CN103543141B - The analytical approach of tin oxide electrode micro impurity element Fe and Cu - Google Patents
The analytical approach of tin oxide electrode micro impurity element Fe and Cu Download PDFInfo
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Abstract
The analytical approach of a kind of tin oxide electrode micro impurity element Fe and Cu, adopt ICP-AES, by sample preparation, experiment condition, standard solution preparation, drawing curve, test, calculating, obtain the percentage composition of micro impurity element Fe and Cu in tin oxide electrode, the present invention has the advantages that operation is easy, analysis speed is fast, measuring accuracy is high, meets the demand of micro impurity element Fe and Cu content in Measurement accuracy tin oxide electrode.
Description
Technical field
The present invention relates to the analytical approach of micro impurity element in a kind of material analysis measuring technology, particularly tin oxide electrode.
Background technology
Tin oxide electrode is a kind of ceramic semiconductor material, has the characteristics such as resistance to elevated temperatures is good, high-temperature resistivity is low, resistance to glass attack corrosive nature is good, and therefore Chang Zuowei electrode material is used for founding of special optical glass.In tin oxide electrode, micro impurity element Fe and Cu can have a strong impact on the absorption loss index of special optical glass.Therefore, the micro impurity element Fe in necessary strict controlled oxidization tin electrode and Cu content.
In high-purity tin oxide electrode, the content of impurity element is very low, generally in ppm magnitude, is difficult to adopt the method such as EDS, x-ray fluorescence method to carry out accurate analysis, therefore mainly adopts ICP-AES (ICP-OES).ICP-OES method is adopted to measure, first tin oxide electrode must be prepared into solution, the ceramic body that tin oxide electrode is particularly formed through high temperature sintering, its physicochemical characteristics and stannic oxide powder have very large difference, and quantitative test tin oxide electrode being carried out to trace impurity needs first to solve sample preparation problem.
In recent years, substantially do not have the relevant report of impurities analysis in tin oxide electrode.The document that can find is only that the analysis of impurity element in tin oxide raw material measures.Adopt 0.5g putty powder to add 2.5g potassium hydroxide with electric furnace calcining in nickel crucible in document, then use the acid-soluble sample of 1+1 salt, though this method is solvable to tin oxide material powder, then cannot dissolve completely for tin oxide electrode.In addition, the mensuration about impurity element in tin oxide electrode does not have concerned countries standard yet, does not have ready-made chemical analysis method, therefore, in the urgent need to setting up for the sample preparation of Analysis of Micro-amount Impurities In Liquid in tin oxide electrode and impurity method of testing.To ensure the quality of special optical glass, improve its quality.
The present invention adopts high-purity mixed base to be dissolved tin oxide electrode by high-temperature melting method, forms glass state material, dissolves afterwards, form supernatant liquid sample with acid to this glass.Adopt the content of Impurity Fe and Cu in ICP-OES method Accurate Determining tin oxide electrode afterwards.The method has and is easy to that operation, analysis speed are fast, measuring accuracy high, Fe and the Cu trace impurity of qualitative assessment tin oxide electrode, for the development of high-quality tin oxide electrode materials and the development of high-end special glass provide important foundation.
Summary of the invention
Technical matters to be solved by this invention is to provide the analytical approach of micro impurity element in a kind of tin oxide electrode.By the sample preparation to tin oxide electrode, fusing sample adopts the kind of reagent, the selection of consumption and method, solves tin oxide electrode not diffluent problem in acid or alkali.The interference problem in test is solved by the experiment condition choose reasonable of ICP-OES and wavelength chooses.According to described method, quantitative measurement is carried out to the content of micro impurity element Fe and Cu in tin oxide electrode, analyze quick, simple to operate, measuring accuracy is high, error at measurment meets the error requirements of traditional conventional method of analysis.
Technical solution of the present invention is:
An analytical approach of tin oxide electrode micro impurity element Fe and Cu, feature is that the concrete steps of the method are:
1. sample preparation: first need to carry out crushing grinding to tin oxide electrode, particulate samples acquisition of sieving is not more than 10 object particulate samples, uses analytical balance accurately to take 0.2000g ~ 2.0000g sample particle; Take 1.0000g ~ 5.0000gNaOH and 0.2000g ~ 1.0000gKOH mixing; Ground tin oxide electrode powder is placed in platinum crucible, at 850 DEG C ~ 950 DEG C pre-burning 10 ~ 30min; Take out crucible, NaOH and KOH potpourri is poured in crucible, put into muffle furnace 850 DEG C ~ 950 DEG C insulation 15 ~ 45min; Taking-up is cooled to room temperature; Be placed in the leaching of beaker warm water, platinum crucible is taken out; In beaker, add 6 ~ 18ml hydrochloric acid, 2 ~ 6ml nitric acid, heating for dissolving is clarified; Be cooled to room temperature, in constant volume 100ml volumetric flask, form sample solution; With step blank solutions such as sample do.
2. experiment condition: the technical parameter of inductive coupling plasma emission spectrograph is set to: radio-frequency generator power: 1150 ~ 1500W; Nebulizer pressure: 18 ~ 30PSI; Sample introduction pump speed: 1.0 ~ 3.0ml/min; Integral time: 5 ~ 15s.Select Fe and Cu optimized analysis line wavelength.
3. working curve standard solution preparation: by Fe and Cu standard mixing storing solution (5 μ g/ml), accurately pipette 0ml, 5ml, 10ml, 20ml standard mixed liquor respectively in 100ml volumetric flask, the sour mixed liquor of hydrochloric acid and nitric acid is added in each volumetric flask, the composition of added sour mixed liquor and quantity and step 1. in hydrochloric acid and nitric acid sour blended liquid phase together, use high purity water constant volume, shake up the standard solution of Fe and the Cu hybrid standard working curve of rear formation variable concentrations;
4. drawing curve: the line strength measuring Fe and Cu mixed standard solution with inductance Coupled Plasma-Atomic emission spectrometer respectively, with the concentration of Fe and Cu for horizontal ordinate, line strength is ordinate, draws out the working curve of Fe and Cu standard solution;
5. test: by step 1. described in sample solution and blank solution be connected to the sampling system of inductive coupling plasma emission spectrograph, start test software programs, the standard working curve of the intensity of emission spectra of solution to be measured and optimized analysis spectral line is analyzed, according to the corresponding optimized analysis line wavelength of selection, obtain the concentration ρ of Fe and Cu in sample solution and blank solution respectively
1and ρ
0(μ g/ml).
6. calculate: calculate Fe and Cu content w respectively by following formula:
In formula:
ρ
1--Fe and Cu measured value (μ g/ml) in sample solution;
ρ
0--Fe and Cu measured value (μ g/ml) in blank sample solution;
The numerical value of V--sample solution volume, unit is milliliter (ml);
M--sample quality numerical value, unit is gram (g).
Described whole chemical reagent are top grade purity, and pure water used is 18.2 mega-ohms ultrapure waters.
Described Fe and Cu optimized analysis line wavelength is chosen as Fe:259.9nm; Cu:324.7nm.
The linear coefficient of described standard working curve is more than 0.99, and the working curve recorded is effective working curve.
Difficult point of the present invention and know-why:
Difficult point of the present invention is the sample preparation of tin oxide electrode.Know-why is: adopt mixed base high-temperature melting method to make tin oxide electrode be melt into glassy state.With acid, the glass containing tin oxide is dissolved afterwards, obtain Analysis of Micro-amount Impurities In Liquid sample.
For tin oxide electrode, first it is considered that acid-soluble, but no matter use which kind of acid, all cannot thoroughly be dissolved; The melting reagent of alkali fusion has sodium carbonate, NaOH, potassium hydroxide etc.With sodium carbonate fusion, after acid adding, sample cannot all dissolve; Use NaOH melting, solubilize clarification after acid adding, but this method corrodes to platinum crucible serious, economic loss is very large; Even and if add excessive hydrogen kali with potassium hydroxide melting, sample also cannot be made after acid adding to dissolve completely.Therefore reasonable sample treatment is selected to seem particularly important.
The ceramic body that tin oxide electrode is particularly formed through high temperature sintering, the reactivity of crystal grain is low, is not easily dissolved.For increasing the reactivity of crystal grain, first sample is adopted crushing grinding, sample sieves to acquire and is not more than 10 object particulate samples; Secondly particulate samples is taked the measure of high temperature pre-burning, and held for some time increases its crystal grain activity.Because NaOH melt oxidation tin electrode sample corrodes excessive to platinum crucible.Present invention employs NaOH and the potassium hydroxide mixed melting sample of rational proportion, the method that the present invention selects and condition, both ensure that sample can be melted completely, and the loss of platinum crucible can have been made to drop to again minimum, met the sample preparation needs that in tin oxide electrode, micro impurity element is analyzed.
Advantageous Effects of the present invention:
The means that the sample preparation that the present invention establishes mixed base melt oxidation tin electrode combines with inductive coupling plasma emission spectrograph Analysis of Micro-amount Impurities In Liquid, define the method for trace impurity Fe and Cu in a kind of quick, accurate and effective mensuration tin oxide electrode.This method overcomes the not diffluent problem of tin oxide electrode, and trace impurity Fe and Cu constituent content in energy Accurate Determining tin oxide electrode, the relative deviation of its measurement result is less than 10%.Measurement result can effectively apply to tin oxide electrode quality judging, the harm that qualitative assessment tin oxide electrode impurity content and impurity may cause special optical glass smelting.To the quality improving tin oxide electrode and special optical glass, there is significant application value.
Embodiment
Below by embodiment, the present invention is further elaborated, but should limit the scope of the invention with this.
Embodiment 1:
In tin oxide electrode of the present invention, micro impurity element Fe and Cu analytical approach comprise sample preparation, experiment condition, standard solution preparation, drawing curve, test, calculating, and the concrete steps of the method are:
1, sample preparation: get stannic oxide electrode sample at random, carries out crushing grinding, and particulate samples is not more than 10 object particulate samples through acquisition of sieving, and uses analytical balance accurately to take 0.3845g sample particle; Take 1.2050gNaOH and 0.5032gKOH mixing; Ground tin oxide electrode powder is placed in platinum crucible, at 850 DEG C of pre-burning 30min; Take out crucible, NaOH and KOH potpourri is poured in crucible, put into muffle furnace 900 DEG C insulation 30min; Taking-up is cooled to room temperature; Be placed in the leaching of beaker warm water, platinum crucible is taken out; In beaker, add 15ml hydrochloric acid, 5ml nitric acid, heating for dissolving is clarified; Be cooled to room temperature, in constant volume 100ml volumetric flask, form sample solution; With step blank solutions such as sample do.
2, experiment condition: the technical parameter of inductive coupling plasma emission spectrograph is set to: radio-frequency generator power: 1150W; Nebulizer pressure: 22PSI; Sample introduction pump speed: 1.8ml/min; Integral time: 5s.Fe and Cu optimized analysis line wavelength is selected to be respectively 259.9nm and 324.7nm.
3, working curve standard solution preparation: by Fe and Cu standard mixing storing solution (5 μ g/ml), accurately pipette 0ml, 5ml, 10ml, 20ml standard mixed liquor respectively in 100ml volumetric flask, the sour mixed liquor of hydrochloric acid and nitric acid is added in each volumetric flask, the sour blended liquid phase of the composition of added sour mixed liquor and quantity and hydrochloric acid in step 1 and nitric acid together, use high purity water constant volume, shake up the standard solution of Fe and the Cu hybrid standard working curve of rear formation variable concentrations.
4, drawing curve: the line strength measuring Fe and Cu mixed standard solution with inductance Coupled Plasma-Atomic emission spectrometer respectively, with the concentration of Fe and Cu for horizontal ordinate, line strength is ordinate, draws out the working curve of Fe and Cu standard solution.
5, test: the sampling system sample solution described in step 1 and blank solution being connected to inductive coupling plasma emission spectrograph, start test software programs, the standard working curve of the intensity of emission spectra of solution to be measured and optimized analysis spectral line is analyzed, according to the corresponding optimized analysis line wavelength of selection, obtain the concentration ρ of Fe and Cu in sample solution and blank solution respectively
1and ρ
0(μ g/ml), duplicate measurements 3 times.
6, calculate: calculate Fe and Cu content w respectively by following formula:
In formula:
ρ
1--Fe and Cu measured value (μ g/ml) in sample solution;
ρ
0--Fe and Cu measured value (μ g/ml) in blank sample solution;
The numerical value of V--sample solution volume, unit is milliliter (ml);
M--sample quality numerical value, unit is gram (g);
7, analysis result is in table 1.
Fe and Cu analysis result in table 1 tin oxide electrode
| Impurity element | Mean value % | RSD/％ | The recovery/% |
| Fe | 0.0065 | 4.3 | 101.5 |
| Cu | 0.0026 | 6.2 | 97.4 |
The RSD<7% of sample measurement; The recovery, between 90% ~ 105%, meets to analyze and detects needs.
Embodiment 2
The standard solution preparation of the present embodiment, drawing curve, Measurement and Computation are identical with example one, sample preparation and experiment condition different, as follows:
1, sample preparation: get stannic oxide electrode sample at random, carries out crushing grinding, and particulate samples is not more than 10 object particulate samples through acquisition of sieving, and uses analytical balance accurately to take 0.5238g sample particle; Take 1.8640gNaOH and 0.6730gKOH mixing; Ground tin oxide electrode powder is placed in platinum crucible, at 950 DEG C of pre-burning 20min; Take out crucible, NaOH and KOH potpourri is poured in crucible, put into muffle furnace 950 DEG C insulation 45min; Taking-up is cooled to room temperature; Be placed in the leaching of beaker warm water, platinum crucible is taken out; In beaker, add 21ml hydrochloric acid, 7ml nitric acid, heating for dissolving is clarified; Be cooled to room temperature, in constant volume 100ml volumetric flask, form sample solution; With step blank solutions such as sample do.
2, experiment condition: the technical parameter of inductive coupling plasma emission spectrograph is set to:
Radio-frequency generator power: 1500W; Nebulizer pressure: 28PSI; Sample introduction pump speed: 3.0ml/min; Integral time: 5s.Fe and Cu optimized analysis line wavelength is selected to be respectively 259.9nm and 324.7nm.
Test result is in table 2.
Fe and Cu analysis result in table 2 tin oxide electrode
| Impurity element | Mean value/% | RSD/％ | The recovery/% |
| Fe | 0.0079 | 2.5 | 95.6 |
| Cu | 0.00385. | 1 | 96.2 |
The RSD<6% of sample measurement; The recovery, between 90% ~ 100%, meets to analyze and detects needs.
Claims (4)
1. an analytical approach of tin oxide electrode micro impurity element Fe and Cu, is characterised in that the concrete steps of the method are:
1. sample preparation: because tin oxide electrode is the dense ceramic body that stannic oxide powder becomes through high temperature sintering: first need to carry out crushing grinding to tin oxide electrode, particulate samples acquisition of sieving is not more than 10 object particulate samples, uses analytical balance accurately to take 0.2000g ~ 2.0000g sample particle; Take 1.0000g ~ 5.0000gNaOH and 0.2000g ~ 1.0000gKOH mixing; Ground tin oxide electrode powder is placed in platinum crucible, at 850 DEG C ~ 950 DEG C pre-burning 10 ~ 30min; Take out crucible, NaOH and KOH potpourri is poured in crucible, put into muffle furnace 850 DEG C ~ 950 DEG C insulation 15 ~ 45min; Taking-up is cooled to room temperature; Be placed in the leaching of beaker warm water, platinum crucible is taken out; In beaker, add 6 ~ 18ml hydrochloric acid, 2 ~ 6ml nitric acid, heating for dissolving is clarified; Be cooled to room temperature, in constant volume 100ml volumetric flask, form sample solution; With step blank solutions such as sample do;
2. experiment condition: the technical parameter of inductive coupling plasma emission spectrograph is set to: radio-frequency generator power: 1150 ~ 1500W; Nebulizer pressure: 18 ~ 30PSI; Sample introduction pump speed: 1.0 ~ 3.0ml/min; Integral time: 5 ~ 15s; Select Fe and Cu optimized analysis line wavelength;
3. working curve standard solution preparation: from 5 μ g/ml Fe and Cu standard mixing storing solution, accurately pipette 0ml, 5ml, 10ml, 20ml standard mixed liquor respectively in 100ml volumetric flask, the sour mixed liquor of hydrochloric acid and nitric acid is added in each volumetric flask, the composition of added sour mixed liquor and quantity and step 1. in hydrochloric acid and nitric acid sour blended liquid phase together, use high purity water constant volume, shake up the standard solution of Fe and the Cu hybrid standard working curve of rear formation variable concentrations;
4. drawing curve: the line strength measuring Fe and Cu mixed standard solution with inductance Coupled Plasma-Atomic emission spectrometer respectively, with the concentration of Fe and Cu for horizontal ordinate, line strength is ordinate, draws out the working curve of Fe and Cu standard solution;
5. test: by step 1. described in sample solution and blank solution be connected to the sampling system of inductive coupling plasma emission spectrograph, start test software programs, the standard working curve of the intensity of emission spectra of solution to be measured and optimized analysis spectral line is analyzed, according to the corresponding optimized analysis line wavelength of selection, obtain the concentration ρ of Fe and Cu in sample solution and blank solution respectively
1and ρ
0;
6. calculate: calculate Fe and Cu content w respectively by following formula:
In formula:
ρ
1--Fe and Cu measured value in sample solution, unit is μ g/ml;
ρ
0--Fe and Cu measured value in blank sample solution, unit is μ g/ml;
The numerical value of V--sample solution volume, unit is milliliter;
M--sample quality numerical value, unit is gram.
2. the analytical approach of micro impurity element Fe and Cu in tin oxide electrode according to claim 1, it is characterized in that described whole chemical reagent are top grade purity, pure water used is 18.2 mega-ohms ultrapure waters.
3. the analytical approach of micro impurity element Fe and Cu in tin oxide electrode according to claim 1, is characterized in that described Fe and Cu optimized analysis line wavelength is chosen as Fe:259.9nm; Cu:324.7nm.
4. the analytical approach of micro impurity element Fe and Cu in tin oxide electrode according to claim 1, it is characterized in that the linear coefficient of described standard working curve is more than 0.99, the working curve recorded is effective working curve.
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| CN106404482A (en) * | 2016-08-31 | 2017-02-15 | 大工（青岛）新能源材料技术研究院有限公司 | Pretreatment method for detection of silicon and aluminum contents in ceramics |
| CN110455598A (en) * | 2019-09-02 | 2019-11-15 | 蚌埠中光电科技有限公司 | The sample treatment of impurity in a kind of detection stannic oxide |
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