CN108918641A - The method for measuring the content of lanthanum, cerium, praseodymium, neodymium and samarium - Google Patents
The method for measuring the content of lanthanum, cerium, praseodymium, neodymium and samarium Download PDFInfo
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- CN108918641A CN108918641A CN201810353223.4A CN201810353223A CN108918641A CN 108918641 A CN108918641 A CN 108918641A CN 201810353223 A CN201810353223 A CN 201810353223A CN 108918641 A CN108918641 A CN 108918641A
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- G—PHYSICS
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- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
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- G—PHYSICS
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- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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Abstract
The present invention provides a kind of methods of the content of measurement lanthanum, cerium, praseodymium, neodymium and samarium, are used for steel alloy, including：It weighs steel samples and clears up；Configure multiple lanthanum mixed standard solutions；Configure multiple cerium mixed standard solutions；Configure multiple neodymium mixed standard solutions；Configure multiple praseodymium mixed standard solutions；Configure multiple samarium mixed standard solutions；It is depicted as lanthanum, cerium, praseodymium, neodymium, samarium calibration curve；Lanthanum, cerium, praseodymium, the neodymium, samarium content in the solution to be measured are measured using icp ms, and obtain the content of lanthanum, cerium, praseodymium, neodymium, samarium in conjunction with the lanthanum, cerium, praseodymium, neodymium, samarium calibration curve.According to the technical solution of the present invention, sample can be made to be completely dissolved rapidly, measures the accuracy height of the method for the content of lanthanum, cerium, praseodymium, neodymium and samarium, shortens operating process.
Description
Technical field
The present invention relates to metallurgical analysis technical fields, in particular to containing for a kind of measurement lanthanum, cerium, praseodymium, neodymium and samarium
The method of amount.
Background technique
Rare earth measuring method has had a large amount of report in steel, but wants single rare earth content in Accurate Determining steel
It is relatively difficult, international at present, the domestic examination criteria for not yet forming rare earth component in measurement steel.Due to rare earth element sheet
The residual quantity of the characteristic of body, rare earth in steel is very low, belongs to trace element, this brings larger to Accurate Determining content of rare earth
It is difficult.Traditional chemical gauging rare earth needs to carry out the enrichment of rare earth element, and process is many and diverse and can only measure total amount of rare earth
The content of each element cannot be measured respectively.Also have and separate inductively coupled plasma atomic emission spectrometry using resin
(ICP-AES) method for measuring rare earth component, but separation method is cumbersome, the measurement period is longer, inductance coupling when content of rare earth is lower
It closes (ICP-AES) sensitivity of plasma atomic-emission light and wants low with respect to inductivity coupled plasma mass spectrometry, accuracy of measurement is difficult
To guarantee, and the spectral line interference of rare earth element brings certain difficulty to measurement component than more serious.
Steel alloy is added to various alloying elements such as silicon, manganese, chromium, nickel, molybdenum, vanadium etc. and certain nonmetalloids such as boron, nitrogen
Deng, and technological measure appropriate is taken, it can obtain and be respectively provided with higher intensity, toughness, corrosion resistance, low temperature resistant resistance to height
The properties such as warm nature.The addition of alloying element is used as industrial every field for steel and is of great significance with steel.To alloy
Each element in steel needs to measure that sample after completely dissolution when being detected.Due to containing there are many alloy element, Yi Xiepin
The steel alloy of kind takes the molten sample of common sample dissolving method difficult, can not quickly dissolve.
Summary of the invention
The present invention is directed to solve at least one of the technical problems existing in the prior art or related technologies.
