CN109238989A - A kind of analysis method of Silver From Ore object phase - Google Patents
A kind of analysis method of Silver From Ore object phase Download PDFInfo
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Abstract
The invention belongs to Silver From Ore object phase measuring method technical fields, and in particular to a kind of analysis method of Silver From Ore object phase；Especially suitable for Silver From Ore total amount < 500g/t Silver From Ore object molybdenum determination, operating process is simplified compared with the conventional method, improves analysis speed and accuracy rate is high.
Description
Technical field
The invention belongs to Silver From Ore object phase measuring method technical fields, and in particular to a kind of analysis of Silver From Ore object phase
Method.
Background technique
Silver is the noble metal very close with human relation, and physicochemical property is relatively stable, thermally conductive, electric conductivity is fine,
Matter is soft, and rich ductility, reflecting rate is high, up to 99% or more.
Ag in geological sample be primarily present form have it is following several: 1 with sulfide existing for Independent Mineral state, such as brightness
Silver ore (Ag2S), owyheeite, dark red silver ore (Ag3SbS3) etc., 2 native silver (Ag0) and silver-colored interphase such as silver gold
Ag in mine, kustelite, galena and copper sulfide mineral, 3 also can with isomorph or with existing for micro-inclusion state,
Such as have under supergene condition secondary mineral horn silver (AgCl) and some iron and manganese oxides and gangue mineral can also wrap up or
Adsorb Ag.The existence form of silver in nature is varied, then the material phase analysis of silver is for the exploitation of silver ore, point in mineral deposit
It is all of great significance in terms of analysis, ore-dressing technique etc..But current silver-colored Phase Analysis is excessively cumbersome, measurement it is mutually excessive,
It is unfavorable in fast and accurately assaying silver-colored object phase.
Summary of the invention
In order to overcome the above problem, the present invention provides a kind of analysis method of Silver From Ore object phase, especially suitable for ore
The Silver From Ore object molybdenum determination of middle silver total amount < 500g/t, simplifies operating process compared with the conventional method, improves analysis speed
Degree and accuracy rate height.
The specific steps of the present invention are as follows:
The measurement of silver content in horn silver (AgCl) in step 1 ore:
Rock sample of 0.5000~1.0000g granularity less than 0.075mm is weighed in 200mL conical flask, leaching is added
The ammonium hydroxide 100ml of agent i.e. 5% covers rubber plug, vibrates 30 minutes under room temperature state, is filtered with qualitative fast grade filter paper, with 2% ammonium hydroxide
Washing precipitating 6~7 times is washed precipitating 2 times again with water, collects filtrate and washing lotion is collectively disposed in 250mL beaker, heating is concentrated into
5mL is added 10mL chloroazotic acid, heats and be steamed near dry on electric furnace, and 8mL concentrated hydrochloric acid is added, and purges watch glass and wall of cup with water, is heated to
Boiling, is removed and is cooled to room temperature, be settled in 50mL volumetric flask, shaken up with water, static 30min is held with aas determination
The silver content of liquid in measuring bottle, the content of Ag as in horn silver (AgCl)；
The measurement of silver content in the sulfide of step 2 Silver From Ore:
Filter residue in step 1 is put into 400mL beaker together with filter paper, concentrated hydrochloric acid 100ml is added, is heated to 250 DEG C of guarantors
Boiling 30 minutes is held, is filtered with qualitative fast grade filter paper, precipitating is washed 3~5 times with 2% dilute hydrochloric acid, is washed with water and washs precipitating 2 times,
It collects filtrate and washing lotion is collectively disposed in 250mL beaker, heating is concentrated into 5mL, and 10mL chloroazotic acid is added, and heating is steamed extremely on electric furnace
It is close dry, 8mL concentrated hydrochloric acid is added, purges watch glass and wall of cup with water, is heated to boiling, removes and be cooled to room temperature, be settled to water
It in 50mL volumetric flask, shakes up, static 30min；With the silver content in liquid in aas determination volumetric flask, i.e. sulphur in ore
