CN103115916B - A kind of method measuring content of niobium in ferrocolumbium - Google Patents
A kind of method measuring content of niobium in ferrocolumbium Download PDFInfo
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- CN103115916B CN103115916B CN201310029484.8A CN201310029484A CN103115916B CN 103115916 B CN103115916 B CN 103115916B CN 201310029484 A CN201310029484 A CN 201310029484A CN 103115916 B CN103115916 B CN 103115916B
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Abstract
The invention discloses a kind of method measuring content of niobium in ferrocolumbium, comprising: dissolve ferrocolumbium sample, the form that the niobium in ferrocolumbium precipitates with niobium pentaoxide is precipitated out, weigh the quality of described niobium pentaoxide precipitation; Ferrocolumbium sample is utilized CSM 04 10 41 01-2001 ferro-niobium-content of niobium mensuration-tannin hydrolysis gravimetric method, obtain niobium pentaoxide secondary precipitate; Preparation niobium pentaoxide precipitation solution, preparing standard solution, described standard solution comprises titanium standard solution and tantalum standard solution; The solution dissolving niobium pentaoxide precipitation is introduced inductively coupled plasma atomic emission spectrometer, measure line strength of titanium and tantalum, according to line strength that the described standard solution of concentration known records, draw the content of titanium and tantalum in described niobium pentaoxide precipitation; The described amount of niobium pentaoxide precipitation and the amount of titanium and tantalum subtract each other the content being niobium in ferrocolumbium.
Description
Technical field
The present invention relates to technical field of ferrous metallurgical analysis, particularly relate to a kind of method measuring content of niobium in ferrocolumbium.
Background technology
Ferrocolumbium is mainly added into steelmaking process as a kind of alloying starting material in smelting iron and steel, and it is expensive, and therefore the content of Accurate Analysis niobium has great significance to starting material clearing, addition and cost control.
In current ferrocolumbium, the analytical approach of niobium, titanium, tantalum has: GB/T3654.8-1983 ferro-niobium chemical analysis method-chromotropic acid spectrphotometric method for measuring titanium amount; GB/T3654.1-1983 ferro-niobium chemical analysis method: on paper, chromatograph separating heavy amount method measures the mensuration-crystal violet benzene extraction spectrophotometric method of niobium, tantalum amount and CSM 04 10 73 01-2001 ferro-niobium-tantalum content.The shortcoming of these methods is: the content that can only measure whole titanium and tantalum in ferrocolumbium, and when measuring content of niobium in ferrocolumbium, titanium in the niobium pentaoxide precipitation obtained and tantalum are the part in ferrocolumbium, therefore the result utilizing said method to record can not represent titanium in niobium pentaoxide precipitation and tantalum content, thus cannot the content of niobium in accurate Calculation ferrocolumbium.And classic method can only once measure a kind of element, complex operation step, meanwhile, consume a large amount of chemicalss, inadequate environmental protection, energy-conservation.
Inductively coupled plasma atomic emission spectrometer (Inductive Coupled Plasma-AtomicEmission Spectrometer, ICP-AES), be excitation source with inductively coupled plasma, have that detection limit is low, the range of linearity wide, ionization and chemistry disruption is few, accuracy and precision advanced analysis performance.
Summary of the invention
The object of this invention is to provide a kind of method measuring content of niobium in ferrocolumbium, the method can measure quickly and accurately in ferrocolumbium with the titanium of niobium co-precipitation and the content of tantalum, thus complete the accurate Calculation of niobium in ferrocolumbium.
Technical scheme is specific as follows:
Measure a method for content of niobium in ferrocolumbium, comprising:
Dissolve ferrocolumbium sample, the form that the niobium in ferrocolumbium precipitates with niobium pentaoxide is precipitated out, weigh the quality of described niobium pentaoxide precipitation; Ferrocolumbium sample is utilized CSM 04 10 4101-2001 ferro-niobium-content of niobium mensuration-tannin hydrolysis gravimetric method, obtain niobium pentaoxide secondary precipitate;
Prepare the solution of described niobium pentaoxide precipitation, preparing standard solution, described standard solution comprises titanium standard solution and tantalum standard solution, in the process for preparation of described titanium standard solution, titania purity used is more than 99.9%, take 0.8340g through 950 DEG C of calcinations to the titania of constant weight in platinum crucible, add 5 ~ 7g potassium pyrosulfate, melt to transparent at 600 DEG C, take off cooling, in 400mL beaker, with the aqueous sulfuric acid leaching frit that volume ratio is 5:95, after frit all dissolves, be diluted in 500mL volumetric flask to scale with the aqueous sulfuric acid that volume ratio is 5:95 again, shake up, finally dilute 10 times with the aqueous sulfuric acid that volume ratio is 5:95, obtain the titanium standard solution that concentration is 100 μ g/mL, in the process for preparation of described tantalum standard solution, take 0.1221g tantalum pentoxide, be placed in platinum crucible, add the melting of 4g potassium pyrosulfate, naturally cool, be placed in aqueous tartaric acid solution heating leaching frit, after frit all dissolves, with aqueous tartaric acid solution accurate dilutions to 1000mL, concentration be the tantalum standard solution of 100 μ g/mL,
Niobium pentaoxide precipitation solution is introduced inductively coupled plasma atomic emission spectrometer, measures line strength of titanium and tantalum, according to line strength that the described standard solution of concentration known records, draw the content of titanium and tantalum in described niobium pentaoxide precipitation; The described quality of niobium pentaoxide precipitation and the amount of titanium and tantalum subtract each other the content being niobium in ferrocolumbium.
Further, in the niobium pentaoxide precipitation solution process of preparation ferrocolumbium sample, by ferrocolumbium sample by iron-content of niobium mensuration-tannin hydrolysis gravimetric method, obtain niobium pentaoxide secondary precipitate; Accurately take the secondary precipitate of 0.2000g niobium pentaoxide, be placed in 35mL porcelain crucible, add 5g potassium pyrosulfate melting 10min in the muffle furnace of 600-650 DEG C bright to fused mass, naturally cool, dissolve with aqueous tartaric acid solution 70mL, be transferred in 250mL volumetric flask, add the aqueous sulfuric acid 20mL that volume ratio is 1:1, be diluted to scale with deionized water to shake up, obtain the niobium pentaoxide precipitation solution dissolving ferrocolumbium sample.
Further, take at least two parts of 0.2000g niobium pentaoxides, make niobium pentaoxide solution according to following operation respectively; Niobium pentaoxide is placed in 35mL porcelain crucible, it is bright to fused mass to add 5g potassium pyrosulfate melting 10min in the muffle furnace of 600-650 DEG C, naturally cools, and dissolves, be transferred in 250mL volumetric flask with aqueous tartaric acid solution 70mL; Add the aqueous sulfuric acid 20mL that titanium standard solution, tantalum standard solution and volume ratio are 1:1 again, shake up with deionized water constant volume, obtain the mixed standard solution of at least two parts of variable concentrations, each mixed standard solution is introduced inductively coupled plasma spectrometry transmitter respectively, measure emitted luminescence intensity, drawing curve; Niobium pentaoxide precipitation solution is introduced inductively coupled plasma spectrometry transmitter, measures titanium and the emitted luminescence intensity corresponding to tantalum, according to the content of working curve determination titanium, tantalum; Described niobium pentaoxide is spectroscopic pure.
Beneficial effect of the present invention:
1, can measure quickly and accurately in ferrocolumbium with the titanium of niobium co-precipitation and the content of tantalum; ICP-AES method once melt sample can simultaneously in Accurate Determining ferrocolumbium with the titanium of niobium co-precipitation and the content of tantalum, thus complete the accurate Calculation of niobium in ferrocolumbium, and simple to operate.
2, environmental protection; ICP-AES method test sample needs less reagent, only sample dissolution, need have the advantage of energy-saving and environmental protection.
Embodiment
The assay method of content of niobium in ferrocolumbium: after ferrocolumbium is dissolved, first add precipitation agent the niobium in ferrocolumbium is precipitated out with niobium pentaoxide, but simultaneously can some titanium and tantalum co-precipitation in niobium pentaoxide precipitation, as long as therefore accurately measure the content of titanium and tantalum in niobium pentaoxide precipitation, the content of niobium in ferrocolumbium just can be calculated.
