CN105466910A - Method for measuring contents of zirconium and zirconia in strengthened dispersion platinum - Google Patents
Method for measuring contents of zirconium and zirconia in strengthened dispersion platinum Download PDFInfo
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Abstract
The invention provides a method capable of rapidly and accurately measuring contents of zirconium element and zirconia in strengthened dispersion platinum. The method for measuring contents of zirconium and zirconia in strengthened dispersion platinum comprises the following steps: 1) weighing strengthened dispersion platinum, adding aqua regia and dissolving; 2) evaporating after dissolving, filtering out undissolved zirconium oxide by adding hydrochloric acid, transferring a filtrate into a volumetric flask and diluting the filtrate by adding pure water to scale so as to obtain a sample of zirconium element; 3) putting the filtered zirconium oxide along with filter paper into a crucible, ashing by an electric furnace, adding ammonium sulfate and sulfuric acid, dissolving and cooling, transferring the liquid into a volumetric flask and diluting the liquid by adding pure water to scale so as to obtain a sample of zirconium oxide content; 4) building a standard curve; 5) testing; and 6) calculating. After strengthened dispersion platinum is dissolved, contents of zirconium element and zirconia in the strengthened dispersion platinum can be rapidly and accurately measured by a plasma atomic emitted spectrometer. By the method, testing accuracy and analysis efficiency are enhanced.
Description
Technical field
The present invention relates to a kind of measuring method strengthening simple substance zirconium and zirconia content in disperse precious metal material, particularly relate to a kind of measuring method strengthening simple substance zirconium and zirconia content in disperse platinum.
Background technology
Dispersion-strengtherning alloy platinum material is oxidized by add simple substance zr element in platinum after, after making simple substance zr element be oxidized to zirconia, improve intensity and the corrosion resistance of material itself, the degree of oxidation of zr element is higher, then the intensity of disperse material self is stronger, and corrosion resistance is better.Therefore, need to judge its intensity and corrosion resistance by the zirconium in test strengthening disperse platinum and zirconic content, but detection method also not relevant at present.
Summary of the invention
Technical matters to be solved by this invention is to provide a kind of method quick and precisely can measuring simple substance zr element and zirconic content in strengthening disperse platinum.
The technical scheme that technical solution problem of the present invention adopts: the measuring method of zirconium and zirconia content in strengthening disperse platinum, the method includes the steps of:
1) take strengthening disperse platinum 0.5-2g, add 20-40mL chloroazotic acid, dissolve 120-180 DEG C of temperature;
2) be evaporated near dry after dissolving, add 10-20 milliliter hydrochloric acid and filter out undissolved zirconia, filtrate to be moved in volumetric flask and to be diluted to scale with pure water, as the sample 1 of the simple substance zr element in strengthening disperse platinum to be measured;
3) by step 2) zirconia that leaches puts into crucible together with filter paper, place electric furnace ashing, then ammonium sulfate 0.5-2g and sulfuric acid 3-5mL is added, to dissolve and after cooling, liquid to be moved in volumetric flask and to be diluted to scale with pure water, as the sample 2 of the zirconia content in strengthening disperse platinum to be measured;
4) Criterion curve
Select Zr constituent content to be the standard stock solution of 1000ug/mL, stepwise dilution is configured to the standard solution that content is 10 μ g/mL, 30 μ g/mL, 100 μ g/mL;
5) test
The signature analysis wavelength of zr element is selected to be respectively 343.823nm, 339.197nm, 257.139nm, using plasma emission spectrometer input step 4) in the number of standard solution of preparation and standard value, set up the typical curve of each impurity element, test sample on this basis, wherein the value C of sample 1
1, the value C of sample 2
2, the reagent blank simultaneously using the difference of acid to obtain according to sample dissolution is respectively C
0and C
0 /, and carry out test agent blank according to same test condition;
6) calculate
Content (mg/kg)=(C of metal zirconium in strengthening disperse platinum
1-C
0) × K
In formula:
The content of the element to be measured of the sample that C--ICP measures, μ g/mL;
C
0--measure the content of the element to be measured of the reagent blank of chloroazotic acid medium with ICP, μ g/mL;
K--represents the extension rate of sample, is set to 100 in this method;
Zirconic content (mg/kg)=(C in strengthening disperse platinum
2-C
0 /) × K × 1.3509
In formula:
The content of the element to be measured of the sample that C--ICP measures, μ g/mL;
C
0 /--measure the content of the element to be measured of the reagent blank of sulfuric acid medium with ICP, μ g/mL;
K--represents the extension rate of sample, is set to 100 in the inventive method;
Simple substance zirconium is converted into zirconic coefficient by 1.3509--.
