CN105548334A - 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. Respectively leaching Pt, Pd and Au in exchangeable phase, organic binding phase and sulfide binding phase with 5% triammonium citrate, sodium pyrophosphate buffer solution and glacial acetic acid-hydrogen peroxide, respectively? The ICP-MS accurately measures the contents of Pt, Pd and Au in each phase state, and provides a theoretical basis for comprehensive utilization of noble metal elements in geological prospecting and black rocks.
Description
Technical field
The invention belongs to mineral deposit analysis technical field, be specifically related to the Phase Analysis Method of Gold of Pt, Pd, Au in a kind of black lithotype platinum group minerals.
Background technology
At present to the essential characteristic of the main Types of platinum-group element deposit and the regularity of distribution, deposit type, the research of PGE enrichment discipline etc. is also nowhere near, and the classification of platinum-group element deposit is not yet shaping.According to petrology, mineralogy and geochemical investigation result, now China's platinum family element is mainly divided into magmatic origin, the magmatic hydrotherm origin cause of formation and sedimentary origin three major types mineral deposit.The many Metal Metallizations of different geochronic black shales become the focus that geologist pays close attention at present, and the metalliferous deposit association particularly in discovery black rock has the organic carbon of platinum family element and high-load.According to black rock chemical composition result of study, show that black shale is the important ore-hosting fissure of platinum family element, platinum family element is normal with organic association, organic significant to the enrichment of platinum family element.Such mineral deposit belongs to Exemplary deposition genetic mineral, namely exogenic platinum-group element deposit, is the platinum-group element deposit formed under giving birth to geologic function outside.Platinum family element is the occurrence form at present mineralization machanism of Research on Regularity platinum family element that mainly changes with layer position from stratal configuration, PGE of a lot of geologist in such mineral, and its distribution in such mineral and enriched form not fully aware of at present, this is also cause platinum family element in black rock to measure unstable main cause.
In recent ten years, domestic and international geologist pays close attention to the many Metal Metallizations of the different geochronic black rock of research, and the metalliferous deposit association particularly in discovery black rock has the organic carbon of platinum family element and high-load.Such mineral deposit is the non-traditional PGE deposit type of one except magma lithotype PGE mineral deposit.By research Pt, Pd, Au in black rock distribution, the difference of the different compatibility of element can be understood, understand Pt, Pd, Au activation under cryogenic, migration and precipitation enrichment discipline, for the geochemical milieu in research black rock residing for precious metal element and the regularity of ore formation thereof provide important information.
2011, Han Tao etc. adopt sequential extraction experiments method to carry out research to the occurrence form of platinum family element in the many metal levels of zunyi, guizhou Black Rock Sequence, think that the PGE in sample may exist in conjunction with state in conjunction with state and residue in conjunction with state, sulfide in conjunction with state, organically-bound, carbonate in commutative.Owing to there is a large amount of carbon and organic matter in black rock, there is stronger suction-operated to PGE, commutatively cannot effectively leach wherein PGE in conjunction with leaching agent during state in leaching.Adopt heavy-fluid separation of carbon and organic matter, because the carbon granule in mineral is too thin, even if sample granularity reaches 600 orders, carbon also cannot be made to be separated completely with mineral facies.Therefore, be commutatively less than 5% of PGE total amount in conjunction with PGE in state and organically-bound, and account for more than 90% of total amount in conjunction with state and residue in conjunction with the PGE in state at sulfide.
Summary of the invention
Object of the present invention provides the Phase Analysis Method of Gold of Pt, Pd, Au in a kind of black lithotype platinum group minerals, thoroughly solves PGE in black rock and measures instability problem, for geological prospecting provides information more accurately.
