CN104062280A - Method for determining content of six impurity elements of manganese, phosphorus, arsenic, lead, zinc and copper in permanent magnetic ferrite mixed materials - Google Patents
Method for determining content of six impurity elements of manganese, phosphorus, arsenic, lead, zinc and copper in permanent magnetic ferrite mixed materials Download PDFInfo
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Abstract
The invention provides a method for determining the content of six impurity elements of manganese, phosphorus, arsenic, lead, zinc and copper in permanent magnetic ferrite mixed materials. According to the method, a to-be-determined sample is added into concentrated hydrochloric acid and concentrated nitric acid and is dissolved at the low temperature, the sample is in a volumetric flask in a constant-volume mode, and the sample, the concentrated hydrochloric acid and the concentrated nitric acid are shaken up for determining. Prepared manganese, phosphorus, arsenic, lead, zinc and copper standard solutions are used for making a manganese, phosphorus, arsenic, lead, zinc and copper spectral line intensity-mass fraction working curve on a plasma atomic emission spectrometer, the curve is used for analyzing the to-be-determined sample, and the content of the manganese, the phosphorus, the arsenic, the lead, the zinc and the copper in the permanent magnetic ferrite mixed materials is obtained. According to the method, operation is convenient and rapid, the analysis cost is low, the determining result has the good stability, reproducibility and accuracy, and the determining requirements for the impurity elements of the manganese, the phosphorus, the arsenic, the lead, the zinc and the copper in the daily permanent magnetic ferrite mixed materials can be met. According to the analysis method, adopted chemical reagents are few, the pollution to the environment is small, the analysis cost is low, the multiple elements can be determined at the same time, the analysis efficiency is improved, and labor intensity of analysis and operation personnel is reduced.
Description
Technical field
The invention belongs to test chemical technical field, be specifically related in a kind of permanent-magnet ferrite batch mixing the assay method of 6 kinds of impurity element manganese, phosphorus, arsenic, lead, zinc, copper content.
Background technology
At present, the permanent magnet industry of China is when preparing permanent-magnet ferrite, and the primary raw material of use is iron oxide, the carbonate of baric, strontium, calcium.Wherein iron oxide has three kinds of source-fine ores, iron scale, iron oxide red.The chemical composition of these materials is not exclusively all di-iron trioxide, also contain a small amount of impurity element, such as manganese, phosphorus, arsenic, lead, zinc, copper etc., these chemical compositions can affect the magnetic of permanent magnet, and the content of these impurity elements must analyzing and testing also be controlled in permanent magnet production run.
Now domestic national standard and the industry standard of measuring impurity element manganese, phosphorus, arsenic, lead, zinc, copper content in permanent-magnet ferrite batch mixing of also not formulating.Adopt these impurity contents of spectrphotometric method for measuring in chemical method, every kind of element will adopt different analyzing detecting methods, use a large amount of chemical reagent, analytical procedure is loaded down with trivial details, running time is long, bring very large trouble to the measurement of permanent magnet composition, not only can pollute border, and the injury of the chemical reagent producing to operating personnel.Therefore the assay method of, developing manganese, phosphorus, arsenic, lead, zinc, copper content in a kind of permanent-magnet ferrite batch mixing is rapidly and efficiently necessary.
Summary of the invention
The object of the present invention is to provide in a kind of permanent-magnet ferrite batch mixing the assay method of 6 kinds of impurity element manganese, phosphorus, arsenic, lead, zinc, copper content.
The object of the present invention is achieved like this, comprises that preparation, the preparation of mark liquid, the test comparison of sample pretreating, stock solution analyzed four steps, and its process is as follows:
A, sample pretreating
(1), in sample to be tested, add the concentrated hydrochloric acid of 10mL, 70 ~ 90 ℃ of heating for dissolving 10 ~ 20min;
(2), the red fuming nitric acid (RFNA) that adds sample to be tested 5mL in the sample of step (1) is to dissolving completely, is cooled to 20 ~ 30 ℃;
(3), the solution distilled water constant volume of step (2), shake up.
The preparation of B, stock solution
(1), take that 0.1000g cleans and dried electrolytic manganese, be placed in the beaker of 250ml, add the nitric acid of 20ml concentration 17.5% to dissolve, boil and drive most oxides of nitrogen, be cooled to 20 ~ 30 ℃, move in the volumetric flask of 1000ml, be diluted with water to scale, mix.Obtain the stock solution of manganese element.This solution 1ml is containing 100 μ g manganese.To this solution numbering A.
