CN113406266B - Chemical analysis method for copper phase in copper concentrate - Google Patents
Chemical analysis method for copper phase in copper concentrate Download PDFInfo
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- CN113406266B CN113406266B CN202110720121.3A CN202110720121A CN113406266B CN 113406266 B CN113406266 B CN 113406266B CN 202110720121 A CN202110720121 A CN 202110720121A CN 113406266 B CN113406266 B CN 113406266B
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- 239000010949 copper Substances 0.000 title claims abstract description 192
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 192
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 190
- 239000012141 concentrate Substances 0.000 title claims abstract description 61
- 238000009614 chemical analysis method Methods 0.000 title abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 55
- OMZSGWSJDCOLKM-UHFFFAOYSA-N copper(II) sulfide Chemical compound [S-2].[Cu+2] OMZSGWSJDCOLKM-UHFFFAOYSA-N 0.000 claims abstract description 35
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 31
- 238000010438 heat treatment Methods 0.000 claims abstract description 27
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000005751 Copper oxide Substances 0.000 claims abstract description 23
- 229910000431 copper oxide Inorganic materials 0.000 claims abstract description 23
- 239000000126 substance Substances 0.000 claims abstract description 22
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000010521 absorption reaction Methods 0.000 claims abstract description 18
- 238000004458 analytical method Methods 0.000 claims abstract description 14
- 229910052742 iron Inorganic materials 0.000 claims abstract description 10
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 238000004448 titration Methods 0.000 claims abstract description 8
- 230000000873 masking effect Effects 0.000 claims abstract description 5
- 238000001704 evaporation Methods 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 22
- 239000000706 filtrate Substances 0.000 claims description 13
- 235000010323 ascorbic acid Nutrition 0.000 claims description 11
- 229960005070 ascorbic acid Drugs 0.000 claims description 11
- 239000011668 ascorbic acid Substances 0.000 claims description 11
- 239000012153 distilled water Substances 0.000 claims description 11
- 239000011521 glass Substances 0.000 claims description 11
- 239000011734 sodium Substances 0.000 claims description 11
- 238000002835 absorbance Methods 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 7
- 239000000779 smoke Substances 0.000 claims description 7
- WTDHULULXKLSOZ-UHFFFAOYSA-N Hydroxylamine hydrochloride Chemical compound Cl.ON WTDHULULXKLSOZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 5
- 150000001879 copper Chemical class 0.000 claims description 4
- 238000009736 wetting Methods 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 2
- FGGPAWQCCGEWTJ-UHFFFAOYSA-M sodium;2,3-bis(sulfanyl)propane-1-sulfonate Chemical compound [Na+].[O-]S(=O)(=O)CC(S)CS FGGPAWQCCGEWTJ-UHFFFAOYSA-M 0.000 claims description 2
- 238000010025 steaming Methods 0.000 claims description 2
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Chemical compound BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 abstract description 9
- 231100000419 toxicity Toxicity 0.000 abstract description 4
- 230000001988 toxicity Effects 0.000 abstract description 4
- 238000004846 x-ray emission Methods 0.000 description 14
- 239000011630 iodine Substances 0.000 description 12
- 229910052740 iodine Inorganic materials 0.000 description 12
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 description 12
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 10
- 238000002441 X-ray diffraction Methods 0.000 description 10
- -1 digenite Inorganic materials 0.000 description 8
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 7
- 229910052951 chalcopyrite Inorganic materials 0.000 description 6
- DVRDHUBQLOKMHZ-UHFFFAOYSA-N chalcopyrite Chemical compound [S-2].[S-2].[Fe+2].[Cu+2] DVRDHUBQLOKMHZ-UHFFFAOYSA-N 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- GBRBMTNGQBKBQE-UHFFFAOYSA-L copper;diiodide Chemical compound I[Cu]I GBRBMTNGQBKBQE-UHFFFAOYSA-L 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 5
- MIMUSZHMZBJBPO-UHFFFAOYSA-N 6-methoxy-8-nitroquinoline Chemical class N1=CC=CC2=CC(OC)=CC([N+]([O-])=O)=C21 MIMUSZHMZBJBPO-UHFFFAOYSA-N 0.000 description 4
- 229920002472 Starch Polymers 0.000 description 4
- 229910052948 bornite Inorganic materials 0.000 description 4
- 229910052927 chalcanthite Inorganic materials 0.000 description 4
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 description 4
- LBJNMUFDOHXDFG-UHFFFAOYSA-N copper;hydrate Chemical compound O.[Cu].[Cu] LBJNMUFDOHXDFG-UHFFFAOYSA-N 0.000 description 4
- 229910052955 covellite Inorganic materials 0.000 description 4
- 238000007865 diluting Methods 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- 238000011084 recovery Methods 0.000 description 4
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 description 4
- 235000019345 sodium thiosulphate Nutrition 0.000 description 4
- 239000002910 solid waste Substances 0.000 description 4
- 235000019698 starch Nutrition 0.000 description 4
- 239000008107 starch Substances 0.000 description 4
- 238000003723 Smelting Methods 0.000 description 3
- 229910052947 chalcocite Inorganic materials 0.000 description 3
- 229910001779 copper mineral Inorganic materials 0.000 description 3
- 230000008676 import Effects 0.000 description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
- 238000002386 leaching Methods 0.000 description 3
- 239000011707 mineral Substances 0.000 description 3
- 238000004451 qualitative analysis Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000012086 standard solution Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 229910017665 NH4HF2 Inorganic materials 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- ZMZDMBWJUHKJPS-UHFFFAOYSA-M Thiocyanate anion Chemical compound [S-]C#N ZMZDMBWJUHKJPS-UHFFFAOYSA-M 0.000 description 2
- 238000001479 atomic absorption spectroscopy Methods 0.000 description 2
- ALSPKRWQCLSJLV-UHFFFAOYSA-N azanium;acetic acid;acetate Chemical compound [NH4+].CC(O)=O.CC([O-])=O ALSPKRWQCLSJLV-UHFFFAOYSA-N 0.000 description 2
- 239000007853 buffer solution Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 229910001431 copper ion Inorganic materials 0.000 description 2
- BWFPGXWASODCHM-UHFFFAOYSA-N copper monosulfide Chemical compound [Cu]=S BWFPGXWASODCHM-UHFFFAOYSA-N 0.000 description 2
- 229910000365 copper sulfate Inorganic materials 0.000 description 2
- PDZKZMQQDCHTNF-UHFFFAOYSA-M copper(1+);thiocyanate Chemical compound [Cu+].[S-]C#N PDZKZMQQDCHTNF-UHFFFAOYSA-M 0.000 description 2
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 2
- BQVVSSAWECGTRN-UHFFFAOYSA-L copper;dithiocyanate Chemical compound [Cu+2].[S-]C#N.[S-]C#N BQVVSSAWECGTRN-UHFFFAOYSA-L 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- ZMZDMBWJUHKJPS-UHFFFAOYSA-N hydrogen thiocyanate Natural products SC#N ZMZDMBWJUHKJPS-UHFFFAOYSA-N 0.000 description 2
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 2
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 description 2
- 229910000360 iron(III) sulfate Inorganic materials 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000005192 partition Methods 0.000 description 2
- ZNNZYHKDIALBAK-UHFFFAOYSA-M potassium thiocyanate Chemical compound [K+].[S-]C#N ZNNZYHKDIALBAK-UHFFFAOYSA-M 0.000 description 2
- 229940116357 potassium thiocyanate Drugs 0.000 description 2
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- 241000123346 Chrysosporium Species 0.000 description 1
- 229910000570 Cupronickel Inorganic materials 0.000 description 1
- 241000784732 Lycaena phlaeas Species 0.000 description 1
- 241000907663 Siproeta stelenes Species 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 229910052599 brucite Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- RYTYSMSQNNBZDP-UHFFFAOYSA-N cobalt copper Chemical compound [Co].[Cu] RYTYSMSQNNBZDP-UHFFFAOYSA-N 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- YOCUPQPZWBBYIX-UHFFFAOYSA-N copper nickel Chemical compound [Ni].[Cu] YOCUPQPZWBBYIX-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910052971 enargite Inorganic materials 0.000 description 1
- 238000005188 flotation Methods 0.000 description 1
- 238000001506 fluorescence spectroscopy Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- SURQXAFEQWPFPV-UHFFFAOYSA-L iron(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Fe+2].[O-]S([O-])(=O)=O SURQXAFEQWPFPV-UHFFFAOYSA-L 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 238000013332 literature search Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 229910052603 melanterite Inorganic materials 0.000 description 1
- 210000004877 mucosa Anatomy 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- LUARRPSPRYCMOT-UHFFFAOYSA-N propane-1,2-dithiol;sodium Chemical compound [Na].CC(S)CS LUARRPSPRYCMOT-UHFFFAOYSA-N 0.000 description 1
- 229910052683 pyrite Inorganic materials 0.000 description 1
- NIFIFKQPDTWWGU-UHFFFAOYSA-N pyrite Chemical compound [Fe+2].[S-][S-] NIFIFKQPDTWWGU-UHFFFAOYSA-N 0.000 description 1
- 239000011028 pyrite Substances 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 210000002345 respiratory system Anatomy 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- WGPCGCOKHWGKJJ-UHFFFAOYSA-N sulfanylidenezinc Chemical compound [Zn]=S WGPCGCOKHWGKJJ-UHFFFAOYSA-N 0.000 description 1
- 150000004763 sulfides Chemical class 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 229910052970 tennantite Inorganic materials 0.000 description 1
- 229910052969 tetrahedrite Inorganic materials 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 229910052984 zinc sulfide Inorganic materials 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
- G01N31/162—Determining the equivalent point by means of a discontinuity
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
- G01N21/79—Photometric titration
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- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/207—Diffractometry using detectors, e.g. using a probe in a central position and one or more displaceable detectors in circumferential positions
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/223—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
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Abstract
