CN105866387A - Manganese ore phase analyzing method - Google Patents
Manganese ore phase analyzing method Download PDFInfo
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- CN105866387A CN105866387A CN201610432502.0A CN201610432502A CN105866387A CN 105866387 A CN105866387 A CN 105866387A CN 201610432502 A CN201610432502 A CN 201610432502A CN 105866387 A CN105866387 A CN 105866387A
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- 239000011572 manganese Substances 0.000 title claims abstract description 76
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 229910052748 manganese Inorganic materials 0.000 title claims abstract description 74
- 238000000034 method Methods 0.000 title claims abstract description 38
- 238000001914 filtration Methods 0.000 claims abstract description 77
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 51
- 238000004458 analytical method Methods 0.000 claims abstract description 40
- 239000002253 acid Substances 0.000 claims abstract description 37
- 239000000243 solution Substances 0.000 claims abstract description 35
- 239000011656 manganese carbonate Substances 0.000 claims abstract description 23
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 claims abstract description 23
- 229940093474 manganese carbonate Drugs 0.000 claims abstract description 22
- 235000006748 manganese carbonate Nutrition 0.000 claims abstract description 22
- XMWCXZJXESXBBY-UHFFFAOYSA-L manganese(ii) carbonate Chemical compound [Mn+2].[O-]C([O-])=O XMWCXZJXESXBBY-UHFFFAOYSA-L 0.000 claims abstract description 22
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims abstract description 17
- 150000001875 compounds Chemical class 0.000 claims abstract description 14
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims abstract description 13
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000007864 aqueous solution Substances 0.000 claims abstract description 8
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 47
- 229910001868 water Inorganic materials 0.000 claims description 40
- VGYYSIDKAKXZEE-UHFFFAOYSA-L hydroxylammonium sulfate Chemical compound O[NH3+].O[NH3+].[O-]S([O-])(=O)=O VGYYSIDKAKXZEE-UHFFFAOYSA-L 0.000 claims description 35
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 32
- 238000003756 stirring Methods 0.000 claims description 28
- 239000000706 filtrate Substances 0.000 claims description 26
- 238000002386 leaching Methods 0.000 claims description 18
- 238000005303 weighing Methods 0.000 claims description 16
- 239000001117 sulphuric acid Substances 0.000 claims description 14
- 235000011149 sulphuric acid Nutrition 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 12
- 238000004380 ashing Methods 0.000 claims description 11
- NVJMLVXGMVTTAN-UHFFFAOYSA-N [Mn].[Si](O)(O)(O)O Chemical compound [Mn].[Si](O)(O)(O)O NVJMLVXGMVTTAN-UHFFFAOYSA-N 0.000 claims description 10
- 235000019504 cigarettes Nutrition 0.000 claims description 9
- 229910052573 porcelain Inorganic materials 0.000 claims description 9
- 238000004090 dissolution Methods 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 230000001684 chronic effect Effects 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- IUYPUOPCLGUJMB-UHFFFAOYSA-N perchloric acid hydrofluoride Chemical compound F.OCl(=O)(=O)=O IUYPUOPCLGUJMB-UHFFFAOYSA-N 0.000 claims description 2
- 238000010298 pulverizing process Methods 0.000 claims description 2
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical compound FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims 1
- 229910052782 aluminium Inorganic materials 0.000 claims 1
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 abstract description 34
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 abstract 2
- 238000000605 extraction Methods 0.000 abstract 1
- NXPHCVPFHOVZBC-UHFFFAOYSA-N hydroxylamine;sulfuric acid Chemical compound ON.OS(O)(=O)=O NXPHCVPFHOVZBC-UHFFFAOYSA-N 0.000 abstract 1
- 229920001131 Pulp (paper) Polymers 0.000 description 17
- 230000000052 comparative effect Effects 0.000 description 9
- 238000009835 boiling Methods 0.000 description 8
- 239000008367 deionised water Substances 0.000 description 7
- 229910021641 deionized water Inorganic materials 0.000 description 7
- 229910052500 inorganic mineral Inorganic materials 0.000 description 7
- 239000007788 liquid Substances 0.000 description 7
- 239000011707 mineral Substances 0.000 description 7
- 229950000845 politef Drugs 0.000 description 7
- 235000010755 mineral Nutrition 0.000 description 6
- 150000003839 salts Chemical class 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 5
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Inorganic materials O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000011435 rock Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- XTEGARKTQYYJKE-UHFFFAOYSA-N chloric acid Chemical compound OCl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-N 0.000 description 1
- 229940005991 chloric acid Drugs 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- ASTZLJPZXLHCSM-UHFFFAOYSA-N dioxido(oxo)silane;manganese(2+) Chemical compound [Mn+2].[O-][Si]([O-])=O ASTZLJPZXLHCSM-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- IMBKASBLAKCLEM-UHFFFAOYSA-L ferrous ammonium sulfate (anhydrous) Chemical compound [NH4+].[NH4+].[Fe+2].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O IMBKASBLAKCLEM-UHFFFAOYSA-L 0.000 description 1
- 229910001655 manganese mineral Inorganic materials 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 229910052883 rhodonite Inorganic materials 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 230000009897 systematic effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/24—Earth materials
