CN114594116A - Method for measuring phase content in iron ore - Google Patents
Method for measuring phase content in iron ore Download PDFInfo
- Publication number
- CN114594116A CN114594116A CN202210250723.1A CN202210250723A CN114594116A CN 114594116 A CN114594116 A CN 114594116A CN 202210250723 A CN202210250723 A CN 202210250723A CN 114594116 A CN114594116 A CN 114594116A
- Authority
- CN
- China
- Prior art keywords
- phase
- sample
- content
- absorption coefficient
- iron ore
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
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
- G01N23/20—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 using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/207—Diffractometry using detectors, e.g. using a probe in a central position and one or more displaceable detectors in circumferential positions
-
- 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
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
-
- 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
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/05—Investigating materials by wave or particle radiation by diffraction, scatter or reflection
- G01N2223/056—Investigating materials by wave or particle radiation by diffraction, scatter or reflection diffraction
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/07—Investigating materials by wave or particle radiation secondary emission
- G01N2223/076—X-ray fluorescence
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/10—Different kinds of radiation or particles
- G01N2223/101—Different kinds of radiation or particles electromagnetic radiation
- G01N2223/1016—X-ray
-
- 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
Landscapes
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Biochemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Crystallography & Structural Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Plasma & Fusion (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
The invention provides a method for measuring the phase content in iron ore, belonging to the technical field of ore measuring methods and comprising the steps of 1, preparing a standard sample; step 2, performing element composition determination on the standard sample, and calculating the mass absorption coefficient of the standard sample; then measuring a phase spectrogram of the standard sample; taking the mass fraction of the phase to be measured as a horizontal coordinate, selecting the product of the net intensity of the spectral line and the mass absorption coefficient of the sample as a vertical coordinate to draw a working curve, and fitting a linear equation; step 3, calculating the mass absorption coefficient of the sample, determining a phase spectrogram of the sample, wherein the determination conditions are consistent with those of a standard sample, and then performing phase analysis on the spectrogram of the sample; the sample phase content is obtained. According to the method for determining the content of the phase in the iron ore, provided by the invention, the sample to be measured does not need to be added with a standard, the influence of the crystallinity of the sample is avoided, the qualitative analysis of all phases of the sample is not needed, and pure phase reagents of all phases to be measured do not need to be obtained.
Description
Technical Field
The invention belongs to the technical field of ore determination methods, and particularly relates to a method for determining phase content in iron ore.
Background
The phase is a phase having a specific physicochemical structure in a substance, and the same element may exist in different compound states in the substance. The accurate quantitative analysis of the iron mineral phase content plays an important role in the quality evaluation and application guidance of the iron ore. The natural environment has found that the variety of common iron-containing minerals is more than 170, but the variety of iron ores with industrial value is not many. When the iron ore value evaluation is carried out, the iron element content and the existence state and content of iron need to be concerned, and the work is established on the basis of phase quantitative analysis. The mineral separation and smelting processes of iron ores composed of different phases are different, and quantitative analysis of the phases can provide important basis for selection and optimization of a mineral separation scheme and a smelting process.
In practical application, the method is difficult to popularize and apply due to the fact that the external standard is not matched with the matrix of the sample to be detected, and the diffraction intensity and the content of each phase in the multi-phase mixture are not in direct proportion.
Disclosure of Invention
The invention aims to provide a method for measuring the phase content in iron ore, and aims to solve the technical problems of difficult matrix matching and narrow application range of an external standard method in the prior art.
In order to realize the purpose, the invention adopts the technical scheme that: the method for determining the content of phase in iron ore comprises the following steps:
step 1, preparing a standard sample;
step 2, performing element composition determination on the standard sample, and calculating the mass absorption coefficient of the standard sample, wherein the calculation formula is as follows:
step 3, calculating the mass absorption coefficient of the sample, determining a phase spectrogram of the sample, wherein the determination conditions are consistent with those of a standard sample, and then performing phase analysis on the spectrogram of the sample; the sample phase content is obtained.
Preferably, step 1 comprises the steps of: selecting reagents, wherein the reagents respectively comprise pure-phase substances of ferroferric oxide, ferric oxide and silicon dioxide; drying each reagent and grinding the reagent into powder; and then preparing a plurality of mixed samples from the components according to the mass ratio according to the phase content range of the iron ore sample to be detected, and preparing the plurality of mixed samples according to different gradient contents.
Preferably, step 1 comprises the steps of: selecting a reagent which is a ferroferric oxide pure-phase substance; selecting a plurality of real iron ore samples, preparing the real iron ore samples into powder samples, and roasting under the oxygen condition to oxidize iron oxide in the real iron ore samples into ferric oxide; then quantitatively mixing the reagents into the roasted iron ore sample, and uniformly mixing.
Preferably, the net intensity of the spectral lines in step 2 is selected to satisfy one or more of no spectral overlap, high peak intensity, and low angle.
Preferably, the calculating of the absorption coefficient of the sample in step 3 comprises the steps of: measuring the content of each element in the sample, and then calculating the mass absorption coefficient of the sample; the calculation formula is as follows:
Preferably, the sum of the parts by mass of each element in the step 3 is in a range of 95-100%.
Preferably, the phase analysis of the sample spectrogram in the step 3 comprises qualitative analysis and quantitative analysis.
Preferably, in the process of quantitative analysis of a sample spectrogram, the net intensity of a selected spectral line is calculated for a phase to be measured with an established curve, and the phase content is calculated by a working curve equation; for the object to be measured without establishing the curve, taking the object phase with known element content as a reference object phase, and calculating the content of the object phase by an RIR value method; the calculation formula is as follows:
Preferably, the determination of the phase spectrum of the standard sample in step 2 comprises the steps of: setting scanning conditions of an X-ray diffractometer, and performing spectrogram scanning on a sample; the scanning conditions were: the radiation source selects one of a copper target, a cobalt target, a chromium target and a molybdenum target; selecting 35-50 KV of light tube voltage; selecting the current of a light pipe to be 30-50 mA; the scanning range comprises 25-35 degrees; the scanning step length is not more than 0.5 degrees; the scanning time is not less than 2S.
Preferably, the number of standard samples in step 1 is at least 5.
The method for determining the phase content in the iron ore has the beneficial effects that: compared with the prior art, the method for determining the phase content in the iron ore expands the linear range and the application range by improving the sample matrix matching mode, correcting the mass absorption and applying the RIR value of the card. The method does not need to add a standard to the sample to be tested, is not influenced by the crystallinity of the sample, does not need to carry out qualitative analysis on all phases of the sample, and does not need to obtain pure-phase reagents of all phases to be tested.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed for the embodiments or the prior art descriptions will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 is a schematic diagram showing a fitting equation in a method for determining the content of phase in iron ore according to an embodiment of the present invention;
FIG. 2 is a schematic diagram showing another fitting equation in the method for determining the content of phase in iron ore according to the embodiment of the present invention;
FIG. 3 is a schematic diagram showing another fitting equation in the method for determining the content of the phase in the iron ore according to the embodiment of the present invention.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects of the present invention more clearly understood, the present invention is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The X-ray diffraction method (XRD method for short) phase quantitative analysis is a technique for measuring the content percentage of each phase in a sample by utilizing the positive correlation relationship between the intensity of the corresponding diffraction line in the diffraction spectrogram of the phase to be measured and the content of the phase to be measured of the multiphase mixed sample under the irradiation of single-wavelength X-rays. In the n-phase mixture, the direct relation between the diffraction intensity of a certain phase j and the corresponding mass fraction is expressed by the formula (1-1):
in which IjDiffraction intensity of j-th phase; wjMass fraction of j-th phase; cjConstants associated with the measurement instrument and the j-phase structure; rhojDensity of the j-th phase; mu.smThe mass absorption coefficient of the sample to be measured can be expressed by the formula
Wherein mumjThe mass absorption coefficient of the j phase.
Further, in the n-phase mixture, the direct relationship between the diffraction intensity of a certain phase j and the corresponding mass fraction can be expressed as (1-2)
As can be seen from the formula (1-2), the mass fraction of the j phase appears in both the numerator and denominator, indicating that the mass fraction of the phase j is not proportional to the diffraction intensity.
The external standard method has good traceability because a public external standard is used as a reference, is easy to carry out standardized operation, and is the most common method in various content tests. However, when the phase analysis is performed by using the X-ray diffraction external standard method, because of the influence of the mass absorption coefficient, it is impossible that the standard substance is required to be completely matched with the matrix of the sample to be tested in the multi-phase test, and the composition and the content of the standard substance are theoretically the same as those of the phase of the sample to be tested. The influence of the mass absorption coefficient results in a narrow applicability of the external standard method, which is applicable to samples consisting of only two phases or all isomers of the same elements, and such samples do not exist in natural minerals in fact.
However, the sample mass absorption coefficient μmRegardless of the phase state, only the types and the contents of the elements of the sample. Is expressed by formula as
Wherein, mumIs the mass absorption coefficient of the standard sample; eiIs the mass fraction of the element i in the standard sample; mu.smiThe mass absorption coefficient of element i to the diffraction light source; n is the number of elements of the measured standard sample.
Formula 1-1 can be varied to
Then for phase j, under fixed test conditions, the product I of the net intensity of the line and the absorption coefficient of the sample massj*μmMass fraction W of sum phasejLinear relation, slope of linear equation being
By measuring the absorption coefficient of the sample mass, a new external standard method can be established.
Referring to fig. 1 to 3 together, a method for determining the content of phase in iron ore according to the present invention will now be described. The method for determining the content of the phase in the iron ore comprises the following steps:
s1, preparing a standard sample;
step S1 may be implemented by:
protocol Single phase reagent preparation Standard sample
Firstly, selecting a single-phase reagent, wherein the crystallinity is not less than 95%, and the types of the reagents are pure-phase substances of ferroferric oxide, ferric oxide and silicon dioxide respectively.
And drying the reagents respectively, and grinding the reagents into powder. Specifically, the drying is carried out at 100-150 ℃, more specifically, the drying temperature is 105 ℃. All the powder passes through a standard sieve with 200 meshes. And then according to the phase content range of the iron ore sample to be detected, preparing the reagents into mixed samples with different gradient contents of ferroferric oxide, ferric oxide and silicon dioxide. And (5) carrying out uniformity inspection on the uniformly mixed sample.
Scheme two-purpose mixture preparation of sample of real iron ore and single-phase reagent ferroferric oxide
Selecting a reagent which is a ferroferric oxide pure-phase substance; selecting a plurality of kinds of real iron ore samples, preparing the plurality of kinds of real iron ore samples into powder samples, and then roasting the powder samples under the oxygen condition (the temperature is 800-1200 ℃, such as 1000 ℃), so that iron oxide (such as ferroferric oxide) in the real iron ore samples is oxidized into ferric oxide; then quantitatively mixing the reagents (1% -99%) into the roasted iron ore sample, and uniformly mixing. In the scheme, the sample and the reagent are dried at 105 ℃ before being mixed uniformly, and are ground until the sample passes through a 200-mesh standard sieve. The uniformity of the uniformly mixed sample needs to be checked. And taking a sample of the iron ore which is burned at high temperature as a substrate, and adding a single-phase high-purity ferroferric oxide reagent. The prepared standard substance can maintain the main characteristics of the sample matrix and reduce the influence of matrix effect during sample test.
Preparation of standard samples the first (A) and/or the second (B) of the scheme are selected, and the number of the preparation gradient standard samples is not less than 5. And (4) the laboratory with a single variety of the test sample is preferred to be the second scheme.
S2, performing element composition measurement on the standard sample by adopting an X-ray fluorescence spectrometry (or a plasma emission spectrometry), and calculating the mass absorption coefficient of the standard sample, wherein the calculation formula is as follows:
then measuring a phase spectrogram of the standard sample; the determination of the phase spectrogram comprises the following steps: setting scanning conditions of an X-ray diffractometer, and performing spectrogram scanning on the sample. The scanning conditions were: the radiation source should be selected from copper target, cobalt target, chromium target or molybdenum target; selecting 35-50 KV of light tube voltage; selecting the current of the light pipe to be 30-50 mA; the scanning range at least comprises 25-35 degrees, the scanning step is not more than 0.5 degree, and the scanning time is not less than 2S.
