CN117092090A - A method for determining the zirconia content in dispersion-strengthened platinum-based materials - Google Patents
A method for determining the zirconia content in dispersion-strengthened platinum-based materials Download PDFInfo
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Abstract
本发明涉及一种弥散强化铂基材料中氧化锆含量的测定方法，所述方法通过锆与氧化锆的溶解性能的差异，用盐酸和硝酸混合酸溶解制备固溶锆测试液，用于反应溶解材料中的锆；用盐酸和硝酸混合加氢氟酸酸溶解制备总锆测试液，用于溶解材料中包含的锆和氧化锆，即总锆。在电感耦合等离子体原子发射光谱仪上，于所推荐的波长处测量试液中锆元素的发射光谱强度，由校准曲线计算总锆和固溶锆的质量分数，通过总锆的质量分数减去固溶锆的质量分数，计算出弥散强化铂基材料中氧化锆的含量，本发明所述方法样品损耗少、简单快速、结果更加精确、可靠。
The invention relates to a method for measuring the content of zirconium oxide in dispersion-strengthened platinum-based materials. The method uses a mixed acid solution of hydrochloric acid and nitric acid to prepare a solid-soluble zirconium test solution based on the difference in the solubility properties of zirconium and zirconium oxide, which is used for reaction and dissolution. Zirconium in the material; use hydrochloric acid and nitric acid mixed with hydrofluoric acid to dissolve to prepare a total zirconium test solution, which is used to dissolve the zirconium and zirconium oxide contained in the material, that is, total zirconium. On an inductively coupled plasma atomic emission spectrometer, measure the emission spectrum intensity of the zirconium element in the test solution at the recommended wavelength. Calculate the mass fraction of total zirconium and solid solution zirconium from the calibration curve. Subtract the mass fraction of solid zirconium from the mass fraction of total zirconium. The mass fraction of dissolved zirconium is used to calculate the zirconium oxide content in the dispersion-strengthened platinum-based material. The method of the present invention has less sample loss, is simple and fast, and has more accurate and reliable results.
Description
Technical Field
The invention relates to a method for measuring substances in a material, in particular to a method for measuring the content of zirconia in a dispersion strengthening platinum-based material.
Background
The dispersion strengthened platinum material has higher high-temperature strength, creep resistance and corrosion resistance than unreinforced platinum, and is a key material for manufacturing crucibles and glass fiber bushing plates for glass industry. How to introduce and add dispersion strengthening particles into a matrix metal material is a key for preparing a dispersion strengthening platinum material, and the introduction method or mode has great influence on the high-temperature performance of the dispersion strengthening platinum material.
The zirconia dispersion strengthening platinum material takes a trace amount of zirconia as a stable second phase, is uniformly distributed in a platinum matrix, and plays roles in preventing grain boundary sliding and improving the strength and high-temperature creep resistance of platinum. The material is produced and prepared by adopting metallic zirconium, and then is converted into zirconia. Therefore, the oxidation efficiency of the reinforced zirconium metal determines the content of zirconium oxide in the material, the production energy consumption, the stability and the like.
At present, many studies have been made on a method for producing a zirconia dispersion-strengthened platinum material, tissue properties, and the like. The Xie Zi article of the invention is specially used for researching the influence of different zirconia contents on the room-temperature physical, mechanical and high-temperature durable fracture life of the dispersion strengthening platinum. Xu Wenge it is also pointed out that the strength and processability of the dispersion-strengthened platinum can be both achieved when the zirconia content is about 0.3%. Therefore, the content of the zirconia in the zirconia dispersion strengthening platinum-based material can be accurately measured, the production process can be guided, the product performance can be clarified, and the yield can be improved.
