CN105548334B - Phase state analysis method of Pt, Pd and Au in black rock type platinum group minerals - Google Patents
Phase state analysis method of Pt, Pd and Au in black rock type platinum group minerals Download PDFInfo
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Abstract
The invention discloses a phase state analysis method of Pt, Pd and Au in black rock type platinum group minerals, which combines the mineral composition of black rock, the enrichment form of noble metal elements in the minerals and the properties of the noble metal elements, and simultaneously divides the occurrence phase states of Pt, Pd and Au in the black rock into four phase states of an exchangeable phase, an organic combined phase, a sulfide combined phase and a residue phase by referring to an analysis method of platinum-palladium-gold active states. 5 percent of triammonium citrate, sodium pyrophosphate buffer solution and glacial acetic acid-hydrogen peroxide are respectively used for leaching Pt, Pd and Au in exchangeable phase, organic combination phase and sulfide combination phase, ICP-MS is used for accurately measuring the content of Pt, Pd and Au in each phase state, and theoretical basis is provided for comprehensive utilization of precious metal elements in geological prospecting and black rock.
Description
Technical field
The invention belongs to mineral deposit analysis technical field, and in particular to Pt, Pd, Au phase in a kind of black lithotype platinum group minerals
State analysis method.
Background technology
Main Types to platinum-group element deposit and the regularity of distribution, the essential characteristic of deposit type at present, PGE enrichment disciplines
Deng research it is also far from enough, the classification of platinum-group element deposit is not yet molded.According to petrology, mineralogy and geochemical investigation
As a result, China's platinum family element is now broadly divided into magmatic origin, the magmatic hydrotherm origin cause of formation and sedimentary origin three major types mineral deposit.Differently
The more Metal Metallizations of black shale in matter age turn into geologist's focus of attention at present, particularly find in black rock
Metalliferous deposit be associated with the organic carbon of platinum family element and high content.According to black rock chemical composition result of study, show black
Color shale is the important ore-hosting fissure of platinum family element, platinum family element often with organic matter association, enrichment of the organic matter to platinum family element
It is significant.Such mineral deposit belongs to Exemplary deposition genetic mineral, that is, exogenic platinum-group element deposit, is in the outer dried rhizome of rehmannia
The lower platinum-group element deposit formed of matter effect.Many geologists are main at present for occurrence form in such mineral for platinum family element
The mineralization machanism of the Research on Regularity platinum family element changed from earth formation, PGE with layer position, and its distribution in such mineral
And enriched form is not fully aware of at present, this is also to cause the main reason for platinum family element measure is unstable in black rock.
In recent ten years, domestic and international geologist pays close attention to the different geochronic more Metals Deposit Ores of black rock of research
Effect, particularly find that the metalliferous deposit in black rock is associated with the organic carbon of platinum family element and high content.Such mineral deposit is to remove
A kind of non-traditional PGE deposit types outside magma lithotype PGE mineral deposits.By studying the distribution shape of Pt, Pd, Au in black rock
State, the difference of element difference compatibility can be understood, understand activation, migration and the precipitation enrichment of Pt, Pd, Au under cryogenic
Rule, important information is provided for the geochemical environment residing for precious metal element in research black rock and its regularity of ore formation.
2011, Han Tao etc. was using sequential extraction experiments method to platinum family element in the more metal levels of zunyi, guizhou Black Rock Sequence
Occurrence form has carried out research, it is believed that the PGE in sample may be in commutative reference state, organically-bound, carbonate combination
State, sulfide reference state and residue reference state are present.Due to substantial amounts of carbon and organic matter in black rock be present, have to PGE stronger
Suction-operated, when leaching commutative reference state, leaching agent can not effectively leach wherein PGE.Using heavy-fluid separation of carbon and organic
Matter, because the carbon particle in mineral is too thin, it even if sample granularity reaches 600 mesh, also can not be kept completely separate carbon and mineral facies.Cause
This, PGE is less than the 5% of PGE total amounts in commutative reference state and organically-bound, and in sulfide reference state and residue knot
The PGE closed in state accounts for more than the 90% of total amount.
The content of the invention
It is an object of the invention to provide the Phase Analysis Method of Gold of Pt, Pd, Au in a kind of black lithotype platinum group minerals, thoroughly solves
PGE measure instability problem, for geological prospecting provides more accurate information in black rock.
To achieve the above object, the present invention uses following technical scheme：
Pt, Pd, Au Phase Analysis Method of Gold in a kind of black lithotype platinum group minerals are mineral composition with reference to black rock, expensive
The property of enriched form and precious metal element of the metallic element in such mineral, referring concurrently to the analysis of platinum porpezite Mobile Forms
Method, the Chemical fraction of Pt, Pd, Au in black rock are divided into commutative phase, organically combine phase, sulfide combination phase, residue
Four phases of phase, specific Phase Analysis Method of Gold step are as follows：
（1）Black rock platinum group minerals 10.0g accurately is weighed in 250mL plastic centrifuge cups, the ammonium leaching liquid of adding citric acid three
100mL, 7g potassium rhodanides and sodium cyanide solution 2mL are added, is stirred, it is small to be placed in vibration 8 in 35 DEG C of waters bath with thermostatic control
When, remove, in centrifuge 20 minutes, supernatant was placed in 250mL conical flasks, washing residue, is divided in centrifuge 10
Clock, aqueous phase discarded, residue are standby；
（2）To step（1）20mL hydrochloric acid is added in obtained supernatant, it is 45mL~55mL to boil to liquor capacity, is mended
Add 20mL hydrochloric acid, after being settled to 200mL, pour into the adsorption column made, filtering velocity is l0 ~ 15mL/min, and decompression filters, and drains
Afterwards, each 3 times with salt acid elution conical flask and filter cake, 10 mL, then with water washing adsorption column is distilled every time, 10 mL, washs 2 every time
It is secondary, drain, take out filter cake, put it into 20mL porcelain crucibles, be placed in Muffle furnace, be warming up to 650 DEG C of, taking-ups complete to being ashed
Porcelain crucible, cooling, add 10mL chloroazotic acid and be placed in 180 DEG C of electric hot plate heating extractions, cool down, be settled to 100mL, shake up, utilize
ICP-MS determines Pt, Pd, Au in commutative phase；
（3）To step（1）Residue obtained middle addition 100mL sodium pyrophosphate cushioning liquid, 2g potassium rhodanides and Cymag are molten
Liquid 4mL, is stirred, and is placed in 90 DEG C of waters bath with thermostatic control and is vibrated 2 hours, removes, in centrifuge 20 minutes, supernatant
It is placed in 250mL conical flasks, washing residue, on centrifuge, centrifuges 10 minutes, aqueous phase discarded, residue is standby；
（4）To step（3）20mL hydrochloric acid is added in obtained supernatant, it is about 50mL to boil to liquor capacity, is grasped below
Make same step（2）, determined using ICP-MS and organically combine Pt, Pd, Au in phase；
（5）By step（3）It is residue obtained in 100 DEG C of drying, move into porcelain Noah's ark, 500 DEG C of calcinations 4 hours, cooling, be transferred to
In 250mL plastic centrifuge cups, 20mL glacial acetic acids are added, 60mL pure water, 5g potassium rhodanides is added, fully stirs evenly, be placed in 95 DEG C
Vibrated 4 hours in water bath with thermostatic control, in oscillatory process, add 5mL hydrogen peroxide per hour, add 20mL hydrogen peroxide altogether, remove,
In centrifuge 20 minutes, supernatant was placed in 250mL conical flasks, washing residue, in centrifuge 10 minutes, discarded water
Phase, residue are standby；
（6）To step（5）20mL hydrochloric acid is added in obtained supernatant, it is the mL of 45mL~55 to boil to liquor capacity, with
The lower same step of operation（2）, Pt, Pd, Au in sulfide combination phase are determined using ICP-MS；
（7）By step（5）It is residue obtained to be dried in 105 DEG C, grinding, scorifier is all put into, is separated using tin ensaying
Pt, Pd, Au in enrichment-ICP-MS measure black rock residue phases.