Ag content in compound；
The measurement of natural silver content in step 3 ore:
Filter residue filtered in step 2 is transferred in 400mL beaker together with filter paper, it is 50% that 100ml concentration, which is added,
HNO3In boiling leaching 30min on electric furnace, filtered with qualitative fast grade filter paper, with 2% HNO3Washing precipitating 3~5 times, then use water
Washing precipitating 2 times, collects filtrate and washing lotion is collectively disposed in 250mL beaker, and heating is concentrated into 5mL, 10mL chloroazotic acid is added, in electricity
Heating is steamed near dry on furnace, and 8mL concentrated hydrochloric acid is added, and is purged watch glass and wall of cup with water, is heated to boiling, removes and be cooled to room temperature,
It is settled in 50mL volumetric flask, is shaken up with water, static 30min, with the silver content in liquid in aas determination volumetric flask,
Native silver (Ag as in ore0) content；
The measurement of silver content in gangue in step 4 ore:
Filter residue filtered in step 3 is put into porcelain crucible together with filter paper, is ashed on electric furnace, and in Muffle furnace
Calcination 1 hour, residue is transferred in polytetrafluoroethylene beaker at 650 DEG C, and 5mL concentrated hydrochloric acid, 3mL concentrated nitric acid, the dense height of 3mL is added
The dense hydrofluoric acid of chloric acid, 2mL is steamed near dry in dissolving by heating on electric furnace, and 8mL concentrated hydrochloric acid is added, and is purged watch glass and wall of cup with water, is added
Heat is removed and is cooled to room temperature, be settled in 50mL volumetric flask, shaken up with water, static 30min is surveyed with atomic absorption method to boiling
Silver in constant volume measuring bottle in liquid, as content silver-colored in gangue in ore；
The measurement of step 5 Silver From Ore total amount:
0.3~0.5g rock sample is weighed in 250mL beaker, water is added to soak, concentrated hydrochloric acid 15mL is added, covers watch glass,
In being heated 2~3 minutes on electric hot plate, remove cooling, 10mL concentrated nitric acid and the dense perchloric acid of 3mL be added, be placed on electric hot plate plus
Heat steams to wet salt, removes and be cooled to room temperature, and 15mL concentrated hydrochloric acid is added, and rinses watch glass and wall of cup with water, is heated to boiling, take
Lower cooling, is settled in 100mL volumetric flask with water, is shaken up, with the silver content of solution in aas determination volumetric flask, as
Silver-colored total amount in rock sample.
It is described Step 1: in step 2 and step 3, the preparation method of chloroazotic acid are as follows: ρ is that 1.19g/mL concentrated hydrochloric acid is with ρ
1.42g/mL concentrated nitric acid volume ratio is 3:1, matching while using.
The step 1 is into step 5, and instrument is Atomic Absorption Spectrometer and silver when using aas determination
Hollow cathode lamp, wavelength 328.1nm；
The preparation method of standard series: pipette 0.00,0.50,1.00,2.00,3.00,4.00,5.00mL silver label standard it is molten
Liquid, is respectively placed in six 100mL volumetric flasks, is diluted to scale with 15% hydrochloric acid solution, mixes, is returned to zero with reagent blank, surveys
Absorbance is measured, using silver concentration as abscissa, absorbance is ordinate, draws working curve；
The preparation method of silver-colored standard solution is as follows:
The configuration of the quasi- stock solution of silver label:
The silver for weighing 0.5000g fine silver i.e. mass fraction >=99.99% of Ag is placed in 100mL beaker, and 20mL nitre is added
Sour (50%), is heated to being completely dissolved, and boils and drives away nitrogen oxide to the disappearance of rufous gas, cooling is removed, with without chlorine
The water of ion moves into 1000mL brown volumetric flask, and addition 30mL ρ is 1.42g/mL concentrated nitric acid, is diluted to not chloride ion-containing water
Scale mixes, this solution 1mL is containing 0.500mg silver；
Silver-colored standard solution: pipetting the quasi- stock solution of the above-mentioned silver label of 50.00mL in 500mL brown volumetric flask, and 10mL ρ is added
For 1.42g/mL concentrated nitric acid, it is diluted to scale with not chloride ion-containing water, is mixed, this solution 1mL is containing 50 μ g silver.