However, in the prior art, the method for testing the content of zirconia in the material is to utilize the solubility difference of zirconium metal and zirconium oxide in the metal alloy material, weigh the zirconium oxide after precipitation crystallization, calculate the content of zirconium oxide in the dispersion strengthening platinum-based material, and further determine the strength and processing performance of the zirconium oxide, but the method cannot avoid the situation of process loss in the weighing process of zirconium oxide, thereby causing the measurement of the content of zirconium oxide to be inaccurate.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a method for measuring the content of zirconium oxide in a dispersion-strengthened platinum-based material, which solves the problem of inaccurate measurement of the content of zirconium oxide in the dispersion-strengthened platinum-based material in the prior art.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
the method for measuring the zirconia content in the dispersion strengthening platinum-based material comprises the following steps:
1) Taking two samples of dispersion strengthening platinum-based material, and setting the mass of sample 1 as m 1 And sample 2 has a mass of m 2 Standby;
2) Preparing a test solution:
preparing a total zirconium test solution and a total zirconium sample blank test solution; solid solution zirconium test solution and solid solution zirconium sample blank test solution;
3) Drawing a calibration curve:
selecting a standard solution with the zirconium element content of 1000 mug/mL, and preparing the standard solution with the zirconium concentration of 100 mug/mL; 0.00mL, 0.50mL, 1.00mL, 2.00mL, 3.00mL, 4.00mL, 5.00mL and 10.00mL of mixed acid of hydrochloric acid and nitric acid and hydrofluoric acid are respectively taken, wherein the mixed acid is as follows: the volume ratio of hydrofluoric acid is 10-5: 1, water is used for constant volume to 100mL, and shaking is carried out uniformly to prepare a series of calibration solutions;
testing the intensity of the zirconium element in the series of calibration solutions at the wavelength 343.8nm or 339.1nm of the spectrometer, and drawing a calibration curve by taking the intensity of the zirconium element as an ordinate and the mass concentration as an abscissa;
4) And (3) calculating the mass concentration of zirconium element in the test solution:
testing the emission intensity of the zirconium element in the total zirconium test solution, the total zirconium sample blank test solution, the solid solution zirconium test solution and the solid solution zirconium sample blank test solution at the wavelength 343.8nm or 339.1nm of the spectrometer, and calculating the mass concentration of the zirconium element in the total zirconium test solution, the total zirconium sample blank test solution, the solid solution zirconium test solution and the solid solution zirconium sample blank test solution by using the following formulas according to the calibration curve drawn by the standard solution in the step 3):
wherein:
omega-zirconia mass fraction in units of;
ρ 1 the mass concentration of zirconium element in the total zirconium sample test solution is expressed in mug/mL;
the mass concentration of zirconium element in the blank solution of the total zirconium sample is expressed in mug/mL;
m 1 -testing the mass of the total zirconium sample in g;
V 1 sample total zirconium test liquid volume in mL;
ρ 2 the mass concentration of zirconium element in the sample solid solution zirconium test solution is expressed in mug/mL;
the mass concentration of zirconium element in a blank solution of a solid solution zirconium sample is presented in the unit of mug/mL;
m 2 testing the mass of the solid solution zirconium sample in g;
V 2 sample solid solution zirconium test liquid volume in mL;
1.3509-zirconium converts to a coefficient of zirconium oxide.
The particle size of the sample in the step 1) is less than 0.5mm
The specific steps for preparing the test solution in the step 2) are as follows:
2.1 Preparation of total zirconium test solution
Sample 1 was added with hydrochloric acid and nitro-compoundIn mixed acid of acid and hydrofluoric acid, heating for dissolution, cooling to room temperature, and constant volume to 100m, the volume is recorded as V 1 Standby;
2.2 Preparation of total zirconium sample blank test solution
Taking mixed acid of hydrochloric acid and nitric acid and hydrofluoric acid, heating to dissolve, cooling to room temperature, and fixing the volume to 100m for later use;
2.3 Preparation of solid solution zirconium test solution
Adding mixed acid of hydrochloric acid and nitric acid into sample 2, heating to dissolve, cooling to room temperature, filtering to precipitate, and fixing volume to 100m, and recording volume as V 2 Standby;
2.4 Preparation of blank test solution for solid solution zirconium sample
And (3) taking a mixed acid of hydrochloric acid and nitric acid, heating and dissolving, cooling to room temperature, and fixing the volume to 100m for standby.
