CN102519942A - Method for determining content of lanthanum and cerium of rare-earth silico-calcium alloy - Google Patents
Method for determining content of lanthanum and cerium of rare-earth silico-calcium alloy Download PDFInfo
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Abstract
The invention discloses a method for determining content of lanthanum and cerium of a rare-earth silico-calcium alloy, and belongs to the technical field of analytical chemistry. The method provided by the invention comprises the following steps of dissolving a sample by nitric acid and hydrofluoric acid, carrying out fluorine removal by perchloric acid fuming, carrying out salt dissolution by dilute hydrochloric acid, carrying out volume metering, and carrying out determination by an inductively-coupled plasma emission spectrometer. The method provided by the invention can realize rapid and accurate determination of the content of lanthanum and cerium of a rare-earth silico-calcium alloy.
Description
One, technical field
The invention belongs to technical field of analytical chemistry, relate to the quantitative analysis tech of lanthanum, cerium in a kind of rare earth silicon-calcium.
Two, background technology
Rare earth silicon-calcium is mainly used in deoxidation, inclusion modification and microalloying effect in smelting process.Because the special role and the cost of lanthanum, cerium are higher, it is extremely important therefore accurately to measure its content, and at present, the analysis of lanthanum, cerium does not still have standard method in the rare earth silicon-calcium, 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 lanthanum, cerium content in a kind of rare earth silicon-calcium, utilize this method can accurately measure the content of lanthanum in the rare earth silicon-calcium, cerium.
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 lanthanum, cerium, 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 1400W from 1000W) of power, line strength of lanthanum, cerium increases, and background intensity also increases;
2) cooling gas flow increases to 0.4L/min from 0.1L/min, and line strength of lanthanum, cerium does not have significant change;
3) the atomization gas flow increases to 1.20L/min from 0.70L/min, wherein increases to 0.95L/min by 0.75L/min, and line strength of lanthanum, cerium obviously reduces, and increases to 1.20L/min from 0.95L/min, and line strength of lanthanum, cerium does not have significant change.
According to the combined influence degree of factors such as power, atomization gas flow, cooling gas flow, lanthanum, cerium 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 0.80L/min, cooling gas flow 0.2L/min, adopt radially and measure.
2, the selection of analysis spectral line
The lanthanum, cerium that adopt the single element titer of a certain amount of lanthanum, cerium and contain a certain amount of calcium base and iron-based mix
Standard solution, the analysis spectral line to lanthanum, cerium scans respectively, select peak shape good, disturb less, spectral line that background is low is as the analytical line of lanthanum, cerium, i.e. La 408.672nm; Ce 418.660nm.
3, coexistence elements interference experiment
Because rare earth silicon-calcium when dissolved samples, adopts nitration mixture such as hydrofluorite, in course of dissolution, silicon disperses with the SiF4 form, and therefore, the content of silicon is extremely low in the mensuration system, does not influence lanthanum, cerium mensuration.
3.1 the influence that matrix element calcium is measured lanthanum, cerium content
Pipette 5% element lanthanum to be measured, cerium respectively, add 0.00%, 5.00%, 10.00%, 15.00% calcium standard solution successively, measure by experimental technique, all within 95%～105% scope, the result sees table 1 to each element determination recovery.
Table 1: matrix element calcium influence %
| Ca standard solution addition | 0.00 | 5.00 | 10.00 | 15.00 |
| La | 5.01 | 4.98 | 4.96 | 5.03 |
| Ce | 4.97 | 4.99 | 5.02 | 5.00 |
The result shows: calcium≤15.00% o'clock, do not have remarkable interference to the mensuration of lanthanum, cerium.Because the content of calcium is about 30% in the calcium-silicon, therefore, when the preparation working curve, the calcium of coupling 15%.
3.2 the influence that matrix element iron is measured lanthanum, cerium content
Pipette 5% element lanthanum to be measured, cerium respectively, add 0.00%, 5.00%, 10.00%, 15.00% iron standard solution successively, measure by experimental technique, lanthanum, cerium are measured the recovery all within 95%～105% scope, and the result sees table 2.
Table 2: matrix element iron influence %
| Fe standard solution addition | 0.00 | 5.00 | 10.00 | 15.00 |
| La | 4.99 | 5.00 | 5.02 | 4.97 |
| Ce | 4.98 | 4.96 | 5.01 | 5.03 |
The result shows: barium≤15.00% o'clock, do not have remarkable interference to the mensuration of lanthanum, cerium.Because the content of iron is about 30% in the calcium-silicon, therefore, when the preparation working curve, the iron of coupling 15%.