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
-
- 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
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- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Pathology (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Analytical Chemistry (AREA)
- Engineering & Computer Science (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Geology (AREA)
- Remote Sensing (AREA)
- Food Science & Technology (AREA)
- Medicinal Chemistry (AREA)
- Biomedical Technology (AREA)
- Molecular Biology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention relates to an analysis determination method for specific compounds in ore, in particular to a manganese ore phase analyzing method. The manganese ore phase analyzing method is characterized in by comprising the following steps that firstly, manganese ore is weighed and smashed; secondly, an aluminum nitrate aqueous solution is added into the smashed manganese ore, extracting and filtering are carried out, filter residues are collected, and the manganese carbonate ore phase of filter liquor is determined; thirdly, a hydroxylamine sulphate and sulfuric acid solution is added into the filter residues collected in the second step, extracting and filtering are carried out, filter residues are collected, and the manganese oxide ore phase of filter liquor is determined; fourthly, the filter residues obtained the third step are ashed, mixed acid including nitric acid, hydrofluoric acid and perchloric acid is added for dissolving the ashed filter residues, and the manganese ore phase is determined. The manganese ore phase analyzing method is accurate and simple, the influence of phase shifting in the extraction processes is greatly relieved, the accuracy of an analyzing result is improved, and the problems that in a traditional manganese ore phase analyzing method, errors are large, phase shifting is serious, and efficiency is low are solved.
Description
Technical field
The present invention relates to the analysis determining method of specific compound in a kind of Ore, be specifically related to a kind of manganese ore material phase analysis
Method.
Background technology
In manganese ore, the material phase analysis of manganese is that research manganese difference composes the method for quantitatively determining depositing valence state or form and relevant reason
Opinion.Manganese is the widest in distributed in nature, it is known that the mineral of manganese there are about kind more than 150, according to manganese existence form and industry in nature
Purposes, generally only requires pyrolusite (MnO2), manganite (Mn2O3·H2O), braunite (Mn2O3), manganese spar (MnCO3) with
And manganous silicate (MnSiO3) carry out material phase analysis.Under certain condition, the row that certain solvent is showed by the compound of these manganese
For being different, so allow the manganese mineral of variform leach one by one, collect respectively, measure containing of every kind of component the most one by one
Amount.Also can be selected for another other components of solvent dissolution, and make to be intended to record a certain component and stay in insoluble sludge, then measure residue
In the content of this component.
Chemical phase analysis is research element existence in various carrier minerals and the method for content thereof, for geology
Prospecting looks for ore deposit, ore-dressing technique research and mineral resource assessment to provide Back ground Information.China's manganese ore material phase analysis does not has skill at present
Art specification, analysis method Main Basis " rock mineral analysis " (4 editions. Beijing: Geology Publishing House, 2011:856-861) provide
Analysis process.But these methods are both for single mineral, a kind of method is not had to can be suitably used for most manganese ore.Example
If it is for the leaching of manganese carbonate phase in manganese oxide ore as leached the leaching agent of manganese carbonate phase, the phenomenon of its string phase will compare
Seriously, the accuracy of manganese carbonate phase result is influenced whether.And according to " ferrum, manganese, chrome ore geological exploration norm " (DZ/T
0200-2002) requirement, as long as manganese thing phase analyzes manganese carbonate, manganese oxide and manganous silicate, and does not has in existing analysis method
To manganese carbonate, manganese oxide and the method for manganous silicate systematic analysis.
Summary of the invention
The invention aims to eliminate above-mentioned the deficiencies in the prior art and shortcoming, a kind of manganese ore material phase analysis is provided
Method, solves in traditional manganese ore Phase Analysis error relatively big, goes here and there problem mutually serious, inefficient.
For reaching above-mentioned technique effect, the present invention adopts the following technical scheme that:
A kind of manganese ore Phase Analysis, employing following steps:
(1) weigh manganese ore, pulverize;
(2) adding aluminum nitrate aqueous solution, leaching in the manganese ore after step (1) is pulverized, filter, collect filtering residue, filtrate measures carbon
Acid manganese ore phase;
(3) adding oxammonium sulfate .-sulfuric acid solution, leaching in the filtering residue that step (2) is collected, filter, collect filtering residue, filtrate measures oxygen
Change manganese ore phase;
(4), after the ashing of step (3) described filtering residue, add the mixed-acid dissolution comprising nitrate acid and hydrofluoric acid-perchloric acid, measure silicic acid
Manganese ore phase.
Preferably, the concentration of the aluminum nitrate solution described in step (1) is 40-80g/L;
Preferably, the temperature of step (2) and step (3) described leaching is 95-100 DEG C;
Preferably, in step (4) described mixed acid, the mol ratio of nitric acid, Fluohydric acid. and perchloric acid is 47:138:12.
Preferably, the concentration of the oxammonium sulfate .-sulfuric acid solution described in step (3) is 30-50g/L;Compound method is for weighing
30-50g oxammonium sulfate. is dissolved in the aqueous sulfuric acid that 1L volume fraction is 1-3%.
Preferably, the addition sequence of the mixed acid described in step (4), for being initially charged nitric acid, after heating 30min, adds height
Chloric acid and Fluohydric acid..
Mixed acid described in step (4) also includes hydrochloric acid;The mol ratio of nitric acid, Fluohydric acid., perchloric acid and hydrochloric acid is 47:
138:12:(60-120).
Preferably, step (2) and the filtration described in step (3) all use chronic quantitative filter paper to filter.
Preferably, the granularity of step (1) described pulverizing is 160-200 mesh.
A kind of manganese ore Phase Analysis, concrete operation method is:
(1) weigh manganese ore, be crushed to 160-200 mesh;
(2) weighing the manganese ore 0.1-0.2g after step (1) is pulverized to be placed in 100mL beaker, adding 50ml concentration is 40-80g/
L aluminum nitrate solution, cap upper surface ware, put in 95-100 DEG C of water-bath, intermittent stirring, water-bath 40-60min, it is cooled to room temperature,
Filtering, collect filtering residue, filtrate measures manganese carbonate ore phase;Preferably, intermittent stirring is to stir once every 10min;
(3) adding 50mL concentration in the filtering residue that step (2) is collected is 30-50g/L oxammonium sulfate .-sulfuric acid solution, cap upper surface ware,
Put in the water-bath of 95-100 DEG C, intermittent stirring, water-bath 20-30min, it is cooled to room temperature, filters, collect filtering residue, filtrate is surveyed
Determine manganese carbonate ore phase;30-50g/L oxammonium sulfate .-sulfuric acid solution compound method is dissolved in 1L volume for weighing 30-50g oxammonium sulfate.
Mark is in the aqueous sulfuric acid of 1-3%;Preferably, intermittent stirring is to stir once every 10min;
(4) filtering residue described in step (3) is put in porcelain crucible, put into Muffle furnace, rise to 700 DEG C of ashing 1h, take out, move into poly-
In tetrafluoroethene crucible, add the hydrochloric acid 9mL, 15.7mol/LHNO of 12.0mol/L3 3mL, heats 30min, adds 11.6mol/
L HClO41mL, 27.6mol/L Fluohydric acid. 5mL, is heated to white cigarette and emits to the greatest extent, add the hydrochloric acid 2mL of 12.0mol/L, go with 10-15ml
Ionized water rinses sidewall of crucible, heating for dissolving, measures silicic acid manganese ore phase.
The present invention establishes a kind of Phase Analysis being applicable to most manganese ore, by more than 8 laboratorys
The common precision coordinated trials participated in, it is determined that analyze repeatability limit and the repeatability limit of method, scientifically have evaluated foundation
The quality level of manganese ore Phase Analysis, for providing with the quality control of laboratory monitoring chemical phase analysis in laboratory
The foundation of science.Manganese ore Phase Analysis accuracy is not evaluated by the present invention first, by rock-mineral determination and not
With the contrast test of method, method of chemical phase analysis is carried out system contrast verification, for lacking the analysis side of standard substance
Method accuracy estimating provides referential technical method and means.
Beneficial effect
(1) the invention provides a kind of accurate, succinct manganese ore Phase Analysis, use aluminum nitrate solution, oxammonium sulfate .-
Manganese carbonate phase in manganese ore, manganese oxide phase are leached mutually by sulfuric acid solution and mixed acid respectively with manganous silicate, are substantially reduced
Leaching process goes here and there the impact of phase, improves precision of analysis, solve in tradition manganese ore Phase Analysis
Error is relatively big, and string is serious mutually, inefficient problem.
(2) present invention establishes a kind of Phase Analysis being applicable to most manganese ore, and first to manganese ore
Phase Analysis correctness is evaluated.
Detailed description of the invention
The present invention is further illustrated with comparative example in conjunction with the embodiments, it should explanation, the description below be only for
The explanation present invention, is not defined its content.
Embodiment 1
(1) the manganese spar 0.1g weighing 160 mesh is placed in 100mL beaker, and wherein Fe content is 21.08%, and addition concentration is 40g/
The aluminum nitrate solution 50mL of L, cap upper surface ware, put in the water-bath boiled, after waiting water again to seethe with excitement, start timing, every 8
Once, (after noticing that the water in water-bath reduces, should add boiling water), water-bath 40min, quantitative filter paper filters at a slow speed for minute stirring
(for preventing from filtering, filter paper pulp to be added on filter paper), collects filtering residue, and filtrate measures manganese carbonate ore phase;
(2) filtering residue described in step (1) is put in former beaker together with filter paper, adds 50mL 30g/L oxammonium sulfate .-1% sulphuric acid molten
Liquid, puts in the water-bath boiled, and after waiting water again to seethe with excitement, starts timing, every stirring in 10 minutes once, and water-bath 20min, slowly
Speed quantitative filter paper filters (for preventing from filtering, filter paper pulp to be added on filter paper), collects filtering residue, and filtrate measures manganese oxide ore phase;30g/L
Oxammonium sulfate .-1% sulfuric acid solution compound method is to weigh 30g oxammonium sulfate. to be dissolved in the aqueous sulfuric acid that 1L volume fraction is 1%;
(3) putting in porcelain crucible by the filtering residue described in step (2) together with filter paper, put into Muffle furnace, low temperature rises to 700 DEG C of ashing
1h, takes out, and moves in politef crucible, adds the hydrochloric acid 9mL, 15.7mol/LHNO of 12.0mol/L3 3mL, heats 30min,
Add 11.6mol/L HClO41mL, 27.6mol/L Fluohydric acid. 5mL is heated to white cigarette and emits to the greatest extent, adds the salt of 12.0mol/L
Acid 2mL, by 10ml deionized water rinsing sidewall of crucible, heating for dissolving, pours mensuration silicic acid manganese ore phase in 50mL color comparison tube.
Embodiment 2
(1) the manganese spar 0.2g weighing 200 mesh is placed in 100mL beaker, and wherein Fe content is 19.77%, and addition concentration is 50g/
The aluminum nitrate solution 50mL of L, cap upper surface ware, put in 95 DEG C of water-baths, after again reaching 95 DEG C etc. water temperature, start timing,
Every stirring in 10 minutes once, (after noticing that the water in water-bath reduces, 95 DEG C of hot water should be added), water-bath 60min, the most quantitatively
Filter paper filtering (for preventing from filtering, filter paper pulp to be added on filter paper), collects filtering residue, and filtrate measures manganese carbonate ore phase;
(2) filtering residue described in step (1) is put in former beaker together with filter paper, adds 50mL 30g/L oxammonium sulfate .-3% sulphuric acid molten
Liquid, puts in 95 DEG C of water-baths, after again reaching 95 DEG C etc. water temperature, starts timing, every stirring in 10 minutes once, and water-bath
30min, quantitative filter paper filters (for preventing from filtering, filter paper pulp to be added on filter paper) at a slow speed, collects filtering residue, and filtrate measures manganese oxide ore
Phase;30g/L oxammonium sulfate .-3% sulfuric acid solution compound method is to weigh 30g oxammonium sulfate. to be dissolved in the sulphuric acid that 1L volume fraction is 3%
In aqueous solution;
(3) putting in porcelain crucible by the filtering residue described in step (2) together with filter paper, put into Muffle furnace, low temperature rises to 650 DEG C of ashing
1h, takes out, and moves in politef crucible, adds the hydrochloric acid 8mL, 15.7mol/LHNO of 12.0mol/L3 3mL, heats 30min,
Add 11.6mol/L HClO41mL, 27.6mol/L Fluohydric acid. 5mL is heated to white cigarette and emits to the greatest extent, adds the salt of 12.0mol/L
Acid 2mL, by 15ml deionized water rinsing sidewall of crucible, heating for dissolving, pours mensuration silicic acid manganese ore phase in 50mL color comparison tube.
Embodiment 3
(1) the manganite 0.1g weighing 150 mesh is placed in 100mL beaker, and wherein Fe content is 46.34%, and addition concentration is 30g/
The aluminum nitrate solution 50mL of L, cap upper surface ware, put in the water-bath boiled, after waiting water again to seethe with excitement, start timing, every
Once, (after noticing that the water in water-bath reduces, should add boiling water), water-bath 70min, quantitative filter paper filters at a slow speed in stirring in 10 minutes
(for preventing from filtering, filter paper pulp to be added on filter paper), collects filtering residue, and filtrate measures manganese carbonate ore phase;
(2) filtering residue described in step (1) is put in former beaker together with filter paper, adds 50mL 50g/L oxammonium sulfate .-3% sulphuric acid molten
Liquid, puts in the water-bath boiled, and after waiting water again to seethe with excitement, starts timing, every stirring in 10 minutes once, and water-bath 30min, slowly
Speed quantitative filter paper filters (for preventing from filtering, filter paper pulp to be added on filter paper), collects filtering residue, and filtrate measures manganese oxide ore phase;50g/L
Oxammonium sulfate .-3% sulfuric acid solution compound method is to weigh 50g oxammonium sulfate. to be dissolved in the aqueous sulfuric acid that 1L volume fraction is 3%;
(3) putting in porcelain crucible by the filtering residue described in step (2) together with filter paper, put into Muffle furnace, low temperature rises to 700 DEG C of ashing
1h, takes out, and moves in politef crucible, adds the hydrochloric acid 9mL, 15.7mol/LHNO of 12.0mol/L3 2mL, heats 30min,
Add 11.6mol/L HClO41mL, 27.6mol/L Fluohydric acid. 5mL is heated to white cigarette and emits to the greatest extent, adds the salt of 12.0mol/L
Acid 2mL, by 15ml deionized water rinsing sidewall of crucible, heating for dissolving, pours mensuration silicic acid manganese ore phase in 50mL color comparison tube.
Embodiment 4
(1) braunite 0.1 gram weighing 210 mesh is placed in 100mL beaker, and wherein Fe content is 45.88%, adds concentration and is
The aluminum nitrate solution 50mL of 90g/L, cap upper surface ware, put in 92 DEG C of water-baths, after again reaching 92 DEG C etc. water temperature, start meter
Time, every stirring in 8 minutes once, (after noticing that the water in water-bath reduces, 92 DEG C of hot water should be added), water-bath 30min, fixed at a slow speed
Amount filter paper filtering (for preventing from filtering, filter paper pulp to be added on filter paper), collects filtering residue, and filtrate measures manganese carbonate ore phase;
(2) filtering residue described in step (1) is put in former beaker together with filter paper, adds 50mL 70g/L oxammonium sulfate .-4% sulphuric acid molten
Liquid, puts in 92 DEG C of water-baths, after again reaching 92 DEG C etc. water temperature, starts timing, every stirring in 10 minutes once, and water-bath
20min, quantitative filter paper filters (for preventing from filtering, filter paper pulp to be added on filter paper) at a slow speed, collects filtering residue, and filtrate measures manganese oxide ore
Phase;
70g/L oxammonium sulfate .-4% sulfuric acid solution compound method is to weigh 70g oxammonium sulfate. to be dissolved in the sulphuric acid that 1L volume fraction is 4%
In aqueous solution;
(3) putting in porcelain crucible by the filtering residue described in step (2) together with filter paper, put into Muffle furnace, low temperature rises to 680 DEG C of ashing
0.6h, takes out, and moves in politef crucible, adds the hydrochloric acid 7mL, 15.7mol/LHNO of 12.0mol/L3 3mL, heating
30min, adds 11.6mol/L HClO41mL, 27.6mol/L Fluohydric acid. 5mL is heated to white cigarette and emits to the greatest extent, adds
The hydrochloric acid 2mL of 12.0mol/L, by 20ml deionized water rinsing sidewall of crucible, heating for dissolving, pours mensuration silicic acid in 50mL color comparison tube
Manganese ore phase.
Embodiment 5
(1) pyrolusite 0.1 gram weighing 180 mesh is placed in 100mL beaker, and wherein Fe content is 54.68%, adds concentration and is
The aluminum nitrate solution 50mL of 60g/L, cap upper surface ware, put in the water-bath boiled, after waiting water again to seethe with excitement, start timing,
Every stirring in 10 minutes once, (after noticing that the water in water-bath reduces, boiling water should be added), water-bath 60min, at a slow speed quantitative filter paper
Filtering (for preventing from filtering, filter paper pulp to be added on filter paper), collect filtering residue, filtrate measures manganese carbonate ore phase;
(2) filtering residue described in step (1) is put in former beaker together with filter paper, adds 50mL 50g/L oxammonium sulfate .-3% sulphuric acid molten
Liquid, puts in the water-bath boiled, and after waiting water again to seethe with excitement, starts timing, every stirring in 10 minutes once, and water-bath 30min, slowly
Speed quantitative filter paper filters (for preventing from filtering, filter paper pulp to be added on filter paper), collects filtering residue, and filtrate measures manganese oxide ore phase;
50g/L oxammonium sulfate .-3% sulfuric acid solution compound method is to weigh 50g oxammonium sulfate. to be dissolved in the sulphuric acid that 1L volume fraction is 3%
In aqueous solution;
(3) putting in porcelain crucible by the filtering residue described in step (2) together with filter paper, put into Muffle furnace, low temperature rises to 700 DEG C of ashing
1h, takes out, and moves in politef crucible, adds the hydrochloric acid 9mL, 15.7mol/LHNO of 12.0mol/L3 3mL, heats 30min,
Add 11.6mol/L HClO41mL, 27.6mol/L Fluohydric acid. 5mL is heated to white cigarette and emits to the greatest extent, adds the salt of 12.0mol/L
Acid 2mL, by 10ml deionized water rinsing sidewall of crucible, heating for dissolving, pours mensuration silicic acid manganese ore phase in 50mL color comparison tube.
Embodiment 6
(1) weighing 160 mesh rhodonite 0.1 gram to be placed in 100mL beaker, wherein Fe content is 25.43%, adds concentration and is
The aluminum nitrate solution 50mL of 50g/L, cap upper surface ware, put in the water-bath boiled, after waiting water again to seethe with excitement, start timing,
Every stirring in 10 minutes once, (after noticing that the water in water-bath reduces, boiling water should be added), water-bath 60min, at a slow speed quantitative filter paper
Filtering (for preventing from filtering, filter paper pulp to be added on filter paper), collect filtering residue, filtrate measures manganese carbonate ore phase;
(2) filtering residue described in step (1) is put in former beaker together with filter paper, adds 50mL 30g/L oxammonium sulfate .-1% sulphuric acid molten
Liquid, puts in the water-bath boiled, and after waiting water again to seethe with excitement, starts timing, every stirring in 10 minutes once, and water-bath 30min, slowly
Speed quantitative filter paper filters (for preventing from filtering, filter paper pulp to be added on filter paper), collects filtering residue, and filtrate measures manganese oxide ore phase;
30g/L oxammonium sulfate .-1% sulfuric acid solution compound method is to weigh 30g oxammonium sulfate. to be dissolved in the sulphuric acid that 1L volume fraction is 1%
In aqueous solution;
(3) putting in porcelain crucible by the filtering residue described in step (2) together with filter paper, put into Muffle furnace, low temperature rises to 700 DEG C of ashing
1h, takes out, and moves in politef crucible, adds the hydrochloric acid 9mL, 15.7mol/LHNO of 12.0mol/L3 3mL, heats 30min,
Add 11.6mol/L HClO41mL, 27.6mol/L Fluohydric acid. 5mL is heated to white cigarette and emits to the greatest extent, adds the salt of 12.0mol/L
Acid 2mL, by 15ml deionized water rinsing sidewall of crucible, heating for dissolving, pours mensuration silicic acid manganese ore phase in 50mL color comparison tube.
Embodiment 7
(1) weighing 180 mesh pyrolusite 0.1 gram to be placed in 100mL beaker, wherein Fe content is 33.72%, and addition concentration is 50g/L
Aluminum nitrate solution 50mL, cap upper surface ware, put in the water-bath boiled, after waiting water again to seethe with excitement, start timing, every 10
Once, (after noticing that the water in water-bath reduces, should add boiling water), water-bath 60min, quantitative filter paper filters at a slow speed for minute stirring
(for preventing from filtering, filter paper pulp to be added on filter paper), collects filtering residue, and filtrate measures manganese carbonate ore phase;
(2) filtering residue described in step (1) is put in former beaker together with filter paper, adds 50mL 40g/L oxammonium sulfate .-2% sulphuric acid molten
Liquid, puts in the water-bath boiled, and after waiting water again to seethe with excitement, starts timing, every stirring in 10 minutes once, and water-bath 30min, slowly
Speed quantitative filter paper filters (for preventing from filtering, filter paper pulp to be added on filter paper), collects filtering residue, and filtrate measures manganese oxide ore phase;
40g/L oxammonium sulfate .-2% sulfuric acid solution compound method is to weigh 40g oxammonium sulfate. to be dissolved in the sulphuric acid that 1L volume fraction is 2%
In aqueous solution;
(3) putting in porcelain crucible by the filtering residue described in step (2) together with filter paper, put into Muffle furnace, low temperature rises to 700 DEG C of ashing
1h, takes out, and moves in politef crucible, adds the hydrochloric acid 9mL, 15.7mol/LHNO of 12.0mol/L3 3mL, heats 30min,
Add 11.6mol/L HClO41mL, 27.6mol/L Fluohydric acid. 5mL is heated to white cigarette and emits to the greatest extent, adds the salt of 12.0mol/L
Acid 2mL, by 15ml deionized water rinsing sidewall of crucible, heating for dissolving, pours mensuration silicic acid manganese ore phase in 50mL color comparison tube.
Comparative example 1
Weighing manganese ore to be placed in 100mL beaker, addition volume fraction is 1%HClO4 40mL, cap upper surface ware, put into and boil
Water-bath in, after waiting water again to seethe with excitement, start timing, every stirring in 10 minutes once, (notice that the water in water-bath reduces
After, boiling water should be added), water-bath 30min;Wherein manganese ore chooses manganese ore used in embodiment 1-7 successively, and remaining operation is with real
Execute example 1.
Comparative example 2
Weighing manganese ore to be placed in 100mL beaker, addition PH is 2, concentration is the (NH of 130g/L4)2SO4Solution 50 mL, covers
Surface plate, puts in 65 DEG C of water-baths, starts timing, every stirring in 10 minutes once, and water-bath 30min;Wherein manganese ore is successively
Choosing manganese ore used in embodiment 1-7, remaining operation is with embodiment 1.
