CN114152489A - Platinum-palladium-gold gray blowing method in black rock by taking tellurium and silver as protective agent - Google Patents
Platinum-palladium-gold gray blowing method in black rock by taking tellurium and silver as protective agent Download PDFInfo
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- CN114152489A CN114152489A CN202111353125.9A CN202111353125A CN114152489A CN 114152489 A CN114152489 A CN 114152489A CN 202111353125 A CN202111353125 A CN 202111353125A CN 114152489 A CN114152489 A CN 114152489A
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- gold
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- bismuth
- silver
- tellurium
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- 239000010931 gold Substances 0.000 title claims abstract description 76
- 229910052737 gold Inorganic materials 0.000 title claims abstract description 75
- 238000007664 blowing Methods 0.000 title claims abstract description 58
- 239000011435 rock Substances 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 36
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 20
- 239000004332 silver Substances 0.000 title claims abstract description 20
- 239000003223 protective agent Substances 0.000 title claims abstract description 12
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 title claims abstract description 11
- 229910052714 tellurium Inorganic materials 0.000 title claims abstract description 10
- 238000012360 testing method Methods 0.000 claims abstract description 57
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 47
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Inorganic materials [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000002245 particle Substances 0.000 claims abstract description 20
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 6
- 229910052797 bismuth Inorganic materials 0.000 claims description 36
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 36
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 17
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(I) nitrate Inorganic materials [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 16
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 15
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- 229910000416 bismuth oxide Inorganic materials 0.000 claims description 10
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 8
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- 238000002844 melting Methods 0.000 claims description 8
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- 241000209140 Triticum Species 0.000 claims description 5
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- 235000017550 sodium carbonate Nutrition 0.000 claims description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 abstract description 34
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 abstract description 28
- 229910052763 palladium Inorganic materials 0.000 abstract description 25
- 229910052697 platinum Inorganic materials 0.000 abstract description 24
- 229910000510 noble metal Inorganic materials 0.000 abstract description 20
- 229910001316 Ag alloy Inorganic materials 0.000 abstract description 10
- 238000005259 measurement Methods 0.000 abstract description 9
- 238000004458 analytical method Methods 0.000 abstract description 8
- 238000011084 recovery Methods 0.000 abstract description 8
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 abstract description 7
- 238000001514 detection method Methods 0.000 abstract description 6
- 239000002253 acid Substances 0.000 abstract description 4
- 238000004090 dissolution Methods 0.000 abstract description 4
- AJZRPMVVFWWBIW-UHFFFAOYSA-N [Au].[Bi] Chemical compound [Au].[Bi] AJZRPMVVFWWBIW-UHFFFAOYSA-N 0.000 abstract description 3
- 230000006378 damage Effects 0.000 abstract description 3
- 239000007800 oxidant agent Substances 0.000 abstract description 3
- 230000009467 reduction Effects 0.000 abstract description 3
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- 239000000155 melt Substances 0.000 abstract description 2
- 230000001590 oxidative effect Effects 0.000 abstract description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 23
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 13
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 13
- 229910052799 carbon Inorganic materials 0.000 description 13
- 229910052759 nickel Inorganic materials 0.000 description 12
- 239000000126 substance Substances 0.000 description 8
- 239000000203 mixture Substances 0.000 description 6
- 239000002893 slag Substances 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 239000010970 precious metal Substances 0.000 description 4
- 229910001961 silver nitrate Inorganic materials 0.000 description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 description 3
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 description 3
- BFPJYWDBBLZXOM-UHFFFAOYSA-L potassium tellurite Chemical compound [K+].[K+].[O-][Te]([O-])=O BFPJYWDBBLZXOM-UHFFFAOYSA-L 0.000 description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 3
- 229910010271 silicon carbide Inorganic materials 0.000 description 3
- 229910052717 sulfur Inorganic materials 0.000 description 3
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- 238000005303 weighing Methods 0.000 description 3
- 101710134784 Agnoprotein Proteins 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 2
