WO2012046201A1 - Method of assaying noble metals - Google Patents
Method of assaying noble metals Download PDFInfo
- Publication number
- WO2012046201A1 WO2012046201A1 PCT/IB2011/054398 IB2011054398W WO2012046201A1 WO 2012046201 A1 WO2012046201 A1 WO 2012046201A1 IB 2011054398 W IB2011054398 W IB 2011054398W WO 2012046201 A1 WO2012046201 A1 WO 2012046201A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- noble metals
- sample
- metals
- noble
- extraction
- Prior art date
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/24—Earth materials
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/32—Gas-filled discharge tubes
- H01J37/32009—Arrangements for generation of plasma specially adapted for examination or treatment of objects, e.g. plasma sources
- H01J37/32082—Radio frequency generated discharge
- H01J37/321—Radio frequency generated discharge the radio frequency energy being inductively coupled to the plasma
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/32—Gas-filled discharge tubes
- H01J37/32917—Plasma diagnostics
- H01J37/32935—Monitoring and controlling tubes by information coming from the object and/or discharge
- H01J37/32972—Spectral analysis
Definitions
- noble metals predominantly occur associated with rocks, with the contents usually being very small.
- platinum occurs in the rocks dunite, peridotite and serpentinite.
- Palladium occurs in the form of heavy metal sulfides such as sperrylite, arsenopalladinite, cooperite and stibiopalladinite.
- the noble metals or the minerals containing the noble metal are firstly concentrated (from 0.1 ppm to 30-500 ppm).
- the assaying of noble metals in rock samples or the matrices obtained during the work-up is therefore an essential prerequisite in order to be able to assess whether a work-up is economically feasible or what type of subsequent further concentration and processing steps (smelting process, refining) are required.
- the matrices may be for example concentrates, tailings, slag or filters.
- This assay has classically been carried out by fire assay.
- fire assay refers generally to the analysis of noble metal-comprising raw materials in which the samples of noble metal-comprising ores are dry-chemically fused with a complex mixture of decomposition agents and fluxes.
- the decomposition agent usually comprises lead.
- a lead button in which the noble metals of the sample are in the ideal case completely dissolved is formed and is separated manually from the slag. Since the noble metals ideally collect completely in the lead button, this is also referred to as collector. Further collectors employed are nickel or nickel sulfides.
- the noble metal content is determined gravimetrically after vaporization of the lead (cupellation).
- spectroscopic and spectrometric analytical methods comprise examining the lead button directly by means of various spectroscopic and spectrometric analytical methods. These can be solid-sampling-graphite furnace-atomic absorption spectrometry (SS-GF-AAS); solid-sampling-electrothermal vaporization-inductively coupled plasma- mass spectrometry (SS-ETV-ICP-MS); laser ablation-inductively coupled plasma- mass spectrometry (LA-ICP-MS); spark-optical emission spectrometry (spark-OES); and glow discharge-mass spectrometry (GD-MS) (M. Resano, E. Garcia-Ruiz, M.A. Bellara; F. Vanhaecke, K.S.
- a disadvantage of fire assay is that methods based on it are relatively time-consuming. Typical working times for the analysis carried out manually are about one week. (M. Rehkamper, A.N. Haliday: Talanta 44 (1997) 663-672). The productivity (number of samples which can be analyzed per employee and working day) is therefore low.
- the detection limits which can be achieved in practice are determined by blank analysis carried out on the reagents used and losses or memory effects of the container materials.
- composition of the complex mixtures of fusion agents and fluxes have to be matched precisely to the respective individual sample. This know-how is described, for example, in DE 1 12006002407T5.
- a method of assaying noble metals in a mineral and/or ceramic matrix in the content range from 0.03 to 500 mg/kg which comprises the following steps:
- an assay is the determination of the total content of a particular noble metal in all states. States are, for example,
- charged (ionized) form e.g. as salt.
- the term “noble metal” comprises silver (Ag), gold (Au) and/or the platinum metals ruthenium (Ru), rhodium (Rh), palladium (Pd), iridium (Ir) and/or platinum (Pt).