Further, described step 1) be: take strengthening disperse platinum 0.5-2g, in beaker, add 20-40mL chloroazotic acid, cover surface plate, be placed on electric hot plate and dissolve by 120-180 DEG C of temperature.
Further, described step 3) be: by step 2) zirconia that leaches puts into silica crucible together with filter paper, place electric furnace 700-800 DEG C of ashing, then add ammonium sulfate 0.5-2g and sulfuric acid 3-5mL and dissolve by 160-180 DEG C of temperature on electric hot plate; After cooling, liquid to be moved in volumetric flask and to be diluted to scale with pure water, as the sample 2 of the zirconia content in strengthening disperse platinum to be measured.
Further, described step 5) middle plasma emission spectrometer, first check before start that whether main frame is connected with computing machine normal, confirms that chilled water is opened and is in normal condition, confirm that air compressor machine is opened also normal, after all meeting, open main frame.
Further, described step 5) in plasma emission spectrometer instrument test condition for: determine that used purity of argon is >=99.99%, regulate argon bottle decompressor to argon pressure within the scope of 0.5-0.8MPa, and ensure that in gas cylinder, argon pressure is not less than 1MPa.
The invention has the beneficial effects as follows: will strengthen after disperse platinum dissolves, by plasma emission spectrometer, can rapid and accurate determination wherein simple substance zr element and zirconic content, the method increase test accuracy and analysis efficiency.
Embodiment
In strengthening disperse platinum of the present invention, the method for testing of simple substance zr element and zirconia content comprises following steps:
1) take strengthening disperse platinum 0.5-2g (being accurate to 0.0001g), in 50mL beaker, add 20-40mL chloroazotic acid (hydrochloric acid: nitric acid=4:1), cover surface plate, be placed on electric hot plate and dissolve by 120-180 DEG C of temperature;
2) be evaporated near dry after dissolving, add 10-20 milliliter 1+1 hydrochloric acid and filter out undissolved zirconia, filtrate to be moved in 100mL volumetric flask and to be diluted to scale with pure water, as the sample 1 of the simple substance zr element in strengthening disperse platinum to be measured;
3) by step 2) zirconia that leaches puts into silica crucible together with filter paper, and place electric furnace 700-800 DEG C of ashing, then add ammonium sulfate 0.5-2g and sulfuric acid 3-5mL and dissolve by 160-180 DEG C of temperature on electric hot plate; After cooling, liquid to be moved in 100mL volumetric flask and to be diluted to scale with pure water, as the sample 2 of the zirconia content in strengthening disperse platinum to be measured;
4) Criterion curve
Select Zr constituent content to be the standard stock solution of 1000ug/mL, stepwise dilution is configured to the standard solution that content is 10 μ g/mL, 30 μ g/mL, 100 μ g/mL;
5) test
The signature analysis wavelength of zr element is selected to be respectively 343.823nm, 339.197nm, 257.139nm, and using plasma emission spectrometer, input step 4) in the number of standard solution of preparation and standard value, set up the typical curve of each impurity element, test sample on this basis.The wherein value C of sample 1
1, the value C of sample 2
2, the reagent blank simultaneously using the difference of acid to obtain according to sample dissolution is respectively C
0(chloroazotic acid medium) and C
0 /(sulfuric acid medium), and carry out test agent blank according to same test condition.
