CN102507538A - Method for measuring content of lanthanum and cerium in rare earth silicon-calcium-barium - Google Patents
Method for measuring content of lanthanum and cerium in rare earth silicon-calcium-barium Download PDFInfo
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Abstract
A method for measuring the content of lanthanum and cerium in rare earth silicon-calcium-barium belongs to the technical field of analytical chemistry. The method includes: using hydrochloric acid, nitric acid and hydrofluoric acid to dissolve a test sample; using smoking perchloric acid to expel fluorine; diluting the test sample to a specified volume; and measuring the content by an inductively coupled plasma emission spectrometer. The method can be used for rapidly and accurately measuring the content of the lanthanum and the cerium in the rare earth silicon-calcium-barium.
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 barium.
Two, background technology
Rare earth silicon-calcium barium 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 barium, 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 barium, utilize this method can accurately measure the content of lanthanum, cerium in the rare earth silicon-calcium barium.
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 1450W 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, barium, iron-based mix
Standardization 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 barium 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 the mensuration of lanthanum, cerium content.
3.1 the influence that matrix element calcium is measured lanthanum, cerium content
Pipette 5.00% element lanthanum to be measured, cerium respectively, add 0.00%, 5.00%, 10.00%, 15.00% calcium standard solution successively, measure by experimental technique, each element determination recovery all within 95%～105% scope, is measured the result and is seen table 1.
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: when calcium≤15.00%, the mensuration of lanthanum, cerium content is not had remarkable interference.Because the content of calcium is about 20% in the calsibar alloy, therefore, when the preparation working curve, the calcium of coupling 15%.
3.2 the influence that matrix element barium is measured lanthanum, cerium content
Pipette 5% element lanthanum to be measured, cerium respectively, add 0.00%, 5.00%, 10.00%, 15.00% barium standard solution successively, measure by experimental technique, lanthanum, cerium are measured the recovery all within 95%～105% scope, measure the result and see table 2.
Table 2: matrix element barium influence %
| Ba standard solution addition | 0.00 | 5.00 | 10.00 | 15.00 |
| La | 5.00 | 4.97 | 5.00 | 5.03 |
| Ce | 4.98 | 5.01 | 5.01 | 5.00 |
The result shows: when barium≤15.00%, the mensuration of lanthanum, cerium content is not had remarkable interference.Because the content of barium is about 20% in the calsibar alloy, therefore, when the preparation working curve, coupling content is 15% barium.
3.3 the influence that matrix element iron is measured lanthanum, cerium content
Pipette 5.00% 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, measure the result and see table 3.
Table 3: 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: when iron≤15.00%, the mensuration of lanthanum, cerium content is not had remarkable interference.Because the content of iron is about 20% in the calsibar alloy, therefore, when the preparation working curve, coupling content is 15% iron (iron can not match yet).
3.4 hydrofluorite is to the influence of lanthanum, cerium
Pipetting content respectively and be 0.50%, 1.00%, 5.00%, 8.00% element lanthanum to be measured, cerium is placed in 4 300mL polytetrafluoroethylene beakers; By experimental technique dissolve, be fuming, constant volume, employing inductive coupling plasma emission spectrograph measure, measure the result and see table 4.
Table 4: 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
With the standard solution of lanthanum, each element of cerium, other coexistence elements that add different content respectively carry out the interference test between element, and the result shows: as Mg≤5%, P
2O
5≤5%, MnO≤5%, 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, measure the result and see table 5.
Table 5: 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, cerium content in the rare earth silicon-calcium barium 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 6mL～8mL of ρ 1.42, add hydrofluorite 4mL～6mL of ρ 1.13; The dissolution in low temperature sample, after the reaction calmness, the hydrochloric acid 3mL～5mL that adds ρ 1.19 dissolves to sample fully; Add perchloric acid 4mL～6mL 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; The dissolving with hydrochloric acid salt that adds 20mL (1+1) 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
Measure calcium that concentration is 1.00mg/mL, barium, iron standard solution 15mL number respectively part in the 250mL volumetric flask; Add the hydrochloric acid 20mL of (1+1), get lanthanum, cerium standard solution 0,0.50,1.00,2.00,4.00,6.00,8.00mL that concentration is 1.00mg/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 content in a kind of rare earth silicon-calcium barium, has filled up the blank of lanthanum, cerium content analysis field in the rare earth silicon-calcium barium.
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 barium, 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 7mL of ρ 1.42, add the hydrofluorite 4mL of ρ 1.13; The dissolution in low temperature sample, after the reaction calmness, the hydrochloric acid 3mL that adds ρ 1.19 dissolves to sample fully; Add 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; The dissolving with hydrochloric acid salt that adds 20mL (1+1) 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, measure the result and see table 6.
The drafting of working curve
Measure calcium that concentration is 1.00mg/mL, barium, iron standard solution 15mL number respectively part in the 250mL volumetric flask; Add the hydrochloric acid 20mL of (1+1), get lanthanum, cerium standard solution 0,0.50,1.00,2.00,4.00,6.00,8.00mL that concentration is 1.00mg/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 barium, 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 7mL of ρ 1.42, add the hydrofluorite 5mL of ρ 1.13, the dissolution in low temperature sample; After the reaction calmness, the hydrochloric acid 3mL that adds ρ 1.19 dissolves to sample fully, the perchloric acid 4mL of adding 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 dissolving with hydrochloric acid salt of 20mL (1+1); 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 6 with embodiment 1.
The drafting of working curve
Measure calcium that concentration is 1.00mg/mL, barium, iron standard solution 15mL number respectively part in the 250mL volumetric flask; Add the hydrochloric acid 20mL of (1+1), get lanthanum, cerium standard solution 0,0.50,1.00,2.00,4.00,6.00,8.00mL that concentration is 1.00mg/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 3
#Broken, the grinding of rare earth silicon-calcium barium, 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 7mL of ρ 1.42, add the hydrofluorite 5mL of ρ 1.13, the dissolution in low temperature sample; After the reaction calmness, the hydrochloric acid 3mL that adds ρ 1.19 dissolves to sample fully, the perchloric acid 4mL of adding 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 dissolving with hydrochloric acid salt of 20mL (1+1); 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 6 with embodiment 1.
The drafting of working curve
Measure calcium that concentration is 1.00mg/mL, barium, iron standard solution 15mL number respectively part in the 250mL volumetric flask; Add the hydrochloric acid 20mL of (1+1), get lanthanum, cerium standard solution 0,0.50,1.00,2.00,4.00,6.00,8.00mL that concentration is 1.00mg/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
With 4
#Broken, the grinding of rare earth silicon-calcium barium, 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 7mL of ρ 1.42, add the hydrofluorite 6mL of ρ 1.13, the dissolution in low temperature sample; After the reaction calmness, the hydrochloric acid 3mL that adds ρ 1.19 dissolves to sample fully, the perchloric acid 4mL of adding 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 dissolving with hydrochloric acid salt of 20mL (1+1); 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 6 with embodiment 1.
The drafting of working curve
Measure calcium that concentration is 1.00mg/mL, barium, iron standard solution 15mL number respectively part in the 250mL volumetric flask; Add the hydrochloric acid 20mL of (1+1), get lanthanum, cerium standard solution 0,0.50,1.00,2.00,4.00,6.00,8.00mL that concentration is 1.00mg/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
With 5
#Broken, the grinding of rare earth silicon-calcium barium, 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 7mL of ρ 1.42, add the hydrofluorite 4mL of ρ 1.13, the dissolution in low temperature sample; After the reaction calmness, the hydrochloric acid 3mL that adds ρ 1.19 dissolves to sample fully, the perchloric acid 4mL of adding 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 dissolving with hydrochloric acid salt of 20mL (1+1); 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 6 with embodiment 1.