For achieving the above object, the present invention is by the following technical solutions:
The Phase Analysis Method of Gold of Pt, Pd, Au in a kind of black lithotype platinum group minerals, in conjunction with the mineral composition of black rock, the enriched form of precious metal element in such mineral and the character of precious metal element, simultaneously with reference to the analytical approach of platinum porpezite Mobile Forms, the Chemical fraction of Pt, Pd, Au in black rock is divided into commutative phase, combination phase, sulfide in conjunction with phase, residue four phases mutually, concrete Phase Analysis Method of Gold step is as follows:
(1) black rock platinum group minerals 10.0g is accurately taken in 250mL plastic centrifuge cup, adding citric acid three ammonium leaching liquid 100mL, then add 7g potassium rhodanide and sodium cyanide solution 2mL, stir, be placed in 35 DEG C of water bath with thermostatic control vibrations 8 hours, take off, in centrifuge 20 minutes, supernatant was placed in 250mL conical flask, washing residue, in centrifuge 10 minutes, aqueous phase discarded, residue is for subsequent use;
(2) 20mL hydrochloric acid is added in the supernatant obtained to step (1), boil to liquor capacity be 45mL ~ 55mL, add 20mL hydrochloric acid, after being settled to 200mL, pour in the adsorption column made, filtering velocity is l0 ~ 15mL/min, decompress filter, after draining, with salt acid elution conical flask and each 3 times of filter cake, each 10mL, adsorption column is washed again with distilled water, each 10mL, wash 2 times, drain, take out filter cake, put it in 20mL porcelain crucible, be placed in muffle furnace, be warmed up to 650 DEG C complete to ashing, take out porcelain crucible, cooling, add 10mL chloroazotic acid and be placed in 180 DEG C of electric hot plate heating extractions, cooling, be settled to 100mL, shake up, ICP-MS is utilized to measure commutative middle Pt mutually, Pd, Au,
(3) 100mL sodium pyrophosphate buffer solution is added in residue obtained to step (1), 2g potassium rhodanide and sodium cyanide solution 4mL, stir, and is placed in 90 DEG C of water bath with thermostatic control vibrations 2 hours, take off, in centrifuge 20 minutes, supernatant was placed in 250mL conical flask, washing residue, on hydro-extractor, centrifugal 10 minutes, aqueous phase discarded, residue is for subsequent use;
(4) add 20mL hydrochloric acid in the supernatant obtained to step (3), boil and be about 50mL to liquor capacity, below operate same step (2), utilize ICP-MS to measure and organically combine Pt, Pd, Au mutually;
(5) by residue obtained for step (3) in 100 DEG C of oven dry, move into porcelain Noah's ark, 500 DEG C of calcinations 4 hours, cooling, proceed in 250mL plastic centrifuge cup, add 20mL glacial acetic acid, 60mL pure water, then add 5g potassium rhodanide, fully stir evenly, be placed in 95 DEG C of waters bath with thermostatic control vibration 4 hours, in oscillatory process, per hourly add 5mL hydrogen peroxide, add 20mL hydrogen peroxide altogether, take off, in centrifuge 20 minutes, supernatant was placed in 250mL conical flask, washing residue, in centrifuge 10 minutes, aqueous phase discarded, residue is for subsequent use;
(6) add 20mL hydrochloric acid in the supernatant obtained to step (5), boiling to liquor capacity is 45mL ~ 55mL, below operates same step (2), utilizes ICP-MS to measure sulfide and combines Pt, Pd, Au mutually;
(7) by residue obtained for step (5) in 105 DEG C of oven dry, grinding, all puts into scorifier, adopt tin ensaying separation and concentration-ICP-MS measure black rock residue mutually in Pt, Pd, Au.
In described step (1), the mass concentration of Triammonium citrate leaching liquid is 5%.
The mass concentration of described step (1) and the middle sodium cyanide solution of step (3) is 2%.
In described step (2), the mass concentration of hydrochloric acid is 5%, and temperature is 50 DEG C ~ 70 DEG C.
In described step (2), the temperature of distilled water is 60 DEG C ~ 80 DEG C.
Described centrifugal time hydro-extractor rotating speed be 4000r/min.