The step 1 is into step 5, the calculation formula of silver content are as follows:
Specific embodiment
Instrument is Atomic Absorption Spectrometer and silver-colored hollow cathode lamp, wavelength 328.1nm when aas determination；
The preparation method of standard series: pipette 0.00,0.50,1.00,2.00,3.00,4.00,5.00mL silver label standard it is molten
Liquid, is respectively placed in six 100mL volumetric flasks, is diluted to scale with 15% hydrochloric acid solution, mixes, is returned to zero with reagent blank, surveys
Absorbance is measured, using silver concentration as abscissa, absorbance is ordinate, draws working curve；
The preparation method of silver-colored standard solution is as follows:
The configuration of the quasi- stock solution of silver label:
The silver for weighing 0.5000g fine silver i.e. mass fraction >=99.99% of Ag is placed in 100mL beaker, and 20mL nitre is added
Sour (50%), is heated to being completely dissolved, and boils and drives away nitrogen oxide to the disappearance of rufous gas, cooling is removed, with without chlorine
The water of ion moves into 1000mL brown volumetric flask, and addition 30mL ρ is 1.42g/mL concentrated nitric acid, is diluted to not chloride ion-containing water
Scale mixes, this solution 1mL is containing 0.500mg silver；
Silver-colored standard solution: pipetting the quasi- stock solution of the above-mentioned silver label of 50.00mL in 500mL brown volumetric flask, and 10mL ρ is added
For 1.42g/mL concentrated nitric acid, it is diluted to scale with not chloride ion-containing water, is mixed, this solution 1mL is containing 50 μ g silver.
Embodiment 1
Due in the market without the standard specimen of silver-colored object phase, use the sample prepared as standard specimen in this method, specific preparation side
Method and content are as follows: accurately weighing silver chlorate 0.0100g, silver sulfide 0.0100g, powdered silver-colored simple substance 0.0100g, silica
49.9700g, silver content in horn silver, to be converted into g/t mono- for silver content in silver content, natural silver content and gangue in silver sulfide
Position is respectively 150.5,87.1,200.0,0.0, and silver-colored total amount standard value is 437.6g/t in the standard sample, is mixed, by with lower section
Method measurement:
The measurement of silver content in horn silver (AgCl) in step 1 ore:
Rock sample of the 0.5105g granularity less than 0.075mm is weighed in 200mL conical flask, leaching agent i.e. 5% is added
Ammonium hydroxide 100ml covers rubber plug, vibrates 30 minutes under room temperature state, is filtered with qualitative fast grade filter paper, with 2% ammonia scrubbing precipitating 6
It~7 times, is washed again with water precipitating 2 times, collects filtrate and washing lotion is collectively disposed in 250mL beaker, heating is concentrated into 5mL, is added
10mL chloroazotic acid is heated on electric furnace and is steamed near dry, and 8mL concentrated hydrochloric acid is added, and is purged watch glass and wall of cup with water, is heated to boiling, take
Under be cooled to room temperature, be settled in 50mL volumetric flask, shaken up with water, static 30min, with liquid in aas determination volumetric flask
The content of Ag in the silver content of body, as horn silver (AgCl)；
In step 2 ore in silver sulfide silver content measurement:
Filter residue in step 1 is put into 400mL beaker together with filter paper, concentrated hydrochloric acid 100ml is added, is heated to 250 DEG C of guarantors
Boiling 30 minutes is held, is filtered with qualitative fast grade filter paper, precipitating is washed 3~5 times with 2% dilute hydrochloric acid, is washed with water and washs precipitating 2 times,
It collects filtrate and washing lotion is collectively disposed in 250mL beaker, heating is concentrated into 5mL, and 10mL chloroazotic acid is added, and heating is steamed extremely on electric furnace
It is close dry, 8mL concentrated hydrochloric acid is added, purges watch glass and wall of cup with water, is heated to boiling, removes and be cooled to room temperature, be settled to water
It in 50mL volumetric flask, shakes up, static 30min；With the silver content in liquid in aas determination volumetric flask, i.e. sulphur in ore
Change Ag content in silver；
The measurement of natural silver content in step 3 ore:
Filter residue filtered in step 2 is transferred in 400mL beaker together with filter paper, it is 50% that 100ml concentration, which is added,
