CN112557429B - Quantitative determination method and sample preparation method for all minerals in graphite ore - Google Patents
Quantitative determination method and sample preparation method for all minerals in graphite ore Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 122
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 108
- 239000010439 graphite Substances 0.000 title claims abstract description 108
- 229910052500 inorganic mineral Inorganic materials 0.000 title claims abstract description 70
- 239000011707 mineral Substances 0.000 title claims abstract description 70
- 238000004445 quantitative analysis Methods 0.000 title claims abstract description 30
- 238000005464 sample preparation method Methods 0.000 title claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 55
- 238000000227 grinding Methods 0.000 claims abstract description 43
- 238000005498 polishing Methods 0.000 claims abstract description 43
- 230000008569 process Effects 0.000 claims abstract description 18
- 238000001514 detection method Methods 0.000 claims abstract description 13
- 238000004458 analytical method Methods 0.000 claims abstract description 12
- 239000004203 carnauba wax Substances 0.000 claims description 29
- 238000005259 measurement Methods 0.000 claims description 27
- 239000003822 epoxy resin Substances 0.000 claims description 18
- 229920000647 polyepoxide Polymers 0.000 claims description 18
- 229910052799 carbon Inorganic materials 0.000 claims description 15
- 238000005520 cutting process Methods 0.000 claims description 15
- 229920005989 resin Polymers 0.000 claims description 15
- 239000011347 resin Substances 0.000 claims description 15
- 238000002360 preparation method Methods 0.000 claims description 13
- 229910021532 Calcite Inorganic materials 0.000 claims description 12
- 239000010432 diamond Substances 0.000 claims description 10
- 229910003460 diamond Inorganic materials 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 10
- 239000000725 suspension Substances 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 238000012545 processing Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 239000012736 aqueous medium Substances 0.000 claims description 6
- 239000002609 medium Substances 0.000 claims description 6
- 244000144992 flock Species 0.000 claims description 5
- 230000010355 oscillation Effects 0.000 claims description 4
- 238000005507 spraying Methods 0.000 claims description 4
- 230000001133 acceleration Effects 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 9
- 238000011160 research Methods 0.000 abstract description 6
- 238000005272 metallurgy Methods 0.000 abstract description 2
- 238000005457 optimization Methods 0.000 abstract description 2
- 238000003672 processing method Methods 0.000 abstract description 2
- 238000011002 quantification Methods 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 abstract description 2
- 239000012141 concentrate Substances 0.000 description 9
- 238000001228 spectrum Methods 0.000 description 8
- 239000013078 crystal Substances 0.000 description 7
- 239000004575 stone Substances 0.000 description 7
- 239000003795 chemical substances by application Substances 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 235000013339 cereals Nutrition 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 238000000691 measurement method Methods 0.000 description 3
- 239000010445 mica Substances 0.000 description 3
- 229910052618 mica group Inorganic materials 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000010453 quartz Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- 239000002734 clay mineral Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052961 molybdenite Inorganic materials 0.000 description 2
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 2
- 238000007517 polishing process Methods 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- 229910052720 vanadium Inorganic materials 0.000 description 2
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 238000001237 Raman spectrum Methods 0.000 description 1
- 241000613130 Tima Species 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000003082 abrasive agent Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 238000009614 chemical analysis method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000007405 data analysis Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000010812 external standard method Methods 0.000 description 1
- 239000010433 feldspar Substances 0.000 description 1
- 235000011868 grain product Nutrition 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 238000010191 image analysis Methods 0.000 description 1
- 238000010813 internal standard method Methods 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- YQCIWBXEVYWRCW-UHFFFAOYSA-N methane;sulfane Chemical compound C.S YQCIWBXEVYWRCW-UHFFFAOYSA-N 0.000 description 1
- 238000000386 microscopy Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000002310 reflectometry Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000000547 structure data Methods 0.000 description 1
- 150000004763 sulfides Chemical class 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 229910052613 tourmaline Inorganic materials 0.000 description 1
- 239000011032 tourmaline Substances 0.000 description 1
- 229940070527 tourmaline Drugs 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910052845 zircon Inorganic materials 0.000 description 1
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/2202—Preparing specimens therefor
-
- 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
- G01N23/225—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 using electron or ion
- G01N23/2251—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 using electron or ion using incident electron beams, e.g. scanning electron microscopy [SEM]
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention belongs to the technical field of mineral analysis and detection, and particularly discloses a quantitative determination method of all minerals in graphite ores, and also discloses a sample preparation method in the quantitative determination of all minerals of the graphite ores. Aiming at the problem that the existing graphite ore is difficult to accurately and quantitatively determine, the invention uses an improved sample processing method based on an automatic process mineralogy quantitative analysis method, and particularly carries out proper mosaic and grinding and polishing treatment on a graphite ore sample, thereby realizing the accurate quantification of the whole mineral of the graphite ore. The invention provides a new technical means for the research fields of geology, mineral separation, metallurgy, materials and the like, and provides a mineralogy basis for the mineral resource mineral exploration, comprehensive utilization and optimization process flow containing graphite.
Description
Technical Field
The invention relates to the technical field of mineral analysis and detection, in particular to a method for detecting graphite ores, especially a method for quantitatively determining all minerals in the graphite ores, and also relates to a sample preparation method in quantitative determination of all minerals in the graphite ores.
Background
Graphite is a natural element mineral composed of carbon elements, and is a special nonmetallic material with excellent performance. With the advent of new materials for lithium ion batteries and graphene high technology in recent years, graphite resources are receiving more and more social attention, and are becoming recognized strategically emerging mineral products at home and abroad. Comprehensive utilization of graphite resources is not separated from intensive researches on technology mineralogy and the like of the type of resources, including researches on relative content, embedding relation, dissociation characteristics, occurrence state of carbon elements and the like of valuable minerals such as graphite. In particular, quantitative analysis and measurement of graphite minerals are the most central contents of the research of graphite technology mineralogy. The existing quantitative analysis and determination methods of graphite mainly comprise a chemical analysis method, a polarizing microscope light sheet and sheet determination method, an X-ray powder crystal diffraction quantitative analysis method, an automatic process mineralogy quantitative analysis method, a Raman spectrum analysis method and the like.
Chemical analysis generally employs fixed carbon measurement or all carbon measurement. The measurement of fixed carbon in graphite ore is determined by adopting a loss-on-ignition method, and when the graphite sample contains mineral components such as sulfides, carbonates and the like which are easy to decompose and volatilize or oxidize, the measurement method has larger error. All-carbon measurement is commonly performed by a carbon-sulfur meter method. Either the fixed carbon measurement method or the all-carbon measurement method can only measure the carbon content or the fixed carbon content in the graphite sample, but not the graphite content, and the quantitative analysis of other components in the graphite resource cannot be performed.
Quantitative analysis by polarized microscopy is to grind the ore into a sheet or flake and measure the mineral content in either reflected or transmitted light. Since the identification of minerals depends on human vision, the subjectivity is strong and the error is large. The OIS system (Optical Image Analysis) developed rapidly in recent years can automatically measure minerals in ores according to differences of visible light reflection signals of the minerals in different wave bands. However, the method is only suitable for ore samples with simple mineral composition and large difference in reflectivity between minerals, and is not suitable for analysis of graphite ores.
The quantitative analysis of the phase of the X-ray powder crystal diffractometer adopts an internal standard method, an external standard method, a K value method, a Rietveld full spectrum fitting method and the like, wherein the Rietveld full spectrum fitting method is based on a known crystal structure model, structural parameters and peak shape functions, and a computer is adopted to adjust the parameters to be approximately fitted with an experimental spectrum, so that the mineral composition and content in a sample, crystal structure data and the like can be obtained. Rietveld full spectrum fitting method reduces the influence of factors such as diffraction overlapping peaks, crystal preferred orientation and the like to a certain extent, but XRD cannot detect low-content minerals (detection limit is different from different substances and is generally about 0.1% -10%). In addition, most of graphite has lamellar crystal form and flexibility, the preferred crystal orientation is very obvious, sample preparation is difficult, powder crystallization is difficult, and therefore XRD quantitative analysis results are affected.
The automatic process mineralogy quantitative analysis method (such as MLA, AMICS, TIMA) based on the scanning electron microscope is to analyze the data image of the sample by the scanning electron microscope, then distinguish different areas according to the differences of the backscattering signals of the mineral particles, analyze the minerals according to the spectral peak database of the energy spectrum, and realize the automatic measurement of the mineralogy parameters of the ore process. The method has the advantages of wide measurement range and large statistical quantity, so the method has higher measurement precision and is a mineral quantitative analysis method widely applied at present. However, for graphite-containing samples, since graphite is composed of carbon atoms, the atomic number is low, the SEM backscattering signal is weak, and is comparable to that of conventional epoxy resin embedding agents, so that conventional automatic process mineralogy quantitative analysis methods cannot realize quantitative analysis of graphite.