Comparative example 3
Weighing manganese ore to be placed in 100mL beaker, addition PH is 2, concentration is the (NH of 130g/L4)2SO4Solution 25mL, room temperature is stirred
Mix 4h;Wherein manganese ore chooses manganese ore used in embodiment 1-7 successively, and remaining operation is with embodiment 1.
Manganese carbonate ore Within Monominerals leaching experiment analysis in above-described embodiment and comparative example is measured, use atomic absorption method or
Ammonium persulfate. oxidation volumetric determination ferrous ammonium sulfate Fe content, it the results are shown in Table 1:
Table 1 Manganous Carbonate in Manganese Ores phase leaching experiment ω (Mn)/10-2
Aluminum nitrate solution is to other phase leaching rate≤1.2% in addition to manganese carbonate as can be seen from the above table, much lower string item
Impact, be better than existing three kinds of methods.
Comparative example 4
(1) weighing manganese ore to be placed in 100mL beaker, addition concentration is the aluminum nitrate solution 50mL of 50g/L, cap upper surface ware,
Put in the water-bath boiled, after waiting water again to seethe with excitement, start timing, every stirring in 10 minutes once, (note in water-bath
After water reduces, boiling water should be added), water-bath 60min, quantitative filter paper filters (for preventing from filtering, filter paper pulp to be added on filter paper) at a slow speed,
Collecting filtering residue, filtrate measures manganese carbonate ore phase;
(2) filtering residue described in step (1) is put in beaker together with filter paper, and adding 30mL volume fraction is the H of 33%2SO3Room temperature is soaked
Carrying 30min, quantitative filter paper filters at a slow speed, collects filtering residue, and filtrate measures manganese oxide ore phase;
Wherein manganese ore chooses manganese ore used in embodiment 3-7 successively, and remaining operation is with embodiment 1.
Comparative example 5
(1) weigh manganese ore to be placed in 100mL beaker, pulverize, add the aluminum nitrate solution 50mL that concentration is 50g/L, cover table
Face ware, puts in the water-bath boiled, and after waiting water again to seethe with excitement, starts timing, every stirring in 10 minutes once, (notes water-bath
After water in Guo reduces, boiling water should be added), water-bath 60min, quantitative filter paper filtration at a slow speed (for preventing from filtering, filter to be added on filter paper
Paper pulp), collect filtering residue, filtrate measures manganese carbonate ore phase;
(2) filtering residue described in step (1) is put in beaker together with filter paper, adds 1mol/LH2SO430mL, 0.066gKF and 3mL
Fluohydric acid., cap upper surface ware, put into leaching 60min in the water-bath that temperature is 95 DEG C, quantitative filter paper filters (for preventing at a slow speed
Filter, filter paper pulp to be added on filter paper), collect filtering residue, filtrate measures manganese oxide ore phase;
Wherein manganese ore chooses manganese ore used in embodiment 3-7 successively, and remaining operation is with embodiment 1.
Measuring manganese oxide leaching experiment analysis in embodiment 3-7, comparative example 4 and comparative example 5, it the results are shown in Table 2
Manganese oxide phase leaching experiment ω (Mn)/10 in table 2 manganese ore-2
As can be seen from the above table, the 2 kinds of leaching agents provided for " rock mineral analysis " and the oxammonium sulfate .-sulfur of present invention research
Acid solution carries out leaching experiment and compares, oxammonium sulfate .-sulphuric acid leaching rate >=99.5% monomineralic to manganese oxide, is far superior to existing
The 2 kinds of methods having.
Claims (9)
1. a manganese ore Phase Analysis, it is characterised in that employing following steps:
(1) weigh manganese ore, pulverize;
(2) adding aluminum nitrate aqueous solution, leaching in the manganese ore after step (1) is pulverized, filter, collect filtering residue, filtrate measures carbon
Acid manganese ore phase;
(3) adding oxammonium sulfate .-sulfuric acid solution, leaching in the filtering residue that step (2) is collected, filter, collect filtering residue, filtrate measures oxygen
Change manganese ore phase;
(4), after the ashing of step (3) described filtering residue, add the mixed-acid dissolution comprising nitrate acid and hydrofluoric acid-perchloric acid, measure silicic acid
Manganese ore phase.
A kind of manganese ore Phase Analysis the most according to claim 1, it is characterised in that the nitric acid described in step (2)
The concentration of aluminum solutions is 40-80g/L;The temperature of step (2) and step (3) described leaching is 95-100 DEG C;Step (4) is described
In mixed acid, the mol ratio of nitric acid, Fluohydric acid. and perchloric acid is 47:138:12.
A kind of manganese ore Phase Analysis the most according to claim 1, it is characterised in that the sulphuric acid described in step (3)
The concentration of azanol-sulfuric acid solution is 30-50g/L;Compound method is 1-for weigh 30-50g oxammonium sulfate. being dissolved in 1L volume fraction
In the aqueous sulfuric acid of 3%.
A kind of manganese ore Phase Analysis the most according to claim 1, it is characterised in that the mixing described in step (4)
The addition sequence of acid, for being initially charged nitric acid, after heating 30min, adds perchloric acid and Fluohydric acid..
A kind of manganese ore Phase Analysis the most according to claim 1, it is characterised in that the mixing described in step (4)
Acid also includes hydrochloric acid;The mol ratio of nitric acid, Fluohydric acid., perchloric acid and hydrochloric acid is 47:138:12:(60-120).
A kind of manganese ore Phase Analysis the most according to claim 1, it is characterised in that step (2) and step (3) institute
The filtration stated all uses chronic quantitative filter paper to filter.
A kind of manganese ore Phase Analysis the most according to claim 1, it is characterised in that step (1) described pulverizing
Granularity is 160-200 mesh.
8. according to a kind of manganese ore Phase Analysis described in any one of claim 1-7, it is characterised in that concrete operations side
Method is:
(1) weigh manganese ore, be crushed to 160-200 mesh;
(2) weighing the manganese ore 0.1-0.2g after step (1) is pulverized to be placed in 100mL beaker, adding 50ml concentration is 40-80g/
L aluminum nitrate solution, cap upper surface ware, put in 95-100 DEG C of water-bath, intermittent stirring, water-bath 40-60min, it is cooled to room temperature,
Filtering, collect filtering residue, filtrate measures manganese carbonate ore phase;
(3) adding 50mL concentration in the filtering residue that step (2) is collected is 30-50g/L oxammonium sulfate .-sulfuric acid solution, cap upper surface ware,
Put in the water-bath of 95-100 DEG C, intermittent stirring, water-bath 20-30min, it is cooled to room temperature, filters, collect filtering residue, filtrate is surveyed
Determine manganese carbonate ore phase;30-50g/L oxammonium sulfate .-sulfuric acid solution compound method is dissolved in 1L volume for weighing 30-50g oxammonium sulfate.
Mark is in the aqueous sulfuric acid of 1-3%;
(4) filtering residue described in step (3) is put in porcelain crucible, put into Muffle furnace, rise to 700 DEG C of ashing 1h, take out, move into poly-
In tetrafluoroethene crucible, add the hydrochloric acid 9mL, 15.7mol/LHNO of 12.0mol/L3 3mL, heats 30min, adds 11.6mol/
L HClO41mL, 27.6mol/L Fluohydric acid. 5mL, is heated to white cigarette and emits to the greatest extent, add the hydrochloric acid 2mL of 12.0mol/L, go with 10-15ml
Ionized water rinses sidewall of crucible, heating for dissolving, measures silicic acid manganese ore phase.
A kind of manganese ore Phase Analysis the most according to claim 8, it is characterised in that step (2) and step (3) institute
The intermittent stirring stated is for stirring once every 10min.
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CN106370510A (en) * | 2016-10-21 | 2017-02-01 | 天津大学 | Method for microwave digestion of glass body |
CN108020857A (en) * | 2016-11-03 | 2018-05-11 | 中国辐射防护研究院 | A kind of method that polonium leaches in aerosol |
WO2019167841A1 (en) * | 2018-03-01 | 2019-09-06 | Jfeスチール株式会社 | Method for manufacturing manganese raw material and method for smelting manganese-containing steel |
CN110286154A (en) * | 2019-07-23 | 2019-09-27 | 长安大学 | A kind of method of complete resolution manganese ore sample |
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CN106370510A (en) * | 2016-10-21 | 2017-02-01 | 天津大学 | Method for microwave digestion of glass body |
CN108020857A (en) * | 2016-11-03 | 2018-05-11 | 中国辐射防护研究院 | A kind of method that polonium leaches in aerosol |
WO2019167841A1 (en) * | 2018-03-01 | 2019-09-06 | Jfeスチール株式会社 | Method for manufacturing manganese raw material and method for smelting manganese-containing steel |
KR20200112947A (en) * | 2018-03-01 | 2020-10-05 | 제이에프이 스틸 가부시키가이샤 | Manufacturing method of manganese raw material and solvent method of manganese-containing steel |
KR102449547B1 (en) | 2018-03-01 | 2022-09-29 | 제이에프이 스틸 가부시키가이샤 | Manufacturing method of manganese raw material and melting method of manganese-containing steel |
CN110286154A (en) * | 2019-07-23 | 2019-09-27 | 长安大学 | A kind of method of complete resolution manganese ore sample |
CN110286154B (en) * | 2019-07-23 | 2021-08-17 | 长安大学 | Method for completely digesting manganese ore sample for element analysis |
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