6) calculate
Content (mg/kg)=(C of metal zirconium in strengthening disperse platinum
1-C
0) × K
In formula:
The content of the element to be measured of the sample that C--ICP measures, μ g/mL;
C
0--measure the content of the element to be measured of the reagent blank of chloroazotic acid medium with ICP, μ g/mL;
K--represents the extension rate of sample, is set to 100 in this method.
Zirconic content (mg/kg)=(C in strengthening disperse platinum
2-C
0 /) × K × 1.3509
In formula:
The content of the element to be measured of the sample that C--ICP measures, μ g/mL;
C
0 /--measure the content of the element to be measured of the reagent blank of sulfuric acid medium with ICP, μ g/mL;
K--represents the extension rate of sample, is set to 100 in the inventive method;
Simple substance zirconium is converted into zirconic coefficient by 1.3509--.
Plasma emission spectrometer and instrument test condition in the present invention's test:
Check before start that whether normally main frame is connected with computing machine, confirm that chilled water is opened and is in normal condition, confirm that air compressor machine is opened and normally, opens main frame after all meeting.Determine that used purity of argon is >=99.99%, regulate argon bottle decompressor to argon pressure within the scope of 0.5-0.8MPa, and ensure that in gas cylinder, argon pressure is not less than 1MPa.
Embodiment 1:
Take 0.5000 gram of strengthening disperse platinum sample (being numbered MPt-1) in glass beaker, add chloroazotic acid 20mL (hydrochloric acid: nitric acid=4:1), dissolve 130 DEG C of temperature.Be evaporated near dry after dissolving, add 10 milliliters of 1+1 hydrochloric acid and filter out undissolved zirconia, filtrate to be moved in 100mL volumetric flask and to be diluted to scale with pure water, as the sample 1 of the simple substance zr element in strengthening disperse platinum to be measured, and according to the blank C of the same terms reagent preparation
0;
The zirconia leached is put into silica crucible together with filter paper, and place electric furnace 700 DEG C of ashing, then add ammonium sulfate 0.5g, sulfuric acid 3mL dissolves by 170 DEG C of temperature on electric hot plate; After cooling, liquid to be moved in 100mL volumetric flask and to be diluted to scale with pure water, as the sample 2 of the zirconia content in strengthening disperse platinum to be measured, and according to the blank C of the same terms reagent preparation
0 /.
Criterion curve
Select Zr constituent content to be the standard stock solution of 1000ug/mL, stepwise dilution is configured to the standard solution that content is 10 μ g/mL, 30 μ g/mL, 100 μ g/mL.
Testing procedure
Select the signature analysis wavelength 343.823nm of zr element and the instrument test condition of table 1, the number of input standard solution and standard value, set up the typical curve of each impurity element, test sample on this basis.The wherein value C of sample 1
1, the value C of sample 2
2, simultaneously and according to the blank C of the same terms reagent preparation
0, C
0 /.
Table 1
Calculate
Content (mg/kg)=(C of metal zirconium in strengthening disperse platinum
1-C
0) × K
In formula: the content of the element to be measured of the sample that C--ICP measures, μ g/mL;
C
0--the content of the element to be measured of the reagent blank measured with ICP, μ g/mL;
K--represents the extension rate of sample, is set to 100 in the method.
Zirconic content (mg/kg)=(C in strengthening disperse platinum
2-C
0 /) × K × 1.3509
In formula: the content of the element to be measured of the sample that C--ICP measures, μ g/mL;
C
0--the content of the element to be measured of the reagent blank measured with ICP, μ g/mL;
K--represents the extension rate of sample, is set to 100 in the method;
1.3509-simple substance zirconium is converted into zirconic coefficient.
The result drawn and proportioning value, disperse time, anticorrosion effect etc. are compared, the results are shown in Table 2:
Table 2
Be added with simple substance zirconium content in sample after transferring zirconia content in sample to simple substance zirconium content, the result obtained is consistent with proportioning value.