The density of the nitric acid is 1.42g/mL, the density of the hydrochloric acid is 1.19g/mL, and the density of the hydrofluoric acid is 1.18g/mL.
The spectrometer is an inductively coupled plasma atomic emission spectrometer.
Hydrochloric acid in the mixed acid: the volume ratio of nitric acid is 3:1.
The volume ratio of the mixed acid to the hydrofluoric acid is 10:1.
Step 2.3) the precipitate is zirconia.
The heating and dissolving in the step 2.3) and the step 2.4), and when the tested material is a platinum-based alloy, adopting electric heating and dissolving; when the measured material is platinum-rhodium alloy, a microwave digestion instrument is adopted for heating and dissolving.
The microwave digestion instrument has programmable temperature, pressure and time control, can monitor the pressure and the temperature in the digestion process, and is matched with the clamping device, the protecting device and the pressure relief device for use.
The method of the invention uses Zr and ZrO 2 The solubility difference is measured by adopting an inductively coupled plasma atomic emission spectrometer to measure the total Zr and the solid solution Zr content, and the ZrO is indirectly measured 2 The content of the sample is accurate in measurement result, the method is simple and quick, and the sample loss is small.
The invention has the beneficial effects that:
1. the method prepares the solid solution zirconium test solution by using zirconium in the hydrochloric acid and nitric acid mixed acid dissolved material, and is used for reacting zirconium in the dissolved material; the method comprises the steps of mixing hydrochloric acid and nitric acid, adding zirconium and zirconium oxide in hydrofluoric acid dissolution materials to prepare total zirconium test solution, wherein the total zirconium test solution is used for dissolving zirconium and zirconium oxide contained in the materials, namely total zirconium. And measuring the emission spectrum intensity of the zirconium element in the test solution at the recommended wavelength on an inductively coupled plasma atomic emission spectrometer, calculating the mass fraction of the zirconium element in total zirconium and solid solution zirconium by a calibration curve, and calculating the content of zirconia in the dispersion strengthening platinum-based material by subtracting the mass fraction of the solid solution zirconium from the mass fraction of the total zirconium. The zirconia content in the dispersion strengthening platinum-based material detected by the method is measured indirectly, the method is simple and rapid, the sample loss is less, and the detection result is more accurate and reliable.
2. According to the method, the blank test solution is prepared while the total zirconium test solution and the solid solution zirconium test solution are prepared, and when the total zirconium and the solid solution zirconium element content of the sample are detected, the zirconium element content of the blank test solution is subtracted, so that the measurement of the total zirconium and the solid solution zirconium in the sample is more accurate, and the measurement of the zirconium oxide content in the dispersion-strengthened platinum-based material is more accurate.
The invention uses Zr and ZrO 2 The solubility difference is measured by adopting an inductively coupled plasma atomic emission spectrometer to measure the total Zr and the solid solution Zr content, and the ZrO is indirectly measured 2 The content of the sample is accurate in measurement result, the method is simple and quick, and the sample loss is small.
Drawings
FIG. 1 is a zirconium mass concentration calibration curve;
fig. 2 is a zirconium mass concentration calibration curve.
Detailed Description
All reagents used in this example were commercially available.