Therefore, it is necessary to provide a quantitative determination method for graphite ore to analyze the graphite ore more accurately, and provide scientific and technical support for the technical mineralogy research of graphite.
Disclosure of Invention
The invention mainly solves the technical problem of providing a quantitative determination method for all minerals in graphite ores.
The invention solves the other technical problem of providing a graphite ore sample preparation method in the quantitative determination of the whole mineral of the graphite ore.
In order to solve the technical problems, the invention adopts the following technical scheme.
In a first aspect, the invention provides a sample preparation method for quantitative determination of all minerals in graphite ore, which comprises a sample preparation step of a graphite ore sample, wherein the sample preparation step of the graphite ore sample comprises the step of inlaying the graphite ore sample, and the inlaying is carried out by adopting palm wax and epoxy resin to treat the graphite ore sample.
As a preferred embodiment of the present invention, the step of preparing a graphite ore sample further includes polishing the inlaid graphite ore sample, where the polishing process sequentially includes: rough grinding, primary fine grinding, secondary fine grinding, rough polishing and fine polishing;
preferably, the coarse grinding is performed in an aqueous medium by adopting a SiC millstone, and the granularity of SiC is 500#; and/or the number of the groups of groups,
the primary fine grinding is carried out in an aqueous medium by adopting a SiC millstone, and the granularity of SiC is 1200#; and/or the number of the groups of groups,
the secondary fine grinding is carried out in an aqueous medium by adopting a SiC millstone, and the granularity of SiC is 2000#; and/or the number of the groups of groups,
the rough polishing is carried out in a diamond suspension medium by adopting a synthetic flock millstone, and the specification of the diamond suspension is 3 mu m; and/or the number of the groups of groups,
the fine polishing is carried out in a diamond suspension medium by using a synthetic flock millstone, and the specification of the diamond suspension is 1 mu m.
As a preferred embodiment of the invention, the inlaying treatment is carried out by inlaying a graphite ore sample by adopting palm wax and then carrying out cold inlaying treatment by adopting epoxy resin.
As a preferred embodiment of the present invention, the graphite ore sample is a graphite-containing ore, including raw graphite ore, graphite concentrate or other graphite-containing product, which is crushed prior to the tessellation process.
As a preferred embodiment of the invention, when the particle size of the graphite ore sample is larger than 0.02mm, the inlaying treatment method comprises the following steps: and (3) placing the sample to be treated into a mould, heating the mould, pouring molten palm wax into the mould, stirring, vacuumizing, cutting the sample into halves along the longitudinal surface by a cutting machine after the sample is completely solidified, placing the two halves of the sample into the mould with the longitudinal surface facing downwards after drying, and injecting epoxy resin for cold inlay to obtain the graphite ore resin polished section.
As a preferred embodiment of the invention, when the particle size of the graphite ore sample is less than 0.02mm, the inlaying treatment method comprises the following steps: placing a sample to be treated into a mould, adding absolute ethyl alcohol into the mould, dispersing by ultrasonic oscillation, pouring molten palm wax into the mould after the absolute ethyl alcohol is completely dispersed and volatilized, uniformly stirring, then carrying out ultrasonic oscillation treatment, then cutting the sample into halves along longitudinal faces by a cutting machine after the sample is completely solidified, placing the longitudinal sections of the two halves of the sample into the mould downwards after drying, and injecting epoxy resin for cold mosaic to obtain the graphite ore resin polished section.
As a preferred embodiment of the invention, the pressure used for the rough grinding is 12-18 kpa and the rotating speed is 75-100 r/min.
The pressure of the primary fine grinding is 8-12 kpa, and the rotating speed is 75-100 r/min.
The pressure of the secondary fine grinding is 12-18 kpa, and the rotating speed is 75-100 r/min.
The pressure of the rough polishing is 15-25 kpa, and the rotating speed is 75-100 r/min.
The pressure of the fine polishing is 15-25 kpa, and the rotating speed is 75-100 r/min.
As a more preferred embodiment of the present invention, the rough grinding is carried out at a pressure of 15kpa, a rotational speed of 90r/min and a rough grinding time of 5min.
The pressure of the primary fine grinding is 10kpa, the rotating speed is 90r/min, and the primary fine grinding time is 3min.
The pressure of the secondary fine grinding is 15kpa, the rotating speed is 90r/min, and the secondary fine grinding time is 3min.
The pressure of rough polishing is 20kpa, the rotating speed is 90r/min, and the rough polishing time is 5min.
The pressure of the fine polishing is 20kpa, the rotating speed is 90r/min, and the fine polishing time is 3min.
In a second aspect, the invention provides a method for quantitatively determining all minerals in graphite ores, comprising a sample preparation step, wherein the sample preparation step adopts the sample preparation method.
As a preferred embodiment of the present invention, the quantitative determination method further comprises a step of detecting the prepared sample;
the step of detecting the prepared sample is to adopt an MLA system to carry out analysis detection and data processing, so as to obtain the quantitative composition of each mineral in the graphite ore.
As a preferred embodiment of the present invention, the step of detecting the prepared sample comprises:
carrying out MLA system measurement after spraying carbon on the graphite ore resin polished section obtained by sample preparation; and an analysis step after the MLA measurement is completed.
The data analysis method adopted in the analysis step is an analysis method commonly used in an MLA (mineral parameter automatic quantitative analysis) system, and comprises the following steps: and (3) sorting and naming the newly built mineral list, carrying out classification batch processing, processing the classified database image, and finally creating an ore process mineralogy database to obtain content data of each mineral contained in the graphite ore.
Preferably, the MLA system model is MLA 650; SEM acceleration voltage is 20kV, and beam spot is 7.0nm;
respectively selecting palm wax and calcite as gray standard samples to adjust the contrast and brightness of SEM in BSE mode, setting the gray value of the palm wax as 0 and setting the gray value of the calcite as 255;
selecting resin polished sections with the grain size of-0.074mm+0.04mm to adopt a standard measurement mode, and adopting XBSE measurement modes for resin polished sections with other grain sizes;
the measurement region selects a representative region.
In the quantitative measurement of all minerals of graphite ore, sample preparation is a key step. At present, the conventional automatic process mineralogy quantitative analysis method (such as MLA) adopts epoxy resin as embedding agent to inlay and prepare samples. However, for the graphite-containing samples, since graphite is composed of carbon atoms, the atomic number is low and the SEM backscatter signal is very weak, comparable to that of the epoxy embedding agent. Therefore, when the graphite ore is detected, the target mineral is usually subtracted as a background due to the fact that the scanning electron microscope back scattering signal of the target mineral is close to that of a conventional epoxy resin embedding agent, and the detection of the graphite is not facilitated. Therefore, the conventional automatic process mineralogy quantitative analysis method cannot realize quantitative analysis of graphite at all. According to the invention, the palm wax is adopted for embedding, and then the epoxy resin is adopted for cold embedding treatment, so that the prepared test sample can effectively separate graphite from the background of the embedding agent. During detection, palm wax and calcite are respectively selected as gray standard samples in the BSE mode to adjust the contrast and brightness of the SEM, the gray value of the palm wax is set to be 0, and the gray value of the calcite is set to be 255, so that accurate detection can be realized.
The polishing process step after the damascene process is also critical. Because graphite ore is different from coal mine samples, the graphite samples have more mineral types, the hardness and brittleness among minerals are very different, and the conventional grinding and polishing method often leads to the falling of high-hardness and brittle minerals from a polished section, so that the inaccuracy of detection results is caused. The polishing scheme of the graphite sample polished section provided by the invention is that coarse polishing, primary fine polishing, secondary fine polishing, coarse polishing and fine polishing are sequentially carried out, and the high-hardness and brittle minerals can be ensured not to fall off from the polished section through the sequence of a plurality of working procedures, so that the minerals can be completely reserved, and the guarantee is provided for the accurate measurement of the next step.
Aiming at the problem that the existing graphite ore is difficult to accurately and quantitatively determine, the invention uses an improved sample processing method based on an automatic process mineralogy quantitative analysis method, particularly carries out proper mosaic and polishing treatment on a graphite ore sample, and realizes the accurate quantification of all the minerals of the graphite ore through proper detection conditions, particularly the setting of measurement parameters. The invention provides a new technical means for the research fields of geology, mineral separation, metallurgy, materials and the like, and provides a mineralogy basis for the mineral resource mineral exploration, comprehensive utilization and optimization process flow containing graphite.
