CN106053507A - Analysis method for measuring contents of calcium oxide, silicon dioxide and sulfur in granular ash or active ash by utilizing X-ray fluorescent spectrometry method - Google Patents
Analysis method for measuring contents of calcium oxide, silicon dioxide and sulfur in granular ash or active ash by utilizing X-ray fluorescent spectrometry method Download PDFInfo
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Abstract
The invention discloses an analysis method for measuring contents of calcium oxide, silicon dioxide and sulfur in granular ash or active ash by utilizing an X-ray fluorescent spectrometry method, and belongs to the field of analysis testing methods. The analysis method comprises the following steps: (1), selecting an analysis instrument and element measurement conditions; (2), selecting a standard sample; (3), preparing glass fuse pieces of the standard sample; (4), drawing a calibration curve; and (5) performing element test of the contents of the calcium oxide, the silicon dioxide and the sulfur in a granular ash sample or an active ash sample. The analysis method provided by the invention can simultaneously measure the contents of a plurality of elements in a measurement sample at a short time by establishing the calibration curve, and has the advantages of short analysis time and high accuracy.
Description
Technical field
The invention belongs to analysis test method field, more particularly to a kind of x-ray fluorescence spectrometry granule ash or
Calcium oxide, silicon dioxide and the analysis method of sulfur content in activity ash.
Background technology
Granule ash grey, active is one of widely used main crude fuel in sintering and steel-making.When adding in sintering process
Add 1% quick lime and about improve mixture temperature 17 DEG C, the impact of excessive moistening layer will be reduced thus improve permeability of sintering material bed,
It it is one of enhancements improving Sintering Yield.Practice of Steelmaking shows, activity ash can improve dephosphorization and desulfurization efficiency 80%, with
Time shorten the heat, can react complete with molten steel middle acid substance completely within 3~5min, can significantly shorten steel-making
The scorification time at converter initial stage, improving furnace life more than 40% in addition, the consumption of furnace charge also reduces by 5~8kg/t steel, with 10,000,000/ton
Calculate, annual saving about 15,000,000 yuan, production economy remarkable benefit.
Measure that granule is grey or component many employings titrimetry in active ash, but the method is long for not only analysis time, and
Terminal is grasped bad, and work efficiency ratio is relatively low, and the expense simultaneously consumed is the highest.
Summary of the invention
For solving above-mentioned technical problem, the invention discloses a kind of x-ray fluorescence spectrometry granule ash or activity ash
The analysis method of middle calcium oxide, silicon dioxide and sulfur content.The method is by setting up calibration curve, and within a short period of time can be simultaneously
Measure the content of several compositions in sample, there is the advantage that analysis time is short and accuracy is high.
The invention discloses calcium oxide in a kind of x-ray fluorescence spectrometry granule ash and activity ash, silicon dioxide and
The analysis method of sulfur content.The method comprises the steps:
1) selection analysis instrument and the measuring condition of element: select the detected spectral line of element, crystal, measurement power and survey
The amount time;
2) select standard sample: combine the content of calcium oxide in granule ash grey, active, use the mode of calcination to improve standard
The content of calcium oxide in sample;
3) bead of standard sample is prepared: use fusion method to prepare bead, be placed in by standard sample and contain in advance
Equipped with in the mold platinum crucible of anhydrous lithium tetraborate solvent, add ammonium iodide, then this mold platinum crucible is placed in pre-
First rise to the melting furnace of 1030~1070 DEG C heats 10~25min, after sample melted terminates, pour in platinum mould, cold
But being poured out by the bead made to room temperature, labelled to put into exsiccator stand-by;
4) calibration curve is drawn: to described step 3) bead prepared carries out X-ray fluorescence spectroscopy measurement, entering
On the basis of row overlap of spectral lines interference correction and matrix correction, draw calcium oxide, silicon dioxide and sulfur content in standard sample
Calibration curve;
5) calcium oxide, silicon dioxide and the composition test of sulfur content in granule ash or activity ash sample.