- -1 Sodium carbonate Silicon dioxide Bismuth oxide Chemical compound 0.000 description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 238000003556 assay Methods 0.000 description 2
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- 239000003638 chemical reducing agent Substances 0.000 description 2
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- 239000012224 working solution Substances 0.000 description 2
- 241001391944 Commicarpus scandens Species 0.000 description 1
- 229910003296 Ni-Mo Inorganic materials 0.000 description 1
- 229910001215 Te alloy Inorganic materials 0.000 description 1
- RWDMAZGBOZOYKZ-UHFFFAOYSA-N [Fe+2].[N+](=O)([O-])[O-].[K+].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-] Chemical compound [Fe+2].[N+](=O)([O-])[O-].[K+].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-] RWDMAZGBOZOYKZ-UHFFFAOYSA-N 0.000 description 1
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- 238000004891 communication Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
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- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
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- 230000029087 digestion Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- PQTCMBYFWMFIGM-UHFFFAOYSA-N gold silver Chemical compound [Ag].[Au] PQTCMBYFWMFIGM-UHFFFAOYSA-N 0.000 description 1
- JVPLOXQKFGYFMN-UHFFFAOYSA-N gold tin Chemical compound [Sn].[Au] JVPLOXQKFGYFMN-UHFFFAOYSA-N 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- 229910001867 inorganic solvent Inorganic materials 0.000 description 1
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- 229910052741 iridium Inorganic materials 0.000 description 1
- 238000012417 linear regression Methods 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 235000014380 magnesium carbonate Nutrition 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- DDTIGTPWGISMKL-UHFFFAOYSA-N molybdenum nickel Chemical compound [Ni].[Mo] DDTIGTPWGISMKL-UHFFFAOYSA-N 0.000 description 1
- YFLLTMUVNFGTIW-UHFFFAOYSA-N nickel;sulfanylidenecopper Chemical compound [Ni].[Cu]=S YFLLTMUVNFGTIW-UHFFFAOYSA-N 0.000 description 1
- 229910052762 osmium Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000000918 plasma mass spectrometry Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
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- 231100000419 toxicity Toxicity 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
- 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
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B11/00—Obtaining noble metals
- C22B11/02—Obtaining noble metals by dry processes
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- 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
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- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
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Abstract
The invention discloses a platinum-palladium gold gray blowing method in black rock by taking tellurium and silver as a protective agent, which aims at improving a bismuth gold test formula according to the characteristics of the black rock and adding a proper oxidant KNO3The reduction medium of the melt is improved, Ag-Te is used as a gray blowing protective agent, secondary gray blowing-open dissolution tellurium-silver alloy particle-ICP-AES is adopted to measure Pt, Pd and Au in the black rock sample, the recovery rate is more than 97 percent, and the problems of poor reproducibility and low accuracy of the measurement result caused by the fact that the conventional gold test formula is not buckled and the gray blowing is not beaded are solved. The method has strong controllability, can digest the noble metal tellurium-silver alloy particles on the electric hot plate by using a small amount of acid, greatly shortens the analysis flow, saves reagents and energy, reduces the environmental pollution andthe method has the advantages of effectively reducing production cost and improving analysis and detection efficiency for harm to operators, and can be applied to determination of Pt, Pd and Au in mass black rock samples.
Description
Technical Field
The invention belongs to the technical field of precious metal recovery, and particularly relates to a platinum-palladium-gold ash blowing method in black rock by taking tellurium and silver as a protective agent.
Background
The noble metal has excellent physical and chemical properties and unique catalytic activity, and is widely applied to the fields of electronics, communication, aerospace, chemical engineering, medical treatment and other industries and modern high and new technology industries. In terms of economic value, its unique monetary attributes are often referred to as national financial reserves. In the field of ornaments, the demand is increased year by year due to the beauty and value retention of the ornaments. With the progress of exploration means, geologists have recently found platinum group elements in black rocks, and this result is expected to alleviate the current situation of shortage of platinum group resources. However, the black rock contains a large amount of carbon, organic carbon and sulfide, and the complex components and reduction characteristics thereof increase the difficulty in analyzing elements such as noble metals in the black rock.
At present, methods for analyzing noble metals mainly include wet methods and fire-assay methods. The wet method mainly adopts aqua regia and HCl-H2O2、HCl-H2O2-KClO3And digesting the sample in an open way or in a high-pressure closed way by using an inorganic solvent. However, the black rock sample contains a large amount of free carbon and organic carbon, and it has been reported that the removal of carbon by burning volatilization causes the loss of noble metal elements by volatilization. And a direct digestion mode is adopted, a large amount of carbon cannot be digested, a strong adsorption effect on noble metal elements is realized, and the result is seriously low. The fire gold testing method is used for capturing precious metals by a high-temperature smelting method, has the advantages of good sampling representativeness, wide applicability, good enrichment effect and the like, and the common capturing modes comprise nickel matte gold testing, lead gold testing, tin gold testing, bismuth gold testing and the like. The nickel matte gold test is a gold test method which is gradually mature in the 90 th of the 20 th century, can simultaneously capture six platinum group elements of Pt, Pd, Rh, Ir, Os and Ru, and forms a national standard method (GB/T17418.7-2010). However, the nickel matte gold test has an unsatisfactory Au trapping effect, and cannot quantitatively trap platinum group elements in the black rock due to the influence of carbon and organic matters. The tin test gold developed by Yan Hongling et al can accurately measure eight noble metal elements in black rock, but the tin test gold has long process and high cost (Yan Hongling, Li Shiwei, Wang Yi, etc.. eight noble metal elements in black rock system are measured simultaneously [ J]Noble metal 2016, 37(3): 66-71.). Lead testing is a classical fire testing method, forms a plurality of standard methods aiming at different minerals, is also an internationally recognized universal method, can simultaneously capture gold, silver, platinum and palladium, and quickly blows ash in a cupel, and has the advantages of simple method and high efficiency. However, the volatilization of a large amount of lead causes serious pollution and damage to the environment and human bodies, and the existence of a large amount of carbon easily causes incrustation when ash is blown, so that the balling effect is not good. Zhang Shilin, Like, etc. adopt bismuth test gold to capture noble metals, and because bismuth is easy to be blown with ash and has small toxicity, the research on noble metals in bismuth test gold enriched ore (Zhang Shilin, Tuhuimin. research on noble metals in bismuth test gold enriched ore [ J)]Mineral and geological, 1981, (2): 90-102; determination of trace amount of gold, platinum and palladium [ J ] in poor platinum ore by Li Ke, Zhao Chaihui, Van Jianxiong, bismuth test-inductive coupling plasma mass spectrometry]Metallurgical analysis, 2013, 33(8): 19-23.). But because ofThe method is not perfect in buckling stability and ash blowing conditions, cannot be popularized and popularized, and particularly cannot form gold and silver beads on black rock samples during ash blowing.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
Aiming at the problems, the invention provides a method for blowing platinum, palladium and gold ash in black rock by taking tellurium and silver as a protective agent, which improves a bismuth gold test formula according to the characteristics of the black rock and adds a proper oxidant KNO3The reduction medium of the melt is improved, Ag-Te is used as a gray blowing protective agent, secondary gray blowing-open dissolution tellurium-silver alloy particle-ICP-AES is adopted to determine Pt, Pd and Au in the black rock sample, the recovery rate is more than 97%, the detection limit of the method is low, the analysis efficiency is high, and the method can be applied to determination of Pt, Pd and Au in large-batch black rock samples.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a platinum-palladium-gold gray blowing method in black rock by taking tellurium and silver as a protective agent comprises the following steps:
(1) enrichment of bismuth test gold: adding a gold test ingredient into a 10.0g black shale sample, and dropwise adding 0.5mL of 60g/L AgNO3Solution and 0.5mL of 76g/L K2TeO3Fully and uniformly mixing the solution, pouring the mixture into a clay crucible, uniformly adding a layer of SiC and light MgO mixed covering agent, placing the clay crucible into a 800 ℃ gold testing furnace, heating for 20min, continuously heating to 1100 ℃ for melting for 30min, taking out the crucible when the mixture is hot, pouring the molten mass into an iron mold, cooling, smashing the glass body, and taking out a bismuth button;
(2) primary ash blowing: placing the magnesia cupel in a high-temperature furnace at 900 ℃ for preheating for 1h, taking out, immediately covering bismuth in the cupel, placing the cupel in the high-temperature furnace again, adjusting the temperature of the furnace to 860 ℃, closing the furnace door for 1-2 min, opening the furnace door for 2-3 cm, introducing air into a hearth, and performing primary ash blowing;
(3) secondary ash blowing: and (3) when the primary ash blowing is about to end, putting the ceramic crucible containing 2-3 g of borax into a high-temperature furnace for melting, when the bismuth button ash is blown to the diameter of 5mm, rapidly pouring the bismuth button into the ceramic crucible containing the molten borax, continuously carrying out secondary ash blowing, when the diameter of the combined particles is 1-2 mm, taking out the crucible, naturally cooling, smashing, and taking out the tellurium-silver combined particles.
Further, the test gold ingredients in the step (1) comprise borax, sodium carbonate, silicon dioxide, bismuth oxide, wheat flour, potassium nitrate, iron powder and a covering agent, wherein 15g of borax, 50g of sodium carbonate, 10g of silicon dioxide, 40g of bismuth oxide, 2g of wheat flour, 15g of potassium nitrate, 8g of iron powder and 5g of the covering agent are required by taking 10.0g of the black shale sample as a reference.
The invention has the beneficial effects that: the invention takes bismuth oxide with low toxicity as a trapping agent, improves the property of black rock sample slag by adjusting the formula of the gold test, and particularly adds AgNO3Solutions and K2TeO3The solution is combined with noble metal at high temperature to form smooth and round tellurium-silver alloy particles, thus solving the problems of poor reproducibility and low accuracy of the measurement result caused by the fact that the conventional gold test formula cannot be buckled and cannot be beaded by blowing ash. The method is strong in controllability, the noble metal tellurium and silver alloy particles can be digested on the electric hot plate by a small amount of acid, the analysis process is greatly shortened, the reagent and the energy are saved, the environmental pollution and the harm to operators are reduced, the production cost is effectively reduced, the analysis and detection efficiency is improved, and the method is suitable for measuring trace Pt, trace Pd and Au in a large batch of black rock samples.
Drawings
Fig. 1 shows loose silver flakes after one ash blow.
FIG. 2 shows the tellurium-silver alloy particles after the second ash blowing.
FIG. 3 shows the effect of potassium nitrate dosage on primary ash blast.
Fig. 4 shows the case of secondary blowing with bismuth button added with silver nitrate.
FIG. 5 shows the case of secondary blowing with bismuth plus silver nitrate and potassium tellurite.
Detailed Description
The invention will be further illustrated with reference to specific examples, without however restricting the scope of the invention thereto.
Example 1
The apparatus and reagents used in this example are as follows:
the iCAP6300 Radial inductively coupled plasma atomic emission spectrometer (ICP-AES, Thermo corporation, USA) has the working conditions shown in Table 1.
TABLE 1 ICP-AES working conditions
GWL-1400 ℃ of a gold testing furnace (Luoyang torch star kiln Co., Ltd.);
a gold test crucible (clay);
a magnesia cupel.
The main reagents used in this example were as follows:
silver nitrate (AgNO)3): 60.0 g/L; potassium tellurite (K)2TeO3): 76.0 g/L; covering agent: silicon carbide + light magnesium oxide; hydrochloric acid, nitric acid, sodium carbonate and silicon dioxide are analytically pure; borax and bismuth oxide are chemically pure; the experimental water was deionized water.
Au, Pt, Pd standard solutions: and preparing 1.000mg/mL standard stock solution by using the metals Au, Pt and Pd with spectral purity or purity (mass fraction) of more than 99.99%. The standard stock solution containing Au, Pt and Pd was diluted stepwise to prepare a mixed standard working solution with ρ (Au, Pt and Pd) 10.0 μ g/mL, and the medium was 5% (V/V) aqua regia.
The platinum-palladium-gold gray blowing method in the black rock by taking tellurium and silver as the protective agent comprises the following steps:
(1) enrichment of bismuth by gold test
Accurately weighing 10.0g of black shale sample, adding a gold test ingredient according to the table 2, and dropwise adding 0.5mL of 60g/L AgNO3Solution and 0.5mL of 76g/L K2TeO3And (3) fully and uniformly mixing the solution, pouring the mixture into a clay crucible, and uniformly adding a layer of SiC and light MgO mixed covering agent. Heating the clay crucible in a 800 ℃ gold testing furnace for 20min, continuously heating the furnace to 1100 ℃ for melting for 30min, taking out the crucible when the crucible is hot, pouring the molten mass into an iron mold, cooling, smashing the glass body, and taking out the bismuth button.
