CN114993969A - Method for enriching and determining gold, platinum and palladium in copper-nickel sulfide ore by fire assay method - Google Patents

Method for enriching and determining gold, platinum and palladium in copper-nickel sulfide ore by fire assay method Download PDF

Info

Publication number
CN114993969A
CN114993969A CN202210576453.3A CN202210576453A CN114993969A CN 114993969 A CN114993969 A CN 114993969A CN 202210576453 A CN202210576453 A CN 202210576453A CN 114993969 A CN114993969 A CN 114993969A
Authority
CN
China
Prior art keywords
lead
gold
palladium
platinum
copper
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202210576453.3A
Other languages
Chinese (zh)
Inventor
邵坤
赵朝辉
李刚
范建雄
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Institute of Multipurpose Utilization of Mineral Resources Chinese Academy of Geological Sciences
Original Assignee
Institute of Multipurpose Utilization of Mineral Resources Chinese Academy of Geological Sciences
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Institute of Multipurpose Utilization of Mineral Resources Chinese Academy of Geological Sciences filed Critical Institute of Multipurpose Utilization of Mineral Resources Chinese Academy of Geological Sciences
Priority to CN202210576453.3A priority Critical patent/CN114993969A/en
Publication of CN114993969A publication Critical patent/CN114993969A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40Concentrating samples
    • G01N1/4044Concentrating samples by chemical techniques; Digestion; Chemical decomposition
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N31/00Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
    • G01N31/16Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

Landscapes

  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Molecular Biology (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)

Abstract

The invention relates to the technical field of precious metal determination, and discloses a method for determining gold, platinum and palladium in copper-nickel sulfide ore by fire assay gold enrichment, which specifically comprises the following steps: s1: adding the mixture into a sample to be detected, uniformly mixing, dripping a silver nitrate solution, and wrapping the mixture into a paper mass by using paper; s2: putting the paper mass into a gold testing vessel in a high-temperature furnace at 1050 ℃ along with 950-; s3: and digesting the alloy particles, and determining the contents of gold, platinum and palladium. The method is simple to operate, accurate in measurement result and suitable for popularization.