- platinum metal comprises ruthenium (Ru), rhodium (Rh), palladium (Pd), iridium (Ir) and/or platinum (Pt).
- platinum (Re) is considered to be a noble metal for the purposes of the present patent application.
- the method of the invention can be used for the single determination of a particular noble metal. Furthermore, the method of the invention can be used for the simultaneous determination of two or more noble metals (multiple determination).
- the noble metals are, according to the invention, the analyte (in the case of a single
- the analytes in the case of a multiple determination, i.e. their content is to be determined.
- matrix refers to the constituents of a sample which are not to be analyzed.
- a mineral matrix is a matrix which is made up entirely or predominantly of one or more minerals. Minerals are naturally occurring solids having a defined chemical composition and a particular physical crystal structure.
- An ore is a mineral mixture which is mined because of its metal content. It comprises metal- comprising ore minerals and the gangue which does not comprise metal.
- a ceramic matrix is a matrix which is made up entirely or predominantly of one or more ceramics. Ceramics are articles which have been molded substantially from finely particulate raw materials with addition of water at room temperature and then dried and, in a subsequent firing process, sintered at above 900°C to give harder, durable articles.
- the raw materials can be inorganic. These include, for example, aluminum silicates such as clays and aluminosilicates such as kaolins. As particular raw materials, oxidic raw materials such as aluminum oxide and beryllium oxide are known. Nontoxic raw materials such as silicon carbide, boron nitride and boron carbide are used for producing nonoxidic ceramics.
- Engineering ceramics are ceramic materials whose properties have been optimized for engineering applications. They are inorganic, nonmetallic and polycrystalline. In general, they are molded at room temperature from a raw composition formed by ceramic powder, organic binder and liquid and acquire their typical materials properties only in a sintering process at high temperatures.
- Ceramics are often used as supports in exhaust gas catalysts.
- the method of the invention is used for determining noble metal in exhaust gas catalysts.
- Preferred noble metals here are Rh, Pd and/or Pt.
- the exhaust gas catalysts can be fresh exhaust gas catalysts.
- the method of the invention can be employed for determining successful application of the noble metal in production.
- the exhaust gas catalysts can also be used exhaust gas catalysts.
- the method of the invention can be employed for determining the loss of noble metal or for determining the remaining noble metal.
- the content range of the noble metal to be determined or the noble metals to be determined is from 0.03 to 500 mg/kg.
- the content range of the noble metal to be determined or the noble metals to be determined is preferably from 0.03 to 50 mg/kg.
- the sample to be analyzed is very often present in macroscopic form and in order to be analyzed at all has to be converted into a suitable form. This is achieved, according to the invention, by homogenization. For this purpose, nonseparating or nondiscriminating methods are employed. The method used is preferably milling.
- the average particle size of the homogenized sample is not more than 100 ⁇ , preferably not more than 50 ⁇ . Preference is given to 95% of the particles being smaller than 70 ⁇ .
- the average particle size is the value obtained by measurement by means of laser light scattering of an aqueous suspension of the particles to be examined. Suitable measuring instruments are, for example, those from the Malvern company, e.g. Malvern Mastersizer 2000, or from Sympatec.
- a dilute sodium pyrophosphate solution can be used as dispersion medium. It is advantageous to predisperse the suspension by means of ultrasound in the measurement vessel before measurement, preferably at an ultrasound intensity in the measurement vessel of 100% before and during measurement.
- the method of the invention is, particularly in the case of samples which are known to be inhomogeneous, carried out a plurality of times in order to obtain a representative result from the mean.
- the dry thermal treatment is also referred to as roasted.
- dry thermal treatment means that the samples have a liquid content of 5% by weight or less immediately before or during roasting.
- One or more reducing agents are introduced during the dry thermal treatment.
- reducing agent preference is given to using hydrogen gas or mixtures comprising hydrogen gas.
- the reducing agent can be introduced continuously, semicontinuously or batchwise.
- the reducing agent is preferably introduced continuously.
- the flow is set so that not more than 1500 ml of H2 per g of sample and hour are supplied to the sample. Preference is given to supplying the sample with 500-1000 ml of H2 per g of sample and hour.
