with the mass concentrations of 100 mu g/mL, 15 mu g/mL and 40 mu g/mL into a group of (6) 100mL volumetric flasks, adding 10mL of the vanadium matrix solution with the mass concentration of 20.23mg/mL, and then supplementing 9mL of high-grade pure hydrochloric acid and 3mL of high-grade pure nitric acid, wherein the mixed standard solutions of iron, phosphorus and titanium with the mass concentrations of 100 mu g/mL, 2.00mL, 4.00mL, 6.00mL, 8.00mL and 10.00 mL. The mixture was diluted to the mark with water and shaken up to prepare a mixed standard solution series as shown in Table 1.
TABLE 1 Mass concentrations of iron, phosphorus and titanium in the Mixed Standard solution
| Numbering | Iron content μ g/mL | Phosphorus content μ g/mL | Titanium content μ g/mL |
| 0 | 0 | 0 | 0 |
| 1 | 2 | 0.3 | 0.8 |
| 2 | 4 | 0.6 | 1.6 |
| 3 | 6 | 0.9 | 2.4 |
| 4 | 8 | 1.2 | 3.2 |
| 5 | 10 | 1.5 | 4.0 |
4. Drawing a standard working curve:
when the method is adopted to measure the iron, phosphorus and titanium elements in the mixed standard solution series of iron, phosphorus and titanium matched with the vanadium matrix on an iCAP6300 type inductively coupled plasma full-spectrum direct-reading spectrometer, the working conditions of the instrument are as follows: the RF generator power is 1250W; the flow of the auxiliary gas Ar is 1.0L/min; the flow rate of the atomized gas is 0.75L/min; the pressure of the atomizer is 0.22 MPa; the pump speed is 50 r/min; the washing time of the sample inlet pipe is 30 s; the height was observed to be 12 mm.
The wavelength of the analysis spectral line of the element to be measured is as follows: iron 238.204nm, phosphorus 213.618nm and titanium 334.941 nm.
And respectively introducing the prepared mixed standard solution series of the vanadium-containing matrix into an ICP emission spectrometer, measuring the intensity of emitted light, and drawing a working curve.
5. Determination of vanadium carbide samples: and (3) according to the working conditions of the instrument in the step 4, simultaneously measuring the mass concentrations of iron, phosphorus and titanium elements of the blank vanadium carbide atomized solution and the iron, phosphorus and titanium mixed standard solution series matched with the vanadium matrix on an inductively coupled plasma emission spectrometer, and calculating an analysis result according to a formula (1). Eight times of measurement are carried out on the same batch of vanadium carbide samples, the same batch of vanadium carbide samples are weighed, a certain amount of mixed standard solution of iron, phosphorus and titanium is respectively added, a standard addition recovery experiment is carried out, and the average value, the standard deviation and the relative standard deviation of the measurement results are calculated and shown in table 2.
TABLE 2 analytical results and precision
| Element(s) | Average value of measurement results | Standard deviation% | Relative standard deviation% | The recovery rate is high |
| Iron | 0.113 | 0.000641 | 0.57 | 96.8 |
| Phosphorus (P) | 0.0161 | 0.000131 | 0.81 | 98.3 |
| Titanium (IV) | 0.0381 | 0.000169 | 0.44 | 99.8 |
According to the method for analyzing and detecting the impurity elements of iron, phosphorus and titanium in the vanadium carbide, the sample is subjected to a standard addition recovery experiment, and the recovery rates are all 96.8-99.8%; the relative standard deviation of the method is less than 0.9 percent when the sample is independently measured for eight times, which shows that the method has good accuracy and precision, namely, the method is accurate and feasible for rapidly and accurately measuring the contents of iron, phosphorus and titanium in the vanadium carbide by utilizing an inductively coupled plasma emission spectrometry.
Claims (10)
1. The method for manufacturing the vanadium carbide sample to be tested is characterized by comprising the following steps:
a. mixing vanadium carbide and aqua regia, decomposing at 80-90 ℃, filtering to obtain filter residue and filtrate, washing the filter residue to obtain washing liquid and filter residue A, and combining the filtrate and the washing liquid to obtain solution A;
b. ashing the filter residue A at 900-950 ℃, adding a mixed flux, preserving the heat at 950-1000 ℃ for 15-20 min, and cooling to obtain a filter residue B, wherein the mixed flux is a mixture of sodium carbonate and boric acid;
c. mixing the filter residue B with a hydrochloric acid aqueous solution, and completely dissolving at 70-80 ℃ to obtain a solution B;
d. and combining the solution A and the solution B to obtain a sample to be detected.
2. The method for preparing the vanadium carbide sample to be tested according to claim 1, wherein the ratio of the vanadium carbide to the aqua regia is 0.5g: 20-30 mL.
3. The method for manufacturing the vanadium carbide sample to be tested according to claim 1 or 2, wherein the mass ratio of the vanadium carbide to the mixed flux is 0.5: 0.3-0.4, and the flux is preferably a mixture of sodium carbonate and boric acid in a mass ratio of 2-2.1: 1.
4. The method for manufacturing the vanadium carbide sample to be tested according to any one of claims 1 to 3, wherein the ratio of the vanadium carbide to the hydrochloric acid aqueous solution is 0.5g:20 to 25 mL; the aqueous hydrochloric acid solution is preferably: the hydrochloric acid and the water are mixed according to the volume ratio of 1: 5-10.
5. The method for manufacturing the vanadium carbide sample to be tested according to any one of claims 1 to 4, wherein filter paper is adopted for the filtration, and the filter paper and the filter residue A are subjected to ashing treatment after the filtration; preferably, the filter paper is a slow-speed quantitative filter paper.
6. The method for measuring the content of the impurity elements such as iron, phosphorus and titanium in vanadium carbide is characterized by comprising the step of processing the vanadium carbide by using the method for manufacturing the vanadium carbide sample to be measured according to any one of claims 1 to 5 to obtain a solution to be measured.
7. The method for determining the impurity element content of iron, phosphorus and titanium in vanadium carbide according to claim 6, further comprising:
a. fixing the volume of the solution to be detected;
b. preparing a standard substance of impurity elements of iron, phosphorus and titanium;
c. measuring the element spectral line intensity of a standard substance of impurity elements of iron, phosphorus and titanium by using an inductively coupled plasma emission spectrometer, and drawing a standard working curve; and measuring the element spectral line intensity of the solution to be measured after constant volume by using an inductively coupled plasma emission spectrometer, obtaining the concentrations of the impurity elements of iron, phosphorus and titanium in the solution to be measured according to the standard working curve, and calculating according to a formula to obtain the content of the impurity elements of iron, phosphorus and titanium in the vanadium carbide.
8. The method for determining the content of impurity elements such as iron, phosphorus and titanium in vanadium carbide according to claim 7, wherein the preparation method of the standard product of impurity elements such as iron, phosphorus and titanium in step b comprises the following steps:
transferring and mixing the iron standard solution, the phosphorus standard solution and the titanium standard solution, and performing constant volume to obtain a mixed standard solution mother solution; mixing the mixed standard solution mother liquor with the vanadium matrix solution, and performing constant volume to obtain a mixed standard solution;
preferably, the concentrations of iron, phosphorus and titanium in the mother liquor of the mixed standard solution are respectively 100 mug/mL, 15 mug/mL and 40 mug/mL; the concentration of the vanadium matrix solution is 20.23 g/L.
9. The method for detecting impurity element contents of iron, phosphorus and titanium in vanadium carbide according to claim 8, characterized by comprising the steps of mixing a mixed standard solution mother solution with a vanadium matrix solution and aqua regia; the volume ratio of the aqua regia to the vanadium matrix solution is 12-18: 10.
10. The method for determining the content of impurity elements such as iron, phosphorus and titanium in vanadium carbide according to claim 8 or 9, wherein the method for preparing the standard of impurity elements such as iron, phosphorus and titanium in step b comprises:
respectively taking 0, 2.00mL, 4.00mL, 6.00mL, 8.00mL and 10.00mL of mixed standard solution mother liquor with iron, phosphorus and titanium concentrations of 100 mu g/mL, 15 mu g/mL and 40 mu g/mL, respectively, putting 10mL and 12mL of vanadium matrix solution with mass concentration of 20.23g/L into 6 100mL volumetric flasks, and adding 12mL of aqua regia; diluting with water to scale and shaking to obtain mixed standard solution.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112051230A (en) * | 2020-09-17 | 2020-12-08 | 攀枝花学院 | Analytical method for determining content of phosphorus in vanadium carbide by spectrophotometry |
| CN113624696A (en) * | 2021-07-02 | 2021-11-09 | 国家能源集团宁夏煤业有限责任公司 | Method for detecting iron content in Fischer-Tropsch synthetic wax |
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