CN109813665A - A method for rapid analysis of rare earth content in rock weathering crust using visible light-near infrared reflectance spectroscopy - Google Patents
A method for rapid analysis of rare earth content in rock weathering crust using visible light-near infrared reflectance spectroscopy Download PDFInfo
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- CN109813665A CN109813665A CN201910083918.XA CN201910083918A CN109813665A CN 109813665 A CN109813665 A CN 109813665A CN 201910083918 A CN201910083918 A CN 201910083918A CN 109813665 A CN109813665 A CN 109813665A
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- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 51
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 45
- 239000011435 rock Substances 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 16
- 238000004458 analytical method Methods 0.000 title abstract description 19
- 238000001320 near-infrared absorption spectroscopy Methods 0.000 title 1
- 238000001228 spectrum Methods 0.000 claims abstract description 16
- 238000012360 testing method Methods 0.000 claims abstract description 9
- 230000003595 spectral effect Effects 0.000 claims description 23
- 238000005259 measurement Methods 0.000 claims description 5
- 238000012545 processing Methods 0.000 claims description 5
- 238000010521 absorption reaction Methods 0.000 claims description 3
- 238000009795 derivation Methods 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 2
- 239000011521 glass Substances 0.000 claims 1
- 238000009499 grossing Methods 0.000 claims 1
- 239000005416 organic matter Substances 0.000 abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 3
- 230000035945 sensitivity Effects 0.000 abstract description 2
- 238000001179 sorption measurement Methods 0.000 abstract description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 abstract 2
- 238000003672 processing method Methods 0.000 abstract 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 9
- 239000011707 mineral Substances 0.000 description 9
- 230000008901 benefit Effects 0.000 description 4
- 238000001514 detection method Methods 0.000 description 3
- 238000004611 spectroscopical analysis Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 2
- 238000005553 drilling Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000005357 flat glass Substances 0.000 description 2
- 239000010438 granite Substances 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000985 reflectance spectrum Methods 0.000 description 2
- 238000007605 air drying Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 238000000295 emission spectrum Methods 0.000 description 1
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000010238 partial least squares regression Methods 0.000 description 1
- 238000000918 plasma mass spectrometry Methods 0.000 description 1
- 238000007781 pre-processing Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
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- 229940088594 vitamin Drugs 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
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Abstract
本发明公开了一种利用可见光‑近红外反射光谱对岩石风化壳中的稀土含量进行测试以及分析数据的方法，利用手持式可见光‑近红外反射光谱仪对岩石风化壳的露头、表层土壤以及钻孔样品中的稀土含量进行测试，并通过特定的样品前处理和数据处理手段，消除样品中水、有机物、铁氧化物等成分对稀土含量测试的准确性造成的干扰，提高岩石风化壳中稀土含量测试的准确性和灵敏性，满足风化壳离子吸附型稀土矿床找矿勘查工作对样品进行快速分析的需求。
The invention discloses a method for testing rare earth content in rock weathering crust and analyzing data by using visible light-near-infrared reflection spectrum. The rare earth content in the sample is tested, and through specific sample pretreatment and data processing methods, the interference caused by the water, organic matter, iron oxide and other components in the sample to the accuracy of the rare earth content test is eliminated, and the rare earth content in the rock weathering crust is improved. The accuracy and sensitivity of the test meet the needs of rapid analysis of samples for prospecting and exploration of weathered crust ion adsorption rare earth deposits.
Description
Technical field:
The present invention relates to analysis fields, and in particular to a kind of quickly to analyze rock using visible light-near-infrared spectral reflectance
The method of weathering crust content of rare earth.
Background technique:
Rare earth element in numerous areas such as defence and military, aerospace, special material, metallurgy, the energy and agriculturals due to having
It is widely used, referred to as " industrial vitamin ".In recent years, fast due to fields such as aerospace, new energy and new materials
Speed development is so that rare earth becomes a kind of crucial strategic resource.Demand due to western developed country to rare earth increases year by year, leads
Rare earth (especially heavy rare earth) price on international market is caused persistently to rise.It is driven by the market demand and economic benefit, the world
The exploration and development and utilization of rare earth mineral deposit are all attached great importance in recent years in various countries.Southern region of China (Guangdong, Guangxi, Fujian, Jiangxi
Etc. ground province) weathering crust ion-adsorbed REE deposit be important one of the rare earth resources type in China, provide the whole world and exceed four
/ tri- heavy rare earth product.
Weathering crust ion-adsorbed REE deposit is largely developed in the rock weathering shell based on granite.These areas
Atmospheric disintegration of rocks shell thickness reaches 10-30 meters, provides advantage for the formation and preservation of such rare earth mineral deposit.In rock weathering shell
Rare earth element be the basement rock (granite, volcanic rock) rich in rare earth by after strong slacking, decompose with mineral and
It is precipitated, is adsorbed on the secondary mineral of weathering crust.If the content of rare earth in rock weathering shell can reach the side for exploitation
Boundary's grade (300ppm or more) can form mineral deposit.In planning ore prospect area, delineation ore body range and assessment ore deposit reserve etc.
In mineral exploration practice, need to divide the content of rare earth in the appearing of rock weathering shell, topsoil and drilling sample
Analysis.
At present for the detection of Geological Samples for Rare Earth content rely primarily on inductivity coupled plasma mass spectrometry (ICP-MS),
The analysis means such as x-ray fluorescence analyzer (XRF), inductively coupled plasma emission spectrum (ICP-ES).These analysis means are although inspection
Rising limit is lower (be better than 1ppm), but requires indoors to pre-process sample, experimental period it is long and expensive (50~
200RMB/ sample).Since weathering crust ion-adsorbed REE deposit has the characteristics that distributed areas are wide, in mineral exploration practice
It generally requires that a large amount of samples in some region are sampled and analyzed.Therefore, mineralising side can be reached in analysis detection limit
Under the premise of boundary's grade (300ppm or more), a kind of cheap and convenient and fast analytical technology is needed to realize to natural rock weathering shell
Content of rare earth in sample carries out quickly, or even instant analysis in situ, to provide effective branch for the work of relevant mineral exploration
Support.
Summary of the invention:
The rare earth in rock weathering shell is contained using visible light-near-infrared spectral reflectance the object of the present invention is to provide a kind of
The method for being tested and being analyzed data is measured, using hand-held visible light-near-infrared spectral reflectance instrument to rock weathering shell
Appear, topsoil and drilling sample in content of rare earth tested, and by specific sample pre-treatments and data at
Reason means are interfered caused by eliminating the accuracy that ingredients such as water, organic matter, ferriferous oxide in sample test content of rare earth, are mentioned
The accuracy and sensitivity that content of rare earth is tested in high rock weathering shell, meet weathering crust ion-adsorbed REE deposit and mine are looked for survey
Look into the demand that sample is quickly analyzed in work.
The present invention is achieved by the following technical programs:
It is a kind of that the content of rare earth in rock weathering shell is tested and analyzed using visible light-near-infrared spectral reflectance
Method, method includes the following steps:
A, by surface do clean rock weathering shell sample put into depth greater than 0.5cm, diameter greater than 1.5cm vessel in, benefit
Surface is flattened with sheet glass；
B, reflective spectral measure, spectral region are carried out to the sample in vessel using visible light-near-infrared spectral reflectance instrument
It is set as 350-1000nm, is rectified an instrument using standard reflection panel；It takes multiple measurements from different directions, records primary light
Modal data；
C, the original spectral data for repeatedly measuring sample is weighted and averaged the spectroscopic data as the sample, to eliminate
Sample inhomogeneities bring random error, draws sample spectra curve, this step can using the softwares such as ViewSpecpro into
Row；
D, smoothly and continuously system removal is carried out to sample spectra curve and handles to obtain treated sample spectra curve, this step
Suddenly it is carried out using softwares such as SpecWin.
E, to the curve of spectrum 743nm wavelength absorption intensity of the step d sample spectra curve sample that obtains that treated into
Row second order derivation processing, show that its second order leads value；
F, the second order that step e is obtained is led into value as x value substitution following formula and obtains the content of rare earth y in rock weathering shell；
Y=58500x3+7200x2+2260x+520。
It is described to take multiple measurements from different directions in step b, powder sample is surveyed from the different directions for being spaced 90 °
Amount 2 times then measures 6 times rock block sample from the different directions for being spaced 30 °, records original spectral data.
Beneficial effects of the present invention are as follows:
1, the present invention is that one kind is quick, lossless, contains without the rare earth in cumbersome sample pre-processing analysis rock weathering shell
Amount can realize instant analysis in situ by handheld device, also can to relevant remote sensing technology connected applications, meet weathering crust from
The demand that sub- absorbent-type rare earth Ore Deposits preliminry basic research quickly analyzes sample.
2, the analysis methods such as ICP-MS, ICP-ES and XRF of the present invention are compared, and have biggish cost advantage, the present invention
Analysis cost be about 2-5RMB/ sample.
3, the present invention can be effectively reduced water, organic matter and ferriferous oxide in soil to the shadow of rare earth elemental analysis
It rings, accuracy with higher and lower detection limit.
4, analysis method editable according to the present invention is program, is implanted into existing spectral analysis software in the market, makes
Its product and equipment have the function of quantitative analysis content of rare earth.
Detailed description of the invention:
Fig. 1 is that the Spectroscopic analysis results of weathering crust sample content of rare earth and ICP-MS analyze result Partial Least Squares Regression mould
It is quasi-
Schematic diagram.
Specific embodiment:
It is to further explanation of the invention, rather than limiting the invention below.
Embodiment 1:
Rock weathering shell of the sample from Ganzhou City, Jiangxi Province ion adsorption rare-earth deposit, in this example, I
Using Analytical Spectral Devices (ASD) FieldSpec-3 spectrometer carry out reflective spectral measure, and will
The Spectroscopic analysis results of weathering crust sample content of rare earth are compared with ICP-MS analysis result.
Steps are as follows:
1, sample chooses about 10g and puts the vessel that 0.5cm is deep, diameter is 1.5cm into after laboratory condition natural air drying
In, surface is flattened using sheet glass.
2, reflectance spectrum survey is carried out using Analytical Spectral Devices (ASD) FieldSpec-3 spectrometer
Amount, wherein spectral region is 350-1000nm.Spectrometer first carries out preheating 30min in measurement process, utilizes standard white plate later
Carry out spectrum correction.
3,2 samples are measured from the different directions for being spaced 90 °, records original spectral data.Utilize ViewSpecpro software
Original spectrum curve is pre-processed, takes the averaged spectrum of each sample as the reflectance spectrum of the sample；Then SpecWin is utilized
Continuum removal processing is carried out to the curve of spectrum.
4, the curve of spectrum 743nm wavelength absorption intensity of the sample obtained to step 3 carries out second order derivation processing, obtains it
Second order leads value 743_2nd, empirical equation y=18045x is substituted into as x value3+2233.5x2+696.5x+80.6(R2>0.8),
The y value obtained, as content of rare earth.
Data precision of the present invention and apply efficiency assessment: by same sample carry out ICP-MS analysis total amount of rare earth (reference
Document: Shi Yihua；Qiu Li；Tang Biyu；Yang Zhongping；Song Cian；Gu Hanggan inductively coupled plasma mass spectrometry measures ionic
Rare Earth Mine intermediate ion phase total amount of rare earth and component [J]；Metallurgical analysis；9th phase in 2014), test result is compared such as 1 institute of table
Show.Although certain data have relatively large deviation (result is referring to table 1), the data that two kinds of analysis methods obtain are after over-fitting
Show stronger correlativity y=1.03x (R2=0.73), wherein y value is total with the rare earth of ICP-MS method analysis acquisition
Content, the rare earth total content (such as Fig. 1) that x refers to be obtained with present invention analysis.In mineral exploration practice, by utilizing the present invention
In technical method a large amount of samples in this region are sampled and are analyzed, planning can be met according to the distribution trend of data
Ore prospect area, delineation ore body range and the requirement for assessing ore deposit reserve.
Table 1
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111678882A (en) * | 2020-06-08 | 2020-09-18 | 中国科学院广州地球化学研究所 | A method for predicting the horizon of ion-adsorbed rare earth deposits in weathering crust by paleophrenic level |
| CN113125374A (en) * | 2021-04-16 | 2021-07-16 | 自然资源实物地质资料中心 | Method, device and equipment for detecting REE content in carbonate type rare earth deposit sample |
| CN113252600A (en) * | 2021-05-24 | 2021-08-13 | 中国科学院广州地球化学研究所 | Method for analyzing ion adsorption state rare earth content of weathering crust sample by reflection spectrum |
| CN113433152A (en) * | 2021-06-23 | 2021-09-24 | 自然资源实物地质资料中心 | Method for identifying carbonate type REE ore deposit mineralization zone based on V-NIR and XRF |
| CN114002410A (en) * | 2021-11-04 | 2022-02-01 | 中国有色桂林矿产地质研究院有限公司 | Method for rapidly delineating heavy rare earth ore exploration target area in weathered shell type based on geological body rare earth distribution |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111678882A (en) * | 2020-06-08 | 2020-09-18 | 中国科学院广州地球化学研究所 | A method for predicting the horizon of ion-adsorbed rare earth deposits in weathering crust by paleophrenic level |
| CN111678882B (en) * | 2020-06-08 | 2021-06-04 | 中国科学院广州地球化学研究所 | Method for predicting weathering crust ion adsorption type rare earth deposit horizon through ancient diving space |
| CN113125374A (en) * | 2021-04-16 | 2021-07-16 | 自然资源实物地质资料中心 | Method, device and equipment for detecting REE content in carbonate type rare earth deposit sample |
| CN113252600A (en) * | 2021-05-24 | 2021-08-13 | 中国科学院广州地球化学研究所 | Method for analyzing ion adsorption state rare earth content of weathering crust sample by reflection spectrum |
| CN113433152A (en) * | 2021-06-23 | 2021-09-24 | 自然资源实物地质资料中心 | Method for identifying carbonate type REE ore deposit mineralization zone based on V-NIR and XRF |
| CN113433152B (en) * | 2021-06-23 | 2023-03-07 | 自然资源实物地质资料中心 | Carbonic acid identification based on V-NIR and XRF method for mineralizing zone of rock-type REE deposit |
| CN114002410A (en) * | 2021-11-04 | 2022-02-01 | 中国有色桂林矿产地质研究院有限公司 | Method for rapidly delineating heavy rare earth ore exploration target area in weathered shell type based on geological body rare earth distribution |
| CN114002410B (en) * | 2021-11-04 | 2024-01-09 | 中国有色桂林矿产地质研究院有限公司 | Method for rapidly delineating target area of heavy rare earth mine in weathered crust based on geologic body rare earth distribution |
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