CN108414558A - A kind of MTG YBCO bulk method measuring ferrochrome chemical composition for x-ray fluorescence spectrum analysis method - Google Patents
A kind of MTG YBCO bulk method measuring ferrochrome chemical composition for x-ray fluorescence spectrum analysis method Download PDFInfo
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- CN108414558A CN108414558A CN201810229025.7A CN201810229025A CN108414558A CN 108414558 A CN108414558 A CN 108414558A CN 201810229025 A CN201810229025 A CN 201810229025A CN 108414558 A CN108414558 A CN 108414558A
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- ferrochrome
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- crucible
- ray fluorescence
- chemical composition
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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
-
- 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
Abstract
A kind of MTG YBCO bulk method measuring ferrochrome chemical composition for x-ray fluorescence spectrum analysis method provided by the invention, first weighs certain ferrochrome sample and oxidant, after mixing is placed in lithium tetraborate crucible, is placed in platinum yellow crucible, adds lithium tetraborate reagent and releasing agent；Then, be heated to sample component element it is fully oxidized after, be continuously heating to 1100 DEG C ± 10 DEG C, the glass print analyzed for X-ray fluorescence spectra is made in heating melting.Once-through operation substep is pre-oxidized and melted in the present invention to complete, and is not only simplified operation, is more advantageous to intelligentized control method, realize automation mechanized operation, improves determination efficiency and accuracy；Platinum yellow crucible is not corroded by sample during can ensure that MTG YBCO bulk.Compared with prior art, the efficiency and reliability of x-ray fluorescence spectrometry ferrochrome chemical composition can be improved in method provided by the invention, has economic benefit directly or indirectly.
Description
Technical field
The invention belongs to method of inspection fields, and in particular to one kind measuring ferrochrome chemistry for x-ray fluorescence spectrum analysis method
The MTG YBCO bulk method of ingredient.
Background technology
Sample preparation is that an important step of ferrochrome sample chemical composition is measured using X-ray fluorescence spectra analytical technology, system
Quadrat method usually influences the accuracy of measurement result.
The method for making sample of ferrochrome Xray fluorescence spectrometer analysis at present is broadly divided into two classes, and one kind is pressed disc method, though the method
It is so fast and convenient, but due to being difficult to overcome the influence of granularity effect, measurement result deviation is larger, thus it is quick to be only applicable to stokehold
Analysis.Another kind of is fusion method, is generally divided into three steps, and first step wall built-up on platinum crucible with lithium tetraborate solvent is protected
Shield crucible does not weather in melting process, and second step is that sample and oxidant mixture are placed in above-mentioned crucible to carry out low temperature
Pre-oxidation, third portion is high-temperature fusion.The method requires operator's operative skill high thus difficult since sample preparation is cumbersome
To popularize.
In recent years, occurs a kind of lithium tetraborate crucible in the market, operation is to set the mixture of sample and oxidant
It transfers in platinum yellow crucible and melts in Muffle furnace after heating pre-oxidation in lithium tetraborate crucible, the method operation is relatively simple
Just, when but filling the lithium tetraborate crucible of sample and pre-oxidized in Muffle furnace, to temperature requirement harshness, easily because of lithium tetraborate earthenware
Crucible leakage and failure, and it need to be transferred to platinum yellow crucible, easily stain.
Invention content
The purpose of the present invention is to provide it is a kind of for x-ray fluorescence spectrum analysis method measure ferrochrome chemical composition melting
Method for making sample, may not need the cumbersome of platinum yellow crucible wall built-up operation, improves detection efficiency, eliminates melting to the maximum extent and prepared
The contamination that journey introduces, it is ensured that testing result has good precision and accuracy.
Specific technical solution of the present invention is as follows：
A kind of MTG YBCO bulk method measuring ferrochrome chemical composition for x-ray fluorescence spectrum analysis method, includes the following steps：
1) claim sample：Ferrochrome sample, oxidant, lithium tetraborate reagent and releasing agent, mixing are weighed, lithium tetraborate crucible is placed in
In, lithium tetraborate crucible is placed in platinum yellow crucible；
2) be heated to sample component element it is fully oxidized after, be continuously heating to 1100 DEG C ± 10 DEG C, use is made in heating melting
In the glass print of X-ray fluorescence spectra analysis.
Ferrochrome sample granularity is less than 120um in step 1).
Ferrochrome sample in step 1), oxidant, lithium tetraborate reagent and releasing agent mass ratio be 1:7.5:35:0.15.
Oxidant described in step 1) is selected from lithium carbonate；The releasing agent is selected from ammonium bromide or lithium bromide.
It is fully oxidized that sample component element is heated to described in step 2), heating temperature is 700 DEG C -900 DEG C.Heating time
For 35-45min.
The melting time is 15-20min in step 2).
Once-through operation substep is pre-oxidized and melted in the present invention to complete, and is not only simplified operation, is more advantageous to intelligentized control method,
It realizes automation mechanized operation, improves determination efficiency and accuracy；Platinum yellow crucible is not corroded by sample during can ensure that MTG YBCO bulk.
Compared with prior art, x-ray fluorescence spectrometry ferrochrome chemical composition can be improved in method provided by the invention
Efficiency and reliability, there is economic benefit directly or indirectly.
Specific implementation mode
Embodiment 1
A kind of MTG YBCO bulk method measuring ferrochrome chemical composition for x-ray fluorescence spectrum analysis method, includes the following steps：
1) it samples
The analysis specimen that granularity is less than 120um is made in ferrochrome by detection method requirement.
2) it weighs
According to measurement method needs, sample 0.2g, oxidant lithium carbonate 1.5g are quantitatively weighed, mixing is placed on lithium tetraborate
In crucible, the lithium tetraborate crucible for filling sample mixture is placed in platinum yellow crucible, lithium tetraborate is supplemented to 7g by thinner ratio
And releasing agent ammonium bromide 0.03g is added.
3) it pre-oxidizes
The interior platinum yellow crucible for containing lithium tetraborate crucible is placed in heating furnace and is warming up to 700 DEG C -900 DEG C, is heated 40 minutes,
It is fully oxidized to sample component element.
4) it melts
Above-mentioned platinum yellow crucible is placed in 1100 DEG C ± 10 DEG C of heating furnace to continue to heat, is melted 20 minutes, platinum yellow earthenware is taken out
Crucible pours out melting print after 1 minute cooling.X-ray fluorescence spectra measurement can be carried out by being cooled to room temperature.
Claims (7)
1. a kind of MTG YBCO bulk method measuring ferrochrome chemical composition for x-ray fluorescence spectrum analysis method, which is characterized in that described
Method includes the following steps：
1) claim sample：Ferrochrome sample, oxidant, lithium tetraborate reagent and releasing agent, mixing are weighed, is placed in lithium tetraborate crucible,
Lithium tetraborate crucible is placed in platinum yellow crucible；
2) be heated to sample component element it is fully oxidized after, be continuously heating to 1100 DEG C ± 10 DEG C, heating melting is made for X
The glass print of fluorescent x ray spectroscopy x.
2. according to the method described in claim 1, it is characterized in that, ferrochrome sample granularity is less than 120um in step 1).
3. method according to claim 1 or 2, which is characterized in that ferrochrome sample, oxidant, lithium tetraborate in step 1)
The mass ratio of reagent and releasing agent is 1:7.5:35:0.15.
4. method according to claim 1 or 3, which is characterized in that oxidant described in step 1) is selected from lithium carbonate.
5. method according to claim 1 or 3, which is characterized in that releasing agent described in step 1) be selected from ammonium bromide or
Lithium bromide.
6. according to claim 1-5 any one of them methods, which is characterized in that be heated to sample component member described in step 2)
Element is fully oxidized, and heating temperature is 700 DEG C -900 DEG C.Heating time is 35-45min.
7. according to claim 1-6 any one of them methods, which is characterized in that the melting time is 15-20min in step 2).
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| CN201810229025.7A CN108414558A (en) | 2018-03-20 | 2018-03-20 | A kind of MTG YBCO bulk method measuring ferrochrome chemical composition for x-ray fluorescence spectrum analysis method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108872203A (en) * | 2018-09-29 | 2018-11-23 | 攀钢集团攀枝花钢铁研究院有限公司 | The detection method of elemental composition in a kind of vanadium chromium slag and its digestion procedure and a kind of measurement vanadium chromium slag |
| 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 |
| CN114166879A (en) * | 2020-09-11 | 2022-03-11 | 株式会社理学 | Method for manufacturing glass beads for fluorescent X-ray analysis device |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108872203A (en) * | 2018-09-29 | 2018-11-23 | 攀钢集团攀枝花钢铁研究院有限公司 | The detection method of elemental composition in a kind of vanadium chromium slag and its digestion procedure and a kind of measurement vanadium chromium slag |
| CN114166879A (en) * | 2020-09-11 | 2022-03-11 | 株式会社理学 | Method for manufacturing glass beads for fluorescent X-ray analysis device |
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Address after: 243003 8 Jiuhua Road, Yushan, Ma'anshan, Anhui Applicant after: Ma'anshan Iron and Steel Co., Ltd. Address before: 243003 Intellectual Property Department, Technical Center No. 8, Hunan West Road, Yushan District, Ma'anshan City, Anhui Province Applicant before: Ma'anshan Iron and Steel Co., Ltd. |
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Application publication date: 20180817 |