CN108508050A - The method of lanthanum, cerium and barium content in x-ray fluorescence spectrometry slag - Google Patents
The method of lanthanum, cerium and barium content in x-ray fluorescence spectrometry slag Download PDFInfo
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- CN108508050A CN108508050A CN201810194333.0A CN201810194333A CN108508050A CN 108508050 A CN108508050 A CN 108508050A CN 201810194333 A CN201810194333 A CN 201810194333A CN 108508050 A CN108508050 A CN 108508050A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/2202—Preparing specimens therefor
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/223—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/07—Investigating materials by wave or particle radiation secondary emission
- G01N2223/076—X-ray fluorescence
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Abstract
The method of lanthanum, cerium and barium content, compounds calibration sample by high purity lanthanum oxide, cerium oxide, barium carbonate and slag standard sample first, standard curve is made after glass print is made in high-temperature fusion in a kind of slag using x-ray fluorescence spectrometry of the present invention；Then glass print is made in slag sample to be measured, this glass print is introduced into Xray fluorescence spectrometer and is detected, the content for calculating surveyed element after the intensity of element to be measured according to standard curve is measured by Xray fluorescence spectrometer.The present invention can quickly, accurately detect lanthanum in slag, cerium and barium constituent content, to determine that steel grade field trash source provides foundation.
Description
Technical field
The present invention relates to lanthanum in a kind of slag, cerium and barium content assay method more particularly to a kind of using x-ray fluorescence
The method of lanthanum, cerium and barium content in spectrographic determination slag.
Background technology
Non-metallic inclusion is one of the key factor for influencing steel performance, sometimes can directly determine that the grade of steel is commented
Sentence.It determines field trash source and effectively control the amount of inclusions is the important topic of process for making research.In recent years, research work
Person is done by adding certain special material, such as lanthana, cerium oxide and barium carbonate in different processes with lanthanum, cerium and barium element
The method of tracer come determine field trash derive from which certain working procedure；Wherein, the slag ingredient after tracer is added
Analysis is also the important content in research field trash source, and about the research of tracer element measurement, there are few reports on document at present.
In general, for the determination of trace elements as lanthanum, cerium and barium, conventional thinking be after slag sample acid dissolving, then
With inductance coupled plasma-atomic emission spectrographic determination, but this method, there are operating process complexity, sample dissolving is not thorough
The shortcomings of；Simultaneously because having used the acid of a large amount of not environment friendly, the developing direction of green laboratory is not met.The present invention carries
A kind of quick, simple, environmental-friendly method for measuring tracer element lanthanum, cerium and barium in slag has been supplied, can be to judge field trash
Source provides foundation.
Invention content
Technical problem to be solved by the invention is to provide lanthanum, cerium and barium in a kind of x-ray fluorescence spectrometry slag
The method of content can quickly, accurately detect lanthanum in slag, cerium and barium constituent content, to determine that steel grade field trash source provides
Foundation.
In order to solve the above technical problems, the technical solution adopted in the present invention is：
A kind of method of lanthanum, cerium and barium content in x-ray fluorescence spectrometry slag, first by high purity lanthanum oxide, cerium oxide,
Barium carbonate and slag standard sample compound calibration sample, and standard curve is made after glass print is made in high-temperature fusion；Then will
Glass print is made in slag sample to be measured, this glass print is introduced into Xray fluorescence spectrometer and is detected, glimmering by X-ray
Photothermal spectroscopic analyzer measures the content for calculating surveyed element after the intensity of element to be measured according to standard curve.
The method of lanthanum, cerium and barium content, more specifically measures in a kind of above-mentioned x-ray fluorescence spectrometry slag
Step is：
A, a certain amount of high purity lanthanum oxide, cerium oxide, barium carbonate and slag standard sample are weighed to be placed in platinum crucible, is added four
Mixing after lithium borate and lithium carbonate is added dropwise ammonium iodide releasing agent, is melted at 1000 ~ 1050 DEG C, prepare making standard curve
Calibration glass print is then fed into Xray fluorescence spectrometer and makes standard curve；
B, it weighs a certain amount of slag sample to be placed in platinum crucible, lithium tetraborate and lithium carbonate mixing is added, ammonium iodide is added dropwise
Releasing agent melts at 1000 ~ 1050 DEG C, prepares mother glass print；
C, slag sample glass print is sent into Xray fluorescence spectrometer and is detected, measured and waited for by Xray fluorescence spectrometer
The content of surveyed element is calculated after the intensity of survey element according to standard curve.
The method of lanthanum, cerium and barium content in a kind of above-mentioned x-ray fluorescence spectrometry slag, in the step a,
The purity of lanthana, cerium oxide and barium carbonate is that mass fraction is more than 99.9%；The mass M of lanthana1, cerium oxide mass M2、
The mass M of barium monoxide3With the mass M of slag standard sample4Meet formula（1）It is required that；The mass M of barium carbonate5Meet formula（2）It wants
It asks:
M1+ M2+ M3+ M4=0.5000~0.7000g （1）
Formula（1）In：M1For the quality of lanthana, unit：g；
M2For the quality of cerium oxide, unit：g；
M3For the quality of barium monoxide, unit：g；
M4For the quality of slag standard sample, unit：g；
M5= M3/0.777 （2）
Formula（2）In：M5For the quality of barium carbonate, unit：g；
M3For the quality of barium monoxide, unit：g；
The method of lanthanum, cerium and barium content in a kind of above-mentioned x-ray fluorescence spectrometry slag, slag tries in the step b
Sample dosage is 0.5000 ~ 0.7000g.
The method of lanthanum, cerium and barium content in a kind of above-mentioned x-ray fluorescence spectrometry slag, the step a and b
In, lithium tetraborate dosage is 5.000 ~ 7.000g；Lithium carbonate dosage is 0.8000 ~ 1.0000g；Ammonium iodide is a concentration of 30g/L
Solution, dosage be 1 ~ 3mL；The molten sample time is 10 ~ 15min.
The advantageous effect generated using above-mentioned technical proposal is：
Compound calibration sample using high purity lanthanum oxide, cerium oxide and barium carbonate and slag standard sample, solve measure lanthanum, cerium and
The problem of barium is without standard sample；Using the lithium tetraborate dissolution characteristics strong to slag, solves and tried with slag when conventional acid extracting
There is insoluble matter in sample；Whole experiment process only sample weighing is manual operation, remaining is all completed by instrument, maximum journey
Degree reduces human interference, has the characteristics that easy to operate, quick and precisely.Measurement process is not related to the use of acid completely, gives up
Gurry is solid glass, simple and quick, and favorable reproducibility is environmentally protective, finishes the measurement of lanthanum, cerium and barium in slag sample not properly
The situation of Fa Keyi has wide popularizing application prospect.
Specific implementation mode
The present invention is described in further details below by way of specific embodiment：
Embodiment 1：
The method of lanthanum, cerium and barium content, includes the following steps in x-ray fluorescence spectrometry slag：
A, the making of standard curve
In the present embodiment, it is specified that the sample weighting amount of calibration sample and slag sample is 0.7000g, therefore the mass M of lanthana1, oxygen
Change the mass M of cerium2, barium monoxide mass M3With slag standard sample mass M4Summation M be 0.7000g, the wherein matter of barium carbonate
Amount is that the quality of barium monoxide is removed in 0.777.Specific proportioning is as shown in table 1；In the present embodiment, the mass M of lanthana1, oxidation
The mass M of cerium2With the mass M of barium monoxide3The percentage for accounting for gross mass M is respectively 0.2 ~ 1.0%, 0.8 ~ 2.3% and 2.0 ~ 4.0%.
1 calibration sample of table matches table
Load weighted lanthana, cerium oxide, barium carbonate and slag standard sample are transferred to platinum crucible according to the proportioning of table 1
In, 7.0000g lithium tetraborates and 1.0000g lithium carbonates, mixing is then added, the iodate ammonium salt solution 2mL of 30g/L is added dropwise, is placed in
15min is melted in sample-melting stove at 1050 DEG C, after taking out cooling, obtains series of calibration glass print；
The series of calibration print made is put into Xray fluorescence spectrometer and is measured, is measured by force by Xray fluorescence spectrometer
Standard curve is drawn out according to known content after degree.
B, the measurement of slag sample
After standard curve making is good, slag sample glass print is produced in melting；It weighs slag sample 0.7000g and is placed in platinum crucible
It is interior, 7.0000g lithium tetraborates and 1.0000g lithium carbonates is added, mixing is added dropwise the iodate ammonium salt solution 2mL of 30 g/L, is placed in molten sample
15min is melted in stove at 1050 DEG C, after taking out cooling, the glass print of slag sample is obtained, is put into Xray fluorescence spectrometer
The intensity that middle basis is measured calculates lanthanum, cerium and barium content by standard curve.
The accuracy of this method is verified by mark-on reclaims, as a result see the table below 2, it can be seen that recovery of standard addition
Between 95-107%, Pass Test requirement disclosure satisfy that the requirement of daily production testing.
2 recovery of standard addition of table is tested
Embodiment 2：
A, the making of standard curve
In the present embodiment, it is specified that the sample weighting amount of calibration sample and slag sample is 0.5000g；Therefore the mass M of lanthana1, oxygen
Change the mass M of cerium2, barium monoxide mass M3With slag standard sample mass M4Summation M be 0.5000g, the wherein matter of barium carbonate
Amount is that the quality of barium monoxide is removed in 0.777.Specific proportioning is as shown in table 3.In the present embodiment, the mass M of lanthana1, oxidation
The mass M of cerium2With the mass M of barium monoxide3The percentage for accounting for gross mass M is respectively 0.2 ~ 1.2%, 1.0 ~ 3.0% and 1.0 ~ 6.0%.
3 calibration sample of table matches table
Load weighted lanthana, cerium oxide, barium carbonate and slag standard sample are transferred to platinum crucible according to the proportioning of table 3
In, 5.0000g lithium tetraborates and 0.8000g lithium carbonates, mixing is then added, the iodate ammonium salt solution 1mL of 30g/L is added dropwise, is placed in
13min is melted in sample-melting stove at 1050 DEG C, after taking out cooling, obtains series of calibration glass print.
The series of calibration print made is put into Xray fluorescence spectrometer and is measured, is surveyed by Xray fluorescence spectrometer
Go out after intensity and standard curve is drawn out according to known content.
B, the measurement of slag sample
After standard curve making is good, slag sample glass print is produced in melting.Slag sample 0.5000g is weighed in platinum crucible
It is interior, 5.0000g lithium tetraborates and 0.8000g lithium carbonates is added, mixing is added dropwise the iodate ammonium salt solution 1mL of 30 g/L, is placed in molten sample
13min is melted in stove at 1050 DEG C, after taking out cooling, the glass print of slag sample is obtained, is put into Xray fluorescence spectrometer
The intensity that middle basis is measured calculates lanthanum, cerium and barium content by standard curve.
The accuracy of this method is verified by mark-on reclaims, as a result see the table below 4, it can be seen that recovery of standard addition
Between 95-107%, Pass Test requirement disclosure satisfy that the requirement of daily production testing.
4 recovery of standard addition of table is tested
Embodiment 3：
A, the making of standard curve
In the present embodiment, it is specified that the sample weighting amount of calibration sample and slag sample is 0.6000g, therefore the mass M of lanthana1, oxygen
Change the mass M of cerium2, barium monoxide mass M3With slag standard sample mass M4Summation M be 0.6000g, the wherein matter of barium carbonate
Amount is that the quality of barium monoxide is removed in 0.777.Specific proportioning is as shown in table 5；The mass M of lanthana1, cerium oxide mass M2And oxygen
Change the mass M of barium3The percentage for accounting for gross mass M is respectively 0.4 ~ 1.4%, 0.8 ~ 2.5% and 0.9 ~ 5.0%.
5 calibration sample of table matches table
Load weighted lanthana, cerium oxide, barium carbonate and slag standard sample are transferred to platinum crucible according to the proportioning of table 5
In, 6.0000g lithium tetraborates and 0.9000g lithium carbonates, mixing is then added, the iodate ammonium salt solution 1.5mL of 30g/L is added dropwise, sets
15min is melted at 1050 DEG C in sample-melting stove, after taking out cooling, obtains series of calibration glass print.
The series of calibration print made is put into Xray fluorescence spectrometer and is measured, is surveyed by Xray fluorescence spectrometer
Go out after intensity and standard curve is drawn out according to known content.
B, the measurement of slag sample
After standard curve making is good, slag sample glass print is produced in melting；Slag sample 0.6000g is weighed in platinum crucible
It is interior, 6.0000g lithium tetraborates and 0.9000g lithium carbonates is added, mixing is added dropwise the iodate ammonium salt solution 1.5mL of 30 g/L, is placed in molten
15min is melted in sample stove at 1050 DEG C, after taking out cooling, obtains the glass print of slag sample；It is put into X-ray fluorescence spectra
Lanthanum, cerium and barium content are calculated by standard curve according to the intensity measured in instrument；
The accuracy of this method is verified by mark-on reclaims, as a result see the table below 6, it can be seen that recovery of standard addition is in 95-
Between 107%, Pass Test requirement disclosure satisfy that the requirement of daily production testing.
6 recovery of standard addition of table is tested
Claims (5)
1. a kind of method of lanthanum, cerium and barium content in x-ray fluorescence spectrometry slag, it is characterised in that：It first will be high-purity
Lanthana, cerium oxide, barium carbonate and slag standard sample compound calibration sample, and mark is made after glass print is made in high-temperature fusion
Directrix curve；Then glass print is made in slag sample to be measured, this glass print is introduced into Xray fluorescence spectrometer and is examined
It surveys, the content for calculating surveyed element after the intensity of element to be measured according to standard curve is measured by Xray fluorescence spectrometer.
2. the method for lanthanum, cerium and barium content, special in a kind of x-ray fluorescence spectrometry slag as described in claim 1
Sign is：More specifically determination step is：
A, a certain amount of high purity lanthanum oxide, cerium oxide, barium carbonate and slag standard sample are weighed to be placed in platinum crucible, is added four
Mixing after lithium borate and lithium carbonate is added dropwise ammonium iodide releasing agent, is melted at 1000 ~ 1050 DEG C, prepare making standard curve
Calibration glass print is then fed into Xray fluorescence spectrometer and makes standard curve；
B, it weighs a certain amount of slag sample to be placed in platinum crucible, lithium tetraborate and lithium carbonate mixing is added, ammonium iodide is added dropwise
Releasing agent melts at 1000 ~ 1050 DEG C, prepares mother glass print；
C, slag sample glass print is sent into Xray fluorescence spectrometer and is detected, measured and waited for by Xray fluorescence spectrometer
The content of surveyed element is calculated after the intensity of survey element according to standard curve.
3. the method for lanthanum, cerium and barium content, special in a kind of x-ray fluorescence spectrometry slag as claimed in claim 2
Sign is：In the step a, the purity of lanthana, cerium oxide and barium carbonate is that mass fraction is more than 99.9%；Lanthana
Mass M1, cerium oxide mass M2, barium monoxide mass M3With the mass M of slag standard sample4Meet formula（1）It is required that；Carbonic acid
The mass M of barium5Meet formula（2）It is required that：
M1+ M2+ M3+ M4=0.5000~0.7000g （1）
Formula（1）In：M1For the quality of lanthana, unit：g；
M2For the quality of cerium oxide, unit：g；
M3For the quality of barium monoxide, unit：g；
M4For the quality of slag standard sample, unit：g；
M5= M3/0.777 （2）
Formula（2）In：M5For the quality of barium carbonate, unit：g；
M3For the quality of barium monoxide, unit：g.
4. the method for lanthanum, cerium and barium content, special in a kind of x-ray fluorescence spectrometry slag as claimed in claim 2
Sign is：Slag sample dosage is 0.5000 ~ 0.7000g in the step b.
5. the method for lanthanum, cerium and barium content, special in a kind of x-ray fluorescence spectrometry slag as claimed in claim 2
Sign is：In the step a and b, lithium tetraborate dosage is 5.000 ~ 7.000g；Lithium carbonate dosage be 0.8000 ~
1.0000g；Ammonium iodide is the solution of a concentration of 30g/L, and dosage is 1 ~ 3mL；The molten sample time is 10 ~ 15min.
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| CN109270101A (en) * | 2018-09-10 | 2019-01-25 | 自贡硬质合金有限责任公司 | A method of utilizing lanthanum content in x-ray fluorescence spectrometry molybdenum product |
| CN111595835A (en) * | 2020-05-25 | 2020-08-28 | 中国科学院金属研究所 | Method for measuring cerium content in high-silicon stainless steel |
| CN113720725A (en) * | 2021-08-31 | 2021-11-30 | 重庆钢铁股份有限公司 | Method for detecting particle steel |
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Application publication date: 20180907 |