CN116380958A - Fluorescence detection method for TiO2 content in ore - Google Patents
Fluorescence detection method for TiO2 content in ore Download PDFInfo
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- CN116380958A CN116380958A CN202310516831.3A CN202310516831A CN116380958A CN 116380958 A CN116380958 A CN 116380958A CN 202310516831 A CN202310516831 A CN 202310516831A CN 116380958 A CN116380958 A CN 116380958A
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- 238000000034 method Methods 0.000 title claims abstract description 43
- 238000001917 fluorescence detection Methods 0.000 title claims abstract description 10
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title 2
- 238000001514 detection method Methods 0.000 claims abstract description 24
- 238000004458 analytical method Methods 0.000 claims abstract description 22
- 229910010413 TiO 2 Inorganic materials 0.000 claims abstract description 13
- 238000001506 fluorescence spectroscopy Methods 0.000 claims abstract description 6
- 238000004519 manufacturing process Methods 0.000 claims abstract description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 54
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 34
- 238000002844 melting Methods 0.000 claims description 30
- 230000008018 melting Effects 0.000 claims description 30
- 229910052742 iron Inorganic materials 0.000 claims description 24
- AMXOYNBUYSYVKV-UHFFFAOYSA-M lithium bromide Chemical compound [Li+].[Br-] AMXOYNBUYSYVKV-UHFFFAOYSA-M 0.000 claims description 24
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 claims description 24
- 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 19
- 229910052697 platinum Inorganic materials 0.000 claims description 17
- 238000005303 weighing Methods 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 10
- 239000003153 chemical reaction reagent Substances 0.000 claims description 7
- 238000004876 x-ray fluorescence Methods 0.000 claims description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 229910052573 porcelain Inorganic materials 0.000 claims description 6
- 238000012360 testing method Methods 0.000 claims description 6
- 230000004907 flux Effects 0.000 claims description 5
- 239000011159 matrix material Substances 0.000 claims description 5
- 238000005259 measurement Methods 0.000 claims description 5
- VJFCXDHFYISGTE-UHFFFAOYSA-N O=[Co](=O)=O Chemical compound O=[Co](=O)=O VJFCXDHFYISGTE-UHFFFAOYSA-N 0.000 claims description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 3
- 239000012141 concentrate Substances 0.000 claims description 3
- 230000005284 excitation Effects 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000003892 spreading Methods 0.000 claims description 3
- MRHSJWPXCLEHNI-UHFFFAOYSA-N [Ti].[V].[Fe] Chemical compound [Ti].[V].[Fe] MRHSJWPXCLEHNI-UHFFFAOYSA-N 0.000 claims description 2
- 239000000126 substance Substances 0.000 abstract description 3
- 239000003814 drug Substances 0.000 abstract description 2
- 229940079593 drug Drugs 0.000 abstract description 2
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 238000009628 steelmaking Methods 0.000 abstract description 2
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(2+);cobalt(3+);oxygen(2-) Chemical group [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- YDZQQRWRVYGNER-UHFFFAOYSA-N iron;titanium;trihydrate Chemical compound O.O.O.[Ti].[Fe] YDZQQRWRVYGNER-UHFFFAOYSA-N 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012921 fluorescence analysis Methods 0.000 description 1
- 239000007850 fluorescent dye Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000005375 photometry Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- GFNGCDBZVSLSFT-UHFFFAOYSA-N titanium vanadium Chemical compound [Ti].[V] GFNGCDBZVSLSFT-UHFFFAOYSA-N 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
Images
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
-
- 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
Abstract
The invention relates to TiO in ore 2 A fluorescence detection method of content belongs to the detection field. TiO in ore 2 The fluorescence detection method of the content comprises the following process steps: s1, preparing a standard sample for drawing a working curve; s2, preparing a molten sample piece; s3, setting the working conditions of a detection instrument: detection of TiO in ore by using melt fluorescence spectrometry 2 The content of the X-ray tube is set to be 50mA for working current, 50KV for voltage and K for the optimal analysis line α Scanning the strength of a standard sample and registering; s4, drawing a working curve; s5, sample analysis: unknown TiO 2 The sample to be measured is processed according to the steps of S2 and S3, and TiO in the ore is obtained by using the standard working curve 2 The content is as follows. The method provided by the invention is used for detecting TiO in ores 2 The elements have short period, less chemical drugs, little environmental pollution and guidance on steelmaking and ironmaking production.
Description
Technical Field
The invention relates to TiO in ore 2 Fluorescence detection formula for contentThe method belongs to the detection field.
Background
Iron ore is a raw material for charging in the iron and steel industry. TiO in ore 2 The main economic effect is as follows, in the iron and steel industry, adding a proper amount of ilmenite into raw materials can improve the wear resistance, strength, hardness, ductility and the like of steel, and reduce the cost by 8-10%.
TiO in iron ore in general 2 The content of the fluorescent dye is about 1%, the detection method adopts a photometry or a titration method in chemical analysis, the wet analysis has long analysis period and complex operation. Aiming at the aim of instrumented inspection, the function of an X fluorescence analyzer is developed, and fluorescence analysis of iron ore TiO is performed 2 Is a test method of (2). The fluorescence spectroscopy samples were prepared by a tabletting method and a melting tablet method. If the tabletting method is adopted, cracks are prevented from being generated in the tabletting process to influence the X-fluorescence measurement analysis result, and in addition, due to mineral effect and particle effect, tiO is influenced 2 The use of the melt sheet method eliminates various matrix effects.
In combination with the requirements, a TiO with high accuracy and precision is developed 2 An element detection method. Detection of TiO by fluorescence melting sheet method 2 The standard sample with certain gradient is accumulated, the working curve is established according to the working principle that the element content is in direct proportion to the strength, the test can also be applied to TiO with certain content in ore by adjusting the concentration of the standard sample, expanding the detection range and changing the method 2 And (5) element detection.
Disclosure of Invention
The invention provides TiO in iron ore 2 And (3) a method for detecting element fluorescence.
TiO in ore 2 The fluorescence detection method of the content comprises the following process steps:
s1, preparing a standard sample of a drawing working curve: selecting TiO 2 Iron ore samples with a certain gradient of element content;
s2, preparing a molten sample piece: the sample is subjected to melting treatment under the following conditions: pouring a certain mass of sample into a platinum yellow crucible filled with anhydrous lithium tetraborate flux and internal standard reagent cobalt trioxide, uniformly stirring, adding a release agent lithium bromide solution lithium nitrate solution, placing the platinum yellow crucible into a melting furnace, setting the melting temperature to 1050 ℃, and setting the melting time to 16 minutes;
s3, setting the working conditions of a detection instrument: detection of TiO in ore by using melt fluorescence spectrometry 2 The content of the X-ray tube is set to be 50mA for working current, 50KV for voltage and K for the optimal analysis line α Scanning the strength of a standard sample and registering;
s4, drawing a working curve: the working curve is formed by correspondingly drawing the net strength of the titanium element analysis line in the selected standard sample and the standard content (%): in the working curve drawing process, determining one block as a standardized sample, setting measurement conditions, and automatically generating a working curve by adopting Simultix software; during sample analysis, an X-ray fluorescence spectrometer is used for testing the intensity value of a sample to be tested, and the intensity value measured by the sample to be tested is converted into a standard content value through an established working curve of standard content and net intensity;
s5, sample analysis: unknown TiO 2 The sample to be measured is processed according to the steps of S2 and S3, and TiO in the ore is obtained by using the standard working curve 2 The content is as follows.
Preferably, in the step S1, the iron ore sample is selected from TiO 2 Iron ore/iron concentrate national standard sample with the element content range of 0.10-0.50 percent.
Preferably, in the step S2, the concentration of the lithium bromide solution is 400g/L; the concentration of the lithium nitrate solution was 300g/L.
Preferably, in the step S2, the volume ratio of the lithium bromide solution to the lithium nitrate solution is 2-5:5.
Preferably, in the step S2, the mass ratio of the sample to the total amount of anhydrous lithium tetraborate is 0.35:5.
Preferably, in the step S2, 0.3500g±0.0002g of the dried sample is weighed and placed in one porcelain crucible, and then 5.000g±0.0002g of anhydrous lithium tetraborate is weighed and placed in the other porcelain crucible; firstly pouring 1g of anhydrous lithium tetraborate into the bottom of a platinum yellow crucible, spreading, pouring 3g of anhydrous lithium tetraborate into the crucible containing the sample, uniformly mixing, pouring into the platinum yellow crucible, cleaning the crucible residual material containing the sample by using the rest anhydrous lithium tetraborate, adding platinum Huang Ganguo, adding 5 drops of lithium nitrate solution with the concentration of 300g/L and 2-5 drops of lithium bromide solution with the concentration of 400g/L, and putting into a high-frequency melting furnace.
Preferably, in the step S2, the pattern is a heat time of 60 seconds and a heat temperature of 800 ℃; the secondary heating time is 120 seconds, the secondary heating temperature is 1050 ℃, the melting time is 240 seconds, the melting temperature is 1050 ℃, the self-cooling time is 120 seconds, the air cooling time is 120 seconds, and the swinging speed is 8 grades.
Preferably, in the step S3, the detection instrument is a single-channel sequential scanning X-ray fluorescence spectrometer of type simux 14 using an Rh target X-ray tube as an excitation source and a simux as analysis software.
The invention has the preferable technical scheme that:
TiO in ore 2 The fluorescence detection method of the content comprises the following process steps:
s1, preparing a standard sample of a drawing working curve: selecting TiO 2 Iron ore samples with certain gradients of element content are needed;
s2, preparing a molten sample piece: the sample is subjected to melting treatment under the following conditions: pouring a certain mass of sample into a platinum yellow crucible filled with anhydrous lithium tetraborate flux and internal standard reagent cobalt trioxide, uniformly stirring, adding release agent lithium bromide solution and lithium nitrate solution, placing the platinum yellow crucible into a melting furnace, setting the melting temperature to 1050 ℃ and the melting time to 16 minutes;
s3, setting the working conditions of a detection instrument: detection of TiO in ore by using melt fluorescence spectrometry 2 The content of the X-ray tube is set to be 50mA for working current and 50KV for voltage, and the optimal analysis line is selected to be K α And (5) scanning the strength of the standard sample and registering.
S4, drawing a working curve: the working curve is formed by correspondingly drawing the net strength of the titanium element analysis line in the selected standard sample and the standard content (%): in the working curve drawing process, determining one block as a standardized sample, setting measurement conditions, and automatically generating a working curve by adopting Simultix software; when the sample is analyzed, the intensity value of the sample to be tested is tested by using the X-ray fluorescence spectrometer, and the intensity value measured by the sample to be tested is converted into a standard content value through the established working curve of standard content and net intensity;
s5, expanding a standard working curve: in actual production of TiO in ores 2 The content is higher than the upper limit of the curve, in order to expand the linear range of the curve, expand the element detection range and improve the accurate area, and under the condition of lacking a standard sample, the method is adopted for processing as follows: the method is characterized in that high-content vanadium-titanium-iron ore is adopted, pure iron powder is added as a matrix, the addition amount of the pure iron is 0.1000 g-1300 g, the content of Fe is 60-68%, the sample weighing amount is 0.1000 g-0.2500 g, and TiO is changed by reducing the sample weighing amount of a vanadium-titanium-ore standard sample 2 According to the content of the pure iron and the sample weighing, repeating the steps S2 and S3, and using the obtained data for expanding a standard working curve.
S6, sample analysis: unknown TiO 2 The sample to be measured is processed according to the steps of S2 and S3, and TiO in the ore is obtained by using the standard working curve 2 The content is as follows.
Preferably, in the step S2, the volume ratio of the lithium bromide solution with the concentration of 400g/L to the lithium nitrate solution with the concentration of 300g/L is 2-5:5.
The beneficial effects of the invention are as follows: the invention provides a TiO in iron ore 2 The element fluorescence detection method comprises the working conditions of an instrument, the melting temperature, the reagent usage amount, the preparation of an analysis sample, the drawing of a standard working curve, the testing steps of a sample and the expansion method of the curve. The method provided by the invention is used for detecting TiO in ores 2 The elements have short period, less chemical drugs, little environmental pollution and guidance on steelmaking and ironmaking production. In addition, the invention provides a method for drawing a fluorescence working curve, which reduces the sample weighing amount of high-content standard samples, adds a pure iron matrix, prolongs the working curve range, ensures the content of unknown samples in the curve range and has accurate results.
Drawings
FIG. 1 is a graph of sample name and content for a work curve;
FIG. 2 is a graph of fit low content work curves;
FIG. 3 is a graph showing the working curve after expanding the detection range;
fig. 4 is a graph of the linear coefficients of the curve shown in fig. 3.
Detailed Description
The following non-limiting examples will enable those of ordinary skill in the art to more fully understand the invention and are not intended to limit the invention in any way.
The test methods described in the following examples, unless otherwise specified, are all conventional; the reagents and materials, unless otherwise specified, are commercially available.
Example 1
TiO in ore 2 The content of fluorescence detection elements comprises the following process steps:
s1, preparing a standard sample of a drawing working curve: selecting TiO 2 Iron ore samples with certain gradients of element content are needed; the purchase standard is TiO 2 The percentage is less than or equal to 0.40 percent, the content of selected standard samples in the standard sample library is within the range of 0.010 percent to 0.50 percent, and 10 standard samples above the national level of 0.01 iron ore/iron ore concentrate are selected.
S2, preparing a molten sample piece: the sample is subjected to melting treatment under the following conditions: pouring a certain mass of sample into a platinum yellow crucible filled with anhydrous lithium tetraborate flux and internal standard reagent cobalt trioxide, uniformly stirring, adding 2-5 drops of lithium bromide solution with the release agent concentration of 400g/L and 5 drops of lithium nitrate solution with the release agent concentration of 300g/L, placing the platinum yellow crucible into a melting furnace, setting the melting temperature to 1050 ℃ and the melting time to 16 minutes; the used flux is anhydrous lithium tetraborate, the release agent is lithium bromide and lithium nitrate solution, the internal standard reagent is cobaltosic oxide, and the ideal fuse piece is prepared, wherein the ratio of the cobaltosic oxide to the anhydrous lithium tetraborate is 1:10, and the fuse piece is mixed and melted, ground into fine powder, dried and stored for standby.
The specific operation is as follows: weighing 0.3500 g+/-0.0002 g of dried standard sample, placing the standard sample in one porcelain crucible, and weighing 5.000 g+/-0.0002 g of anhydrous lithium tetraborate in the other porcelain crucible; firstly pouring 1g of anhydrous lithium tetraborate into the bottom of a platinum yellow crucible, spreading, pouring 3g of anhydrous lithium tetraborate into the crucible containing a sample, uniformly mixing, pouring into the platinum yellow crucible, cleaning the crucible residual materials containing the sample by using the rest anhydrous lithium tetraborate, adding platinum Huang Ganguo, adding lithium nitrate and lithium bromide solution, and putting into a high-frequency melting furnace;
the melting mode is that the heating time is 60 seconds, and the heating temperature is 800 ℃; the secondary heating time is 120 seconds, the secondary heating temperature is 1050 ℃, the melting time is 240 seconds, the melting temperature is 1050 ℃, the self-cooling time is 120 seconds, the air cooling time is 120 seconds, and the swinging speed is 8 grades.
S3, setting the working conditions of a detection instrument: detection of TiO in ore by using melt fluorescence spectrometry 2 The content of the X-ray tube is set to be 50mA for working current and 50KV for voltage, and the optimal analysis line is selected to be K α And (5) scanning the strength of the standard sample and registering. The detection instrument is a Simultix14 type single-channel sequential scanning X-ray fluorescence spectrometer which takes an Rh target X-ray tube as an excitation source and a Simultix as analysis software.
S4, drawing a working curve: the working curve is formed by correspondingly drawing the net strength of the titanium element analysis line in the selected standard sample and the standard content (%): in the working curve drawing process, determining one block as a standardized sample, setting measurement conditions, and automatically generating a working curve by adopting Simultix software; when the sample is analyzed, the intensity value of the sample to be tested is tested by using the X-ray fluorescence spectrometer, and the intensity value measured by the sample to be tested is converted into a standard content value through the established working curve of standard content and net intensity;
s5, expanding a standard working curve: in actual production of TiO in ores 2 The content is higher than the upper limit of the curve, in order to expand the linear range of the curve, expand the element detection range and improve the accurate area, and under the condition of lacking a standard sample, the method is adopted for processing as follows: adding pure iron powder with the addition of 0.1000 g-0.1300 g into high-content vanadium ilmenite serving as a matrix to meet the requirement that the Fe content is 60% -68%, obtaining standard samples with different contents of 1.0% -3.0%, and using the obtained data for expanding a standard working curve; the weighing amount of the sample is between 0.1000g and 0.2500g, and the TiO is changed by reducing the weighing amount of the vanadium titanium ore standard sample 2 Repeating steps S2 and S3, and using the obtained data to develop a standard working curve. Obtain 4Standard samples with the following contents: 0.697%, 0.709%, 0.949% and 2.75%. The working curve was extended to 2.75%. And adjusting the demand point according to the content at any time.
S6, sample analysis: unknown TiO 2 The sample to be measured is processed according to the steps of S2 and S3, and TiO in the ore is obtained by using the standard working curve 2 The content is as follows.
Precision and accuracy test
And (3) testing by using a drawn working curve with a linear correlation coefficient R of more than 0.999 to obtain a result meeting the requirements of precision and accuracy.
Claims (7)
1. TiO in ore 2 The fluorescence detection method of the content comprises the following process steps:
s1, preparing a standard sample of a drawing working curve: selecting TiO 2 Iron ore samples with a certain gradient of element content;
s2, preparing a molten sample piece: the sample is subjected to melting treatment under the following conditions: pouring a certain mass of sample into a platinum yellow crucible filled with anhydrous lithium tetraborate flux and internal standard reagent cobalt trioxide, uniformly stirring, adding release agent lithium bromide solution and lithium nitrate solution, placing the platinum yellow crucible into a melting furnace, setting the melting temperature to 1050 ℃, and setting the melting time to 16 minutes;
s3, setting the working conditions of a detection instrument: detection of TiO in ore by using melt fluorescence spectrometry 2 The content of the X-ray tube is set to be 50mA for working current, 50KV for voltage and K for the optimal analysis line α Scanning the strength of a standard sample and registering;
s4, drawing a working curve: the working curve is formed by correspondingly drawing the net strength of the titanium element analysis line in the selected standard sample and the standard content (%): in the working curve drawing process, determining one block as a standardized sample, setting measurement conditions, and automatically generating a working curve by adopting Simultix software; during sample analysis, an X-ray fluorescence spectrometer is used for testing the intensity value of a sample to be tested, and the intensity value measured by the sample to be tested is converted into a standard content value through an established working curve of standard content and net intensity;
s5, sample analysis: unknown TiO 2 The sample to be measured is processed according to the steps of S2 and S3, and TiO in the ore is obtained by using the standard working curve 2 The content is as follows.
2. The method according to claim 1, characterized in that: in the step S1, the iron ore sample is TiO 2 Iron ore/iron concentrate national standard sample with the element content range of 0.10-0.50 percent.
3. The method according to claim 1, characterized in that: in the step S2, weighing 0.3500 g+/-0.0002 g of the dried sample, placing the sample in one porcelain crucible, and weighing 5.000 g+/-0.0002 g of anhydrous lithium tetraborate in the other porcelain crucible; firstly pouring 1g of anhydrous lithium tetraborate into the bottom of a platinum yellow crucible, spreading, pouring 3g of anhydrous lithium tetraborate into the crucible containing the sample, uniformly mixing, pouring into the platinum yellow crucible, cleaning the crucible residual material containing the sample by using the rest anhydrous lithium tetraborate, adding platinum Huang Ganguo, adding 5 drops of lithium nitrate solution with the concentration of 300g/L and 2-5 drops of lithium bromide solution with the concentration of 400g/L, and putting into a high-frequency melting furnace.
4. A method according to claim 1 or 3, characterized in that: in the step S2, the melting mode is that the heating time is 60 seconds, and the heating temperature is 800 ℃; the secondary heating time is 120 seconds, the secondary heating temperature is 1050 ℃, the melting time is 240 seconds, the melting temperature is 1050 ℃, the self-cooling time is 120 seconds, the air cooling time is 120 seconds, and the swinging speed is 8 grades.
5. The method according to claim 1, characterized in that: in the step S3, the detection instrument is a simux 14 type single-channel sequential scanning X-ray fluorescence spectrometer using an Rh target X-ray tube as an excitation source and a simux as analysis software.
6. The method according to claim 1, characterized in that: the method comprises the following process steps:
S1-S4, which are the same as steps S1-S4 of claim 1;
s5, expanding a standard working curve: in actual production of TiO in ores 2 The content is higher than the upper limit of the curve, in order to expand the linear range of the curve, expand the element detection range and improve the accurate area, and under the condition of lacking a standard sample, the method is adopted for processing as follows: the method adopts high-content vanadium-titanium-iron ore, and adds pure iron powder as a matrix, wherein the addition amount of the pure iron is 0.1000 g-0.1300 and g g, the Fe content is 60-68%, the sample weighing amount is 0.1000 g-0.2500 g, and the TiO is changed by reducing the sample weighing amount of the vanadium-titanium-ore standard sample 2 According to the content of the pure iron and the sample weighing, repeating the steps S2 and S3, and using the obtained data for expanding a standard working curve.
S6, sample analysis: unknown TiO 2 The sample to be measured is processed according to the steps of S2 and S3, and TiO in the ore is obtained by using the standard working curve 2 The content is as follows.
7. The method according to claim 1 or 6, characterized in that: in the step S2, the volume ratio of the lithium bromide solution with the concentration of 400g/L to the lithium nitrate solution with the concentration of 300g/L is 2-5:5.
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