CN115575430A - Method for measuring elements in blast furnace slag by melting sample preparation-X-ray fluorescence - Google Patents
Method for measuring elements in blast furnace slag by melting sample preparation-X-ray fluorescence Download PDFInfo
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- CN115575430A CN115575430A CN202211181783.9A CN202211181783A CN115575430A CN 115575430 A CN115575430 A CN 115575430A CN 202211181783 A CN202211181783 A CN 202211181783A CN 115575430 A CN115575430 A CN 115575430A
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- furnace slag
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- 238000000034 method Methods 0.000 title claims abstract description 28
- 239000002893 slag Substances 0.000 title claims abstract description 21
- 238000004876 x-ray fluorescence Methods 0.000 title claims abstract description 9
- 238000002844 melting Methods 0.000 title claims description 14
- 230000008018 melting Effects 0.000 title claims description 14
- 238000004458 analytical method Methods 0.000 claims abstract description 14
- 239000011521 glass Substances 0.000 claims abstract description 4
- 238000010309 melting process Methods 0.000 claims description 8
- PSHMSSXLYVAENJ-UHFFFAOYSA-N dilithium;[oxido(oxoboranyloxy)boranyl]oxy-oxoboranyloxyborinate Chemical compound [Li+].[Li+].O=BOB([O-])OB([O-])OB=O PSHMSSXLYVAENJ-UHFFFAOYSA-N 0.000 claims description 7
- 239000000919 ceramic Substances 0.000 claims description 6
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 6
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 6
- 238000005259 measurement Methods 0.000 claims description 6
- 229910001020 Au alloy Inorganic materials 0.000 claims description 5
- 239000003353 gold alloy Substances 0.000 claims description 5
- JUWSSMXCCAMYGX-UHFFFAOYSA-N gold platinum Chemical compound [Pt].[Au] JUWSSMXCCAMYGX-UHFFFAOYSA-N 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 238000001304 sample melting Methods 0.000 claims description 3
- 238000007873 sieving Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- SWLVFNYSXGMGBS-UHFFFAOYSA-N ammonium bromide Chemical class [NH4+].[Br-] SWLVFNYSXGMGBS-UHFFFAOYSA-N 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 10
- 229910052717 sulfur Inorganic materials 0.000 abstract description 9
- 238000004846 x-ray emission Methods 0.000 abstract description 4
- 238000002360 preparation method Methods 0.000 description 6
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 239000011593 sulfur Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- UKFWSNCTAHXBQN-UHFFFAOYSA-N ammonium iodide Chemical class [NH4+].[I-] UKFWSNCTAHXBQN-UHFFFAOYSA-N 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000004907 flux Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000009614 chemical analysis method Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000001066 destructive effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000006082 mold release agent Substances 0.000 description 1
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
Classifications
-
- 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
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
The invention relates to a measuring method for detecting 7 elements in blast furnace slag by using an X-ray fluorescence spectrometry, which is used for solving the problem that a plurality of elements in the blast furnace slag cannot be detected simultaneously and rapidly by using the existing chemical method. Firstly, a pretreated blast furnace slag standard sample is prepared into a glass sheet after being melted, a working curve is established by using the standard sample, and then the blast furnace slag sample is analyzed and tested by an X-ray fluorescence spectrometer. The method can detect the contents of Ca, mg, al, si, ti, mn and S in the blast furnace slag, and has the advantages of short analysis time, high accuracy, good repeatability, no pollution and the like.
Description
Technical Field
The invention belongs to the technical field of chemical detection, and discloses a measuring method for detecting multiple elements in blast furnace slag by using an X-ray fluorescence spectrometry.
Background
The chemical composition analysis of the blast furnace slag has important guiding significance for the production of blast furnaces and converters. At present, the main analysis methods of slag include a chemical method, an inductively coupled plasma-atomic emission spectrometry (ICP-AES), and the like. Because the metallurgical slag matrix has complex components and more elements to be analyzed, the conventional detection method for sample treatment is relatively complicated, the analysis speed is low, and the method is not suitable for the production requirement of high pace.
Compared with the traditional chemical method which has the defects of complicated steps, long analysis time, large environmental pollution and the like, the X-ray spectrometer (XRF) analysis is used as a mature and high-precision rapid analysis technology, and is widely applied to the field of metallurgical chemical analysis and measurement due to good reproducibility, simultaneous measurement of multiple elements, simple sample preparation and non-destructive property, wherein the particle size effect and the mineral effect can be eliminated through melting and sample preparation, so that the analysis result is more accurate and has stronger persuasion. The melting method can oxidize the sulfur element in the sample into SO 2 The gas is released, so this method cannot measure sulfur. The sulfur content in the blast furnace slag is high, and the sulfur mainly exists in the form of molybdenum sulfide. And the blast furnace slag also contains components such as reduced metal, and the sample has serious corrosion to the crucible in the melting process.
Therefore, further development of a method for accurately and simultaneously detecting the contents of various elements of Ca, mg, al, si, ti, mn, S in blast furnace slag is required.
Disclosure of Invention
The invention aims to provide a method for measuring 7 elements in blast furnace slag by melting sample preparation-X-ray fluorescence so as to accurately and quickly measure impurity elements in the blast furnace slag.
In order to achieve the purpose, the invention adopts the following technical scheme:
the method for analyzing the impurity elements of the blast furnace slag by using the X-ray fluorescence spectrometer comprises the following steps:
(1) Preparation of a sample: drying the standard sample or the sample to be detected at 105 ℃ for 2-4h, grinding and sieving the sample to ensure that the particles of the sample reach more than 200 meshes,
(2) Placing the pretreated standard sample or sample to be detected, anhydrous lithium tetraborate and lithium carbonate in a ceramic crucible, uniformly stirring, transferring the ceramic crucible into a platinum-gold alloy crucible, then dropwise adding a release agent into the ceramic crucible, placing the ceramic crucible on a sample melting machine, cooling the ceramic crucible to obtain a glass fuse piece after the melting process is finished,
(3) Measurement conditions were as follows: the measurement conditions for each substance in the sample were as follows:
ti, mn: selecting a Kalpha line, controlling the pipe pressure to be 40kV, controlling the pipe flow to be 70mA, controlling the secondary target to be LiF, and measuring the time to be 20s;
al, si: selecting a Kalpha line, the pipe pressure is 40kV, the pipe flow is 70mA, the secondary target is PET, and the measuring time is 20s;
s: selecting a K alpha line, performing tube pressure of 40kV, performing tube flow of 70mA, performing secondary target Ge, and measuring for 20s;
ca: selecting a Kalpha line, performing tube pressure of 30kV, performing tube flow of 40mA, performing secondary target LiF, and measuring for 20s;
(4) And (3) standard curve preparation: preparing a standard substance according to the steps, and then analyzing by using an X-ray fluorescence spectrometer to establish a standard curve.
Further, the conditions of the melting process are: the temperature was set at 1500 ℃ and the melting time included: preheating time 180s, melting time 700s and standing time 10s.
Further, in the step (2), the sample to be detected, the anhydrous lithium tetraborate and the lithium carbonate are mixed according to the mass ratio of 1:12:1 in the ratio of 1. Lithium tetraborate is used as a flux, lithium carbonate is used as a fluxing agent, the dilution ratio of the flux to a sample is properly improved, the fluidity of the sample in the melting process can be increased, the matrix effect can be reduced, and the lithium tetraborate can be used as a protective layer for isolating the sample from a platinum-gold alloy crucible.
Further, the mold release agent in the step (1) is saturated ammonium iodide, and the addition amount of each gram of sample is 0.95g, namely 0.8mL of saturated ammonium iodide solution.
Has the advantages that: the invention provides a method for measuring Ca, mg, al, si, ti, mn and S elements in blast furnace slag by using melting sample preparation-X-ray fluorescence spectroscopy, which is simple and convenient to operate, can be effectively applied to the analysis and detection of the blast furnace slag, and has accurate and convincing detection results.
Detailed Description
In order to further explain the technical scheme of the invention, the invention is explained in detail by the specific embodiment.
The process according to the invention is described in detail with reference to the following examples:
1. preparation of a sample: and (3) drying the standard sample or the sample to be detected for 2-4h at 105 ℃, grinding the standard sample or the sample to be detected, and sieving the ground sample to enable the particles of the sample to reach more than 200 meshes.
2. Preparation of a sample melt sheet: taking the pretreated standard sample, anhydrous lithium tetraborate and lithium carbonate, and mixing the raw materials in a proportion of 1:12:1, transferring the mixture to a platinum crucible, adding 0.8ml of saturated ammonium iodide solution, placing the mixture in an automatic sample melting machine for melting, wherein the conditions of the melting process are as follows: the temperature was set at 1500 ℃, and the melting time included: preheating time 180s, melting time 700s and standing time 10s, taking out after the melting process is finished, cooling to room temperature and measuring.
TABLE 1 measurement conditions for each standard substance in the samples
3. Drawing a standard curve: 14 iron standard samples were selected to make glass fuse pieces, and the standard sample numbers and contents are shown in table 2 below.
TABLE 2 Standard samples and detailed tables of their contents
After the instrument is started up stably, according to the instrument parameter conditions listed in the table 1, a standard curve is established according to the intensity and the content, the correlation coefficient of Ca is 0.999, the correlation coefficient of Mg is 0.999, the correlation coefficient of Ti is 0.999, the correlation coefficient of Mn is 0.998, the correlation coefficient of Si is 0.999, the correlation coefficient of Al is 0.999, and the correlation coefficient of S is 0.999.
4. The contents of Ca, mg, al, si, ti, mn and S in the sample were measured.
(1) Testing of method accuracy
Three national standard substances (SX 74-04, SX74-03 and 612-1) are adopted for accuracy verification, and the measured value and the standard value are better in accordance with table 3.
TABLE 3 method accuracy test
(2) Method precision test
A standard sample (802-1) was taken and prepared in steps to prepare 10 samples, and the results are shown in Table 4.
TABLE 4 method precision test
As can be seen from Table 4, the RSD (%) of each element was less than 5%, indicating that the method is excellent in precision and has a certain feasibility of implementation.
In conclusion, the method for measuring the contents of Ca, mg, al, si, ti, mn and S in the slag by melting sample preparation-X fluorescence has the advantages of simple operation, environmental protection and safety, can simultaneously and quickly detect multiple elements, can replace the currently and commonly used chemical analysis method, X fluorescence tabletting method and the like, and has good analysis accuracy and precision and high analysis efficiency.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and amendments can be made without departing from the principle of the present invention, and these modifications and amendments should also be considered as the protection scope of the present invention.
Claims (5)
1. A method for melting and preparing sample-X-ray fluorescence blast furnace slag elements is characterized by comprising the following steps:
(1) Drying the standard sample or the sample to be detected for 2-4h, then grinding and sieving;
(2) Placing the standard sample or the sample to be detected, anhydrous lithium tetraborate and lithium carbonate which are processed in the step (1) into a ceramic crucible, uniformly stirring, transferring the mixture into a platinum-gold alloy crucible, then dropwise adding a release agent into the platinum-gold alloy crucible, placing the platinum-gold alloy crucible on a sample melting machine, and cooling to obtain a glass fuse piece after the melting process is finished;
(3) Selecting a corresponding standard sample, setting analysis conditions, analyzing by using an X-ray fluorescence spectrometer, and establishing a standard curve;
(4) And detecting the sample to be detected by using an X-ray fluorescence spectrometer.
2. The method of claim 1, wherein the melting process in step (2) comprises: the temperature was set at 1500 ℃, the preheating time was 180s, the melting time was 700s, and the standing time was 10s.
3. The method according to claim 1, wherein the analysis conditions in the step (3) are: ti, mn: selecting a Kalpha line, 40KV of pipe pressure, 70mA of pipe flow, liF of a secondary target and 20s of measuring time,
al, si: selecting a Kalpha line, 40kV of pipe pressure, 70mA of pipe flow, PET of a secondary target, measuring for 20s,
s: selecting a K alpha line, the pipe pressure is 40kV, the pipe flow is 70mA, the secondary target is Ge, the measuring time is 20s,
ca: the K.alpha.line was chosen, the tube pressure was 30kV, the tube flow was 40mA, the secondary target was LiF, and the measurement time was 20s.
4. The method according to claim 1, wherein the sample to be tested in the step (1), the anhydrous lithium tetraborate and the lithium carbonate are mixed according to a mass ratio of 1:12:1, and mixing.
5. The method of claim 1, wherein the release agent of step (1) is saturated ammonium bromide.
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| CN202211181783.9A CN115575430A (en) | 2022-09-27 | 2022-09-27 | Method for measuring elements in blast furnace slag by melting sample preparation-X-ray fluorescence |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116148296A (en) * | 2023-04-19 | 2023-05-23 | 中国科学院过程工程研究所 | Detection method of automatic XRF detection integrated device for metal-containing solid materials |
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| KR20030025549A (en) * | 2001-09-21 | 2003-03-29 | 스톨베르그 앤드 삼일 주식회사 | Method of analysing a fluorine content in a mold flux using fluorescent x-rays |
| CN112858361A (en) * | 2021-01-13 | 2021-05-28 | 广东韶钢松山股份有限公司 | Detection method for measuring slag pressing agent by melting method sample preparation X-ray fluorescence spectrometry |
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- 2022-09-27 CN CN202211181783.9A patent/CN115575430A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| KR20030025549A (en) * | 2001-09-21 | 2003-03-29 | 스톨베르그 앤드 삼일 주식회사 | Method of analysing a fluorine content in a mold flux using fluorescent x-rays |
| CN112858361A (en) * | 2021-01-13 | 2021-05-28 | 广东韶钢松山股份有限公司 | Detection method for measuring slag pressing agent by melting method sample preparation X-ray fluorescence spectrometry |
Non-Patent Citations (2)
| Title |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116148296A (en) * | 2023-04-19 | 2023-05-23 | 中国科学院过程工程研究所 | Detection method of automatic XRF detection integrated device for metal-containing solid materials |
| CN116148296B (en) * | 2023-04-19 | 2023-08-25 | 中国科学院过程工程研究所 | Detection method of automatic XRF detection integrated device for metal-containing solid materials |
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