The invention discloses a chemical analysis method for copper phases in copper concentrate, belonging to the field of chemical analysis. The method comprises the following steps: s1, separating the water-soluble copper in the copper concentrate to be detected, and determining the content of the water-soluble copper by adopting an atomic absorption method; s2, separating the copper oxide in the filter residue A obtained in the step S1, and determining the content of the copper oxide by adopting an atomic absorption method; s3, separating the native copper in the filter residue B obtained in the step S2, and determining the content of the native copper by adopting an atomic absorption method; s4, separating the copper sulfide in the filter residue C obtained in the step S3, and determining the content of the copper sulfide by adopting a titration method; wherein the step of separating copper sulfide in the step of S4 includes: firstly, heating and dissolving the filter residue C by using dilute nitric acid, then adding dilute sulfuric acid to continue heating and decomposing, then evaporating the solution to dryness, adding dilute sulfuric acid to heat and dissolve to obtain a mixture of copper and iron, then masking iron and determining the content of copper sulfide by using a titration method. The method avoids the use of liquid bromine with strong toxicity, and the determination process is safer.
Description
Technical Field
The invention belongs to the field of chemical analysis, and particularly relates to a chemical analysis method for a copper phase in copper concentrate.
Background
Copper is an important strategic resource, with an average content of 1 × 10 in the crust-2Copper is a typical thiophilic element, and the primary minerals of the copper are almost all sulfides, so that single hydrothermal deposits and skarn-type deposits of various types can be formed, magma-type copper-nickel or cobalt-copper deposits can be formed together with nickel and cobalt, and copper-containing polymetallic deposits can be formed together with lead and zinc. There are more than 200 kinds of copper minerals found in nature, and there are more than ten kinds of common copper minerals, mainlyThe copper minerals include chalcopyrite, bornite, chalcocite, digenite, covellite, tetrahedrite, tennantite, enargite, malachite, chalcocite, cuprite, melanterite, chrysosporium, native copper, chalcanthite, etc., which are formed in different geological environments of copper ore beds with different causes and constitute various types of copper ores.
For many years, copper ore is listed as an urgent demand and shortage mineral of mineral resources in China, and a large amount of import is needed every year. The imported copper ore in China is generally copper concentrate which is subjected to flotation in foreign mines and has higher grade, the copper concentrate is an important resource commodity in imported raw materials in China, in 2020, the imported copper concentrate at various ports in China is about 2200 ten thousand tons, and the copper concentrate is generally bulk cargo and is free of package, so that the influence on the environment is great. The total copper content of the imported copper concentrate is determined by chemical analysis method GB/T3884.1 (determination of copper content: iodometry) for tax-related assays and trade settlement, and this occurs when the imported copper concentrate is contaminated with solid waste "blending-off". Whereas for the solid waste "mix-off" case, the identification of the doping of the imported copper concentrate is required, the traditionally used method is X-ray fluorescence spectroscopy (XRF) combined with X-ray diffraction (XRD). The XRF combined with XRD method is only qualitative but not accurate quantitative for various copper phases in imported copper concentrate.
For the reasons mentioned above, at present, the inspection and identification work of imported copper concentrate includes quantitative determination of total copper content and qualitative analysis of main copper phase, and there is no method for quantitative analysis of main copper phase in imported copper concentrate. According to literature search, a small amount of chemical analysis methods for copper phases in copper ores exist at present, while the imported copper concentrate and the original copper ore have certain difference in the composition of the copper phases, and the situation that water-soluble copper possibly exists in the imported copper concentrate needs to develop a method for separating and measuring the main copper phases in the imported copper concentrate.
In addition, the national standard GB/T3884.1-2012 describes the use of iodometry to measure the total copper content, wherein, in the treatment of the sample, the method of adding liquid bromine is used to assist the dissolution of copper, but liquid bromine is easy to volatilize, and at normal temperature, it can volatilize smoke with strong irritation, irritate the mucosa of eyes and respiratory tract, burn skin, and have strong toxicity and corrosiveness to the human body. Therefore, a non-toxic and harmless way for replacing liquid bromine is urgently needed in the chemical analysis of copper phases in copper concentrates.