The step（1）The mass concentration of middle Triammonium citrate leaching liquid is 5%.
The step（1）And step（3）The mass concentration of middle sodium cyanide solution is 2%.
The step（2）The mass concentration of middle hydrochloric acid is 5%, and temperature is 50 DEG C~70 DEG C.
The step（2）The temperature of middle distilled water is 60 DEG C~80 DEG C.
The rotating speed of centrifuge is 4000r/min during the centrifugation.
Beneficial effects of the present invention：The foundation of black lithotype platinum group minerals chemistry Phase Analysis Method of Gold, chemically angle look into
Understand that Pt, Pd, Au are being measured existing for each phase, thoroughly solve PGE measure instability problem in black rock, carried for geological prospecting
For more accurate information.Utilize simultaneously " according to it is black look for it is black " and Pt, Pd, Au in the distribution of each phase, opened up prospecting thinking,
Realize the deficient situation looked for ore deposit new breakthrough, thoroughly alleviate China's platinum family Mineral resource of platinum-group element deposit in China.This method
According to the mineralization machanism of black rock, mineralogical property and mineral composition, the occurrence status of platinum family element in black rock are divided into：Can
Exchange phase, organically combine phase, sulfide combination phase, residue phase.Pass through development of new strippant-potassium rhodanide-Cymag, make
Pt, Pd, Au are exposed in potassium rhodanide-Cymag mixing strippant under conditions of aerobic with cyanide complex, and by each phase
State leaching agent effectively leaches, 2Au+4NaCN+O2+2H2O──2NaAu(CN)2+ 2NaOH, it is suppressed that organic matter and carbonaceous are to each
Pt, Pd, Au absorption in phase.Leached respectively with 5% Triammonium citrate, sodium pyrophosphate cushioning liquid, glacial acetic acid-hydrogen peroxide
Commutative phase, Pt, Pd, Au in phase, sulfide combination phase are organically combined, inhaled using 717 anion exchange resin-activated carbon mixing
Attached dose of separation interference element, Pt, Pd, Au content in each phase of ICP-MS Accurate Determinings.Basic understanding Pt, Pd, Au are in black
The distribution of each phase of rock, the comprehensive utilization for precious metal element in geological prospecting and black rock provide theoretical foundation.
At present, in the Chengkou, Chongqing of China Sichuan Wanyuan one area, Hunan Dayong and Cili area, zunyi, guizhou, Yi Jiyun
Different scales platinum family element mineralising is found that in the Black Rock Sequences on ground such as southern Zhanyi County De Ze, Jiangxi Duchang, Zhuji, zhejiang and Tonglu.
The method of the present invention is adapted to the phase state analysis of Pt, Pd, Au in the black rock sample product of each department.
Brief description of the drawings
Fig. 1 is the flow chart of phase state analysis of the present invention.
Fig. 2 is Pt Phase velocity map figures in black lithotype platinum group minerals.
Fig. 3 is Pd Phase velocity map figures in black lithotype platinum group minerals.
Fig. 4 is Au Phase velocity map figures in black lithotype platinum group minerals.
Embodiment
Collection China Guizhou Nayong water Dongxiang, Zun Yi Huang Jiawan, the farming family gulf of Hunan Zhangjiajie, Tong Mushan, three Cha Ping are each
Class black lithotype platinum group minerals, using frequency conversion rotating stainless steel ball-milling crusher machine to 200 mesh, fully mix, be stored in plastics
It is standby in bottle.Raw ore obtains mineral composition and visual estimation content, is shown in Table 1 through light, thin slice isolith ore deposit identification and analysis.