TABLE 2 formula of gold test flux
| Test specimen | Sample size | Borax | Sodium carbonate | Silicon dioxide | Bismuth oxide | Wheat flour | Potassium nitrate | Iron powder | Covering agent |
| Black shale | 10g | 15g | 50g | 10g | 40g | 2g | 15g | 8g | 5g |
(2) Two times of ash blowing
Placing the magnesite cupel in a high-temperature furnace at 900 ℃ for preheating for 1h, taking out, immediately covering bismuth in the cupel, placing the cupel in the high-temperature furnace again, adjusting the temperature of the furnace to 860 ℃, closing the furnace door for 1-2 min, opening the furnace door for 2-3 cm, introducing air into a hearth, and performing primary ash blowing. And (3) when the primary ash blowing is about to end, putting the ceramic crucible containing 2-3 g of borax into a high-temperature furnace for melting, when the bismuth button ash is blown to the diameter of about 5mm, rapidly pouring the bismuth button into the ceramic crucible containing the molten borax, continuously carrying out secondary ash blowing, when the diameter of the combined particles is 1-2 mm, taking out the crucible, naturally cooling, smashing, and taking out the tellurium-silver combined particles.
Dissolution and measurement of the conjugate particles: putting the tellurium-silver alloy particles into a 50mL small beaker, adding 5mL of 1+3 nitric acid, placing the mixture on an electric hot plate at 150 ℃ for heating and dissolving, adding 5mL of concentrated HCl when the alloy particles do not bubble any more, continuing heating and dissolving until the alloy particles are completely decomposed, taking down and cooling, metering the volume with 10% hydrochloric acid into a 10mL colorimetric tube, and shaking up uniformly. And measuring the contents of Pt, Pd and Au by ICP-AES.
Selection of ingredients for testing gold
The fire test gold deduction condition has close relation with the sample composition and the selection and proportion of the test gold ingredients. The black rock sample contains high carbon, organic carbon, a large amount of metal sulfides and other components, and the molten slag with good fluidity and the smooth and complete gold testing button cannot be obtained by adopting the gold testing formula of the samples of common soil, rocks and the like. And the method adopts Bi2O3As a trapping agent, the analysis procedure can be simplified by blowing ash, but many platinum group elements in the black rock are wrapped in Ni-Mo sulfide, and Bi2O3When the precious metal is collected, part of metal elements such as Ni and Cu also enter the bismuth button, and a nickel skin appears during primary ash blowing, so that the ash blowing process is seriously hindered. In the test, 10.0g of black rock sample is taken, different test gold ingredients are added, melting is carried out at 1100 ℃, and the conditions of fire test gold slagging, buckling and primary ash blowing are observed, and the results are shown in table 3. As can be seen from Table 3, the formulation No. 5 can obtain the smooth and complete bismuth button with metallic luster, and the melting point of the slag is low, the specific gravity is small, the fluidity is good, the button slag is easy to separate, the bismuth button is not easy to break, and the ash is blown without the influence of nickel skin.
TABLE 3 batching of gold testing flux
Second, selection of ash blowing mode
General geological samples are analyzed for Pt, Pd and Au, and a bismuth button formed after bismuth test gold enrichment can be subjected to one time of ash blowing to obtain round noble metal silver beads, but because the components of black rock are too complex, only non-granular loose silver sheets can be formed after one time of ash blowing, the loose silver sheets are adhered to a magnesia cupel and cannot be completely taken out, and the determination result is lower, as shown in figure 1. Through tests, a certain amount of tellurium is added into a test gold ingredient, when primary ash is blown to about 5mm of bismuth button in a high-temperature furnace at 860 ℃ in a magnesia cupel, the bismuth button is rapidly poured into a porcelain crucible or a porcelain crucible cover filled with molten borax, secondary ash blowing is completed under the condition of borax wrapping, and round and bright tellurium-silver alloy particles can be obtained after cooling, as shown in figure 2.