Further, described step 2) select standard sample detailed process as follows:
Select 10~20 limestone with different calcium oxide content or dolomite standard sample, be placed in 100~110
DEG C baking oven in dry 40~80min, be then placed in exsiccator cooling, after being cooled to room temperature, according to the height of calcium oxide content
Low, the standard sample selecting 10~15 calcium oxide contents to come forward position carries out calcination;
The standard sample selecting above-mentioned 10~15 calcium oxide contents to come forward position is numbered, and weighs the most respectively
2.0~3.0g, the quality of each standard sample of accurate recording simultaneously, then be sequentially placed into that indicate sequence number and burnt the ash to constant weight
In ware, and each burning to the quality of the cupel of constant weight weighs in advance and notes down, then the cupel that will be equipped with standard sample is put
Enter temperature to control calcination 1.5~3h in the Muffle furnace between 920~980 DEG C and, to constant weight, be put in exsiccator and be cooled to room temperature,
Then weigh and note down, calculating igloss COEFFICIENT K simultaneously, and
The quality before the standard sample calcination of quality ÷ after K=standard sample calcination.
Yet further, described step 2) select standard sample detailed process as follows:
Select 14 limestone with different calcium oxide content or dolomite standard sample, be placed in the baking oven of 105 DEG C
Middle baking 60min, is then placed in exsiccator cooling, after being cooled to room temperature, according to the height of calcium oxide content, selects 11 oxygen
The standard sample changing calcium content big carries out calcination;
Being numbered above-mentioned 11 calcium oxide standard sample, weigh 2.0~3.0g the most respectively, accurate recording is every simultaneously
The quality of individual standard sample, then be sequentially placed into that indicate sequence number and burnt to the cupel of constant weight, and each burning is to the ash of constant weight
The quality of ware weighs in advance and notes down, then calcination 2h in the Muffle furnace of 950 DEG C put into by the cupel that will be equipped with standard sample
To constant weight, it is put in exsiccator and is cooled to room temperature, then weigh and note down.
Yet further, when preparing bead, the mass ratio of anhydrous lithium tetraborate solvent and each standard sample be 8~
12:1, the mass concentration of described ammonium iodide is 150~200g/L, and the consumption of ammonium iodide is 1~10mL.
Yet further, described step 4) in, the AC+MC synthesized modeling using OXSAS software to provide carries out spectral line simultaneously
Overlapping interference correction and matrix correction, and the formula that correction utilizes is:
In this formula, CiFor to be measured point of concentration: a after calibrated0、a1、a2For the coefficient of fundamental curve, IiFor measure
The intensity of component to be measured, CjFor spectral line interference component or the concentration of matrix interference component, CkFor the concentration of spectral line interference component,
a1k、a2jIt is respectively spectral line interference coefficient and matrix interference coefficient.
The beneficial effect of the analysis method of the present invention:
The inventive method, by setting up calibration curve, measures various component contents in activity ash or granule ash sample, phase
Than conventional titrimetry (also known as wet method), there is short advantage analysis time, and can measure in sample within a short period of time simultaneously
The content of several composition, measurement result accuracy is high.
Accompanying drawing explanation
Fig. 1 is the calibration graph of calcium oxide in granule ash;
Fig. 2 is the calibration graph of silicon dioxide in granule ash;
Fig. 3 is the calibration graph of sulfur in granule ash;
Detailed description of the invention
In order to preferably explain the present invention, it is further elucidated with the main contents of the present invention below in conjunction with specific embodiment, but
Present disclosure is not limited solely to following example.
A kind of x-ray fluorescence spectrometry granule is grey or calcium oxide, silicon dioxide and the analysis of sulfur content in active ash
Method, comprises the steps:
1) selection analysis instrument and the measuring condition of element: select the detected spectral line of element, crystal, measurement power and survey
The amount time;
Wherein, the analytical tool of selection is as follows:
ARL-9900X ray fluorescence spectrometer (power & light company of the U.S.);
HK-4 melting furnace (Wuhan China Tech company limited);
Platinum crucible (95%Pt-5%Au) and platinum mould.