Drawings
FIG. 1 is a graph of the polished back scattering of a sample of graphite ore of example 1 of the present invention;
FIG. 2 is a graph of the polished back scattering of a sample of graphite concentrate of example 2 of the present invention.
Detailed Description
The technical scheme of the invention is described in detail through specific embodiments.
Example 1
The embodiment is a method for quantitatively measuring all minerals in a certain graphite ore, which comprises the following specific processes:
step one: representative graphite ore was crushed to-0.2 mm and 100g of the sample was again collected and sieved and water-separated to obtain 4 fractions of +0.074mm, +0.04mm, +0.02mm and-0.02 mm.
Step two: for 3 grain products with the grain size larger than 0.02mm, respectively taking 2-4 g of samples, respectively placing the samples into 3 moulds with the diameter of 25mm, placing the moulds on stone slabs, and then placing the stone slabs into a baking oven with the temperature of 130 ℃ for standby. About 10g of palm wax was weighed and put into a 50mL beaker and heated on an electric furnace to completely melt the palm wax. Taking out the stone slab and the mould from the oven, pouring the melted palm wax into the membrane, rapidly stirring, putting into a vacuum drying box, exhausting for 5 minutes, taking out, cutting the sample into halves along the longitudinal surface by a cutting machine after the sample is completely solidified, putting the two halves of the sample into the mould with the longitudinal surface facing downwards after drying, and injecting the prepared epoxy resin for cold inlaying.
Step three: aiming at the problem that mud samples with granularity smaller than 0.02mm are difficult to disperse due to caking and agglomeration, ultrasonic wave is adopted for sample preparation. Grinding the dried mud sample, taking 0.3-0.5 g of sample, putting the sample into a mould, adding 3-5 mL of absolute ethyl alcohol into the mould by using a dropper, putting the sample into an ultrasonic cleaner for vibrating and pre-dispersing, pouring molten palm wax into a grinding tool after the agglomerate particles in the sample are completely dispersed and the absolute ethyl alcohol volatilizes completely, uniformly stirring, putting the sample into an ultrasonic cleaner for vibrating for 5 minutes in a water bath at 100 ℃, taking out the sample, cutting the sample into halves along longitudinal faces by using a cutting machine after the sample is completely solidified, putting the longitudinal sections of the two halves of the sample into the mould downwards after the sample is dried, and injecting the prepared epoxy resin for cold mosaic.
Step four: and (3) cutting off surface resin from the test surface of the polished wafer sample after curing in the second step and the third step to expose ore particles, and then polishing. Grinding and polishing adopt a Siterl device, consumable materials such as millstone abrasive materials are purchased from Siterl company, and the grinding and polishing steps are sequentially as follows: rough grinding, primary fine grinding, secondary fine grinding, rough polishing and fine polishing, and specific operations are shown in table 1. Wherein DP is the diamond suspension medium, and 3 μm and 1 μm are all specifications of the diamond suspension. MD-Nap is the synthetic flock millstone.
Table 1 sample polishing step operating conditions
Step five: the polished resin polished wafer was subjected to MLA system (model: MLA 650) measurement after carbon spraying.
The SEM acceleration voltage is 20kV, the beam spot is 7.0nm, and the contrast and brightness of SEM are respectively adjusted by selecting palm wax and calcite as gray scale standard samples in BSE mode, the gray scale value of the palm wax is set to be 0, the gray scale value of the calcite is set to be 255, and the polished back scattering diagram of the graphite ore sample is shown in figure 1.
The standard measurement mode is adopted by selecting the-0.074mm+0.04mm particle-size polished sections, the XBSE measurement mode is adopted by other particle-size resin polished sections, and the representative rectangular area is selected by the measurement area.
Step six: after the MLA measurement is completed, the newly built mineral list is arranged and named, classified batch processing is carried out, the classified database image is processed, the distinction of epoxy resin and graphite is paid attention to, and finally an ore process mineralogy database is created, so that a data table of the accurate content of all minerals containing graphite is obtained, and the data table is shown in Table 2 in detail.
TABLE 2 composition and content of each mineral in graphite ore
| Mineral material | Relative content (wt%) | Mineral material | Relative content (wt%) |
| Graphite | 26.70 | Limonite iron ore | 0.15 |
| Vanadium mica | 21.45 | Rutile type | 0.21 |
| Quartz | 50.52 | Zircon | 0.02 |
| Feldspar | 0.09 | Solitary stone | 0.03 |
| Tourmaline | 0.04 | Molybdenite (molybdenite) | 0.02 |
| Clay mineral | 0.20 | Others | 0.61 |
Example 2
The embodiment is a quantitative determination method for all minerals in graphite concentrate, which comprises the following specific processes:
step one: and taking 1-2 g of representative sample, ultrasonically cleaning the representative sample with absolute ethyl alcohol for 5 minutes, and drying for later use.
Step two: and (5) placing the dried sample into a mold with the diameter of 25mm, placing the mold on a stone plate, and then placing the stone plate into a baking oven with the temperature of 130 ℃ for standby. About 3g of palm wax was weighed and put into a 50mL beaker and heated on an electric furnace to completely melt the palm wax. Taking out the stone slab and the mould from the oven, pouring the melted palm wax into the membrane, rapidly stirring, putting into a vacuum drying box, exhausting for 5 minutes, taking out, cutting the sample into halves along the longitudinal surface by a cutting machine after the sample is completely solidified, putting the two halves of the sample into the mould with the longitudinal surface facing downwards after drying, and injecting the prepared epoxy resin for cold inlaying.
Step three: and cutting off surface resin from the test surface of the cured polished section sample to expose ore particles, and polishing. The polishing step was the same as in step four of example 1, and polishing was performed using the equipment and consumables of stell, and the specific method is shown in table 1.
Step four: the prepared resin polished section was subjected to MLA system (model: MLA 650) measurement after carbon spraying.
The SEM accelerating voltage is 20kV, the beam spot is 7.0nm, the contrast and brightness of the SEM are adjusted by respectively selecting palm wax and calcite as gray standard samples in the BSE mode, the gray value of the palm wax is set to be 0, the gray value of the calcite is set to be 255, and the standard measuring mode is adopted. The polished back-scattering plot of the graphite concentrate sample is shown in fig. 2.
Step five: after the MLA measurement is completed, the newly built mineral list is arranged and named, classified batch processing is carried out, the classified database image is processed, the distinction of epoxy resin and graphite is paid attention to, and finally an ore process mineralogy database is created, so that a data table containing the accurate content of all minerals of graphite concentrate is obtained, and the data table is shown in Table 3 in detail.
TABLE 3 composition and content of certain graphite concentrate minerals
| Mineral material | Relative content (wt%) | Mineral composition | Relative content (wt%) |
| Graphite | 97.49 | Limonite iron ore | 0.19 |
| Vanadium mica | 1.05 | Clay mineral | 0.12 |
| Quartz | 1.04 | Others | 0.11 |
The graphite concentrate sample was subjected to X-ray diffraction Rietveld full spectrum fitting quantitative analysis, and the results are shown in table 4.
TABLE 4 XRD Rietveld full spectrum fitting quantitative analysis results of graphite concentrate
| Mineral material | Relative content (wt%) |
| Graphite | 86.6 |
| Mica | 0.1 |
| Quartz | 13.3 |
The graphite concentrate sample was also subjected to fixed carbon chemical analysis, resulting in 96.45%. It can be seen that the method of the invention is used for carrying out full mineral determination on the graphite-containing ore, and the result is better than the XRD Rietveld full spectrum fitting quantitative analysis method and is closer to the chemical analysis result.
As can be seen from the above examples 1 and 2, the present invention adopts palm wax to inlay and then adopts epoxy resin to conduct cold inlay treatment through the improvement of the sample preparation step, and the prepared test sample can effectively separate graphite from embedding medium background. And then adopting a grinding and polishing scheme of coarse grinding, primary fine grinding, secondary fine grinding, coarse polishing and fine polishing, reasonably setting parameters and reagents in the grinding and polishing scheme, and ensuring that the high-hardness and brittle minerals are not fallen off from the polished section through the sequence of a plurality of working procedures, so that the minerals are completely reserved, and a guarantee is provided for accurate determination. During detection, palm wax and calcite are respectively selected as gray standard samples in the BSE mode to adjust the contrast and brightness of the SEM, the gray value of the palm wax is set to be 0, and the gray value of the calcite is set to be 255, so that accurate detection can be realized. Finally, the accurate quantitative detection of the whole mineral of the graphite ore is realized.
While the invention has been described in detail in the foregoing general description, embodiments and experiments, it will be apparent to those skilled in the art that modifications and improvements can be made thereto. Accordingly, such modifications or improvements may be made without departing from the spirit of the invention and are intended to be within the scope of the invention as claimed.