- the dry thermal treatment is carried out at a temperature of from 400 to 1200°C preferably from 600 to 1000°C, particularly preferably from 700 to 900°C.
- a very particularly preferred embodiment is thermal treatment at a temperature of 800°C.
- the dry thermal treatment is carried out for a time of from 0.5 to 10 hours, preferably from one to four hours, particularly preferably from 1 .5 to three hours. In a very particularly preferred embodiment, the dry thermal treatment is carried out for a time of two hours.
- a space which is suitable for this purpose.
- such a space will be referred to as a furnace.
- Furnaces suitable for the purposes of the invention are, for example, smelting furnaces, heat treatment furnaces, tube furnaces, chamber furnaces, muffle furnaces, air convection furnaces, vacuum furnaces, rotary tube furnaces or convection drying ovens.
- a preferred furnace is a tube furnace.
- the extraction takes place in an oxidizing medium.
- mixtures of hydrochloric acid and nitric acid preferably a mixture of hydrochloric acid and nitric acid in a volume ratio of 3:1 , which is also known to those skilled in the art as aqua regia.
- the extraction takes place at a temperature of from 20°C to 200°C.
- the extraction preferably commences at a low temperature, e.g. room temperature, and the temperature is increased in steps.
- the extraction can take place with or without movement of the sample. Preference is given to the extraction beginning without movement of the sample and ending with movement of the sample.
- the duration of the extraction is from 10 minutes to 10 hours.
- the duration of the extraction at room temperature is preferably from one to 10 hours, preferably from two to eight hours, very particularly preferably from three to six hours.
- the duration of the extraction at elevated temperature, i.e. at a temperature above room temperature, is preferably from one to
- 60 minutes preferably from five to 30 minutes, very particularly preferably from 10 to
- the extraction begins at a hold time of 4 hours at room temperature and is continued with the following heating profile, with frequent shaking:
- the noble metals are determined quantitatively by means of an atom ic spectrometric analysis method .
- the determination of the noble metals is carried out by means of ICP-MS (inductively coupled plasma mass spectrometry). This method is, for example, described in "Inorganic Mass Spectrometry, Principles and Applications" J.S. Becker, WILEY, 2007, ISBN 978-04-0470- 01200-0; Houk, R. S., Fassel, V. A., Flesch, G. D., Svec, H. J., Gray, A. L. and Taylor, C. E., 1980. Inductively coupled argon plasma as an ion source for mass spectrometric determination of trace elements. Analytical Chemistry 52, 2283-2289; US 5,218,204 and US 6,265,717 B1 . These documents are fully incorporated by reference.
- a measurement system suitable for this task comprises the following basic components:
- ICP flame as ion source for an argon plasma generated by high frequency induction o Interface which connects the plasma operating under atmospheric pressure to the mass spectrometer which is under a high vacuum
- o Lens system for focusing/guiding the ions into a reaction/collision cell
- the measurement system has to be stable against matrix influences on the samples, i.e. the system stability has to be ensured or changes in the signal intensity have to be compensated via internal standardization.
- Possible systematic errors due to matrix-based mass-spectroscopic superimpositions make an effective method for minimizing interference necessary, e.g. in the form of a collision/reaction cell in the ICP-QMS. Solutions to these problems are known to those skilled in the art.
- the acids, water and the gases used have to be sufficiently free of the elements to be determined. The same applies to the apparatuses used.
- Fused silica tube with spherical ground joint and NS 29/32 female ground joint Fused silica tube with spherical ground joint and NS 29/32 female ground joint
- Nitrogen purity at least 99.999% by volume
- Shielding gas shielding gas 5, from Praxair
- a maximum of 7.5 g (+/- 0.1 g) of the sample were weighed to within 0.1 mg into a fused silica boat.
- a Mettler AT 250 analytical balance was used for this purpose. The boat was positioned in the middle of the large fused silica boat.
- the tube furnace was flushed with nitrogen, flow about 4 standard l/h. After the indicator on the furnace showed 800°C, the charged fused silica boat was pushed into the middle of the tube furnace.
- the gas was changed over from nitrogen to hydrogen or a hydrogen-comprising gas mixture and the nitrogen was shut off.
- the flow rate of the hydrogen or hydrogen-comprising gas mixture was recorded.
- the sample was then reduced for 2 hours at the final temperature under hydrogen or a hydrogen-comprising gas mixture.
- the gas was finally changed over to nitrogen again (flow rate about 4 standard l/h) and the introduction of hydrogen or hydrogen-comprising gas mixture was stopped.
- the fused silica boat was pulled into the "cold zone" of the fused silica tube. After cooling, the sample was reweighed.
- the loss on ignition was calculated via the difference from the initial weight.
- the respective final temperature, hydrogen or hydrogen-comprising gas and flow of the hydrogen or hydrogen-comprising gas are shown in table 1 .
- step (a) The sample from step (a) was weighed into a 100 ml volumetric flask and admixed with 20 ml of aqua regia.
- aqua regia is a freshly prepared mixture of hydrochloric acid (density about 1 .18 g/ml) and nitric acid (density about 1 .41 g/ml) in a volume ratio of 3:1.
- the sample was treated on a hotplate according to the following heating profile, with frequent shaking:
- the volumetric flask was made up to the mark with deionized water.
- the clear supernatant solution was diluted one to ten with simultaneous addition of an internal standard.
- an internal standard a mixture of indium, holmium and thallium in a concentration of 10 g/l based on the solution to be measured was added. This solution was analyzed.
- the analysis was carried out using an Agilent 7700x ICP-MS instrument equipped with integrated sample introduction system (ISIS) and high matrix interface (HMI).
- ISIS integrated sample introduction system
- HMI high matrix interface
- Nebulizer pump 0.08 rps
- Atomizer Meinhard; spray chamber: Scott-type; temperature of spray chamber: 2°C
- Plasma conditions RF power: 1550 W; RF matching: 2.1 V; sample depth: 8 mm;
- Ion lenses extract 1 : 0 V; extract 2: -195 V; omega bias: -1 10 V; omega lens: 8.2 V; cell entrance: -40 V; cell exit: -60 V; deflect: -0.6 V; plate bias: -60 V
- Octopole parameters OctP RF: 170 V; OctP bias: -18 V
- Q-pole parameters AMU gain: 122 V; AMU offset: 127 V; axis gain: 0.9992; axis offset: 0.06; QP bias: -15 V
- Detector parameters discriminator 4.5 mV; analogue HV: 1699 V; pulse HV: 933V
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Abstract
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Priority Applications (7)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN2011800486527A CN103154722A (en) | 2010-10-08 | 2011-10-06 | Method of assaying noble metals |
CA2813975A CA2813975A1 (en) | 2010-10-08 | 2011-10-06 | Method of assaying noble metals |
RU2013120716/28A RU2013120716A (en) | 2010-10-08 | 2011-10-06 | METHOD FOR DETERMINING THE CONTENT OF NOBLE METALS |
KR1020137011791A KR20130097788A (en) | 2010-10-08 | 2011-10-06 | Method of assaying noble metals |
EP11830279.3A EP2625516A4 (en) | 2010-10-08 | 2011-10-06 | Method of assaying noble metals |
JP2013532305A JP2013539050A (en) | 2010-10-08 | 2011-10-06 | Analytical method for precious metals |
ZA2013/03258A ZA201303258B (en) | 2010-10-08 | 2013-05-06 | Method of assaying noble metals |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP10187017 | 2010-10-08 | ||
EP10187017.8 | 2010-10-08 |
Publications (1)
Publication Number | Publication Date |
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WO2012046201A1 true WO2012046201A1 (en) | 2012-04-12 |
Family
ID=45927287
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/IB2011/054398 WO2012046201A1 (en) | 2010-10-08 | 2011-10-06 | Method of assaying noble metals |
Country Status (8)
Country | Link |
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EP (1) | EP2625516A4 (en) |
JP (1) | JP2013539050A (en) |
KR (1) | KR20130097788A (en) |
CN (1) | CN103154722A (en) |
CA (1) | CA2813975A1 (en) |
RU (1) | RU2013120716A (en) |
WO (1) | WO2012046201A1 (en) |
ZA (1) | ZA201303258B (en) |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102967568A (en) * | 2012-11-23 | 2013-03-13 | 四川中自尾气净化有限公司 | Method for testing dual-wavelength of light splitting luminosity |
CN103575676A (en) * | 2013-11-07 | 2014-02-12 | 广州有色金属研究院 | Method for analyzing palladium in palladium-carbon catalyst |
CN113075200A (en) * | 2021-03-22 | 2021-07-06 | 成都光明派特贵金属有限公司 | Method for measuring platinum and rhodium content in platinum-rhodium mixed solution |
CN113075199A (en) * | 2021-03-22 | 2021-07-06 | 成都光明派特贵金属有限公司 | Method for measuring rhodium content in high-rhodium-content solution |
Families Citing this family (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106872382A (en) * | 2017-03-24 | 2017-06-20 | 兰州金川新材料科技股份有限公司 | The rapid assay methods of gold in a kind of powdered copper concentrate |
CN113267421A (en) * | 2021-06-29 | 2021-08-17 | 巴斯夫公司 | Method for determining noble metal content |
Family Cites Families (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101526478B (en) * | 2009-02-17 | 2011-09-28 | 中国嘉陵工业股份有限公司(集团) | Method for detecting bullion content of metal carrier catalytic converter |
-
2011
- 2011-10-06 JP JP2013532305A patent/JP2013539050A/en not_active Withdrawn
- 2011-10-06 CN CN2011800486527A patent/CN103154722A/en active Pending
- 2011-10-06 EP EP11830279.3A patent/EP2625516A4/en not_active Withdrawn
- 2011-10-06 CA CA2813975A patent/CA2813975A1/en not_active Abandoned
- 2011-10-06 RU RU2013120716/28A patent/RU2013120716A/en not_active Application Discontinuation
- 2011-10-06 KR KR1020137011791A patent/KR20130097788A/en not_active Application Discontinuation
- 2011-10-06 WO PCT/IB2011/054398 patent/WO2012046201A1/en active Application Filing
-
2013
- 2013-05-06 ZA ZA2013/03258A patent/ZA201303258B/en unknown
Non-Patent Citations (2)
Title |
---|
DATE A.R. ET AL.: "The Potential of fire assay and inductively coupled plasma source mass spectrometry for the determination of platinum group elements in geological materials", ANALYST, vol. 112, September 1987 (1987-09-01), pages 1217 - 1222, XP055081767 * |
See also references of EP2625516A4 * |
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102967568A (en) * | 2012-11-23 | 2013-03-13 | 四川中自尾气净化有限公司 | Method for testing dual-wavelength of light splitting luminosity |
CN102967568B (en) * | 2012-11-23 | 2015-05-20 | 四川中自尾气净化有限公司 | Method for testing dual-wavelength of light splitting luminosity |
CN103575676A (en) * | 2013-11-07 | 2014-02-12 | 广州有色金属研究院 | Method for analyzing palladium in palladium-carbon catalyst |
CN113075200A (en) * | 2021-03-22 | 2021-07-06 | 成都光明派特贵金属有限公司 | Method for measuring platinum and rhodium content in platinum-rhodium mixed solution |
CN113075199A (en) * | 2021-03-22 | 2021-07-06 | 成都光明派特贵金属有限公司 | Method for measuring rhodium content in high-rhodium-content solution |
CN113075199B (en) * | 2021-03-22 | 2023-03-24 | 成都光明派特贵金属有限公司 | Method for measuring rhodium content in high-rhodium-content solution |
CN113075200B (en) * | 2021-03-22 | 2023-03-24 | 成都光明派特贵金属有限公司 | Method for measuring platinum and rhodium content in platinum-rhodium mixed solution |
Also Published As
Publication number | Publication date |
---|---|
RU2013120716A (en) | 2014-11-20 |
CA2813975A1 (en) | 2012-04-12 |
KR20130097788A (en) | 2013-09-03 |
JP2013539050A (en) | 2013-10-17 |
CN103154722A (en) | 2013-06-12 |
EP2625516A1 (en) | 2013-08-14 |
ZA201303258B (en) | 2014-07-30 |
EP2625516A4 (en) | 2015-06-03 |
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