The measuring condition of each element is as shown in table 1:
The measuring condition of each element of table 1
2) select standard sample: combine the content of calcium oxide in granule ash grey, active, use the mode of calcination to improve standard
The content of calcium oxide in sample;
Owing in granule ash grey, active, the content of calcium oxide has reached 70%~90%, currently without so high-load
Calcium oxide standard sample, therefore uses the method for calcination to improve the content of calcium oxide in standard sample;The method of calcination is as follows:
Select the standard sample of 14 different calcium oxide contents, dry prior to putting into after 105 DEG C of baking ovens dry one hour
Cooling down in device, after being cooled to room temperature, the standard sample picking out wherein 11 calcium oxide contents higher carries out scaling loss;By these 11
Standard sample is numbered, and weighs 2g~3g, the simultaneously quality of each standard sample of accurate recording the most respectively, then is sequentially placed into
Indicate sequence number and burnt to the cupel of constant weight, and under each burning to the quality of the cupel of constant weight weighs in advance and notes down
Come, then (the present embodiment is preferably 950 DEG C) calcination 1.5 in the Muffle furnace of 920~980 DEG C put into by the cupel that will be equipped with standard sample
~3h is to constant weight, calcination time controls at 2h, is put in exsiccator and is cooled to room temperature, then weighs and note down, and calculates simultaneously and burns
Subtract the quality before the quality ÷ standard sample calcination after COEFFICIENT K, and K=standard sample calcination.
11 standard sample quality before calcination and the mass change after calcination are as shown in table 2:
The mass change of table 2 standard sample
As shown in Table 2, each standard sample is after calcination, and igloss COEFFICIENT K is the most inconsistent, but mobility is little, explanation
The method using calcination improves this method of the content of calcium oxide in standard sample and has feasibility.
Table 3 be 14 standard sample of above-mentioned selection before calcination, the content distribution table of each material and element;Table 4 is bright
Each material and the content distribution table of element in 11 standard sample after burning.
The content distribution table (%) of table 3 standard sample each material and element before calcination
According to the quality before the quality ÷ standard sample calcination after K=standard sample calcination, calcination is utilized to improve in sample
Each material and the concentration of element, obtained after the calcination shown in table 4 each material and the content distribution of element in 11 standard sample
Table.
The content distribution table (%) of table 4 standard sample each material and element after calcination
As can be seen from Table 4, after using calcination method, the calcium oxide content in each standard sample all improves, substantially
All control between 70~90%, therefore granule can be replaced grey with the standard sample selected or active ash carrys out Criterion work
Curve.
3) bead of standard sample is prepared: use fusion method to prepare bead, by 14 marks without calcination
Quasi-sample and the most accurately weigh 0.6000g through 11 standard sample of calcination, is placed in standard sample and is loaded with in advance
In the mold platinum crucible of 6.0000g anhydrous lithium tetraborate solvent, anhydrous lithium tetraborate, as cosolvent, reduces melt temperature,
Adding 5.0mL ammonium iodide, mass concentration is 180g/L, and this mold platinum crucible, as releasing agent, is then placed in by ammonium iodide
Rise to the melting furnace of 1030~1070 DEG C heats 10~25min in advance, after sample melted terminates, pour in platinum mould,
Being poured out by the bead made after being cooled to room temperature, labelled to put into exsiccator stand-by.
4) calibration curve is drawn: to described step 3) bead prepared carries out X-ray fluorescence spectroscopy measurement, entering
On the basis of row overlap of spectral lines interference correction and matrix correction, draw calcium oxide, silicon dioxide and sulfur content in standard sample
Calibration curve.
The AC+MC synthesized modeling using OXSAS software to provide carries out overlap of spectral lines interference correction and matrix correction simultaneously, and
The formula that correction utilizes is:
In this formula, CiFor to be measured point of concentration: a after calibrated0、a1、a2For the coefficient of fundamental curve, IiFor measure
The intensity of component to be measured, CjFor spectral line interference component or the concentration of matrix interference component, CkFor the concentration of spectral line interference component,
a1k、a2jIt is respectively spectral line interference coefficient and matrix interference coefficient.
