CN105466910B - Strengthen the measuring method of zirconium and zirconia content in disperse platinum - Google Patents
Strengthen the measuring method of zirconium and zirconia content in disperse platinum Download PDFInfo
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Abstract
The present invention provides a kind of method that can quick and precisely measure and strengthen the content of simple substance zr element and zirconium oxide in disperse platinum.Strengthen the measuring method of zirconium and zirconia content in disperse platinum, the method includes the steps of：1) weigh and strengthen disperse platinum, add chloroazotic acid, dissolved；2) evaporated after dissolving, add hydrochloric acid to filter out undissolved zirconium oxide, filtrate is moved into volumetric flask and is diluted to scale with pure water, the sample as simple substance zr element；3) zirconium oxide filtered out is put into crucible together with filter paper, places electric furnace ashing, then add ammonium sulfate and sulfuric acid, after dissolving and cooling down, liquid moved into volumetric flask and is diluted to scale with pure water, the sample as zirconia content；4) standard curve is established；5) test；6) calculate.After the present invention will strengthen the dissolving of disperse platinum, by plasma emission spectrometer, test accuracy and analysis efficiency can be improved with the rapid and accurate determination wherein content of simple substance zr element and zirconium oxide.
Description
Technical field
The present invention relates to the measuring method of simple substance zirconium and zirconia content in a kind of reinforcing disperse precious metal material, it is particularly
It is related to the measuring method of simple substance zirconium and zirconia content in a kind of reinforcing disperse platinum.
Background technology
Dispersion-strengtherning alloy platinum material is by being aoxidized after adding simple substance zr element in platinum, aoxidizing simple substance zr element
Into after zirconium oxide, material intensity and corrosion resistance in itself is improved, the degree of oxidation of zr element is higher, then disperse material itself
Intensity is stronger, and corrosion resistance is more preferable.Therefore, it is necessary to be judged by testing the content of the zirconium and zirconium oxide strengthened in disperse platinum
Its intensity and corrosion resistance, but there is presently no the detection method of correlation.
The content of the invention
The technical problems to be solved by the invention, which are to provide one kind, can quick and precisely measure simple substance in reinforcing disperse platinum
The method of the content of zr element and zirconium oxide.
The technical proposal for solving the technical problem of the invention：Strengthen the measurement of zirconium and zirconia content in disperse platinum
Method, the method includes the steps of：
1) weigh and strengthen disperse platinum 0.5-2g, add 20-40mL chloroazotic acid, dissolved in 120-180 DEG C of temperature；
2) it is evaporated to after dissolving and closely does, adds 10-20 milliliter hydrochloric acid to filter out undissolved zirconium oxide, filtrate is moved into capacity
Scale is diluted in bottle and with pure water, the sample 1 as the simple substance zr element in reinforcing disperse platinum to be measured；
3) zirconium oxide that step 2) filters out is put into crucible together with filter paper, places electric furnace ashing, then add sulphur
Sour ammonium 0.5-2g and sulfuric acid 3-5mL, after dissolving and cooling down, liquid is moved into volumetric flask and is diluted to scale with pure water, is made
For the sample 2 of the zirconia content in reinforcing disperse platinum to be measured；
4) standard curve is established
From the standard stock solution that Zr constituent contents are 1000ug/mL, it is 10 μ g/mL, 30 μ g/ that dilution, which is configured to content, step by step
ML, 100 μ g/mL standard liquid；
5) test
The signature analysis wavelength of selection zr element is respectively 343.823nm, 339.197nm, 257.139nm, using etc. from
Daughter emission spectrometer input step 4) in the number and standard value of standard liquid prepared, the standard for establishing each impurity element is bent
The value C of line, on this basis test sample, wherein sample 11, the value C of sample 22, while the difference according to sample dissolution using acid
Obtained reagent blank is respectively C0And C0 /, and carry out test agent blank according to same test condition；
6) calculate
Strengthen content (mg/kg)=(C of metal zirconium in disperse platinum1-C0)×K
In formula：
C1-- with the content of the element to be measured of the sample 1 of ICP measure, μ g/mL；
C0-- the content of the element to be measured of the reagent blank of chloroazotic acid medium, μ g/mL are determined with ICP；
K-- represents the extension rate of sample, and 100 are arranged in this method；
Strengthen content (mg/kg)=(C of zirconium oxide in disperse platinum2-C0 /)×K×1.3509
In formula：
C2-- with the content of the element to be measured of the sample 2 of ICP measure, μ g/mL；
C0 /-- the content of the element to be measured of the reagent blank of sulfuric acid medium, μ g/mL are determined with ICP；
K-- represents the extension rate of sample, and 100 are arranged in the inventive method；
Simple substance zirconium is converted into the coefficient of zirconium oxide by 1.3509--.
