CN103234967A - Measuring method of zirconium content in high-purity niobium oxide or tantalum oxide - Google Patents
Measuring method of zirconium content in high-purity niobium oxide or tantalum oxide Download PDFInfo
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Abstract
The invention discloses a measuring method of zirconium content in high-purity niobium oxide or tantalum oxide. The method comprises the following steps: melting a sample, leaching a trace of zirconium and co-precipitating the zirconium and iron, washing precipitates, masking interfering elements, developing colors, and measuring absorbance. According to the measuring method, potassium hydroxide and potassium carbonate melts of columbium oxide and/or tantalum oxide is utilized, when leaching is carried out with water, soluble potassium niobate or potassium tantalate is obtained; and in an alkaline solution, a small amount of iron is taken as a vector, zirconium precipitates are completely separated from the potassium niobate or potassium tantalate solution, ferrozirconium precipitates are then dissolved with hydrochloric acid, and the zirconium content is measured by using an arsenazo III colorimetry. The measuring method is simple in operation, the metal zirconium can be separated without being interfered by metal ions such as niobium and tantalum, and the measuring result of the zirconium content is high in precision.
Description
Technical field
The present invention relates to metal material field, be specifically related to zirconium Determination on content method in a kind of high purity niobium oxide or the tantalum oxide.
Background technology
High purity niobium oxide, tantalum oxide are produced capacitor as raw material, and the product of optical glass is subjected to the influence of end product, and market is more and more higher to the purity requirement of niobium oxide, tantalum oxide.Yet the analytical approach research at impurity element in high purity niobium oxide, the tantalum oxide is less.Although the instrumental analysis of recent years development rapidly, as the analysis of impurity content in ICP-OES mensuration niobium oxide, the tantalum oxide, but because some element is subjected to the limitation of instrumental analysis sensitivity, and the restriction of standard substance, Sensitivity of Analytical Method is relatively poor, and the result precision of mensuration is bad.Most of medium-sized and small enterprises also lack and acquire these expensive analytical instrument in addition.
The chemical stability of niobium oxide, tantalum oxide is good especially, does not only react with air, water, can also resist hydrofluorite all mineral acids in addition, comprises the erosion of chloroazotic acid.Be soluble in the acid mixture of nitric acid and hydrofluorite, but after removing hydrofluorite, be easy to be hydrolyzed into niobic acid and tantalic acid precipitation, zirconium ion is adsorbed on niobic acid and the tantalic acid precipitation, and niobium tantalum zirconium is separated not exclusively.
Summary of the invention
Goal of the invention: the object of the invention is to provide zirconium Determination on content method in a kind of high purity niobium oxide or the tantalum oxide.This method is utilized potassium hydroxide and the sal tartari fused mass of niobium oxide or tantalum oxide, when using water extraction, obtains potassium niobate or the potassium tantalate of solubility, in alkaline solution, is carrier with a spot of iron again, and the zirconium precipitation is separated with potassium niobate or potassium tantalate solution.The ferrozirconium precipitation is used dissolving with hydrochloric acid again, utilizes the arsenazo colourimetry, measures zirconium content.
Technical scheme: technical scheme of the present invention is as follows: zirconium Determination on content method in a kind of high purity niobium oxide or the tantalum oxide said method comprising the steps of:
1) molten sample: obtain niobium oxide or tantalum oxide fused mass with 4-6g potassium hydroxide and 2-3g sal tartari fusion high purity niobium oxide or tantalum oxide sample in high temperature furnace;
2) leaching: leach above-mentioned niobium oxide or the tantalum oxide fused mass obtains leaching liquid with 80-90 ℃ of hot water;
3) trace zirconium and iron co-precipitation: in above-mentioned leaching liquid, add ferric ion solutions, make zirconium and iron co-precipitation;
4) washing precipitation: be after the potassium hydroxide solution of 20g/l washs above-mentioned co-precipitation 3-5 time with massfraction, add massfraction again and be the ammonium nitrate solution washing precipitation 2 times of 10g/l, obtain the ferrozirconium precipitation of hydroxide;
5) shelter interference element: with the above-mentioned ferrozirconium post precipitation of dissolving with hydrochloric acid of 4.5mol/l, add tartaric acid solution and superoxol, heating is boiled to emitting air pocket, cooling, move in the 100ml volumetric flask, be diluted to scale with 4.5mol/l hydrochloric acid and obtain mixed solution;
6) colour developing: draw above-mentioned mixed solution, fully react and obtain solution more than the 10min to wherein adding concentrated hydrochloric acid, ethanol and arsenazo;
7) an above-mentioned solution part is poured in the cuvette, added 5 of 200g/l ammonium fluoride solutions in the surplus solution as reference liquid, measure light absorption value.