Example 1 measurement of zirconia content in platinum rhodium alloy materials
S1, sampling, namely taking two particle samples with the granularity smaller than 0.5mm, accurately weighing 0.05g of each sample to 0.0001, and marking 1 mass m of the sample 1 And sample 2 massIs m 2 Standby;
s2, preparing test liquid
Preparing a total zirconium test solution and a total zirconium sample blank test solution; solid solution zirconium test solution and solid solution zirconium sample blank test solution. Wherein the volume of the total zirconium test solution is marked as V 1 The volume of the solid solution zirconium test solution is marked as V 2 。
S21, preparation of total zirconium test solution
Placing the sample 1 into a 100mL polytetrafluoroethylene microwave digestion tank, adding 20mL of mixed acid of hydrochloric acid and nitric acid and 2mL of hydrofluoric acid, placing into a microwave digestion instrument, heating for dissolution, cooling after the completion, transferring into a 100mL plastic volumetric flask, fixing the volume to 100mL, and recording the volume as V 1 Standby;
s22, preparing blank test solution of total zirconium sample
Adding mixed acid of 20mL hydrochloric acid and nitric acid and 2mL hydrofluoric acid into a 100mL polytetrafluoroethylene microwave digestion tank, putting into a microwave digestion instrument, heating for dissolution, cooling after finishing, transferring into a 100mL plastic volumetric flask, and fixing the volume to 100mL for later use;
s23, preparation of solid solution zirconium test solution
Placing the sample 2 in a 100mL polytetrafluoroethylene microwave digestion tank, adding 20mL of mixed acid of hydrochloric acid and nitric acid, heating for dissolution, cooling, transferring into a 100mL volumetric flask, and fixing the volume to 100mL, wherein the volume is recorded as V 2 Standby; after heating to dissolve the metal sample, white powder zirconia exists at the bottom of the container when cooling, and the zirconia powder is filtered to prevent the zirconia powder from being adsorbed into equipment in the testing process to damage the service life of the equipment.
In this embodiment, the content of zirconia in the dispersion-strengthened platinum-rhodium alloy is detected, so that a microwave digestion instrument is used for heating and dissolving.
S24, preparing blank test solution of solid solution zirconium sample
Adding 20mL of mixed acid of hydrochloric acid and nitric acid into a 100mL polytetrafluoroethylene microwave digestion tank, transferring to a 100mL plastic volumetric flask, and fixing the volume to 100mL for later use;
s3, drawing a calibration curve
Selecting standard solution with zirconium element content of 1000 mug/mL, placing 10.00mL into a 100mL polytetrafluoroethylene volumetric flask, adding 2mL hydrofluoric acid and 10mL nitric acid, diluting the standard solution to 100 mug/mL by adding water, respectively transferring 0.00mL, 0.50mL, 1.00mL, 2.00mL, 3.00mL, 4.00mL, 5.00mL and 10.00mL of diluted solution into 8 plastic volumetric flasks, adding 10mL of mixed acid of hydrochloric acid and nitric acid and 2mL of hydrofluoric acid, diluting with water, and shaking uniformly;
the density of the nitric acid is 1.42g/mL, the density of the hydrochloric acid is 1.19g/mL, the density of the hydrofluoric acid is 1.18g/mL, and the ratio of the mixed acid of the hydrochloric acid and the nitric acid is 3:1.
And testing the intensity of the zirconium element in the diluted standard solution at the wavelength 343.823nm by adopting an inductively coupled plasma atomic emission spectrometer, drawing a calibration curve by taking the emission spectrum intensity of the zirconium element as an ordinate and the mass concentration as an abscissa, and establishing a binary one-time equation to obtain the relationship between the zirconium spectrum intensity I and the zirconium mass concentration rho as follows:
I＝aρ+b
wherein:
the illumination intensity of the element I-zirconium;
the mass concentration of rho-zirconium element;
a-coefficient of variable;
b-coefficient of variable;
it follows that i= 7426.8 ρ -130.25
S4, calculating the mass concentration of the zirconium element in the test solution, detecting the emission intensity of the zirconium element in the total zirconium test solution, the total zirconium sample blank test solution, the solid solution zirconium test solution and the solid solution zirconium sample blank test solution at the wavelength of 343.8nm by adopting an inductively coupled plasma atomic emission spectrometer, and calculating the total zirconium test solution and the total zirconium sample blank test solution by using a binary one-time equation corresponding to a calibration curve drawn by the standard solution in the step S3; the mass concentration of zirconium element in the solid solution zirconium test solution and the solid solution zirconium blank test solution are ρ respectively 1 、ρ 2 、
ω is calculated according to the following formula:
wherein:
omega-zirconia mass fraction in units of;
ρ 1 -the mass concentration of zirconium element in the sample total zirconium test solution in micrograms per milliliter (μg/mL);
-the mass concentration of zirconium element in the blank solution of the total zirconium sample, in micrograms per milliliter (μg/mL);
m 1 -testing the mass of the total zirconium sample in grams (g);
V 1 sample total zirconium test liquid volume in milliliters (mL);
ρ 2 -the mass concentration of zirconium element in the sample solid solution zirconium test solution in micrograms per milliliter (μg/mL);
-the mass concentration of zirconium element in the blank solution of the solid-solution zirconium sample, in micrograms per milliliter (μg/mL);
m 2 testing the mass of the solid-solution zirconium sample in grams (g);
V 2 sample-sampleSolid solution zirconium test liquid volume in milliliters (mL);
1.3509-the coefficient of zirconium oxide is converted by zirconium alone.