Description

Method for enriching and determining gold, platinum and palladium in copper-nickel sulfide ore by fire assay method
Technical Field
The invention relates to the technical field of precious metal determination, in particular to a method for determining gold, platinum and palladium in copper-nickel sulfide ore by fire assay gold enrichment.
Background
The copper nickel sulfide ore is an important strategic metal mineral resource in China, and is usually accompanied by a certain amount of precious metals such as gold, platinum, palladium and the like. Because the copper, nickel and sulfur contents in the copper-nickel sulfide ore are relatively high and the gold, platinum and palladium contents are relatively low, the difficulty in measuring the contents of gold, platinum and palladium elements in the copper-nickel sulfide ore is high. The accurate analysis of the gold, platinum and palladium contents in the copper-nickel sulfide ore is carried out, so that the comprehensive utilization rate of the copper-nickel sulfide ore is increased, the consumption of the copper-nickel sulfide ore is reduced, and the comprehensive utilization level of the copper-nickel sulfide ore is improved.
The fire gold testing method is one of the main methods for determining precious metals in geological mineral samples, and is divided into lead, nickel matte, antimony, bismuth, tin, copper and other gold testing methods according to different collectors, wherein the lead gold testing method is most long and common in application, and other gold testing methods are developed on the basis of lead gold testing. The lead gold testing method has the advantages of strong precious metal capturing capacity, strong slagging capacity, suitability for almost all ore species, simple ash blowing and fast flow, and especially the convenience of the operation of the lead gold testing method is beyond that of other derivative methods, so the lead gold testing method still has irreplaceable effects in the field of precious metal analysis.
At present, the pretreatment of gold, platinum and palladium analysis in geological mineral samples mainly adopts a lead test gold method, such as the current analysis standard: method for analysis of precious metals in geochemical samples part 6: determination of platinum amount, palladium amount and gold amount fire test gold enrichment-emission spectrometry (GBT 17418.6-2010 State quality supervision and inspection headquarters), gold ore chemical analysis method part 1 determination of gold amount (GB/T20899.1-2019 State quality supervision and inspection headquarters), gold concentrate chemical analysis method (GB/T7739.1-2019 State quality supervision and inspection headquarters), regional geochemical sample analysis method part 31: platinum and palladium content determination fire test gold enrichment-inductively coupled plasma mass spectrometry (DZ/T0279.31-2016 department of homeland resources), regional geochemical sample analysis method part 12: platinum, palladium and gold content determination fire test gold enrichment-emission spectrometry (DZ/T0279.12-2016 department of homeland resources), platinum and palladium determination inductively coupled plasma mass spectrometry (DB 51/T2114-2016 Sichuan province quality and technology supervision agency) in geochemical samples, and the like. In addition, in the current analysis standards of the industries of commodity inspection, nonferrous metals and the like, samples containing copper and nickel are also mainly processed by a lead-assay method, such as part 3 of a chemical analysis method of nickel concentrate: determination of gold, platinum and palladium contents inductively coupled plasma mass spectrometry (SN/T4501.3-2017 State quality supervision, inspection and quarantine Bureau), determination of platinum amount in scrap copper chemical analysis method (DB 44/T1816 one 2016 Guangdong province market supervision and management Bureau), copper anode mud chemical analysis method part 3: determination of platinum amount and palladium amount fire test gold enrichment-inductively coupled plasma emission spectrometry (YS/T745.3-2010), copper smelting silver separation slag chemical analysis method part 2: the method for measuring the contents of platinum and palladium comprises a fire-test gold enrichment-inductively coupled plasma atomic method (YS/T1314.2-2019), a 7 th part of a black copper chemical analysis method, a platinum amount and a palladium amount measurement fire-test gold enrichment-inductively coupled plasma atomic emission spectrometry and a flame atomic absorption spectrometry (YS/T716.7-2016), and the like.
Therefore, the lead gold testing method still has strong vitality due to strong trapping capacity, convenient ash blowing process and simple and convenient operation mode. However, the above method has particular difficulties for enrichment determination of a copper nickel sulphide ore sample:
1. copper, nickel and sulfur are easy to form sulfonium in the lead gold testing process, and compete with lead to capture precious metals, so that the loss of the precious metals in smelting is caused;
2. during smelting, part of copper and nickel can enter the lead button to influence the ash blowing of the lead button, so that the loss of precious metals during ash blowing is caused;
3. when sulfur enters the lead button, the lead button becomes brittle and hard, and a large amount of black smoke is generated during ash blowing, so that ash blowing is difficult to perform.
Aiming at the common problem of enriching copper, nickel and sulfur samples by a lead gold testing method, for example, Chinese patent (method CN 108680565B for measuring platinum and palladium content in nickel ore by using inductively coupled plasma emission spectrum) adopts the steps of firstly roasting to remove sulfur, then adding lead oxide with the amount 7-10 times of the sample amount, slagging by using redundant lead oxide to remove nickel interference, and blowing lead buttons in a magnesia cupel for ash blowing. According to the Chinese patent (the method for measuring the amount of palladium in copper matte CN 113376145A), by controlling the addition of lead oxide, 5-8g of copper matte sample and the addition of lead oxide of 150-250g, and utilizing the strong oxidizing property of molten lead, almost all of copper, iron, arsenic, zinc and the like, an acid flux and an alkaline flux can form corresponding salts to enter slag, so that the optimal ash blowing effect is achieved, and the interference of other impurity elements in the copper matte on the measurement of the amount of palladium can be effectively eliminated. The method has the disadvantages of complicated roasting for sulfur removal and time consumption, and the lead oxide added in a large amount seriously pollutes the environment. The method comprises the above-mentioned various analysis standard methods of nickel and copper-containing substrates, and mainly adopts the method of increasing the use amount of lead oxide to remove impurities. According to the literature (experimental research and improvement of a fire gold testing method for gold concentrate containing sulfur, Liyu province and the like, 2016 (non-ferrous metals in the world)), aiming at gold concentrate containing high sulfur content, a saltpeter method is adopted to eliminate the interference of sulfur, namely, the reducing power of sulfur in a sample is firstly tested, then potassium nitrate is added to remove sulfur, and the size of a lead button is adjusted by adjusting the using amount of potassium nitrate. The improved method is suitable for gold concentrate samples with higher sulfur content, and the batching method, especially the amount of lead oxide, for the samples with higher copper and nickel content is properly adjusted after calculation according to the copper and nickel content. The method needs to test the reducing force of the sample, is very troublesome and tedious, and is not easy to control the size of the lead button. Therefore, a method for enriching gold, platinum and palladium in copper-nickel sulfide ore by a lead assay method, which can overcome the difficulties, is simple to operate and accurate in measurement, is needed.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a method for determining gold, platinum and palladium in copper-nickel sulfide ore by fire test gold enrichment, so that at least the method is simple and the determination result is accurate.
The purpose of the invention is realized by the following technical scheme:
a method for enriching and measuring gold, platinum and palladium in copper-nickel sulfide ore by a fire assay method comprises the following steps:
s1: adding the mixture into a sample to be detected, uniformly mixing, dripping a silver nitrate solution, and wrapping the mixture into a dough by using paper;
s2: putting the paper mass into a gold testing vessel in a high-temperature furnace at 1050 ℃ with 950 plus materials, closing a furnace door after outer-layer paper is carbonized, preserving heat for 5-20min, then concentrating lead buttons formed above slag into lead buttons, reducing the temperature of the high-temperature furnace to 950 ℃ with 900 plus materials, blowing ash of the lead buttons in the gold testing vessel into alloy granules, then taking out the gold testing vessel, cooling and taking out the alloy granules;
s3: and digesting the alloy particles, and determining the contents of gold, platinum and palladium.
It is worth noting that if the sulfur content of the sample is high, lead sulfide is easy to generate with lead, and at the moment, the sample can be discharged from the furnace urgently, and the sample can be discharged from the furnace after the sulfur is oxidized to a little smoke, so that satisfactory lead buttons and results can be obtained; in the later stage of ash blowing, along with the reduction of the lead melting beads, the lead melting beads are easily covered by the molten slag, so that the interruption of oxidized ash blowing is caused, therefore, the observation at any time is needed in the ash blowing process, the lead melting beads are ensured to be always exposed in the air, and if the lead melting beads are covered by the molten slag, the ash blowing is continued after a small amount of molten slag is poured out.
Further, in step S1, the amount of the sample to be tested is 5-10 g; and/or the concentration of the silver nitrate is 10g/L, and the dosage is 2-5 drops.
Further, the purpose of wrapping the paper into a dough in step S1 is to prevent loss during the transfer process, and plain paper is used.
Further, in step S1, the mixed ingredients include the following components in parts by weight: 5-10 parts of trapping agent, 1-5 parts of acid fusing agent, 1-5 parts of alkaline fusing agent and 1-3 parts of reducing agent, wherein the mass ratio of the mixed ingredients to the sample to be detected is 5-10: 1.
The trapping agent comprises any one of litharge (PbO), yellow lead (Pb2O3), red lead (Pb3O4), lead acetate, basic lead carbonate, lead granules, lead powder, lead nitrate or lead sulfate;
the acid fusing agent comprises any one of boric acid, anhydrous borax, silicon dioxide, glass powder, quartz sand or quartz powder;
the alkaline flux comprises any one of sodium carbonate, potassium carbonate, calcium oxide or lime;
the reducing agent comprises any one of flour, wheat flour, buckwheat flour, corn flour, starch, sucrose, animal fiber, active carbon or charcoal powder;
further, the mixed ingredients also comprise a protective agent; the protective agent comprises any one of silver, tellurium or lead.
It is worth noting that if potassium carbonate is added into the ingredients, the melting point of the flux is low, the flux is quickly spread in a porcelain dish, and partial lead grains are easily not concentrated and are oxidized and lost in advance, so that the potassium carbonate is not added or is not added.
Further, in step S2, the gold test utensil is preheated to 950-.
Further, in step S2, the gold test vessel is a butterfly vessel with a flat bottom.
Further, the butterfly-shaped utensil is a butterfly-shaped porcelain utensil, a butterfly-shaped crucible, a small porcelain dish or a ceramic crucible cover; a porcelain crucible cover is preferred because the bottom of the porcelain crucible cover is the flattest.
According to the increase or decrease of the sample amount, the specification of the butterfly-shaped vessel can be increased or decreased properly, for example, the butterfly-shaped vessel for 10g sample measurement is about 2cm in height, and 5g of samples can be directly carried out on a 150-200 mL ceramic crucible cover.
Traditional clay crucible, inside is darker, is favorable to the lead button at the in-process entrapment noble metal that sinks, is favorable to the separation of slag and knot, avoids lead oxidation in the melting process simultaneously, but to the sample that contains high sulphur, sulphur can't be got rid of in the melting process, and sulphur can act as the reductant, leads to reductant excessive in the batching, and partly sulphur can get into in the sediment, and partly sulphur can get into lead and detain, influences follow-up ash and blows. Therefore, when a clay crucible is used for measuring a high-sulfur sample, the processing method is to bake the sample in advance or add potassium nitrate to oxidize excessive sulfur, but the reduction force of the sample needs to be calculated, the analysis steps are increased, and the size of the lead button is not easy to control.
By adopting the butterfly-shaped porcelain vessel, the slag generated by oxidation diffuses to the periphery, so that the lead melting beads can be exposed in the slag, the lead melting beads can be more fully contacted with oxygen, the forward proceeding of the blowing of the oxidized ash is promoted, the residual lead ash can be blown to the minimum, and even the lead can be completely removed.
Further, in step S2, the centralized method is: and opening the furnace door, and shaking the lead shot to be concentrated.
Further, in step S2, the centralized method may further include: and continuously closing the furnace door and preserving heat until the lead shot is concentrated.
Further, in step S2, the particle size of the combined particles is 1-2 mm.
Further, in step S3, the digestion method is:
cleaning and drying the combined particles, transferring the combined particles to a closed digestion tank, adding nitric acid, carrying out pre-digestion on an electric heating plate at the temperature of 120-150 ℃, then adding aqua regia, closing the digestion tank after the violent reaction is stopped, carrying out digestion in an oven at the temperature of 180-240 ℃ for 60-360min, taking out after cooling, transferring the solution to a 50mL volumetric flask, carrying out volume determination with water, shaking up uniformly, and standing.
Further, in step S3, the measuring method includes a titration method, a spectrophotometry method and an instrumental analysis method.
It is worth noting that the principle of the method is as follows: 1. and 2, opening the furnace door ash to blow, oxidizing the metallic lead into lead oxide at high temperature after oxygen in the air enters, wherein the lead oxide has strong basicity and strong oxidizing property, can further participate in the slagging of gangue in the sample, and simultaneously oxidizes impurities (nickel, copper and the like) entering the lead button and discharges the impurities into slag, and sulfur, arsenic, antimony and the like are oxidized into gas to be volatilized. Therefore, the lead oxide is not only a trapping agent, but also an oxidant and a slagging agent, and the melting and the ash blowing are integrally completed.
The invention has the beneficial effects that:
1. the invention does not adopt a special gold test crucible and a cupel, does not need to test the reducing power of a sample in advance, combines the advantages of the reduction smelting enrichment and the oxidized ash blowing of a crucible gold test method, integrates the reduction smelting of the gold test and the oxidized ash blowing into a whole, mixes a sample and ingredients, then carries out the reduction smelting in a butterfly-shaped cupel, then carries out the oxidative smelting by utilizing the air entering after opening a furnace door, oxidizes the base metals such as copper, nickel and the like entering the lead by lead oxide, leads the base metals such as copper, nickel and the like to be dissolved in slag, simultaneously oxidizes sulfur, generates low-valence oxides to be volatilized into the air, and partially directly oxidizes the oxides into sulfate to enter molten slag. The analysis method is simple, the gold testing speed is high, and the ash blowing loss is less.
2. The invention adopts a simple butterfly-shaped porcelain vessel or a porcelain crucible cover and the like as the gold test vessel, and lead molten beads are easily exposed in the air due to the small concave surface of the butterfly-shaped porcelain vessel, so that the lead molten beads directly enter into substantial oxidation ash blowing. Compared with the prior art that the batching can be determined only by carrying out complicated steps such as reducing power test on the sample, the method can simplify the complex gold testing batching process into a unified batching, and does not need to specially remove impurities such as sulfur, copper, nickel and the like. The analysis cost is reduced, the analysis time is shortened, and the result is accurate and reliable.
3. The invention is different from the traditional gold testing method of the extraction vessel, the extraction vessel method is only oxidizing smelting and is mainly used for purifying precious metal-containing metallurgical products or crude lead with relatively single components, and aiming at sulfide ore samples with complex compositions, the extraction vessel method is poor in representativeness because of less samples (less than 3g) and cannot well decompose the ore samples by simply utilizing the oxidizing smelting. The method combines reduction smelting and oxidized ash blowing into a whole, can well dissolve and form complex sulfide ore samples, has relatively larger sample weighing amount, relatively lower lead oxide consumption and relatively smaller environmental influence.
4. The existing standard method does not have an analysis method for the content of gold, platinum and palladium in the copper-nickel sulfide ore, but the invention establishes an analysis method for determining the content of gold, platinum and palladium in the copper-nickel sulfide ore by fire test gold enrichment-inductively coupled plasma mass spectrometry.
Drawings
FIG. 1 is a top view of the porcelain crucible cover;
FIG. 2 is a side view photograph of the porcelain crucible cover;
FIG. 3 is a top view of the butterfly-shaped porcelain;
FIG. 4 is a side view photograph of the butterfly shaped porcelain;
FIG. 5 is a photograph when ash is blown using the porcelain crucible cover (taking out the high temperature furnace for shooting) for convenience.
Detailed Description
The technical solutions of the present invention are further described in detail below with reference to the accompanying drawings, but the scope of the present invention is not limited to the following.
Example 1
Taking a national primary standard substance GBW07195 of the copper-nickel sulfide ore for accuracy verification, wherein the specific method comprises the following steps (GBW 07196, GBW07197 and GBW07198 are determined by the same method):
1) gold testing ingredient
Weighing 5g of sample, adding the mixed ingredients according to the mass ratio (1: 7) of the sample flux, uniformly mixing, adding 3 drops of 10g/L silver nitrate, and wrapping the mixed ingredients with paper into a dough.
2) Melting and blowing ash
Putting the paper mass into a gold testing vessel preheated in a 950 ℃ high-temperature furnace for 30min, closing the furnace door after the paper mass is carbonized, preserving heat for 10min, opening the furnace door, reducing lead oxide into small lead particles to float above slag, carefully shaking the lead particles until the lead particles are concentrated into a lead button (or closing the furnace door to continuously preserve heat until the lead particles are concentrated), reducing the temperature to 900 ℃, directly blowing the lead button into small alloy particles (2mm) in the gold testing vessel through oxidized ash, taking out, cooling and hammering out the alloy particles.
