Analysis Of Impurities In 24 Karat (99.9%) Gold Using The .

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APPLICATION NOTE:TECHNOLOGY:INDUSTRY:AN1805ICPMiningAnalysis of Impurities in 24 Karat (99.9%) Gold Using the TeledyneLeeman Labs’ Prodigy Plus ICP-OESJohn Condon, Applications Chemist and Bruce MacAllister, Applications Chemist; Teledyne Leeman LabsP a g e 1IntroductionGold is a bright, reddish-yellow, dense, soft and malleable metal. Normallyfound pure in nuggets or as grains in rocks and alluvial deposits, it can alsobe found alloyed with silver, copper or palladium and occasionally as goldcompounds in minerals. While gold is resistant to most acids, it can bedissolved in aqua regia, as well as alkaline solutions of cyanide, both ofwhich are used in mining and electroplating industries.Due to gold’s resistance to corrosion and electrical conductivity, gold’s primary industrial application is forelectrical connectors, but it can also be used for infrared shielding, colored glass production and dentalapplications. Approximately 10% of the total gold mined is used for industrial purposes, while theremainder is used for investment and jewelry.This application note will demonstrate the ability of the Teledyne Leeman Labs’ Prodigy Plus ICPspectrometer to analyze 24 karat (99.9%) gold for impurities.InstrumentA Prodigy Plus High Dispersion Inductively Coupled Plasma (ICP) Spectrometer equipped with an axialview torch and a Teledyne Cetac ASX-280 120-position autosampler was used to generate the data forthis application note.Figure 1 Prodigy Plus ICP-OESFigure 2 Teledyne CETAC ASX-280 AutosamplerThe Prodigy Plus is a compact benchtop simultaneous ICP-OES system featuring an 800 mm focal lengthEchelle optical system coupled with a mega-pixel Large Format CMOS (L-CMOS) detector. At28 x 28 mm, the active area of the L-CMOS is significantly larger than any other solid-state detectorcurrently used for ICP-OES. This combination allows the Prodigy Plus to achieve higher optical resolutionthan other solid-state detector-based ICP systems. The detector also provides continuous wavelengthcoverage from 165 to 1100 nm permitting measurement over the entire ICP spectrum in a single reading,without sacrificing wavelength range or resolution. This detector design is inherently anti-blooming and iscapable of random access, non-destructive readout that results in a dynamic range of more than sixorders of magnitude. The Prodigy Plus uses a 40.68 MHz rugged, free-running RF Generator, allowing itto handle the most difficult sample matrices, as well as common organic solvents.AN1805 Gold ProdigyPlus ICP OES.docm; 6-Mar-18Sales/Support: 800-634-9942 Main: 603-886-8400110 Lowell Rd, Hudson, NH 03051www.teledyneleemanlabs.com

P a g e 2Sample IntroductionA high-sensitivity sample introduction system ensures that sufficient and steady emission signals aretransmitted to the spectrometer. The sample introduction configuration used for this application note isshown in Table I.Table ISample IntroductionComponentDescriptionPart NumberGlass ConikalPN 120-00463-1Glass Cyclonic with No Center Knockout TubePN 120-00461-2Sample Uptake Tubing0.76 mmPN 309-00069-7Sample Drain Tubing1.14 mmPN 309-00069-4NebulizerSpray ChamberThe Prodigy Plus’s torch is mounted using an innovative twist-n-lock cassette system shown in Figure 3.The design permits operators to remove and replace the torch to the exact same position, providing dayto-day reproducibility and simplified training. Additionally, the twist-lock design automatically connects thecoolant and auxiliary gas flows, eliminating potential errors.Figure 3 Twist-n-Lock Sample IntroductionMethodFor all elements of interest, background correction was performed simultaneously with the peakmeasurement, resulting in improved detection limits. All data was generated using the instrumentoperating parameters listed in Table II.Table IIInstrument Operating ConditionsParameterValueRF Power1.20 kWCoolant Flow16.0 LPMAuxiliary Flow0.2 LPMNebulizer Pressure31 PSIPart NumberPump Rate25 RPMTorchQuartz DemountablePN 318-00167-1Injector2.5 mmPN 318-00161-AQ1Integration TimeAxial 60 secAN1805 Gold ProdigyPlus ICP OES.docm; 6-Mar-18Sales/Support: 800-634-9942 Main: 603-886-8400110 Lowell Rd, Hudson, NH 03051www.teledyneleemanlabs.com

P a g e 3Instrument Detection LimitsA study was performed to determine the Instrument Detection Limits (IDL) in axial view mode for theelements of interest. Detection Limits shown in Table III were determined as concentrationscorresponding to three times the standard deviation of 10 consecutive measurements of the calibrationblank.Table IIIInstrument Detection LimitsElementWavelength (nm)DL .0003Sample PreparationThree gold reference samples were obtained from the Rand Refinery, South Africa for analysis. Thesamples were dissolved in 10% aqua regia and brought to 100 ml in volumetric flasks.Calibration StandardsCalibration Standards were prepared from single-element stock solutions (VHG Labs Standards,Manchester, NH). The final concentrations are listed in Table IV. The standards were not matrix matchedto the samples.AN1805 Gold ProdigyPlus ICP OES.docm; 6-Mar-18Sales/Support: 800-634-9942 Main: 603-886-8400110 Lowell Rd, Hudson, NH 03051www.teledyneleemanlabs.com

P a g e 4Table IV Calibration Standards, ppmElementWavelength, .512Zn202.54800.512AN1805 Gold ProdigyPlus ICP OES.docm; 6-Mar-18Sales/Support: 800-634-9942 Main: 603-886-8400110 Lowell Rd, Hudson, NH 03051www.teledyneleemanlabs.com

P a g e 5An example calibration curve is shown in Figure 4. The curve was based on the calibration of Cd at226.502 nm in axial-view mode.Figure 4 Calibration Curve of Cd at 226.502nmResultsAfter igniting the plasma and allowing a 15-minute warm-up period, the Prodigy Plus was calibrated.Once the calibration was complete, a QC standard was analyzed with acceptance criteria of 10%.Results from the sample analysis are shown in Table V, Table IV and Table VII. Results for each sampleare reported in units of parts per million (mg/Kg), along with standard deviation of the analysis, thecertified value and % recovery. Results are listed as Not Detected (ND), if the measured concentrationwas at or below the IDL.AN1805 Gold ProdigyPlus ICP OES.docm; 6-Mar-18Sales/Support: 800-634-9942 Main: 603-886-8400110 Lowell Rd, Hudson, NH 03051www.teledyneleemanlabs.com

P a g e 6Table VRAuHP1ElementWavelength (nm)Result(mg/Kg)Std DevCertified Value (mg/Kg)% 1.60.0675.1108.7Zn202.54892.30.3187.2105.9AN1805 Gold ProdigyPlus ICP OES.docm; 6-Mar-18Sales/Support: 800-634-9942 Main: 603-886-8400110 Lowell Rd, Hudson, NH 03051www.teledyneleemanlabs.com

P a g e 7Table VI RAuP2ElementWavelength (nm)Result(mg/Kg)Std DevCertified Value (mg/Kg)% .54818.20.1016.2112.3AN1805 Gold ProdigyPlus ICP OES.docm; 6-Mar-18Sales/Support: 800-634-9942 Main: 603-886-8400110 Lowell Rd, Hudson, NH 03051www.teledyneleemanlabs.com

P a g e 8Table VII RAuP5ElementWavelength (nm)Result(mg/Kg)Std DevCertified Value (mg/Kg)% RecoveryAg328.06816.80.0216.5101.9As189.042NDNA 1Bi223.0613.90.30 1Cd226.5020.20.02 1Co228.6150.60.05 1Cr206.149NDNA Mn257.6101.10.001 1Ni221.6480.50.04 1Pb220.3533.10.10 1Pd340.458NDNA 1Pt265.945NDNA 1Rh343.489NDNA 1Sb206.833NDNA 1Se196.090NDNA 2Sn189.991NDNA 1Te214.2812.60.01 1Ti337.280NDNA 1Zn202.5483.50.113.3106.1ConclusionsThe analysis of pure gold for 20 elements was successful using a Teledyne Leeman Labs’ axial-viewProdigy Plus High-Dispersion ICP. Accurate results were obtained for all samples. The image stabilizedplasma and the simultaneous data collection of both peak and background data combine to provideexceptionally precise and stable results.AN1805 Gold ProdigyPlus ICP OES.docm; 6-Mar-18Sales/Support: 800-634-9942 Main: 603-886-8400110 Lowell Rd, Hudson, NH 03051www.teledyneleemanlabs.com

applications. Approximately 10% of the total gold mined is used for industrial purposes, while the remainder is used for investment and jewelry. This application note will demonstrate the ability of the Teledyne Leeman Labs’ Prodigy Plus ICP spectrometer to analyze 24 karat (99.9%) gold for impurities. Instrument

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