The calculation results are that:
in this embodiment, the microwave digestion instrument has programmable temperature, pressure and time control, can monitor pressure and temperature in digestion process, and cooperates clamping device, protector and pressure release device to use.
In this embodiment, the inductively coupled plasma atomic emission spectrometer is equipped with a hydrofluoric acid resistant atomization system and a peristaltic pump for sample injection. Recommended instrument operating parameters are shown in table 1.
Table 1 instrument operating conditions
Conclusion:
the zirconia content in the zirconia dispersion strengthened platinum rhodium alloy tested in this example was 0.330%.
Example 2 measurement of zirconia content in platinum Material
When the material to be measured is a dispersion strengthening platinum material, the method for measuring the zirconia content in the platinum material except the sample in the step S1 accurately weighs 0.1g of each sample; and (3) heating and dissolving in the step (S3), wherein the rest steps are the same as 1 except that the electric heating plate is adopted for heating and dissolving.
The calibration curve is plotted according to the formula i=aρ+b, see fig. 2.
It follows that i= 8251.4 ρ -142.57
Binary one-time equation corresponding to the calibration curve drawn by the standard solution is used for calculating total zirconium test solution and totalZirconium sample blank test solution, solid solution zirconium test solution and mass concentration of zirconium element in solid solution zirconium blank test solution are ρ respectively 1 、ρ 2 、
ω is calculated according to the formula:
conclusion: this example shows that the zirconia content of the zirconia dispersion strengthened platinum material is 0.193%.
Variations and modifications to the above would be obvious to persons skilled in the art to which the invention pertains from the foregoing description and teachings. Therefore, the invention is not limited to the specific embodiments disclosed and described above, but some modifications and changes of the invention should be also included in the scope of the claims of the invention. In addition, although specific terms are used in the present specification, these terms are used for convenience of description only and do not limit the present invention in any way, and other devices identical or similar to the present invention are used within the scope of the present invention.
Claims (9)
1. The method for measuring the content of zirconia in the dispersion strengthening platinum-based material is characterized by comprising the following steps of:
1) Taking two samples of dispersion strengthening platinum-based material, and setting the mass of sample 1 as m 1 And sample 2 qualityThe amount is m 2 Standby;
2) Preparing a test solution:
preparing a total zirconium test solution and a total zirconium sample blank test solution; solid solution zirconium test solution and solid solution zirconium sample blank test solution;
3) Drawing a calibration curve:
selecting a standard solution with the zirconium element content of 1000 mug/mL, and preparing the standard solution with the zirconium concentration of 100 mug/mL; 0.00mL, 0.50mL, 1.00mL, 2.00mL, 3.00mL, 4.00mL, 5.00mL and 10.00mL of mixed acid of hydrochloric acid and nitric acid and hydrofluoric acid are respectively taken, wherein the mixed acid is as follows: the volume ratio of hydrofluoric acid is 10-5: 1, water is used for constant volume to 100mL, and shaking is carried out uniformly to prepare a series of calibration solutions;
testing the intensity of the zirconium element in the series of calibration solutions at the wavelength 343.8nm or 339.1nm of the spectrometer, and performing linear regression by taking the intensity of the zirconium element as an ordinate and the mass concentration of the zirconium in the calibration solution as an abscissa;
4) And (3) calculating the mass concentration of zirconium element in the test solution:
