CN105651801B - Online analysis method for ore pulp minerals - Google Patents
Online analysis method for ore pulp minerals Download PDFInfo
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- CN105651801B CN105651801B CN201511022579.2A CN201511022579A CN105651801B CN 105651801 B CN105651801 B CN 105651801B CN 201511022579 A CN201511022579 A CN 201511022579A CN 105651801 B CN105651801 B CN 105651801B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/223—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—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
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Abstract
The invention discloses an ore pulp mineral online analysis method, which comprises the following steps: irradiating the ore pulp to be analyzed by using X rays emitted by an X-ray tube, and respectively arranging a detector at two sides of the ore pulp to perform X-ray fluorescence detection and diffraction detection; carrying out quantitative analysis on mineral components in the ore pulp according to an X-ray fluorescence detection result and a qualitative standard diffraction library; the quantitative analysis result of the mineral components is combined with the diffraction detection result, and the diffraction peak of the water is analyzed to establish a correction equation of the diffraction peak and the concentration, so that the online analysis of the ore pulp is finally realized. By adopting the method disclosed by the invention, the online analysis of mineral components in the ore pulp can be realized, and the mineral component information is provided for the flotation and beneficiation process in real time. Meanwhile, the problems of the traditional technologies such as ore pulp on-line analysis and field calibration are solved, and the method is beneficial to popularization and application.
Description
Technical field
The present invention relates to pulp-assay technical field more particularly to a kind of ore pulp mineral on-line analysis.
Background technology
Ore dressing is to be divided mineral and gangue using different technique according to the physics of different minerals, chemical property in ore
The process opened.
At present, both at home and abroad widely used current-carrying X-fluorescence ore grade analyzer realize metallic element during floatation process
Line detects, and carries out Instructing manufacture and process control；Few part mine carries out offline mineral constituent analysis in laboratory.Due to member
The case where cellulose content is simultaneously not equal to mineral content, multi mineral symbiosis containing same element generally existing, laboratory mineral
It is component analysis poor in timeliness, of high cost, it is not used to produce real-time monitoring.
Invention content
The object of the present invention is to provide a kind of ore pulp mineral on-line analysis, may be implemented ore pulp Mineralss
Line analysis provides mineral constituent information in real time for flotation beneficiation technique.
The purpose of the present invention is what is be achieved through the following technical solutions：
A kind of ore pulp mineral on-line analysis, which is characterized in that including：
The x-ray bombardment projected using X-ray tube is respectively set one for X to ore pulp to be analyzed, and in the both sides of ore pulp
Ray fluorescence detects the detector with diffracted probe；
The content that each metallic element is calculated according to x-ray fluorescence result of detection completes the quantitative analysis of metallic element；Root
The characteristic value obtained according to diffracted probe result confirms mineral species with qualitative criteria's diffraction picture library, completes qualitative point of mineral constituent
Analysis, and diffracted probe result is combined to calculate mineral constituent ratio；Quantitative analysis in conjunction with metallic element and mineral constituent ratio,
Mineral constituent content is calculated, the quantification and qualification of ore pulp Mineralss is completed.
Further, a detector packet for x-ray fluorescence detection and diffracted probe is respectively set in the both sides of ore pulp
It includes：
It using X-ray Low Energy Region as the excitaton source of ore pulp x-ray fluorescence, is excited and is detected using reflection mode, visited
Survey device is SDD type detectors；
Using X-ray high energy region as the excitaton source of ore pulp X-ray diffraction ray, is excited and visited using transmission mode
It surveys, detector is CdTe type detectors；
The SDD types detector is respectively arranged at the both sides of ore pulp with CdTe type detectors.
Further, this method further includes：Mineral constituent quantitative analysis results are combined with diffracted probe result, are passed through
The diffraction maximum of moisture is analyzed, establish fluorescence spectrum, moisture diffraction maximum and metal element content correction equation, to most
The on-line analysis of ore pulp is realized eventually.
As seen from the above technical solution provided by the invention, in conjunction with x-ray fluorescence analysis technology (XRF) and energy color
X-ray diffraction analysis technology (EDXRD) is dissipated, realizes the on-line analysis of ore pulp Mineralss, is carried in real time for flotation beneficiation technique
For mineral constituent information；Meanwhile the traditional technologies problems faced such as also solve ore pulp on-line analysis, field calibration, be conducive to
It promotes and applies.
Description of the drawings
In order to illustrate the technical solution of the embodiments of the present invention more clearly, required use in being described below to embodiment
Attached drawing be briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for this
For the those of ordinary skill in field, without creative efforts, other are can also be obtained according to these attached drawings
Attached drawing.
Fig. 1 is energy dispersion type X-ray diffraction analysis instrument structural schematic diagram provided in an embodiment of the present invention；
Fig. 2 is the system structure diagram provided in an embodiment of the present invention for ore pulp mineral on-line analysis；
Fig. 3 is the working curve schematic diagram of CdTe types detector provided in an embodiment of the present invention；
Fig. 4 is the working curve schematic diagram of SDD types detector provided in an embodiment of the present invention；
Fig. 5 provides the flow chart that ore pulp Mineralss are carried out with quantification and qualification for the embodiment of the present invention.
Specific implementation mode
With reference to the attached drawing in the embodiment of the present invention, technical solution in the embodiment of the present invention carries out clear, complete
Ground describes, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on this
The embodiment of invention, every other implementation obtained by those of ordinary skill in the art without making creative efforts
Example, belongs to protection scope of the present invention.
The embodiment of the present invention provides a kind of ore pulp mineral on-line analysis, and this method is by x-ray fluorescence analysis technology
(XRF) it is combined with energy dispersion X-ray diffraction analysis technology (EDXRD).
Energy dispersion type X-ray diffraction analysis instrument structural schematic diagram in x-ray bombardment to substance as shown in Figure 1, occur to dissipate
It penetrates, wherein diffraction phenomena is generation when X-ray is scattered by crystalline solid, is a kind of phenomenon specific to crystalline solid.Crystal can
The direction that diffraction can be generated is decided by that crystal surrounds and watches the type (structure cell type) and its basic size (interplanar distance, structure cell of structure
Parameter etc.), diffracted intensity is decided by crystal structure the type of each component and its arranged evenly, therefore diffraction analysis technology
It is the effective means for carrying out analyzing crystal object phase.Mineral are also a kind of crystal, and it is fixed can to carry out mineral using diffraction analysis technology
Property, quantitative analysis；The no accurate bulky angular instrument of energy dispersion type X-ray diffractometer, it is low to sample preparation requirement, it is applicable to mine
Starch on-line measurement.
Energy dispersion type X-ray diffraction analysis instrument is using continuous x ray as incident ray, and the angle of diffraction is fixed, in diffraction side
X-ray detector detection of diffracted ray is used upwards.Diffraction ray meets Bragg's equation：
N λ=2dsin θ
Wherein, λ is wavelength, and d is the spacing of lattice of crystal, and θ is the angle of diffraction, should under the conditions of energy dispersion diffraction analysis
Formula can be rewritten as：
Wherein, E is the energy of diffraction ray, and h is Planck's constant, and c is the light velocity.
When the energy value for measuring diffraction ray from a fixed diffraction angle direction, be can with counting lattice spacing, into
And carry out the material phase analysis of mineral crystal.
In the embodiment of the present invention, the structure for ore pulp mineral on-line analysis is as shown in Fig. 2, include mainly：X-ray tube, height
Voltage source, diffraction ray detector, fluorescent x ray detector and optical path component.
With this configuration carry out ore pulp mineral on-line analysis the step of be：
Step 1: being respectively set to ore pulp to be analyzed, and in the both sides of ore pulp using the x-ray bombardment that X-ray tube projects
One detector for x-ray fluorescence detection and diffracted probe.
In the embodiment of the present invention, using the X-ray Low Energy Region of X-ray tube as the excitaton source of ore pulp x-ray fluorescence, using reflection
Mode is excited and is detected, and detector is SDD type detectors；
Using the X-ray high energy region of X-ray tube as the excitaton source of ore pulp X-ray diffraction ray, swashed using transmission mode
Hair and detection, detector are CdTe type detectors；
In the embodiment of the present invention, high energy region and Low Energy Region can be distinguished according to the size of ray energy and preset value；Example
Such as, high energy region is the ray of ＞ 30keV, and Low Energy Region is the ray of ＜ 30keV, but there is no stringent boundaries.Common elements quilt
The characteristic ray ejected, common analytical energy section is Low Energy Region, usually above-mentioned value, and the part beyond the value is tested
Object diffraction is measured, diffraction ray is formed.
The SDD types detector is respectively arranged at the both sides of ore pulp with CdTe type detectors, can reduce fluorescence and diffraction
Between interfere with each other.
The working curve of CdTe type detectors is as shown in figure 3, the working curve of SDD type detectors is as shown in Figure 4.
In the embodiment of the present invention, pass through the X-fluorescence result of detection and diffracted probe knot of the mineral that above-mentioned detection process obtains
Fruit；Meanwhile the present embodiment also detects the water in ore pulp using CdTe, obtains corresponding diffracted probe as a result, it is specific
Purposes sees below text.
Step 2: according to x-ray fluorescence result of detection, diffracted probe result and qualitative criteria's diffraction picture library to ore pulp chats
Object component carries out quantification and qualification.