3) Granule combination digestion
Cleaning the combined grains with distilled water for 3 times, drying, transferring the combined grains into a closed digestion tank, adding 3mL of nitric acid, carrying out pre-digestion on a temperature-controlled electric heating plate at 140 ℃ for 40min, then adding 5mL of aqua regia into the closed digestion tank, standing for half an hour until the violent reaction stops, closing the digestion tank, placing the digestion tank in an oven for digestion at 200 ℃ for 150min, turning off the power supply of the oven, cooling, taking out, transferring the digestion tank into a 50mL volumetric flask with water for opening the cover, diluting the digestion tank with water to a scale, shaking up, and standing. Diluting different times according to the content to be detected.
4) Standard solution
The standard stock solution (1000mg/L) of the single element is purchased from national analysis and test centers for nonferrous metals and electronic materials, and is a certified standard substance. The mixed standard solution is prepared by diluting and mixing the single element standard stock solution step by step, and is a mixed standard solution A (the mass concentrations of gold, platinum and palladium are all 10 mu g/mL) and a mixed solution B (the mass concentrations of gold, platinum and palladium are all 250ng/mL) respectively. Transferring 0mL, 0.1mL, 0.4mL and 1.0mL of mixed solution B and 0.1mL, 0.25mL and 1.0mL of mixed standard solution A into 7 50mL volumetric flasks, sequentially adding a small amount of water and 3.5mL of nitric acid, uniformly mixing, adding 4.5mL of hydrochloric acid, diluting to scale, and uniformly mixing. The mass concentrations of the gold platinum palladium standard working solution are 0ng/mL, 0.50ng/mL, 2.0ng/mL, 5.0ng/mL, 20.0ng/mL, 50.0ng/mL and 200.0 ng/mL.
5) Instrumental determination
And (3) tuning various indexes of the instrument by using the tuning liquid, editing the measuring method and selecting measuring elements and internal elements after various indexes such as sensitivity, oxides, double charges, background values, resolution ratio and the like reach measuring requirements, accessing an internal standard solution by using a three-way pipe, and sequentially measuring the standard solution, the blank solution and the solution to be measured. If the measurement result is out of the measurement range of the standard curve, the sample solution should be diluted and measured. The mass numbers of gold, platinum, palladium and internal elements selected are shown in table 1.
TABLE 1
Element(s) Gold (Au) Platinum (II) Palladium (II)
Mass number 197 195 106
Internal standard element 185Re 185Re 115In
6) Calculation of results
The calculation formula for the gold, platinum and palladium contents is as follows:
Figure BDA0003662337550000061
in the formula: w is the mass fraction of gold, platinum or palladium, ng/g; rho 1 is the mass concentration of gold, platinum or palladium in the solution to be tested, which is obtained by searching the calibration curve, and is ng/mL; rho 0 is the mass concentration of gold, platinum or palladium in the blank test solution checked from the calibration curve, ng/mL; v is the total volume of the solution to be tested, mL; m is the weight of the sample, g.
The experimentally determined values were compared with the standard values and the results are shown in table 2:
TABLE 2
Figure BDA0003662337550000062
Figure BDA0003662337550000071
Example 2
Two copper nickel sulphide ore samples are selected, wherein 1# (Cu 0.86%, Ni 1.07%, S3.85%), 2# (Cu 0.46%, Ni 0.81%, S2.77%) are compared and verified by different methods respectively, the detailed operation steps of the method are the same as those of example 1 (some parameters such as temperature, reaction time and the like are slightly adjusted according to specific conditions), and the experimental results are shown in Table 3:
TABLE 3
Figure BDA0003662337550000072
Wherein SN/T4501.3-2017 is a nickel concentrate chemical analysis method in the standard of the export-import inspection and quarantine industry of the people's republic of China; reference is made to the literature document "fire test study and improvement of gold test method for sulfur-containing gold concentrate, 2016, world nonferrous metals, Liyu province, etc.". According to experimental data, the content of the gold, platinum and palladium measured by the method is not much different from the data measured by the prior art, and the method has higher accuracy, but obviously simpler and easier operation and can be used for actual production.
The foregoing is illustrative of the preferred embodiments of this invention, and it is to be understood that the invention is not limited to the precise form disclosed herein and that various other combinations, modifications, and environments may be resorted to, falling within the scope of the concept as disclosed herein, either as described above or as apparent to those skilled in the relevant art. And that modifications and variations may be effected by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.

