CN103234994A - Method for analyzing element contents in high titanium residue by adopting X-ray fluorescence spectrum - Google Patents
Method for analyzing element contents in high titanium residue by adopting X-ray fluorescence spectrum Download PDFInfo
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Abstract
The invention relates to a method for analyzing elements in high titanium residue by adopting an X-ray fluorescence spectrum, wherein the method can be provided for concurrently analyzing titanium content, iron content, calcium content, magnesium content, aluminum content, silicon content, phosphorus content, potassium content, vanadium content, manganese content, and copper content in high titanium residue by adopting an X-ray fluorescence spectrum method, and can be used for determining 11 elements such as titanium, iron, calcium and the like in high titanium residue so as to achieve rapid and comprehensive high titanium residue analysis and meet requirements of imported high titanium residue quality inspection.
Description
Technical field
The invention belongs to the metallurgical analysis technical field, be specifically related to a kind of method of utilizing X-ray fluorescence spectra to analyze constituent content in the high titanium slag, i.e. the X-ray fluorescence spectra analytical approach of titanium, iron, calcium, magnesium, aluminium, silicon, phosphorus, potassium, vanadium, manganese, copper content in a kind of high titanium slag.
Background technology
High titanium slag belongs to a type of titanium slag, stem from ilmenite, allocate ilmenite into a certain amount of carbon containing reducer and join and carry out retailoring in the electric furnace, the oxide of iron is reduced to metallic iron by selectivity in the ore deposit, and titanyl compound is formed product by enrichment, and this is exactly titanium slag.High titanium slag is a kind of titanium ore enrichment or enrichment titanium ore, and its content of titanium dioxide can be up to 90%, and it is the quality raw materials of producing titanium dioxide, and its " three wastes " generation is few, resource and energy utilization rate height.China implements incentives to the import high titanium slag, and year import volume is about 1,000,000 tons, and from 2009, the import high titanium slag was put into the Chinese customs entry commodity tariff number " 38249099 " item down, and the tax rate is decided to be zero.Therefore, trouble titanium white production enterprise elaboration titanium material scarcity and the difficult import problem of high-quality titanium material for many years and solved substantially, this is lasting, healthy to China's titanium dioxide industry, strong impetus has been played in allegro development.
Although high titanium slag is categorized in chemicals, also the same as with mineral products the grade clearing of valuating, the research of at present relevant high titanium slag focuses mostly at aspects such as high titanium slag production technology, performance, purposes.Because the import volume of high titanium slag just progressively rises in recent years, and is illegally to examine commodity, the inspection and quarantine system does not cause enough concerns as yet yet, and is less to the research of its quick measurement aspect.For accurately check high titanium slag grade and impurity content preventing external supplier's void force up commodity prices lattice, containment counterfeit and shoddy goods, effective detection method that must a kind of high titanium slag of exploitation.But the at present main titrimetry of analytical approach of high titanium slag, colourimetry, atomic absorption method etc., complicated operation, reagent consumption are big, can't measure multiple element simultaneously.
Summary of the invention
The purpose of this invention is to provide a kind of method of utilizing X-ray fluorescence spectra to analyze constituent content in the high titanium slag, can analyze with the X-ray fluorescence spectra method titanium, iron, calcium, magnesium, aluminium, silicon, phosphorus, potassium, vanadium, manganese, copper content in the high titanium slag, can be applicable to the mensuration of 11 kinds of elements such as titanium in the high titanium slag, iron, calcium, can realize the quick multianalysis of high titanium slag, satisfy the requirement of China's import high titanium slag quality restriction.
Method of the present invention comprises the steps:
1) preparation of calibration sample
At first preparation is used for setting up the calibration sample of calibration curve, and calibration sample includes the element of variety classes, different content respectively;
Element wherein be in titanium, iron, calcium, magnesium, aluminium, silicon, phosphorus, potassium, vanadium, manganese, the copper any or several;
The used calibration sample of the present invention can be the potpourri of national standard material or national standard material and high purity reagent.
2) preparation calibration sample print
After the calibration sample after the calcination and flux mixing, fusion under the high temperature is poured into after being mixed in the platinum-Jin mould of preheating, and the calibration sample print is made in cooling.
3) foundation of calibration curve
Utilize Xray fluorescence spectrometer to measure the fluorescence intensity level of titanium, iron, calcium, magnesium, aluminium, silicon, phosphorus, potassium, vanadium, manganese, copper in the prepared calibration sample print respectively, utilize theoretical side reaction coefficient to carry out correction between the element, set up constituent content and the calibration curve of proofreading and correct the back fluorescence intensity level; Obtain slope and the intercept of calibration curve;
4) mensuration of testing sample element
According to step 2) method for preparing the calibration sample print prepares the testing sample print, the recycling Xray fluorescence spectrometer is analyzed the testing sample print, fluorescence intensity level after acquisition titanium, iron, calcium, magnesium, aluminium, silicon, phosphorus, potassium, vanadium, manganese, copper are proofreaied and correct, the constituent content of testing sample after the calculating calcination, constituent content value in the final testing sample that obtains after loss on ignition is proofreaied and correct, used formula is as follows:
Wherein, a: calibration curve slope; B: calibration curve intercept; I
C: element is proofreaied and correct back fluorescence intensity (Kcps);
E
x: the constituent content of the testing sample after the calcination (%).
Wherein, E
Cx: loss on ignition is proofreaied and correct the back constituent content; LOI: sample loss on ignition (%).
Wherein, m
0: the initial sample quality; m
1: sample quality after the calcination (g).
Above-mentioned steps 2) flux is the potpourri of lithium tetraborate, di-iron trioxide, silicon dioxide in, and wherein the mass ratio of lithium tetraborate, di-iron trioxide, silicon dioxide is 16:1:1, and above-mentioned flux and the mass ratio of sample are 15:1;
Step 2) temperature of high-temperature fusion is 1050 ℃ in, and the melting time is 20min.
The invention provides the X-ray fluorescence spectra analytical approach of titanium in a kind of high titanium slag, iron, calcium, magnesium, aluminium, silicon, phosphorus, potassium, vanadium, manganese, copper content, method fast, accurately, can realize the needs of import high titanium slag quality restriction, treatment effeciency height of the present invention, social benefit are obvious.
Description of drawings
Fig. 1: titania typical curve (the y=4.0893x-0.2318 R that the present invention sets up
2=0.9999)
Fig. 2: magnesium oxide working curve (the y=0.3706x-0.03051 R that the present invention sets up
2=0.9999)
Fig. 3: kali working curve (the y=0.3108x-0.01071 R that the present invention sets up
2=0.9996)
Fig. 4: calcium oxide working curve (the y=4.206x-0.1477 R that the present invention sets up
2=0.9999)
Fig. 5: vanadium pentoxide working curve (the y=0.3538x+0.01622 R that the present invention sets up
2=0.9987)
Fig. 6: manganese dioxide working curve (the y=0.1974x+0.00868 R that the present invention sets up
2=0.9999)
Fig. 7: di-iron trioxide working curve (the y=1.6285x-0.08026 R that the present invention sets up
2=0.9999)
Fig. 8: cupric oxide working curve (the y=0.1032x-0.02409 R that the present invention sets up
2=0.9999)
Fig. 9: alundum (Al working curve (the y=0.5759x-0.01353 R that the present invention sets up
2=0.9999)
Figure 10: silicon dioxide working curve (the y=7.4631x+0.0004176 R that the present invention sets up
2=0.9999)
Figure 11: phosphorus pentoxide working curve (the y=0.8593x+0.00221 R that the present invention sets up
2=0.9997)
Embodiment
Method of the present invention specifically comprises following step:
1) preparation of calibration sample
At first preparation is used for setting up the calibration sample of calibration curve, and calibration sample includes the element of variety classes, different content respectively.Wherein the number of calibration sample should satisfy the requirement of calibration curve precision, and its number is The more the better.
The mode that the present invention adopts national standard material and national standard material to cooperate with high purity reagent is prepared calibration sample.The national standard material that adopts has GSBH42001-92 (vanadium iron blast furnace slag), GBW07225 (vanadium titano-magnetite), GBW07226 (vanadium titano-magnetite), GBW07226a (vanadium titano-magnetite), GBW07227 (vanadium titano-magnetite), 511 (blast furnace slags), 512 (blast furnace slags), BH0125-6 (open hearth slag), GSBH42012-94 (vessel slag), 514 (open hearth slags), GBW07266 (manganese ore), YSBC15705-94 (vessel slag), GBW07223 (haematite), YSBC14722-98 (containing symplesite), GSB 03-1805-2005 (iron ore), PI3.10 (sintering iron ore); High purity reagent has TiO
2, SiO
2, V
2O
5, Fe
2O
3A kind of concrete compound method of calibration sample sees Table 1.
Table 1: the preparation of calibration sample
2) the serial calibration sample print of preparation
Take by weighing 2.0g left and right sides calibration sample (being accurate to 0.1mg), in muffle furnace 1000 ℃ of following calcinations to constant weight, be cooled to room temperature, place exsiccator standby, calculate burning decrement by formula (3).
Accurately take by weighing sample and 9.0g flux (being accurate to 0.1mg) after the 0.6g calcination respectively, after both are fully mixed, place platinum-Jin crucible, in 1050 ℃ of following fusion 20min, the centre is shaken 3 times at least and is carried out mixing, pour in the platinum-Jin mould of preheating, cooling is made calibration sample and is analyzed print;
The present invention has carried out a large amount of screening experiments to flux, determines that finally flux is the potpourri of lithium tetraborate, di-iron trioxide, silicon dioxide, and wherein the mass ratio of lithium tetraborate, di-iron trioxide, silicon dioxide is 16:1:1.The mixed flux that the present invention uses is compared the fusion that simple lithium tetraborate more is conducive to the high titanium slag sample owing to contain di-iron trioxide, silicon dioxide.This is because the affinity of silicon, iron and oxygen is stronger, causes the randomness of boron-oxygen network to increase behind embedding boron-oxygen network, and cyberspace increases, and the easier dissolving of titanium wherein.
3) foundation of calibration curve
The analysis print of preparation is measured the fluorescence intensity level of titanium, iron, calcium, magnesium, aluminium, silicon, phosphorus, potassium, vanadium, manganese, copper respectively with Xray fluorescence spectrometer, utilize theoretical side reaction coefficient to carry out correction between the element, and set up constituent content and proofread and correct working curve (accompanying drawing 1-11) between the fluorescence intensity of back; Wherein the measurement parameter of each element is as shown in table 2.
Table 2: the X-ray fluorescence spectra measured parameter value of each element
4) mensuration of testing sample element
According to step 2) method obtain the print of the X-ray fluorescence spectra analysis usefulness of testing sample, recycling Xray fluorescence spectrometer analytic sample print, obtain titanium, iron, calcium, magnesium, aluminium, silicon, phosphorus, potassium, vanadium, manganese, the fluorescence intensity level of copper, utilize theoretical side reaction coefficient to carry out correction between the element, obtain proofreading and correct the back fluorescence intensity level, to proofread and correct back fluorescence intensity level substitution formula (1), the constituent content of the testing sample after the calculating calcination, obtain the testing sample constituent content (by formula calculate (2)) after loss on ignition is proofreaied and correct at last, formula (1) and formula (2) are documented in the summary of the invention part.
Come method of the present invention is described in detail below in conjunction with specific embodiment.
1) preparation of standard series print
Take by weighing the national standard material and high purity reagent prepares calibration sample with reference to table 1 proportioning, all weighings all are accurate to 0.1mg, add 8.0g lithium tetraborate, 0.5g di-iron trioxide, 0.5g silicon dioxide respectively, after fully mixing, place platinum-Jin crucible, in 1050 ℃ of fusion 20min, midfeather is shaken and is carried out mixing more than 3 times, pour into afterwards in the platinum-Jin mould of preheating, the standard model print is made in cooling.
2) foundation of calibration curve
Select serial calibration sample print to draw calibration curve, each element should have enough content ranges, and the measuring condition of each elemental characteristic spectral line obtains (as shown in table 2) by optimizing.The content of each element is with shown in the following tabulation of correction back fluorescence intensity level.
Table 3:TiO
2Content and corresponding correction of fluorescence intensity value
Table 4:MgO content and corresponding correction of fluorescence intensity value
Table 5:K
2O content and corresponding correction of fluorescence intensity value
Table 6:CaO content and corresponding correction of fluorescence intensity value
Table 7:V
2O
5Content and corresponding correction of fluorescence intensity value
Table 8:MnO
2Content and corresponding correction of fluorescence intensity value
Table 9:Fe
2O
3Content and corresponding correction of fluorescence intensity value
Table 10:CuO content and corresponding correction of fluorescence intensity value
Table 11:Al
2O
3Content and corresponding correction of fluorescence intensity value
Table 12:SiO
2Content and corresponding correction of fluorescence intensity value
Table 13:P
2O
5Content and corresponding correction of fluorescence intensity value
From above-mentioned data, set up the calibration curve of each element, titania calibration curve (y=4.0893x-0.2318 R
2=0.9999); Magnesium oxide calibration curve (y=0.3706x-0.03051 R
2=0.9999); Kali calibration curve (y=0.3108x-0.01071 R
2=0.9996); Calcium oxide calibration curve (y=4.206x-0.1477 R
2=0.9999); Vanadium pentoxide calibration curve (y=0.3538x+0.01622 R
2=0.9987); Manganese dioxide calibration curve (y=0.1974x+0.00868 R
2=0.9999); Di-iron trioxide calibration curve (y=1.6285x-0.08026 R
2=0.9999); Cupric oxide calibration curve (y=0.1032x-0.02409 R
2=0.9999); Alundum (Al calibration curve (y=0.5759x-0.01353 R
2=0.9999); Silicon dioxide calibration curve (y=7.4631x+0.0004176 R
2=0.9999); Phosphorus pentoxide calibration curve (y=0.8593x+0.00221 R
2=0.9997).
3) analytic sample preparation
Utilize planetary-type grinding machine to grind high titanium slag sample Ti00, prepared sizes place exsiccator standby less than 100 order analytic samples.
The mensuration of burning decrement: clean porcelain crucible with distilled water, oven dry to constant weight, is cooled off standby in 1000 ℃ of calcinations.Take by weighing the 2.0g left and right sides predrying sample Ti00 to be measured, be accurate to 0.1mg, calcination is cooled to room temperature to constant weight in 1000 ℃ of muffle furnaces, places exsiccator, and by formula (3) calculate burning decrement.
4) analytic sample fusion
The high titanium slag sample Ti00(that accurately takes by weighing after 8.0g lithium tetraborate, 0.5g di-iron trioxide, 0.5g silicon dioxide and the 0.6g calcination all is accurate to 0.1mg), after fully mixing, place platinum-Jin crucible, in 1050 ℃ of fusion 20min, midfeather is shaken and is carried out mixing more than 3 times, pour into afterwards in the platinum-Jin mould of preheating, the print of testing sample is made in cooling.
5) analytic sample is measured
Behind the instrument stabilizer, select appropriate calibration sample print to carry out the drift correction of instrument, carry out the analytic sample print then and measure, the correction equation of each element of fluorescence intensity level substitution after the element that obtains is proofreaied and correct namely obtains results of elemental analyses.Ti00 sample analysis result is TiO
2: 81.15%; MgO:0.55%; Al
2O
3: 1.43%; SiO
2: 3.17%; P
2O
5＜0.005%; K
2O:0.099%; CaO:0.31%; V
2O
5: 0.49%; MnO
2: 1.98%; Fe
2O
3: 10.76%; CuO:0.0054%.
1) preparation of standard series print
The preparation of standard series print is with example 1.
2) foundation of calibration curve
The foundation of calibration curve is with example 1
3) analytic sample preparation
Utilize planetary-type grinding machine to grind high titanium slag sample Ti01, prepared sizes place exsiccator standby less than 100 order analytic samples.
The mensuration of burning decrement: clean porcelain crucible with distilled water, oven dry to constant weight, is cooled off standby in 1000 ℃ of calcinations.Take by weighing the 2.0g left and right sides predrying sample Ti01 to be measured, be accurate to 0.1mg, calcination is cooled to room temperature to constant weight in 1000 ℃ of muffle furnaces, places exsiccator, calculates burning decrement by formula (4).
4) analytic sample fusion
The high titanium slag sample Ti01(that accurately takes by weighing respectively after 8.0g lithium tetraborate, 0.5g di-iron trioxide, 0.5g silicon dioxide and the 0.6g calcination all is accurate to 0.1mg) 8 parts, after fully mixing, place platinum-Jin crucible, in 1050 ℃ of fusion 20min, midfeather is shaken and is carried out mixing more than 3 times, pour into afterwards in the platinum-Jin mould of preheating, cooling obtains 8 and analyzes print in flakes.
6) analytic sample is measured
Measuring method is with example 1.The relative standard deviation that this method magnesium, aluminium, silicon, potassium, calcium, titanium, vanadium, manganese, iron, copper are analyzed is as shown in table 14, and the result shows that this method has higher precision.
The precision of table 14 method
1) preparation of standard series print
The preparation of standard series print is with example 1.
2) foundation of calibration curve
The foundation of calibration curve is with example 1
3) analytic sample preparation
Utilize planetary-type grinding machine to grind ilmenite concentrate standard substance YSBC19716-2003, prepared sizes place exsiccator standby less than 100 order analytic samples.
The mensuration of burning decrement: clean porcelain crucible with distilled water, oven dry to constant weight, is cooled off standby in 1000 ℃ of calcinations.Take by weighing the 2.0g left and right sides predrying ilmenite concentrate standard substance YSBC19716-2003 to be measured, be accurate to 0.1mg, calcination is cooled to room temperature to constant weight in 1000 ℃ of muffle furnaces, places exsiccator, calculates burning decrement by formula (4)
4) analytic sample fusion
The ilmenite concentrate standard substance YSBC19716-2003(that accurately takes by weighing respectively after 8.0g lithium tetraborate, 0.5g di-iron trioxide, 0.5g silicon dioxide and the 0.6g calcination all is accurate to 0.1mg) 8 parts, after fully mixing, place platinum-Jin crucible, in 1050 ℃ of fusion 20min, midfeather is shaken and is carried out mixing more than 3 times, pour into afterwards in the platinum-Jin mould of preheating, cooling obtains 8 and analyzes print in flakes.
5) analytic sample is measured
Measuring method is with example 1, and ilmenite concentrate standard substance YSBC19716-2003 measurement result is consistent with given value, and the result is as shown in Table 15, method accuracy height.(CV: standard value; AVE: testing mean)
The accuracy of table 15 method
The above results shows, method of the present invention can detect the content of titanium in the high titanium slag, iron, calcium, magnesium, aluminium, silicon, phosphorus, potassium, vanadium, manganese, copper accurately, method has higher precision and accuracy, can realize the quick multianalysis of high titanium slag, satisfy the requirement of China's import high titanium slag quality restriction.
Claims (5)
1. method of utilizing X-ray fluorescence spectra to analyze element in the high titanium slag, described element is titanium, iron, calcium, magnesium, aluminium, silicon, phosphorus, potassium, vanadium, manganese and copper, it is characterized in that, described method includes following step:
1) preparation of calibration sample:
Preparation is used for setting up the calibration sample of calibration curve, and calibration sample includes the element of variety classes, different content respectively; Element wherein be in titanium, iron, calcium, magnesium, aluminium, silicon, phosphorus, potassium, vanadium, manganese, the copper any or several;
2) preparation calibration sample print
After the calibration sample after the calcination and flux mixing, fusion under the high temperature is poured into after being mixed in the platinum-Jin mould of preheating, and the calibration sample print is made in cooling;
3) foundation of calibration curve
Utilize Xray fluorescence spectrometer to measure the fluorescence intensity level of titanium, iron, calcium, magnesium, aluminium, silicon, phosphorus, potassium, vanadium, manganese, copper in the prepared calibration sample print respectively, utilize theoretical side reaction coefficient to carry out correction between the element, set up constituent content and the calibration curve of proofreading and correct the back fluorescence intensity level; Obtain slope and the intercept of calibration curve;
4) mensuration of testing sample element
According to step 2) method for preparing the calibration sample print prepares the testing sample print, the recycling Xray fluorescence spectrometer is analyzed the testing sample print, fluorescence intensity level after acquisition titanium, iron, calcium, magnesium, aluminium, silicon, phosphorus, potassium, vanadium, manganese, copper are proofreaied and correct, the constituent content of testing sample after the calculating calcination, constituent content value in the final testing sample that obtains after loss on ignition is proofreaied and correct, used formula is as follows:
Wherein, a: calibration curve slope; B: calibration curve intercept; I
C: element is proofreaied and correct back fluorescence intensity Kcps;
E
x: the constituent content of the testing sample after the calcination;
Wherein, E
Cx: loss on ignition is proofreaied and correct the back constituent content; LOI: sample loss on ignition (%);
Wherein, m
0: the initial sample quality; m
1: sample quality after the calcination.
2. the method for claim 1 is characterized in that described step 2) in flux be the potpourri of lithium tetraborate, di-iron trioxide, silicon dioxide.
3. the method for claim 1, the mass ratio that it is characterized in that described lithium tetraborate, di-iron trioxide, silicon dioxide is 16:1:1.
4. the method for claim 1 is characterized in that described step 2) in the mass ratio of flux and sample be 15:1.
5. the method for claim 1 is characterized in that described step 2) in the temperature of high-temperature fusion be 1050 ℃, the melting time is 20min.
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