HNO3In boiling leaching 30min on electric furnace, filtered with qualitative fast grade filter paper, with 2% HNO3Washing precipitating 3~5 times, then use water
Washing precipitating 2 times, collects filtrate and washing lotion is collectively disposed in 250mL beaker, and heating is concentrated into 5mL, 10mL chloroazotic acid is added, in electricity
Heating is steamed near dry on furnace, and 8mL concentrated hydrochloric acid is added, and is purged watch glass and wall of cup with water, is heated to boiling, removes and be cooled to room temperature,
It is settled in 50mL volumetric flask, is shaken up with water, static 30min, with the silver content in liquid in aas determination volumetric flask,
Native silver (Ag as in ore0) content；
The measurement of silver content in gangue in step 4 ore:
Filter residue filtered in step 3 is put into porcelain crucible together with filter paper, is ashed on electric furnace, and in Muffle furnace
Calcination 1 hour, residue is transferred in polytetrafluoroethylene beaker at 650 DEG C, and 5mL concentrated hydrochloric acid, 3mL concentrated nitric acid, the dense height of 3mL is added
The dense hydrofluoric acid of chloric acid, 2mL is steamed near dry in dissolving by heating on electric furnace, and 8mL concentrated hydrochloric acid is added, and is purged watch glass and wall of cup with water, is added
Heat is removed and is cooled to room temperature, be settled in 50mL volumetric flask, shaken up with water, static 30min is surveyed with atomic absorption method to boiling
Silver in constant volume measuring bottle in liquid, as content silver-colored in gangue in ore；
The measurement of step 5 Silver From Ore total amount:
0.5105g rock sample is weighed in 250mL beaker, water is added to soak, concentrated hydrochloric acid 15mL is added, covers watch glass, in
It is heated 2~3 minutes on electric hot plate, cooling is removed, 10mL concentrated nitric acid and the dense perchloric acid of 3mL is added, is placed on electric hot plate and heats,
It steams to wet salt, removes and be cooled to room temperature, 15mL concentrated hydrochloric acid is added, watch glass and wall of cup are rinsed with water, is heated to boiling, remove cold
But, it is settled in 100mL volumetric flask, is shaken up with water, with the silver content of solution in aas determination volumetric flask, as ore
Silver-colored total amount in sample.
It is described Step 1: in step 2 and step 3, the preparation method of chloroazotic acid are as follows: ρ is that 1.19g/mL concentrated hydrochloric acid is with ρ
1.42g/mL concentrated nitric acid volume ratio is 3:1, matching while using.
The step 1 is into step 5, the calculation formula of silver content are as follows:
In formula: the mass fraction of ω (Ag)-silver, g/t；
The concentration for the silver that c-is checked in from working curve, unit are μ g/mL；
V-test solution constant volume, unit mL；
M-sample quality, wherein step 2 this quality into step 4 is that the matter of rock sample is weighed in step 1
Amount, unit g；
Analysis result indicate to decimal point after first.
Concentrated hydrochloric acid ρ described in the step 1 to step 5 kind is 1.19g/mL, and concentrated nitric acid ρ is 1.42g/mL, perchloric acid ρ
For 1.67g/mL, hydrofluoric acid 1.15g/mL.
Data processing:
According to rock sample quality m0The concentration of=0.5105g, the silver checked in from working curve are respectively in horn silver
Silver concentration C1=1.52 μ g/mL, silver concentration C in silver sulfide2=0.90 μ g/mL, silver concentration C in native silver3=2.02 μ g/mL, arteries and veins
Silver concentration C in stone4=0.001 μ g/mL, the silver concentration C in silver-colored total amount5=1.32 μ g/mL, constant volume are respectively V1=
50mL, V2=50mL, V3=50, V4=50mL, V5=100mL calculates separately every silver content according to above-mentioned formula, specifically
Data and the result is as follows:
The calculation formula of silver-colored standard value is as follows in the sample wherein prepared:
In formula: the mass fraction of ω (Ag)-silver is indicated with g/t；
m0The quality of this compound, unit g are weighed when-preparation standard specimen；
MAgThe relative atomic weight of-silver, 108g/mol；
M0- weigh the relative molecular weight of silver compound, unit g/mol；
mAlwaysGross mass when-production standard specimen, unit g.