testing the emission intensity of the zirconium element in the total zirconium test solution, the total zirconium sample blank test solution, the solid solution zirconium test solution and the solid solution zirconium sample blank test solution at the wavelength 343.8nm or 339.1nm of the spectrometer, and calculating the mass concentration of the zirconium element in the total zirconium test solution, the total zirconium sample blank test solution, the solid solution zirconium test solution and the solid solution zirconium sample blank test solution by using the following formulas according to the calibration curve drawn by the standard solution in the step 3):
wherein:
omega-zirconia mass fraction in units of;
ρ 1 the mass concentration of zirconium element in the total zirconium sample test solution is expressed in mug/mL;
blank solution of total zirconium sampleThe mass concentration of the element zirconium is in mug/mL;
m 1 -testing the mass of the total zirconium sample in g;
V 1 sample total zirconium test liquid volume in mL;
ρ 2 the mass concentration of zirconium element in the sample solid solution zirconium test solution is expressed in mug/mL;
the mass concentration of zirconium element in a blank solution of a solid solution zirconium sample is presented in the unit of mug/mL;
m 2 testing the mass of the solid solution zirconium sample in g;
V 2 sample solid solution zirconium test liquid volume in mL;
1.3509-zirconium converts to a coefficient of zirconium oxide.
2. The assay of claim 1, wherein: the particle size of the sample in the step 1) is smaller than 0.5mm.
3. The method according to claim 1, wherein the specific steps for preparing the test solution in step 2) are as follows:
2.1 Preparation of total zirconium test solution
Adding mixed acid of hydrochloric acid and nitric acid and hydrofluoric acid into sample 1, heating for dissolution, cooling to room temperature, and constant volume to 100m, and recording volume as V 1 Standby;
2.2 Preparation of total zirconium sample blank test solution
Taking mixed acid of hydrochloric acid and nitric acid and hydrofluoric acid, heating to dissolve, cooling to room temperature, and fixing the volume to 100m for later use;
2.3 Preparation of solid solution zirconium test solution
Adding mixed acid of hydrochloric acid and nitric acid into sample 2, heating to dissolve, cooling to room temperature, precipitating, and fixing volume to 100m, and recording volume as V 2 Standby;
2.4 Preparation of blank test solution for solid solution zirconium sample
And (3) taking a mixed acid of hydrochloric acid and nitric acid, heating and dissolving, cooling to room temperature, and fixing the volume to 100m for standby.
4. A method according to claim 1 or 3, wherein: the density of the nitric acid is 1.42g/mL, the density of the hydrochloric acid is 1.19g/mL, and the density of the hydrofluoric acid is 1.18g/mL.
5. The assay of claim 1, wherein: the spectrometer is an inductively coupled plasma atomic emission spectrometer.
6. A method according to claim 1 or 3, wherein: hydrochloric acid in the mixed acid: the volume ratio of nitric acid is 3:1.
7. The assay of claim 3, wherein: the volume ratio of the mixed acid to the hydrofluoric acid is 10:1.
8. The assay of claim 3, wherein: step 2.3) the precipitate is zirconia.
9. The assay of claim 3, wherein: step 2.3) and step 2.4) of heating and dissolving, wherein if the measured material is platinum-based alloy, electric heating and dissolving are adopted; and if the measured material is platinum-rhodium alloy, heating and dissolving by adopting a microwave digestion instrument.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310855312.XA CN117092090B (en) | 2023-07-12 | 2023-07-12 | A method for determining zirconium oxide content in dispersion-strengthened platinum-based materials |
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| CN202310855312.XA CN117092090B (en) | 2023-07-12 | 2023-07-12 | A method for determining zirconium oxide content in dispersion-strengthened platinum-based materials |
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| CN117092090A true CN117092090A (en) | 2023-11-21 |
| CN117092090B CN117092090B (en) | 2024-12-06 |
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