(2), by mass concentration 0.4393g/L, get potassium dihydrogen phosphate and water, potassium dihydrogen phosphate is placed in to beaker, water dissolves, the preparation P elements concentration stock solution identical with manganese element concentration in A solution.To this solution numbering B.
(3), by mass concentration 0.1320g/L, get benchmark arsenic trioxide and water, benchmark arsenic trioxide is placed in to beaker, with red fuming nitric acid (RFNA), dissolves, the preparation arsenic element concentration stock solution identical with manganese element concentration in A solution.To this solution numbering C.
(4), by mass concentration 5g/L, get pure lead and concentration nitric acid, pure lead is placed in to beaker, with nitric acid dissolve, the preparation lead element concentration stock solution identical with manganese element concentration in A solution.To this solution numbering D.
(5), by mass concentration 4.15g/L, get benchmark zinc paste and hydrochloric acid, take 0.1245 g benchmark zinc paste, with dissolving with hydrochloric acid, the preparation zinc concentration of element stock solution identical with manganese element concentration in A solution.To this solution numbering E.
(6), by mass concentration 3.33g/L, get metallic copper and hydrochloric acid, metallic copper is placed in to beaker, with dissolving with hydrochloric acid, the preparation copper concentration stock solution identical with manganese element concentration in A solution.To this solution numbering F.
The preparation of C, mark liquid
(1), in 6 100mL volumetric flasks, add respectively 10mL concentrated hydrochloric acid, 5 mL red fuming nitric acid (RFNA) dissolution in low temperature are to volume 2mL, cooling, add 10mL distilled water.
(2), in 6 parts of solution of step (1) gained, add respectively 0mL, 0.50mL, 1.00mL, 2.00mL, 3.00mL, A, the B in 4.00mL step B, C, D, E, F standard inventory solution, add distilled water constant volume to shake up.
D, test comparison analysis
With the manganese preparing, phosphorus, arsenic, lead, zinc, copper standard solution, on plasma atomic emission spectrometer, make manganese, phosphorus, arsenic, lead, zinc, copper line strength-massfraction working curve, with this tracing analysis sample to be tested, obtain manganese in permanent magnet, phosphorus, arsenic, lead, zinc, copper content.
The present invention adopts the manganese, phosphorus, arsenic, lead, zinc, the copper standard solution that prepare on plasma atomic emission spectrometer, to make manganese, phosphorus, arsenic, lead, zinc, copper line strength-massfraction working curve, with this tracing analysis sample to be tested, obtain manganese in permanent magnet, phosphorus, arsenic, lead, zinc, copper content.The chemical reagent that the analytical approach that the present invention uses is used is less, and environmental pollution is little, and analysis cost is low.The analytical approach that the present invention uses, can multielement simultaneous determination, and easy to operate, analysis speed is fast, has shortened analytical cycle, has improved analysis efficiency, has alleviated analysis operation personnel's labour intensity.Adopt method of the present invention to measure manganese, phosphorus, arsenic, lead, zinc, copper content in permanent magnet oxygen, its measurement result has good stability, reappearance and accuracy.Evidence the inventive method is reliable, practical, can meet the mensuration needs of manganese in daily permanent magnet, phosphorus, arsenic, lead, zinc, copper content.
Accompanying drawing explanation
Fig. 1 is the invention process step;
Fig. 2 is manganese line strength-massfraction figure;
Fig. 3 is phosphorus line strength-massfraction figure;
Fig. 4 is arsenic line strength-massfraction figure;
Fig. 5 is plumbous line strength-massfraction figure;
Fig. 6 is zinc line strength-massfraction figure;
Fig. 7 is copper line strength-massfraction figure.
Embodiment
Below in conjunction with embodiment, the present invention is further illustrated, but never in any form the present invention is limited, and any change or the improvement based on training centre of the present invention, done, all belong to protection scope of the present invention.
The preparation, the preparation of mark liquid, the test comparison that the present invention includes sample pretreating, stock solution are analyzed four steps, and its process is as follows:
A, sample pretreating
(1), in sample to be tested, add the concentrated hydrochloric acid of 10mL, 70 ~ 90 ℃ of heating for dissolving 10 ~ 20min of low temperature;
(2), the red fuming nitric acid (RFNA) that adds sample to be tested 5mL in the sample of step (1) is to dissolving completely, is cooled to 20 ~ 30 ℃;
(3), the solution distilled water constant volume of step (2), shake up.
The preparation of B, stock solution
(6), take that 0.1000g cleans and dried electrolytic manganese, be placed in the beaker of 250ml, add the nitric acid of 20ml concentration 17.5% to dissolve, boil and drive most oxides of nitrogen, be cooled to 20 ~ 30 ℃, move in the volumetric flask of 1000ml, be diluted with water to scale, mix.Obtain the stock solution of manganese element.This solution 1ml is containing 100 μ g manganese.To this solution numbering A.
(7), by mass concentration 0.4393g/L, get potassium dihydrogen phosphate and water, potassium dihydrogen phosphate is placed in to beaker, water dissolves, the preparation P elements concentration stock solution identical with manganese element concentration in A solution.To this solution numbering B.
(8), by mass concentration 0.1320g/L, get benchmark arsenic trioxide and water, benchmark arsenic trioxide is placed in to beaker, with red fuming nitric acid (RFNA), dissolves, the preparation arsenic element concentration stock solution identical with manganese element concentration in A solution.To this solution numbering C.
(9), by mass concentration 5g/L, get pure lead and concentration nitric acid, pure lead is placed in to beaker, with nitric acid dissolve, the preparation lead element concentration stock solution identical with manganese element concentration in A solution.To this solution numbering D.
(10), by mass concentration 4.15g/L, get benchmark zinc paste and hydrochloric acid, take 0.1245 g benchmark zinc paste, with dissolving with hydrochloric acid, the preparation zinc concentration of element stock solution identical with manganese element concentration in A solution.To this solution numbering E.
(6), by mass concentration 3.33g/L, get metallic copper and hydrochloric acid, metallic copper is placed in to beaker, with dissolving with hydrochloric acid, the preparation copper concentration stock solution identical with manganese element concentration in A solution.To this solution numbering F.
The preparation of C, mark liquid
(1), in 6 100mL volumetric flasks, add respectively 10mL concentrated hydrochloric acid, 5 mL red fuming nitric acid (RFNA) dissolution in low temperature are to volume 2mL, cooling, add 10mL distilled water.
(2), in 6 parts of solution of step (1) gained, add respectively 0mL, 0.50mL, 1.00mL, 2.00mL, 3.00mL, A, the B in 4.00mL step B, C, D, E, F standard inventory solution, add distilled water constant volume to shake up.
D, test comparison analysis
With the manganese preparing, phosphorus, arsenic, lead, zinc, copper standard solution, on plasma atomic emission spectrometer, make manganese, phosphorus, arsenic, lead, zinc, copper line strength-massfraction working curve, with this tracing analysis sample to be tested, obtain manganese in permanent magnet, phosphorus, arsenic, lead, zinc, copper content.
The purity of electrolytic manganese is more than 99.9%.
Described potassium dihydrogen phosphate in advance with 100 ℃ ~ 110 ℃ bakings to constant and be stored in exsiccator.
Described plumbous purity is more than 99.9%.
Described zinc paste in advance prior to 900 ℃ ~ 1100 ℃ calcinations to constant cooling in exsiccator.
Described metallic copper purity is more than 99.9%.
The hydrochloric acid using when described zinc element stock solution or the preparation of copper stock solution is concentration 19% analytical reagent, and water is secondary deionized water.
The analytical reagent that the nitric acid that described lead element stock solution preparation or sample to be tested are used while processing is concentration 39%, water is secondary deionized water.
Embodiment 1
In permanent-magnet ferrite batch mixing sample to be tested, add 70 ℃ of about 10min of heating for dissolving of 10mL concentrated hydrochloric acid; In the sample of gained, add 5mL red fuming nitric acid (RFNA), continue to add and dissolve completely, be cooled to 20 ℃; Resulting solution is settled to 100 mL with distilled water, shakes up.
Taking 0.1000g cleans and dried electrolytic manganese (more than 99.9%), be placed in 250mL beaker, the nitric acid that adds 20mL concentration 17.5% dissolves, boil and drive most oxides of nitrogen, take off and be cooled to 20 ℃, move in 1000mL volumetric flask, be diluted with water to scale, mix, be numbered a, this solution 1mL is containing 100 μ g manganese.Take 0.4393g and prior to 100 ℃ of bakings, to constant the potassium dihydrogen phosphate that is stored in exsiccator, be dissolved in suitable quantity of water in advance, move in 1000mL volumetric flask, be diluted with water to scale, mix, be numbered b, this solution 1mL is containing 100 μ g phosphorus.Take 0.1320g benchmark arsenic trioxide in 100mL beaker, slowly add the about 10mL of nitric acid of concentration 39%, dissolve, add concentrated sulphuric acid 2mL, slowly heating, most of nitric acid is removed in evaporation, and high temperature emits sulfuric acid cigarette, take off slightly coldly, with water, rinse wall of cup and table ware, heating is smoldered again, take off slightly coldly, add about 10mL water, heating for dissolving salt, Deng all, after dissolving, take off, be cooled to 20 ℃, move in 1000mL volumetric flask, be diluted with water to scale, be numbered c, this solution 1mL is containing 100 μ g arsenic.Take the pure lead of 0.1000g (99.99%), be placed in 200mL beaker, add the nitric acid dissolve of 20mL concentration 39%, boil and remove oxides of nitrogen, be cooled to 20 ℃, move in 1000mL volumetric flask, be diluted with water to scale, mix, be numbered d, this solution 1mL is plumbous containing 100 μ g.Take 0.1245g in advance prior to 900 ℃ of calcinations to constant and in exsiccator cooling benchmark zinc paste, be dissolved in the hydrochloric acid of 30mL concentration 19% dilute with water, move in 1000mL volumetric flask, be diluted with water to scale, mix, be numbered e, this solution 1mL is containing 100 μ g zinc.Take 0.1000g metallic copper (more than 99.9%) in 250mL beaker, the hydrochloric acid that adds 30mL concentration 19% covers table ware, dissolves, and boils and removes oxides of nitrogen, take off and be cooled to 20 ℃, move in 1000mL volumetric flask, be diluted with water to scale, mix, be numbered f, this solution 1mL is containing 100 μ g copper.
In 6 100mL volumetric flasks, add respectively 10mL concentrated hydrochloric acid, 5mL red fuming nitric acid (RFNA), dissolution in low temperature is to the about 2mL of volume, takes off coolingly, adds 10mL distilled water.In 6 parts of solution of gained, add respectively a, b, c, d, e, the f stock solution 0mL of above-mentioned gained, 0.50mL, 1.00mL, 2.00mL, 3.00mL, 4.00mL, adds distilled water constant volume to shake up.
With the manganese preparing, phosphorus, arsenic, lead, zinc, copper standard solution, on plasma atomic emission spectrometer, make manganese, phosphorus, arsenic, lead, zinc, copper line strength-massfraction working curve, the condition of work of instrument is as shown in table 1, with this tracing analysis sample to be tested, the percentage composition that obtains manganese in permanent magnet, phosphorus, arsenic, lead, zinc, copper is respectively 0.47%, 0.012%, 0.010%, 0.011%, 0.013%, 0.032%.
Line strength-massfraction figure of manganese, phosphorus, arsenic, lead, zinc, copper is shown in Fig. 2, Fig. 3, Fig. 4, Fig. 5, Fig. 6, Fig. 7.
Table 1 instrument condition of work
| Power (W) | Atomizing pressure (psi) | Assisted gas flow (L/min) | Pump speed (rpm) | Integral time (s) |
| 1150 | 26.08 | 0.5 | 130 | 15 |
Table 2 element wavelength to be measured and progression
| Element | Wavelength (nm) | Progression |
| Mn | 279.482 | 120 |
| P | 213.618 | 458 |
| As | 193.759 | 474 |
| Pb | 216.999 | 455 |
| Zn | 206.200 | 463 |
| Cu | 327.396 | 103 |
Embodiment 2
In permanent-magnet ferrite batch mixing sample to be tested, add 10mL concentrated hydrochloric acid, 80 ℃ of about 15min of heating for dissolving; In the sample of gained, add 5mL red fuming nitric acid (RFNA), continue to add and dissolve completely, be cooled to 25 ℃; The solution of step B is settled to 100 mL with distilled water, shakes up.
Taking 0.1000g cleans and dried electrolytic manganese (more than 99.9%), be placed in 250mL beaker, the nitric acid that adds 20mL concentration 17.5% dissolves, boil and drive most oxides of nitrogen, take off and be cooled to 25 ℃, move in 1000mL volumetric flask, be diluted with water to scale, mix, be numbered a, this solution 1mL is containing 100 μ g manganese.Take 0.4393g and prior to 105 ℃ of bakings, to constant the potassium dihydrogen phosphate that is stored in exsiccator, be dissolved in suitable quantity of water in advance, move in 1000mL volumetric flask, be diluted with water to scale, mix, be numbered b, this solution 1mL is containing 100 μ g phosphorus.Take 0.1320g benchmark arsenic trioxide in 100mL beaker, slowly add the about 10mL of nitric acid of concentration 39%, heating for dissolving, adds concentrated sulphuric acid 2mL, slowly heating, most of nitric acid is removed in evaporation, and high temperature emits sulfuric acid cigarette, take off slightly coldly, with water, rinse wall of cup and table ware, heating is smoldered again, take off slightly coldly, add about 10mL water, heating for dissolving salt, Deng all, after dissolving, take off, be cooled to 25 ℃, move in 1000mL volumetric flask, be diluted with water to scale, be numbered c, this solution 1mL is containing 100 μ g arsenic.Take the pure lead of 0.1000g (99.99%), be placed in 200mL beaker, add the nitric acid dissolve of 20mL concentration 39%, boil and remove oxides of nitrogen, be cooled to 25 ℃, move in 1000mL volumetric flask, be diluted with water to scale, mix, be numbered d, this solution 1mL is plumbous containing 100 μ g.Take 0.1245g in advance prior to 1000 ℃ of calcinations to constant and in exsiccator cooling benchmark zinc paste, be dissolved in the hydrochloric acid of 30mL concentration 19% dilute with water, move in 1000mL volumetric flask, be diluted with water to scale, mix, be numbered e, this solution 1mL is containing 100 μ g zinc.Take 0.1000g metallic copper (more than 99.9%) in 250mL beaker, add the dissolving with hydrochloric acid of 30mL concentration 19%, boil and remove oxides of nitrogen, take off and be cooled to 25 ℃, move in 1000mL volumetric flask, be diluted with water to scale, mix, be numbered f, this solution 1mL is containing 100 μ g copper.
In 6 100mL volumetric flasks, add respectively 10mL concentrated hydrochloric acid, 5mL red fuming nitric acid (RFNA), dissolution in low temperature is to the about 5mL of volume, takes off coolingly, adds 10mL distilled water.In 6 parts of solution of gained, add respectively a, b, c, d, e, the f stock solution 0mL of above-mentioned gained, 0.50mL, 1.00mL, 2.00mL, 3.00mL, 4.00mL, adds distilled water constant volume to shake up.
With the manganese preparing, phosphorus, arsenic, lead, zinc, copper standard solution, on plasma atomic emission spectrometer, make manganese, phosphorus, arsenic, lead, zinc, copper line strength-massfraction working curve, the condition of work of instrument is as shown in table 1, with this tracing analysis sample to be tested, the percentage composition that obtains manganese in permanent magnet, phosphorus, arsenic, lead, zinc, copper is respectively 0.47%, 0.012%, 0.010%, 0.011%, 0.013%, 0.032%.
Embodiment 3
In permanent-magnet ferrite batch mixing sample to be tested, add 10mL concentrated hydrochloric acid, 90 ℃ of about 20min of heating for dissolving; In the sample of gained, add 5mL red fuming nitric acid (RFNA), continue to add and dissolve completely, be cooled to 30 ℃; The solution of step B is settled to 100 mL with distilled water, shakes up.
Taking 0.1000g cleans and dried electrolytic manganese (more than 99.9%), be placed in 250mL beaker, the nitric acid that adds 20mL concentration 17.5% dissolves, boil and drive most oxides of nitrogen, take off and be cooled to 30 ℃, move in 1000mL volumetric flask, be diluted with water to scale, mix, be numbered a, this solution 1mL is containing 100 μ g manganese.Take 0.4393g and prior to 110 ℃ of bakings, to constant the potassium dihydrogen phosphate that is stored in exsiccator, be dissolved in suitable quantity of water in advance, move in 1000mL volumetric flask, be diluted with water to scale, mix, be numbered b, this solution 1mL is containing 100 μ g phosphorus.Take 0.1320g benchmark arsenic trioxide in 100mL beaker, slowly add the about 10mL of nitric acid of concentration 39%, heating for dissolving, adds concentrated sulphuric acid 2mL, slowly heating, most of nitric acid is removed in evaporation, and high temperature emits sulfuric acid cigarette, take off slightly coldly, with water, rinse wall of cup and table ware, heating is smoldered again, take off slightly coldly, add about 10mL water, heating for dissolving salt, Deng all, after dissolving, take off, be cooled to 30 ℃, move in 1000mL volumetric flask, be diluted with water to scale, be numbered c, this solution 1mL is containing 100 μ g arsenic.Take the pure lead of 0.1000g (99.99%), be placed in 200mL beaker, add the nitric acid dissolve of 20mL concentration 39%, boil and remove oxides of nitrogen, be cooled to 30 ℃, move in 1000mL volumetric flask, be diluted with water to scale, mix, be numbered d, this solution 1mL is plumbous containing 100 μ g.Take 0.1245g in advance prior to 1100 ℃ of calcinations to constant and in exsiccator cooling benchmark zinc paste, be dissolved in the hydrochloric acid of 30mL concentration 19% dilute with water, move in 1000mL volumetric flask, be diluted with water to scale, mix, be numbered e, this solution 1mL is containing 100 μ g zinc.Take 0.1000g metallic copper (more than 99.9%) in 250mL beaker, add the dissolving with hydrochloric acid of 30mL concentration 19%, boil and remove oxides of nitrogen, take off and be cooled to 30 ℃, move in 1000mL volumetric flask, be diluted with water to scale, mix, be numbered f, this solution 1mL is containing 100 μ g copper.
In 6 100mL volumetric flasks, add respectively 10mL concentrated hydrochloric acid, 5mL red fuming nitric acid (RFNA), dissolution in low temperature is to the about 5mL of volume, takes off coolingly, adds 10mL distilled water.In 6 parts of solution of gained, add respectively a, b, c, d, e, the f stock solution 0mL of above-mentioned gained, 0.50mL, 1.00mL, 2.00mL, 3.00mL, 4.00mL, adds distilled water constant volume to shake up.
With the manganese preparing, phosphorus, arsenic, lead, zinc, copper standard solution, on plasma atomic emission spectrometer, make manganese, phosphorus, arsenic, lead, zinc, copper line strength-massfraction working curve, the condition of work of instrument is as shown in table 1, with this tracing analysis sample to be tested, the percentage composition that obtains manganese in permanent magnet, phosphorus, arsenic, lead, zinc, copper is respectively 0.47%, 0.012%, 0.010%, 0.011%, 0.013%, 0.032%.
Claims (8)
1. the assay method of 6 kinds of impurity element manganese, phosphorus, arsenic, lead, zinc, copper content in a permanent-magnet ferrite batch mixing, it is characterized in that: the preparation, the preparation of mark liquid, the test comparison that comprise sample pretreating, stock solution are analyzed four steps, and its process is as follows:
A, sample pretreating
(1), in sample to be tested, add the concentrated hydrochloric acid of 10mL, 70 ~ 90 ℃ of heating for dissolving 10 ~ 20min of low temperature;
(2), the red fuming nitric acid (RFNA) that adds sample to be tested 5mL in the sample of step (1) is to dissolving completely, is cooled to 20 ~ 30 ℃;
(3), the solution distilled water constant volume of step (2), shake up;
The preparation of B, stock solution
(1), take that 0.1000g cleans and dried electrolytic manganese, be placed in the beaker of 250ml, add the nitric acid of 20ml concentration 17.5% to dissolve, boil and drive most oxides of nitrogen, be cooled to 20 ~ 30 ℃, move in the volumetric flask of 1000ml, be diluted with water to scale, mix; Obtain the stock solution of manganese element;
(1)
2.this solution 1ml is containing 100 μ g manganese;
(1)
3.to this solution numbering A;
(2), by mass concentration 0.4393g/L, get potassium dihydrogen phosphate and water, potassium dihydrogen phosphate is placed in to beaker, water dissolves, the preparation P elements concentration stock solution identical with manganese element concentration in A solution;
(2)
4.to this solution numbering B;