Bismuth oxide dosage test
Weighing 10.0g of black rock standard substance GBW07737 in parts, and adding 20g, 30g, 40g and 50g of Bi according to Table 42O3Mixing with the gold testing material to develop Bi2O3The dosage of (A) is tested. And (3) measuring Pt, Pd and Au by using the ICP-AES (inductively coupled plasma-atomic emission Spectrometry) for dissolving and fixing the volume after the secondary ash blowing according to the flow of the 1.3 experimental method. As can be seen from the measurement results in Table 4, Bi is present in the case of reasonable amount of the reagent and good fluidity of the slag2O3The amount of the bismuth oxide is more than 30g, the measurement results of Pt, Pd and Au have no obvious difference from the set values, and the addition amount of the bismuth oxide is generally 40g in order to ensure the trapping rate of the noble metal.
TABLE 4 amounts of bismuth oxide
Influence of potassium nitrate dosage on button forming and noble metal element enrichment
Because the black rock contains a large amount of elements such as carbon, sulfur, nickel and the like, the gold is directly tested on the premise of no burning, and a complete bismuth button is difficult to form due to strong reducibility. And when the bismuth button is subjected to primary ash blowing, a large amount of nickel skin appears, so that the normal operation of the ash blowing is seriously hindered. Through tests, the reducing agent flour in the formula is reduced, and the carbon in the black rock is used as the reducing agent, so that the buckling condition can not be formed, and the test selects adding the oxidizing agent potassium nitrate to adjust the buckling condition. 8g, 10g, 12g and 15g of potassium nitrate are respectively added into the best trial-gold ingredient of a 10g black rock standard substance GBW07737, and are melted into buttons at high temperature, wherein when 8g and 10g of potassium nitrate bismuth buttons are added and are subjected to primary gray blowing at 860 ℃, nickel skin is formed seriously, the gray blowing can be completed only by pulling the nickel skin apart in the gray blowing process, the primary gray blowing nickel skin is gradually reduced along with the increase of the using amount of the potassium nitrate, and the state after the gray blowing is shown in figure 3. From the ash blowing condition, when the dosage of potassium nitrate is 15g, the formed bismuth button is complete, and the influence of nickel skin can be eliminated. The conditions are selected, a secondary ash blowing test is carried out, round and bright tellurium-silver alloy particles can be obtained, the measurement results of Pt, Pd and Au after the alloy particles are dissolved in acid are shown in Table 5, and the measurement results show that when the addition amount of potassium nitrate is 15g, the measurement results are accurate and reliable.
TABLE 5 Potassium nitrate dosage test
Fifthly, the influence of the iron powder on the button forming and the enrichment of the noble metal elements
The black shale sample has high sulfur content, the reducing force is difficult to master, the button is small and large, matte or yellow slag is sometimes generated, the buttons are not gathered and can not quantitatively capture precious metals, and the bismuth button is brittle and fragile. 10g of black rock standard substance GBW07737 is weighed respectively, different amounts of iron powder are added into the best gold testing ingredients according to the table 6, and the deduction condition and the influence of twice ash blowing on the enrichment of the precious gold elements are shown in the table 6. The result shows that the adding amount of the iron powder is more than 6g, bright and unbreakable bismuth buttons can be obtained, the measuring results of Pt, Pd and Au after secondary ash blowing are better, and 8g of the iron powder is selected to be added in the test in order to ensure the recovery rates of the Pt, Pd and Au.
Table 6 iron powder dosage test
Influence of potassium tellurite on gold-silver combined particles
Ag. Te can be used as an ash blowing protective agent, but Te has strong oxidation resistance, a certain amount of Bi can be reserved in the combined particles during one-time ash blowing as long as Te exists, and the loss can be reduced as the noble metal elements are protected by Bi. And, Te can form compounds with noble metals (e.g., PtTe)2) And the protective effect is also achieved. Tests show that the bismuth button only added with silver nitrate can only form flat and rough silver flakes during the secondary ash blowing, as shown in figure 4, and the silver flakes disappear after a slightly longer ash blowing time. 0.5mL of 60g/L AgNO was added by assay3And 0.5mL of 76g/L K2TeO3The obtained bismuth button can form smooth and round tellurium-silver alloy particles through secondary ash blowing, and the figure is shown in figure 5. The measurement results of Pt, Pd and Au after the dissolution by adding acid have no obvious difference with the determined values.