Further, the step 1) is：Weigh and strengthen disperse platinum 0.5-2g, 20-40mL chloroazotic acid is added in beaker,
Cap upper surface ware, it is placed on electric hot plate and is dissolved with 120-180 DEG C of temperature.
Further, the step 3) is：The zirconium oxide that step 2) is filtered out is put into silica crucible together with filter paper,
The ashing of 700-800 DEG C of electric furnace is placed, then adds ammonium sulfate 0.5-2g and sulfuric acid 3-5mL in using 160-180 DEG C on electric hot plate
Temperature is dissolved；After cooling, liquid is moved into volumetric flask and is diluted to scale with pure water, as reinforcing disperse platinum to be measured
In zirconia content sample 2.
Further, step 5) the plasma emission spectrometer, first check that main frame is connected with computer before start
It is whether normal, confirm that cooling water is opened and is in normal condition, the unlatching of confirmation air compressor machine is simultaneously normal, and main frame is opened after all meeting.
Further, the instrument test condition of step 5) the plasma emission spectrometer is：It is it is determined that used
Purity of argon is >=99.99%, adjusts argon bottle pressure reducer to argon pressure in the range of 0.5-0.8MPa, and ensure in gas cylinder
Argon pressure is not less than 1MPa.
The beneficial effects of the invention are as follows：, can be fast by plasma emission spectrometer after the dissolving of disperse platinum will be strengthened
The fast Accurate Determining wherein content of simple substance zr element and zirconium oxide, the method increase test accuracy and analysis efficiency.
Embodiment
The method of testing of simple substance zr element and zirconia content comprises the steps of in the reinforcing disperse platinum of the present invention：
1) weigh and strengthen disperse platinum 0.5-2g (being accurate to 0.0001g), 20-40mL chloroazotic acid is added in 50mL beakers
(hydrochloric acid：Nitric acid=4：1), cap upper surface ware, it is placed on electric hot plate and is dissolved with 120-180 DEG C of temperature；
2) it is evaporated to after dissolving and closely does, adds 10-20 milliliter 1+1 hydrochloric acid to filter out undissolved zirconium oxide, filtrate is moved into
Scale is diluted in 100mL volumetric flasks and with pure water, the sample 1 as the simple substance zr element in reinforcing disperse platinum to be measured；
3) zirconium oxide that step 2) filters out is put into silica crucible together with filter paper, places 700-800 DEG C of ash of electric furnace
Change, then add ammonium sulfate 0.5-2g and sulfuric acid 3-5mL in being dissolved on electric hot plate with 160-180 DEG C of temperature；After cooling,
Liquid is moved into 100mL volumetric flasks and is diluted to scale with pure water, as the zirconia content in reinforcing disperse platinum to be measured
Sample 2；
4) standard curve is established
From the standard stock solution that Zr constituent contents are 1000ug/mL, it is 10 μ g/mL, 30 μ g/ that dilution, which is configured to content, step by step
ML, 100 μ g/mL standard liquid；
5) test
The signature analysis wavelength of selection zr element is respectively 343.823nm, 339.197nm, 257.139nm, and using etc.
Ionomer emission spectrum instrument, input step 4) in the number and standard value of standard liquid prepared, establish the mark of each impurity element
Directrix curve, on this basis test sample.The wherein value C of sample 11, the value C of sample 22, while acid is used according to sample dissolution
The reagent blank that difference obtains is respectively C0(chloroazotic acid medium) and C0 /(sulfuric acid medium), and tested according to same test condition
Reagent blank.
6) calculate
Strengthen content (mg/kg)=(C of metal zirconium in disperse platinum1-C0)×K
In formula：
C1-- with the content of the element to be measured of the sample 1 of ICP measure, μ g/mL；
C0-- the content of the element to be measured of the reagent blank of chloroazotic acid medium, μ g/mL are determined with ICP；
K-- represents the extension rate of sample, and 100 are arranged in this method.
Strengthen content (mg/kg)=(C of zirconium oxide in disperse platinum2-C0 /)×K×1.3509
In formula：
C2-- with the content of the element to be measured of the sample 2 of ICP measure, μ g/mL；
C0 /-- the content of the element to be measured of the reagent blank of sulfuric acid medium, μ g/mL are determined with ICP；
K-- represents the extension rate of sample, and 100 are arranged in the inventive method；
Simple substance zirconium is converted into the coefficient of zirconium oxide by 1.3509--.