Having respectively obtained the calibration curve of main component in granule ash, wherein, Fig. 1 is that the calibration of calcium oxide in granule ash is bent
Line chart;Fig. 2 is the calibration graph of silicon dioxide in granule ash;Fig. 3 is the calibration graph of sulfur in granule ash, and table 5 is calibration
The relevant operating parameter of curve;
The running parameter of table 5 calibration curve
Understanding in conjunction with table 5, the correlation coefficient of calcium oxide calibration curve is 0.99995, the phase of the calibration curve of silicon dioxide
Close coefficient be 0.99983, the correlation coefficient of the calibration curve of sulfur is 0.99872, the correlation coefficient of working curve all 0.998 with
On, therefore, the relative error range of standard curve is all within each element tolerance scope, the most well.
5) calcium oxide, silicon dioxide and the composition test of sulfur content in granule ash or activity ash sample, and therefore test
Demonstrate,prove the preci-sion and accuracy of the calibration curve of above-mentioned making;
51) precision test: using two kinds of methods to carry out precision test, method one is will to be numbered YB1K15010803
Granule ash sample, carry out adding heat fusing and prepare bead, be prepared as two and plural bead, this enforcement is excellent
Select five beads, use X-ray fluorescence spectroscopy to measure these five beads, carrying out overlap of spectral lines interference correction
With measure calcium oxide, silicon dioxide and the content of sulfur in this granule ash sample on the basis of matrix correction, and respectively with chemical score
Contrast also, has obtained the precision data shown in table 6;Method two is to be prepared by the granule ash sample being numbered YB1K15010804
Become a bead, and this bead is used X-ray fluorescence spectroscopy METHOD FOR CONTINUOUS DETERMINATION five times, measure the granule obtained
Calcium oxide, silicon dioxide and the content of sulfur in ash sample, and contrast with chemical score respectively and calculate, obtain the essence shown in table 7
Density data;
The precision (%) of table 6 method one
The precision (%) of table 7 method two
Understand in conjunction with table 6, table 7, use two kinds of different methods to obtain the numerical value of standard deviation and relative standard deviation all
Ratio is relatively low, in the range of allowable error, therefore uses the melting furnace sample preparation in above-mentioned steps and uses X-ray fluorescence spectroscopy
The precision measuring the working curve obtained is all preferable, is entirely capable of meeting the requirement on producing.
52) precision test: choose 9 limestone standard sample without calcination and 29 actual granule ash samples are carried out
This law and wet method measure, and result are compared with asserting value or wet method value, and result is shown in Table 8 respectively, table 9.
Table 8: unburnt limestone standard standard specimen product accuracy test (%)
As shown in Table 8, the content using the unburnt limestone standard standard specimen product of x-ray fluorescence spectrometry is being permitted
Within the range of error permitted.
Table 9: the accuracy test (%) of actual sample
In like manner, as shown in Table 9, use this method x-ray fluorescence spectrometry granule grey or main component in active ash
The method of content is compared with conventional wet method, and measurement range can fluctuate in the range of error allowed.
Therefore, the accuracy using the working curve of this method making is preferable, is entirely capable of meeting granule ash, activity ash online
Analyze the requirement transmitted messages.
Above example is only optimal citing, and is not the restriction to embodiments of the present invention.Except above-described embodiment
Outward, the present invention also has other embodiments.The technical scheme that all employing equivalents or equivalent transformation are formed, all falls within the present invention
The protection domain required.
Claims (5)
1. an x-ray fluorescence spectrometry granule is grey or calcium oxide, silicon dioxide and the analysis side of sulfur content in active ash
Method, it is characterised in that: comprise the steps:
1) selection analysis instrument and the measuring condition of element: when selecting the detected spectral line of element, crystal, measurement power and measure
Between;
2) select standard sample: combine the content of calcium oxide in granule ash grey, active, use the mode of calcination to improve standard sample
The content of middle calcium oxide;
3) bead of standard sample is prepared: use fusion method to prepare bead, be placed in by standard sample and be loaded with in advance
In the mold platinum crucible of anhydrous lithium tetraborate solvent, add ammonium iodide, then this mold platinum crucible is placed in and rises in advance
To the melting furnaces of 1030~1070 DEG C, heat 10~25min, after sample melted terminates, pour in platinum mould, be cooled to
Being poured out by the bead made after room temperature, labelled to put into exsiccator stand-by;
4) calibration curve is drawn: to described step 3) bead prepared carries out X-ray fluorescence spectroscopy measurement, composing
On the basis of line overlap interference correction and matrix correction, draw calcium oxide, silicon dioxide and the calibration of sulfur content in standard sample
Curve;
5) calcium oxide, silicon dioxide and the composition test of sulfur content in granule ash or activity ash sample.
X-ray fluorescence spectrometry granule the most according to claim 1 is grey or calcium oxide in active ash, silicon dioxide and
The analysis method of sulfur content, it is characterised in that: described step 2) select standard sample detailed process as follows:
Select 10~20 limestone with different calcium oxide content or dolomite standard sample, be placed in 100~110 DEG C
Baking oven dries 40~80min, is then placed in exsiccator cooling, after being cooled to room temperature, according to the height of calcium oxide content, choosing
Select 10~15 calcium oxide contents to come the standard sample of forward position and carry out calcination;
The standard sample selecting above-mentioned 10~15 calcium oxide contents to come forward position is numbered, and weighs 2.0 the most respectively
~3.0g, the quality of each standard sample of accurate recording simultaneously, then it is sequentially placed into that indicate sequence number and has burnt the cupel to constant weight
In, and each burning to the quality of the cupel of constant weight weighs in advance and notes down, then the cupel that will be equipped with standard sample is put into
Temperature controls calcination 1.5~3h in the Muffle furnace between 920~980 DEG C and, to constant weight, is put in exsiccator and is cooled to room temperature, so
Rear weighing is also noted down, and calculates igloss COEFFICIENT K simultaneously, and
The quality before the standard sample calcination of quality ÷ after K=standard sample calcination.
X-ray fluorescence spectrometry granule the most according to claim 2 is grey or calcium oxide in active ash, silicon dioxide and
The analysis method of sulfur content, it is characterised in that: described step 2) select standard sample detailed process as follows:
Select 14 limestone with different calcium oxide content or dolomite standard sample, be placed in the baking oven of 105 DEG C baking
60min, is then placed in exsiccator cooling, after being cooled to room temperature, according to the height of calcium oxide content, selects 11 calcium oxide
Content comes the standard sample of forward position and carries out calcination;
Above-mentioned 11 calcium oxide standard sample are numbered, weigh 2.0~3.0g the most respectively, each mark of accurate recording simultaneously
The quality of quasi-sample, then be sequentially placed into that indicate sequence number and burnt to the cupel of constant weight, and each burning is to the cupel of constant weight
Quality weighs in advance and notes down, then the cupel that will be equipped with standard sample is put in the Muffle furnace that temperature control is 950 DEG C
Calcination 2h, to constant weight, is put in exsiccator and is cooled to room temperature, then weigh and note down.
X-ray fluorescence spectrometry granule the most according to claim 1 is grey or calcium oxide in active ash, silicon dioxide and
The analysis method of sulfur content, it is characterised in that: when preparing bead, anhydrous lithium tetraborate solvent and the matter of each standard sample
Amount ratio is 8~12:1, and the mass concentration of described ammonium iodide is 150~200g/L, and the consumption of ammonium iodide is 1~10mL.
X-ray fluorescence spectrometry granule the most according to claim 1 is grey or calcium oxide in active ash, silicon dioxide and
The analysis method of sulfur content, it is characterised in that: described step 4) in, use the AC+MC synthesized modeling that OXSAS software provides simultaneously
Carry out overlap of spectral lines interference correction and matrix correction, and the formula that correction utilizes be:
In this formula, CiFor to be measured point of concentration after calibrated, a0、a1、a2For the coefficient of fundamental curve, IiTo be measured for measure
The intensity of component, CjFor spectral line interference component or the concentration of matrix interference component, CkFor the concentration of spectral line interference component, a1k、a2j
It is respectively spectral line interference coefficient and matrix interference coefficient.
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