CN103154722A - Method of assaying noble metals - Google Patents

Method of assaying noble metals Download PDF

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CN103154722A
CN103154722A CN2011800486527A CN201180048652A CN103154722A CN 103154722 A CN103154722 A CN 103154722A CN 2011800486527 A CN2011800486527 A CN 2011800486527A CN 201180048652 A CN201180048652 A CN 201180048652A CN 103154722 A CN103154722 A CN 103154722A
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noble metal
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W·格拉塞尔
A·格罗斯
H·帕贝斯特
I·多姆克
A·米哈伊洛夫斯基
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    • 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

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Abstract

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: (a) Dry thermal treatment of a homogenized sample in a reducing atmosphere; (b) Extraction in an oxidizing medium; (c) Atomic spectrometric quantification of the noble metals by means of ICP-QMS.

Description

Measure the method for noble metal
Noble metal plays an important role in our society.They are used for industrial purpose, for example are used for catalyzer, perhaps are used for the jewel purpose.
At occurring in nature, noble metal is mainly with minimum content and rock association usually.For example, platinum is present in rock dunite, peridotite and serpentinite.Palladium exists with the form of heavy metal sulfide such as sperrylite, arsenic palladium ore deposit, cooperite and stibiopalladinite.
They reclaim by means of floatation process or leaching method.In these post-processing steps, at first with noble metal (mineral that perhaps contain described noble metal) concentrated (being concentrated into 30-500ppm by 0.1ppm).
Therefore, in order to assess whether economically feasible or need which kind of further concentrated and procedure of processing (smelting process, refining) subsequently of aftertreatment, it is the prerequisite of necessity that the noble metal in the matrix that obtains during rock sample or aftertreatment is measured.Described matrix can be for example concentrate, mine tailing, slag or filtrate.This mensuration is undertaken by fire assaying usually.At present, term " fire assaying " typically refer to the ore sample that wherein will contain noble metal and distintegrant and flux the fusion of complex mixture dry chemical contain the precious metal raw material analytical approach.
Distintegrant comprises lead usually.In this fire assaying, the noble metal that forms sample wherein is consoluet lead button and with it and slag is manual separates in the ideal case.Because noble metal is collected in lead button ideally fully, so this is also referred to as collecting agent.Other collecting agents used are nickel or nickel sulfide.
In the simplest situation, measure bullion content (cupellation) in the gravimetric analysis mode after the evaporation of lead.
Can also make collecting agent dissolving and by (atom) spectrographic determination noble metal.This for example is described in Date, A.R., Davis, A.E. and Cheung, Y.Y., 1987, The potential of fire assay and inductively coupled plasma source mass spectrometry for the determination of platinum group elements in geological materials, Analyst112 is in 1217-1222.
Other method comprises by various spectrum and spectroscopic analysis methods direct-detection lead button.these can be solid sampling-GFAAS (graphite furnace atomic absorption spectrometry) (SS-GF-AAS), solid sampling electric heating evaporation-inductively coupled plasma mass spectrometry (SS-ETV-ICP-MS), laser ablation-inductively coupled plasma mass spectrometry (LA-ICP-MS), spark emission spectroscopic method (spark-OES) and glow discharge spectrometry (GD-MS) (M.Resano, E.Garcia-Ruiz, M.A.Bellara, F.Vanhaecke, K.S.MacIntosh, Trends in Analytical Chemistry, the 26th volume, the 5th phase, 2007, the 385-395 page).As the modification of dry chemical method, another trace Matrix separation (J.G.Gupta that precipitates by tellurium has for example been described after sample fusion and dissolving subsequently; Talanta36 (1989), 651-656).
Zhiqiang Li, Zhanbo Li, Determination of micro-content gold in geochemical exploration sample by inductively coupled plasma mass spectrometry (ICP-MS) Xibu Tankuang Gongcheng (2010), 22 (6), 116-117 has described and extracted gold by chloroazotic acid from rock sample.Carry out subsequently the trace Matrix separation, the gold of dissolving is adsorbed on the foam of ashing.Subsequently, gold being dissolved in chloroazotic acid and by ICP-MS again analyzes.
Charles Gowing, Philip Potts, Evaluation of a rapid technique for the determination of precious metals in geological samples based on a selective aqua regia leach, Analyst (Cambridge, United Kingdom) (1991), 116 (8), 773-779 has described and extracted noble metal from rock sample.Can measure quantitatively gold, also can measure quantitatively palladium to a certain extent, but can not measure quantitatively all the other platinum metals.
At G.E.M.Hall, C.J.Oates, Performance of commercial laboratories in analysis of geochemical samples for gold and the platinum group elements, Geochemistry:Exploration, Environment, Analysis (2003), 3 (2), in 107-120, by reference material, various the Determining of Noble Metals are compared each other.Find, the analyte recovery of extracting by chloroazotic acid is low and alter a great deal in various matrixes herein.Roasting in advance has different-effect: the recovery of platinum is not higher than 75% of actual value.
The shortcoming of fire assaying is based on its method relatively consuming time.The exemplary operation time of manual analysis is about a week (M.
Figure BDA00003019873600021
, A.N.Haliday:Talanta44 (1997), 663-672).Therefore throughput rate (every analyzable sample size of employee's every workday) is low.
Personnel are intensive takies, uses special analysis equipment and high energy demand to cause the analysis cost of fire assaying high.
In some modification of fire assaying (comprise when with Ni as collecting agent time), in fact attainable detection limit can be determined by the blank analysis that carries out on agents useful for same and loss or the memory effect of container material.
In addition, the composition of the complex mixture of fusion agent and flux must accurately mate with corresponding independent sample.This proprietary technology for example is described in DE112006002407T5.
In order to meet relevant MWC value, for the analyst, the use of noxious material needs the specific safety measure.In addition, due to noxious material evaporation and/or other processing, must take measures with protection of the environment.
Method beyond fire assaying can not quantitative measurement noble metal to be analyzed.
Therefore, the purpose of this invention is to provide the method with above-mentioned shortcoming.
According to the present invention, this purpose is present in the method realization of the noble metal in mineral and/or ceramic matrix with the content of 0.03-500mg/kg by a kind of mensuration, said method comprising the steps of:
(a) in reducing atmosphere dry heat treatment through the sample of homogenizing;
(b) extract in oxide isolation;
(c) by the described metal of ICP-QMS atomic spectrum quantitative test.
With regard to present patent application, also should always think the combination that the invention discloses preferred embodiment.
For the present invention, mensuration is the mensuration that is in the specific noble metal total content under all states.Described state is for example:
-metal (natural);
-with other metal alloy (solid solution);
-exist with the chemical compound form with other element, and/or
-with charged (ionization) form, for example exist as salt.
With regard to present patent application, term " noble metal " comprises silver (Ag), gold (Au) and/or platinum metals ruthenium (Ru), rhodium (Rh), palladium (Pd), iridium (Ir) and/or platinum (Pt).With regard to present patent application, term " platinum metals " comprises ruthenium (Ru), rhodium (Rh), palladium (Pd), iridium (Ir) and/or platinum (Pt).In addition, with regard to present patent application, rhenium (Re) is considered as noble metal.
Method of the present invention can be for measuring separately specific noble metal.In addition, method of the present invention can be used for measuring simultaneously two or more noble metals (many measure).
According to the present invention, described noble metal is a kind of analyte (in the situation that measuring separately) or multiple analytes (in the situation that many measure),, measures their content that is.
Term " matrix " refers to each composition of the sample do not analyzed.
Mineral matrices is matrix whole or that mainly be made of one or more mineral.Mineral are the naturally occurring solid with definite chemical composition and specific physics crystal structure.
The mineral intermixture of ore for exploiting due to its tenor.It comprises metallic ore mineral and metal-free gangue.
Ceramic matrix is matrix whole or that mainly be made of one or more potteries.Pottery is basically by the molded goods of fine grained raw material, wherein at room temperature adds water, and is then dry, and in burning process subsequently, thereby obtain harder and durable goods at 900 ° of above sintering of C.
Raw material can be inorganic.These comprise for example alumina silicate such as clay and aluminosilicate such as porcelain earth.As specific raw material, known oxide raw material such as aluminium oxide and beryllia.Use poisonous material such as silit, boron nitride and boron carbide to prepare non-oxide ceramics.
Engineering ceramics has been optimized the stupalith of using to be used for engineering for its performance.It is inorganic, nonmetallic and polycrystalline.It is usually at room temperature molded by the feedstock composition that forms by ceramic powders, organic binder bond and liquid and only at high temperature obtain its typical material property in sintering process.
The carrier of pottery in being commonly used for exhaust gas catalyst.
In embodiments of the invention, method of the present invention is used for measuring the noble metal of exhaust gas catalyst.Preferred noble metal is Rh, Pd and/or Pt herein.
Described exhaust gas catalyst can be the new system exhaust gas catalyst.In this case, method of the present invention can be used for determining noble metal successful Application aborning.
Described exhaust gas catalyst also can be the exhaust gas catalyst of using.In this case, method of the present invention can be used for measuring the loss of noble metal or is used for measuring remaining noble metal.
According to the present invention, the content of one or more noble metals to be determined is 0.03-500mg/kg.The content of one or more noble metals to be determined is preferably 0.03-50mg/kg.
Sample to be analyzed often exists with macroscopical form, for abundant analysis must convert it into suitable form.According to the present invention, this realizes by homogenizing.For this reason, employing does not separate or stepless method.Method therefor is preferably grinding.
Implement the optimal way of homogenizing for sample is carried out wet-milling.For example, with 100g sample, 575g ZrO 2Ball (
Figure BDA00003019873600041
) and 100g water ground together in bowl mill 15 minutes.After grinding, by screening described sample is separated with ball and with its under reduced pressure at the temperature of 110 ° of C drying at least 12 hours to constant weight.After drying, by manual mortar, that sample is again broken.
According to the present invention, the particle mean size of homogenizing sample preferably is not more than 50 μ m for being not more than 100 μ m.Preferred 95% particle is less than 70 μ m.More preferably 97% particle is less than 75 μ m.
With regard to the application, the value of particle mean size for obtaining by the measurement by the aqueous suspension thing of laser light scattering particle to be detected.Suitable surveying instrument is for example available from those (for example Malvern Mastersizer2000) of Malvern company, perhaps available from those of Sympatec.
In order to prepare the aqueous suspension thing, can be with rare sodium pyrophosphate solution as dispersion medium.Advantageously before measurement by the ultrasound wave in measuring vessel, preferred pre-dispersed suspension under the ultrasonic intensity in 100% measuring vessel before measurement and during measuring.
Those skilled in the art know, due to the heterogencity in rock sample (for example nugget effect), in order to obtain representational result, should analyze material up to 10-20g (paper of M.M ü ller,
Figure BDA00003019873600051
Mainz, 2001, the 119 pages).
For this reason, implement method of the present invention repeatedly to obtain representational result from mean value, particularly be known as in the sample situation of non-homogeneous.
Dry heat treatment is also referred to as roasting.
For the present invention, dry heat treatment means sample have 5 % by weight or content liquid still less before being close to roasting or during roasting.
Introduce one or more reductive agents during dry heat treatment.As reductive agent, preferably use hydrogen or comprise the potpourri of hydrogen.
Described reductive agent can be introduced continuous, semicontinuous or in batches.The preferred reductive agent of introducing continuously.Flow is set so that be not more than the H of 1500ml/g sample hour for described offering sample 2Be preferably the H of described offering sample 500-1000ml/g sample hour 2
Dry heat treatment is at 400-1200 ° of C, and preferred 600-1000 ° of C particularly preferably carries out at the temperature of 700-900 ° of C.Embodiment very particularly preferably is for to heat-treat at the temperature of 800 ° of C.
Dry heat treatment was carried out 0.5-10 hour, and preferred 1-4 hour, particularly preferably 1.5-3 hour.In embodiment very particularly preferably, dry heat treatment was carried out 2 hours.
In order lower sample to be heated the required time temperature required, it advantageously is transferred in the space that is suitable for this purpose.Hereinafter, this space-like refers to heating furnace.
The heating furnace that is suitable for the object of the invention for example is smelting furnace, heat-treatment furnace, tubular furnace, batch-type furnace, muffle furnace, cross-ventilation heating furnace, vacuum furnace, rotary tube furnace or convective drying case.Preferred heating furnace is tubular furnace.
Be extracted in oxide isolation and carry out.Particularly preferably in producing the medium of chlorine under nascent state.According to the present invention, be preferably the potpourri of hydrochloric acid and nitric acid, preferred volume ratio is the hydrochloric acid of 3:1 and the potpourri of nitric acid, those skilled in the art also are called chloroazotic acid.According to the present invention, the potpourri of preferred hydrochloric acid and hydrogen peroxide also.
According to the present invention, be extracted at the temperature of 20-200 ° of C and carry out.Extraction preferably for example begins under room temperature at low temperature, and progressively heats up.
Extraction can in the situation that mobile example or not mobile example carry out.Preferably be extracted in the situation of mobile example not beginning and mobile example when finishing.
Extraction time is 10 minutes to 10 hours.At room temperature, extraction time is preferably 1-10 hour, and preferred 2-8 hour, very particularly preferably 3-6 hour.(namely at the temperature more than room temperature) at elevated temperatures, extraction time is preferably 1-60 minute, and preferred 5-30 minute, very particularly preferably 10-20 minute.
In particularly preferred embodiments, extraction starts from room temperature keeping 4 hours, and proceeds following heating schedule, jolting subsequently:
Under 60 ° of C 15 minutes,
Under 80 ° of C 15 minutes,
Under 100 ° of C 15 minutes,
Under 180 ° of C 15 minutes.
After sample extraction, by atomic spectrometry determination quantitative measurement noble metal.According to the present invention, the mensuration of noble metal is undertaken by ICP-MS (inductively coupled plasma mass spectrometry).The method for example is described in " Inorganic Mass Spectrometry, Principles and Applications ", J.S.Becker, WILEY, 2007, ISBN978-04-0470-01200-0; 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 Chemistry52,2283-2289; US5,218,204 and US6, in 265,717B1.These documents are incorporated in full with for referencial use.
The measuring system that is suitable for this task comprises following basic module:
Zero is used for measuring by internal standardization Sample introduction system (flow injection Sample introduction system), atomizer, the jet chamber of fluid sample)
The zero ionogenic ICP flame as the argon plasma that produces by high-frequency induction
The interface that zero plasma that will under atmospheric pressure operate is connected with mass spectrometer under high vacuum
Zero lens combination for reactive/collision pond that ion is focused/guided to; Gas by the definition of user in described pond minimizes spectral interference
Zero quadrupole rod massenfilter
Zero detecting unit
Zero is used for the vacuum system of interface, ion optics, quadrupole rod and detecting device
Zero data are processed and evaluation unit
Measuring system must be stable for matrix on the impact of sample, that is, must guarantee Systems balanth or must come by internal standardization the variation of compensation signal intensity.The possible systematic error that is caused by the stack of the mass spectrum of matrix base makes must use effective ways so that interference minimizes, for example the collision in ICP-QMS/reaction tank form.These solution of problem schemes are that those skilled in the art are known.
Following examples are set forth the present invention but not are limited by any way.
Embodiment
For the Overall Steps of hereinafter implementing, acid used, water and gas must be substantially free of element to be determined.This is equally applicable to equipment used.
Homogenizing
As specimen material, use with " the Merensky Reef ore " of SARM76 title available from MIKTEK (South Africa).This material is ground (being the homogenizing in the application's intended scope), it has by using available from Sympatec and having the 70 μ m particle mean sizes that the laser light scattering of the instrument of assessment software WINDOX records.Do not carry out further homogenizing.
Step (a): dry heat treatment (roasting)
Equipment:
Little vitreosil boat, L * W * H is about 40 * 13 * 11 (external dimensions) in mm
Large vitreosil boat, L * W * H is about 140 * 23 * 17 (the perforated external dimensions of tool) in mm
Have mark and be used for importing the metal bar of large vitreosil boat
Vitreosil pipe with the cloudy ground connection of spherical ground connection and NS29/32
Model is the Carbolite tubular furnace of STF15/---/180
Reagent:
Hydrogen: purity is at least 99.999 volume %
Nitrogen: purity is at least 99.999 volume %
Protection gas: protection gas 5, available from Praxair
The 7.5g of weighing maximum in the vitreosil boat (+/-0.1g) sample (error range is 0.1mg).For this reason, use Mettler AT250 analytical balance.Described boat is placed in the centre of large vitreosil boat.
With diamond heating during the finishing temperature, be this tubular furnace of nitrogen blowing of approximately 4 standard L/h with flow velocity.After 800 ° of C of the indicator for displaying on heating furnace, the vitreosil boat of charging is pushed the centre of described tubular furnace.
After " purge time " of at least 10 minutes, gas is become hydrogen by nitrogen or comprises the gaseous mixture of hydrogen and close nitrogen.Record hydrogen or comprise the flow velocity of the gaseous mixture of hydrogen.
Then, with sample under described finishing temperature in hydrogen or comprise under the gaseous mixture of hydrogen reductase 12 hour.At last, be nitrogen (flow velocity be approximately 4 standard L/h) again with gas and changing, stop the gaseous mixture of introducing hydrogen or comprising hydrogen.
After " purge time " of other 10 minutes, described vitreosil boat is pulled in " cold-zone " of vitreosil pipe.After cooling, weighing sample again.