In view of this, technical solution of the present invention provides a kind of method of content for measuring lanthanum, cerium, praseodymium, neodymium and samarium,
For steel alloy, including：Steel samples are weighed, by steel samples in micro-wave diminishing pot, 10mL is added and prepares in advance
Sal prunella nitration mixture, be placed at room temperature for 10 minutes, cover and be fitted into after sealing cover in resolution outer tank, is fitted into protects in cup together, be fixed on
It clears up on rotor, is put into microwave dissolver after screwing discouraged screw rod, carry out micro-wave digestion according to default reaction condition.Resolution
Counteracting tank is taken out after the completion, digestion solution is transferred in 100mL volumetric flask, forms solution to be measured；Configure multiple lanthanum content difference
For 10 μ g/mL, 1 μ g/mL, 0.1 μ g/mL, 0.01 μ g/mL solution 10ml in 100mL volumetric flask, add 10mL hydrochloric acid (ρ
Scale 1.19g/mL) is diluted to water and forms lanthanum mixed standard solution；Configuring multiple cerium contents is respectively 1 μ g/mL, 0.1 μ g/
ML, 0.01 μ g/mL solution 10ml in 100mL volumetric flask, add 10mL hydrochloric acid (ρ 1.19g/mL) to be diluted to scale shape with water
At cerium mixed standard solution；Configure multiple praseodymium contents be respectively 1 μ g/mL, 0.1 μ g/mL, 0.01 μ g/mL solution 10ml in
In 100mL volumetric flask, adds 10mL hydrochloric acid (ρ 1.19g/mL) to be diluted to scale with water and form praseodymium mixed standard solution；It configures more
A neodymium content is respectively the solution 10ml of 1 μ g/mL, 0.1 μ g/mL, 0.01 μ g/mL in 100mL volumetric flask, adds 10mL hydrochloric acid
(ρ 1.19g/mL) is diluted to scale with water and forms neodymium mixed standard solution；Configuring multiple samarium contents is respectively 1 μ g/mL, 0.1 μ
G/mL, 0.01 μ g/mL solution 10ml in 100mL volumetric flask, add 10mL hydrochloric acid (ρ 1.19g/mL) to be diluted to scale with water
Form samarium mixed standard solution；Configure iron-based liquid solution 100mg/mL；0.01 μ g/mL, 0.1 μ g/mL and 1 μ g/ are pipetted respectively
The lanthanum of mL, cerium, praseodymium, neodymium, samarium mixed standard solution 0.00mL, 5.00mL, 10.00mL, 20.00mL are in 100mL plastics volumetric flask
In, it is separately added into the iron-based liquid solution of 10.00mL, 3mL hydrochloric acid (ρ 1.19g/mL) and 2mL nitric acid (ρ 1.42g/mL) is added, uses water
It is diluted to scale, is mixed, the calibration curve standard solution of measurement lanthanum, cerium, praseodymium, neodymium, samarium is formed, using inductively coupled plasma
Lanthanum, cerium, praseodymium, neodymium, samarium content in body aes determination calibration curve standard solution, and be depicted as respectively lanthanum,
Cerium, praseodymium, neodymium, samarium calibration curve；Using sense coupled plasma-atomic emission spectrographic determination solution to be measured in lanthanum, cerium,
Praseodymium, neodymium, samarium content, and lanthanum, cerium, praseodymium, neodymium, samarium calibration curve is combined to obtain the content of lanthanum, cerium, praseodymium, neodymium, samarium.
Further, default reaction condition is：240 DEG C of the digestion condition upper limit, clear up pressure 60bar, resolution boosting
15min, rate of rise 0.3bar/s keep 20min, cooling 15min.
Compared with the existing technology, the method for the content of measurement lanthanum provided by the invention, cerium, praseodymium, neodymium and samarium has following excellent
Point：
Quickly, accurately using rare-earth elements of lanthanum, cerium, praseodymium, neodymium, samarium component in this method measurement steel alloy.By using micro-
Wave clears up sampler-dissolving method, sample can be made to be completely dissolved rapidly, operating process is simple, and method is easily grasped.It can analyze simultaneously
The multielement contents such as lanthanum, cerium, praseodymium, neodymium, samarium, the use compared to chemical method substantially reduce operating process, have saved drug,
Reduce manpower expenditure, improves production efficiency.New instrument analytical method is established, Determination Limit can be substantially reduced, together
Shi Caiyong mass spectrograph measures the overlapping for avoiding spectral line, improves the accuracy of measurement.
Additional aspect and advantage of the invention will be set forth in part in the description, partially will from the following description
Become obvious, or practice through the invention is recognized.
Specific embodiment
In order to be more clearly understood that aforementioned aspect of the present invention, feature and advantage, With reference to embodiment
The present invention is further described in detail.It should be noted that in the absence of conflict, embodiments herein and
Feature in embodiment can be combined with each other.
In the following description, numerous specific details are set forth in order to facilitate a full understanding of the present invention, still, the present invention may be used also
To be implemented using other than the one described here other modes, therefore, protection scope of the present invention is not by described below
Specific embodiment limitation.