Claims (10)

1. A method for determining gold, platinum and palladium in copper-nickel sulfide ore by fire assay gold enrichment is characterized by comprising the following steps:
s1: adding the mixture into a sample to be detected, uniformly mixing, dripping a silver nitrate solution, and wrapping the mixture into a dough by using paper;
s2: putting the paper mass into a gold testing vessel in a high-temperature furnace at 1050 ℃ with 950 plus materials, closing a furnace door after outer-layer paper is carbonized, preserving heat for 5-20min, then concentrating lead buttons formed above slag into lead buttons, reducing the temperature of the high-temperature furnace to 950 ℃ with 900 plus materials, blowing ash of the lead buttons in the gold testing vessel into alloy granules, then taking out the gold testing vessel, cooling and taking out the alloy granules;
s3: and digesting the alloy particles, and determining the contents of gold, platinum and palladium.
2. The method of claim 1, wherein: in step S1, the dosage of the sample to be detected is 5-10 g; and/or the concentration of the silver nitrate is 10g/L, and the dosage is 2-5 drops.
3. The method of claim 1, wherein: in step S1, the mixed ingredients comprise the following components in parts by weight: 5-10 parts of trapping agent, 1-5 parts of acid flux, 1-5 parts of alkaline flux and 1-3 parts of reducing agent; the mass ratio of the mixed ingredients to the sample to be detected is 5-10: 1.
4. The method of claim 3, wherein:
the trapping agent comprises any one of litharge, yellow lead, red lead, lead acetate, basic lead carbonate, lead granules, lead powder, lead nitrate or lead sulfate;
the acid fusing agent comprises any one of boric acid, anhydrous borax, silicon dioxide, glass powder, quartz sand or quartz powder;
the alkaline flux comprises any one of sodium carbonate, potassium carbonate, calcium oxide or lime;
the reducing agent comprises any one of flour, wheat flour, buckwheat flour, corn flour, starch, sucrose, animal fiber, activated carbon or charcoal powder.
5. The method of claim 1, wherein: in step S2, the gold test vessel is preheated to 950 ℃ and 1050 ℃ in a high temperature furnace.
6. The method of claim 1, wherein: in step S2, the gold test vessel is a butterfly vessel with a flat bottom.
7. The method of claim 6, wherein: the butterfly-shaped utensil is a butterfly-shaped porcelain utensil, a butterfly-shaped crucible, a small porcelain dish or a porcelain crucible cover.
8. The method of claim 1, wherein: in step S2, the method for centralizing includes: and opening the furnace door to shake the lead shot into a concentrated state, or continuously closing the furnace door to keep the temperature until the lead shot is concentrated.
9. The method of claim 1, wherein: in step S2, the particle size of the combined particles is 1-2 mm.
10. The method of claim 1, wherein: in step S3, the digestion method is:
cleaning and drying the combined particles, transferring the combined particles into a closed digestion tank, adding nitric acid, carrying out pre-digestion on an electric heating plate at the temperature of 120-150 ℃, adding aqua regia, closing the digestion tank after the severe reaction stops, carrying out digestion in an oven at the temperature of 180-240 ℃ for 60-360min, taking out after cooling, transferring the solution into a 50mL volumetric flask, carrying out volume determination with water, shaking up, and standing;
and/or the methods of said determination include titration, spectrophotometry and instrumental analysis.
CN202210576453.3A 2022-05-25 2022-05-25 Method for enriching and determining gold, platinum and palladium in copper-nickel sulfide ore by fire assay method Pending CN114993969A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202210576453.3A CN114993969A (en) 2022-05-25 2022-05-25 Method for enriching and determining gold, platinum and palladium in copper-nickel sulfide ore by fire assay method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202210576453.3A CN114993969A (en) 2022-05-25 2022-05-25 Method for enriching and determining gold, platinum and palladium in copper-nickel sulfide ore by fire assay method