The sample rock-mineral determination result of table 1（Mating plate）
1st, Pt, Pd, Au complete analysis method in black rock
（Tin Fire Assay Concentration-ICP-MS measure Pt Pd Au）
10~20g of sample is weighed, is accurate to 0.1g, by sample and preparative materials（Sodium carbonate 20g, potassium carbonate 20g, borax
25g, silica 25g, glass putty 20g, flour 2g, calcirm-fluoride 2g, the g of potassium nitrate 10）It is put into after mixing in clay crucible, and
Even coverture of the addition with reducing property（Light magnesium oxide+carborundum）, melted 55 minutes at 1130 DEG C.Molten mass is poured into iron
In mould, take out tin button, flatten, be put into ground conical flask.40 mLHC1 are added, load onto forced air cooled tube, it is micro- on 120 DEG C of electric hot plates
It is limpid that boiling decomposes to solution, removes, adds 40ml pure water, slightly cold, and with 0.45 μm of filtering with microporous membrane, precipitation and conical flask are used
5% HCl is washed 5~6 times.Precipitation and filter membrane are put into former conical flask, add chloroazotic acid 10mL, under the protection of forced air cooled tube, in
Dissolve by heating to solution and clarify on low temperature electric hot plate, remove, be dissolved in surely in 50mL colorimetric cylinders.Using Lu as internal standard element, ICP- is used
MS determines Pt, Pd, Au content.
2nd, in black lithotype platinum group minerals Pt, Pd, Au Phase Analysis Method of Gold, mineral composition, your gold with reference to black rock
Belong to the property of enriched form and precious metal element of the element in such mineral, referring concurrently to the analysis side of platinum porpezite Mobile Forms
Method, the Chemical fraction of Pt, Pd, Au in black rock are divided into commutative phase, organically combine phase, sulfide combination phase, residue phase
Four phases, as shown in figure 1, specific Phase Analysis Method of Gold step is as follows：
（1）Black rock platinum group minerals 10.0g accurately is weighed in 250mL plastic centrifuge cups, the ammonium leaching liquid of adding citric acid three
(mass concentration 5%) 100mL, 7g potassium rhodanides and sodium cyanide solution (mass concentration 2%) 2mL are added, be sufficiently stirred
It is even, it is placed in 35 DEG C of waters bath with thermostatic control and vibrates 8 hours, remove, in centrifuge 20 minutes, supernatant was placed in 250mL conical flasks
In, washing residue is standby in centrifuge 10 minutes, aqueous phase discarded, residue；
（2）To step（1）20mL hydrochloric acid is added in obtained supernatant, it is 45mL~55mL to boil to liquor capacity, is mended
Add 20mL hydrochloric acid, after being settled to 200mL, pour into the adsorption column made, filtering velocity is l0 ~ 15mL/min, and decompression filters, and drains
Afterwards, hydrochloric acid is used（Mass concentration is 5%, and temperature is 50 DEG C~70 DEG C）Wash conical flask and each 3 times of filter cake, every time 10 mL, then use
Distilled water（Temperature is 60 DEG C~80 DEG C）Adsorption column is washed, every time 10 mL, wash 2 times, drain, taken out filter cake, put it into
In 20mL porcelain crucibles, it is placed in Muffle furnace, is warming up to 650 DEG C to being ashed completely, takes out porcelain crucible, cooling, add 10mL chloroazotic acid
Be placed in 180 DEG C of electric hot plate heating extractions, cool down, be settled to 100mL, shake up, using ICP-MS determine Pt, Pd in commutative phase,
Au；
（3）To step（1）Residue obtained middle addition 100mL sodium pyrophosphate cushioning liquid, 2g potassium rhodanides and Cymag are molten
Liquid（Mass concentration is 2%）4mL, stir, be placed in 90 DEG C of waters bath with thermostatic control and vibrate 2 hours, remove, in centrifuge from
The heart 20 minutes, supernatant is placed in 250mL conical flasks, washing residue, on centrifuge, is centrifuged 10 minutes, aqueous phase discarded, residue
It is standby；
（4）To step（3）20mL hydrochloric acid is added in obtained supernatant, it is about 50mL to boil to liquor capacity, is grasped below
Make same step（2）, determined using ICP-MS and organically combine Pt, Pd, Au in phase；
（5）By step（3）It is residue obtained in 100 DEG C of drying, move into porcelain Noah's ark, 500 DEG C of calcinations 4 hours, cooling, be transferred to
In 250mL plastic centrifuge cups, 20mL glacial acetic acids are added, 60mL pure water, 5g potassium rhodanides is added, fully stirs evenly, be placed in 95 DEG C
Vibrated 4 hours in water bath with thermostatic control, in oscillatory process, add 5mL hydrogen peroxide per hour, add 20mL hydrogen peroxide altogether, remove,
In centrifuge 20 minutes, supernatant was placed in 250mL conical flasks, washing residue, in centrifuge 10 minutes, discarded water
Phase, residue are standby；
（6）To step（5）20mL hydrochloric acid is added in obtained supernatant, it is the mL of 45mL~55 to boil to liquor capacity, with
The lower same step of operation（2）, Pt, Pd, Au in sulfide combination phase are determined using ICP-MS；
（7）By step（5）It is residue obtained to be dried in 105 DEG C, grinding, scorifier is all put into, is separated using tin ensaying
Pt, Pd, Au in enrichment-ICP-MS measure black rock residue phases.
The rotating speed of centrifuge is 4000r/min when being centrifuged in above steps.
The making of adsorption column：To 20 adsorption columns（Φ32mm）In be separately added into the quantitative filter paper paper pulp of 15mL 0.5% and press
Tightly.The 5%717 anion exchange resin 30mL and activated carbon 2g handled well are added in 600mL0.5% paper pulp, are stirred evenly, so
Each 15mL divides 2 times afterwards is added into 20 adsorption columns respectively, and decompression filters, and compresses.
3rd, the rate of recovery of each phase
The measure of noble metal does not have the related analysis method of thing phase, phase not only so far in black rock, is exactly black
Noble metal full dose is all without the standard method of analysis of correlation in rock, also without corresponding standard substance.Therefore this method is studied
Pt, P d, Au Phase Analysis Method of Gold, its accuracy can only determine the degree of accuracy of method by mark-on reclaims.Take 10g
Tri- different regions of HNY1, HZY1, HTY1, different types of black rock sample product, it is separately added into Pt, Pd, Au standard of respective amount
Solution, recovery testu is carried out by the extracting method of each phase, it the results are shown in Table 2.
The rate of recovery of 2 each phase of table
From experiment, by adding the strippant of development in leaching agent, it can effectively suppress organic carbon substantially, dissociate
Carbon adsorbs to Pt, Pd, Au, the Pt rate of recovery is reached 92.0%~98.1%, the Pd rate of recovery and reaches 92.2%~101%, Au and exist
Commutative phase and the combination phase rate of recovery are slightly insufficient, but can also reach 89.6%~99.2%, meet related specifications requirement.
4th, the detection limit and precision of each phase and full dose method
Black rock HZY1 samples are taken, 12 extraction experiments is carried out respectively by the analysis method of each phase, is united with measured result
The precision of meter method.Equally, by the extraction flow of each phase, 20 blank assays are done, define 3 times of standard deviations of measured value
As the detection limit of method, while consider the sample weighting amount and extension rate of sample, calculate the detection limit of each phase.It the results are shown in Table 3.
Each phase detection limit (3 of table 3σ) and precision (RSD%)
5th, sample phase state analysis
（1）Sample phase state analysis result
Flow is extracted using the phase of this method, to Guizhou Nayong water Dongxiang（HNY1）, Zun Yi Huang Jiawan（HZY1）, Hunan
The farming family gulf of Zhangjiajie（HTY1）, Tong Mushan（HMY2）, San Chaping（HSH12）5 typical black rock sample product carry out Pt, Pd, Au
Phase state analysis, and overall merit is carried out, it is shown in Table 4.From result, each phase leaching sum of each element is total with sample each element
The ratio between amount Pt is 94.4%~101%, Pd is 95.8%~101%, Au is 96.7%~102%.The index fully meets current form
And the ratio between phase state analysis component sum and total amount for using be in 70%~120% technical requirements, illustrate the method for research with compared with
Good accuracy and reappearance.
The sample phase state analysis result of table 4
（2）Pt, Pd, Au Phase velocity map in black lithotype platinum group minerals
According to the result of sample phase state analysis, Pt, Pd, Au can be obtained in black lithotype platinum group minerals in each phase
Distribution map is shown in Fig. 2, Fig. 3, Fig. 4.
From black lithotype platinum group minerals it was found from the distribution situation of Pt, Pd, Au in each phase：
(a), understood with reference to the result of rock-mineral determination, sulphide ore in HMY2 samples（Predominantly pyrite）Content is minimum, Pt,
Pd, Au are also significantly lower than other samples in the distribution of the sample sulfide combination phase.Illustrate Pt, Pd in black rock platinum group minerals,
Au has thiophilicity, and it has certain correlation in the amount of the mineral distributed mutually and the content of sulfide.
(b) distribution of Pt, Pd, Au in phase is organically combined is only second to the distribution of sulfide combination phase, illustrates Pt, Pd, Au
Enrichment in addition to relevant with sulfide, it is also relevant with the absorption of organic carbon.But point of Pt, Pd, Au in phase is organically combined
The content of cloth and organic carbon, full carbon does not have an obvious correlation, and with black rock existing for area it is relevant, that is to say, that it is same
The distribution proportion of individual regional Pt, Pd, Au in phase is organically combined is closer to.Explanation：1）Organic carbon enrichment Pt, Pd, Au energy
Power is very strong, and Pt, Pd, Au enrichment is only and organic carbon is with the presence or absence of relevant, does not have obvious correlation with its content；2）Pt、Pd、
Au enrichment is relevant with geological conditions that black lithotype platinum group minerals are formed, geologic setting.The research conclusion pushes away with some scholars
The conclusion that disconnected PGE enrichment is relevant with organic carbon is coincide.
(c) Pt, Pd except being distributed in combining mutually and organically combining phase in sulfide, are also deposited in commutative phase in black rock
In a part of Pt, Pd.Illustrate under warm and moist environment, Pt, Pd can be adsorbed in the form of compound or complex viscous
Native mineral surfaces exist in clay mineral interlayer.Distributions of the Au in commutative phase and combination phase is relatively low, is because Au
Mainly with sulfide association, and understand some and exist in the form of simple substance Au, structure is more close, stably.
(d) distribution from results showed that Pt, Pd, Au in residue phase is higher, and a portion is probably due to quilt
Silicate is wrapped up and brought into, more important is explanation in black rock some Pt, Pd, Au be with interphase phase and
The form of Independent Mineral is present.
The foundation of black lithotype platinum group minerals chemistry Phase Analysis Method of Gold, chemically angle found out Pt, Pd, Au in each phase
State is existing to be measured, and thoroughly solves PGE measure instability problem in black rock, more accurate information is provided for geological prospecting.
Utilize simultaneously " according to it is black look for it is black " and Pt, Pd, Au in the distribution of each phase, opened up prospecting thinking, it is entirely possible to real in China
The deficient situation looked for ore deposit new breakthrough, thoroughly alleviate China's platinum family Mineral resource of existing platinum-group element deposit.
The general principle and principal character and advantages of the present invention of the present invention has been shown and described above.The skill of the industry
For art personnel it should be appreciated that the present invention is not limited to the above embodiments, described in above-described embodiment and specification is explanation
The principle of the present invention, without departing from the spirit and scope of the present invention, various changes and modifications of the present invention are possible, these
Changes and improvements all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and
Its equivalent thereof.
Claims (6)
1. Pt, Pd, Au Phase Analysis Method of Gold in a kind of black lithotype platinum group minerals, it is characterised in that：With reference to the ore deposit of black rock
Thing composition, the property of enriched form and precious metal element of the precious metal element in such mineral, live referring concurrently to platinum porpezite
Dynamic analysis method, the Chemical fraction of Pt, Pd, Au in black rock are divided into commutative phase, organically combine phase, sulfide knot
Four phase, residue phase phases are closed, specific Phase Analysis Method of Gold step is as follows：
（1）Black rock platinum group minerals 10.0g accurately is weighed in 250mL plastic centrifuge cups, the ammonium leaching liquid of adding citric acid three
100mL, 7g potassium rhodanides and sodium cyanide solution 2mL are added, is stirred, it is small to be placed in vibration 8 in 35 DEG C of waters bath with thermostatic control
When, remove, in centrifuge 20 minutes, supernatant was placed in 250mL conical flasks, washing residue, is divided in centrifuge 10
Clock, aqueous phase discarded, residue are standby；
（2）To step（1）20mL hydrochloric acid is added in obtained supernatant, it is 45mL~55mL to boil to liquor capacity, is added
20mL hydrochloric acid, after being settled to 200mL, pour into the adsorption column made, filtering velocity is l0 ~ 15mL/min, and decompression filters, and drains
Afterwards, each 3 times with salt acid elution conical flask and filter cake, 10 mL, then with water washing adsorption column is distilled every time, 10 mL, washs 2 every time
It is secondary, drain, take out filter cake, put it into 20mL porcelain crucibles, be placed in Muffle furnace, be warming up to 650 DEG C of, taking-ups complete to being ashed
Porcelain crucible, cooling, add 10mL chloroazotic acid and be placed in 180 DEG C of electric hot plate heating extractions, cool down, be settled to 100mL, shake up, utilize
ICP-MS determines Pt, Pd, Au in commutative phase；
（3）To step（1）Residue obtained middle addition 100mL sodium pyrophosphate cushioning liquid, 2g potassium rhodanides and sodium cyanide solution
4mL, stir, be placed in 90 DEG C of waters bath with thermostatic control and vibrate 2 hours, remove, in centrifuge 20 minutes, supernatant was put
In 250mL conical flasks, washing residue, on centrifuge, centrifuge 10 minutes, aqueous phase discarded, residue is standby；
（4）To step（3）20mL hydrochloric acid is added in obtained supernatant, it is 50mL to boil to liquor capacity, and operation is synchronous below
Suddenly（2）, determined using ICP-MS and organically combine Pt, Pd, Au in phase；
（5）By step（3）It is residue obtained in 100 DEG C of drying, move into porcelain Noah's ark, 500 DEG C of calcinations 4 hours, cooling, be transferred to 250mL
In plastic centrifuge cup, 20mL glacial acetic acids are added, 60mL pure water, 5g potassium rhodanides is added, fully stirs evenly, be placed in 95 DEG C of thermostatted waters
Vibrated 4 hours in bath, in oscillatory process, add 5mL hydrogen peroxide per hour, add 20mL hydrogen peroxide altogether, remove, in centrifugation
Machine is centrifuged 20 minutes, and supernatant is placed in 250mL conical flasks, washing residue, and in centrifuge 10 minutes, aqueous phase discarded was residual
Slag is standby；
（6）To step（5）20mL hydrochloric acid is added in obtained supernatant, it is the mL of 45mL~55 to boil to liquor capacity, is grasped below
Make same step（2）, Pt, Pd, Au in sulfide combination phase are determined using ICP-MS；
（7）By step（5）It is residue obtained to be dried in 105 DEG C, grinding, scorifier is all put into, is separated using tin ensaying rich
Pt, Pd, Au in collection-ICP-MS measure black rock residue phases.
2. Pt, Pd, Au Phase Analysis Method of Gold in black lithotype platinum group minerals according to claim 1, it is characterised in that：
The step（1）The mass concentration of middle Triammonium citrate leaching liquid is 5%.
3. Pt, Pd, Au Phase Analysis Method of Gold in black lithotype platinum group minerals according to claim 1, it is characterised in that：
The step（1）And step（3）The mass concentration of middle sodium cyanide solution is 2%.
4. Pt, Pd, Au Phase Analysis Method of Gold in black lithotype platinum group minerals according to claim 1, it is characterised in that：
The step（2）The mass concentration of middle hydrochloric acid is 5%, and temperature is 50 DEG C~70 DEG C.
5. Pt, Pd, Au Phase Analysis Method of Gold in black lithotype platinum group minerals according to claim 1, it is characterised in that：
The step（2）The temperature of middle distilled water is 60 DEG C~80 DEG C.
6. Pt, Pd, Au Phase Analysis Method of Gold in black lithotype platinum group minerals according to claim 1, it is characterised in that：
The rotating speed of centrifuge is 4000r/min during the centrifugation.
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