CN103234994B - 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 metallurgical analysis technical field, be specifically related to a kind of method utilizing X-ray fluorescence spectra to analyze constituent content in 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, ilmenite is allocated into a certain amount of carbon containing reducer and join in electric furnace and carry out retailoring, in ore deposit, the oxide of iron is reduced to metallic iron by selectivity, and titanyl compound is formed product by enrichment, this is exactly titanium slag.High titanium slag is a kind of titanium ore enriched substance or enrichment titanium ore, and its content of titanium dioxide can up to 90%, and it is the quality raw materials producing titanium dioxide, and its " three wastes " generation is few, resource and energy utilization rate high.China implements incentives to import high titanium slag, and year, import volume was at about 1,000,000 tons, and from 2009, under import high titanium slag is put into the Chinese customs entry commodity tariff number " 38249099 " item, the tax rate was decided to be zero.Therefore, trouble the deficient and difficult import problem of high-quality titanium material of titanium white production enterprise fine work titanium material for many years and substantially solved, this serves strong impetus to China's titanium white powder industry keeps, health, allegro development.
Although high titanium slag is categorized in chemicals, also equally with mineral products carry out valuation clearing, at present about the research of high titanium slag focuses mostly in high titanium slag production technology, performance, purposes etc. by grade.Because the import volume of high titanium slag just progressively rises in recent years, and be illegally examine commodity, inspection and quarantine system also not yet causes enough concerns, less to the research of its Quick Measurement aspect.In order to accurately check high titanium slag grade and impurity content to force up commodity prices lattice, containment counterfeit and shoddy goods to prevent external supplier's void, a kind of effective detection method of high titanium slag must be developed.But the main titrimetry of analytical approach, colourimetry, atomic absorption method etc. of high titanium slag at present, complicated operation, reagent consumption greatly, cannot Simultaneously test multiple elements.
Summary of the invention
The object of this invention is to provide a kind of method utilizing X-ray fluorescence spectra to analyze constituent content in high titanium slag, can analyze titanium, iron, calcium, magnesium, aluminium, silicon, phosphorus, potassium, vanadium, manganese, copper content X-ray fluorescence spectra method in high titanium slag, can be applicable to the mensuration of 11 kinds of elements such as titanium in high titanium slag, iron, calcium, the quick multianalysis of high titanium slag can be realized, meet the requirement of China's import high titanium slag quality restriction.
Method of the present invention, comprises the steps:
1) preparation of calibration sample
First prepare the calibration sample for setting up calibration curve, calibration sample includes the element of variety classes, different content respectively;
Element is wherein any one or several in titanium, iron, calcium, magnesium, aluminium, silicon, phosphorus, potassium, vanadium, manganese, copper;
Calibration sample used by the present invention can be the potpourri of national standard material or national standard material and high purity reagent.
2) calibration sample print is prepared
After the calibration sample after calcination and flux mixing, melting under high temperature, pours in the platinum-Jin mould of preheating after being mixed, calibration sample print is made in cooling.
3) foundation of calibration curve
Xray fluorescence spectrometer is utilized to measure the fluorescence intensity level of titanium, iron, calcium, magnesium, aluminium, silicon, phosphorus, potassium, vanadium, manganese, copper in prepared calibration sample print respectively, utilize the correction that Theoretical Alpha carries out between element, the calibration curve of fluorescence intensity level after setting up constituent content and correcting; Obtain slope and the intercept of calibration curve;
4) mensuration of testing sample element
According to step 2) method of preparing calibration sample print prepares testing sample print, recycling Xray fluorescence spectrometer analyzes testing sample print, obtain the fluorescence intensity level after titanium, iron, calcium, magnesium, aluminium, silicon, phosphorus, potassium, vanadium, manganese, copper correction, the constituent content of testing sample after calculating calcination, constituent content value in testing sample after final acquisition loss on ignition corrects, used formula is as follows:
Wherein, a: Slope of Calibration Curve; B: calibration curve intercept; I
c: fluorescence intensity (Kcps) after element correction;
E
x: the constituent content (%) of the testing sample after calcination.
Wherein, E
cx: constituent content after loss on ignition corrects; LOI: sample loss on ignition (%).
Wherein, m
0: initial sample mass; m
1: sample quality (g) after calcination.
Above-mentioned steps 2) in flux be the potpourri of lithium tetraborate, di-iron trioxide, silicon dioxide, 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) in the temperature of high-temperature fusion be 1050 DEG C, 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 of the present invention is high, social benefit is obvious.
Accompanying drawing explanation
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 (Al2O3) 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
First prepare the calibration sample for setting up calibration curve, calibration sample includes the element of variety classes, different content respectively.Wherein the number of calibration sample should meet 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 coordinate with high purity reagent prepares calibration sample.The national standard material adopted 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
3.A kind of concrete compound method of calibration sample is in table 1.