Embodiment 2:
Take 1.0000 grams of strengthenings disperse platinum sample (being numbered MPt-2) in glass beaker, add chloroazotic acid 30mL (hydrochloric acid: nitric acid=4:1), dissolve 150 DEG C of temperature.Be evaporated near dry after dissolving, add 15 milliliters of 1+1 hydrochloric acid and filter out undissolved zirconia, filtrate to be moved in 100mL volumetric flask and to be diluted to scale with pure water, as the sample 1 of the simple substance zr element in strengthening disperse platinum to be measured, and according to the blank C of the same terms reagent preparation
0;
The zirconia leached is put into silica crucible together with filter paper, and place electric furnace 750 DEG C of ashing, then add ammonium sulfate 1.0g, sulfuric acid 4mL dissolves by 160 DEG C of temperature on electric hot plate; After cooling, liquid to be moved in 100mL volumetric flask and to be diluted to scale with pure water, as the sample 2 of the zirconia content in strengthening disperse platinum to be measured, and according to the blank C of the same terms reagent preparation
0 /.
Criterion curve
Select Zr constituent content to be the standard stock solution of 1000ug/mL, stepwise dilution is configured to the standard solution that content is 10 μ g/mL, 30 μ g/mL, 100 μ g/mL.
Testing procedure
Select the signature analysis wavelength 339.197nm of zr element and the instrument test condition of table 1, the number of input standard solution and standard value, set up the typical curve of each impurity element, test sample on this basis.The wherein value C of sample 1
1, the value C of sample 2
2, test the reagent blank C of the same terms simultaneously
0, C
0 /.
Calculate
Content (mg/kg)=(C of metal zirconium in strengthening disperse platinum
1-C
0) × K
In formula: the content of the element to be measured of the sample that C--ICP measures, μ g/mL;
C
0--the content of the element to be measured of the reagent blank measured with ICP, μ g/mL;
K--represents the extension rate of sample, is set to 100 in the method.
Zirconic content (mg/kg)=(C in strengthening disperse platinum
2-C
0 /) × K × 1.3509
In formula: the content of the element to be measured of the sample that C--ICP measures, μ g/mL;
C
0--the content of the element to be measured of the reagent blank measured with ICP, μ g/mL;
K--represents the extension rate of sample, is set to 100 in the method;
1.3509-simple substance zirconium is converted into zirconic coefficient.
The result drawn and proportioning value, disperse time, anticorrosion effect etc. are compared, the results are shown in Table 3:
Table 3
Be added with simple substance zirconium content in sample after transferring zirconia content in sample to simple substance zirconium content, the result obtained is consistent with proportioning value.
Embodiment 3:
Take 2.0000 grams of strengthenings disperse platinum sample (being numbered MPt-3) in glass beaker, add chloroazotic acid 40mL (hydrochloric acid: nitric acid=4:1), dissolve 180 DEG C of temperature.Be evaporated near dry after dissolving, add 20 milliliters of 1+1 hydrochloric acid and filter out undissolved zirconia, filtrate to be moved in 100mL volumetric flask and to be diluted to scale, as the sample 1 of the simple substance zr element in strengthening disperse platinum to be measured, and according to the blank C of the same terms reagent preparation
0;
Zirconia and filter paper are put into silica crucible, and place electric furnace 800 DEG C of ashing, then add ammonium sulfate 2.0g, sulfuric acid 5mL dissolves by 180 DEG C of temperature on electric hot plate; After cooling, liquid to be moved in 100mL volumetric flask and to be diluted to scale, as the sample 2 of the zirconia content in dispersion intensifying platinum to be measured, and according to the blank C of the same terms reagent preparation
0 /.
Criterion curve
Select Zr constituent content to be the standard stock solution of 1000ug/mL, stepwise dilution is configured to the standard solution that content is 10 μ g/mL, 30 μ g/mL, 100 μ g/mL.
Testing procedure
Select the signature analysis wavelength 257.139nm of zr element and the instrument test condition of table 1, the number of input standard solution and standard value, set up the typical curve of each impurity element, test sample on this basis.The wherein value C of sample 1
1, the value C of sample 2
2, test the reagent blank C of the same terms simultaneously
0, C
0 /.
Calculate
Content (mg/kg)=(C of metal zirconium in strengthening disperse platinum
1-C
0) × 100
In formula: the content of the element to be measured of the sample that C--ICP measures, μ g/mL;
C
0--the content of the element to be measured of the reagent blank measured with ICP, μ g/mL;
K--represents the extension rate of sample, is set to 100 in the method.
Zirconic content (mg/kg)=(C in strengthening disperse platinum
2-C
0 /) × K × 1.3509
In formula: the content of the element to be measured of the sample that C--ICP measures, μ g/mL;
C
0--the content of the element to be measured of the reagent blank measured with ICP, μ g/mL;
K--represents the extension rate of sample, is set to 100 in the method.
1.3509-simple substance zirconium is converted into zirconic coefficient.
The result drawn and proportioning value, disperse time, anticorrosion effect etc. are compared, the results are shown in Table 4:
Table 4
Be added with simple substance zirconium content in sample after transferring zirconia content in sample to simple substance zirconium content, the result obtained is consistent with proportioning value.
Data in above-described embodiment show, test result of the present invention is consistent with initial ratio value, and the test result accurate and effective of method of testing of the present invention is described.
Also match with experimental test data in process conditions and later stage result of use according to the material that different technique draws, prove that method of testing of the present invention correctly can judge the quality of material.
Claims (5)
1. strengthen the measuring method of zirconium and zirconia content in disperse platinum, it is characterized in that, the method includes the steps of:
1) take strengthening disperse platinum 0.5-2g, add 20-40mL chloroazotic acid, dissolve 120-180 DEG C of temperature;
2) be evaporated near dry after dissolving, add 10-20 milliliter hydrochloric acid and filter out undissolved zirconia, filtrate to be moved in volumetric flask and to be diluted to scale with pure water, as the sample 1 of the simple substance zr element in strengthening disperse platinum to be measured;
3) by step 2) zirconia that leaches puts into crucible together with filter paper, place electric furnace ashing, then ammonium sulfate 0.5-2g and sulfuric acid 3-5mL is added, to dissolve and after cooling, liquid to be moved in volumetric flask and to be diluted to scale with pure water, as the sample 2 of the zirconia content in strengthening disperse platinum to be measured;
4) Criterion curve
Select Zr constituent content to be the standard stock solution of 1000ug/mL, stepwise dilution is configured to the standard solution that content is 10 μ g/mL, 30 μ g/mL, 100 μ g/mL;
5) test
The signature analysis wavelength of zr element is selected to be respectively 343.823nm, 339.197nm, 257.139nm, using plasma emission spectrometer input step 4) in the number of standard solution of preparation and standard value, set up the typical curve of each impurity element, test sample on this basis, wherein the value C of sample 1
1, the value C of sample 2
2, the reagent blank simultaneously using the difference of acid to obtain according to sample dissolution is respectively C
0and C
0 /, and carry out test agent blank according to same test condition;
6) calculate
Content (mg/kg)=(C of metal zirconium in strengthening disperse platinum
1-C
0) × K
In formula:
The content of the element to be measured of the sample that C--ICP measures, μ g/mL;
C
0--measure the content of the element to be measured of the reagent blank of chloroazotic acid medium with ICP, μ g/mL;
K--represents the extension rate of sample, is set to 100 in this method;
Zirconic content (mg/kg)=(C in strengthening disperse platinum
2-C
0 /) × K × 1.3509
In formula:
The content of the element to be measured of the sample that C--ICP measures, μ g/mL;
C
0 /--measure the content of the element to be measured of the reagent blank of sulfuric acid medium with ICP, μ g/mL;
K--represents the extension rate of sample, is set to 100 in the inventive method;
Simple substance zirconium is converted into zirconic coefficient by 1.3509--.
