CN102393386A - Method for measuring content of calcium, magnesium and silicon in aluminum-based compound deoxidizing slagging constituent - Google Patents
Method for measuring content of calcium, magnesium and silicon in aluminum-based compound deoxidizing slagging constituent Download PDFInfo
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Abstract
A method for measuring the content of calcium, magnesium and silicon in an aluminum-based compound deoxidizing slagging constituent, and belongs to the technical field of analytical chemistry. The method is that hydrochloric acid with finite concentration is used for dissolving a sample, un-dissolved substances is fused by mixed fusion agent after being filtered, washed and incinerated; fused blocks are leached from filtered liquid and diluted to the specified volume; and an inductive coupling plasma emission spectrometer is adopted for measurement. The method has the advantages that the type of reagents used in the measuring process is less, the time is short, the operation is simple and convenient, and the precision and the accuracy are higher, thereby particularly suitable for analyzing a large number of samples.
Description
One, technical field
The invention belongs to technical field of analytical chemistry, relate to the quantitative analysis tech of calcium, magnesium, silicon in a kind of aluminium base complex deoxidization slag former.
Two, background technology
Aluminium base complex deoxidization slag former is mainly used in the sex change of slag in smelting process, the content of its calcium, magnesium, silicon has certain area requirement.At present, the analysis of calcium, magnesium, silicon does not still have method in the aluminium base complex deoxidization slag former, and we have invented this method through experiment.
Three, summary of the invention
The objective of the invention is to disclose the assay method of calcium, magnesium, silicone content in a kind of aluminium base complex deoxidization slag former, utilize this method can accurately measure the content of calcium, magnesium, silicon in the aluminium base complex deoxidization slag former.
At first, confirm the span of correlation parameter through experiment and to the influence factor of assay method.
1, the selection of instrument test condition
With the mixed standard solution that contains calcium, magnesium, silicon, carry out the condition test of power, atomization gas flow, cooling gas flow, mensuration mode (axially, radially) etc. successively, the result shows:
1) along with the increase (increasing to 1450W from 1000W) of power, line strength of calcium, magnesium, silicon increases, and background intensity also increases;
2) cooling gas flow increases to 0.4L/min from 0.1L/min, and line strength of each element does not have significant change;
3) the atomization gas flow increases to 1.20L/min from 0.65L/min, wherein increases to 0.95L/min by 0.75L/min, and line strength of each element obviously reduces, and increases to 1.20L/min from 0.95L/min, and line strength of each element does not have significant change.
According to the combined influence degree of factors such as power, atomization gas flow, cooling gas flow, each element character and high low content to the mensuration result; It is test condition that the related data that line strength is big, background is low is selected in decision; Selection result is: power 1300W, atomization gas flow 0.85L/min, cooling gas flow 0.2L/min, adopt radially and measure.
2, the selection of analysis spectral line
Adopt the single element titer of a certain amount of calcium, magnesium, silicon and contain a certain amount of aluminium base calcium, magnesium, silicon hybrid standard mark liquid; Analysis spectral line to calcium, magnesium, silicon scans respectively; Consult the spectral line storehouse simultaneously; Select peak shape good, disturb less, spectral line that background is low is as the analytical line of calcium, magnesium, silicon, i.e. Ca 317.933nm; Mg 279.077nm; Si 251.611nm, 288.158nm.
3, coexistence elements interference experiment
3.1 matrix element aluminium is to the influence of calcium, magnesium, silica test:
Pipette 2% Elements C a to be measured, Si, Mg respectively; The aluminum standard solution that adds 0%, 5%, 10%, 20%, 30%, 40% different amounts successively; Measure by experimental technique, all within 95%～105% scope, the result sees table 1 to each element determination recovery.
Table 1: aluminium is to the % that influences of calcium, magnesium, silica test
The result shows: when aluminium≤40.00%, the mensuration of calcium, silicon, magnesium is not had remarkable interference.
3.2 the interference of coexistence elements:
With the standard solution (content is seen table 2) of Ca, Si, each element of Mg, other coexistence elements that add different amounts respectively carry out the interference test between element, and the result shows: as MgO≤30%, CaO≤40%, SiO
2≤40%, P
2O
5≤10%, MnO≤15%, Ti≤3.00%, V≤5.00%, BaO≤10.00%, Ni, Nb≤1%,, Mo≤0.5%,, Cr, Cu≤0.2%, F≤11.98% o'clock do not disturb the mensuration of calcium, silicon, magnesium, the result sees table 2.