Publications (1)

Publication Number Publication Date
CN114993969A true CN114993969A (en) 2022-09-02

Family

ID=83029694

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202210576453.3A Pending CN114993969A (en) 2022-05-25 2022-05-25 Method for enriching and determining gold, platinum and palladium in copper-nickel sulfide ore by fire assay method

Country Status (1)

Country Link
CN (1) CN114993969A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117025960A (en) * 2023-07-21 2023-11-10 江西三和金业有限公司 Treatment process for recovering noble metal from graphite gold-containing material

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117025960A (en) * 2023-07-21 2023-11-10 江西三和金业有限公司 Treatment process for recovering noble metal from graphite gold-containing material
CN117025960B (en) * 2023-07-21 2024-06-07 江西三和金业有限公司 Treatment process for recovering noble metal from graphite gold-containing material

Similar Documents

Publication Publication Date Title
CN103267736A (en) Analysis and detection method of gold element in smelting material
Paukert et al. Effects of fusion charge composition on the determination of platinum group elements using collection into a minimized nickel sulphide button
CN114993969A (en) Method for enriching and determining gold, platinum and palladium in copper-nickel sulfide ore by fire assay method
CN102706860A (en) Chemical analysis method of rhodium content
CN102253072A (en) Pyrometallurgical ensaying method for controlling quality of lead button
Norrish et al. XRS analysis of sulphides by fusion methods
CN103018191A (en) Analytic method of trace gold contained in composition brass
CN103115886A (en) Method for analyzing gold in tin and tin alloy waste
Ni et al. Simultaneous determination of ultra-trace Pt, Pd, Rh and Ir in geochemical samples by inductively coupled plasma mass spectrometry following tin fire assay preconcentration and microwave digestion
RU2494160C1 (en) Method of determination of gold and silver content in sulphide ores and products of their processing
RU2288288C1 (en) Method of assay determination of content of gold in ores and in products of their processing
CN106756085B (en) A kind of smelting process of platinum concentrate
Luke Photometric Determination of Antimony in Lead Using Rhodamine B Method
Petrović et al. The determination of the content of gold and silver in geological samples
CN111896530A (en) Analysis method for measuring total iron content in blast furnace cloth bag dedusting ash
CN113834709A (en) Plasma mass spectrum/spectrum determination method for noble metal in bismuth gold test enrichment geological sample
CN113466215B (en) Method for simultaneously determining contents of gold, silver, platinum and palladium in low nickel matte and application
CN113376145A (en) Method for measuring amount of palladium in copper matte
Vinci Analytical Chemistry of Beryllium
Raju Comparison of different extraction methods to determine gold in geological samples
RU2365644C1 (en) Method of identification of noble metals in sulfide ores and their processing products
CN114152489B (en) Platinum-palladium-gold gray blowing method in black rock by taking tellurium-silver as protective agent
Ni et al. Bismuth‐Remaining Cupellation Fire Assay Preconcentration Combined with Inductively Coupled Plasma Mass Spectrometry for the Simultaneous Determination of Ultratrace Au, Pt, Pd, Ru, Rh, and Ir in Geologic Samples
RU2245931C1 (en) Gold content determination in gold-containing raw material
Young Analysis for gold: A review of methods

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination