CN102253030A - Method for determining impurity content in high-titanium slag - Google Patents
Method for determining impurity content in high-titanium slag Download PDFInfo
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Abstract
The invention discloses a method for determining the impurity content in high-titanium slag, and belongs to the metallurgical chemical field. According to the method, a high-titanium slag sample is molten by a mixed flux; a frit is leached by a sulfuric acid solution to prepare a test solution; and the impurity component in the diluted high-titanium slag test solution is determined by an inductive coupling plasma emission spectrometer. With the invention, the content of the impurity component in high-titanium slag can be determined accurately, simply, and rapidly.
Description
Technical field
The invention belongs to field of metallurgy and chemical engineering.
Background technology
In order to improve the comprehensive utilization value of vanadium titano-magnetite and its resource, need to will be as metallurgical raw material, form complexity, high titanium slag composition that the impurity component content is bigger carries out quantitative measurement accurately, to improve its utilization factor.Mensuration to impurity element components such as Si, Al, Ca, Mg, Fe in the high titanium slag adopts chemical analysis method more at present, the mensuration disturbing factor is many, analysis process long, it is many to consume reagent, and need change or seek proper method at any time according to the variation of element to be measured and interference element content.
Have not yet to see Si, the Al that uses in the ICP-AES mensuration high titanium slag, the report of impurities analysis methods such as Ca, Mg.There is the Yang Hongchun that climbs steel to adopt ICP-AES in the literature to V in the vanadium slag
2O
5, TFe, SiO
2, Al
2O
3, CaO, MgO, MnO, TIO
2, P, S the experimental study report that carries out of mensuration, sample after 1020 ℃ of fusions, use hydrochloric acid leaching through sodium carbonate and sodium tetraborate mixed flux, by the matrix coupling with just add in the yttrium calibration, mensuration when having realized constant in the vanadium slag sample, trace element.Because the titania in the vanadium slag has only the content about 10%, therefore leaching and measuring in the hydrochloric acid solution of percent by volume 10%, sample can hydrolysis, can carry out the mensuration of series components in the sample solution.But the content of titania is about 80% in the high titanium slag, measures the serious hydrolysis of sample solution meeting with hydrochloric acid leaching, influence the accurate mensuration of component to be measured, and its flux sodium carbonate and sodium tetraborate melt temperature height, relatively poor to the fusion effect of high titanium slag, be not suitable for the high titanium slag resolution measurement.
Summary of the invention
The objective of the invention is to address the above problem and the method for impurity content in a kind of simple, fast measuring high titanium slag is provided, utilize the present invention can determine impurity content in the high titanium slag accurately.
The technical solution adopted in the present invention is:
A kind of method of measuring impurity content in the high titanium slag may further comprise the steps:
1) get 1 part of sample to be tested, add the mixed solvent that 10 parts～20 parts natrium carbonicum calcinatum and boric acid mass ratio are 1.5: 1～2: 1, under 950 ℃～1150 ℃ high temperature fusion complete, cooling obtains frit;
2) described frit being put into percent by volume is to heat in 4%～6% the sulfuric acid, leaches frit, is 4%～6% Dilution of sulphuric acid constant volume with percent by volume, dilutes to obtain test solution to be measured again;
3) make the working curve titer;
4) on inductive coupling plasma emission spectrograph, measure the calibration curve of working curve standard solution impurities and the spectral intensity of described test solution impurity to be measured, directly draw the result of impurity component in the sample to be tested by the automatic regression Calculation of computing machine.
Further, described step 3) is made the working curve titer: get the titania standard solution, make the quality of titania in the quality of taking out titania in the standard solution and the described test solution to be measured suitable, make the sulfuric acid amount in the titania standard solution suitable simultaneously with the sulfuric acid quality in the described test solution to be measured, at least 4 parts of described titania standard solution are placed volumetric flask, the standard solution that adds impurity component in the sample to be tested respectively, be settled to scale, obtain some parts of working curve standard solution; Impurity component content is linear distribution in the different described titania standard solution, and the content of impurity is between the highs and lows of described calibration curve in the sample to be tested.
Further, described step 3) is made the working curve titer: get titania benchmark reagent, make the quality of titania of the standard reagent titania quality of taking-up and sample to be tested suitable, with titania matrix reagent and step 1), 2) fusion leaching under the same terms, constant volume is in volumetric flask, obtain matrix solution, be taken to few 4 parts of above-mentioned matrix solution, the standard solution that adds impurity component in the sample to be tested respectively, make the content of the impurity component of measuring in the sample to be tested in the described some parts matrix solution be linear distribution, be settled to scale, obtain some parts of working curve standard solution; Impurity component content is linear distribution in the different described titania standard solution, and the content of impurity is between the highs and lows of described calibration curve in the sample to be tested.
Preferably, described natrium carbonicum calcinatum and boric acid mass ratio are 2: 1.
Further, described sample to be tested places fusion under the platinum crucible high temperature.
Preferably, described sample impurity component is iron, silicon dioxide, alundum (Al, calcium oxide, magnesium oxide, manganese oxide.
The present invention has the following advantages:
Method of the present invention can be measured impurity content in the high titanium slag simply, fast and accurately, adopts melting method of the present invention, sample can be decomposed fully, and leaching rapidly; The influence of adopting leaching of the present invention and dilution process to avoid the hydrolysis of sample to be tested that analytical element is measured; The solution dilution of high salt and high sulfuric acid medium is measured for 10 times, greatly reduced the influence of salinity and sour effect, improved accuracy and the precision analyzed; The standard solution of two kinds of scheme preparation working curves can freely be selected, and each needs institute to get.Method one, titania standard solution [sulfuric acid medium (the 1+19)] bottoming that the adds 1.00mg/mL curve of working, and add sulfuric acid amount and flux, make consistent with sulfuric acid amount and flux amount in the sample solution to be measured, and the acidity and the flux amount of solution of having guaranteed the solution of working curve and sample to be tested is consistent, improved accuracy and the precision analyzed, energy consumption is low, and is simple to operate; Method two, with the standard reagent titania that is equivalent to titania amount in the sample to be tested directly with the step synchronous operation of sample fusion, divide and get the bottoming of solution titania, synchronous operation has guaranteed the consistance of condition to have improved the accuracy and the precision of analysis.
Description of drawings
The present invention is further detailed explanation below in conjunction with drawings and embodiments.
Fig. 1 is SiO in the sample to be tested of embodiment 1
2Calibration curve;
Fig. 2 is Al in the sample to be tested of embodiment 1
2O
3Calibration curve;
Fig. 3 is the calibration curve of CaO in the sample to be tested of embodiment 1;
Fig. 4 is the calibration curve of MgO in the sample to be tested of embodiment 1;
Fig. 5 is the calibration curve of TFe in the sample to be tested of embodiment 1;
Fig. 6 is the calibration curve of MnO in the sample to be tested of embodiment 1;
Embodiment
(1) fusion of sample to be tested: take by weighing a sample to be tested 0.2000g, place Platinum crucible, the amount of taking by weighing of sample to be tested general with sample to be tested homogeneity, representativeness and during later analysis used amount of reagent and constant volume dilute volume etc. direct relation arranged.For the powder raw material sample, representative if the sample to be tested preparation is evenly, to the composition measurement of varying number level content, claim that generally the sample to be tested amount is 0.1g～1g.During the inductively coupled plasma spectrometry method is measured usually in the sample to be tested greater than 0.1% composition measurement, sample weighting amount is decided to be 0.1g～0.5g, enough reaches the sensitivity of its mensuration for the mensuration of impurity customary amount composition iron, silicon dioxide, alundum (Al, calcium oxide, magnesium oxide, manganese oxide etc. in the high titanium slag.Add the flux of using natrium carbonicum calcinatum and boric acid to mix at 2: 1 that takes by weighing 15 times of test portion quality, mixing by mass ratio.When claiming that sample to be tested is low, need to add the flux amount of high multiple, when for example taking by weighing 0.10g～0.20g sample to be tested, add 2.0g～3.0g mixed flux, when taking by weighing 0.20g～0.50g sample to be tested, can only add the flux of 10 times of test portion amounts, as the 0.20g sample, add the 2.0g mixed flux, the 0.30g sample, add the 3.0g mixed flux, 0.40g～0.50g sample adds 4.0～5.0g mixed flux, all can, but the flux amount will accurately take by weighing, and is consistent.Behind the mixing in 1000 ℃ high temperature furnace fusion 15min, take out, cooling obtains frit.
(2) leaching of frit and dilution: clean the crucible outer wall, in the beaker of 250mL, add 80mL sulfuric acid (5+95), heating, leach frit, in the 200mL volumetric flask, pipette the 10.00mL constant volume with sulfuric acid (5+95) dilution constant volume in the 100mL volumetric flask, obtain test solution to be measured.
(3) preparation of working curve standard solution: take by weighing the 0.2000g sample to be tested, by 80% the titania bottoming curve of working, titania standard solution [sulfuric acid medium (the 1+19)] 16.00mL that pipettes 1.00mg/mL is in five 100mL volumetric flasks, respectively add 0.20mL sulfuric acid and 5mL concentrated hydrochloric acid, respectively add the 0.30g mixed flux flux amount of sample to be tested solution basically identical (keep with) again, shake to flux and dissolve.Content range according to the sample to be tested composition, the standard solution that adds iron, silicon dioxide, alundum (Al, calcium oxide, magnesium oxide, manganese oxide successively, make the content of iron, silicon dioxide, alundum (Al, calcium oxide, magnesium oxide, manganese oxide in five some standard solution become the suitable range of linearity, and highs and lows (minimum point of non-zero points) content has comprised the sample content range of being measured, be settled to scale, obtain the working curve standard solution.
(4) on inductive coupling plasma emission spectrograph, can be silicon 212.412nm, 251.612nm also rule of thumb at the optimum measurement spectral line of recommending; Aluminium 308.215nm, 396.152nm; Calcium 317.933nm, 393.367nm; Magnesium 279.553nm, 280.213nm, 285.213nm; Iron 239.562nm, 259.940nm; Among manganese 257.610nm, 259.373nm, the 293.930nm, select the optimum measurement spectral line of iron, silicon, aluminium, calcium, magnesium, manganese according to the measuring condition of each instrument, also can select other optimum measurement spectral line according to instrument state, measure the spectral intensity of impurity in the calibration curve of working curve standard solution and the sample to be tested, directly draw the analysis result of sample by the automatic regression Calculation of computing machine.The optimized analysis spectral line of the used instrument of present embodiment respectively is silicon 251.612nm, aluminium 396.152nm, calcium 317.933nm, magnesium 285.213nm, iron 239.562nm, manganese 259.373nm.The spectral intensity of each impurity component is silicon 42.067ksp, aluminium 16.397ksp, calcium 17.103ksp, magnesium 17.690ksp, iron 338.001ksp, manganese 156.223ksp among the sample to be tested 1#, the calibration curve of each impurity component is seen Fig. 1 to Fig. 6, and wherein Fig. 1 is SiO in the sample to be tested
2Calibration curve, Fig. 2 is Al in the sample to be tested
2O
3Calibration curve, Fig. 3 is the calibration curve of CaO in the sample to be tested, Fig. 4 is the calibration curve of MgO in the sample to be tested, Fig. 5 is the calibration curve of TFe in the sample to be tested; Fig. 6 is the calibration curve of MnO in the sample to be tested, calculates the content that demonstrates impurity in the sample to be tested automatically by computer program, and it the results are shown in Table the 1# sample in 1.
(5) sample to be tested in the present embodiment is carried out recovery test, it the results are shown in Table the recovery related data in the 1# sample in 1.
(1) fusion of sample to be tested: take by weighing a sample to be tested 0.1000g, place Platinum crucible; Add the flux of using natrium carbonicum calcinatum and boric acid to mix at 2: 1 that takes by weighing 20 times of test portion quality, mixing by mass ratio; Behind the mixing in 950 ℃ high temperature furnace fusion 30min, take out, cooling obtains frit.
(2) leaching of sample to be tested fuse piece and dilution: clean the crucible outer wall, in the beaker of 250mL, add 100mL sulfuric acid (4+96), heating, leach frit, in the 200mL volumetric flask, pipette the 10.00mL constant volume with sulfuric acid (4+96) dilution constant volume in the 100mL volumetric flask, obtain test solution to be measured.
(3) preparation of working curve standard solution: titania benchmark reagent (purity is more than the 99.99%) portion that takes by weighing sample to be tested amount 90%, under the condition identical, carry out the fusion leaching with sample to be tested, constant volume is in the 200mL volumetric flask, branch is got five parts of 10.00mL and is put in respectively in five 100mL volumetric flasks, content range according to mensuration sample constituents, add iron successively, silicon dioxide, alundum (Al, calcium oxide, magnesium oxide, the standard solution of manganese oxide, make silicon dioxide in five some standard solution, alundum (Al, calcium oxide, magnesian content becomes the suitable range of linearity, and highs and lows (minimum point of non-zero points) content has comprised the sample content range of being measured, be settled to scale, obtain the working curve standard solution.
(4) on inductive coupling plasma emission spectrograph according to the measurement spectral line of the optimum measurement choice of spectrum iron of each instrument, silicon, aluminium, calcium, magnesium, manganese, measure the spectral intensity of impurity in working curve standard solution calibration curve and the sample to be tested, directly draw the analysis result of sample by the automatic regression Calculation of computing machine, the analysis spectral line of the used instrument of this project respectively is silicon 251.612nm, aluminium 396.152nm, calcium 317.933nm, magnesium 285.213nm, iron 239.562nm, manganese 259.373nm.Automatically calculate by computer program and to demonstrate the content of impurity in the sample to be tested and see Table 3# sample in 1.
(5) by the inventive method, the present embodiment testing sample is carried out 8 times measured, and calculated its relative standard deviation, it the results are shown in Table the 3# sample related data in 1.
(1) fusion of sample to be tested: take by weighing a sample to be tested 0.5000g, place Platinum crucible; Add the flux of using natrium carbonicum calcinatum and boric acid to mix at 2: 1 that takes by weighing 10 times of test portion quality, mixing by mass ratio; Behind the mixing in 1150 ℃ high temperature furnace fusion 10min, take out, cooling obtains frit.
(2) leaching of sample fuse piece and dilution: clean the crucible outer wall, in the beaker of 250mL, add 120mL sulfuric acid (6+94), heating, leach frit, in the 200mL volumetric flask, pipette the 10.00mL constant volume with sulfuric acid (6+94) dilution constant volume in the 100mL volumetric flask, obtain test solution to be measured.
(3) preparation of working curve standard solution: take by weighing titania benchmark reagent (purity is more than the 99.99%) portion of sample size 60%, carry out the fusion leaching under the condition identical with sample, constant volume is in the 200mL volumetric flask.Branch is got five parts of 10.00mL and is put in respectively in five 100mL volumetric flasks, content range according to mensuration sample constituents, the standard solution that adds iron, silicon dioxide, alundum (Al, calcium oxide, magnesium oxide, manganese oxide successively, make that silicon dioxide, alundum (Al, calcium oxide, magnesian content become the suitable range of linearity in five some standard solution, and highs and lows (minimum point of non-zero points) content has comprised the sample content range of being measured, be settled to scale, obtain the working curve standard solution.
(4) on inductive coupling plasma emission spectrograph according to the measurement spectral line of the optimum measurement choice of spectrum iron of each instrument, silicon, aluminium, calcium, magnesium, manganese, the spectral intensity of measuring impurity in the calibration curve of working curve standard solution and the sample to be tested is directly drawn the analysis result of sample by the automatic regression Calculation of computing machine.The analysis spectral line of the used instrument of this project respectively is silicon 251.612nm, aluminium 396.152nm, calcium 317.933nm, magnesium 285.213nm, iron 239.562nm, manganese 259.373nm, is automatically calculated by computer program to demonstrate the content of impurity in the sample to be tested and see Table 2# sample in 1.
(5) by the inventive method, the present embodiment testing sample has been carried out recovery test, it the results are shown in Table the recovery related data of the 2# sample in 1.
The measurement result of table 1 testing sample
By above embodiment and table 1 as can be seen, the relative standard deviation 0.61%～1.94% of sample to be tested, the recovery illustrate that 98.9%～102.3% the inventive method has the precision that high accuracy is become reconciled.
Above embodiment is only unrestricted in order to technical scheme of the present invention to be described, although the present invention is had been described in detail with reference to preferred embodiment, those of ordinary skill in the art is to be understood that, can make amendment or be equal to replacement technical scheme of the present invention, and not breaking away from the spirit and scope of technical solution of the present invention, it all should be encompassed in the middle of the claim scope of the present invention.
Claims (7)
1. a method of measuring impurity content in the high titanium slag is characterized in that, may further comprise the steps:
1) get 1 part of sample to be tested, the natrium carbonicum calcinatum and the boric acid mass ratio that add 10 parts～20 parts are the mixed solvent of 1.5:1～2:1, under 950 ℃～1150 ℃ high temperature fusion complete, the cooling, obtain frit;
2) described frit being put into percent by volume is to heat in 4%～6% the sulfuric acid, leaches frit, is 4%～6% Dilution of sulphuric acid constant volume with percent by volume, dilutes to obtain test solution to be measured again;
3) make the working curve titer;
4) on inductive coupling plasma emission spectrograph, measure the calibration curve of working curve standard solution impurities and the spectral intensity of described test solution impurity to be measured, directly draw the result of impurity component in the sample to be tested by the automatic regression Calculation of computing machine.
2. the method for impurity content in the mensuration high titanium slag according to claim 1, it is characterized in that, described step 3) is made the working curve titer: get the titania standard solution, make the quality of titania in the quality of taking out titania in the standard solution and the described test solution to be measured suitable, make the sulfuric acid amount in the titania standard solution suitable simultaneously with the sulfuric acid quality in the described test solution to be measured, at least 4 parts of described titania standard solution are placed volumetric flask, the standard solution that adds impurity component in the sample to be tested respectively, be settled to scale, obtain some parts of working curve standard solution; Impurity component content is linear distribution in the different described titania standard solution, and the content of impurity is between the highs and lows of described calibration curve in the sample to be tested.
3. the method for impurity content in the mensuration high titanium slag according to claim 1, it is characterized in that, described step 3) is made the working curve titer: get titania benchmark reagent, make the quality of titania of the standard reagent titania quality of taking-up and sample to be tested suitable, with titania matrix reagent and step 1), 2) fusion leaching under the same terms, constant volume is in volumetric flask, obtain matrix solution, be taken to few 4 parts of above-mentioned matrix solution, the standard solution that adds impurity component in the sample to be tested respectively, make the content of the impurity component of measuring in the sample to be tested in the described some parts matrix solution be linear distribution, be settled to scale, obtain some parts of working curve standard solution; Impurity component content is linear distribution in the different described titania standard solution, and the content of impurity is between the highs and lows of described calibration curve in the sample to be tested.
4. according to the method for impurity content in any described mensuration high titanium slag of claim 1 to 3, it is characterized in that described natrium carbonicum calcinatum and boric acid mass ratio are 2:1.
5. according to the method for impurity content in any described mensuration high titanium slag of claim 1 to 3, it is characterized in that in the described step 1), described sample to be tested places fusion under the platinum crucible high temperature.
6. the method for impurity content is characterized in that in the mensuration high titanium slag according to claim 4, and described sample impurity component is iron, silicon dioxide, alundum (Al, calcium oxide, magnesium oxide, manganese oxide.
7. the method for impurity content is characterized in that in the mensuration high titanium slag according to claim 5, and described sample impurity component is iron, silicon dioxide, alundum (Al, calcium oxide, magnesium oxide, manganese oxide.
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| CN106814062A (en) * | 2015-11-27 | 2017-06-09 | 中冶建筑研究总院有限公司 | The method for determining various chemical element contents in slag simultaneously |
| CN106885800A (en) * | 2015-12-15 | 2017-06-23 | 云南冶金新立钛业有限公司 | The method drawn the working curve of sial calcium and magnesium manganese vanadium chromium in high titanium slag sample to be measured and determine wherein sial calcium and magnesium manganese vanadium chromium content |
| CN105693116A (en) * | 2016-02-03 | 2016-06-22 | 重庆大学 | Method for removing calcium and magnesium impurities by using waste heat of high-temperature titanium slag |
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| CN106048256A (en) * | 2016-06-30 | 2016-10-26 | 重庆大学 | Method for removing calcium and magnesium impurities in titanium slag by using modified additive |
| CN106048256B (en) * | 2016-06-30 | 2018-01-05 | 重庆大学 | Method for removing calcium and magnesium impurities in titanium slag by using modified additive |
| CN112782343A (en) * | 2021-02-18 | 2021-05-11 | 包头钢铁（集团）有限责任公司 | Method for analyzing content of titanium dioxide in high-titanium bauxite |
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