8) utilize the zirconium standard solution to carry out standard curve making;
9) utilize the light absorption value measured in the step 7) by checking in the amount of zirconium on the above-mentioned typical curve, utilize formula to calculate zirconium content.
High-temperature fusion temperature in the described step 1) is 650-700 ℃.
Described step 2) hot water volume 80ml in, potassium concentration is 1mol/l-2mol/l in the leaching liquid.
The iron ion content of ferric ion solutions is 2mg/ml in the described step 3).
The potassium hydroxide solution addition is 5-10ml in the described step 4), and the ammonium nitrate solution addition is 3-5ml.
Described step 5) mesotartaric acid solution addition is 10ml, and massfraction is 200g/l, and it is 30% superoxol that dropping 7-8 drips massfraction.
Amount of alcohol added is 20ml in the described step 6), and 10g/l arsenazo addition is 2.5ml.
In the described step 7) on spectrophotometer wavelength be that the 665nm place measures light absorption value.
Beneficial effect: compared with prior art, advantage of the present invention is as follows: this assay method utilizes potassium hydroxide and the sal tartari fused mass of niobium oxide or tantalum oxide, when using water extraction, obtaining potassium niobate or the potassium tantalate of solubility, in alkaline solution, is carrier with a spot of iron again, the zirconium precipitation is separated fully with potassium niobate or potassium tantalate solution, the ferrozirconium precipitation is used dissolving with hydrochloric acid again, utilizes the arsenazo colourimetry, measures zirconium content.This assay method is simple to operate, can make metal zirconium not be subjected to the interference of metallic ions such as niobium, tantalum and separates zirconium Determination on content result precision height.
Description of drawings
Fig. 1 is the canonical plotting in the embodiment of the invention 1.
Embodiment
According to specific embodiment, further set forth the present invention below.
1, the reagent of using in this experiment: in the analysis, unless otherwise indicated, only use analytical reagent and distilled water.
1.1 potassium hydroxide solid
1.2 potash solid
1.3 ferric ion solutions: 2.0mg/ml
Take by weighing the 1.00g pure iron, add 20ml nitric acid (1+1), heating for dissolving, cooling is diluted with water to 500ml
1.4 potassium hydroxide solution 20g/l
1.5 ammonium nitrate solution: 10g/l
1.6 hydrochloric acid: 4.5mol/L
1.7 tartaric acid solution: 200g/l
1.8 superoxol: 30%
1.9 ammonium fluoride solution: 200g/l
1.10 arsenazo solution: 10g/l
1.11 zirconium standard solution: 2 μ g/ml
Accurately take by weighing 0.3533 gram chloride zirconium acyl in the 300ml beaker, add 10% hydrochloric acid 20ml, the low-grade fever dissolving moves into solution in 1 liter of volumetric flask, is diluted to scale with 4.5mol/L hydrochloric acid, shakes up.This zirconium standard reserving solution concentration is 100 μ g/ml.
Pipette the above-mentioned standard inventory solution of 10.00ml before the use in the 500ml volumetric flask, be diluted to scale with 4.5mol/L hydrochloric acid, mixing.This concentration of standard solution is 2 μ g/ml.
2, operation steps
Take by weighing 1.0g high purity niobium oxide tantalum oxide potpourri sample (being accurate to 0.0001g) in nickel crucible, do blank assay in company with sample, add 4g sal tartari and 4g potassium hydroxide, add a cover, in high temperature furnace, melt to transparent in 650 ℃, take off cooling, in the 250ml beaker, be heated to 90 ℃ with 80ml boiling water leaching frit, adding 2.5ml concentration is the 2.0mg/ml ferric ion solutions, abundant stirring is filtered with middling speed filter paper, washs beaker and precipitates 3-5 time with the 20g/l potassium hydroxide solution, again with 10g/l ammonium nitrate solution washing secondary, 4.5mol/l dissolving with hydrochloric acid with heat is deposited in the former beaker, adds the tartaric acid solution that 10ml concentration is 200g/l, drips 7-8 and drips hydrogen peroxide, heating is boiled to emitting air pocket, cooling moves in the 100ml volumetric flask, is diluted to scale with 4.5mol/l hydrochloric acid.
Draw 10ml solution in the 50ml volumetric flask, add the 16ml concentrated hydrochloric acid, add 20ml ethanol, 2.5ml arsenazo solution, be diluted with water to scale, shake up, behind the placement 10min, above-mentioned solution is poured in the cuvette of 3cm, 5 of ammonium fluoride solutions that in surplus solution, add 200g/l, as reference liquid, at 665nm wavelength place, measure its absorbance with this.
3, standard curve making
Divide and get 0,0.5,1.00,2.00,3.00,4.00,5.00ml zirconium standard solution (2 μ g/ml) in one group of 50ml volumetric flask, is added 10ml respectively with 4.5mol/L hydrochloric acid, adds the 16ml concentrated hydrochloric acid, add 20ml ethanol, 2.5ml arsenazo solution is diluted with water to scale, shakes up, after placing 10min, above-mentioned solution is poured in the cuvette of 3cm, in surplus solution, is added 5 of ammonium fluorides, with this as reference liquid, at 665nm wavelength place, measure its absorbance, and the production standard curve, as shown in Figure 1, that wherein horizontal ordinate is represented among the figure is zirconium amount (μ g), and ordinate is expressed as light absorption value.
4, interpretation of result and discussion
4.1 sample weighting amount
Middle zirconium (Zr) content is selected different sample weighting amounts per sample.When sample weighting amount during greater than 2.00g, the sample fusion sometimes not exclusively, have insolubles during leaching.So generally be not more than 2.00g when selecting sample weighting amount, select 1.0g at this.
4.2 the selection of optimal wavelength
Testing under the different wave length of 600-700nm respectively by above-mentioned experimental technique, record the maximum absorption wavelength of complex compound at 665nm, is that the zirconium of 4 μ g carries out colorimetric below under the different wave length condition.
Table 1
| λ | 600 | 640 | 650 | 660 | 665 | 670 | 680 | 700 |
| A | 0.010 | 0.025 | 0.07 | 0.119 | 0.130 | 0.121 | 0.068 | 0.022 |
4.3 mark-on recovery test
Accurately take by weighing high purity niobium oxide 1.0000g4 part identical in quality, carry out the fusion leaching by operation steps, before the ferric ion solutions that adds 2.0mg/ml, add 2 μ g/ml zirconium standard solution of different amounts respectively, continue to analyze by operation steps.Be that reference carries out colorimetric with the sample that does not add the zirconium standard solution.Result such as table 2:
Table 2
The result shows that in standard curve range, the recovery of zirconium (Zr) satisfies analyzes requirement.
4.4 the calculating of analysis result zirconium content
In the formula: the zirconium amount that m1-----checks in from the typical curve (see figure 1), μ g
V---test solution cumulative volume, ml
The v1---branch is got test solution volume, ml
The m----sample size, g
Embodiment 1:
Zirconic mensuration in the high purity niobium oxide, carry out according to following steps:
1) molten sample: the high purity niobium oxide sample of 700 ℃ of following fusion 1.0045g in high temperature furnace obtains fused mass with 4g potassium hydroxide and 3g sal tartari;
2) leaching: leach above-mentioned fused mass with 90 ℃ of hot water 80ml and obtain leaching liquid, potassium concentration is 1mol/l in the leaching liquid;
3) trace zirconium and iron co-precipitation: in above-mentioned leaching liquid, add the ferric ion solutions that iron ion content is 2mg/ml, make zirconium and iron co-precipitation;
4) washing precipitation: after washing above-mentioned co-precipitation 3-5 time with the potassium hydroxide solution of the 20g/l of 10ml, add the ammonium nitrate solution washing precipitation 2 times of the 10g/l of 3ml again, obtain the ferrozirconium precipitation of hydroxide;
5) shelter interference element: with the above-mentioned ferrozirconium post precipitation of dissolving with hydrochloric acid of 4.5mol/l, the 200g/l tartaric acid solution that adds 10ml, it is 30% superoxol that dropping 7-8 drips massfraction, heating is boiled to emitting air pocket, cooling, move in the 100ml volumetric flask, be diluted to scale with 4.5mol/l hydrochloric acid and obtain mixed solution;
6) colour developing: draw above-mentioned mixed solution, fully react and obtain solution more than the 10min to wherein adding concentrated hydrochloric acid, 20ml ethanol and 2.5ml arsenazo;
7) an above-mentioned solution part is poured in the cuvette, added 5 of 200g/l ammonium fluoride solutions in the surplus solution as reference liquid, wavelength is 665nm place mensuration light absorption value on spectrophotometer.
8) utilize the zirconium standard solution to carry out standard curve making;
9) utilize the light absorption value measured in the step 7) by checking in the amount of zirconium on the above-mentioned typical curve, utilize formula to calculate zirconium content.
Embodiment 2
Zirconic mensuration in the high purity niobium oxide, carry out according to following steps:
1) molten sample: the high purity niobium oxide sample of 650 ℃ of following fusion 1.0023g in high temperature furnace obtains fused mass with 6g potassium hydroxide and 2g sal tartari;
2) leaching: leach above-mentioned fused mass with 80 ℃ of hot water 80ml and obtain leaching liquid, potassium concentration is 2mol/l in the leaching liquid;
3) trace zirconium and iron co-precipitation: in above-mentioned leaching liquid, add the ferric ion solutions that iron ion content is 2mg/ml, make zirconium and iron co-precipitation;
4) washing precipitation: after washing above-mentioned co-precipitation 3-5 time with the potassium hydroxide solution of the 20g/l of 5ml, add the ammonium nitrate solution washing precipitation 2 times of the 10g/l of 5ml again, obtain the ferrozirconium precipitation of hydroxide;
5) shelter interference element: with the above-mentioned ferrozirconium post precipitation of dissolving with hydrochloric acid of 4.5mol/l, the 200g/l tartaric acid solution that adds 10ml, it is 30% superoxol that dropping 7-8 drips massfraction, heating is boiled to emitting air pocket, cooling, move in the 100ml volumetric flask, be diluted to scale with 4.5mol/l hydrochloric acid and obtain mixed solution;
6) colour developing: draw above-mentioned mixed solution, fully react and obtain solution more than the 10min to wherein adding concentrated hydrochloric acid, 20ml ethanol and 2.5ml arsenazo;
7) an above-mentioned solution part is poured in the cuvette, added 5 of 200g/l ammonium fluoride solutions in the surplus solution as reference liquid, wavelength is 665nm place mensuration light absorption value on spectrophotometer.
8) utilize the zirconium standard solution to carry out standard curve making;
9) utilize the light absorption value measured in the step 7) by checking in the amount of zirconium on the above-mentioned typical curve, utilize formula to calculate zirconium content.
Embodiment 3
Zirconic mensuration in the high purity tantalum oxide, carry out according to following steps:
1) molten sample: the high purity tantalum oxide sample of 675 ℃ of following fusion 1.0068g in high temperature furnace obtains fused mass with 5g potassium hydroxide and 2.5g sal tartari;
2) leaching: leach above-mentioned fused mass with 85 ℃ of hot water 80ml and obtain leaching liquid, potassium concentration is 1.5mol/l in the leaching liquid;
3) trace zirconium and iron co-precipitation: in above-mentioned leaching liquid, add the ferric ion solutions that iron ion content is 2mg/ml, make zirconium and iron co-precipitation;
4) washing precipitation: after washing above-mentioned co-precipitation 3-5 time with the potassium hydroxide solution of the 20g/l of 7.5ml, add the ammonium nitrate solution washing precipitation 2 times of the 10g/l of 4ml again, obtain the ferrozirconium precipitation of hydroxide;
5) shelter interference element: with the above-mentioned ferrozirconium post precipitation of dissolving with hydrochloric acid of 4.5mol/l, the 200g/l tartaric acid solution that adds 10ml, it is 30% superoxol that dropping 7-8 drips massfraction, heating is boiled to emitting air pocket, cooling, move in the 100ml volumetric flask, be diluted to scale with 4.5mol/l hydrochloric acid and obtain mixed solution;
6) colour developing: draw above-mentioned mixed solution, fully react and obtain solution more than the 10min to wherein adding concentrated hydrochloric acid, 20ml ethanol and 2.5ml arsenazo;
7) an above-mentioned solution part is poured in the cuvette, added 5 of 200g/l ammonium fluoride solutions in the surplus solution as reference liquid, wavelength is 665nm place mensuration light absorption value on spectrophotometer.
8) utilize the zirconium standard solution to carry out standard curve making;
9) utilize the light absorption value measured in the step 7) by checking in the amount of zirconium on the above-mentioned typical curve, utilize formula to calculate zirconium content.
Embodiment 4
Zirconic mensuration in the high purity tantalum oxide, carry out according to following steps:
1) molten sample: the high purity tantalum oxide sample of 675 ℃ of following fusion 1.0068g in high temperature furnace obtains fused mass with 5g potassium hydroxide and 2.5g sal tartari;
2) leaching: leach above-mentioned fused mass with 85 ℃ of hot water 80ml and obtain leaching liquid, potassium concentration is 1.5mol/l in the leaching liquid;
3) trace zirconium and iron co-precipitation: in above-mentioned leaching liquid, add the ferric ion solutions that iron ion content is 2mg/ml, make zirconium and iron co-precipitation;
4) washing precipitation: after washing above-mentioned co-precipitation 3-5 time with the potassium hydroxide solution of the 20g/l of 7.5ml, add the ammonium nitrate solution washing precipitation 2 times of the 10g/l of 4ml again, obtain the ferrozirconium precipitation of hydroxide;
5) shelter interference element: with the above-mentioned ferrozirconium post precipitation of dissolving with hydrochloric acid of 4.5mol/l, the 200g/l tartaric acid solution that adds 10ml, it is 30% superoxol that dropping 7-8 drips massfraction, heating is boiled to emitting air pocket, cooling, move in the 100ml volumetric flask, be diluted to scale with 4.5mol/l hydrochloric acid and obtain mixed solution;
6) colour developing: draw above-mentioned mixed solution, fully react and obtain solution more than the 10min to wherein adding concentrated hydrochloric acid, 20ml ethanol and 2.5ml arsenazo;
7) an above-mentioned solution part is poured in the cuvette, added 5 of 200g/l ammonium fluoride solutions in the surplus solution as reference liquid, wavelength is 665nm place mensuration light absorption value on spectrophotometer.
8) utilize the zirconium standard solution to carry out standard curve making;
9) utilize the light absorption value measured in the step 7) by checking in the amount of zirconium on the above-mentioned typical curve, utilize formula to calculate zirconium content.
Specifically about the computational data of the zirconium content of above-mentioned 1-4 embodiment referring to table 3, wherein v/v1 is 10:1.
Table 3
The above only is preferred implementation of the present invention; be noted that for those skilled in the art; under the prerequisite that does not break away from the principle of the invention, can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (8)
1. zirconium Determination on content method in a high purity niobium oxide or the tantalum oxide is characterized in that said method comprising the steps of:
1) molten sample: obtain niobium oxide or tantalum oxide fused mass with 4-6g potassium hydroxide and 2-3g sal tartari fusion high purity niobium oxide or tantalum oxide sample in high temperature furnace;
2) leaching: leach above-mentioned niobium oxide or the tantalum oxide fused mass obtains leaching liquid with 80-90 ℃ of hot water;
3) trace zirconium and iron co-precipitation: in above-mentioned leaching liquid, add ferric ion solutions, make zirconium and iron co-precipitation;
4) washing precipitation: be after the potassium hydroxide solution of 20g/l washs above-mentioned co-precipitation 3-5 time with massfraction, add massfraction again and be the ammonium nitrate solution washing precipitation 2 times of 10g/l, obtain the ferrozirconium precipitation of hydroxide;
5) shelter interference element: with the above-mentioned ferrozirconium post precipitation of dissolving with hydrochloric acid of 4.5mol/l, add tartaric acid solution and superoxol, heating is boiled to emitting air pocket, cooling, move in the 100ml volumetric flask, be diluted to scale with 4.5mol/l hydrochloric acid and obtain mixed solution;
6) colour developing: draw above-mentioned mixed solution, fully react and obtain solution more than the 10min to wherein adding concentrated hydrochloric acid, ethanol and arsenazo;
7) an above-mentioned solution part is poured in the cuvette, added 5 of 200g/l ammonium fluoride solutions in the surplus solution as reference liquid, measure absorbance;
8) utilize the zirconium standard solution to carry out standard curve making;
9) utilize the light absorption value measured in the step 7) by checking in the amount of zirconium on the above-mentioned typical curve, utilize formula to calculate zirconium content.
2. according to zirconium Determination on content method in the described high purity niobium oxide of claim 1 or the tantalum oxide, it is characterized in that: the high-temperature fusion temperature in the described step 1) is 650-700 ℃.
3. according to zirconium Determination on content method in the described high purity niobium oxide of claim 1 or the tantalum oxide, it is characterized in that: hot water volume 80ml described step 2), potassium concentration is 1mol/l-2mol/l in the leaching liquid.
4. according to zirconium Determination on content method in the described high purity niobium oxide of claim 1 or the tantalum oxide, it is characterized in that: the iron ion content of ferric ion solutions is 2mg/ml in the described step 3).
5. according to zirconium Determination on content method in the described high purity niobium oxide of claim 1 or the tantalum oxide, it is characterized in that: the potassium hydroxide solution addition is 5-10ml in the described step 4), and the ammonium nitrate solution addition is 3-5ml.
6. according to zirconium Determination on content method in the described high purity niobium oxide of claim 1 or the tantalum oxide, it is characterized in that: described step 5) mesotartaric acid solution addition is 10ml, and massfraction is 200g/l, and it is 30% superoxol that dropping 7-8 drips massfraction.
7. according to zirconium Determination on content method in the described high purity niobium oxide of claim 1 or the tantalum oxide, it is characterized in that: amount of alcohol added is 20ml in the described step 6), and 10g/l arsenazo addition is 2.5ml.
8. according to zirconium Determination on content method in the described high purity niobium oxide of claim 1 or the tantalum oxide, it is characterized in that: in the described step 7) on spectrophotometer wavelength be that the 665nm place measures light absorption value.
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| CN111413168A (en) * | 2020-03-20 | 2020-07-14 | 合肥国轩高科动力能源有限公司 | Method for testing zirconia in zirconia-coated nickel-cobalt-manganese ternary positive electrode material |
| CN111413168B (en) * | 2020-03-20 | 2022-03-11 | 合肥国轩高科动力能源有限公司 | Method for testing zirconia in zirconia-coated nickel-cobalt-manganese ternary positive electrode material |
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Application publication date: 20130807 |