By calculating calcination loss with the difference of initial weight.
Finishing temperature, hydrogen or the flow that comprises gas and the hydrogen of hydrogen or comprise the gas of hydrogen are shown in table 1.
Step (b): extract in oxide isolation
Weighing is available from the sample of step (a) and it is mixed with the 20ml chloroazotic acid in the 100ml volumetric flask." chloroazotic acid " is the hydrochloric acid (density is 1.18g/ml approximately) of freshly prepd 3:1 volume ratio and the potpourri of nitric acid (density is 1.41g/ml approximately).
After this, with its at room temperature standing 4 hours.
According to following heating schedule, described sample is processed on hot plate, subsequently jolting:
Under 60 ° of C 15 minutes,
Under 80 ° of C 15 minutes,
Under 100 ° of C 15 minutes,
Under 180 ° of C 15 minutes.
After being cooled to room temperature, with deionized water, volumetric flask is complemented to scale.In the target situation, the supernatant of clarifying is diluted 1-10 doubly in adding at the same time.As interior mark, adding is the potpourri of indium, holmium and the thallium of 10 μ g/l based on solution concentration to be measured.Analyze this solution.
Carry out blank assay according to this description.
Step (c): by ICP-QMS atomic spectrum quantitative measurement noble metal
Use is equipped with the Agilent7700x ICP-MS instrument of integrated Sample introduction system (ISIS) and high basal body interface (HMI) and analyzes.
Operating conditions about analysis is as follows:
Acid concentration: mate with sample
Measurement range: 0.1-30 μ g/l
Calibration: 2/10/30 μ g/l
Atomizer pump: 0.08rps
Atomizer: Meinhard; Jet chamber: Scott type; Jet chamber's temperature: 2 ° of C
Gas arranges: carrier gas: 0.7L/ minute; Plasma gas: 0.9L/ minute: refrigerating gas: 15L/ minute; Diluents: 0.44L/ minute; Pond gas: helium, 4.4ml/ minute; Reaction pattern: open
Condition of plasma: radio-frequency power: 1550W; Radio-frequency match: 2.1V; The sample degree of depth: 8mm; Torch-H:0mm; Torch-V:0.2mm
Ion lens: extract 1:0V; Extract 2:-195V; ω bias voltage :-110V; ω lens: 8.2V; Pond entrance :-40V; Pond outlet :-60V; Deviation :-0.6V; Plate bias voltage :-60V
Ends of the earth bar parameter: ends of the earth bar radio frequency: 170V; Ends of the earth bar bias voltage :-18V
Q utmost point parameter: AMU gain: 122V; AMU skew: 127V; On-axis gain: 0.9992; Axle offset: 0.06; Q utmost point bias voltage :-15V
Detector parameters: recognizer 4.5mV; Simulated high-pressure: 1699V; High voltage pulse: 933V
Table 1: to the experimental result of SARM76 mensuration
Figure BDA00003019873600091
Figure BDA00003019873600101
? Experiment 1 ? Experiment 2 ? Experiment 3 ?
Finishing temperature 800°C ? 800°C ? 800°C ?
Gas H 2 ? H 2 ? H 2 ?
Flow 1.6L/h ? 4L/h ? 10L/h ?
? ? ? ? ? ? ?
? mg/kg RSD mg/kg RSD mg/kg RSD
Pd 1.39 7.52 1.37 5.32 1.38 4.29
Pt 3.81 5.02 3.64 9.89 3.80 4.79
Rh 0.22 3.67 0.22 9.73 0.22 4.89
Au 0.24 11.28 0.21 13.37 0.57 124.73
Figure BDA00003019873600102
N.f.: do not provide data/unavailable
RSD: the relative standard deviation of each result is (in %; N=6, i.e. each measurement is carried out six times)

Claims (5)

1. a mensuration is present in the method for the noble metal in mineral and/or ceramic matrix with the content of 0.03-500mg/kg, said method comprising the steps of:
(a) in reducing atmosphere dry heat treatment through the sample of homogenizing;
(b) extract in oxide isolation;
(c) by the described noble metal of ICP-QMS atomic spectrum quantitative measurement.
2. according to claim 1 method, wherein said noble metal is the platinum metals.
3. according to claim 2 method, wherein said noble metal is platinum, palladium, rhodium and/or iridium.
4. according to claim 1 method, wherein said noble metal is rhenium.
5. according to claim 1 method, wherein said noble metal is gold.
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