Disclosure of Invention
1. Problems to be solved
The invention aims to provide a set of sequential extraction and measurement methods for different copper phases contained in imported copper concentrates. The establishment of the method not only has good guiding significance for copper concentrate smelting enterprises in the aspects of raw material purchase, use, proportion and the like, but also can effectively judge the condition that imported copper concentrate is doped with solid wastes, thereby achieving the purpose of protecting the ecological environment.
Aiming at the problem that liquid bromine is adopted to dissolve out copper sulfide in the existing national standard, the invention provides a chemical analysis method for copper phases in copper concentrate, which adopts the combination of dilute nitric acid and dilute sulfuric acid, avoids the adoption of liquid bromine with strong toxicity, and ensures the safer determination process.
The invention also aims to solve the problem that the existing method for leaching the water-soluble copper by using pure water cannot accurately measure the content of the water-soluble copper due to iron ions, and the ascorbic acid and Na are adopted2S2O3The technical scheme of dissolving out the water-soluble copper under the alkalescent condition can effectively avoid the influence of iron ions on the water-soluble copper.
2. Technical scheme
In order to solve the problems, the technical scheme adopted by the invention is as follows:
a method for chemical analysis of copper phases in copper concentrates, comprising the steps of:
S1, separating the water-soluble copper in the copper concentrate to be detected, and determining the content of the water-soluble copper by adopting an atomic absorption method;
s2, separating the copper oxide in the filter residue A obtained in the step S1, and determining the content of the copper oxide by adopting an atomic absorption method;
s3, separating the native copper in the filter residue B obtained in the step S2, and determining the content of the native copper by adopting an atomic absorption method;
s4, separating the copper sulfide in the filter residue C obtained in the step S3, and determining the content of the copper sulfide by adopting a titration method;
wherein the step of separating copper sulfide in the step of S4 includes:
firstly, heating and dissolving the filter residue C by using dilute nitric acid, then adding dilute sulfuric acid to continue heating and decomposing, then evaporating the solution to dryness, adding dilute sulfuric acid to heat and dissolve to obtain a mixture of copper and iron, then masking iron and determining the content of copper sulfide by using a titration method.
Preferably, the step of separating copper sulfide in the step of S4 includes:
putting the filter residue in a cone-shaped beaker, wetting the filter residue with a small amount of distilled water, adding 20 ml of dilute nitric acid (50%), covering a watch glass, heating the watch glass for 10 minutes at 180 +/-5 ℃, adding 20 ml of dilute sulfuric acid (50%), continuously heating to decompose a sample, cleaning the watch glass with a small amount of water after a violent reaction stops (about 1-2 hours), continuously heating at a high temperature (about 300 ℃) until dense white smoke is emitted, taking the watch glass down after the dense white smoke is completely dispersed, and cooling. The wall of the flask was washed with a small amount of distilled water and then heated to near dryness. Adding 10 mL of 0.5% dilute sulfuric acid, heating to dissolve soluble salt, adding 30mL of distilled water, heating to slightly boil to completely dissolve, taking down and cooling to room temperature to completely dissolve the generated copper salt.
Preferably, the method for separating water-soluble copper in step S1 includes: using ascorbic acid and Na2S2O3And dissolving out the water-soluble copper under the alkalescent condition.
Further preferably, the weak alkaline condition is pH 7.5-8.5.
Preferably, the method for separating water-soluble copper in step S1 specifically includes: preparing ascorbic acid and Na2S2O3And adjusting the pH value to 8, adding a sample to be detected into the mixed solution, stirring, and filtering to obtain a filtrate sample 1 containing water-soluble copper.
Further preferably, the method for separating water-soluble copper in step S1 specifically includes: what is neededAscorbic acid and Na2S2O3The mixed solution of (1) is prepared by adding 1g Na into 50ml 2.5% ascorbic acid solution2S2O3。
Preferably, the method for separating copper oxide in step S2 specifically includes: adding the filter residue obtained in the step S1 into a mixture of 50mL of 3% ethylenediamine solution, 0.125g of sodium 2, 3-dimercaptopropane sulfonate and 1.5g of NH4Cl and 2gNa2SO3The prepared mixed solution is leached for 30min at 37 ℃ and then filtered to obtain a filtrate sample 2.
Preferably, the method for separating native copper in step S3 specifically includes: adding the filter residue obtained in the step S2 into a mixture of 50mL of 30g/L hydroxylamine hydrochloride and 20g/LHgCl2-ethanol solution for 30min and filtering to obtain filtrate sample 3.
Preferably, before step S1, the elements in the sample to be tested are first qualitatively analyzed by X-ray fluorescence spectroscopy (XRF).