M when wherein measuring silver chlorate0=0.0100g, M0It is the relative molecular weight of silver chlorate；M when measuring silver sulfide0
=0.0100g, M0It is the relative molecular weight of silver sulfide；M when measuring native silver0=0.0100g, M0It is the relative molecular weight of silver；It surveys
M when measuring silver in gangue0=0.0000g, M0It is the relative molecular weight of gangue；MAlways=50.0000g.
It can be seen that compared with standard specimen by above-mentioned experiment, difference is small, it was demonstrated that the analysis method of silver-colored object phase can in this method
It leans on.
Claims (5)
1. a kind of analysis method of Silver From Ore object phase, it is characterised in that include the following steps:
The measurement of silver content in horn silver (AgCl) in step 1 ore:
Rock sample of 0.5000~1.0000g granularity less than 0.075mm is weighed in 200mL conical flask, leaching agent, which is added, is
5% ammonium hydroxide 100ml covers rubber plug, vibrates 30 minutes under room temperature state, is filtered with qualitative fast grade filter paper, with 2% ammonia scrubbing
Precipitating 6~7 times is washed precipitating 2 times again with water, collects filtrate and washing lotion is collectively disposed in 250mL beaker, and heating is concentrated into 5mL,
10mL chloroazotic acid is added, heats and is steamed near dry on electric furnace, 8mL concentrated hydrochloric acid is added, purges watch glass and wall of cup with water, is heated to boiling
It rises, removes and be cooled to room temperature, be settled in 50mL volumetric flask, shaken up with water, static 30min, with aas determination capacity
The silver content of liquid, the content of Ag as in horn silver (AgCl) in bottle；
The measurement of silver content in the sulfide of step 2 Silver From Ore:
Filter residue in step 1 is put into 400mL beaker together with filter paper, concentrated hydrochloric acid 100ml is added, is heated to 250 DEG C of holding boilings
It rises 30 minutes, is filtered with qualitative fast grade filter paper, wash precipitating 3~5 times with 2% dilute hydrochloric acid, be washed with water and wash precipitating 2 times, collect
Filtrate and washing lotion are collectively disposed in 250mL beaker, and heating is concentrated into 5mL, and 10mL chloroazotic acid is added, and heating is steamed to close on electric furnace
It is dry, 8mL concentrated hydrochloric acid is added, purges watch glass and wall of cup with water, is heated to boiling, removes and be cooled to room temperature, 50mL is settled to water
It in volumetric flask, shakes up, static 30min；With the silver content in liquid in aas determination volumetric flask, i.e. sulfide in ore
Middle Ag content；
The measurement of natural silver content in step 3 ore:
Filter residue filtered in step 2 is transferred in 400mL beaker together with filter paper, the HNO that 100ml concentration is 50% is added3In
Leaching 30min is boiled on electric furnace, is filtered with qualitative fast grade filter paper, with 2% HNO3Washing precipitating 3~5 times, be washed with water wash it is heavy
It forms sediment 2 times, collects filtrate and washing lotion is collectively disposed in 250mL beaker, heating is concentrated into 5mL, and 10mL chloroazotic acid is added, and adds on electric furnace
Heat is steamed near dry, and 8mL concentrated hydrochloric acid is added, and is purged watch glass and wall of cup with water, is heated to boiling, removes and be cooled to room temperature, fixed with water
Hold into 50mL volumetric flask, shakes up, static 30min, with the silver content in liquid in aas determination volumetric flask, as mine
Native silver (Ag in stone0) content；
The measurement of silver content in gangue in step 4 ore:
Filter residue filtered in step 3 is put into porcelain crucible together with filter paper, is ashed on electric furnace, and 650 in Muffle furnace
Calcination 1 hour, residue is transferred in polytetrafluoroethylene beaker at DEG C, be added 5mL concentrated hydrochloric acid, 3mL concentrated nitric acid, the dense perchloric acid of 3mL,
The dense hydrofluoric acid of 2mL is steamed near dry in dissolving by heating on electric furnace, and 8mL concentrated hydrochloric acid is added, and is purged watch glass and wall of cup with water, is heated to
Boiling, is removed and is cooled to room temperature, be settled in 50mL volumetric flask, shaken up with water, static 30min is held with aas determination
Silver in measuring bottle in liquid, as content silver-colored in gangue in ore；
The measurement of step 5 Silver From Ore total amount:
0.3~0.5g rock sample is weighed in 250mL beaker, water is added to soak, concentrated hydrochloric acid 15mL is added, watch glass is covered, in electricity
It is heated 2~3 minutes on hot plate, cooling is removed, 10mL concentrated nitric acid and the dense perchloric acid of 3mL is added, is placed on electric hot plate and heats, is steamed
It to wet salt, removes and is cooled to room temperature, 15mL concentrated hydrochloric acid is added, watch glass and wall of cup are rinsed with water, is heated to boiling, remove cold
But, it is settled in 100mL volumetric flask, is shaken up with water, with the silver content of solution in aas determination volumetric flask, as ore
Silver-colored total amount in sample.