Claims (3)
1. The sample preparation method for quantitative determination of all minerals in the graphite ore is characterized by comprising a sample preparation step of a graphite ore sample, wherein the sample preparation step of the graphite ore sample comprises the step of inlaying the graphite ore sample, the inlaying is carried out on the graphite ore sample by adopting palm wax and epoxy resin, the graphite ore sample is inlaid by adopting the palm wax, and then the graphite ore sample is cold inlaid by adopting the epoxy resin;
when the particle size of the graphite ore sample is larger than 0.02mm, the adopted mosaic treatment method comprises the following steps: placing a sample to be treated into a mould, heating the mould, pouring molten palm wax into the mould, stirring, vacuumizing, splitting the sample into halves along longitudinal surfaces by a cutting machine after the sample is completely solidified, placing the two halves of the sample into the mould with the longitudinal surfaces facing downwards after drying, and injecting epoxy resin for cold inlay to obtain a graphite ore resin polished section;
when the particle size of the graphite ore sample is smaller than 0.02mm, the adopted mosaic treatment method comprises the following steps: placing a sample to be treated into a mould, adding absolute ethyl alcohol into the mould, dispersing by ultrasonic oscillation, pouring molten palm wax into the mould after the absolute ethyl alcohol is completely dispersed and volatilized, uniformly stirring, then carrying out ultrasonic oscillation treatment, then cutting the sample into halves along longitudinal faces by a cutting machine after the sample is completely solidified, placing the two halves of the longitudinal faces of the sample into the mould after drying, injecting epoxy resin into the mould for cold mosaic, and obtaining a graphite ore resin polished section;
the graphite ore sample preparation step further comprises grinding and polishing treatment of the inlaid graphite ore sample, and the grinding and polishing treatment adopts the following procedures in sequence: rough grinding, primary fine grinding, secondary fine grinding, rough polishing and fine polishing;
the coarse grinding is carried out in an aqueous medium by adopting a SiC millstone, and the granularity of SiC is 500#; the pressure adopted by the rough grinding is 15kpa, the rotating speed is 90r/min, and the rough grinding time is 5min;
the primary fine grinding is carried out in an aqueous medium by adopting a SiC millstone, and the granularity of SiC is 1200#; the pressure of the primary fine grinding is 10kpa, the rotating speed is 90r/min, and the primary fine grinding time is 3min;
the secondary fine grinding is carried out in an aqueous medium by adopting a SiC millstone, and the granularity of SiC is 2000#; the pressure of the secondary fine grinding is 15kpa, the rotating speed is 90r/min, and the secondary fine grinding time is 3min;
the rough polishing is carried out in a diamond suspension medium by adopting a synthetic flock millstone, and the specification of the diamond suspension is 3 mu m; the pressure of rough polishing is 20kpa, the rotating speed is 90r/min, and the rough polishing time is 5min;
the fine polishing is carried out in a diamond suspension medium by adopting a synthetic flock millstone, and the specification of the diamond suspension is 1 mu m;
the pressure of the fine polishing is 20kpa, the rotating speed is 90r/min, and the fine polishing time is 3min.
2. A method for quantitatively determining all minerals in graphite ore, which is characterized by comprising the steps of the sample preparation method according to claim 1; further comprising the step of detecting the prepared sample;
the step of detecting the prepared sample is to adopt an MLA system for analysis detection and data processing to obtain the quantitative composition of each mineral in the graphite ore;
the MLA system model is MLA 650; SEM acceleration voltage is 20kV, and beam spot is 7.0nm;
respectively selecting palm wax and calcite as gray standard samples to adjust the contrast and brightness of SEM in BSE mode, setting the gray value of the palm wax as 0 and setting the gray value of the calcite as 255;
resin light sheets with the particle size of-0.074mm+0.04mm are selected to adopt a standard measurement mode, and resin light sheets with the particle size of +0.074mm and-0.04 mm are selected to adopt an XBSE measurement mode.
3. The quantitative determination method according to claim 2, wherein the step of detecting the prepared sample comprises:
carrying out MLA system measurement after spraying carbon on the graphite ore resin polished section obtained by sample preparation; the method comprises the steps of,
after the MLA measurement is completed, the newly built mineral list is arranged and named, classified batch processing is carried out, the classified database image is processed, and finally an ore process mineralogy database is created, so that the content data of each mineral contained in the graphite ore is obtained.
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