Present invention test plasma emission spectrometer and instrument test condition：
Check that whether main frame is connected with computer normal, confirms that cooling water is opened and is in normal condition, confirms before start
Air compressor machine unlatching is simultaneously normal, and main frame is opened after all meeting.It is determined that used purity of argon is >=99.99%, argon bottle is adjusted
Pressure reducer in the range of 0.5-0.8MPa, and ensures that argon pressure is not less than 1MPa in gas cylinder to argon pressure.
Embodiment 1：
Weigh 0.5000 gram and strengthen disperse platinum sample (numbering MPt-1) in glass beaker, add chloroazotic acid 20mL (salt
Acid：Nitric acid=4：1), dissolved in 130 DEG C of temperature.It is evaporated to after dissolving and closely does, adds 10 milliliters of 1+1 hydrochloric acid to filter out not molten
The zirconium oxide of solution, filtrate is moved into 100mL volumetric flasks and is diluted to scale with pure water, as in reinforcing disperse platinum to be measured
The sample 1 of simple substance zr element, and according to the same terms reagent preparation blank C0；
The zirconium oxide filtered out is put into silica crucible together with filter paper, 700 DEG C of ashing of electric furnace is placed, then adds ammonium sulfate
0.5g, sulfuric acid 3mL on electric hot plate with 170 DEG C of temperature in being dissolved；After cooling, liquid is moved into 100mL volumetric flasks and is used in combination
Pure water is diluted to scale, as the sample 2 of the zirconia content in reinforcing disperse platinum to be measured, and prepares and tries according to the same terms
Agent blank C0 /。
Establish standard curve
From the standard stock solution that Zr constituent contents are 1000ug/mL, it is 10 μ g/mL, 30 μ g/ that dilution, which is configured to content, step by step
ML, 100 μ g/mL standard liquid.
Testing procedure
The signature analysis wavelength 343.823nm of zr element and the instrument test condition of table 1 are selected, inputs of standard liquid
Number and standard value, the standard curve of each impurity element is established, on this basis test sample.The wherein value C of sample 11, sample 2
Value C2, while and according to the same terms reagent preparation blank C0,C0 /。
Table 1
Calculate
Strengthen content (mg/kg)=(C of metal zirconium in disperse platinum1-C0)×K
In formula：C1-- with the content of the element to be measured of the sample 1 of ICP measure, μ g/mL；
C0-- with the content of the element to be measured of the reagent blank of ICP measure, μ g/mL；
K-- represents the extension rate of sample, is arranged to 100 in the method.
Strengthen content (mg/kg)=(C of zirconium oxide in disperse platinum2-C0 /)×K×1.3509
In formula：C2-- with the content of the element to be measured of the sample 2 of ICP measure, μ g/mL；
C0-- with the content of the element to be measured of the reagent blank of ICP measure, μ g/mL；
K-- represents the extension rate of sample, is arranged to 100 in the method；
1.3509-simple substance zirconium is converted into the coefficient of zirconium oxide.
By the result drawn compared with ratio, disperse time, anticorrosion effect etc., 2 are the results are shown in Table：
Table 2
Zirconia content in sample is switched to be added with simple substance zirconium content in sample after simple substance zirconium content, obtained result with
It is consistent with ratio.
Embodiment 2：
Weigh 1.0000 grams and strengthen disperse platinum sample (numbering MPt-2) in glass beaker, add chloroazotic acid 30mL (salt
Acid：Nitric acid=4：1), dissolved in 150 DEG C of temperature.It is evaporated to after dissolving and closely does, adds 15 milliliters of 1+1 hydrochloric acid to filter out not molten
The zirconium oxide of solution, filtrate is moved into 100mL volumetric flasks and is diluted to scale with pure water, as in reinforcing disperse platinum to be measured
The sample 1 of simple substance zr element, and according to the same terms reagent preparation blank C0；
The zirconium oxide filtered out is put into silica crucible together with filter paper, 750 DEG C of ashing of electric furnace is placed, then adds ammonium sulfate
1.0g, sulfuric acid 4mL on electric hot plate with 160 DEG C of temperature in being dissolved；After cooling, liquid is moved into 100mL volumetric flasks and is used in combination
Pure water is diluted to scale, as the sample 2 of the zirconia content in reinforcing disperse platinum to be measured, and prepares and tries according to the same terms
Agent blank C0 /。
Establish standard curve
From the standard stock solution that Zr constituent contents are 1000ug/mL, it is 10 μ g/mL, 30 μ g/ that dilution, which is configured to content, step by step
ML, 100 μ g/mL standard liquid.