Table 2: the interference % of coexistence elements
| Element | Ca | Mg | Si | Ca | Mg | Si |
| Mark liquid | 2.00 | 2.00 | 2.00 | 10.00 | 10.00 | 10.00 |
| Measured value | 2.03 | 1.96 | 1.97 | 9.95 | 10.07 | 10.02 |
| The recovery | 102 | 98 | 99 | 99 | 101 | 100 |
3.3 confirming of working curve, related coefficient
Adopting the series standard solution disposed, is horizontal ordinate with the mass percent of calcium, silicon, magnesium, and emissive porwer is an ordinate, draws serial working curve, and the facies relationship number average of each element determination is more than 0.999.
Result according to above-mentioned experiment obtains is applied to the related parameter of confirming that has in the assay method of calcium, magnesium, silicone content in the aluminium base complex deoxidization slag former.
The technical scheme that realizes this method is such, and is sample is broken, to be ground to its granularity be 120 orders; Take by weighing the 0.1000g sample and place the 300mL glass beaker, add 10mL water and make its disperse, add 7mL-13mL hydrochloric acid (ρ 1.19); The dissolution in low temperature sample takes off, filters in the 300mL beaker, the hydrochloric acid solution washing residue with 2% 8～10 times; Wash 2～10 times, residue moves in the platinum crucible together with filter paper, low temperature dry ashing; Add the fusion in 900 ℃ muffle furnace of 1.0g mixed flux and took out cooling in 15 minutes; Extract with mother liquor low temperature, move in the 250mL volumetric flask, be diluted with water to scale, shake up (in company with the band reagent blank) to be measured.The employing inductive coupling plasma emission spectrograph is measured.
The drafting of working curve:
Take by weighing several parts of 0.0250g rafifinals in the 300mL glass beaker, add 30mL (1+1) hydrochloric acid, drip hydrogen peroxide in dissolution in low temperature aluminium; Move in the 250mL volumetric flask; Getting concentration respectively is 1.0mg/mL calcium, magnesium standard solution 0,0.50,1.00,3.00,5.00,7.00,9.00mL, and getting concentration is 0.50mg/mL silicon standard solution 0,0.50,1.00,3.00,5.00,7.00,10.00mL, adds the 1.0g mixed flux; Be diluted with water to scale and shake up employing inductively coupled plasma atomic emission spectrometer mensuration; With calcium, magnesium, siliceous amount mark is horizontal ordinate, and intensity is ordinate, the drawing curve.
Computing formula is:
W in the formula (M)-the represent massfraction of calcium, magnesium, silicon, %;
The concentration numerical value of calcium, magnesium, silicon in the C-sample solution, mg/mL;
C
0The concentration numerical value of calcium, magnesium, silicon in the-blank solution, mg/mL;
The quality numerical value of m-test portion, g.
Outstanding advantage of the present invention is to have set up the assay method of calcium, magnesium, silicon in a kind of aluminium base complex deoxidization slag former, has filled up the blank of calcium, magnesium, silicone content analysis field in the aluminium base complex deoxidization slag former.
The sensing range of this method is: calcium oxide 0.50%～12.00%., magnesium oxide 0.50%～15.00%., silicon dioxide 0.50%～10.00%.
Four, embodiment:
Below in conjunction with embodiment the present invention is done further description.
Embodiment 1
With 1
#Broken, the grinding of aluminium base complex deoxidization slag former, making it become granularity is 120 purpose samples.
Take by weighing the 0.1000g sample and place the 300mL glass beaker, add 10mL water and make its disperse, add 10mL hydrochloric acid (ρ 1.19); The dissolution in low temperature sample takes off, filters in the 300mL beaker, the hydrochloric acid solution washing residue with 2% 10 times; Wash 8 times, residue moves in the platinum crucible together with filter paper, low temperature dry ashing; Add the fusion in 900 ℃ muffle furnace of 1.0g mixed flux and took out cooling in 15 minutes, extract, move in the 250mL volumetric flask with mother liquor low temperature; Be diluted with water to scale, shake up (in company with the band reagent blank); The employing inductive coupling plasma emission spectrograph is measured, and its measured value is the mass percent of calcium oxide, magnesium oxide, silicon dioxide in the aluminium base complex deoxidization slag former, and the result sees table 2.