The drafting of working curve
Measure calcium that concentration is 1.00mg/mL, barium, iron standard solution 15mL number respectively part in the 250mL volumetric flask; Add the hydrochloric acid 20mL of (1+1), get lanthanum, cerium standard solution 0,0.50,1.00,2.00,4.00,6.00,8.00mL that concentration is 1.00mg/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 6
With 6
#Broken, the grinding of rare earth silicon-calcium barium, 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 7mL of ρ 1.42, add the hydrofluorite 5mL of ρ 1.13, the dissolution in low temperature sample; After the reaction calmness, the hydrochloric acid 3mL that adds ρ 1.19 dissolves to sample fully, the perchloric acid 4mL of adding 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 dissolving with hydrochloric acid salt of 20mL (1+1); 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 6 with embodiment 1.
The drafting of working curve
Measure calcium that concentration is 1.00mg/mL, barium, iron standard solution 15mL number respectively part in the 250mL volumetric flask; Add the hydrochloric acid 20mL of (1+1), get lanthanum, cerium standard solution 0,0.50,1.00,2.00,4.00,6.00,8.00mL that concentration is 1.00mg/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 7
With 4
#Broken, the grinding of rare earth silicon-calcium barium, making it become granularity is 120 purpose samples.
Take by weighing the 0.1000g sample and place the 300mL polytetrafluoroethylene beaker, add and to be equivalent in the 0.1000g sample 5.00% lanthanum, cerium standard solution, add the nitric acid 7mL of ρ 1.42, add the hydrofluorite 5mL of ρ 1.13; The dissolution in low temperature sample, after the reaction calmness, the hydrochloric acid 3mL that adds ρ 1.19 dissolves to sample fully, the perchloric acid 4mL of adding 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 dissolving with hydrochloric acid salt of 20mL (1+1); 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 6 with embodiment 1.
The drafting of working curve
Measure calcium that concentration is 1.00mg/mL, barium, iron standard solution 15mL number respectively part in the 250mL volumetric flask; Add the hydrochloric acid 20mL of (1+1), get lanthanum, cerium standard solution 0,0.50,1.00,2.00,4.00,6.00,8.00mL that concentration is 1.00mg/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 8
Take by weighing 0.1000g silico-calcium barium standard model and place the 300mL polytetrafluoroethylene beaker, be equivalent in the 0.1000g sample 0.50% lanthanum, cerium standard solution, add the nitric acid 7mL of ρ 1.42; The hydrofluorite 6mL that adds ρ 1.13, the dissolution in low temperature sample is after the reaction calmness; The hydrochloric acid 3mL that adds ρ 1.19 dissolves to sample fully, and the perchloric acid 4mL of adding 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 dissolving with hydrochloric acid salt of 20mL (1+1), 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 6 with embodiment 1.
The drafting of working curve
Measure calcium that concentration is 1.00mg/mL, barium, iron standard solution 15mL number respectively part in the 250mL volumetric flask; Add the hydrochloric acid 20mL of (1+1), get lanthanum, cerium standard solution 0,0.50,1.00,2.00,4.00,6.00,8.00mL that concentration is 1.00mg/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 9
Take by weighing 0.1000g silico-calcium barium standard model and place the 300mL polytetrafluoroethylene beaker, add and to be equivalent in the 0.1000g sample 2.00% lanthanum, cerium standard solution, add the nitric acid 7mL of ρ 1.42; The hydrofluorite 5mL that adds ρ 1.13, the dissolution in low temperature sample is after the reaction calmness; The hydrochloric acid 3mL that adds ρ 1.19 dissolves to sample fully, and the perchloric acid 4mL of adding 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 dissolving with hydrochloric acid salt of 20mL (1+1), 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 6 with embodiment 1.
The drafting of working curve
Measure calcium that concentration is 1.00mg/mL, barium, iron standard solution 15mL number respectively part in the 250mL volumetric flask; Add the hydrochloric acid 20mL of (1+1), get lanthanum, cerium standard solution 0,0.50,1.00,2.00,4.00,6.00,8.00mL that concentration is 1.00mg/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 6: measure % as a result
| Sample | Element | Theoretical value | Measured value | Error | Element | Theoretical value | Measured value | Error |
| 1 # | La | / | 1.44 | Ce | / | 0.125 | ||
| 2 # | La | / | 3.83 | Ce | / | 0.0213 | ||
| 3 # | La | / | 1.85 | Ce | / | 0.152 | ||
| 4 # | La | / | 2.27 | Ce | / | 0.904 | ||
| 5 # | La | / | 0.275 | Ce | / | 2.16 | ||
| 6 # | La | / | 0.649 | Ce | / | 1.61 | ||
| 4 #+5.00％ | La | 7.27 | 7.32 | +0.05 | Ce | 5.90 | 5.87 | -0.03 |
| Silico-calcium barium standard specimen+0.50% | La | 0.50 | 0.495 | -0.005 | Ce | 0.50 | 0.498 | -0.002 |
| Silico-calcium barium standard specimen+2.00% | La | 2.00 | 2.00 | 0.00 | Ce | 2.00 | 2.01 | +0.01 |
Claims (2)
1. the assay method of lanthanum, cerium content in the rare earth silicon-calcium barium, 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 polytetrafluoroethylene beaker, add nitric acid 6mL～8mL of ρ 1.42, add hydrofluorite 4mL～6mL of ρ 1.13; The dissolution in low temperature sample, after the reaction calmness, the hydrochloric acid 3mL～5mL that adds ρ 1.19 dissolves to sample fully; Add perchloric acid 4mL～6mL 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; The dissolving with hydrochloric acid salt that adds 20mL (1+1) 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, pipette calcium that concentration is 1.00mg/mL, barium, iron standard solution 15mL number respectively part in the 250mL volumetric flask, add the hydrochloric acid 20mL of (1+1); Get lanthanum, cerium standard solution 0,0.50,1.00,2.00,4.00,6.00,8.00mL that concentration is 1.00mg/mL respectively; Being diluted with water to scale and shaking up, adopt inductively coupled plasma atomic emission spectrometer to measure, is horizontal ordinate with lanthanum, cerium massfraction; Intensity is ordinate, the drawing curve.
2. the assay method of lanthanum, cerium content is characterized in that the nitration mixture sample dissolution in the rare earth silicon-calcium barium according to claim 1, the perchloric acid defluorination.
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| CN103512879A (en) * | 2013-09-16 | 2014-01-15 | 内蒙古包钢钢联股份有限公司 | Complexometry joint measurement method for calcium, barium and magnesium contents in silico-calcium barium magnesium alloy |
| CN106290314A (en) * | 2016-08-02 | 2017-01-04 | 内蒙古包钢钢联股份有限公司 | The assay method of content of niobium in rare earth alloy |
| CN112834488A (en) * | 2021-01-05 | 2021-05-25 | 包头钢铁（集团）有限责任公司 | Method for determining contents of lanthanum, cerium, praseodymium, neodymium, samarium, calcium and magnesium in iron ore |
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| 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 |
| CN103512879A (en) * | 2013-09-16 | 2014-01-15 | 内蒙古包钢钢联股份有限公司 | Complexometry joint measurement method for calcium, barium and magnesium contents in silico-calcium barium magnesium alloy |
| CN103512879B (en) * | 2013-09-16 | 2016-06-01 | 内蒙古包钢钢联股份有限公司 | The method of calcium, barium, Mg content in Si Si bond surveyed by a kind of complexometric titration connection |
| CN106290314A (en) * | 2016-08-02 | 2017-01-04 | 内蒙古包钢钢联股份有限公司 | The assay method of content of niobium in rare earth alloy |
| CN112834488A (en) * | 2021-01-05 | 2021-05-25 | 包头钢铁（集团）有限责任公司 | Method for determining contents of lanthanum, cerium, praseodymium, neodymium, samarium, calcium and magnesium in iron ore |
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