Testing procedure
The signature analysis wavelength 339.197nm of zr element and the instrument test condition of table 1 are selected, inputs of standard liquid
Number and standard value, the standard curve of each impurity element is established, on this basis test sample.The wherein value C of sample 11, sample 2
Value C2, while test the reagent blank C of the same terms0,C0 /。
Calculate
Strengthen content (mg/kg)=(C of metal zirconium in disperse platinum1-C0)×K
In formula：C1-- with the content of the element to be measured of the sample 1 of ICP measure, μ g/mL；
C0-- with the content of the element to be measured of the reagent blank of ICP measure, μ g/mL；
K-- represents the extension rate of sample, is arranged to 100 in the method.
Strengthen content (mg/kg)=(C of zirconium oxide in disperse platinum2-C0 /)×K×1.3509
In formula：C2-- with the content of the element to be measured of the sample 2 of ICP measure, μ g/mL；
C0-- with the content of the element to be measured of the reagent blank of ICP measure, μ g/mL；
K-- represents the extension rate of sample, is arranged to 100 in the method；
1.3509-simple substance zirconium is converted into the coefficient of zirconium oxide.
By the result drawn compared with ratio, disperse time, anticorrosion effect etc., 3 are the results are shown in Table：
Table 3
Zirconia content in sample is switched to be added with simple substance zirconium content in sample after simple substance zirconium content, obtained result with
It is consistent with ratio.
Embodiment 3：
Weigh 2.0000 grams and strengthen disperse platinum sample (numbering MPt-3) in glass beaker, add chloroazotic acid 40mL (salt
Acid：Nitric acid=4：1), dissolved in 180 DEG C of temperature.It is evaporated to after dissolving and closely does, adds 20 milliliters of 1+1 hydrochloric acid to filter out not molten
The zirconium oxide of solution, filtrate is moved into 100mL volumetric flasks and is diluted to scale, as the simple substance zirconium in reinforcing disperse platinum to be measured
The sample 1 of element, and according to the same terms reagent preparation blank C0；
Zirconium oxide and filter paper are put into silica crucible, 800 DEG C of ashing of electric furnace is placed, then adds ammonium sulfate 2.0g, sulphur
Sour 5mL on electric hot plate with 180 DEG C of temperature in being dissolved；After cooling, liquid is moved into 100mL volumetric flasks and is diluted to quarter
Degree, as the sample 2 of the zirconia content in dispersion intensifying platinum to be measured, and according to the same terms reagent preparation blank C0 /。
Establish standard curve
From the standard stock solution that Zr constituent contents are 1000ug/mL, it is 10 μ g/mL, 30 μ g/ that dilution, which is configured to content, step by step
ML, 100 μ g/mL standard liquid.
Testing procedure
The signature analysis wavelength 257.139nm of zr element and the instrument test condition of table 1 are selected, inputs of standard liquid
Number and standard value, the standard curve of each impurity element is established, on this basis test sample.The wherein value C of sample 11, sample 2
Value C2, while test the reagent blank C of the same terms0,C0 /。
Calculate
Strengthen content (mg/kg)=(C of metal zirconium in disperse platinum1-C0)×100
In formula：C1-- with the content of the element to be measured of the sample 1 of ICP measure, μ g/mL；
C0-- with the content of the element to be measured of the reagent blank of ICP measure, μ g/mL；
K-- represents the extension rate of sample, is arranged to 100 in the method.
Strengthen content (mg/kg)=(C of zirconium oxide in disperse platinum2-C0 /)×K×1.3509
In formula：C2-- with the content of the element to be measured of the sample 2 of ICP measure, μ g/mL；
C0-- with the content of the element to be measured of the reagent blank of ICP measure, μ g/mL；
K-- represents the extension rate of sample, is arranged to 100 in the method.
1.3509-simple substance zirconium is converted into the coefficient of zirconium oxide.
By the result drawn compared with ratio, disperse time, anticorrosion effect etc., 4 are the results are shown in Table：
Table 4
Zirconia content in sample is switched to be added with simple substance zirconium content in sample after simple substance zirconium content, obtained result with
It is consistent with ratio.
As shown by data in above-described embodiment, test result of the present invention is consistent with initial ratio value, illustrates the survey of the present invention
The test result accurate and effective of method for testing.
According to the material that different technique is drawn process conditions and later stage using effect also with experimental test data kissing
Close, it was demonstrated that method of testing of the present invention is capable of the quality of correct judgement material.
Claims (5)
1. strengthen the measuring method of zirconium and zirconia content in disperse platinum, it is characterised in that the method includes the steps of：
1) weigh and strengthen disperse platinum 0.5-2g, add 20-40mL chloroazotic acid, dissolved in 120-180 DEG C of temperature；
2) it is evaporated to after dissolving and closely does, add 10-20 milliliter hydrochloric acid to filter out undissolved zirconium oxide, filtrate is moved into volumetric flask
And scale is diluted to pure water, the sample 1 as the simple substance zr element in reinforcing disperse platinum to be measured；
3) zirconium oxide that step 2) filters out is put into crucible together with filter paper, places electric furnace ashing, then add ammonium sulfate
0.5-2g and sulfuric acid 3-5mL, after dissolving and cooling down, liquid is moved into volumetric flask and with pure water is diluted to scale, as treating
Survey the sample 2 for strengthening the zirconia content in disperse platinum；
4) standard curve is established
From Zr constituent contents be 1000ug/mL standard stock solution, step by step dilution be configured to content for 10 μ g/mL, 30 μ g/mL,
100 μ g/mL standard liquid；
5) test
The signature analysis wavelength of selection zr element is respectively 343.823nm, 339.197nm, 257.139nm, using plasma
Emission spectrometer input step 4) in the number and standard value of standard liquid prepared, establish the standard curve of each impurity element,
The value C of test sample on this basis, wherein sample 11, the value C of sample 22, while obtained according to sample dissolution using the different of acid
To reagent blank be respectively C0And C0 /, and carry out test agent blank according to same test condition；
6) calculate
Strengthen content (mg/kg)=(C of metal zirconium in disperse platinum1-C0)×K
In formula：
C1-- with the content of the element to be measured of the sample 1 of ICP measure, μ g/mL；
C0-- the content of the element to be measured of the reagent blank of chloroazotic acid medium, μ g/mL are determined with ICP；
K-- represents the extension rate of sample, and 100 are arranged in this method；
Strengthen content (mg/kg)=(C of zirconium oxide in disperse platinum2-C0 /)×K×1.3509
In formula：
C2-- with the content of the element to be measured of the sample 2 of ICP measure, μ g/mL；
C0 /-- the content of the element to be measured of the reagent blank of sulfuric acid medium, μ g/mL are determined with ICP；
K-- represents the extension rate of sample, and 100 are arranged in this method；
Simple substance zirconium is converted into the coefficient of zirconium oxide by 1.3509--.
2. strengthen the measuring method of zirconium and zirconia content in disperse platinum as claimed in claim 1, it is characterised in that described
Step 1) is：Weigh and strengthen disperse platinum 0.5-2g, 20-40mL chloroazotic acid is added in beaker, cap upper surface ware, is placed on electric heating
Dissolved on plate with 120-180 DEG C of temperature.
3. strengthen the measuring method of zirconium and zirconia content in disperse platinum as claimed in claim 1, it is characterised in that described
Step 3) is：The zirconium oxide that step 2) is filtered out is put into silica crucible together with filter paper, places 700-800 DEG C of ash of electric furnace
Change, then add ammonium sulfate 0.5-2g and sulfuric acid 3-5mL in being dissolved on electric hot plate with 160-180 DEG C of temperature；After cooling,
Liquid is moved into volumetric flask and is diluted to scale with pure water, the sample as the zirconia content in reinforcing disperse platinum to be measured
2。
4. strengthen the measuring method of zirconium and zirconia content in disperse platinum as claimed in claim 1, it is characterised in that described
Step 5) plasma emission spectrometer, first check that whether main frame is connected with computer normal, confirms that cooling water is opened before start
Open and be in normal condition, the unlatching of confirmation air compressor machine is simultaneously normal, and main frame is opened after all meeting.
5. strengthen the measuring method of zirconium and zirconia content in disperse platinum as claimed in claim 1, it is characterised in that described
The instrument test condition of step 5) plasma emission spectrometer is：It is determined that used purity of argon is >=99.99%, adjust
Argon bottle pressure reducer is saved to argon pressure in the range of 0.5-0.8MPa, and ensures that argon pressure is not less than 1MPa in gas cylinder.
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| 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 |
| CN117092090A (en) * | 2023-07-12 | 2023-11-21 | 重庆材料研究院有限公司 | Method for measuring content of zirconium oxide in dispersion strengthening platinum-based material |
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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 |
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| 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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| 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 |
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