CN113866143A - Rapid detection of SiO in resource sample2And/or CaO content - Google Patents
Rapid detection of SiO in resource sample2And/or CaO content Download PDFInfo
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- CN113866143A CN113866143A CN202111103036.9A CN202111103036A CN113866143A CN 113866143 A CN113866143 A CN 113866143A CN 202111103036 A CN202111103036 A CN 202111103036A CN 113866143 A CN113866143 A CN 113866143A
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- 238000001514 detection method Methods 0.000 title claims abstract description 25
- 230000003647 oxidation Effects 0.000 claims abstract description 53
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 53
- 238000000034 method Methods 0.000 claims abstract description 35
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 17
- 238000002844 melting Methods 0.000 claims abstract description 16
- 230000008018 melting Effects 0.000 claims abstract description 16
- 238000002795 fluorescence method Methods 0.000 claims abstract description 15
- 230000001590 oxidative effect Effects 0.000 claims abstract description 15
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- 238000002156 mixing Methods 0.000 claims abstract description 5
- 230000001603 reducing effect Effects 0.000 claims abstract description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 34
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 27
- 239000000377 silicon dioxide Substances 0.000 claims description 23
- 229910052681 coesite Inorganic materials 0.000 claims description 19
- 229910052906 cristobalite Inorganic materials 0.000 claims description 19
- 229910052682 stishovite Inorganic materials 0.000 claims description 19
- 229910052905 tridymite Inorganic materials 0.000 claims description 19
- 229910052742 iron Inorganic materials 0.000 claims description 17
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 claims description 12
- 239000000126 substance Substances 0.000 claims description 11
- 239000002893 slag Substances 0.000 claims description 9
- 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 8
- HZRMTWQRDMYLNW-UHFFFAOYSA-N lithium metaborate Chemical compound [Li+].[O-]B=O HZRMTWQRDMYLNW-UHFFFAOYSA-N 0.000 claims description 8
- XZXYQEHISUMZAT-UHFFFAOYSA-N 2-[(2-hydroxy-5-methylphenyl)methyl]-4-methylphenol Chemical compound CC1=CC=C(O)C(CC=2C(=CC=C(C)C=2)O)=C1 XZXYQEHISUMZAT-UHFFFAOYSA-N 0.000 claims description 7
- 229940107816 ammonium iodide Drugs 0.000 claims description 7
- SWLVFNYSXGMGBS-UHFFFAOYSA-N ammonium bromide Chemical compound [NH4+].[Br-] SWLVFNYSXGMGBS-UHFFFAOYSA-N 0.000 claims description 5
- 238000004364 calculation method Methods 0.000 claims description 5
- 238000001304 sample melting Methods 0.000 claims description 5
- 230000004907 flux Effects 0.000 claims description 4
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 3
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 3
- 239000000155 melt Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 abstract description 20
- 238000004458 analytical method Methods 0.000 abstract description 12
- 229910052697 platinum Inorganic materials 0.000 abstract description 10
- 239000007787 solid Substances 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 5
- 230000009471 action Effects 0.000 abstract description 4
- 239000000292 calcium oxide Substances 0.000 description 64
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 62
- 239000002910 solid waste Substances 0.000 description 10
- 238000004519 manufacturing process Methods 0.000 description 7
- 230000008569 process Effects 0.000 description 5
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 235000012239 silicon dioxide Nutrition 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 230000004927 fusion Effects 0.000 description 2
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 206010039897 Sedation Diseases 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 229940006460 bromide ion Drugs 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 210000003710 cerebral cortex Anatomy 0.000 description 1
- 238000012790 confirmation Methods 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
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- 230000007613 environmental effect Effects 0.000 description 1
- 238000001917 fluorescence detection Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
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- 239000010703 silicon Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
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- 230000005619 thermoelectricity Effects 0.000 description 1
- 238000010200 validation analysis Methods 0.000 description 1
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- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
-
- 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
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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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
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- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
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- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The application relates to the technical field of solid secondary resource sample detection, in particular to a method for rapidly detecting SiO in a resource sample2And/or CaO content. The method comprises the steps of burning and oxidizing a sample to be detected to obtain a primary oxidized sample; obtaining the burning loss value of the sample to be detected according to the sample to be detected and the primary oxidation sample; mixing and melting the primary oxidation sample with a fluxing agent and an oxidizing agent, and reducing the melting temperature of the primary oxidation sample through the combined action of the fluxing agent and the oxidizing agent to obtain a secondary oxidation sample; obtaining various SiO-containing materials2And SiO of standard sample of CaO2And/or a CaO standard curve; detecting the secondary oxidation sample by a fluorescence method to obtain SiO in the sample to be detected2And/or of CaOThe usage times of the yellow platinum crucible are increased, the melting temperature of a primary oxidation sample is reduced, and the sample to be detected can be detected by a fluorescence method; the detection is carried out by a fluorescence method, the detection and analysis time is shortened, and the labor consumption is low.
Description
Technical Field
The application relates to the technical field of solid secondary resource sample detection, in particular to a method for rapidly detecting SiO in a resource sample2And/or CaO content.
Background
In order to promote the comprehensive utilization and efficiency improvement of solid secondary resources and develop the research on the production process of kiln slag of a rotary kiln, the detection of solid waste raw materials such as iron making dry ash, gas ash, mixed materials, OG fine mud, fine ash, anhydrous precipitated mud, pipeline ash and the like and finished products such as kiln slag, zinc hypoxide and the like is urgently needed to be completed, detection elements comprise more than ten types of iron, metallic iron, carbon, sulfur, calcium oxide, silicon dioxide and the like, wherein alkalinity indexes influenced by the content of the silicon dioxide and the calcium oxide are particularly important for guiding the production of the rotary kiln.
The solid waste is various in types, the components are complex, the content of metallic iron is high (up to 65%), when various acids are tried, a sample cannot be completely dissolved, a platinum pot or a yellow platinum crucible is needed for alkali fusion, the metallic iron content of the sample is high, the platinum crucible can be destroyed, and analysis cannot be performed. If acid dissolution is adopted, metal substances are dissolved firstly, the insoluble substances are filtered and then subjected to alkali fusion treatment, and finally the solutions are combined, and the chemical wet method analysis is adopted, so that the analysis time is long, the manpower consumption is high, the analysis of 1 batch of samples needs 2 persons for 8 hours, and the production requirements are not met.
The solid secondary resource sample has the problems of high metal iron content, various types, complex components, incapability of adopting fluorescence fuse analysis, long chemical wet analysis time, high labor consumption and incapability of meeting production requirements.
Disclosure of Invention
The application provides a rapid detection of SiO in a resource sample2And/or CaO content to solve the problem that SiO in a solid secondary resource sample cannot be detected by a fluorescence method2And/or the chemical content of CaO.
In a first aspect, the present application provides a method for rapidly detecting SiO in a resource sample2And/or CaO content, the method comprising the steps of:
for SiO-containing2And/or burning and oxidizing a CaO sample to be detected to obtain a primary oxidized sample;
obtaining the burning loss value of the sample to be detected according to the sample to be detected and the primary oxidation sample;
mixing and melting the primary oxidation sample with a fluxing agent and an oxidizing agent, and reducing the melting temperature of the primary oxidation sample through the fluxing agent to obtain a secondary oxidation sample;
obtaining various SiO-containing materials2And/or SiO of a standard sample of CaO2And/or a CaO standard curve;
detecting the secondary oxidation sample by a fluorescence method and according to the SiO2And/or determining SiO in the secondary oxidation sample by a CaO standard curve2And/or a detected value of CaO;
according to the detection value and the burning loss value, obtaining SiO in the sample to be detected2And/or the content of CaO.
Optionally, the SiO is contained in the pair2And/or burning and oxidizing a CaO sample to be detected to obtain a primary oxidized sample, wherein the primary oxidized sample comprises: and (3) burning the sample to be detected for 2-4 hours at the temperature of 700 ℃ and 800 ℃ to obtain a primary oxidation sample.
Optionally, the calculation expression of the burning loss value is as follows:
in the formula, omega is a burning loss value, and m is the mass of a sample to be detected before burning; m is1Mass of primary oxidized sample.
Optionally, the mass ratio of the primary oxidation sample to the oxidizing agent is 1: 1-1.5.
Optionally, the oxidizing agent comprises lithium nitrate or lithium carbonate.
Optionally, the flux includes lithium tetraborate and lithium metaborate, and a mass ratio of the lithium tetraborate to the lithium metaborate is 1: 1-67: 33.
optionally, the detecting the secondarily oxidized sample by a fluorescence method includes:
carrying out sample melting and demoulding on the secondary oxidation sample to obtain a melt sheet;
detecting the fuse piece by a fluorescence method;
the demolding release agent comprises: ammonium iodide or ammonium bromide.
Optionally, the method further includes:
determining various standard samples according to the chemical components of the sample to be detected, and obtaining SiO of the various standard samples2And/or the content of CaO;
according to the SiO of each standard sample2And/or content of CaO to form SiO2And/or a CaO standard curve;
the various types of standard samples comprise slag standard samples and iron ore standard samples.
Optionally, the SiO in the sample to be detected2And/or the calculation expression of the content of CaO is as follows:
M＝m2×(100-ω)/100
wherein M is SiO in the sample to be detected2Or the mass content of CaO, m2SiO in the fuse sheet2Or CaO detection value, omega is a burning loss value.
In a second aspect, the present application provides a method for rapidly detecting SiO in a resource sample2And/or CaO content, the rapid detection of the SiO in the resource sample according to the first aspect2And/or CaO content in a rotary kiln.
Compared with the prior art, the technical scheme provided by the embodiment of the application has the following advantages:
the method provided by the embodiment of the application is used for treating SiO-containing2Burning and oxidizing a CaO sample to be detected to obtain a primary oxidized sample; mixing the primary oxidation sample with a fluxing agent and an oxidant, and melting to reduce the melting temperature of the primary oxidation sample, protect a yellow platinum crucible, improve the use times of the yellow platinum crucible, and provide possibility for the sample to be detected by a fluorescence method; simultaneously solves the problem that the metal iron content of the sample to be measured is higherThe problem that fluorescence cannot be used for analysis; detecting the secondary oxidation sample by fluorescence, according to the SiO2And/or determining SiO in the secondary oxidation sample by a CaO standard curve2And/or the detection value of CaO to obtain SiO in the sample to be detected2And/or the content of CaO, so that the detection and analysis time is shortened, the labor consumption is low, and the production requirement can be met.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the invention and together with the description, serve to explain the principles of the invention.
In order to more clearly illustrate the embodiments or technical solutions in the prior art of the present invention, the drawings used in the description of the embodiments or prior art will be briefly described below, and it is obvious for those skilled in the art that other drawings can be obtained according to these drawings without any creative effort.
FIG. 1 is a schematic diagram illustrating an embodiment of the present disclosure for rapidly detecting SiO in a resource sample2And/or a schematic flow diagram of a method of CaO content;
FIG. 2 is a schematic diagram of SiO process according to an embodiment of the present application2A standard curve graph;
FIG. 3 is a CaO standard curve provided in the examples of the present application;
FIG. 4 is a SiO solid layer provided in the examples of the present application2And a single-valued control map of CaO accuracy;
FIG. 5 is a schematic diagram of SiO process according to an embodiment of the present application2And a single value control chart for CaO precision.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are some embodiments of the present application, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
In a first aspect, the present application provides a method for rapidly detecting SiO in a resource sample2And/or CaO content, as shown in fig. 1, comprising the steps of:
s1, for SiO2And/or burning and oxidizing a CaO sample to be detected to obtain a primary oxidized sample;
as an alternative embodiment, the SiO-containing component2And/or burning and oxidizing a CaO sample to be detected to obtain a primary oxidized sample, wherein the primary oxidized sample comprises: and (3) burning the sample to be detected for 2-4 hours at the temperature of 700 ℃ and 800 ℃ to obtain a primary oxidation sample.
S2, obtaining a burning loss value of the sample to be detected according to the sample to be detected and the primary oxidation sample;
as an alternative embodiment, the calculation expression of the burning loss value is:
in the formula, omega is a burning loss value, and m is the mass of a sample to be detected before burning; m is1Mass of primary oxidized sample.
As an alternative embodiment, the mass ratio of the primary oxidation sample to the oxidizing agent is 1: 1 to 1.5.
S3, mixing the primary oxidation sample with a fluxing agent and an oxidant, melting, and reducing the melting temperature of the primary oxidation sample through the fluxing agent to obtain a secondary oxidation sample;
in the embodiment of the application, a fluxing agent is weighed in a yellow platinum crucible, then a primary oxidation sample and an oxidant are weighed, the primary oxidation sample is poured on the fluxing agent, the sample is not stirred, the oxidant covers the primary oxidation sample (slightly stirred with the primary oxidation sample and does not contact the bottom of the pot), the oxidation is carried out at the low temperature of 800-850 ℃ on a high-frequency sample melting machine, then the temperature is raised to about 1000 ℃, the sample melting time is 3min, the sample is taken down and shaken into pieces, and a secondary oxidation sample is obtained; can protect the yellow platinum crucible and provide the service life of the yellow platinum crucible.
As an alternative embodiment, the flux includes lithium tetraborate and lithium metaborate, and the mass ratio of the lithium tetraborate to the lithium metaborate is 1: 1-67: 33.
as an alternative embodiment, the oxidizing agent comprises lithium nitrate or lithium carbonate.
As an alternative embodiment, the detecting the secondarily oxidized sample by the fluorescence method includes:
carrying out sample melting and demoulding on the secondary oxidation sample to obtain a melt sheet;
detecting the fuse piece by a fluorescence method;
the demolding release agent comprises: ammonium iodide or ammonium bromide.
In this application, both ammonium iodide and ammonium bromide can achieve the demolding effect, and the ammonium bromide is colorless or white crystalline powder. Is tasteless and odorless. It has slight hygroscopicity in air. Sublimation at 452 deg.C, bromide ion can enhance the inhibitory process of cerebral cortex, produce sedation, and ammonium iodide is preferred for environmental and experimenter safety considerations.
S4, obtaining various SiO-containing materials2And/or SiO of a standard sample of CaO2And/or a CaO standard curve;
in the embodiment of the application, SiO-containing materials can be obtained2Or CaO standard to obtain SiO2Or CaO, or SiO-containing2And CaO standard to obtain SiO2Or CaO, or simultaneously obtaining SiO2And a standard curve for CaO. The content of the step S4 may be performed after the step S3, at any time position from the steps S1 to S3, or before the step S1.
As an alternative embodiment, the types of standard samples include slag standard samples and iron ore standard samples.
In the embodiment of the application, the content and the property of silicon dioxide and calcium oxide in the solid waste secondary resource sample and the iron content in the solid waste secondary resource sample are finally determined, and a standard curve is established by adopting slag and iron ore standard samples as shown in table 1.
Table 1 fluorescence-establishing standard curves for the contents of the components of various slag standard samples and various iron ore standard samples used.
In the examples of the present application, SiO2The linearity of the standard curve and the linearity of the CaO standard curve are respectively as follows: r (SiO)2) 0.9995, as shown in fig. 2; r (cao) ═ 0.9996, as shown in fig. 3.
S5, detecting the secondary oxidation sample by a fluorescence method, and detecting the secondary oxidation sample according to the SiO2And/or determining SiO in the secondary oxidation sample by a CaO standard curve2And/or a detected value of CaO;
s6, according to the detection value and the burning loss value, obtaining SiO in the sample to be detected2And/or the content of CaO.
As an optional implementation, the method further comprises:
determining various standard samples according to the chemical components of the sample to be detected, and obtaining SiO of the various standard samples2And/or the content of CaO;
according to the SiO of each standard sample2And/or content of CaO to form SiO2And/or a CaO standard curve;
the various types of standard samples comprise slag standard samples and iron ore standard samples.
As an optional implementation mode, SiO in the sample to be detected2And/or the calculation expression of the content of CaO is as follows:
M＝m2×(100-ω)/100
wherein M is SiO in the sample to be detected2Or the mass content of CaO, m2SiO in the fuse sheet2Or CaO detection value, omega is a burning loss value.
In the embodiment of the application, the solid waste secondary resource sample is oxidized twice, so that the solid waste secondary resource sample containing metallic iron can be analyzed by adopting the fluorescent fuse piece, the highest iron content can reach 65%, and the rapid, accurate and efficient detection is realized.
In the embodiment of the application, the silicon-containing oxide film can be prepared by2Or burning and oxidizing a CaO sample to be detected to respectively detect SiO2Or the content of CaO, or SiO2Burning and oxidizing a sample to be detected of CaO to obtain SiO2Or CaO content, or SiO content measured simultaneously2And the content of CaO.
In a second aspect, the present application provides a method for rapidly detecting SiO in a resource sample2And/or CaO content, the rapid detection of SiO in a resource sample according to the first aspect2And/or CaO content in a rotary kiln.
The method of the present invention will be described in detail below with reference to experimental data.
In the embodiment of the application, the method is used for treating SiO in the resource sample2And CaO content, the following instruments and reagents can be used. The instrument comprises the following steps: ARL 9900X-ray fluorescence spectrometer (us thermoelectricity); high frequency melt machine (Analymate-V2). Reagent: lithium tetraborate and lithium metaborate are mixed with a flux and a high-purity reagent; ammonium iodide, analytically pure; lithium nitrate, premium grade purity.
In order to ensure the precision and accuracy of the analyzed samples, the analysis conditions of the X-ray fluorescence spectrometer were selected and shown in Table 2.
Table 2 main analytical parameters of the instrument.
(1) Preliminary oxidation (ignition reduction treatment) of the sample: weighing 1.5g of solid waste secondary resource sample in a ceramic crucible, adjusting the temperature of a muffle furnace to 800 ℃, burning for 2 hours, preliminarily oxidizing metal substances in the sample, and calculating a burning loss value to obtain a preliminary oxidation sample.
(2) Secondary oxidation (oxidation using lithium nitrate): weighing 4g of fluxing agent (the mass ratio of lithium tetraborate to lithium metaborate is 1: 1) in a yellow platinum crucible, weighing 0.4g of primary oxidation sample, pouring the primary oxidation sample on the fluxing agent, weighing 0.4g of lithium nitrate to cover the primary oxidation sample (slightly stirring the primary oxidation sample without contacting the bottom of a pot), and heating the primary oxidation sample on a high-frequency melting machine at the temperature of 800-.
(3) Melt sample
Adjusting the high-frequency melting machine to 1000 ℃ melting piece, adding a proper amount of ammonium iodide release agent, demoulding, melting the sample for 3min, taking down, and shaking to obtain the melting piece.
(4) Establishing a fluorescence standard curve: finally determining by researching the content and the property of silicon dioxide and calcium oxide in the solid waste secondary resource sample, wherein a slag standard sample and an iron ore standard sample are adopted, and are shown in the table 1; and establishing a standard curve, SiO2Is shown in FIG. 2, wherein x1As intensity of fluorescence, Y1By content of SiO2In the standard curve of (2), Y1＝1.7337x1+0.2039R1 2＝0.9995，R1 2The correlation coefficient, i.e., the degree of fit of the curve, is better as approaching 1; the standard curve for CaO is shown in FIG. 3, x2As intensity of fluorescence, Y2In the standard curve of CaO by content, Y2＝0.225x2-0.3255，R2 2＝0.9991，R22The more the correlation coefficient, i.e., the degree of fitting of the curve, approaches 1, the better.
(5) Burn out correction
The fluorescence detection result is m2Since the sample is burned before analysis, the burning loss value is used to convert the final result M.
(6) Accuracy validation
Carrying out conventional chemical method detection and fluorescence method detection analysis on 15 batches of solid waste secondary resource samples, wherein the absolute value of the difference value of the two methods is the accuracy of the method, and the accuracy of the method is shown in figure 4, wherein in the figure, SiO is shown in the figure2The average accuracy value is 0.20 percent, the average accuracy value of CaO is 0.25 percent, and the production requirement is met.
(7) Confirmation of precision
Respectively analyzing 15 batches of solid waste secondary resource samples twice by a fluorescence method, wherein the relative extreme difference is the precision, and the precision is shown in figure 5, wherein in the figure, SiO is2The precision average value is 2.10 percent, the precision average value of CaO is 2.50 percent, and the production requirement is met.
It is noted that, in this document, relational terms such as "first" and "second," and the like, may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
The foregoing are merely exemplary embodiments of the present invention, which enable those skilled in the art to understand or practice the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. Rapid detection of SiO in resource sample2And/or CaO content, characterized in that it comprises the steps of:
for SiO-containing2And/or burning and oxidizing a CaO sample to be detected to obtain a primary oxidized sample;
obtaining the burning loss value of the sample to be detected according to the sample to be detected and the primary oxidation sample;
mixing and melting the primary oxidation sample with a fluxing agent and an oxidizing agent, and reducing the melting temperature of the primary oxidation sample through the fluxing agent to obtain a secondary oxidation sample;
obtaining various SiO2And/or SiO of a standard sample of CaO2And/or a CaO standard curve;
detecting the secondary oxidation sample by a fluorescence method and according to the SiO2And/or determining SiO in the secondary oxidation sample by a CaO standard curve2And/or a detected value of CaO;
according to the detection value and the burning loss value, obtaining SiO in the sample to be detected2And/or the content of CaO.
2. The method of claim 1, wherein the SiO-containing component is present in the mixture2And/or burning and oxidizing a CaO sample to be detected to obtain a primary oxidized sample, wherein the primary oxidized sample comprises: and (3) burning the sample to be detected for 2-4 hours at the temperature of 700 ℃ and 800 ℃ to obtain a primary oxidation sample.
3. The method of claim 2, wherein the calculated expression for the burnout value is:
in the formula, omega is a burning loss value, and m is the mass of a sample to be detected before burning; m is1Mass of primary oxidized sample.
4. The method of claim 1, wherein the mass ratio of the primary oxidation sample to the oxidizing agent is 1: 1 to 1.5.
5. The method of claim 1, wherein the flux comprises lithium tetraborate and lithium metaborate, and wherein the mass ratio of the lithium tetraborate to the lithium metaborate is from 1: 1 to 67: 33.
6. The method of claim 1, wherein the oxidizing agent comprises lithium nitrate or lithium carbonate.
7. The method of claim 1, further comprising:
determining various SiO-containing substances according to the chemical components of the sample to be detected2And CaO standard samples, and obtaining SiO of various standard samples2And/or the content of CaO;
according to the SiO of each standard sample2And/or content of CaO to form SiO2And/or a CaO standard curve;
the various types of standard samples comprise slag standard samples and iron ore standard samples.
8. The method of claim 1, wherein the fluorescently detecting the secondarily oxidized sample comprises:
carrying out sample melting and demoulding on the secondary oxidation sample to obtain a melt sheet;
detecting the fuse piece by a fluorescence method;
the demolding release agent comprises: ammonium iodide or ammonium bromide.
9. The method of claim 8, wherein the sample to be tested is SiO2And/or the calculation expression of the content of CaO is as follows:
M＝m2×(100-ω)/100
wherein M is SiO in the sample to be detected2Or the mass content of CaO, m2SiO in the fuse sheet2Or CaO detection value, omega is a burning loss value.
10. Rapid detection of SiO in resource sample2And/or CaO content, in which the rapid detection of CaO as claimed in any one of claims 1 to 9 is carried outSiO in source sample2And/or CaO content in a rotary kiln.
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000121623A (en) * | 1998-10-16 | 2000-04-28 | Ngk Insulators Ltd | Decomposing method and analyzing method for nonoxidizing sample |
| JP2013246115A (en) * | 2012-05-29 | 2013-12-09 | Seiko Epson Corp | Optical device and detector |
| CN104977266A (en) * | 2015-04-24 | 2015-10-14 | 河北中医学院 | Apparatus and method for rapidly measuring sulfur dioxide residue level in Chinese herb |
| CN105784747A (en) * | 2016-05-30 | 2016-07-20 | 内蒙古包钢钢联股份有限公司 | Method for detecting silicon dioxide, aluminum sesquioxide, calcium oxide and magnesium oxide in acetylene sludge |
| CN107024468A (en) * | 2017-03-17 | 2017-08-08 | 唐山钢铁集团有限责任公司 | The assay method of iron, aluminium, manganese, calcium, titanium, silicon, magnesium in covering slag |
| CN107543807A (en) * | 2017-07-10 | 2018-01-05 | 首钢京唐钢铁联合有限责任公司 | Detect TiO in high titanium powder2Method of content |
| EA201800466A1 (en) * | 2018-07-24 | 2020-01-31 | Белорусский Национальный Технический Университет | METHOD FOR PREPARING A FLUX ON THE BASIS OF SECONDARY ALUMINUM CONTAINING SLAG |
| CN111982951A (en) * | 2020-08-31 | 2020-11-24 | 广东韶钢松山股份有限公司 | Method for processing sample and determining element content |
| CN113402167A (en) * | 2021-07-13 | 2021-09-17 | 中国振华集团云科电子有限公司 | Method for improving uniformity of high-temperature melting calcium-boron-silicon glass |
-
2021
- 2021-09-18 CN CN202111103036.9A patent/CN113866143B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000121623A (en) * | 1998-10-16 | 2000-04-28 | Ngk Insulators Ltd | Decomposing method and analyzing method for nonoxidizing sample |
| JP2013246115A (en) * | 2012-05-29 | 2013-12-09 | Seiko Epson Corp | Optical device and detector |
| CN104977266A (en) * | 2015-04-24 | 2015-10-14 | 河北中医学院 | Apparatus and method for rapidly measuring sulfur dioxide residue level in Chinese herb |
| CN105784747A (en) * | 2016-05-30 | 2016-07-20 | 内蒙古包钢钢联股份有限公司 | Method for detecting silicon dioxide, aluminum sesquioxide, calcium oxide and magnesium oxide in acetylene sludge |
| CN107024468A (en) * | 2017-03-17 | 2017-08-08 | 唐山钢铁集团有限责任公司 | The assay method of iron, aluminium, manganese, calcium, titanium, silicon, magnesium in covering slag |
| CN107543807A (en) * | 2017-07-10 | 2018-01-05 | 首钢京唐钢铁联合有限责任公司 | Detect TiO in high titanium powder2Method of content |
| EA201800466A1 (en) * | 2018-07-24 | 2020-01-31 | Белорусский Национальный Технический Университет | METHOD FOR PREPARING A FLUX ON THE BASIS OF SECONDARY ALUMINUM CONTAINING SLAG |
| CN111982951A (en) * | 2020-08-31 | 2020-11-24 | 广东韶钢松山股份有限公司 | Method for processing sample and determining element content |
| CN113402167A (en) * | 2021-07-13 | 2021-09-17 | 中国振华集团云科电子有限公司 | Method for improving uniformity of high-temperature melting calcium-boron-silicon glass |
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