3.3 hydrofluorite is to the influence of lanthanum, cerium
Pipetting 0.50%, 1.00%, 5.00%, 8.00% element lanthanum to be measured, cerium respectively is placed in 4 300mL polytetrafluoroethylene beakers; By experimental technique dissolve, be fuming, constant volume, employing inductive coupling plasma emission spectrograph measure, the result sees table 3.
Table 3: hydrofluorite is to the % that influences of lanthanum, cerium
The result shows: fluorine does not produce interference (fluorine and rare earth do not generate deposition, so do not influence its accurate mensuration) to the mensuration of rare earth during sample dissolution.
3.5 the interference of coexistence elements
Standard solution with lanthanum, each element of cerium; Other coexistence elements that add different amounts respectively carry out the interference test between element; The result shows: when Mg≤5%, Al≤5%, P≤3%, Mn≤3%, Ti≤3.00%, V≤5.00%, Ni, Nb≤1%;, Mo≤0.5%,, Cr, Cu≤0.2% o'clock do not disturb the mensuration of lanthanum, cerium, the result sees table 4.
Table 4: the interference % of coexistence elements
3.4 confirming of working curve, related coefficient
Adopting the series standard solution disposed, is horizontal ordinate with the mass percent of lanthanum, cerium, and emissive porwer is an ordinate, draws serial working curve, and the facies relationship number average that lanthanum, cerium are measured is more than 0.9999.
Result according to above-mentioned experiment obtains is applied to the assay method of lanthanum in the rare earth silicon-calcium, cerium content with the related parameter of confirming that has.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 polytetrafluoroethylene beaker, add nitric acid 8mL～10mL of ρ 1.42, add hydrofluorite 4mL～6mL of ρ 1.13; Low-temperature heat to sample dissolves fully, adds perchloric acid 4mL～6mL of ρ 1.67, continues to be heated to and emits the white cigarette of perchloric acid and be concentrated into the wet salt shape; Take off; The hydrochloric acid 10mL dissolved salts that adds 10mL water, ρ 1.19 moves in the 250mL volumetric flask, is diluted with water to scale, shakes up; In company with the band reagent blank, adopt inductive coupling plasma emission spectrograph to measure.
The drafting of working curve
In one group of 250mL volumetric flask; Pipetting concentration respectively is the calcium standard solution 3.00mL of 10.00mg/mL and the iron standard solution 3.00mL that concentration is 5.00mg/mL; Add the hydrochloric acid 10mL of 10mL water, ρ 1.19, get lanthanum, cerium standard solution 0,0.50,1.00,2.00,4.00,6.00,8.00mL that concentration is 1.0mg/mL respectively, be diluted with water to scale and shake up; The employing inductively coupled plasma atomic emission spectrometer is measured; With lanthanum, cerium massfraction is horizontal ordinate, and intensity is ordinate, the drawing curve.
Computing formula is:
W in the formula (M)-the represent massfraction of lanthanum, cerium, %;
The concentration numerical value of lanthanum, cerium in the C-sample solution, mg/mL;
C
0The concentration numerical value of lanthanum, cerium 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 lanthanum, cerium in a kind of rare earth silicon-calcium, has filled up the blank of lanthanum, cerium content analysis field in the rare earth silicon-calcium.
The sensing range of this method is: lanthanum 0.01%～8.00%., cerium 0.01%～8.00%.
Four, embodiment:
Below in conjunction with embodiment the present invention is done further description.
Embodiment 1
With 1
#Broken, the grinding of rare earth silicon-calcium, making it become granularity is 120 purpose samples.
Take by weighing the 0.1000g sample and place the 300mL polytetrafluoroethylene beaker, add the nitric acid 8mL of ρ 1.42, add the hydrofluorite 4mL of ρ 1.13; Low-temperature heat to sample dissolves fully, adds the perchloric acid 4mL of ρ 1.67, continues to be heated to and emits the white cigarette of perchloric acid and be concentrated into the wet salt shape; Take off, add the hydrochloric acid 10mL dissolved salts of 10mL water, ρ 1.19, 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, measure the result and see table 5.
The drafting of working curve
In one group of 250mL volumetric flask; Pipetting concentration respectively is the calcium standard solution 3.00mL of 10.00mg/mL and the iron standard solution 3.00mL that concentration is 5.00mg/mL; Add the hydrochloric acid 10mL of 10mL water, ρ 1.19, get lanthanum, cerium standard solution 0,0.50,1.00,2.00,4.00,6.00,8.00mL that concentration is 1.0mg/mL respectively, be diluted with water to scale and shake up; The employing inductively coupled plasma atomic emission spectrometer is measured; With lanthanum, cerium massfraction is horizontal ordinate, and intensity is ordinate, the drawing curve.
Computing formula is:
W in the formula (M)-the represent massfraction of lanthanum, cerium, %;
The concentration numerical value of lanthanum, cerium in the C-sample solution, mg/mL;
C
0The concentration numerical value of lanthanum, cerium in the-blank solution, mg/mL;
The quality numerical value of m-test portion, g.
Embodiment 2
With 2
#Broken, the grinding of rare earth silicon-calcium, making it become granularity is 120 purpose samples.
Take by weighing the 0.1000g sample and place the 300mL polytetrafluoroethylene beaker, add the nitric acid 10mL of ρ 1.42, add the hydrofluorite 5mL of ρ 1.13; Low-temperature heat to sample dissolves fully, adds the perchloric acid 5mL of ρ 1.67, continues to be heated to and emits the white cigarette of perchloric acid and be concentrated into the wet salt shape; Take off, add the hydrochloric acid 10mL dissolved salts of 10mL water, ρ 1.19, move in the 250mL volumetric flask; Be diluted with water to scale, shake up,, adopt inductive coupling plasma emission spectrograph to measure in company with the band reagent blank; Computing formula is measured the result and is seen table 5 with embodiment 1.
The drafting of working curve
In one group of 250mL volumetric flask; Pipetting concentration respectively is the calcium standard solution 3.00mL of 10.00mg/mL and the iron standard solution 3.00mL that concentration is 5.00mg/mL; Add the hydrochloric acid 10mL of 10mL water, ρ 1.19, get lanthanum, cerium standard solution 0,0.50,1.00,2.00,4.00,6.00,8.00mL that concentration is 1.0mg/mL respectively, be diluted with water to scale and shake up; The employing inductively coupled plasma atomic emission spectrometer is measured; With lanthanum, cerium massfraction is horizontal ordinate, and intensity is ordinate, the drawing curve.
Embodiment 3
With 1
#Broken, the grinding of rare earth silicon-calcium, making it become granularity is 120 purpose samples.
Take by weighing the 0.1000g sample and place the 300mL polytetrafluoroethylene beaker, add the nitric acid 10mL of ρ 1.42, add the hydrofluorite 5mL of ρ 1.13; Low-temperature heat to sample dissolves fully, adds the perchloric acid 5mL of ρ 1.67, continues to be heated to and emits the white cigarette of perchloric acid and be concentrated into the wet salt shape; Take off, add the hydrochloric acid 10mL dissolved salts of 10mL water, ρ 1.19, move in the 250mL volumetric flask; Be diluted with water to scale, shake up,, adopt inductive coupling plasma emission spectrograph to measure in company with the band reagent blank; Computing formula is measured the result and is seen table 5 with embodiment 1.
The drafting of working curve
In one group of 250mL volumetric flask; Pipetting concentration respectively is the calcium standard solution 3.00mL of 10.00mg/mL and the iron standard solution 3.00mL that concentration is 5.00mg/mL; Add the hydrochloric acid 10mL of 10mL water, ρ 1.19, get lanthanum, cerium standard solution 0,0.50,1.00,2.00,4.00,6.00,8.00mL that concentration is 1.0mg/mL respectively, be diluted with water to scale and shake up; The employing inductively coupled plasma atomic emission spectrometer is measured; With lanthanum, cerium massfraction is horizontal ordinate, and intensity is ordinate, the drawing curve.
Embodiment 4
Take by weighing 0.1000g silico-calcium standard model and place the 300mL polytetrafluoroethylene beaker, add and to be equivalent in the 0.1000g silico-calcium standard model 2.00% lanthanum, cerium standard solution, add the nitric acid 8mL of ρ 1.42; Add the hydrofluorite 5mL of ρ 1.13, low-temperature heat to sample dissolves fully, adds the perchloric acid 4mL of ρ 1.67; Continue to be heated to and emit the white cigarette of perchloric acid and be concentrated into the wet salt shape, take off, add the hydrochloric acid 10mL dissolved salts of 10mL water, ρ 1.19; Move in the 250mL volumetric flask, 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 computing formula is measured the result and seen table 5 with embodiment 1.
The drafting of working curve
In one group of 250mL volumetric flask; Pipetting concentration respectively is the calcium standard solution 3.00mL of 10.00mg/mL and the iron standard solution 3.00mL that concentration is 5.00mg/mL; Add the hydrochloric acid 10mL of 10mL water, ρ 1.19, get lanthanum, cerium standard solution 0,0.50,1.00,2.00,4.00,6.00,8.00mL that concentration is 1.0mg/mL respectively, be diluted with water to scale and shake up; The employing inductively coupled plasma atomic emission spectrometer is measured; With lanthanum, cerium massfraction is horizontal ordinate, and intensity is ordinate, the drawing curve.
Embodiment 5
Take by weighing 0.1000g silico-calcium standard model and place the 300mL polytetrafluoroethylene beaker, add and to be equivalent in the 0.1000g silico-calcium standard model 5.00% lanthanum, the nitric acid 9mL that the cerium standard solution adds ρ 1.42, add the hydrofluorite 6mL of ρ 1.13; Low-temperature heat to sample dissolves fully, adds the perchloric acid 4mL of ρ 1.67, continues to be heated to and emits the white cigarette of perchloric acid and be concentrated into the wet salt shape; Take off, add the hydrochloric acid 10mL dissolved salts of 10mL water, ρ 1.19, move in the 250mL volumetric flask; Be diluted with water to scale, shake up,, adopt inductive coupling plasma emission spectrograph to measure in company with the band reagent blank; Computing formula is measured the result and is seen table 5 with embodiment 1.
The drafting of working curve
In one group of 250mL volumetric flask; Pipetting concentration respectively is the calcium standard solution 3.00mL of 10.00mg/mL and the iron standard solution 3.00mL that concentration is 5.00mg/mL; Add the hydrochloric acid 10mL of 10mL water, ρ 1.19, get lanthanum, cerium standard solution 0,0.50,1.00,2.00,4.00,6.00,8.00mL that concentration is 1.0mg/mL respectively, be diluted with water to scale and shake up; The employing inductively coupled plasma atomic emission spectrometer is measured; With lanthanum, cerium massfraction is horizontal ordinate, and intensity is ordinate, the drawing curve.
Table 5: measure % as a result
| Sample | Element | Theoretical value | Measured value | Error | Element | Theoretical value | Measured value | Error |
| 1 # | La | 0.154 | Ce | 3.39 | ||||
| 2 # | La | 0.0764 | Ce | 5.37 | ||||
| 1 #+4.00％ | La | 4.15 | 4.18 | +0.03 | Ce | 7.39 | 7.37 | -0.02 |
| Silico-calcium standard specimen+2.00% | La | 1.993 | -0.01 | Ce | 1.988 | -0.01 | ||
| Silico-calcium standard specimen+5.00% | La | 5.02 | +0.02 | Ce | 5.00 | 0.00 |
Claims (2)
1. the assay method of lanthanum, cerium in the rare earth silicon-calcium, it is characterized in that sample through broken, grind, its granularity is 120 orders, determination step is following:
1), taking by weighing the 0.1000g sample places the 300mL polytetrafluoroethylene beaker, nitric acid 8mL～10mL of adding ρ 1.42, hydrofluorite 4mL～6mL of adding ρ 1.13; Low-temperature heat to sample dissolves fully, adds perchloric acid 4mL～6mL of ρ 1.67, continues to be heated to and emits the white cigarette of perchloric acid and be concentrated into the wet salt shape; Take off; The hydrochloric acid 10mL dissolved salts that adds 10mL water, ρ 1.19 moves in the 250mL volumetric flask, is diluted with water to scale, shakes up; In company with the band reagent blank, adopt inductive coupling plasma emission spectrograph to measure;
2), the drafting of working curve
In one group of 250mL volumetric flask; Pipetting concentration respectively is the calcium standard solution 3.00mL of 10.00mg/mL and the iron standard solution 3.00mL that concentration is 5.00mg/mL; Add the hydrochloric acid 10mL of 10mL water, ρ 1.19, get lanthanum, cerium standard solution 0,0.50,1.00,2.00,4.00,6.00,8.00mL that concentration is 1.0mg/mL respectively, be diluted with water to scale and shake up; The employing inductively coupled plasma atomic emission spectrometer is measured; With lanthanum, cerium massfraction is horizontal ordinate, and intensity is ordinate, the drawing curve.
2. the assay method of lanthanum, cerium is characterized in that the nitration mixture sample dissolution in the rare earth silicon-calcium according to claim 1, the perchloric acid defluorination.
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Cited By (10)
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| CN102928426A (en) * | 2012-11-16 | 2013-02-13 | 内蒙古包钢钢联股份有限公司 | Method for detecting cerium content in Fe-Ce intermediate alloy |
| CN102980882A (en) * | 2012-11-16 | 2013-03-20 | 内蒙古包钢钢联股份有限公司 | Measuring method of cerium content of Fe-Ce intermediate alloy |
| CN104777063A (en) * | 2015-03-16 | 2015-07-15 | 内蒙古包钢钢联股份有限公司 | Method for measuring lanthanum content in lanthanum-iron alloy |
| CN104777163A (en) * | 2015-03-16 | 2015-07-15 | 内蒙古包钢钢联股份有限公司 | Method for measuring cerium content in cerium-iron alloy |
| CN105158234A (en) * | 2015-09-18 | 2015-12-16 | 宁夏共享集团股份有限公司 | Method for measuring contents of lanthanum, cerium and yttrium elements in multi-component nodulizing agent by applying ICP-AES method |
| CN105510301A (en) * | 2016-02-14 | 2016-04-20 | 内蒙古包钢钢联股份有限公司 | Method for measuring aluminum, magnesium, calcium, vanadium, titanium, nickel, copper and manganese in rare earth silicon-magnesium alloy |
| CN105738349A (en) * | 2016-02-26 | 2016-07-06 | 内蒙古包钢钢联股份有限公司 | Method for measuring content of vanadium in rare earth alloy |
| CN108037113A (en) * | 2017-11-27 | 2018-05-15 | 西北矿冶研究院 | Method for reducing and dissolving lanthanum-cerium-rare earth polishing powder by adopting liquid-solid phase |
| CN110044943A (en) * | 2019-03-28 | 2019-07-23 | 包头钢铁（集团）有限责任公司 | A method of detection rare earth in steel and field trash chemical combination form |
| CN110987907A (en) * | 2019-12-18 | 2020-04-10 | 北京达博有色金属焊料有限责任公司 | Method for simultaneously measuring cerium content and lanthanum content in gold alloy by using plasma atomic emission spectrometry |
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| CN102928426A (en) * | 2012-11-16 | 2013-02-13 | 内蒙古包钢钢联股份有限公司 | Method for detecting cerium content in Fe-Ce intermediate alloy |
| CN102980882A (en) * | 2012-11-16 | 2013-03-20 | 内蒙古包钢钢联股份有限公司 | Measuring method of cerium content of Fe-Ce intermediate alloy |
| CN104777063A (en) * | 2015-03-16 | 2015-07-15 | 内蒙古包钢钢联股份有限公司 | Method for measuring lanthanum content in lanthanum-iron alloy |
| CN104777163A (en) * | 2015-03-16 | 2015-07-15 | 内蒙古包钢钢联股份有限公司 | Method for measuring cerium content in cerium-iron alloy |
| CN105158234A (en) * | 2015-09-18 | 2015-12-16 | 宁夏共享集团股份有限公司 | Method for measuring contents of lanthanum, cerium and yttrium elements in multi-component nodulizing agent by applying ICP-AES method |
| CN105510301A (en) * | 2016-02-14 | 2016-04-20 | 内蒙古包钢钢联股份有限公司 | Method for measuring aluminum, magnesium, calcium, vanadium, titanium, nickel, copper and manganese in rare earth silicon-magnesium alloy |
| CN105738349A (en) * | 2016-02-26 | 2016-07-06 | 内蒙古包钢钢联股份有限公司 | Method for measuring content of vanadium in rare earth alloy |
| CN108037113A (en) * | 2017-11-27 | 2018-05-15 | 西北矿冶研究院 | Method for reducing and dissolving lanthanum-cerium-rare earth polishing powder by adopting liquid-solid phase |
| CN110044943A (en) * | 2019-03-28 | 2019-07-23 | 包头钢铁（集团）有限责任公司 | A method of detection rare earth in steel and field trash chemical combination form |
| CN110987907A (en) * | 2019-12-18 | 2020-04-10 | 北京达博有色金属焊料有限责任公司 | Method for simultaneously measuring cerium content and lanthanum content in gold alloy by using plasma atomic emission spectrometry |
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Application publication date: 20120627 |