Preferably, before step S1, the copper phase in the sample to be tested is first qualitatively analyzed by X-ray diffraction (XRD) according to the XRF qualitative result, so as to obtain the categories of water-soluble copper, copper oxide, native copper and copper sulfide in the sample to be tested.
Preferably, an air-acetylene flame is used to plot the operating curve at an atomic absorption spectrometer wavelength of 324.7nm with copper concentration on the abscissa and absorbance on the ordinate.
Preferably, the absorbance of the solution to be detected of the samples 1, 2 and 3 is measured at the wavelength of 324.7nm of the atomic absorption spectrometer, and the content of the water-soluble copper, the copper oxide and the native copper is calculated.
3. Advantageous effects
Compared with the prior art, the invention has the beneficial effects that:
(1) aiming at the fact that no method for respectively measuring different phases in copper concentrate exists in the prior art, the method adopts a step-by-step extraction method to obtain the copper of phases of water-soluble copper, copper oxide, native copper and copper sulfide in the copper concentrate, and measures the copper content of various phases; in addition, aiming at the copper sulfide phase in the copper concentrate, dilute nitric acid and dilute sulfuric acid are used in a matched mode to dissolve out copper in the copper sulfide phase, so that liquid bromine with strong toxicity in the national standard GB/T3884.1-2012 is avoided, and the determination process is safer;
(2) In the prior art, the water-soluble copper phase in the copper concentrate is only leached by distilled water at room temperature or under the heating condition, but the treatment method has the following problems: firstly, zinc blende exists in part of imported copper concentrate, and CuS precipitate is generated when the imported copper concentrate is immersed in water, so that the determination of water-soluble copper is low; secondly, the imported copper concentrate usually contains ferric sulfate, and the ferric sulfate and the water-soluble copper enter a solution together to cause partial dissolution of copper sulfide, so that the determination of the water-soluble copper is higher; therefore, it is difficult to obtain accurate measurement results simply by immersing the water-soluble copper with distilled water at room temperature or under heating; the invention adopts ascorbic acid and Na2S2O3Dissolving out water soluble copper under alkalescent condition, forming a complex with iron by ascorbic acid, and passing Na2S2O3Copper is dissolved out, so that the problem of inaccurate measurement of the water-soluble copper caused by the interference of iron ions is effectively avoided;
(3) according to the method, through chemical solution pretreatment, water-soluble copper, copper oxide and native copper are leached out respectively, an atomic absorption spectrometer is used for accurately measuring, and the pretreated filter residue is dissolved and titrated to obtain an accurate value; the establishment of the method can improve the current situation that the main copper phase in the imported copper concentrate cannot be quantified at present, has good guiding significance for copper concentrate smelting enterprises in the aspects of raw material purchase, use, proportion and the like, and can also effectively judge the condition of doping solid wastes in the imported copper concentrate, thereby achieving the purpose of protecting the ecological environment.
(4) The method judges the category of the main copper phase in the sample in advance by combining X-ray fluorescence spectrometry (XRF) with X-ray diffraction (XRD) according to the chemical analysis method of the copper phase in the imported copper concentrate, and reasonably draws up the experimental process.
Drawings
FIG. 1 is a flowchart of an experiment in example 1 of the present invention;
FIG. 2 is the XRF pattern of the copper concentrate of example 2;
FIG. 3 is the XRD pattern of the copper concentrate of example 2; (Ccp: chalcopyrite; Bn: bornite; Cv: covellite; Clt: chalcanthite; Py: pyrite; Q: quartz)
Figure 4 is the XRF pattern of the copper concentrate of example 3;
figure 5 is the XRD pattern of copper concentrate in example 3.
Detailed Description
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs; as used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The invention is further described with reference to specific examples.