(3), by mass concentration 0.1320g/L, get benchmark arsenic trioxide and water, benchmark arsenic trioxide is placed in to beaker, with red fuming nitric acid (RFNA), dissolves, the preparation arsenic element concentration stock solution identical with manganese element concentration in A solution;
(3)
5.to this solution numbering C;
(4), by mass concentration 5g/L, get pure lead and concentration nitric acid, pure lead is placed in to beaker, with nitric acid dissolve, the preparation lead element concentration stock solution identical with manganese element concentration in A solution;
(4)
6.to this solution numbering D;
(5), by mass concentration 4.15g/L, get benchmark zinc paste and hydrochloric acid, take 0.1245 g benchmark zinc paste, with dissolving with hydrochloric acid, the preparation zinc concentration of element stock solution identical with manganese element concentration in A solution;
(5)
7.to this solution numbering E;
(6), by mass concentration 3.33g/L, get metallic copper and hydrochloric acid, metallic copper is placed in to beaker, with dissolving with hydrochloric acid, the preparation copper concentration stock solution identical with manganese element concentration in A solution;
To this solution numbering F;
The preparation of C, mark liquid
(1), in 6 100mL volumetric flasks, add respectively 10mL concentrated hydrochloric acid, 5 mL red fuming nitric acid (RFNA) dissolution in low temperature are to volume 2mL, cooling, add 10mL distilled water;
(2), in 6 parts of solution of step (1) gained, add respectively 0mL, 0.50mL, 1.00mL, 2.00mL, 3.00mL, A, the B in 4.00mL step B, C, D, E, F standard inventory solution, add distilled water constant volume to shake up;
D, test comparison analysis
With the manganese preparing, phosphorus, arsenic, lead, zinc, copper standard solution, on plasma atomic emission spectrometer, make manganese, phosphorus, arsenic, lead, zinc, copper line strength-massfraction working curve, with this tracing analysis sample to be tested, obtain manganese in permanent magnet, phosphorus, arsenic, lead, zinc, copper content.
2. the assay method of 6 kinds of impurity element manganese, phosphorus, arsenic, lead, zinc, copper content in magnetic ferrites batch mixing according to claim 1, is characterized in that: the purity of electrolytic manganese is more than 99.9%.
3. the assay method of 6 kinds of impurity element manganese, phosphorus, arsenic, lead, zinc, copper content in permanent-magnet ferrite batch mixing according to claim 1, is characterized in that: described potassium dihydrogen phosphate in advance with 100 ℃ ~ 110 ℃ bakings to constant and be stored in exsiccator.
4. the assay method of 6 kinds of impurity element manganese, phosphorus, arsenic, lead, zinc, copper content in permanent-magnet ferrite batch mixing according to claim 1, is characterized in that: described plumbous purity is more than 99.9%.
5. the assay method of 6 kinds of impurity element manganese, phosphorus, arsenic, lead, zinc, copper content in permanent-magnet ferrite batch mixing according to claim 1, is characterized in that: described zinc paste in advance prior to 900 ℃ ~ 1100 ℃ calcinations to constant cooling in exsiccator.
6. the assay method of 6 kinds of impurity element manganese, phosphorus, arsenic, lead, zinc, copper content in permanent-magnet ferrite batch mixing according to claim 1, is characterized in that: described metallic copper purity is more than 99.9%.
7. the assay method of 6 kinds of impurity element manganese, phosphorus, arsenic, lead, zinc, copper content in permanent-magnet ferrite batch mixing according to claim 1, it is characterized in that: the hydrochloric acid using when described zinc element stock solution or the preparation of copper stock solution is concentration 19% analytical reagent, and water is secondary deionized water.
8. the assay method of 6 kinds of impurity element manganese, phosphorus, arsenic, lead, zinc, copper content in permanent-magnet ferrite batch mixing according to claim 1, it is characterized in that: the analytical reagent that the nitric acid that described lead element stock solution is used while preparing is concentration 39%, water is secondary deionized water.
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| CN113433115A (en) * | 2021-06-07 | 2021-09-24 | 武钢集团昆明钢铁股份有限公司 | Method for measuring lead and zinc content in direct reduced iron |
| CN114199858A (en) * | 2021-12-09 | 2022-03-18 | 湖南柿竹园有色金属有限责任公司 | Method for continuously measuring sulfur, iron, manganese, arsenic and calcium in tungsten concentrate sample and multi-metal geological sample |
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| CN114199858A (en) * | 2021-12-09 | 2022-03-18 | 湖南柿竹园有色金属有限责任公司 | Method for continuously measuring sulfur, iron, manganese, arsenic and calcium in tungsten concentrate sample and multi-metal geological sample |
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