Taking the mass fraction of the phase to be measured as an abscissa, selecting the product of the net intensity of a spectral line and the mass absorption coefficient of the sample as an ordinate to draw a working curve, and fitting a linear equation in the form of Y (aX + b); y represents the product of the net intensity of the spectral line of the phase to be measured and the mass absorption coefficient, X represents the mass fraction of the phase to be measured, a is the slope of the regression equation, and b is the intercept of the regression equation.
The net intensity refers to the integrated intensity after overlap and background subtraction. A phase to be measured generally has a plurality of lines that can be selected. The net intensity of the spectral lines is selected in step S2 to satisfy one or more of no spectral line overlap, high peak intensity, and low angle. Preferentially selecting spectral lines with high spectral peak intensity and low angular spectral lines without spectral line overlapping.
S3, calculating the mass absorption coefficient of the sample, determining a phase spectrogram of the sample, wherein the determination conditions are consistent with those of a standard sample, and then performing phase analysis on the spectrogram of the sample; the sample phase content is obtained.
Step S3 may be implemented by:
measuring the content of each element in the sample, and calculating the mass absorption coefficient of the sample according to the content of each element and the mass absorption coefficient; the calculation formula is as follows:
The sum of the mass parts of the elements is 95-100%.
The phase analysis of the sample spectrogram comprises qualitative analysis and quantitative analysis, wherein the qualitative analysis is to analyze the type of phase composition contained in the sample, and the main composition of the sample is usually magnetite Fe3O4Hematite Fe2O3Quartz SiO2Goethite FeOOH, pyrite FeS2Iron olivine Fe2SiO4Phase of equivalentOne or more combinations of (a). The quantitative analysis is the analysis of the content of the phase.
In the quantitative analysis process of a sample spectrogram, the net intensity of a selected spectral line is calculated for a phase to be measured with an established curve, and the phase content is calculated by a working curve equation;
the net intensity calculation method comprises the following steps: the net intensity is the integrated intensity of the spectral peaks minus the background intensity.
And (3) for the phase to be measured without establishing the curve, taking the phase with the known content as a reference phase (in the process of quantitative analysis of the sample spectrogram, calculating the net intensity of the selected spectral line for the phase to be measured with the established curve), and calculating the content of the phase of the sample by an RIR value method. The calculation formula is as follows:
Compared with the prior art, the method for measuring the phase content in the iron ore expands the linear range and the application range by improving the sample matrix matching mode, correcting the mass absorption and applying the RIR value of the card. The method does not need to add a standard to the sample to be tested, is not influenced by the crystallinity of the sample, does not need to carry out qualitative analysis on all phases of the sample, and does not need to obtain pure-phase reagents of all phases to be tested.
Example one
1.1 Instrument and test conditions
X-ray diffractometer PANALYtic Empyrean, diffraction source Cu Ka, tube pressure 45kV, tube flow 40mA, goniometer radius 240 mm. The glass plate was sampled and filled to a depth of 0.5 mm. Step scanning mode, step 0.0131 degree, point scanning time 43.10s, 2 theta angle range 10-80 degree, PHD 45-70%. All reagents used for preparing the standard sample are guaranteed reagent, and an electronic balance with the sensing quantity of 0.000lg is adopted. All tests were measured by two parallel slides.
1.2 Standard substance and sample
Grinding the raw materials until all the raw materials pass through a standard sieve of 200 meshes, and drying the raw materials for 1 hour at 105 ℃ in a muffle furnace for later use.
1.3 Standard sample
1.4 working curve
1.5 sample testing
The method for determining the phase content in the iron ore can provide a standard sample with high matching degree of a matrix, has high accuracy and repeatability of a test result, and is convenient for comparison and verification among laboratories. The method has wide adaptability and can be used for various types of iron ore samples. The method has the advantages of easy evaluation and verification of adaptability and accuracy, suitability for developing standardized detection and convenience for popularization and application.
Example two:
external standard method: the brilliant blue adopts an X-ray diffraction-external standard method to carry out phase quantitative analysis on the powder mixture of the zinc oxide and the yttrium oxide, and the application of the external standard method in the test of the two-phase mixture is verified. Wujianpeng establishes X-ray diffraction-external standard method phase quantitative standard curves for 9 components such as quartz, corundum and the like commonly used in inorganic non-metallic materials, and each curve is established based on a two-phase gradient mixture. The external standard method is influenced by the mass absorption coefficient, and the standard substance required in the multiphase test needs to be completely matched with the matrix of the sample to be tested, so that the composition and the content of the standard substance are theoretically the same as those of the phase of the sample to be tested, which is impossible. The influence of the mass absorption coefficient results in a narrow applicability of the external standard method, which is applicable to samples consisting of only two phases or all isomers of the same elements, and such samples do not exist in natural minerals in fact.
Example three:
full spectrum fitting method: ever civil X-ray diffraction-Rietveld full-spectrum fitting method for analyzing Fe in iron ore2O3，FeOOH，SiO2，A12(Si2O5)(0H)4The total composition of 4 mineral phases, their content was 86.20%, 9.59%, 3.58%, 0.64%, respectively. The full spectrum fitting method is a method for obtaining the content of each phase when a theoretical spectrogram is corrected by adjusting experimental parameters, peak shape parameters and the like according to the structural data of each phase and the theoretical spectrogram and an actually measured spectrogram are matched to the maximum extent. The full-spectrum fitting method belongs to a semi-quantitative method essentially, and is a theoretical presumption value, all phases in a sample need to be accurately and qualitatively analyzed, which is difficult to realize in a real mineral sample, the composition of natural minerals is very complex, and diffraction peaks of low-content phases are too small to be qualitatively detected. The result of the full-spectrum fitting method is calculated according to the phase structure data theory, and the accuracy of the calculation result is difficult to evaluate and verify due to the difference between the actual structure data and the theoretical structure data of the actual sample caused by the ore-forming temperature, the solid solution and the like; the detection results of different laboratories are difficult to trace and compare, and the method is not suitable for standardized popularization and application.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (10)
1. A method for determining the content of phases in iron ore, characterized by comprising the following steps:
step 1, preparing a standard sample;
step 2, performing element composition determination on the standard sample, and calculating the mass absorption coefficient of the standard sample, wherein the calculation formula is as follows:
step 3, calculating the mass absorption coefficient of the sample, determining a phase spectrogram of the sample, wherein the determination conditions are consistent with those of a standard sample, and then performing phase analysis on the spectrogram of the sample; the sample phase content is obtained.
2. The method of claim 1, wherein step 1 comprises the steps of: selecting reagents which are pure-phase substances of ferroferric oxide, ferric oxide and silicon dioxide respectively; drying each reagent and grinding the reagent into powder; and then preparing a plurality of mixed samples from the components according to the mass ratio according to the phase content range of the iron ore sample to be detected, and preparing the plurality of mixed samples according to different gradient contents.
3. The method of claim 1, wherein step 1 comprises the steps of: selecting a reagent which is a ferroferric oxide pure-phase substance; selecting a plurality of real iron ore samples, preparing the plurality of real iron ore samples into powder samples, and roasting in an oxygen atmosphere to oxidize iron oxide in the real iron ore samples into ferric oxide; then quantitatively mixing the reagents into the roasted iron ore sample, and uniformly mixing.
4. A method according to any one of claims 1 to 3, wherein the method comprises the steps of: the net intensity of the spectral lines in step 2 is selected to satisfy one or more of no spectral line overlap, high peak intensity, and low angle.
5. The method of claim 4, wherein the step of calculating the absorption coefficient of the sample in step 3 comprises the steps of: measuring the content of each element in the sample, and then calculating the mass absorption coefficient of the sample; the calculation formula is as follows:
6. The method for determining the content of phase in iron ore according to claim 5, wherein the sum of the mass fractions of the elements in step 3 is in the range of 95% to 100%.
7. The method of claim 5, wherein the step 3 of performing phase analysis on the sample spectrum comprises qualitative analysis and quantitative analysis.
8. The method of claim 7A method for determining the content of a phase in iron ore is characterized in that in the process of quantitative analysis of a sample spectrogram, the net intensity of a selected spectral line is calculated for the phase to be measured with an established curve, and the phase content is calculated by a working curve equation; for a phase to be measured without establishing a curve, taking the phase with known content as a reference phase, and calculating the content of the sample phase by an RIR value method; the calculation formula is as follows:
wherein WjThe mass fraction of the phase j to be calculated is; RIRjRIR value for phase j; i ishjThe peak height value of the strongest peak of the phase j; waThe mass fraction of the known phase a is obtained; RIRaRIR value for phase a; i ishaThe peak height of the strongest peak of phase a.
9. The method of claim 1, wherein the determination of the phase spectrum of the standard sample in step 2 comprises the steps of: setting scanning conditions of an X-ray diffractometer, and performing spectrogram scanning on a sample; the scanning conditions were: the radiation source selects one of a copper target, a cobalt target, a chromium target and a molybdenum target; selecting 35-50 KV of light tube voltage; selecting the current of the light pipe to be 30-50 mA; the scanning range comprises 25-35 degrees; the scanning step length is not more than 0.5 degrees; the scanning time is not less than 2S.
10. The method of determining the content of phase in iron ore according to claim 1, wherein the number of standard samples in step 1 is at least 5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210250723.1A CN114594116B (en) | 2022-03-15 | 2022-03-15 | Method for measuring phase content in iron ore |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210250723.1A CN114594116B (en) | 2022-03-15 | 2022-03-15 | Method for measuring phase content in iron ore |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114594116A true CN114594116A (en) | 2022-06-07 |
| CN114594116B CN114594116B (en) | 2023-06-16 |
Family
ID=81808523
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210250723.1A Active CN114594116B (en) | 2022-03-15 | 2022-03-15 | Method for measuring phase content in iron ore |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114594116B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115629091A (en) * | 2022-10-14 | 2023-01-20 | 江苏省沙钢钢铁研究院有限公司 | Method for measuring phase reference strength |
| CN116559210A (en) * | 2023-03-21 | 2023-08-08 | 南京海关工业产品检测中心 | Mineral product phase detection method and system |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006257477A (en) * | 2005-03-16 | 2006-09-28 | Nippon Steel Corp | METHOD FOR MEASURING QUANTITY OF gamma-Fe2O3 IN IRON ORE |
| CN102636509A (en) * | 2012-04-20 | 2012-08-15 | 中华人民共和国北仑出入境检验检疫局 | Method for analyzing ferrous iron in iron ore based on X fluorescence spectrum |
| CN106053503A (en) * | 2016-08-09 | 2016-10-26 | 重庆大学 | Iron ore sintering method and quantitative characterization method of mineral phase contents |
| CN106053500A (en) * | 2016-05-18 | 2016-10-26 | 北方奥钛纳米技术有限公司 | Method for detecting phase purity of lithium titanate composition |
| CN110927195A (en) * | 2018-09-19 | 2020-03-27 | 核工业北京地质研究院 | Quantitative analysis method for trace phase |
-
2022
- 2022-03-15 CN CN202210250723.1A patent/CN114594116B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006257477A (en) * | 2005-03-16 | 2006-09-28 | Nippon Steel Corp | METHOD FOR MEASURING QUANTITY OF gamma-Fe2O3 IN IRON ORE |
| CN102636509A (en) * | 2012-04-20 | 2012-08-15 | 中华人民共和国北仑出入境检验检疫局 | Method for analyzing ferrous iron in iron ore based on X fluorescence spectrum |
| CN106053500A (en) * | 2016-05-18 | 2016-10-26 | 北方奥钛纳米技术有限公司 | Method for detecting phase purity of lithium titanate composition |
| CN106053503A (en) * | 2016-08-09 | 2016-10-26 | 重庆大学 | Iron ore sintering method and quantitative characterization method of mineral phase contents |
| CN110927195A (en) * | 2018-09-19 | 2020-03-27 | 核工业北京地质研究院 | Quantitative analysis method for trace phase |
Non-Patent Citations (4)
| Title |
|---|
| MUSHTAGATTE MANJUNATHA 等: "XRD, internal field-NMR and Mössbauer spectroscopy study of composition, structure and magnetic properties of iron oxide phases in iron ores", 《JOURNAL OF MATERIALS RESEARCH AND TECHNOLOGY》, vol. 8, no. 2, pages 2192 - 2200 * |
| 卞欣: "X射线衍射仪在氧化铁皮物相分析中的应用", vol. 41, no. 6, pages 12 - 15 * |
| 赵伟 等: "X射线衍射法快速测定矿产品中的主要物相和主元素含量", vol. 51, no. 4, pages 523 - 527 * |
| 辛艳青 等: "基于X射线衍射物相定量分析外标法的研究", vol. 5, no. 34, pages 48 - 101 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115629091A (en) * | 2022-10-14 | 2023-01-20 | 江苏省沙钢钢铁研究院有限公司 | Method for measuring phase reference strength |
| CN115629091B (en) * | 2022-10-14 | 2024-06-11 | 江苏省沙钢钢铁研究院有限公司 | Method for measuring phase reference intensity |
| CN116559210A (en) * | 2023-03-21 | 2023-08-08 | 南京海关工业产品检测中心 | Mineral product phase detection method and system |
| CN116559210B (en) * | 2023-03-21 | 2024-04-30 | 南京海关工业产品检测中心 | Mineral product phase detection method and system |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114594116B (en) | 2023-06-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN114594116B (en) | Method for measuring phase content in iron ore | |
| 木村純一 et al. | Evaluation of major and trace element XRF analyses using a flux to sample ratio of two to one glass beads. | |
| Stosnach | Environmental trace-element analysis using a benchtop total reflection X-ray fluorescence spectrometer | |
| CN103364426A (en) | Method for determining content of zinc in zinc concentrate through energy-dispersive X-ray fluorescence spectrometry | |
| CN110161067A (en) | A kind of concentrate tenor measuring method based on Portable X RF | |
| CN106841263A (en) | A kind of Electron probe quantitative analysis method for determining F contents in natural minerals | |
| Harouaka et al. | A novel method for measuring ultra-trace levels of U and Th in Au, Pt, Ir, and W matrices using ICP-QQQ-MS employing an O 2 reaction gas | |
| CN113607611A (en) | Coupling evaluation method for mixing uniformity of powder material | |
| CN102967614A (en) | Analysis method for determining total iron content in iron ore by using X-ray fluorescence spectrum fusion method | |
| CN112378939A (en) | Method for determining age of Tiuranium ore by using electronic probe chemical analysis | |
| CN103278488B (en) | A kind of method of rapid semi-quantitative GH4169 alloy trace element | |
| Oreščanin et al. | Applicability of MiniPal 4 compact EDXRF spectrometer for soil and sediment analysis | |
| CN106324004A (en) | Industrial strontium carbonate chemical component content detection method | |
| CN105486707A (en) | Quantitative fluorescence analysis method for cobalt-based alloy | |
| CN116223768A (en) | Method for rapidly determining rock type rubidium ore grade in field | |
| CN106979930B (en) | A kind of method of free iron content in quantitative analysis Soil/Sediment Samples | |
| CN115639188A (en) | Method for measuring contents of calcium oxide, magnesium oxide and silicon dioxide in high-silicon composite flux by inductively coupled plasma emission spectrometer | |
| CN108037148A (en) | The development of x-ray fluorescence spectrometry Copper making clinker multielement standard sample | |
| RU2240543C2 (en) | Method for x-ray fluorescent analysis of elemental composition of substance | |
| Belozerova et al. | Investigation of synthesized Be-bearing silicate glass as laboratory reference sample at X-ray electron probe microanalysis of silicates | |
| Pashkova et al. | A Workflow for Uncertainty Assessment in Elemental Analysis of Archaeological Ceramics | |
| CN112924485B (en) | Method for measuring spinel Fe by electronic probe secondary standard sample correction method3+Method for producing Fe/∑ Fe | |
| CN108195861A (en) | A kind of method of iron content in rapid semi-quantitative detection blind sample of fireworks and firecrackers pyrotechnic composition | |
| CN107991334A (en) | A kind of method of aluminium content in rapid semi-quantitative detection blind sample of fireworks and firecrackers pyrotechnic composition | |
| Margolin et al. | Some experience in using the MECA‐10‐44 (XR‐500) x‐ray fluorescence analyser for solving geological problems |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |