CN113252600A - Method for analyzing ion adsorption state rare earth content of weathering crust sample by reflection spectrum - Google Patents
Method for analyzing ion adsorption state rare earth content of weathering crust sample by reflection spectrum Download PDFInfo
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- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 56
- 238000001228 spectrum Methods 0.000 title claims abstract description 38
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000010521 absorption reaction Methods 0.000 claims abstract description 22
- 230000003595 spectral effect Effects 0.000 claims abstract description 21
- 239000011435 rock Substances 0.000 claims abstract description 12
- 238000004458 analytical method Methods 0.000 claims abstract description 11
- 238000005259 measurement Methods 0.000 claims abstract description 4
- 239000000843 powder Substances 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 3
- 238000012545 processing Methods 0.000 claims abstract description 3
- 150000002500 ions Chemical class 0.000 claims description 37
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 18
- 239000011707 mineral Substances 0.000 claims description 18
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 7
- 229910052622 kaolinite Inorganic materials 0.000 claims description 7
- 238000012937 correction Methods 0.000 claims description 6
- 239000006228 supernatant Substances 0.000 claims description 6
- 238000012935 Averaging Methods 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 4
- 239000012452 mother liquor Substances 0.000 claims description 4
- 238000001055 reflectance spectroscopy Methods 0.000 claims description 4
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- 230000010355 oscillation Effects 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 description 3
- 230000033558 biomineral tissue development Effects 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000010438 granite Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000001320 near-infrared absorption spectroscopy Methods 0.000 description 2
- 230000004075 alteration Effects 0.000 description 1
- 229910052586 apatite Inorganic materials 0.000 description 1
- IKNAJTLCCWPIQD-UHFFFAOYSA-K cerium(3+);lanthanum(3+);neodymium(3+);oxygen(2-);phosphate Chemical compound [O-2].[La+3].[Ce+3].[Nd+3].[O-]P([O-])([O-])=O IKNAJTLCCWPIQD-UHFFFAOYSA-K 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000002734 clay mineral Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000006253 efflorescence Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000009533 lab test Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052590 monazite Inorganic materials 0.000 description 1
- VSIIXMUUUJUKCM-UHFFFAOYSA-D pentacalcium;fluoride;triphosphate Chemical compound [F-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O VSIIXMUUUJUKCM-UHFFFAOYSA-D 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 206010037844 rash Diseases 0.000 description 1
- 238000010223 real-time analysis Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/359—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using near infrared light
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
Abstract
The invention discloses a method for rapidly analyzing rare earth occurrence state by using visible light-near infrared reflection spectrum, which comprises the following steps: (1) drying the weathering crust sample, placing the weathering crust sample in a vessel, and flattening the surface of the weathering crust sample; (2) performing reflection spectrum measurement on a sample in the vessel by using a visible light-near infrared reflection spectrometer, wherein the spectrum range is set to be 350-2500 nm; measuring the powder sample for a plurality of times from different directions at intervals of 90 degrees, measuring the rock block sample for a plurality of times from different directions at intervals of 30 degrees, and recording original spectrum data; (3) and processing the obtained original spectral data, performing peak shape fitting on the 800nm absorption band characteristics, obtaining the position and relative intensity information of the absorption band, and judging the occurrence state of the rare earth elements. The method can meet the requirement of weathering crust ion adsorption type rare earth deposit prospecting work on rapid sample analysis.
Description
Technical Field
The invention relates to a method for rapidly analyzing the content of ion-adsorbed rare earth, in particular to a method for analyzing the content of ion-adsorbed rare earth in a weathering crust sample by reflection spectrum.
Background
Since the rare earth elements have wide application in various fields such as national defense and military industry, aerospace, special materials, metallurgy, energy, agriculture and the like, the rare earth elements are called as industrial vitamins. In recent years, due to rapid development in the fields of aerospace, new energy, new materials and the like, rare earth becomes a key strategic resource.
The weathering crust ion-adsorbing rare earth deposits have developed in large numbers in rock weathering crust based on granite. The weathering crust of rocks in the regions is as thick as 10-30 meters, and favorable conditions are provided for the formation and the preservation of the rare earth deposits. The rare earth elements in the rock weathering crust are separated out and adsorbed on secondary minerals of the weathering crust along with mineral decomposition after strong efflorescence of rare earth-rich bedrock (granite and volcanic). If the rare earth content in the rock weathering crust can reach the boundary grade (above 300 ppm) available for mining, an ore deposit can be formed.
In the ion-adsorption type rare earth deposit, rare earth elements mainly have two occurrence states. One is rare earth accessory mineral (such as monazite and apatite); the other one is formed on the surface of the secondary clay mineral in an ion adsorption state. However, compared with the mineral phase, the ion-adsorbed rare earth elements are low in content, but the extraction process of the mineral is simple and easy to mine. This makes it industrially more valuable in ion-adsorbing type rare earth ores. In contrast, mineral phase rare earths are not effectively utilized. At present, visible light-near infrared reflection spectrum is widely applied to the characterization of ores in various rare earth ore deposits. However, previous studies have focused primarily on the characterization of rare earth content using visible-near infrared reflectance spectroscopy. The environment (coordination number, valence charge, etc.) around the rare earth element can change the position and relative strength of the absorption band significantly, however, the research on the rare earth occurrence state is obviously insufficient. Therefore, on the premise that the analysis detection limit can reach the mineralization boundary grade (more than 300 ppm), a cheap and convenient analysis technology is needed to realize the real-time analysis of the ion adsorption state rare earth content in the natural ion adsorption type rare earth deposit, thereby providing effective support for related ore exploration work.
Therefore, on the premise that the analysis detection limit can reach the mineralization boundary grade (above 300 ppm), a cheap and convenient analysis technology is needed to realize the instant analysis of the rare earth occurrence state in the natural rock weathering crust sample, thereby providing an effective support for the related ore exploration work.
Disclosure of Invention
The invention aims to provide a method for quickly analyzing the ion adsorption state rare earth content of a weathering crust sample by reflection spectrum, solves the problem of low efficiency of the existing method, and can meet the requirement of quick analysis on the sample by weathering crust ion adsorption type rare earth deposit prospecting operation.
In order to achieve the aim, the invention provides a method for rapidly analyzing the ion adsorption state rare earth content of a weathering crust sample by reflection spectroscopy, which comprises the following steps: drying the weathering crust sample, placing the weathering crust sample in a vessel, and flattening the surface of the weathering crust sample; performing reflection spectrum measurement on a sample in the vessel by using a visible light-near infrared reflection spectrometer, wherein the spectrum range is set to be 350-2500 nm; measuring the powder sample for a plurality of times from different directions at intervals of 90 degrees, measuring the rock block sample for a plurality of times from different directions at intervals of 30 degrees, and recording original spectrum data; performing splicing correction and spectrum average processing on the acquired spectrum data, and performing peak shape fitting on an 800nm absorption band; judging the occurrence state of the rare earth elements according to the fitting result, wherein the occurrence state of the rare earth elements is as follows: for an ionic phase, two characteristic peaks with wavelengths of 794nm and 802nm respectively exist near 800nm, the absorption of the 802nm wavelength is weaker than that of the 794nm wavelength, the difference of the absorption intensities of the 794nm wavelength and the 802nm wavelength is used for indicating the content of ion-adsorbed rare earth, and the difference of the absorption intensities of the 794nm wavelength and the 802nm wavelength and the content of ion-adsorbed rare earth are in positive correlation; for the mineral phase, there are two characteristic peaks at wavelengths of 798nm and 807nm, respectively, near 800nm and the absorption at 807nm is stronger than that at 798 nm.
Preferably, the visible-near infrared reflectance spectrometer calibrates the instrument with a standard reflective panel.
Preferably, the raw spectral data measured by the sample is subjected to stitching correction, spectral averaging and peak shape fitting.
Preferably, the vessel is 1.5cm in diameter and 0.5cm deep.
Preferably, the spectral absorption characteristics of rare earth elements of the sample are analyzed, the spectral characteristics of rare earth mineral phases refer to the existing spectrum, and the spectral characteristics of the ion-phase rare earth elements are obtained by simulating the formation process of an ion-adsorption type rare earth deposit, adsorbing the rare earth elements by using kaolinite to obtain the sample and measuring the sample by reflection spectrum.
Preferably, the method for obtaining the spectral characteristics of the ionic phase rare earth elements comprises the following steps: the mother liquor with the concentration of C0Mixing the rare earth mother liquor with the volume of V with the kaolinite with the mass of M, and oscillating; after completion, the supernatant was centrifuged to give a solid, and the supernatant was measured by ICP-MS to obtain a supernatant concentration Ca(ii) a The content of ion phase rare earth in kaolinite is C ═ Co-Ca) Obtaining V/M; and measuring the sample by a visible light-near infrared reflection spectrometer to obtain the ion phase rare earth element reflection spectrum.
Preferably, the oscillation time is 24 h.
The method for rapidly analyzing the ion adsorption state rare earth content of the weathering crust sample by reflection spectrum solves the problem of low efficiency of the existing method, and has the following advantages:
(1) the method disclosed by the invention is rapid and lossless, does not need complicated sample pretreatment, can be used for analyzing the rare earth occurrence state in the rock weathering crust, can be used for realizing in-situ instant analysis through a handheld device, and can also be combined with a related remote sensing technology for application, so that the actual requirement of ore exploration is met;
(2) according to the method, the content of the ion adsorption state rare earth is very conveniently analyzed by utilizing the visible light-near infrared reflection spectrum, and the ion adsorption state rare earth can be judged only according to the position and the relative intensity of the characteristic adsorption peak;
(3) the invention does not need chemical laboratory experiment analysis, not only can shorten the period, but also has higher economic value.
Drawings
FIG. 1 shows the ion adsorption state spectrum characteristic (A) and the relation between its content and the spectrum parameter (B) of the present invention.
FIG. 2 Prior art reports a rare earth element spectrum profile for a mineral phase.
FIG. 3 shows the visible light-near infrared reflection spectrum characteristics (A) and the relation (B) between the spectrum parameters and the ion adsorption state rare earth content of rare earth elements of ion adsorption type rare earth deposit samples in south China.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The method for rapidly analyzing the ion adsorption state rare earth content of the weathering crust sample by reflection spectrum is suitable for rapidly analyzing the rare earth occurrence state in the rock weathering crust sample, and comprises the following specific operation steps:
(1) the weathering crust sample is air-dried to remove moisture in the weathering crust sample, and for a dry rock block sample, the treatment before the experiment is not needed, and only the surface is ensured to be dry and clean;
(2) selecting about 2.0g of sample, putting the sample into a vessel with the depth of 0.5cm and the diameter of 1.5cm, and flattening the surface by using a glass sheet;
(3) performing reflection spectrum measurement on a sample in a vessel by using a visible light-near infrared reflection spectrometer, setting the spectrum range to be 350-2500 nm, and correcting the instrument by using a standard reflection panel;
(4) measuring the powder sample 2 times from different directions at intervals of 90 degrees, measuring the rock block sample 6 times from different directions at intervals of 30 degrees, and recording original spectrum data;
(5) and performing splicing correction and spectrum averaging treatment on the acquired spectrum data, and performing peak shape fitting on the 800nm absorption band characteristic. Then, comparing the position and relative strength of the adsorption zone near 800nm to judge the occurrence state of the rare earth element and the content of the rare earth element in an ion adsorption state; in the step (5), the occurrence state of the rare earth element is judged by comparing the absorption peak position and the relative intensity near 800nm, the existing document can be consulted by the rare earth mineral phase spectral characteristics (see figure 2), and the ionic phase rare earth element spectral characteristics are obtained by simulating the formation process of the ion adsorption type rare earth mineral deposit, adsorbing the rare earth element by kaolinite to obtain a series of standard samples and measuring the samples by a visible light-near infrared reflection spectrometer (see figure 1).
(64) A series of standard samples are measured by a visible light-near infrared reflection spectrometer, and the spectral characteristics and spectral parameters of the ion adsorption state rare earth elements and the relationship between the ion adsorption state rare earth content are obtained (see figure 1).
According to the invention, the ion adsorption state rare earth element content (see table 1) of the ion adsorption type rare earth deposit sample in south China is measured in a laboratory through a sequential extraction process, so that the rare earth element in the deposit sample can be found to exist in an ion phase; on the other hand, the spectral characteristics of the sample were measured by visible-near infrared reflectance spectroscopy (fig. 3). Comparing fig. 3, fig. 2 and fig. 1, it is found that the absorption characteristics of the rare earth elements in the natural sample are identical to the spectral characteristics of the ion-phase rare earth elements simulated in the laboratory, but are very different from the mineral phase (after the obtained spectral data are subjected to splicing correction and spectral averaging, the peak shape fitting is performed on the 800nm absorption band characteristics, and the comparison fitting result shows that (1) the ion phase is near 800nm, the wavelength is 794 and 802nm, and the long-wavelength absorption is relatively weak, and H794 u2ndAnd H802 \u2ndThe difference value of (the difference of the absorption intensity of the wavelengths of 794nm and 802 nm) and the content of the rare earth in the ion adsorption state show positive correlation; (2) mineral phases (according to the prior literature, taking the opposite stone as an example, other minerals are similar): the 800nm peak positions were 798 and 807nm, respectively, and the long wavelength absorption was relatively strong), which is consistent with the simulation experiment. Therefore, in the practice of mineral exploration, the ion adsorption state rare earth content can be rapidly analyzed by sampling and analyzing a large number of samples in the area by using the method disclosed by the invention.