2. a kind of analysis method of Silver From Ore object phase according to claim 1, it is characterised in that described Step 1: step
Two and step 3 in, the preparation method of chloroazotic acid are as follows: ρ is 1.19g/mL concentrated hydrochloric acid and ρ be 1.42g/mL concentrated nitric acid volume ratio is 3:
1, matching while using.
3. a kind of analysis method of Silver From Ore object phase according to claim 1, it is characterised in that the step 1 to step
In rapid five, instrument is Atomic Absorption Spectrometer and silver-colored hollow cathode lamp, wavelength when using aas determination
328.1nm；
The preparation method of standard series: pipetting 0.00,0.50,1.00,2.00,3.00,4.00,5.00mL silver standard solution, point
It is not placed in six 100mL volumetric flasks, is diluted to scale with 15% hydrochloric acid solution, mix, returned to zero with reagent blank, measure extinction
Degree, using silver concentration as abscissa, absorbance is ordinate, draws working curve；
The preparation method of silver-colored standard solution is as follows:
The configuration of the quasi- stock solution of silver label:
The silver for weighing 0.5000g fine silver i.e. mass fraction >=99.99% of Ag is placed in 100mL beaker, and 20mL nitric acid is added
(50%), be heated to being completely dissolved, boil drive away nitrogen oxide to rufous gas disappear, remove cooling, with without chlorine from
The water of son moves into 1000mL brown volumetric flask, and addition 30mL ρ is 1.42g/mL concentrated nitric acid, is diluted to quarter with not chloride ion-containing water
Degree mixes, this solution 1mL is containing 0.500mg silver；
Silver-colored standard solution: pipetting the quasi- stock solution of the above-mentioned silver label of 50.00mL in 500mL brown volumetric flask, and 10mL ρ is added and is
1.42g/mL concentrated nitric acid is diluted to scale with not chloride ion-containing water, mixes, this solution 1mL is containing 50 μ g silver.
4. a kind of analysis method of Silver From Ore object phase according to claim 1, it is characterised in that the step 1 to step
In rapid five, the calculation formula of silver content are as follows:
In formula: the mass fraction of ω (Ag)-silver, g/t；
The concentration for the silver that c-is checked in from working curve, unit are μ g/mL；
V-test solution constant volume, unit mL；
M-sample quality, wherein step 2 this quality into step 4 is that the quality of rock sample is weighed in step 1, single
Position is g；
Analysis result indicate to decimal point after first.
5. a kind of analysis method of Silver From Ore object phase according to claim 1, it is characterised in that the step 1 to step
Concentrated hydrochloric acid ρ described in rapid five kinds is 1.19g/mL, and concentrated nitric acid ρ is 1.42g/mL, and perchloric acid ρ is 1.67g/mL, and hydrofluoric acid is
1.15g/mL。
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111551509A (en) * | 2020-05-15 | 2020-08-18 | 广东省资源综合利用研究所 | Chemical quantitative analysis method for occurrence state of silver in iron-manganese oxidized ore |
| CN112129718A (en) * | 2020-09-07 | 2020-12-25 | 长沙矿冶研究院有限责任公司 | Chemical phase analysis method for potassium in ore |
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