Table 1: the preparation of calibration sample
2) series of calibration sample print is prepared
Take about 2.0g calibration sample (being accurate to 0.1mg), in muffle furnace, at 1000 DEG C, calcination, to constant weight, is cooled to room temperature, is placed in exsiccator for subsequent use, calculates burning decrement by formula (3).
Sample after accurately taking 0.6g calcination respectively and 9.0g flux (being accurate to 0.1mg), after both fully mixing, be placed in platinum-Jin crucible, melting 20min at 1050 DEG C, centre is at least shaken 3 times and is mixed, 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 experiment to flux, and finally determine that flux is the potpourri of lithium tetraborate, di-iron trioxide, silicon dioxide, wherein the mass ratio of lithium tetraborate, di-iron trioxide, silicon dioxide is 16:1:1.The mixed flux that the present invention uses, due to containing di-iron trioxide, silicon dioxide, compares the melting that simple lithium tetraborate is more conducive to high titanium slag sample.This is that cause the randomness of boron-oxygen network to increase after embedding boron-oxygen network, cyberspace increases, and titanium more easily dissolves wherein because the affinity of silicon, iron and oxygen is comparatively strong.
3) foundation of calibration curve
The analysis print Xray fluorescence spectrometer of preparation is measured respectively the fluorescence intensity level of titanium, iron, calcium, magnesium, aluminium, silicon, phosphorus, potassium, vanadium, manganese, copper, utilize the correction that Theoretical Alpha carries out between element, and set up constituent content and the working curve (accompanying drawing 1-11) after correcting between fluorescence intensity; 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 X-ray fluorescence spectra analysis of testing sample, recycling Xray fluorescence spectrometer analyzes sample print, obtain titanium, iron, calcium, magnesium, aluminium, silicon, phosphorus, potassium, vanadium, manganese, the fluorescence intensity level of copper, utilize the correction that Theoretical Alpha carries out between element, obtain correcting rear fluorescence intensity level, after correcting, fluorescence intensity level substitutes into formula (1), calculate the constituent content of the testing sample after calcination, finally obtain the testing sample constituent content (calculating by formula (2)) after loss on ignition correction, formula (1) and formula (2) are documented in summary of the invention part.
Below in conjunction with specific embodiment, method of the present invention is described in detail.
Embodiment 1
1) preparation of standard series print
Reference table 1 proportioning takes national standard material and calibration sample prepared by high purity reagent, all weighings are all accurate to 0.1mg, add 8.0g lithium tetraborate, 0.5g di-iron trioxide, 0.5g silicon dioxide respectively, after abundant mixing, be placed in platinum-Jin crucible, in 1050 DEG C of melting 20min, midfeather is shaken more than 3 times and is mixed, pour in the platinum-Jin mould of preheating afterwards, standard model print is made in cooling.
2) foundation of calibration curve
Select series of 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 rear following list of fluorescence intensity level of correction.
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
The calibration curve of each element is set up, titania calibration curve (y=4.0893x-0.2318 R from above-mentioned data
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 (Al2O3) 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) sample preparation is analyzed
Utilize planetary-type grinding machine to grind high titanium slag sample Ti00, prepared sizes are less than 100 orders and analyze sample, are placed in exsiccator for subsequent use.
The mensuration of burning decrement: clean porcelain crucible with distilled water, dries, in 1000 DEG C of calcinations to constant weight, cools for subsequent use.Take about 2.0g predrying sample Ti00 to be measured, be accurate to 0.1mg, in 1000 DEG C of muffle furnaces, calcination is to constant weight, is cooled to room temperature, is placed in exsiccator, calculates burning decrement by formula (3).
4) sample melted is analyzed
Accurately take the high titanium slag sample Ti00(after 8.0g lithium tetraborate, 0.5g di-iron trioxide, 0.5g silicon dioxide and 0.6g calcination and be all accurate to 0.1mg), after abundant mixing, be placed in platinum-Jin crucible, in 1050 DEG C of melting 20min, midfeather is shaken more than 3 times and is mixed, pour in the platinum-Jin mould of preheating afterwards, the print of testing sample is made in cooling.
5) analyze sample to measure
After instrument stabilizer, select suitable calibration sample print to carry out the drift correction of instrument, then carry out analysis sample print and measure, the fluorescence intensity level after the element correction obtained is substituted into the correction equation of each element, namely obtain 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%.
Embodiment 2
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) sample preparation is analyzed
Utilize planetary-type grinding machine to grind high titanium slag sample Ti01, prepared sizes are less than 100 orders and analyze sample, are placed in exsiccator for subsequent use.
The mensuration of burning decrement: clean porcelain crucible with distilled water, dries, in 1000 DEG C of calcinations to constant weight, cools for subsequent use.Take about 2.0g predrying sample Ti01 to be measured, be accurate to 0.1mg, in 1000 DEG C of muffle furnaces, calcination is to constant weight, is cooled to room temperature, is placed in exsiccator, calculates burning decrement by formula (4).
4) sample melted is analyzed
Accurately take the high titanium slag sample Ti01(after 8.0g lithium tetraborate, 0.5g di-iron trioxide, 0.5g silicon dioxide and 0.6g calcination respectively and be all accurate to 0.1mg) 8 parts, after abundant mixing, be placed in platinum-Jin crucible, in 1050 DEG C of melting 20min, midfeather is shaken more than 3 times and is mixed, pour in the platinum-Jin mould of preheating afterwards, cooling in flakes, obtains 8 and analyzes print.
6) analyze sample to measure
Measuring method is with example 1.The relative standard deviation that the method magnesium, aluminium, silicon, potassium, calcium, titanium, vanadium, manganese, iron, copper are analyzed is as shown in table 14, and result shows, the method has higher precision.
The precision of table 14 method
Embodiment 3
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) sample preparation is analyzed
Utilize planetary-type grinding machine to grind ilmenite concentrate standard substance YSBC19716-2003, prepared sizes are less than 100 orders and analyze sample, are placed in exsiccator for subsequent use.
The mensuration of burning decrement: clean porcelain crucible with distilled water, dries, in 1000 DEG C of calcinations to constant weight, cools for subsequent use.Take about 2.0g predrying ilmenite concentrate standard substance YSBC19716-2003 to be measured, be accurate to 0.1mg, in 1000 DEG C of muffle furnaces, calcination is to constant weight, is cooled to room temperature, is placed in exsiccator, calculates burning decrement by formula (4)
4) sample melted is analyzed
Accurately take the ilmenite concentrate standard substance YSBC19716-2003(after 8.0g lithium tetraborate, 0.5g di-iron trioxide, 0.5g silicon dioxide and 0.6g calcination respectively and be all accurate to 0.1mg) 8 parts, after abundant mixing, be placed in platinum-Jin crucible, in 1050 DEG C of melting 20min, midfeather is shaken more than 3 times and is mixed, pour in the platinum-Jin mould of preheating afterwards, cooling in flakes, obtains 8 and analyzes print.
5) analyze sample to measure
Measuring method is with example 1, and ilmenite concentrate standard substance YSBC19716-2003 measurement result is consistent with given value, and result is as shown in Table 15, and method accuracy is high.(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 high titanium slag, iron, calcium, magnesium, aluminium, silicon, phosphorus, potassium, vanadium, manganese, copper accurately, method has higher preci-sion and accuracy, the quick multianalysis of high titanium slag can be realized, meet the requirement of China's import high titanium slag quality restriction.
Claims (2)
1. utilize X-ray fluorescence spectra to analyze a method for element in 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:
The calibration sample of preparation for setting up calibration curve, calibration sample includes the element of variety classes, different content respectively; Element is wherein any one or several in titanium, iron, calcium, magnesium, aluminium, silicon, phosphorus, potassium, vanadium, manganese, copper;
2) calibration sample print is prepared
After the calibration sample after calcination and flux mixing, melting under high temperature, pours in the platinum-Jin mould of preheating after being mixed, calibration sample print is made in cooling;
3) foundation of calibration curve
Xray fluorescence spectrometer is utilized to measure the fluorescence intensity level of titanium, iron, calcium, magnesium, aluminium, silicon, phosphorus, potassium, vanadium, manganese, copper in prepared calibration sample print respectively, utilize the correction that Theoretical Alpha carries out between element, the calibration curve of fluorescence intensity level after setting up constituent content and correcting; Obtain slope and the intercept of calibration curve;
4) mensuration of testing sample element
According to step 2) method of preparing calibration sample print prepares testing sample print, recycling Xray fluorescence spectrometer analyzes testing sample print, obtain the fluorescence intensity level after titanium, iron, calcium, magnesium, aluminium, silicon, phosphorus, potassium, vanadium, manganese, copper correction, the constituent content of testing sample after calculating calcination, constituent content value in testing sample after final acquisition loss on ignition corrects, used formula is as follows:
E
x＝(a×I
c+b) (1)
Wherein, a: Slope of Calibration Curve; B: calibration curve intercept; I
c: fluorescence intensity Kcps after element correction; Ex: the constituent content of the testing sample after calcination:
E
cx＝E
x(100-LOI)/100 (2)
Wherein, E
cx: constituent content after loss on ignition corrects;
LOI: sample loss on ignition (%);
Wherein, m
0: initial sample mass; m
1: sample quality after calcination;
Described step 2) in flux be the potpourri of lithium tetraborate, di-iron trioxide, silicon dioxide, and the mass ratio of lithium tetraborate, di-iron trioxide, silicon dioxide is 16:1:1; And the mass ratio of flux and sample is 15:1.
2. the method for claim 1, is characterized in that described step 2) in the temperature of high-temperature fusion be 1050 DEG C, the melting time is 20min.
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