As shown in figure 5, according to x-ray fluorescence result of detection, and use x-ray fluorescence analysis technology and empirical coefficient method meter
The content for calculating each metallic element completes the quantitative analysis of metallic element；It (is obtained according to diffracted probe result) according to characteristic value
Confirm mineral species with standard diffraction picture library, completes mineral constituent qualitative analysis, and diffracted probe result is combined to calculate mineral group
Divide ratio；Quantitative analysis in conjunction with metallic element and mineral constituent ratio calculate mineral constituent content.Specifically：
1. measuring one group of mineral samplers (being more than 30), the tenor in mineral samplers has certain variation range, surveys
The fluorescence spectrum of mineral metal element, the synchronous difraction spectrum for reading mineral, the tested mine of division during measurement are read during measuring
Sample；
2. it is higher than the reduced sample that the apparatus measures step 1 of in-line analyzer obtains with chemical analysis method or precision,
Obtain concentration value and tenor value；
3. establishing model using multiple linear regression analysis, that is, establish sample metal content and photoluminescence spectrum intensity, moisture
The mathematical relationship equation of difraction spectrum intensity (being obtained using CdTe detections)；
4. above-mentioned is modeling process, another 1 on condition that standard diffraction picture library has been off foundation (process of foundation sees below text)；
5. mineral samplers are measured, it is synchronous to read difraction spectrum, characteristic value is read, it is synchronous to read fluorescence spectrum and moisture diffraction
Spectral intensity；
6. according to fluorescence spectrum and model, each metal element content is calculated；
7. characteristic value is matched with picture library, mineral species are confirmed, complete mineral qualitative analysis；
8. according to the ratio of different minerals diffraction spectral intensity, mineral constituent ratio is calculated；
9. according to metal element content and mineral constituent ratio, mineral constituent content is calculated；
Standard diffraction picture library establishes process：
Normative mineral 1 measures diffracting spectrum；
Diffracting spectrum is subjected to peak-seeking processing, the peak position of characteristic peak is obtained, as the 1st group of characteristic value；
According to peak position, the peak width of characteristic peak is calculated, as the 2nd group of characteristic value；
It calculates peak-to-peak away from as the 3rd group of characteristic value；
Three groups of characteristic values of normative mineral 1 are put in storage.
By the above process as can be seen that the scheme of the embodiment of the present invention need not demarcate " mineral constituent ", mineral group
Point calibration process is the component chemical examination that the division sample that will be taken in measurement process carries out mineral compound, is to establish mineral constituent content
The premise of model.But this procedure technical difficulty is big, of high cost, the inspection unit in most of country mine does not have
The ability.Fluorescence and diffraction are combined in the embodiment of the present invention, diffracted probe result is qualitative analysis mineral, calculates mineral
Between relative scale, calculate the total tenor of certain mineral with fluorescent method, further according to relative scale calculate mineral it is true
Real content, and the chemical examination difficulty of metal is small, at low cost and mine inspectionization unit routine work.Mineral are carried out using the technology
Component is monitored on-line, and increasing only a part of normal metal in the modelling phase chemically examines workload, and online metal content analysis
The staking-out work of instrument is the same.
In addition, the ore pulp is a kind of suspension, the content size of moisture is to x-ray fluorescence intensity and X-ray diffraction
Intensity has a great impact, and to realize that liquid mine pulp measures analysis, then needs the correction for realizing water.
In the embodiment of the present invention, mineral constituent quantitative analysis results are combined with diffracted probe result, by moisture
Diffraction maximum analyzed, establish fluorescence spectrum, moisture diffraction maximum and metal element content correction equation, to finally realizing
The on-line analysis of liquid mine pulp.
The said program combination x-ray fluorescence analysis technology (XRF) and energy dispersion X-ray diffraction of the embodiment of the present invention point
Analysis technology (EDXRD) realizes the on-line analysis of ore pulp Mineralss, and mineral constituent letter is provided in real time for flotation beneficiation technique
Breath；Meanwhile the traditional technologies problems faced such as also solve ore pulp on-line analysis, field calibration, be conducive to promote and apply.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Any one skilled in the art is in the technical scope of present disclosure, the change or replacement that can be readily occurred in,
It should be covered by the protection scope of the present invention.Therefore, protection scope of the present invention should be with the protection model of claims
Subject to enclosing.
Claims (3)
1. a kind of ore pulp mineral on-line analysis, which is characterized in that including：
The x-ray bombardment projected using X-ray tube is respectively set one for X-ray to ore pulp to be analyzed, and in the both sides of ore pulp
The detector of fluorescence detection and diffracted probe；
The content that each metallic element is calculated according to x-ray fluorescence result of detection completes the quantitative analysis of metallic element；According to spreading out
The characteristic value and qualitative criteria's diffraction picture library for penetrating result of detection acquisition confirm mineral species, complete mineral constituent qualitative analysis, and
Mineral constituent ratio is calculated in conjunction with diffracted probe result；Quantitative analysis in conjunction with metallic element and mineral constituent ratio calculate
Mineral constituent content completes the quantification and qualification of ore pulp Mineralss；Its process is as follows：
One group of mineral samplers is measured, the tenor in mineral samplers has certain variation range, mineral are read in measurement process
The fluorescence spectrum of metallic element, the synchronous difraction spectrum for reading mineral, the tested sample ore of division during measurement；Use chemical analysis method
Or precision obtains concentration value and tenor value higher than the reduced sample that the apparatus measures of in-line analyzer obtain；Using more
Model is established in first linear regression analysis, that is, establishes sample metal content and photoluminescence spectrum intensity, the number of moisture difraction spectrum intensity
Learn relation equation；Measurement mineral samplers, it is synchronous to read difraction spectrum, characteristic value is read, synchronous reading fluorescence spectrum and moisture spread out
Penetrate spectral intensity；According to fluorescence spectrum and model, each metal element content is calculated；Characteristic value and the progress of standard diffraction picture library
Match, confirm mineral species, completes mineral qualitative analysis；According to the ratio of different minerals diffraction spectral intensity, mineral constituent ratio is calculated；
According to metal element content and mineral constituent ratio, mineral constituent content is calculated.
2. according to the method described in claim 1, it is characterized in that, being respectively set one for x-ray fluorescence in the both sides of ore pulp
It detects and includes with the detector of diffracted probe：
Using X-ray Low Energy Region as the excitaton source of ore pulp x-ray fluorescence, is excited and detected using reflection mode, detector
For SDD type detectors；
It using X-ray high energy region as the excitaton source of ore pulp X-ray diffraction ray, is excited and is detected using transmission mode, visited
Survey device is CdTe type detectors；
The SDD types detector is respectively arranged at the both sides of ore pulp with CdTe type detectors.
3. according to the method described in claim 1, it is characterized in that, this method further includes：By mineral constituent quantitative analysis results
It is combined with diffracted probe result, is analyzed by the diffraction maximum to moisture, establish fluorescence spectrum, moisture diffraction maximum and metal
The correction equation of constituent content, to finally realize the on-line analysis of ore pulp.
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| CN107228871B (en) * | 2017-07-21 | 2023-07-04 | 中国地质大学（武汉） | Portable X-ray analysis device |
| CN109117759A (en) * | 2018-07-27 | 2019-01-01 | 北京矿冶科技集团有限公司 | A kind of automatic identifying method of bacterial attachment optical microscopic image |
| CN109632854B (en) * | 2019-01-14 | 2022-10-11 | 东华理工大学 | Massive uranium ore multi-element online X fluorescence analyzer with double detection structures |
| CN110208303B (en) * | 2019-07-11 | 2021-10-15 | 深圳市应星开物科技有限公司 | Detection method of purple sand ware |
| CN111380887A (en) * | 2020-04-14 | 2020-07-07 | 青海盐湖工业股份有限公司 | Online detection system and method for raw ore |
| CN113295723B (en) * | 2021-07-27 | 2021-09-28 | 西南石油大学 | Molecular simulation characterization method for clay minerals in rock |
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| CN87102281A (en) * | 1987-03-23 | 1988-10-12 | 冶金工业部包头稀土研究院 | Isotope and X fluorescent current-carrying is measured the method for pulp density |
| CN101788508A (en) * | 2010-02-03 | 2010-07-28 | 北京矿冶研究总院 | Ore pulp grade on-line measuring device |
| CN102128845A (en) * | 2009-10-22 | 2011-07-20 | 帕纳科有限公司 | Combination device of XRD and XRF |
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| GB2476255B (en) * | 2009-12-17 | 2012-03-07 | Thermo Fisher Scient Ecublens Sarl | Method and apparatus for performing x-ray analysis of a sample |
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| CN87102281A (en) * | 1987-03-23 | 1988-10-12 | 冶金工业部包头稀土研究院 | Isotope and X fluorescent current-carrying is measured the method for pulp density |
| CN102128845A (en) * | 2009-10-22 | 2011-07-20 | 帕纳科有限公司 | Combination device of XRD and XRF |
| CN101788508A (en) * | 2010-02-03 | 2010-07-28 | 北京矿冶研究总院 | Ore pulp grade on-line measuring device |
Non-Patent Citations (1)
| Title |
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| EDXRF法矿浆品位在线分析系统的探讨;庹先国等;《金属矿山》;20061231(第5期);第59-62页 * |
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