CN108760722A - The method for measuring the content of La, Ce, Pr, Nd and Sm - Google Patents
The method for measuring the content of La, Ce, Pr, Nd and Sm Download PDFInfo
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- CN108760722A CN108760722A CN201810255441.4A CN201810255441A CN108760722A CN 108760722 A CN108760722 A CN 108760722A CN 201810255441 A CN201810255441 A CN 201810255441A CN 108760722 A CN108760722 A CN 108760722A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
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Abstract
The present invention provides a kind of methods for the content measuring La, Ce, Pr, Nd and Sm, are used for iron ore and clinker, including：Step 1, test solution is prepared；Step 2, standard working solution is prepared；Step 3, calibration curve working solution is prepared；Step 4, the test solution made from the method by step 1 is put into the content that La, Ce, Pr, Nd and Sm element are measured in test equipment with the calibration curve working solution made from step 3 simultaneously.Technical solution through the invention, the precision of the method for the content of measurement La, Ce, Pr, Nd and Sm is good, accuracy is high, detection limit is low.
Description
Technical field
The present invention relates to metallurgical analysis technical fields, in particular to a kind of content measuring La, Ce, Pr, Nd and Sm
Method.
Background technology
Rare earth element plays an important role in terms of metallurgy, is good deoxidation, desulfurizing agent, it, which can eliminate or weaken many, has
The influence of evil impurity, moreover it is possible to improve oxidation resistance, elevated temperature strength and plasticity, fatigue life, corrosion resistance and the crack resistance of steel
Deng.In recent years, the utilization of rare earth element is quickly grown in modern science and technological development application, and the analysis of rare earth element seems
It is particularly important.
Through consulting normative document data, analysis method of traditional analysis method to low content rare earth in iron ore, clinker
For spectrophotometry, such as Arsenazo Ⅲ Photometric Method, DBC-arsenazo photometry, the detection and analysis of these methods are total amount of rare earth,
The content of each rare earth element cannot accurately be analyzed.The maximum feature of photometry is to need to eliminate interference element and flow
Longer, analytical reagent used is more, comparatively laborious.Instrumental method has：X-ray fluorescence spectrometry method measures trace in geological sample
Measure rare earth element；Mass spectrometric determination high-purity scandium, yttrium, holmium, thulium, lutetium oxide in 14 Rare Earths Impurities analysis.
Currently, using La in inductively coupled plasma atomic emission spectrometry and mass spectrometric determination iron ore, clinker,
The analysis method of Ce, Pr, Nd and Sm constituent content fails to develop and use well.
Invention content
The present invention is directed to solve at least one of the technical problems existing in the prior art or related technologies.
For this purpose, one aspect of the present invention is, a kind of method for the content measuring La, Ce, Pr, Nd and Sm is provided.
In view of this, the technical solution of first aspect present invention provides a kind of content measuring La, Ce, Pr, Nd and Sm
Method, be used for iron ore and clinker, which is characterized in that including：
Step 1, test solution is prepared, iron ore is weighed or clinker sample 0.1000g is placed in 250mL polytetrafluoroethylene beakers
(sample, should be placed in porcelain crucible in 600~800 DEG C of 10~15min of calcination by carbon containing sulphur and when higher organic matter in as samples,
Move into beaker again after cooling), add 5mL hydrofluoric acid (ρ 1.13), 10mL hydrochloric acid (ρ 1.19), electric hot plate low-temperature heat to make sample
After decomposition, add 2mL perchloric acid (ρ 1.68), continue to heat, makes perchloric acid smoke to residual volume 1mL hereinafter, slightly cold.Add 5mL salt
Sour (ρ 1.19) heating makes salt dissolve, and removes after nature is cooled to room temperature, is transferred in 100mL volumetric flasks, quarter is diluted to pure water
It spends, shake up, reagent blank is done in company with sample；
Step 2, standard working solution is prepared, the standard working solution includes：La2O3(1000 μ g/mL), CeO2(1000