Seventh, detection limit and linear equation of method
5% (V/V) aqua regia is used as a medium, Pt, Pd and Au mixed standard working solution is prepared according to the formula 7, corresponding spectral line intensity is measured under the condition of an optimal instrument, a calibration curve is drawn, and a linear regression equation, a correlation coefficient and a linear range are shown in the formula 7. The 12 independent blank tests in the whole process were carried out according to the experimental method, and the detection limit of the method was calculated with 3 times of standard deviation, and the results are shown in table 7.
TABLE 7 Linear Range, Linear equation, correlation coefficient and detection limits
Eighth, recovery rate of the method
Weighing a plurality of parts of 10.0g of black rock standard substance GBW07737, respectively adding Pt, Pd and Au standard solutions with different amounts, smelting according to an experimental method, blowing ash, and calculating the recovery rate of the added standard, wherein the result is shown in Table 8. Experiments show that the recovery rates of Pt, Pd and Au are all more than 97%.
TABLE 8 method recovery test
Nine, precision and accuracy of the method
Selecting black rock standard substances GBW07736 and GBW07737 and copper nickel sulfide ore standard substances GBW07194 and GBW07195 with high carbon and sulfur contents, carrying out parallel analysis for 12 times according to an experimental method, and inspecting the precision and the accuracy of the method, wherein the results are shown in Table 9. The result shows that the Relative Error (RE) of the measured result of the standard substance and the determined value is-4.31-3.77%, and the Relative Standard Deviation (RSD) is less than 6.92%.
Precision and accuracy of the method of table 9 (n ═ 12)
Although the present invention has been described in detail with reference to the embodiments, it will be understood by those skilled in the art that various changes in the specific parameters of the embodiments may be made without departing from the spirit of the present invention, and a plurality of specific embodiments are formed, which are common variations of the present invention, and will not be described in detail herein.
Claims (2)
1. A platinum-palladium-gold gray blowing method in black rock by taking tellurium and silver as a protective agent is characterized by comprising the following steps:
(1) enrichment of bismuth test gold: adding a gold test ingredient into a 10.0g black shale sample, and dropwise adding 0.5mL of 60g/L AgNO3Solution and 0.5mL of 76g/L K2TeO3Mixing the solution, pouring into a clay crucible, adding a layer of SiC and light MgO mixed covering agent, heating the clay crucible in a 800 deg.C gold test furnace for 20min, heating to 1100 deg.C, melting for 30min, taking out the crucible when it is hot, and pouring the molten mass into an iron moldAfter cooling, smashing the glass body, and taking out the bismuth button;
(2) primary ash blowing: placing the magnesia cupel in a high-temperature furnace at 900 ℃ for preheating for 1h, taking out, immediately covering bismuth in the cupel, placing the cupel in the high-temperature furnace again, adjusting the temperature of the furnace to 860 ℃, closing the furnace door for 1-2 min, opening the furnace door for 2-3 cm, introducing air into a hearth, and performing primary ash blowing;
(3) secondary ash blowing: and (3) when the primary ash blowing is about to end, putting the ceramic crucible containing 2-3 g of borax into a high-temperature furnace for melting, when the bismuth button ash is blown to the diameter of 5mm, rapidly pouring the bismuth button into the ceramic crucible containing the molten borax, continuously carrying out secondary ash blowing, when the diameter of the combined particles is 1-2 mm, taking out the crucible, naturally cooling, smashing, and taking out the tellurium-silver combined particles.
2. The platinum-palladium-gold gray blowing method in black rock by taking tellurium and silver as a protective agent, which is characterized by comprising the following steps of: the reagent gold ingredients in the step (1) comprise borax, sodium carbonate, silicon dioxide, bismuth oxide, wheat flour, potassium nitrate, iron powder and a covering agent, wherein 15g of borax, 50g of sodium carbonate, 10g of silicon dioxide, 40g of bismuth oxide, 2g of wheat flour, 15g of potassium nitrate, 8g of iron powder and 5g of the covering agent are required by taking 10.0g of a black shale sample as a reference.
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