The drafting of working curve:
Take by weighing several parts of 0.0250g rafifinals in the 300mL glass beaker, add 30mL (1+1) hydrochloric acid, drip hydrogen peroxide in dissolution in low temperature aluminium; Move in the 250mL volumetric flask, getting concentration respectively is 1.0mg/mL calcium, magnesium standard solution 0,0.50,1.00,3.00,5.00,7.00,9.00mL, and getting concentration is 0.50mg/mL silicon standard solution 0,0.50,1.00,3.00,5.00,7.00,10.00mL; Add the 1.0g mixed flux; Being diluted with water to scale and shaking up, adopt inductively coupled plasma atomic emission spectrometer to measure, is horizontal ordinate with calcium, magnesium, siliceous amount mark; Intensity is ordinate, the drawing curve.
Computing formula is:
W in the formula (M)-the represent massfraction of calcium, magnesium, silicon, %;
The concentration numerical value of calcium, magnesium, silicon in the C-sample solution, mg/mL;
C
0The concentration numerical value of calcium, magnesium, silicon in the-blank solution, mg/mL;
The quality numerical value of m-test portion, g.
Embodiment 2
With 2
#Broken, the grinding of aluminium base complex deoxidization slag former, making it become granularity is 120 purpose samples.
Take by weighing the 0.1000g sample and place the 300mL glass beaker, add 10mL water and make its disperse, add 10mL hydrochloric acid (ρ 1.19); The dissolution in low temperature sample takes off, filters in the 300mL beaker, the hydrochloric acid solution washing residue with 2% 10 times; Wash 8 times, residue moves in the platinum crucible together with filter paper, low temperature dry ashing; Add the fusion in 900 ℃ muffle furnace of 1.0g mixed flux and took out cooling in 15 minutes, extract, move in the 250mL volumetric flask with mother liquor low temperature; Be diluted with water to scale, shake up (in company with the band reagent blank), adopt inductive coupling plasma emission spectrograph to measure, its measured value is the mass percent of calcium oxide, magnesium oxide, silicon dioxide in the aluminium base complex deoxidization slag former; Computing formula is with embodiment 1, and the result sees table 2.
The drafting of working curve:
Take by weighing several parts of 0.0250g rafifinals in the 300mL glass beaker, add 30mL (1+1) hydrochloric acid, drip hydrogen peroxide in dissolution in low temperature aluminium; Move in the 250mL volumetric flask, getting concentration respectively is 1.0mg/mL calcium, magnesium standard solution 0,0.50,1.00,3.00,5.00,7.00,9.00mL, and getting concentration is 0.50mg/mL silicon standard solution 0,0.50,1.00,3.00,5.00,7.00,10.00mL; Add the 1.0g mixed flux; Being diluted with water to scale and shaking up, adopt inductively coupled plasma atomic emission spectrometer to measure, is horizontal ordinate with calcium, magnesium, siliceous amount mark; Intensity is ordinate, the drawing curve.
Embodiment 3
With 3
#Broken, the grinding of aluminium base complex deoxidization slag former, making it become granularity is 120 purpose samples.
Take by weighing the 0.1000g sample and place the 300mL glass beaker, add 10mL water and make its disperse, add 10mL hydrochloric acid (ρ 1.19); The dissolution in low temperature sample takes off, filters in the 300mL beaker, the hydrochloric acid solution washing residue with 2% 10 times; Wash 6 times, residue moves in the platinum crucible together with filter paper, low temperature dry ashing; Add the fusion in 900 ℃ muffle furnace of 1.0g mixed flux and took out cooling in 15 minutes, extract, move in the 250mL volumetric flask with mother liquor low temperature; Be diluted with water to scale, shake up (in company with the band reagent blank), adopt inductive coupling plasma emission spectrograph to measure, its measured value is the mass percent of calcium oxide, magnesium oxide, silicon dioxide in the aluminium base complex deoxidization slag former; Computing formula is with embodiment 1, and the result sees table 2.
The drafting of working curve:
Take by weighing several parts of 0.0250g rafifinals in the 300mL glass beaker, add 30mL (1+1) hydrochloric acid, drip hydrogen peroxide in dissolution in low temperature aluminium; Move in the 250mL volumetric flask, getting concentration respectively is 1.0mg/mL calcium, magnesium standard solution 0,0.50,1.00,3.00,5.00,7.00,9.00mL, and getting concentration is 0.50mg/mL silicon standard solution 0,0.50,1.00,3.00,5.00,7.00,10.00mL; Add the 1.0g mixed flux; Being diluted with water to scale and shaking up, adopt inductively coupled plasma atomic emission spectrometer to measure, is horizontal ordinate with calcium, magnesium, siliceous amount mark; Intensity is ordinate, the drawing curve.
Embodiment 4
With 3
#Broken, the grinding of aluminium base complex deoxidization slag former, making it become granularity is 120 purpose samples.
Take by weighing the 0.1000g sample and place the 300mL glass beaker, add calcium oxide standard solution 2.80%, magnesium oxide standard solution 3.32%, silicon dioxide standard solution 4.28% respectively, add 10mL water and make its disperse; Add 11mL hydrochloric acid (ρ 1.19), the dissolution in low temperature sample takes off, filters in the 300mL beaker; Hydrochloric acid solution washing residue with 2% 8 times is washed 8 times, and residue moves in the platinum crucible together with filter paper; Low temperature dry ashing adds the fusion in 900 ℃ muffle furnace of 1.0g mixed flux and took out cooling in 15 minutes, extracts with mother liquor low temperature; Move in the 250mL volumetric flask; Be diluted with water to scale, shake up (in company with the band reagent blank), adopt inductive coupling plasma emission spectrograph to measure, its measured value is the mass percent of calcium oxide, magnesium oxide, silicon dioxide in the aluminium base complex deoxidization slag former; Computing formula is with embodiment 1, and the result sees table 2.
The drafting of working curve:
Take by weighing several parts of 0.0250g rafifinals in the 300mL glass beaker, add 30mL (1+1) hydrochloric acid, drip hydrogen peroxide in dissolution in low temperature aluminium; Move in the 250mL volumetric flask, getting concentration respectively is 1.0mg/mL calcium, magnesium standard solution 0,0.50,1.00,3.00,5.00,7.00,9.00mL, and getting concentration is 0.50mg/mL silicon standard solution 0,0.50,1.00,3.00,5.00,7.00,10.00mL; Add the 1.0g mixed flux; Being diluted with water to scale and shaking up, adopt inductively coupled plasma atomic emission spectrometer to measure, is horizontal ordinate with calcium, magnesium, siliceous amount mark; Intensity is ordinate, the drawing curve.
Embodiment 5
With 3
#Broken, the grinding of aluminium base complex deoxidization slag former, making it become granularity is 120 purpose samples.
Take by weighing the 0.1000g sample and place the 300mL glass beaker, add calcium oxide standard solution 7.00%, magnesium oxide standard solution 5.00% respectively, add 10mL water and make its disperse; Add 10mL hydrochloric acid (ρ 1.19), the dissolution in low temperature sample takes off, filters in the 300mL beaker; Hydrochloric acid solution washing residue with 2% 10 times is washed 8 times, and residue moves in the platinum crucible together with filter paper; Low temperature dry ashing adds the fusion in 900 ℃ muffle furnace of 1.0g mixed flux and took out cooling in 15 minutes, extracts with mother liquor low temperature; Move in the 250mL volumetric flask, be diluted with water to scale, shake up (in company with the band reagent blank), adopt inductive coupling plasma emission spectrograph to measure; Its measured value is the mass percent of calcium oxide, magnesium oxide, silicon dioxide in the aluminium base complex deoxidization slag former, and computing formula is with embodiment 1, and the result sees table 2.
The drafting of working curve:
Take by weighing several parts of 0.0250g rafifinals in the 300mL glass beaker, add 30mL (1+1) hydrochloric acid, drip hydrogen peroxide in dissolution in low temperature aluminium; Move in the 250mL volumetric flask, getting concentration respectively is 1.0mg/mL calcium, magnesium standard solution 0,0.50,1.00,3.00,5.00,7.00,9.00mL, and getting concentration is 0.50mg/mL silicon standard solution 0,0.50,1.00,3.00,5.00,7.00,10.00mL; Add the 1.0g mixed flux; Being diluted with water to scale and shaking up, adopt inductively coupled plasma atomic emission spectrometer to measure, is horizontal ordinate with calcium, magnesium, siliceous amount mark; Intensity is ordinate, the drawing curve.