Beneficial effect of the present invention: the foundation of black lithotype platinum group minerals chemistry Phase Analysis Method of Gold, chemically angle has found out the amount that Pt, Pd, Au exist in each phase, thoroughly solve PGE in black rock and measure instability problem, for geological prospecting provides information more accurately.Utilize simultaneously " according to black look for black " and Pt, Pd, Au in the distribution of each phase, opened up prospecting thinking, what realize platinum-group element deposit in China looks for ore deposit new breakthrough, thoroughly alleviates the situation of the scarcity of China's platinum family Mineral resource.The occurrence status of platinum family element in black rock, according to the mineralization machanism of black rock, mineralogical property and mineral composition, is divided into by this method: commutative phase, organically combine phase, sulfide in conjunction with phase, residue phase.By development of new strippant-potassium rhodanide-sodium cyanide, makes Pt, Pd, Au under the condition of aerobic, is exposed in potassium rhodanide-sodium cyanide mixing strippant, and is effectively leached by each phase leaching agent, 2Au+4NaCN+O with cyanide complex
2+ 2H
2o--2NaAu (CN)
2+ 2NaOH, inhibits organic matter and carbonaceous to the absorption of Pt, Pd, Au in each phase.Pt, Pd, Au in commutative phase, combination phase, sulfide combination is mutually leached respectively with 5% Triammonium citrate, sodium pyrophosphate buffer solution, glacial acetic acid-hydrogen peroxide, 717 anion exchange resins-active carbon mixed adsorbent is utilized to be separated interference element, the content of Pt, Pd, Au in each phase of ICP-MS Accurate Determining.Basic understanding Pt, Pd, Au in the distribution of each phase of black rock, in geological prospecting and black rock, the comprehensive utilization of precious metal element provides theoretical foundation.
At present, in the Black Rock Sequence on the ground such as Wanyuan one, China Sichuan Chengkou, Chongqing area, Dayong, Hunan and area, Cili, zunyi, guizhou and Zhanyi, Yunnan moral pool, Jiangxi Duchang, Zhuji, zhejiang and Tonglu, different scales platinum family element mineralising has been found.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.
Accompanying drawing explanation
Fig. 1 is the process flow diagram of phase state analysis of the present invention.
Fig. 2 is Pt Phase velocity map figure in black lithotype platinum group minerals.
Fig. 3 is Pd Phase velocity map figure in black lithotype platinum group minerals.
Fig. 4 is Au Phase velocity map figure in black lithotype platinum group minerals.
Embodiment
Gather water Dongxiang, Nayong, China Guizhou, Zun Yi Huang Jiawan, the farming family gulf of Zhangjiajie, Hunan, all kinds of black lithotype of Tong Mushan, San Chaping platinum group minerals, adopt frequency conversion rotating stainless steel ball-milling crusher machine to 200 order, fully mix, be stored in plastic bottle for subsequent use.Raw ore, through light, thin slice isolith ore deposit identification and analysis, obtains mineral composition and visual estimation content, in table 1.
Table 1 sample rock-mineral determination result (mating plate)
1, Pt, Pd, Au complete analysis method in black rock
(tin Fire Assay Concentration-ICP-MS measures PtPdAu)
Take sample 10 ~ 20g, be accurate to 0.1g, clay crucible is put into by after sample and preparative materials (sodium carbonate 20g, sal tartari 20g, borax 25g, silicon dioxide 25g, glass putty 20g, flour 2g, calcium fluoride 2g, potassium nitrate 10g) mixing, and evenly add the coverture (light magnesium oxide+silit) of band reducing property, 1130 DEG C of meltings 55 minutes.Molten mass is poured in swage, takes out tin button, flattening, put into ground conical flask.Add 40mLHC1, load onto forced air cooled tube, micro-ly on 120 DEG C of electric hot plates boil that to decompose to solution limpid, take off, add 40ml pure water, slightly cold, with the filtering with microporous membrane of 0.45 μm, precipitation and the conical flask HCl of 5% washs 5 ~ 6 times.Precipitation and filter membrane are put into former conical flask, adds chloroazotic acid 10mL, under the protection of forced air cooled tube, on low temp. electric hot plate, heating for dissolving is clarified to solution, takes off, and is surely dissolved in 50mL color comparison tube.Take Lu as internal standard element, measure the content of Pt, Pd, Au with ICP-MS.
2, the Phase Analysis Method of Gold of Pt, Pd, Au in black lithotype platinum group minerals, in conjunction with the mineral composition of black rock, the enriched form of precious metal element in such mineral and the character of precious metal element, simultaneously with reference to the analytical approach of platinum porpezite Mobile Forms, the Chemical fraction of Pt, Pd, Au in black rock is divided into commutative phase, combination phase, sulfide in conjunction with phase, residue four phases mutually, as shown in Figure 1, concrete Phase Analysis Method of Gold step is as follows:
(1) black rock platinum group minerals 10.0g is accurately taken in 250mL plastic centrifuge cup, adding citric acid three ammonium leaching liquid (mass concentration is 5%) 100mL, then add 7g potassium rhodanide and sodium cyanide solution (mass concentration is 2%) 2mL, stir, be placed in 35 DEG C of water bath with thermostatic control vibrations 8 hours, take off, in centrifuge 20 minutes, supernatant was placed in 250mL conical flask, washing residue, in centrifuge 10 minutes, aqueous phase discarded, residue is for subsequent use;
(2) 20mL hydrochloric acid is added in the supernatant obtained to step (1), boil to liquor capacity be 45mL ~ 55mL, add 20mL hydrochloric acid, after being settled to 200mL, pour in the adsorption column made, filtering velocity is l0 ~ 15mL/min, decompress filter, after draining, with hydrochloric acid, (mass concentration is 5%, temperature is 50 DEG C ~ 70 DEG C) washing conical flask and each 3 times of filter cake, each 10mL, distilled water (temperature is 60 DEG C ~ 80 DEG C) is used to wash adsorption column again, each 10mL, wash 2 times, drain, take out filter cake, put it in 20mL porcelain crucible, be placed in muffle furnace, be warmed up to 650 DEG C complete to ashing, take out porcelain crucible, cooling, add 10mL chloroazotic acid and be placed in 180 DEG C of electric hot plate heating extractions, cooling, be settled to 100mL, shake up, ICP-MS is utilized to measure commutative middle Pt mutually, Pd, Au,
(3) 100mL sodium pyrophosphate buffer solution is added in residue obtained to step (1), 2g potassium rhodanide and sodium cyanide solution (mass concentration is 2%) 4mL, stir, and is placed in 90 DEG C of water bath with thermostatic control vibrations 2 hours, take off, in centrifuge 20 minutes, supernatant was placed in 250mL conical flask, washing residue, on hydro-extractor, centrifugal 10 minutes, aqueous phase discarded, residue is for subsequent use;
(4) add 20mL hydrochloric acid in the supernatant obtained to step (3), boil and be about 50mL to liquor capacity, below operate same step (2), utilize ICP-MS to measure and organically combine Pt, Pd, Au mutually;
(5) by residue obtained for step (3) in 100 DEG C of oven dry, move into porcelain Noah's ark, 500 DEG C of calcinations 4 hours, cooling, proceed in 250mL plastic centrifuge cup, add 20mL glacial acetic acid, 60mL pure water, then add 5g potassium rhodanide, fully stir evenly, be placed in 95 DEG C of waters bath with thermostatic control vibration 4 hours, in oscillatory process, per hourly add 5mL hydrogen peroxide, add 20mL hydrogen peroxide altogether, take off, in centrifuge 20 minutes, supernatant was placed in 250mL conical flask, washing residue, in centrifuge 10 minutes, aqueous phase discarded, residue is for subsequent use;
(6) add 20mL hydrochloric acid in the supernatant obtained to step (5), boiling to liquor capacity is 45mL ~ 55mL, below operates same step (2), utilizes ICP-MS to measure sulfide and combines Pt, Pd, Au mutually;
(7) by residue obtained for step (5) in 105 DEG C of oven dry, grinding, all puts into scorifier, adopt tin ensaying separation and concentration-ICP-MS measure black rock residue mutually in Pt, Pd, Au.
Time centrifugal in above steps, the rotating speed of hydro-extractor is 4000r/min.
The making of adsorption column: add 15mL0.5% quantitative filter paper paper pulp respectively and compress in 20 adsorption columns (Φ 32mm).In the paper pulp of 600mL0.5%, add the 5%717 anion exchange resins 30mL and activated charcoal 2g that handle well, stir evenly, then each 15mL divides and is added 20 adsorption columns for 2 times respectively, decompress filter, compresses.
3, the recovery of each phase
In black rock, the mensuration of noble metal does not only have the analytical approach that thing phase, phase are relevant so far, is exactly the standard method of analysis that in black rock, noble metal full dose is all not relevant, does not have corresponding standard substance yet.Therefore Pt, Pd, Au Phase Analysis Method of Gold of studying of this method, its accuracy can only retrieve the accuracy of defining method by mark-on.Get 10gHNY1, HZY1, HTY1 tri-different regions, dissimilar black rock sample product, add Pt, Pd, Au standard solution of respective amount respectively, carry out recovery testu by the extracting method of each phase, it the results are shown in Table 2.
The recovery of each phase of table 2
From test, by adding the strippant of development in leaching agent, substantially organic carbon, uncombined carbon can be effectively suppressed to adsorb Pt, Pd, Au, make the recovery of Pt reach 92.0% ~ 98.1%, the recovery of Pd reaches 92.2% ~ 101%, Au is slightly not enough with the combination phase recovery in commutative phase, but also can reach 89.6% ~ 99.2%, meet related specifications requirement.
4, the detection limit of each phase and full dose method and precision
Get black rock HZY1 sample, carry out 12 times respectively by the analytical approach of each phase and extract test, by the precision of measured result statistical method.Equally, by the extraction flow process of each phase, do 20 blank assays, 3 times of standard deviations of definition measured value, as the detection limit of method, are considered sample weighting amount and the extension rate of sample simultaneously, are calculated the detection limit of each phase.The results are shown in Table 3.
The each phase detection limit of table 3 (3 σ) and precision (RSD%)
5, sample phase state analysis
(1) sample phase state analysis result
The phase of this method is adopted to extract flow process, Pt, Pd, Au phase state analysis is carried out to the farming family gulf (HTY1) of water Dongxiang, Nayong, Guizhou (HNY1), Zun Yi Huang Jiawan (HZY1), Zhangjiajie, Hunan, the typical black rock sample product of Tong Mushan (HMY2), San Chaping (HSH12) 5, and carry out comprehensive evaluation, in table 4.From result, each element each phase leaching sum is 94.4% ~ 101% with the ratio Pt of the total amount of each element of sample, Pd is 95.8% ~ 101%, Au is 96.7% ~ 102%.This index meets the ratio of component sum that current form and phase state analysis adopt and total amount completely in the technical requirement of 70% ~ 120%, illustrates that the method studied has good accuracy and reappearance.
Table 4 sample phase state analysis result
(2) Pt, Pd, Au Phase velocity map in black lithotype platinum group minerals
The result of phase state analysis per sample, can obtain Pt, Pd, Au distribution plan in each phase in black lithotype platinum group minerals and see Fig. 2, Fig. 3, Fig. 4.
From black lithotype platinum group minerals, Pt, Pd, Au distribution situation in each phase is known:
A (), known in conjunction with the result of rock-mineral determination, in HMY2 sample, sulphide ore (being mainly pyrite) content is minimum, and Pt, Pd, Au are also starkly lower than other samples at this sample sulfide in conjunction with the distribution of phase.Illustrate that in black rock platinum group minerals, Pt, Pd, Au have thiophilicity, and the content of its amount distributed in these mineral facies and sulfide there is certain correlativity.
B the distribution of () Pt, Pd, Au in combination is mutually only second to the distribution of sulfide in conjunction with phase, illustrate that the enrichment of Pt, Pd, Au is except relevant with sulfide, also relevant with the absorption of organic carbon.But Pt, Pd, Au do not have obvious correlativity in the distribution organically combined mutually and organic carbon, the full content of carbon, and relevant with the area that black rock exists, and that is, same regional Pt, Pd, Au distribution proportion in combination is mutually comparatively close.Illustrate: 1) organic carbon enrichment Pt, Pd, Au's is very capable, whether the enrichment of Pt, Pd, Au only exists relevant with organic carbon, does not have obvious correlativity with its content; 2) enrichment and the geologic condition that black lithotype platinum group minerals is formed of Pt, Pd, Au, geologic background are relevant.This research conclusion and some scholars infer that the enrichment of the PGE conclusion relevant with organic carbon is coincide.
C in () black rock, Pt, Pd are except combining mutually at sulfide and organically combining distribution mutually, commutative mutually in also there is a part of Pt, Pd.Illustrate under warm and moist environment, Pt, Pd can be adsorbed on clay mineral surface with the form of compound or complex or exist at clay mineral interlayer.Au is lower with the distribution organically combined mutually in commutative phase, and be because Au is main and sulfide association, and understand some with the existence of the form of simple substance Au, structure is comparatively tight, stable.
D () is from test findings, Pt, Pd, Au residue mutually in distribution higher, wherein a part may be bring into owing to being wrapped up by silicate, more importantly illustrates that some Pt, Pd, Au exist with the form of intermetallics phase and Independent Mineral in black rock.
The foundation of black lithotype platinum group minerals chemistry Phase Analysis Method of Gold, chemically angle has found out the amount that Pt, Pd, Au exist in each phase, thoroughly solves PGE in black rock and measures instability problem, for geological prospecting provides information more accurately.Utilize simultaneously " according to black look for black " and Pt, Pd, Au in the distribution of each phase, opened up prospecting thinking, what completely likely realize platinum-group element deposit in China looks for ore deposit new breakthrough, thoroughly alleviates the situation of the scarcity of China's platinum family Mineral resource.
More than show and describe ultimate principle of the present invention and principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and instructions just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.Application claims protection domain is defined by appending claims and equivalent thereof.
Claims (6)
1. the Phase Analysis Method of Gold of Pt, Pd, Au in a black lithotype platinum group minerals, it is characterized in that: in conjunction with the mineral composition of black rock, the enriched form of precious metal element in such mineral and the character of precious metal element, simultaneously with reference to the analytical approach of platinum porpezite Mobile Forms, the Chemical fraction of Pt, Pd, Au in black rock is divided into commutative phase, combination phase, sulfide in conjunction with phase, residue four phases mutually, concrete Phase Analysis Method of Gold step is as follows:
(1) black rock platinum group minerals 10.0g is accurately taken in 250mL plastic centrifuge cup, adding citric acid three ammonium leaching liquid 100mL, then add 7g potassium rhodanide and sodium cyanide solution 2mL, stir, be placed in 35 DEG C of water bath with thermostatic control vibrations 8 hours, take off, in centrifuge 20 minutes, supernatant was placed in 250mL conical flask, washing residue, in centrifuge 10 minutes, aqueous phase discarded, residue is for subsequent use;
(2) 20mL hydrochloric acid is added in the supernatant obtained to step (1), boil to liquor capacity be 45mL ~ 55mL, add 20mL hydrochloric acid, after being settled to 200mL, pour in the adsorption column made, filtering velocity is l0 ~ 15mL/min, decompress filter, after draining, with salt acid elution conical flask and each 3 times of filter cake, each 10mL, adsorption column is washed again with distilled water, each 10mL, wash 2 times, drain, take out filter cake, put it in 20mL porcelain crucible, be placed in muffle furnace, be warmed up to 650 DEG C complete to ashing, take out porcelain crucible, cooling, add 10mL chloroazotic acid and be placed in 180 DEG C of electric hot plate heating extractions, cooling, be settled to 100mL, shake up, ICP-MS is utilized to measure commutative middle Pt mutually, Pd, Au,
(3) 100mL sodium pyrophosphate buffer solution is added in residue obtained to step (1), 2g potassium rhodanide and sodium cyanide solution 4mL, stir, and is placed in 90 DEG C of water bath with thermostatic control vibrations 2 hours, take off, in centrifuge 20 minutes, supernatant was placed in 250mL conical flask, washing residue, on hydro-extractor, centrifugal 10 minutes, aqueous phase discarded, residue is for subsequent use;
(4) add 20mL hydrochloric acid in the supernatant obtained to step (3), boil and be about 50mL to liquor capacity, below operate same step (2), utilize ICP-MS to measure and organically combine Pt, Pd, Au mutually;
(5) by residue obtained for step (3) in 100 DEG C of oven dry, move into porcelain Noah's ark, 500 DEG C of calcinations 4 hours, cooling, proceed in 250mL plastic centrifuge cup, add 20mL glacial acetic acid, 60mL pure water, then add 5g potassium rhodanide, fully stir evenly, be placed in 95 DEG C of waters bath with thermostatic control vibration 4 hours, in oscillatory process, per hourly add 5mL hydrogen peroxide, add 20mL hydrogen peroxide altogether, take off, in centrifuge 20 minutes, supernatant was placed in 250mL conical flask, washing residue, in centrifuge 10 minutes, aqueous phase discarded, residue is for subsequent use;
(6) add 20mL hydrochloric acid in the supernatant obtained to step (5), boiling to liquor capacity is 45mL ~ 55mL, below operates same step (2), utilizes ICP-MS to measure sulfide and combines Pt, Pd, Au mutually;
(7) by residue obtained for step (5) in 105 DEG C of oven dry, grinding, all puts into scorifier, adopt tin ensaying separation and concentration-ICP-MS measure black rock residue mutually in Pt, Pd, Au.
2. the Phase Analysis Method of Gold of Pt, Pd, Au in black lithotype platinum group minerals according to claim 1, is characterized in that: in described step (1), the mass concentration of Triammonium citrate leaching liquid is 5%.
3. the Phase Analysis Method of Gold of Pt, Pd, Au in black lithotype platinum group minerals according to claim 1, is characterized in that: in described step (1) and step (3), the mass concentration of sodium cyanide solution is 2%.
4. the Phase Analysis Method of Gold of Pt, Pd, Au in black lithotype platinum group minerals according to claim 1, is characterized in that: in described step (2), the mass concentration of hydrochloric acid is 5%, and temperature is 50 DEG C ~ 70 DEG C.
5. the Phase Analysis Method of Gold of Pt, Pd, Au in black lithotype platinum group minerals according to claim 1, is characterized in that: in described step (2), the temperature of distilled water is 60 DEG C ~ 80 DEG C.
6. the Phase Analysis Method of Gold of Pt, Pd, Au in black lithotype platinum group minerals according to claim 1, is characterized in that: described centrifugal time hydro-extractor rotating speed be 4000r/min.
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| 来雅文等: "《峨嵋玄武岩铂钯赋存状态分析》", 《岩矿测试》 * |
| 王君玉等: "《锡试金富集-电感耦合等离子体质谱法测定黑色页岩中的铂族元素》", 《理化检验-化学分册》 * |
| 赵素利等: "《锍镍试金富集-电感耦合等离子体质谱法测定黑色页岩中的铂族元素》", 《岩矿测试》 * |
| 韩涛等: "《贵州遵义黑色岩系多金属层中铂族元素的赋存状态》", 《矿物岩石地球化学通报》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114199978A (en) * | 2020-08-26 | 2022-03-18 | 中国石油化工股份有限公司 | Method for determining contents of metal elements in different occurrence forms in sedimentary rock |
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| CN105548334B (en) | 2018-02-27 |
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