Table 1 shows the content of ionic phase rare earth elements measured by ICP-MS
While the present invention has been described in detail with reference to the preferred embodiments, it should be understood that the above description should not be taken as limiting the invention. Various modifications and alterations to this invention will become apparent to those skilled in the art upon reading the foregoing description. Accordingly, the scope of the invention should be determined from the following claims.
Claims (7)
1. A method for rapidly analyzing the ion adsorption state rare earth content of a weathering crust sample by reflection spectroscopy is characterized by comprising the following steps:
drying the weathering crust sample, placing the weathering crust sample in a vessel, and flattening the surface of the weathering crust sample;
performing reflection spectrum measurement on a sample in the vessel by using a visible light-near infrared reflection spectrometer, wherein the spectrum range is set to be 350-2500 nm; measuring the powder sample for a plurality of times from different directions at intervals of 90 degrees, measuring the rock block sample for a plurality of times from different directions at intervals of 30 degrees, and recording original spectrum data;
performing splicing correction and spectrum average processing on the acquired spectrum data, and performing peak shape fitting on an 800nm absorption band;
judging the occurrence state of the rare earth elements according to the fitting result, wherein the occurrence state of the rare earth elements is as follows:
for an ionic phase, two characteristic peaks with wavelengths of 794nm and 802nm respectively exist near 800nm, the absorption of the 802nm wavelength is weaker than that of the 794nm wavelength, the difference of the absorption intensities of the 794nm wavelength and the 802nm wavelength is used for indicating the content of ion-adsorbed rare earth, and the difference of the absorption intensities of the 794nm wavelength and the 802nm wavelength and the content of ion-adsorbed rare earth are in positive correlation;
for the mineral phase, there are two characteristic peaks at wavelengths of 798nm and 807nm, respectively, near 800nm and the absorption at 807nm is stronger than that at 798 nm.
2. The method for rapid analysis of ion-adsorbed rare earth content of weathering crust samples according to claim 1, wherein the visible-near infrared reflectance spectrometer calibrates the instrument with a standard reflective panel.
3. The method for rapidly analyzing the ion adsorption state rare earth content of the weathering crust sample according to claim 1, wherein the raw spectral data measured by the sample is subjected to stitching correction, spectral averaging and peak shape fitting.
4. The method for rapid analysis of ion adsorption state rare earth content of weathering crust sample according to claim 1, wherein the vessel is 1.5cm in diameter and 0.5cm deep.
5. The method for rapidly analyzing the ion adsorption state rare earth content of the weathering crust sample by reflection spectroscopy according to any one of claims 1 to 4, characterized in that the spectral absorption characteristics of rare earth elements of the sample are analyzed, the spectral characteristics of rare earth mineral phases refer to the existing spectrum, and the spectral characteristics of the ion phase rare earth elements are obtained by simulating the formation process of ion adsorption type rare earth mineral deposits, adsorbing the rare earth elements by kaolinite to obtain the sample, and measuring the sample by reflection spectroscopy.
6. The method for rapidly analyzing the ion adsorption state rare earth content of the weathering crust sample according to the reflection spectrum of claim 5, wherein the method for obtaining the ion phase rare earth element spectral characteristics comprises:
the mother liquor with the concentration of C0Mixing the rare earth mother liquor with the volume of V with the kaolinite with the mass of M, and oscillating; after completion, the supernatant was centrifuged to give a solid, and the supernatant was measured by ICP-MS to obtain a supernatant concentration Ca(ii) a The content of ion phase rare earth in kaolinite is C ═ Co-Ca) Obtaining V/M; measuring the sample by a visible-near infrared reflectance spectrometer to obtainAnd taking the ion phase rare earth element reflection spectrum.
7. The method for rapidly analyzing the ion adsorption state rare earth content of the weathering crust sample according to claim 6, wherein the oscillation time is 24 h.
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Cited By (2)
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| CN114280684A (en) * | 2021-12-24 | 2022-04-05 | 成都理工大学 | Hydrothermal deposit prospecting method and system based on muscovite wavelength change |
| CN116754588A (en) * | 2023-05-18 | 2023-09-15 | 中国科学院广州地球化学研究所 | Method for predicting ion adsorption type rare earth deposit burial depth in weathered crust |
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