Table 2 is measured the result
| Sample number into spectrum | Measure element | Theoretical value | This law measured value | Error |
| Aluminium base complex deoxidization slag former 1 #Sample | Calcium oxide | / | 3.23 | |
| Aluminium base complex deoxidization slag former 2 #Sample | Calcium oxide | / | 2.92 | |
| Aluminium base complex deoxidization slag former 3 #Sample | Calcium oxide | / | 3.09 | |
| Aluminium base complex deoxidization slag former 3 #Sample+2.80%, | Calcium oxide | 5.89 | 5.88 | -0.01 |
| Aluminium base complex deoxidization slag former 3 #Sample+7.00%, | Calcium oxide | 10.09 | 10.12 | +0.03 |
| Aluminium base complex deoxidization slag former 1 #Sample | Magnesium oxide | / | 4.45 | |
| Aluminium base complex deoxidization slag former 2 #Sample | Magnesium oxide | / | 4.51 | |
| Aluminium base complex deoxidization slag former 3 #Sample | Magnesium oxide | / | 4.35 | |
| Aluminium base complex deoxidization slag former 3 #Sample+3.32%, | Magnesium oxide | 7.67 | 7.61 | -0.07 |
| Aluminium base complex deoxidization slag former 3 #Sample+5.00%, | Magnesium oxide | 9.35 | 9.31 | -0.04 |
| Aluminium base complex deoxidization slag former 1 #Sample | Silicon dioxide | / | 6.64 | |
| Aluminium base complex deoxidization slag former 2 #Sample | Silicon dioxide | / | 6.44 | |
| Aluminium base complex deoxidization slag former 3 #Sample | Silicon dioxide | / | 6.00 | |
| Aluminium base complex deoxidization slag former 3 #Sample+4.28%, | Silicon dioxide | 10.28 | 10.39 | +0.11 |
Claims (2)
1. the assay method of calcium, magnesium, silicone content in the aluminium base complex deoxidization slag former, it is characterized in that sample through broken, grind, its granularity is 120 orders, determination step is following:
1), take by weighing the 0.1000g sample and place the 300mL glass beaker, add 10mL water and make its disperse, add hydrochloric acid 7～13mL of ρ 1.19; The dissolution in low temperature sample takes off, filters in the 300mL beaker, the hydrochloric acid solution washing residue with 2% 8～10 times; Wash 6～8 times, residue moves in the platinum crucible together with filter paper, low temperature dry ashing; Add the fusion in 900 ℃ muffle furnace of 1.0g mixed flux and took out cooling in 15 minutes,, move in the 250mL volumetric flask with the leaching of mother liquor low temperature; Be diluted with water to scale, shake up,, adopt inductive coupling plasma emission spectrograph to measure in company with the band reagent blank;
2), the drafting of working curve
Take by weighing several parts of 0.0250g rafifinals in the 300mL glass beaker, add the hydrochloric acid 30mL of (1+1), drip hydrogen peroxide in dissolution in low temperature aluminium; Move in the 250mL volumetric flask, get calcium, magnesium standard solution 0,0.50,1.00,3.00,5.00,7.00,9.00mL that concentration is 1.0mg/mL respectively, getting concentration is 0.50mg/mL silicon standard solution 0,0.50,1.00,3.00,5.00,7.00,10.00mL; Add the 1.0g mixed flux; Being diluted with water to scale and shaking up, adopt inductively coupled plasma atomic emission spectrometer to measure, is horizontal ordinate with calcium, magnesium, siliceous amount mark; Intensity is ordinate, the drawing curve.
2. the assay method of calcium, magnesium, silicone content is characterized in that the dissolving with hydrochloric acid sample in the aluminium base complex deoxidization slag former according to claim 1, and insolubles adopts the mixed flux high-temperature fusion.
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| CN102980880A (en) * | 2012-12-06 | 2013-03-20 | 武汉钢铁(集团)公司 | Method for quickly determining calcium fluoride and calcium oxide contents in desulfurizer for steel making |
| CN103175824A (en) * | 2013-02-25 | 2013-06-26 | 内蒙古包钢钢联股份有限公司 | Method for measuring content of silicon and phosphorus in ferromanganese iron by inductively coupled plasma spectrum emission instrument |
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Application publication date: 20120328 |