The method of the content according to an embodiment of the invention for measuring lanthanum, cerium, praseodymium, neodymium and samarium, including：
1 reagent and material
1.1 hydrochloric acid：(ρ1.19g/mL)
1.2 nitric acid：(ρ1.42g/mL)
1.3 sal prunella nitration mixture：Hydrochloric acid, nitric acid and water are with 1:1:3 ratio mixing.
1.4 high purity iron：Spectroscopic pure
1.5 La standard reserving solutions, 1000 μ g/mL (medium 10%HCL), national standard solution
1.6 Ce standard reserving solutions, 1000 μ g/mL (medium 10%HNO3), national standard solution
1.7 Pr standard reserving solutions, 1000 μ g/mL (medium 10%HCL), national standard solution
1.8 Nd standard reserving solutions, 1000 μ g/mL (medium 10%HCL), national standard solution
1.9 Sm standard reserving solutions, 1000 μ g/mL (medium 10%HCL), national standard solution
1.10 La, Ce, Pr, Nd, Sm mixed standard solutions, 10 μ g/mL：La (1000 μ g/mL), Ce (1000 μ are taken respectively
G/mL), Pr (1000 μ g/mL), Nd (1000 μ g/mL), Sm (1000 μ g/mL) standard reserving solution 10mL are in 1000mL volumetric flask
In, add 100mL hydrochloric acid (ρ 1.19g/mL) to be diluted to scale with water, mixes.
1.11La, Ce, Pr, Nd, Sm mixed standard solution, 1 μ g/mL：La, Ce, Pr, Nd, Sm mixed standard solution, (10
μ g/mL) 10mL in 100mL volumetric flask, adds 10mL hydrochloric acid (ρ 1.19g/mL) to be diluted to scale with water, it mixes.
1.12La, Ce, Pr, Nd, Sm mixed standard solution, 0.1 μ g/mL：La, Ce, Pr, Nd, Sm mixed standard solution (1
μ g/mL) 10mL in 100mL volumetric flask, adds 10mL hydrochloric acid (ρ 1.19g/mL) to be diluted to scale with water, it mixes.
1.13La, Ce, Pr, Nd, Sm mixed standard solution, 0.01 μ g/mL：
La, Ce, Pr, Nd, Sm mixed standard solution (0.1 μ g/mL) 10mL is taken in 100mL volumetric flask, to add 10mL respectively
Hydrochloric acid (ρ 1.19g/mL) is diluted to scale with water, mixes.
1.14 iron-based liquid solution 100mg/mL
Weigh 1g high purity iron (being accurate to 0.01mg) and be transferred in 250ml beaker, be added 20ml ultrapure water, then plus
Enter 10mL hydrochloric acid (ρ 1.19g/mL) and 5mL nitric acid (ρ 1.42g/mL).Low-temperature heat dissolution, it is until completely dissolved, cooling, turn
It moves in 100mL volumetric flask, is diluted to scale with ultrapure water, mix.
1.15 caesium standard reserving solutions, 1000 μ g/mL (medium 5%HNO3), national standard solution
1.16 caesium standard solution, 1.0 μ g/mL (medium 5%HNO3)：Draw 1mL caesium standard reserving solution (1.0 μ g/mL) in
In 1000mL volumetric flask, 50mL hydrochloric acid (ρ 1.19g/mL) is added with water and is diluted to scale, mixes.
1.17 ultrapure water
1.18 mass spectrograph cleaning solution：About 400mL ultrapure water is injected in 500mL plastic bottle, and 20mL hydrochloric acid is then added
(ρ 1.19g/mL), 10mL nitric acid (ρ 1.42g/mL), and ultrapure water is added to 500mL.
2 analytical procedures
2.1 sample size
Weigh sample 0.1000g
2.2 blank test
Blank test is done in company with sample.
2.3 measurement
Sample is added 10mL prepared sal prunella nitration mixture in advance, is placed at room temperature for 10 minutes, covers in micro-wave diminishing pot
It is fitted into resolution outer tank, is fitted into protection cup together after sealing cover, be fixed on resolution rotor, be put into after screwing discouraged screw rod
It in microwave dissolver, sets reaction condition and carries out micro-wave digestion, 240 DEG C of the digestion condition upper limit, clear up pressure 60bar, resolution
Boost 15min, rate of rise 0.3bar/s, keeps 20min, cooling 15min.Counteracting tank is taken out after the completion of resolution, by digestion solution
It is transferred in 100mL volumetric flask, forms solution to be measured after constant volume.
It is internal standard with the caesium of 10ppm, online adding manner is taken to be added.
The drafting of 3 calibration curves:
Standard serial solution one：La, Ce, Pr, Nd, Sm mixed standard solution (0.01 μ g/mL) 0.00mL is pipetted respectively,
5.00mL, 10.00mL, 20.00mL, La, Ce, Pr, Nd, Sm mixed standard solution (0.1 μ g/mL) 5.00mL, 10.00mL, in
In 6 100mL plastics volumetric flasks, 10.00mL (4.1.3.13) iron-based liquid solution (100mg/mL) is respectively added, 3mL hydrochloric acid is added
(ρ 1.19g/mL) and 2mL nitric acid (ρ 1.42g/mL), is diluted with water to scale, mixes.
Standard serial solution two：La, Ce, Pr, Nd, Sm mixed standard solution (0.1 μ g/mL) 0.00mL is pipetted respectively,
10.00mL, 20.00mL, 5.00mL, La, Ce, Pr, Nd, Sm mixed standard solution (1 μ g/mL) 10.00mL, 20.00mL,
5.00mL is respectively added 10.00mL (4.1.3.13) iron-based liquid solution (100mg/mL), adds in 7 100mL plastics volumetric flasks
Enter 3mL hydrochloric acid (ρ 1.19g/mL) and 2mL nitric acid (ρ 1.42g/mL), be diluted with water to scale, mixes.
Lanthanum, cerium, praseodymium, the neodymium, samarium in the calibration curve standard solution are measured using icp ms
Content, and it is depicted as lanthanum, cerium, praseodymium, neodymium, samarium calibration curve respectively；Wherein, the setting ginseng of icp ms
Number as shown in table 1, then measures lanthanum, cerium, praseodymium, neodymium, samarium in the solution to be measured using icp ms
Content, and the content of lanthanum, cerium, praseodymium, neodymium, samarium is obtained in conjunction with the lanthanum, cerium, praseodymium, neodymium, samarium calibration curve.
Table 1
3. method accuracy
2 are shown in Table using the accuracy of the content of lanthanum, cerium, praseodymium, neodymium and samarium in the method test rare earth of the present embodiment.
Table 2
Difference is smaller between the given reference value of the measurement result and standard substance of the method for the present embodiment, illustrates this implementation
The method accuracy with higher of example, can accurately measure the content of each rare earth element in sample.
Quickly, accurately using rare-earth elements of lanthanum, cerium, praseodymium, neodymium, samarium component in the method measurement steel alloy of the present embodiment.It is logical
It crosses using On Dissolved Sample By Microwave Digestion, sample can be made to be completely dissolved rapidly, operating process is simple, and method is easily grasped.It can be same
When analysis lanthanum, cerium, praseodymium, neodymium, multielement contents, the use compared to chemical method such as samarium substantially reduce operating process, save
Drug reduces manpower expenditure, improves production efficiency.New instrument analytical method is established, can be substantially reduced under measurement
Limit, while the overlapping for avoiding spectral line is measured using mass spectrograph, improve the accuracy of measurement.
Technical solution of the present invention is explained above, according to the technical solution of the present invention, measures rare earth element in steel alloy
Lanthanum, cerium, praseodymium, neodymium, samarium component are quickly, accurately.By using On Dissolved Sample By Microwave Digestion, sample can be made to be completely dissolved rapidly,
Operating process is simple, and method is easily grasped.The multielement contents such as lanthanum, cerium, praseodymium, neodymium, samarium can be analyzed simultaneously, compared to chemical method
Use substantially reduce operating process, saved drug, reduce manpower expenditure, improve production efficiency.It establishes new
Instrument analytical method can substantially reduce Determination Limit, while the overlapping of spectral line is avoided using mass spectrograph measurement, improve
The accuracy of measurement.
In the description of this specification, term " one embodiment ", " some embodiments ", " specific embodiment " etc. are retouched
It states and means that particular features, structures, materials, or characteristics described in conjunction with this embodiment or example are contained at least one of the invention
In embodiment or example.In the present specification, schematic expression of the above terms be not necessarily referring to identical embodiment or
Example.Moreover, the particular features, structures, materials, or characteristics of description can be in any one or more of the embodiments or examples
It can be combined in any suitable manner.
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, made any
Modification, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (2)
1. a kind of method of the content of measurement lanthanum, cerium, praseodymium, neodymium and samarium, is used for steel alloy, which is characterized in that including：
Steel samples are weighed, by the steel samples in micro-wave diminishing pot, 10mL is added, and prepared sal prunella is mixed in advance
Acid is placed at room temperature for 10 minutes, is fitted into resolution outer tank after covering sealing cover, is fitted into protection cup together, is fixed on resolution rotor
On, it is put into microwave dissolver after screwing discouraged screw rod, carries out micro-wave digestion according to default reaction condition.It is taken out after the completion of resolution
Digestion solution is transferred in 100mL volumetric flask by counteracting tank, forms solution to be measured；
Solution 10ml that multiple lanthanum contents are respectively 1 μ g/mL, 0.1 μ g/mL, 0.01 μ g/mL is configured in 100mL volumetric flask, is added
10mL hydrochloric acid (ρ 1.19g/mL) is diluted to scale with water and forms lanthanum mixed standard solution；
Solution 10ml that multiple cerium contents are respectively 1 μ g/mL, 0.1 μ g/mL, 0.01 μ g/mL is configured in 100mL volumetric flask, is added
10mL hydrochloric acid (ρ 1.19g/mL) is diluted to scale with water and forms cerium mixed standard solution；
Solution 10ml that multiple praseodymium contents are respectively 1 μ g/mL, 0.1 μ g/mL, 0.01 μ g/mL is configured in 100mL volumetric flask, is added
10mL hydrochloric acid (ρ 1.19g/mL) is diluted to scale with water and forms praseodymium mixed standard solution；
Solution 10ml that multiple neodymium contents are respectively 1 μ g/mL, 0.1 μ g/mL, 0.01 μ g/mL is configured in 100mL volumetric flask, is added
10mL hydrochloric acid (ρ 1.19g/mL) is diluted to scale with water and forms neodymium mixed standard solution；
Solution 10ml that multiple samarium contents are respectively 1 μ g/mL, 0.1 μ g/mL, 0.01 μ g/mL is configured in 100mL volumetric flask, is added
10mL hydrochloric acid (ρ 1.19g/mL) is diluted to scale with water and forms samarium mixed standard solution；
Configure iron-based liquid solution 100mg/mL；
0.01 μ g/mL, the lanthanum of 0.1 μ g/mL and 1 μ g/mL, cerium, praseodymium, neodymium, samarium mixed standard solution 0.00mL are pipetted respectively,
5.00mL, 10.00mL, 20.00mL are separately added into the iron-based liquid solution of 10.00mL in 100mL plastics volumetric flask, and 3mL salt is added
Sour (ρ 1.19g/mL) and 2mL nitric acid (ρ 1.42g/mL), are diluted with water to scale, mix, and form measurement lanthanum, cerium, praseodymium, neodymium, samarium
Calibration curve standard solution, measured using icp ms lanthanum in the calibration curve standard solution,
Cerium, praseodymium, neodymium, samarium content, and it is depicted as lanthanum, cerium, praseodymium, neodymium, samarium calibration curve respectively；
Lanthanum, cerium, praseodymium, the neodymium, samarium content in the solution to be measured are measured using icp ms, and combine institute
It states lanthanum, cerium, praseodymium, neodymium, samarium calibration curve and obtains the content of lanthanum, cerium, praseodymium, neodymium, samarium.
2. the method for the content according to measurement lanthanum described in claim 1, cerium, praseodymium, neodymium and samarium, which is characterized in that described default anti-
The condition is answered to be：240 DEG C of the digestion condition upper limit, pressure 60bar is cleared up, resolution boosting 15min, rate of rise 0.3bar/s are kept
20min, cooling 15min.
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| CN113295760A (en) * | 2021-04-12 | 2021-08-24 | 包头钢铁（集团）有限责任公司 | Method for simultaneously measuring low contents of lanthanum, cerium, praseodymium, neodymium, samarium and barium in furnace slag and mold powder |
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