Measuring titanium and the total thinking of tantalum content in niobium pentaoxide precipitation is: by the melting in muffle furnace of niobium pentaoxide deposit sample potassium pyrosulfate, extract with tartrate, constant volume is in certain volume, atomized soln is introduced inductively coupled plasma atomic emission spectrometer, measures line strength of element to be measured; According to line strength that concentration known standard solution records, obtain the content of titanium and tantalum in niobium pentaoxide precipitation.
In the present invention, agents useful for same is preferred: aqueous tartaric acid solution concentration is 60g/L; Potassium pyrosulfate is that top grade is pure; Niobium pentaoxide is spectroscopic pure.
Preferred ICP spectrometer is that PE company of the U.S. produces, and direct-reading plasma-speetrometer composed entirely by Optima5300DV Bidirectional observation type, and Winlab32 software, Instrument working parameter is as shown in table 1.
Table 1
| Parameter | Higher frequency | Power | Cooling gas flow | Assisted gas flow | Carrier gas flux | Solution elevating amount |
| Numerical value | 40.68MHZ | 1300W | 15L/min | 0.2L/min | 0.8L/min | 1.5mL/min |
| Parameter | Flush time | Preburn time | Integral time | Reading time delay | Observed altitude | Observed pattern |
| Numerical value | 8s | 45s | 2 ~ 10s is automatic | 30s | 15mm | Axially |
Step 1: the niobium pentaoxide precipitation solution preparing ferrocolumbium sample;
In the present invention, have chosen two kinds of ferrocolumbium samples, be respectively GSB03-2208-2008 ferro-niobium and YSBC25691-93 ferro-niobium.
Ferrocolumbium sample is utilized CSM 04 10 41 01-2001 ferro-niobium-content of niobium mensuration-tannin hydrolysis gravimetric method, obtain niobium pentaoxide secondary precipitate.Accurately take the secondary precipitate of 0.2000g niobium pentaoxide, be placed in 35mL porcelain crucible, add 5g potassium pyrosulfate melting 10min in the muffle furnace of 600-650 DEG C bright to fused mass, naturally cool, dissolve with aqueous tartaric acid solution 70mL, be transferred in 250mL volumetric flask, add the aqueous sulfuric acid 20mL that volume ratio is 1:1, be diluted to scale with deionized water to shake up, the niobium pentaoxide precipitation solution of obtained ferrocolumbium sample.
Like this, GSB03-2208-2008 ferro-niobium and YSBC25691-93 ferro-niobium two kinds of niobium pentaoxide precipitation solutions can just be obtained.
Step 2: the preparation of standard solution;
The preparation of titanium standard solution: titania purity used is more than 99.9%, take 0.8340g through 950 DEG C of calcinations to the titania of constant weight in platinum crucible, add 5 ~ 7g potassium pyrosulfate, melt to transparent at 600 DEG C, take off cooling, in 400mL beaker, with the aqueous sulfuric acid leaching frit that volume ratio is 5:95, after frit all dissolves, be diluted in 500mL volumetric flask to scale with the aqueous sulfuric acid that volume ratio is 5:95 again, shake up, finally dilute 10 times with the aqueous sulfuric acid that volume ratio is 5:95, obtain the titanium standard solution that concentration is 100 μ g/mL.
The preparation of tantalum standard solution: take 0.1221g tantalum pentoxide, be placed in platinum crucible, add the melting of 4g potassium pyrosulfate, naturally cool, be placed in aqueous tartaric acid solution heating leaching frit, after frit all dissolves, with aqueous tartaric acid solution accurate dilutions to 1000mL, concentration be the tantalum standard solution of 100 μ g/mL.
Preferred titanium, tantalum analysis of line wavelength are: titanium 336.121nm, tantalum 240.063nm.
Calibration curve: measure that each element Cmax solution launches definitely or relative light intensity 10 times, calculate its standard deviation, relative standard deviation should be less than 0.9%.
Step 3: niobium pentaoxide precipitation solution is introduced inductively coupled plasma atomic emission spectrometer, measures element spectral line intensity to be measured, according to line strength that concentration known standard solution records, draws the content of titanium and tantalum in niobium pentaoxide precipitation.
Take 5 parts of 0.2000g niobium pentaoxides, make 5 parts of solution according to following operation respectively; Niobium pentaoxide is placed in 35mL porcelain crucible, it is bright to fused mass to add 5g potassium pyrosulfate melting 10min in the muffle furnace of 600-650 DEG C, naturally cools, and dissolves, be transferred in 250mL volumetric flask with aqueous tartaric acid solution 70mL; The aqueous sulfuric acid 20mL that titanium standard solution, tantalum standard solution and volume ratio are 1:1 is added respectively by table 2, shake up with deionized water constant volume, make 5 parts of mixed standard solutions, each mixed standard solution is introduced inductively coupled plasma atomic emission spectrometer respectively, measure emitted luminescence intensity, drawing curve.
Table 2
| Label | Titanium standard solution (mL) | Suitable concentration (%) | Tantalum standard solution (mL) | Suitable concentration (%) |
| 1 | 0.00 | 0.00 | 0.00 | 0.00 |
| 2 | 1.00 | 0.050 | 1.00 | 0.050 |
| 3 | 0.50 | 0.250 | 5.00 | 0.025 |
| 4 | 1.00 | 0.500 | 10.00 | 0.050 |
| 5 | 2.00 | 1.00 | 10.00 | 0.500 |
Correction work curve linear: check the linear of working curve by calculating related coefficient, related coefficient should be greater than 0.999.
Each niobium pentaoxide precipitation solution is introduced inductively coupled plasma atomic emission spectrometer, measures titanium and the emitted luminescence intensity corresponding to tantalum, according to the content of working curve determination titanium and tantalum, result is as shown in table 3.
Table 3
In ferrocolumbium, the content of whole titanium, tantalum is standard value; The content recording titanium, tantalum in niobium pentaoxide precipitation through colourimetry is chemical score.
Can be found out by above-mentioned steps, by the inventive method, plasma emission spectrometry can be utilized to measure the content of titanium and tantalum in ferrocolumbium sample niobium pentaoxide precipitation fast and accurately.
Data in table 3 show: measured value, compared with standard value, illustrates that in niobium pentaoxide precipitation, contained titanium and tantalum are not titaniums whole in ferrocolumbium and tantalum; The data of two kinds of samples are compared, and illustrate that in ferrocolumbium, titanium and tantalum content are higher, in niobium pentaoxide precipitation in titanium and tantalum content and ferrocolumbium all titanium and tantalum content difference larger.
Claims (3)
1. measure a method for content of niobium in ferrocolumbium, comprising:
Dissolve ferrocolumbium sample, the form that the niobium in ferrocolumbium precipitates with niobium pentaoxide is precipitated out, weigh the quality of described niobium pentaoxide precipitation; Ferrocolumbium sample is utilized CSM 04 10 4101-2001 ferro-niobium-content of niobium mensuration-tannin hydrolysis gravimetric method, obtain niobium pentaoxide secondary precipitate;
Prepare the solution of described niobium pentaoxide precipitation, preparing standard solution, described standard solution comprises titanium standard solution and tantalum standard solution, in the process for preparation of described titanium standard solution, titania purity used is more than 99.9%, take 0.8340g through 950 DEG C of calcinations to the titania of constant weight in platinum crucible, add 5 ~ 7g potassium pyrosulfate, melt to transparent at 600 DEG C, take off cooling, in 400mL beaker, with the aqueous sulfuric acid leaching frit that volume ratio is 5:95, after frit all dissolves, be diluted in 500mL volumetric flask to scale with the aqueous sulfuric acid that volume ratio is 5:95 again, shake up, finally dilute 10 times with the aqueous sulfuric acid that volume ratio is 5:95, obtain the titanium standard solution that concentration is 100 μ g/mL, in the process for preparation of described tantalum standard solution, take 0.1221g tantalum pentoxide, be placed in platinum crucible, add the melting of 4g potassium pyrosulfate, naturally cool, be placed in aqueous tartaric acid solution heating leaching frit, after frit all dissolves, with aqueous tartaric acid solution accurate dilutions to 1000mL, concentration be the tantalum standard solution of 100 μ g/mL,
Niobium pentaoxide precipitation solution is introduced inductively coupled plasma atomic emission spectrometer, measures line strength of titanium and tantalum, according to line strength that the described standard solution of concentration known records, draw the content of titanium and tantalum in described niobium pentaoxide precipitation; The described quality of niobium pentaoxide precipitation and the amount of titanium and tantalum subtract each other the content being niobium in ferrocolumbium.
2. the method measuring content of niobium in ferrocolumbium as claimed in claim 1, it is characterized in that: in the niobium pentaoxide precipitation solution process of preparation ferrocolumbium sample, by ferrocolumbium sample by ferro-niobium-content of niobium mensuration-tannin hydrolysis gravimetric method, obtain niobium pentaoxide secondary precipitate; Accurately take the secondary precipitate of 0.2000g niobium pentaoxide, be placed in 35mL porcelain crucible, add 5g potassium pyrosulfate melting 10min in the muffle furnace of 600-650 DEG C bright to fused mass, naturally cool, dissolve with aqueous tartaric acid solution 70mL, be transferred in 250mL volumetric flask, add the aqueous sulfuric acid 20mL that volume ratio is 1:1, be diluted to scale with deionized water to shake up, obtain the niobium pentaoxide precipitation solution dissolving ferrocolumbium sample.
3. the method measuring content of niobium in ferrocolumbium as claimed in claim 1, is characterized in that: take at least two parts of 0.2000g niobium pentaoxides, make niobium pentaoxide solution respectively according to following operation; Niobium pentaoxide is placed in 35mL porcelain crucible, it is bright to fused mass to add 5g potassium pyrosulfate melting 10min in the muffle furnace of 600-650 DEG C, naturally cools, and dissolves, be transferred in 250mL volumetric flask with aqueous tartaric acid solution 70mL; Add the aqueous sulfuric acid 20mL that titanium standard solution, tantalum standard solution and volume ratio are 1:1 again, shake up with deionized water constant volume, obtain the mixed standard solution of at least two parts of variable concentrations, each mixed standard solution is introduced inductively coupled plasma spectrometry transmitter respectively, measure emitted luminescence intensity, drawing curve; Niobium pentaoxide precipitation solution is introduced inductively coupled plasma spectrometry transmitter, measures titanium and the emitted luminescence intensity corresponding to tantalum, according to the content of working curve determination titanium, tantalum; Described niobium pentaoxide is spectroscopic pure.
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| CN103353453A (en) * | 2013-06-25 | 2013-10-16 | 彩虹集团电子股份有限公司 | Inductively coupled plasma-atomic emission spectrometry (ICP-AES) method for testing chemical components of blue phosphors of plasma display panel (PDP) |
| CN103454175B (en) * | 2013-08-15 | 2015-04-01 | 贵州航天精工制造有限公司 | Method for determining niobium content in aeronautical material Ti45Nb titanium alloy |
| CN104101573B (en) * | 2014-07-07 | 2016-12-07 | 攀钢集团江油长城特殊钢有限公司 | The method of beryllium hydroxide separation Sulphochlorophenol S spectrphotometric method for measuring Niobium in Steel content |
| CN104237208A (en) * | 2014-09-19 | 2014-12-24 | 内蒙古包钢钢联股份有限公司 | Method for measuring niobium content in iron ore |
| CN104569130B (en) * | 2014-12-29 | 2018-12-14 | 内蒙古包钢钢联股份有限公司 | The measuring method of content of niobium is aoxidized in steel |
| CN105699364B (en) * | 2016-01-25 | 2019-02-01 | 王君玉 | Routine and the method for microelement in a kind of Fast Continuous Determination niobium tantalum concentrate |
| CN106290314A (en) * | 2016-08-02 | 2017-01-04 | 内蒙古包钢钢联股份有限公司 | The assay method of content of niobium in rare earth alloy |
| CN106226192A (en) * | 2016-08-29 | 2016-12-14 | 成都飞机工业（集团）有限责任公司 | A kind of method of content of niobium in gravimetric detemination titanium-niobium alloy |
| CN113189087A (en) * | 2021-04-22 | 2021-07-30 | 江苏永钢集团有限公司 | Method for measuring Nb and P contents in ferrocolumbium ball |
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