2. the measuring method strengthening zirconium and zirconia content in disperse platinum as claimed in claim 1, it is characterized in that, described step 1) be: take strengthening disperse platinum 0.5-2g, 20-40mL chloroazotic acid is added in beaker, cover surface plate, be placed on electric hot plate and dissolve by 120-180 DEG C of temperature.
3. the measuring method strengthening zirconium and zirconia content in disperse platinum as claimed in claim 1, it is characterized in that, described step 3) be: by step 2) zirconia that leaches puts into silica crucible together with filter paper, place electric furnace 700-800 DEG C of ashing, then add ammonium sulfate 0.5-2g and sulfuric acid 3-5mL and dissolve by 160-180 DEG C of temperature on electric hot plate; After cooling, liquid to be moved in volumetric flask and to be diluted to scale with pure water, as the sample 2 of the zirconia content in strengthening disperse platinum to be measured.
4. the measuring method strengthening zirconium and zirconia content in disperse platinum as claimed in claim 1, it is characterized in that, described step 5) middle plasma emission spectrometer, first check before start whether main frame is connected with computing machine normal, confirm that chilled water is opened and is in normal condition, confirm that air compressor machine is opened and normally, opens main frame after all meeting.
5. the measuring method strengthening zirconium and zirconia content in disperse platinum as claimed in claim 1, it is characterized in that, described step 5) in plasma emission spectrometer instrument test condition for: determine that used purity of argon is >=99.99%, regulate argon bottle decompressor to argon pressure within the scope of 0.5-0.8MPa, and ensure that in gas cylinder, argon pressure is not less than 1MPa.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109837498A (en) * | 2017-11-24 | 2019-06-04 | 彩虹显示器件股份有限公司 | A kind of method in indirect dispersion-strengtherning platinum channel |
| CN113155811A (en) * | 2021-03-24 | 2021-07-23 | 天津巴莫科技有限责任公司 | Method for measuring content of zirconium element in lithium ion battery anode material |
| CN113267421A (en) * | 2021-06-29 | 2021-08-17 | 巴斯夫公司 | Method for determining noble metal content |
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| CN102879384A (en) * | 2012-10-12 | 2013-01-16 | 中国航空工业集团公司北京航空材料研究院 | Method for detecting zirconium content in tantalum-cobalt-base alloy in microwave solution sample dissolving manner |
| CN104597037A (en) * | 2015-01-09 | 2015-05-06 | 江苏省沙钢钢铁研究院有限公司 | Method for measuring zirconium content in silicon-zirconium alloy |
| CN104614365A (en) * | 2013-11-04 | 2015-05-13 | 青岛天恒机械有限公司 | Inductively coupled plasma-atomic emission spectrometry for measuring chromium and zirconium in Cu-Cr-Zr alloy |
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- 2015-11-23 CN CN201510819664.5A patent/CN105466910B/en active Active
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102879384A (en) * | 2012-10-12 | 2013-01-16 | 中国航空工业集团公司北京航空材料研究院 | Method for detecting zirconium content in tantalum-cobalt-base alloy in microwave solution sample dissolving manner |
| CN104614365A (en) * | 2013-11-04 | 2015-05-13 | 青岛天恒机械有限公司 | Inductively coupled plasma-atomic emission spectrometry for measuring chromium and zirconium in Cu-Cr-Zr alloy |
| CN104597037A (en) * | 2015-01-09 | 2015-05-06 | 江苏省沙钢钢铁研究院有限公司 | Method for measuring zirconium content in silicon-zirconium alloy |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109837498A (en) * | 2017-11-24 | 2019-06-04 | 彩虹显示器件股份有限公司 | A kind of method in indirect dispersion-strengtherning platinum channel |
| CN113155811A (en) * | 2021-03-24 | 2021-07-23 | 天津巴莫科技有限责任公司 | Method for measuring content of zirconium element in lithium ion battery anode material |
| CN113267421A (en) * | 2021-06-29 | 2021-08-17 | 巴斯夫公司 | Method for determining noble metal content |
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|---|---|
| CN105466910B (en) | 2018-03-20 |
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