Example 1
According to the earlier stage experimental results and the significance of various copper phases in relative smelting and customs supervision, the various copper phases in the imported copper concentrate can be divided into four main classes, namely water-soluble copper (mainly chalcanthite and brucite), copper oxide (mainly cuprite and chalcopyrite), native copper and copper sulfide (mainly chalcopyrite, bornite, chalcocite and copper blue). The chemical analysis method for the copper phase in the copper concentrate mainly comprises the following experimental steps:
1. after a representative sample is adopted according to the specification, uniformly mixing, dividing and grinding the sample, and sieving the sample with a 150-mesh sieve to obtain a sample to be detected;
2. carrying out qualitative analysis on elements in a sample to be detected by utilizing an X fluorescence spectrometry (XRF);
3. carrying out qualitative analysis on the copper phase in the sample to be detected by utilizing an X-ray diffraction method (XRD) and according to the XRF qualitative result to obtain the categories of water-soluble copper, copper oxide, native copper and copper sulfide in the sample to be detected;
4. drawing up an experimental flow according to the categories obtained by the analysis, and sequentially measuring the water-soluble copper, the copper oxide, the native copper and the copper sulfide as shown in figure 1;
5. determination of water-soluble copper: preparing 50 mL2.5% ascorbic acid solution, adding 1gNa2S2O3Adjusting the pH value to 8, accurately weighing 10g of a sample to be detected, adding the sample to the solution, stirring for 10min, filtering, transferring the filtrate into a 200mL volumetric flask, diluting the filtrate to a scale with water, uniformly mixing, standing for 2h, marking a sample 1, and washing filter residue A for later use;
6. Determination of copper oxide: 50mL of 3% ethylenediamine solution was prepared, and 0.125g of 2, 3-dimercaptopropane sodium sulfonate and 1.5g of NH were added4Cl and 2gNa2SO3Adding the filter residue A into the solution, leaching for 30min at 37 ℃, filtering, transferring the filtrate into a 200mL volumetric flask, diluting to a scale with water, mixing uniformly, standing for 2h, marking a sample 2, and washing the filter residue B for later use;
7. determination of native copper: 50mL of 30g/L hydroxylamine hydrochloride and 20g/LHgCl were prepared2-ethanol solution, adding the filter residue B, continuously leaching for 30min, filtering, transferring the filtrate into a 200mL volumetric flask, diluting with water to a scale, uniformly mixing, standing for 2h, marking a sample 3, and washing the filter residue C for later use;
8. determination of copper sulfide: placing the filter residue C in a 300 ml conical beaker, wetting the filter residue C with a small amount of distilled water, and adding 20 ml of 50% dilute nitric acid (dissolving copper sulfide phases CuS + FeS + HNO)3→Cu2++Fe2++NO3 -) Covering the surface dish, heating at about 180 deg.C (180 + -5 deg.C) for 10 min, and adding 20 ml of 50% dilute sulfuric acid (capable of dissolving copper sulfide phase completely into Cu2++Fe2++NO3 -+H2SO4→Cu2++Fe3++SO4 2-) And continuously heating to decompose the sample, after the violent reaction is stopped (about 1-2 hours), cleaning and removing the surface dish by using a small amount of water, continuously heating at a high temperature (about 300 ℃) until dense white smoke is emitted (sulfur and nitrogen are removed), taking down the sample after the dense white smoke is completely dispersed, and cooling. The wall of the flask was washed with a small amount of distilled water and then heated to near dryness (to make the resulting copper salt non-stick to the wall). Adding 10 mL of 0.5% dilute sulfuric acid, heating to dissolve soluble salt, adding 30mL of distilled water, and heating to Slightly boiling to completely dissolve, taking down and cooling to room temperature to completely dissolve the generated copper salt;
an appropriate amount of acetic acid-ammonium acetate buffer solution was added until the solution became no longer reddish and 3 ml in excess (the solution was adjusted to pH 3-4). Adding a proper amount of saturated ammonium bifluoride solution until the red color fades, and adding 1 ml of saturated ammonium bifluoride solution (masking Fe)3++NH4HF2→(FeF6)3-). Adding about 3g of excessive potassium iodide powder (the excessive potassium iodide powder causes copper iodide and iodine ions to generate copper iodide precipitate and elemental iodine Cu2++I-→CuI+I2) After the solution turns brown, the solution is immediately titrated to light yellow by a sodium thiosulfate standard solution (sodium thiosulfate reacts with iodine elementary substance, the iodine elementary substance is gradually reduced, and the solution becomes light I2+S2O3 2-→I-+S4O6 2-) Adding 5 ml of starch solution (starch turns blue when meeting iodine, and checking whether the iodine elementary substance completely reacts), continuing to titrate until the blue color basically disappears, and then adding 5 ml of potassium thiocyanate (100g/L) (thiocyanate and copper iodide react to form more insoluble copper thiocyanate and iodine elementary substance, so that the wrapped copper ions are further precipitated to completely precipitate CuI + SCN-→CuSCN+I2) And continuously titrating until blue just disappears, namely, the end point is obtained, and calculating to obtain the copper sulfide.
9. Preparing a copper standard curve: transferring 0mL, 1.00 mL, 2.00 mL, 3.00 mL, 4.00 mL and 5.00mL of copper standard solution, respectively placing in a set of 200mL volumetric flasks, adding 1.0mL of sulfuric acid, diluting with water to scale, and uniformly mixing;
10. Drawing a working curve: using air-acetylene flame, adjusting the wavelength of an atomic absorption spectrometer to 324.7nm by water to zero, measuring the absorbance of the solution, subtracting the absorbance of the solution with zero concentration, and drawing a working curve by taking the concentration of copper as an abscissa and the absorbance as an ordinate;
11. determination of samples 1 to 3: and (3) measuring the absorbance of the solution to be measured of the samples 1-3 at the wavelength of 324.7nm of an atomic absorption spectrometer by using air-acetylene flame, and calculating to obtain the content of the water-soluble copper, the copper oxide and the native copper.
Example 2
An import copper concentrate sample is processed according to the experimental procedure in example 1 to obtain XRF and XRD patterns as shown in fig. 2 and fig. 3, which show that the import copper concentrate sample contains phases of chalcanthite (water soluble copper), cuprite (copper oxide), chalcopyrite and bornite (copper sulfide), and the content of native copper is low and is not clearly shown in the patterns.
The contents of the water-soluble copper, the copper oxide and the native copper measured by adopting an atomic absorption spectrometry are respectively as follows: 6.05% (allocated, i.e. 25.74% of the total copper content), 0.15% (allocated 0.64%), 0.08% (allocated 0.34%); the copper sulphide content was determined by titration to be 17.20% (partition 73.28%) and the total copper content was 23.48%.
Copper sulfate and copper sulfide are artificially added into the imported copper concentrate, a standard addition recovery experiment is carried out, the recovery rate is 90-110%, and the accuracy of the method can be verified.
Comparative example A
Aiming at the same batch of copper concentrate samples to be tested which are sieved by a 150-mesh sieve in the embodiment 2; the total copper content was determined using the liquid bromine method described in the national standard GB/T3884.1-2012, namely:
determination of total copper: putting the filter residue in a 500mL triangular beaker, wetting the filter residue with a small amount of water, adding 10mL hydrochloric acid, putting the beaker on an electric hot plate, heating the beaker at a low temperature for 5min, taking the beaker down for cooling slightly, adding 5mL nitric acid and 1mL bromine, covering a watch glass, mixing the cells uniformly, heating the beaker at a low temperature of about 60 ℃, taking the beaker down for cooling slightly after a sample is completely decomposed, washing the watch glass with a small amount of water, continuously heating and steaming the beaker until the sample is nearly dry, and cooling the beaker. An appropriate amount of acetic acid-ammonium acetate buffer solution was added until the red color of the solution did not deepen, and 3 ml of excess was added (the acidity of the solution was adjusted to pH 3-4). Adding a proper amount of saturated ammonium bifluoride solution until the red color fades, and adding 1ml of saturated ammonium bifluoride solution (masking Fe)3++NH4HF2→(FeF6 )3-). Adding about 3g of potassium iodide powder in excess (the excess potassium iodide powder causes copper iodide ions and iodine ions to generate copper iodide precipitate and elementary iodine Cu2++I-→CuI+I2) The solution turns brown and is immediately titrated to light yellow by a sodium thiosulfate standard solution (sodium thiosulfate reacts with iodine simple substance, the iodine simple substance is gradually reduced, and the solution becomes light I 2+S2O3 2-→I-+S4O6 2-) Adding 5 ml of starch solution (starch turns blue when meeting iodine, and detecting whether iodine elementary substance completely reacts or not), continuously titrating until blue basically disappears, adding 5 ml of potassium thiocyanate (100g/L) (thiocyanate and copper iodide react to form more insoluble copper thiocyanate and iodine elementary substance, and further precipitating the wrapped copper ions completely by CuI + SCN-→CuSCN+I2) And continuously titrating until blue just disappears, namely, the end point is obtained, and calculating to obtain the copper sulfide.
With this method, the total copper content was found to be 23.56%.
And (4) conclusion: the method of the national standard only measures the total content of copper element in imported copper concentrate by adopting an acid-soluble pretreatment method, but the method utilizes a plurality of reagents to leach out water-soluble copper, copper oxide and native copper, and measures copper sulfide by an improved method to obtain the content of each phase in the imported copper concentrate, rather than the content of the copper element.
Example 3
Another batch of the imported copper concentrate was processed according to the experimental procedure of example 1 to obtain XRF and XRD patterns as shown in fig. 4 and 5, which revealed that the imported copper concentrate sample contained phases of cuprite (copper oxide) and chalcopyrite (copper sulfide), and the content of water-soluble copper was low and not clearly shown in the patterns.
The contents of the water-soluble copper, the copper oxide and the native copper are respectively measured by adopting an atomic absorption spectrometry: 0.008% (0.03% dispensed), 0.026% (0.10% dispensed), 0% (0% dispensed); the copper sulphide content was determined by titration to be 26.30% (partition 99.87%).
Copper sulfate and copper sulfide are artificially added into the imported copper concentrate, a standard addition recovery experiment is carried out, the recovery rate is 90-110%, and the accuracy of the method can be verified.
The above description is illustrative of the present invention and its embodiments, and is not to be construed as limiting, and the embodiments shown in the examples are only one embodiment of the present invention, and the actual embodiments are not limited thereto. Therefore, if the person skilled in the art receives the teaching, the embodiment and the embodiment similar to the technical solution should be designed without creativity without departing from the spirit of the invention, and shall fall within the protection scope of the invention.
Claims (9)
1. A method for chemical analysis of copper phases in copper concentrates, characterized by comprising the steps of:
s1, separating the water-soluble copper in the copper concentrate to be detected, and determining the content of the water-soluble copper by adopting an atomic absorption method;
s2, separating the copper oxide in the filter residue A obtained in the step S1, and determining the content of the copper oxide by adopting an atomic absorption method;
S3, separating the native copper in the filter residue B obtained in the step S2, and determining the content of the native copper by adopting an atomic absorption method;
s4, separating the copper sulfide in the filter residue C obtained in the step S3, and determining the content of the copper sulfide by adopting a titration method;
wherein, the method for separating the water-soluble copper in the step S1 comprises the following steps: using ascorbic acid and Na2S2O3Dissolving out water-soluble copper under the alkalescent condition; ascorbic acid and Na2S2O3The mixed solution of (2) is prepared by adding 1g of Na into 50ml of 2.5% ascorbic acid solution2S2O3(ii) a The weak alkaline condition is pH7.5-8.5;
the step of separating copper sulfide in the step of S4 includes:
firstly, heating and dissolving the filter residue C by using dilute nitric acid, then adding dilute sulfuric acid to continue heating and decomposing, then evaporating the solution to dryness, adding dilute sulfuric acid to heat and dissolve to obtain a mixture of copper and iron, then masking iron and determining the content of copper sulfide by using a titration method.
2. The method of chemical analysis of copper phases in copper concentrate according to claim 1, wherein the step of separating copper sulfide in step S4 comprises:
putting the filter residue in a beaker, wetting the filter residue with distilled water, adding dilute nitric acid, covering a watch glass, heating the beaker at 180 +/-5 ℃ for 10 minutes, adding dilute sulfuric acid, continuously heating to decompose a sample, after the violent reaction stops, cleaning the watch glass with a small amount of water, removing the watch glass, continuously heating at high temperature until dense white smoke is emitted, taking down the watch glass after the dense white smoke is completely dispersed, and cooling the watch glass; washing the bottle wall with distilled water, and then heating and steaming to be nearly dry; adding 0.5% dilute sulfuric acid, heating to dissolve soluble salt, adding distilled water, heating to slightly boil to dissolve, cooling to room temperature, and dissolving the generated copper salt completely.
3. The method for chemical analysis of copper phases in copper concentrate according to claim 2, characterized in that the method for separating water-soluble copper in step S1 is specifically: preparing ascorbic acid and Na2S2O3Adjusting the pH value to 8, adding the sample to be tested into the mixed solution, stirring, and filtering to obtain a filtrate sample 1 containing the water-soluble copper.
4. The method for chemical analysis of copper phases in copper concentrates according to claim 1 or 2, characterized in that the method for separating copper oxide in step S2 is embodied as follows: adding the filter residue obtained in the step S1 into a mixture of 50mL of 3% ethylenediamine solution, 0.125g of sodium 2, 3-dimercaptopropane sulfonate and 1.5g of NH4Cl and 2gNa2SO3The prepared mixed solution is leached for 30min at 37 ℃ and then filtered to obtain a filtrate sample 2.
5. The method for chemical analysis of copper phases in copper concentrates according to claim 1, characterized in that the method for separating native copper in step S3 is embodied as follows: adding the filter residue obtained in the step S2 into a mixture of 50mL of 30g/L hydroxylamine hydrochloride and 20g/LHgCl2-ethanol solution for 30min and filtering to obtain filtrate sample 3.
6. The method of chemical analysis of copper phases in copper concentrates according to claim 1, characterized in that an air-acetylene flame is used to draw a working curve at the wavelength 324.7nm of an atomic absorption spectrometer with copper concentration as abscissa and absorbance as ordinate.
7. The method for chemical analysis of copper phases in copper concentrate according to claim 3, characterized in that the absorbance of the solution to be measured of the filtrate sample 1 is measured at 324.7nm wavelength of the atomic absorption spectrometer, and the content of water-soluble copper is calculated.
8. The method for chemical analysis of copper phases in copper concentrates according to claim 4, characterized in that the absorbance of the solution to be measured of the filtrate sample 2 is measured at 324.7nm wavelength of the atomic absorption spectrometer, and the content of copper oxide is calculated.
9. The method for chemical analysis of copper phases in copper concentrates according to claim 5, characterized in that the absorbance of the solution to be measured of the filtrate sample 3 is measured at 324.7nm wavelength of the atomic absorption spectrometer, and the native copper content is calculated.
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