μ g/mL), Pr6O11(1000 μ g/mL), Nd2O3(1000 μ g/mL), Sm2O3(1000 μ g/mL), Al2O3(1000 μ g/mL), CaO
(1000 μ g/mL), Fe (1000 μ g/mL), MgO (1000 μ g/mL), MnO (1000 μ g/mL) and TiO2(1000 μ g/mL), it is described
Standard liquid is formulated as 100 μ g/mL, 10 μ g/mL, tri- kinds of 1 μ g/mL respectively；
Step 3, calibration curve working solution is prepared, wherein configuring iron ore working curve standard solution includes：At 9
In 250mL polytetrafluoroethylene beakers, iron ore standard specimens of 8 parts of 0.1000g without La, Ce, Pr, Nd and Sm is weighed as bottoming base
Body is shifted by the decomposition of the method acid adding progress sample of step 1, perchloric acid smoked, dissolving with hydrochloric acid salt after being cooled to room temperature respectively
In 9 100mL plastics volumetric flasks made from step 2, La is then pipetted respectively2O3、CeO2、Pr6O11、Nd2O3、Sm2O3Standard
Solution is diluted to scale in 9 100mL volumetric flasks, with pure water, shakes up, and it is hydrochloric acid or hydrochloric acid+tartaric acid to be configured to medium
Measure 2 sets of the standard solution working curve of 9 points of La, Ce, Pr, Nd and Sm constituent content in iron ore；Configure clinker work
Curve standard solution includes：In 6 250mL polytetrafluoroethylene beakers, weighs 5 parts of 0.1000g and be free of La, Ce, Pr, Nd and Sm
Clinker standard specimen as bottoming matrix, carry out the decomposition of sample, perchloric acid smoked, dissolving with hydrochloric acid salt by the method acid adding of step 1
Class is cooled to after room temperature and shifts respectively in 6 100mL plastics volumetric flasks made from step 2, then pipettes La respectively2O3、CeO2、
Pr6O11、Nd2O3、Sm2O3Standard solution is diluted to scale in 6 100mL volumetric flasks, with pure water, shakes up, and is configured to medium and is
The calibration curve working solution 2 for measuring 6 points of La, Ce, Pr, Nd and Sm constituent content in slag of hydrochloric acid or hydrochloric acid+tartaric acid
Set；
Step 4, the test solution made from the method by step 1 and the calibration curve working solution made from step 3 are same
When be put into test equipment measure La, Ce, Pr, Nd and Sm element content, wherein the group of each solvent is divided into：Hydrochloric acid (ρ 1.19,
Top pure grade), hydrochloric acid (5+95), hydrochloric acid (2+98), hydrofluoric acid (ρ 1.13, top pure grade), perchloric acid (ρ 1.68, top pure grade), winestone
Sour (200g/L), mixed solvent：Natrium carbonicum calcinatum+boric acid=2+1 (top pure grade), experimental water are two level pure water.
Wherein, W (tested component) (%)=Wi-W0, in formula：W is the mass percentage of element in the sample；WiFor member
Mass percent of the element in sample to be tested；W0For mass percent of the element in blank solution to be measured.
Preferably, the fit analysis spectral line of La, Ce, Pr, Nd and Sm element is：La 408.672nm,Ce 418.660nm,
Pr 422.293nm、Nd 406.109nm、Sm 359.260nm、Sm 442.434nm。
Further, in step 1, if carbon containing sulphur and when higher organic matter in the iron ore or clinker sample, the iron
Ore or clinker sample are placed in porcelain crucible in 600~800 DEG C of 10~15min of calcination, and it is poly- to move into the 250mL again after cooling
In tetrafluoroethene beaker.
Compared with the existing technology, the method for the content provided by the invention for measuring La, Ce, Pr, Nd and Sm has following excellent
Point：
(1) it selects to be used as bottoming matrix, preparation calibration curve without the iron ore of La, Ce, Pr, Nd and Sm, clinker standard specimen
Working solution keeps measurement result more accurate to eliminate matrix element interference.
(2) the method for the present invention agents useful for same is less, thus has fewer environmental impacts；The range of linearity is wider, and precision is good, accurate
Exactness is high.Measurement range is：
Iron ore each element measurement range：
La:0.0020-5.00%, Ce:0.0020-10.00%, Pr:0.0050-1.00%, Nd:0.005-2.00%,
Sm:0.0050-1.00%
Each element measurement range in clinker：
Ranging from 0.005-the 0.50% of La, Ce, Pr, Nd, Sm.
It measures relative standard deviation and is less than 5%, the rate of recovery is between 97%~104%.
The additional aspect and advantage of the present invention will be set forth in part in the description, and will partly become from the following description
Obviously, or practice through the invention is recognized.
Description of the drawings
The above-mentioned and/or additional aspect and advantage of the present invention will become in the description from combination following accompanying drawings to embodiment
Obviously and it is readily appreciated that, wherein：
Fig. 1 shows the stream of the method for the content according to an embodiment of the invention for measuring La, Ce, Pr, Nd and Sm
Journey schematic diagram；
Specific implementation mode
It is below in conjunction with the accompanying drawings and specific real in order to be more clearly understood that aforementioned aspect of the present invention, feature and advantage
Mode is applied the present invention is further described in detail.It should be noted that in the absence of conflict, the implementation of the application
Feature in example and embodiment can be combined with each other.
Many details are elaborated in the following description to facilitate a thorough understanding of the present invention, still, the present invention may be used also
To be implemented different from other modes described here using other, therefore, protection scope of the present invention is not by described below
Specific embodiment limitation.
As shown in Figure 1, the method for the content according to an embodiment of the invention for measuring La, Ce, Pr, Nd and Sm, packet
It includes：
Step S102 prepares test solution, weighs iron ore or clinker sample 0.1000g is placed in 250mL polytetrafluoroethylene beakers
In, as samples in carbon containing sulphur and when higher organic matter, sample should be placed in porcelain crucible in 600~800 DEG C of calcinations 10~
15min is moved into beaker again after cooling, adds 5mL hydrofluoric acid (ρ 1.13), 10mL hydrochloric acid (ρ 1.19), electric hot plate low-temperature heat
After so that sample is decomposed, adds 2mL perchloric acid (ρ 1.68), continue to heat, make perchloric acid smoke to residual volume 1mL hereinafter, slightly cold.
Add 5mL hydrochloric acid (ρ 1.19) heating that salt is made to dissolve, removes after nature is cooled to room temperature, be transferred in 100mL volumetric flasks, it is dilute with pure water
It releases scale, shake up, reagent blank is done in company with sample；
Step S104, prepares standard working solution, and the standard working solution includes：La2O3(1000 μ g/mL), CeO2
(1000 μ g/mL), Pr6O11(1000 μ g/mL), Nd2O3(1000 μ g/mL), Sm2O3(1000 μ g/mL), Al2O3(1000μg/
ML), CaO (1000 μ g/mL), Fe (1000 μ g/mL), MgO (1000 μ g/mL), MnO (1000 μ g/mL) and TiO2(1000μg/
), mL the standard liquid is formulated as 100 μ g/mL, 10 μ g/mL, tri- kinds of 1 μ g/mL respectively；
Step S106 prepares calibration curve working solution, wherein configuring iron ore working curve standard solution includes：9
In a 250mL polytetrafluoroethylene beakers, iron ore standard specimens of 8 parts of 0.1000g without La, Ce, Pr, Nd and Sm is weighed as bottoming
Matrix is divided by the decomposition of the method acid adding progress sample of step S102, perchloric acid smoked, dissolving with hydrochloric acid salt after being cooled to room temperature
It does not shift in 9 100mL plastics volumetric flasks made from step S104, then pipettes La respectively2O3、CeO2、Pr6O11、Nd2O3、
Sm2O3Standard solution is diluted to scale in 9 100mL volumetric flasks, with pure water, shakes up, be configured to medium be hydrochloric acid or hydrochloric acid+
2 sets of the standard solution working curve for measuring 9 points of La, Ce, Pr, Nd and Sm constituent content in iron ore of tartaric acid, rare earth
Each element content is shown in such as table 1；Configuring slaggers' composition line standard solution includes：In 6 250mL polytetrafluoroethylene beakers, claim
Take clinker standard specimens of 5 parts of 0.1000g without La, Ce, Pr, Nd and Sm as bottoming matrix, by step S102 method acid adding into
The decomposition of row sample, perchloric acid smoked, dissolving with hydrochloric acid salt are cooled to after room temperature and shift made from step S104 6 respectively
In 100mL plastics volumetric flasks, La is then pipetted respectively2O3、CeO2、Pr6O11、Nd2O3、Sm2O3Standard solution holds in 6 100mL
In measuring bottle, be diluted to scale with pure water, shake up, be configured to La, Ce in the measurement slag that medium is hydrochloric acid or hydrochloric acid+tartaric acid, Pr,
2 sets of the calibration curve working solution of 6 points of Nd and Sm constituent contents, rare earth each element series concentration is identical：0%, 0.01%,
0.10%, 0.20%, 0.40%, 0.60%；
Table 1 measures iron ore middle rare earth standard solution working curve
Step S108, by the calibration curve work made from the test solution made from the method for step S102 and step S106
Make solution while being put into the content for measuring La, Ce, Pr, Nd and Sm element in test equipment,
Wherein, the group of each solvent is divided into：Hydrochloric acid (ρ 1.19, top pure grade), hydrochloric acid (5+95), hydrochloric acid (2+98), hydrofluoric acid (ρ
1.13, top pure grade), perchloric acid (ρ 1.68, top pure grade), tartaric acid (200g/L), mixed solvent：Natrium carbonicum calcinatum+boric acid=2+
1 (top pure grade), experimental water are two level pure water.
Further, the fit analysis spectral line of La, Ce, Pr, Nd and Sm element is：La 408.672nm,Ce
418.660nm、Pr 422.293nm、Nd 406.109nm、Sm 359.260nm、Sm 442.434nm。
Test equipment：PE companies of the U.S. produce, Optima5300DV inductively-coupled plasma spectrometers.
Instrument parameter：It is shown in Table 2
Running parameter table 2
La, Ce, Pr, Nd and Sm constituent content in iron ore, clinker, operation letter are measured simultaneously using ICP plasma spectrometer
Just quickly, operating cost is low.
The calculation of the mass percentage of rare earth element in the sample is：
W (tested component) (%)=Wi-W0,
In formula：W is the mass percentage of element in the sample；WiThe mass percent for being rare earth element in test solution；W0
For mass percent of the rare earth element in blank solution to be measured.
The precision of the test method of the present embodiment：
Precision Experiment is carried out to mine, 1# slag synthetic samples by determining experimental method.Experimental result is shown in Table 3-1 and 3-2.
Result is found out from table 3-1 and table 3-2, and the RSD of iron ore and slag middle rare earth each element is respectively less than 5%, has preferable essence
Density.
Table 3-1 Precision Experiments
Table 3-2 Precision Experiments
The accuracy of the test method of the present embodiment
Existing mine, slag standard sample are analyzed by inventive method, standard solution calibration curve is done with batch, by curve
The content of each rare earth element is calculated, measurement result is shown in Table 4.Since existing mine, slag standard sample rare earth standard value are total amount of rare earth,
It compares with total amount of rare earth standard value without each rare earth element content value, thus by the addition and value of each Rare-earth Element Dy value, as a result
Display relatively coincide.
Baogang's Research Institute of Rare Earths is sent to analyze sample baotite R-715 and blast furnace slag R-711, measurement result is shown in Table 4.The number from table
According to obtaining, different experiments room, two different analysis methods, different analysis personnel, the analysis result of different instruments are consistent.
(%) is tested in 4 accuracy of table
Table 5 is tested for the rare earth each element rate of recovery, and as known from Table 5, each rare earth element recovery of standard addition is 97%~104%
Between, it can also show that this method has high accuracy.
The 5 rare earth each element rate of recovery of table tests (%)
Above in association with having illustrated technical scheme of the present invention, technical solution through the invention, measure La, Ce, Pr,
The precision of the method for the content of Nd and Sm is good, accuracy is high, detection limit is low, is fully able to meet the analysis inspection of scientific research and production
It surveys and needs.
In the description of this specification, the description of term " one embodiment ", " some embodiments ", " specific embodiment " etc.
Mean that particular features, structures, materials, or characteristics described in conjunction with this embodiment or example are contained at least one reality of the present invention
It applies in example or example.In the present specification, schematic expression of the above terms are not necessarily referring to identical embodiment or reality
Example.Moreover, description particular features, structures, materials, or characteristics can in any one or more of the embodiments or examples with
Suitable mode combines.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, any made by repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (4)
1. a kind of method for the content measuring La, Ce, Pr, Nd and Sm, is used for iron ore and clinker, which is characterized in that including：
Step 1, test solution is prepared, iron ore is weighed or clinker sample 0.1000g is placed in 250mL polytetrafluoroethylene beakers, add 5mL
Hydrofluoric acid (ρ 1.13), 10mL hydrochloric acid (ρ 1.19) add 2mL perchloric acid (ρ 1.68) after electric hot plate low-temperature heat makes sample decompose,
Continue to heat, makes perchloric acid smoke to residual volume 1mL hereinafter, slightly cold.Add 5mL hydrochloric acid (ρ 1.19) heating that salt is made to dissolve, takes
It is lower be cooled to room temperature naturally after, be transferred in 100mL volumetric flasks, be diluted to scale with pure water, shake up, do reagent blank in company with sample；
Step 2, standard working solution is prepared, the standard working solution includes：La2O3(1000 μ g/mL), CeO2(1000μg/
ML), Pr6O11(1000 μ g/mL), Nd2O3(1000 μ g/mL), Sm2O3(1000 μ g/mL), Al2O3(1000 μ g/mL), CaO
(1000 μ g/mL), Fe (1000 μ g/mL), MgO (1000 μ g/mL), MnO (1000 μ g/mL) and TiO2(1000 μ g/mL), it is described
Standard liquid is formulated as 100 μ g/mL, 10 μ g/mL, tri- kinds of 1 μ g/mL respectively；
Step 3, calibration curve working solution is prepared, wherein configuring iron ore working curve standard solution includes：In 9 250mL
In polytetrafluoroethylene beaker, iron ore standard specimens of 8 parts of 0.1000g without La, Ce, Pr, Nd and Sm is weighed as bottoming matrix, is pressed
The decomposition of the method acid adding progress sample of step 1, perchloric acid smoked, dissolving with hydrochloric acid salt, are cooled to after room temperature and are shifted respectively in step
In 9 100mL plastics volumetric flasks made from rapid 2, La is then pipetted respectively2O3、CeO2、Pr6O11、Nd2O3、Sm2O3Standard solution
In 9 100mL volumetric flasks, it is diluted to scale with pure water, is shaken up, is configured to the measurement that medium is hydrochloric acid or hydrochloric acid+tartaric acid
2 sets of the standard solution working curve of 9 points of La, Ce, Pr, Nd and Sm constituent content in iron ore；Configure clinker working curve
Standard solution includes：In 6 250mL polytetrafluoroethylene beakers, the stove that 5 parts of 0.1000g are free of La, Ce, Pr, Nd and Sm is weighed
Slag standard specimen is cold by the decomposition of the method acid adding progress sample of step 1, perchloric acid smoked, dissolving with hydrochloric acid salt as bottoming matrix
It is shifted respectively after to room temperature in 6 100mL plastics volumetric flasks made from step 2, then pipettes La respectively2O3、CeO2、
Pr6O11、Nd2O3、Sm2O3Standard solution is diluted to scale in 6 100mL volumetric flasks, with pure water, shakes up, and is configured to medium and is
The calibration curve working solution 2 for measuring 6 points of La, Ce, Pr, Nd and Sm constituent content in slag of hydrochloric acid or hydrochloric acid+tartaric acid
Set；
Step 4, the test solution made from the method by step 1 is put simultaneously with the calibration curve working solution made from step 3
Enter to measure the content of La, Ce, Pr, Nd and Sm element in test equipment,
Wherein, the group of each solvent is divided into：Hydrochloric acid (ρ 1.19, top pure grade), hydrochloric acid (5+95), hydrochloric acid (2+98), hydrofluoric acid (ρ
1.13, top pure grade), perchloric acid (ρ 1.68, top pure grade), tartaric acid (200g/L), mixed solvent：Natrium carbonicum calcinatum+boric acid=2+
1 (top pure grade), experimental water are two level pure water.
2. according to the method for the content described in claim 1 for measuring La, Ce, Pr, Nd and Sm, which is characterized in that
W (tested component) (%)=Wi-W0,
In formula：W is the mass percentage of element in the sample；WiThe mass percent for being rare earth element in test solution；W0It is dilute
Mass percent of the earth elements in blank solution to be measured.
3. it is according to claim 1 measure La, Ce, Pr, Nd and Sm content method, which is characterized in that La, Ce, Pr,
The fit analysis spectral line of Nd and Sm elements is：
La 408.672nm、Ce 418.660nm、Pr 422.293nm、Nd 406.109nm、Sm 359.260nm、Sm
442.434nm。
4. the method for the content according to claim 1 for measuring La, Ce, Pr, Nd and Sm, which is characterized in that in step 1,
If carbon containing sulphur and when higher organic matter in the iron ore or clinker sample, the iron ore or clinker sample are placed in porcelain crucible
In 600~800 DEG C of 10~15min of calcination, move into again after cooling in the 250mL polytetrafluoroethylene beakers.
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| 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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| 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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Application publication date: 20181106 |