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InductivelyCoupledPlasmaMassSpectrometryStudyonDeltaOre 05-24-2015
Edward Mausolf,PhD
mausolfe@unlv.nevada.edu
Abstract
In orderto compare previousmicroscopystudiesthatwascompletedonconverted Deltarecovered
metal phases,abulkICP-MSstudywas completedonthe startingDeltaOre thatis inmy possession.
The figuresinthisreportwere generated duringthe materialdigestandrecovery,while the standards
prepared tocompare the signal response wereprovidedin-house atthe University of NevadaLasVegas
(UNLV). The ICP-MSstandard usedwasa multi-elementstandard(seefigure6,table 2) that containsall
elementsat50 µL/mL (50 ppm) dilutedfrom0to 50 ppb that issuitable formeasurementswithinthe
instrument. The deltasample (5.1509 g) was thenrecoveredinthe solutionphaseafterdigestion. Total
mass withinthe solutionwasestimatedbyevaporatingaknownvolume of solutioncontainingsolutes
and comparedto the driedmass (Figure 4). Thiswas thenbroughtup in1% HNO3 (analytical grade)
thenseriallydiluteduntil asolutionof approximately35.86 ppbDeltasolutionwasproduced. Priorto
introductionintothe instrument,all solutionswere filteredthrough0.2micronsyringe filters.
It shouldbe knownthatthe iron signal appearstobe higherthanthe real value withinthe sampledue to
chargingof argon (Ar) inthe plasma: Iron formulaweight~56 whereasAr-Ohasa formulaweightof ~56
and thisintroduceserrorinthe signal. All otherspecieslistedwithinthat of table 2 trendwell withthe
calibrationpreparedandcomparedtothe Deltasample prepared.
From the resultsof thisdigest,the 4 tonsavailable currently(where thissamplewascollectedfrom) has
a calculatedvalue of approximately$480,000 perton inPGMs (Rh/Pd/Pt/Au),notincludingother
elementsof highconcentrationsuchasCu,Fe,Ni,Ti, Zr, and Mo.
In a fieldof 38,000,000 tons,the predictedvalue of the mine hasavalue of approximately
$18,400,000,000,000 whichiswithinanorderof magnitude of thatpredictedfromthe microscopy
studies. The elementsof primaryvalue andconcentrationare Palladium(Pd),Gold(Au),andPlatinum
(Pt) while otherplatinum-groupmetalssuchasOs bringconcerndue to the toxicityof thiselement.
Future Work
Identificationof uranium, thorium,andvariouslanthanideshave recentlybeenidentifiedinthe Delta
ore. A separationsystemhasbeendevelopedtoremove the Rare EarthElements(REEs) onthe front
endand the projecthas beenfunded. The resultsof thisstudywill be made available followingits
completioninJuly2015.
Figure 1. Bulkdeltaore (5.1509 g) (left),groundinmortarandpestle (center),thenplacedinglassflask
[extractantinorange flask]
Figure 2. Beginningof digest(left) andconsumptionof deltaore (centerlefttoright)
Figure 3. Completeddigestof deltaore (forstudy)
Figure 4. Resultingsolutionphase andrecovereddeltaore afterdigestion(left),comparisonof original
deltaore to digested deltaore (center),andcrystalline phase resultingfromdeltadigestwith sample
usedforICP-MS study(right)
Figure 5. DeltadigeststandardsandsamplesforICP-MSstudy. Deltadigestdilutionfactor:27886224.2
Figure 6. ICP-MSconcentration versussignal countcalibrationcurve (0,1,2, 5, 10, 25, and 50 ppb
standard) – comprehensivestandardcontainsall PGMelementsthatwere compared: Ni,Os,Pd,Pt,Ir,
Os,Pt, Au,Rh. OnlyAu,Pd,and Pt are showninthe standardregression
Table 1. Estimatedconcentrationof keyelementsfoundindeltaore post-digest(yieldperpound)
0
2000
4000
6000
8000
10000
12000
14000
16000
0 10 20 30 40 50 60
SignalCounts
Concentration (ppb)
ICP-MS Standard Signals
Gold
Palladium
Platinum
Analyte g/pound
Ru 0.95
Rh 0.80
Pd 4.15
Os 0.59
Ir 0.26
Pt 1.22
Au 1.67
Table 2. Estimatedvalue of mine calculatedat38,000,000 tons(assumingthe field is isocompositional)
Analyte Mass Conc. Mean (ppb) g/g DF x g/g g in sample g in mine Troy Ounce Value/Oz Pounds Value/lb Estimated Value
Li 7 6.688 6.688E-09 0.187 0.897 6.01E+12 1.32E+10 2.27$ 30,052,296,641.95$
Ti 47 1.03 1.03E-09 0.029 0.138 9.26E+11 2.98E+10 2.04E+09 2.55$ 5,199,157,220.91$
V 51 0.257 2.57E-10 0.007 0.034 2.31E+11 7.43E+09 5.09E+08 9.28$ 4,721,028,747.60$
Cr 52 0.641 6.41E-10 0.018 0.086 5.76E+11 1.85E+10 1.27E+09 1.00$ 1,268,859,614.93$
Mn 55 0.404 4.04E-10 0.011 0.054 3.63E+11 1.17E+10 8.00E+08 0.93$ 743,737,807.36$
Fe 57 14.462 1.4462E-08 0.403 1.940 1.30E+13 4.18E+11 2.86E+10 0.29$ 8,173,160,269.77$
Co 59 0.065 6.5E-11 0.002 0.009 5.84E+10 1.88E+09 1.29E+08 13.65$ 1,756,311,534.08$
Ni 60 0.422 4.22E-10 0.012 0.057 3.79E+11 1.22E+10 8.35E+08 5.90$ 4,928,559,546.40$
Cu 63 19.501 1.9501E-08 0.544 2.616 1.75E+13 5.64E+11 3.86E+10 2.83$ 109,244,319,379.66$
Zn 66 63.156 6.3156E-08 1.761 8.473 5.68E+13 1.83E+12 1.25E+11 1.00$ 125,017,313,323.28$
Zr 90 1.322 1.322E-09 0.037 0.177 1.19E+12 3.82E+10 2.62E+09 13.17$ 34,464,562,951.58$
Nb 93 0.06 6E-11 0.002 0.008 5.39E+10 1.73E+09 1.19E+08 -$ -$
Mo 98 0.103 1.03E-10 0.003 0.014 9.26E+10 2.98E+09 2.04E+08 7.76$ 1,582,174,903.30$
Ru 102 0.08 8E-11 0.002 0.011 7.19E+10 2.31E+09 50.00$ 115,587,534,584.95$
Rh 103 0.068 6.8E-11 0.002 0.009 6.11E+10 1.96E+09 1,080.00$ 2,122,187,134,979.58$
Pd 106 0.351 3.51E-10 0.010 0.047 3.15E+11 1.01E+10 785.50$ 7,967,174,238,545.59$
Sn 118 0.584 5.84E-10 0.016 0.078 5.25E+11 1.69E+10 1.16E+09 7.21$ 8,334,962,634.93$
Hf 180 0.049 4.9E-11 0.001 0.007 4.40E+10 1.42E+09 9.70E+07 -$ -$
W 184 -0.039 0.00E+00 0.00E+00 -$ -$
Os 192 0.05 5E-11 0.001 0.007 4.49E+10 1.44E+09 360.00$ -$ 520,143,905,632.25$
Ir 193 0.022 2.2E-11 0.001 0.003 1.98E+10 6.36E+08 580.00$ -$ 368,724,235,325.97$
Pt 195 0.103 1.03E-10 0.003 0.014 9.26E+10 2.98E+09 1,147.50$ -$ 3,415,394,920,357.77$
Au 197 0.141 1.41E-10 0.004 0.019 1.27E+11 4.07E+09 1,206.00$ -$ 4,913,799,476,507.87$
Valu/lb
Total 519,960.47$
PGM Total 511,131.88$
Rh/Pd/Pt/Au 93.2% 484,698.84$18,418,555,770,390.80$
19,758,497,890,509.70$
19,423,011,445,934.00$

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Delta ICPMS Report Mausolf

  • 1. InductivelyCoupledPlasmaMassSpectrometryStudyonDeltaOre 05-24-2015 Edward Mausolf,PhD mausolfe@unlv.nevada.edu Abstract In orderto compare previousmicroscopystudiesthatwascompletedonconverted Deltarecovered metal phases,abulkICP-MSstudywas completedonthe startingDeltaOre thatis inmy possession. The figuresinthisreportwere generated duringthe materialdigestandrecovery,while the standards prepared tocompare the signal response wereprovidedin-house atthe University of NevadaLasVegas (UNLV). The ICP-MSstandard usedwasa multi-elementstandard(seefigure6,table 2) that containsall elementsat50 µL/mL (50 ppm) dilutedfrom0to 50 ppb that issuitable formeasurementswithinthe instrument. The deltasample (5.1509 g) was thenrecoveredinthe solutionphaseafterdigestion. Total mass withinthe solutionwasestimatedbyevaporatingaknownvolume of solutioncontainingsolutes and comparedto the driedmass (Figure 4). Thiswas thenbroughtup in1% HNO3 (analytical grade) thenseriallydiluteduntil asolutionof approximately35.86 ppbDeltasolutionwasproduced. Priorto introductionintothe instrument,all solutionswere filteredthrough0.2micronsyringe filters. It shouldbe knownthatthe iron signal appearstobe higherthanthe real value withinthe sampledue to chargingof argon (Ar) inthe plasma: Iron formulaweight~56 whereasAr-Ohasa formulaweightof ~56 and thisintroduceserrorinthe signal. All otherspecieslistedwithinthat of table 2 trendwell withthe calibrationpreparedandcomparedtothe Deltasample prepared. From the resultsof thisdigest,the 4 tonsavailable currently(where thissamplewascollectedfrom) has a calculatedvalue of approximately$480,000 perton inPGMs (Rh/Pd/Pt/Au),notincludingother elementsof highconcentrationsuchasCu,Fe,Ni,Ti, Zr, and Mo. In a fieldof 38,000,000 tons,the predictedvalue of the mine hasavalue of approximately $18,400,000,000,000 whichiswithinanorderof magnitude of thatpredictedfromthe microscopy studies. The elementsof primaryvalue andconcentrationare Palladium(Pd),Gold(Au),andPlatinum (Pt) while otherplatinum-groupmetalssuchasOs bringconcerndue to the toxicityof thiselement. Future Work Identificationof uranium, thorium,andvariouslanthanideshave recentlybeenidentifiedinthe Delta ore. A separationsystemhasbeendevelopedtoremove the Rare EarthElements(REEs) onthe front endand the projecthas beenfunded. The resultsof thisstudywill be made available followingits completioninJuly2015.
  • 2. Figure 1. Bulkdeltaore (5.1509 g) (left),groundinmortarandpestle (center),thenplacedinglassflask [extractantinorange flask] Figure 2. Beginningof digest(left) andconsumptionof deltaore (centerlefttoright)
  • 3. Figure 3. Completeddigestof deltaore (forstudy) Figure 4. Resultingsolutionphase andrecovereddeltaore afterdigestion(left),comparisonof original deltaore to digested deltaore (center),andcrystalline phase resultingfromdeltadigestwith sample usedforICP-MS study(right)
  • 4. Figure 5. DeltadigeststandardsandsamplesforICP-MSstudy. Deltadigestdilutionfactor:27886224.2 Figure 6. ICP-MSconcentration versussignal countcalibrationcurve (0,1,2, 5, 10, 25, and 50 ppb standard) – comprehensivestandardcontainsall PGMelementsthatwere compared: Ni,Os,Pd,Pt,Ir, Os,Pt, Au,Rh. OnlyAu,Pd,and Pt are showninthe standardregression Table 1. Estimatedconcentrationof keyelementsfoundindeltaore post-digest(yieldperpound) 0 2000 4000 6000 8000 10000 12000 14000 16000 0 10 20 30 40 50 60 SignalCounts Concentration (ppb) ICP-MS Standard Signals Gold Palladium Platinum Analyte g/pound Ru 0.95 Rh 0.80 Pd 4.15 Os 0.59 Ir 0.26 Pt 1.22 Au 1.67
  • 5. Table 2. Estimatedvalue of mine calculatedat38,000,000 tons(assumingthe field is isocompositional) Analyte Mass Conc. Mean (ppb) g/g DF x g/g g in sample g in mine Troy Ounce Value/Oz Pounds Value/lb Estimated Value Li 7 6.688 6.688E-09 0.187 0.897 6.01E+12 1.32E+10 2.27$ 30,052,296,641.95$ Ti 47 1.03 1.03E-09 0.029 0.138 9.26E+11 2.98E+10 2.04E+09 2.55$ 5,199,157,220.91$ V 51 0.257 2.57E-10 0.007 0.034 2.31E+11 7.43E+09 5.09E+08 9.28$ 4,721,028,747.60$ Cr 52 0.641 6.41E-10 0.018 0.086 5.76E+11 1.85E+10 1.27E+09 1.00$ 1,268,859,614.93$ Mn 55 0.404 4.04E-10 0.011 0.054 3.63E+11 1.17E+10 8.00E+08 0.93$ 743,737,807.36$ Fe 57 14.462 1.4462E-08 0.403 1.940 1.30E+13 4.18E+11 2.86E+10 0.29$ 8,173,160,269.77$ Co 59 0.065 6.5E-11 0.002 0.009 5.84E+10 1.88E+09 1.29E+08 13.65$ 1,756,311,534.08$ Ni 60 0.422 4.22E-10 0.012 0.057 3.79E+11 1.22E+10 8.35E+08 5.90$ 4,928,559,546.40$ Cu 63 19.501 1.9501E-08 0.544 2.616 1.75E+13 5.64E+11 3.86E+10 2.83$ 109,244,319,379.66$ Zn 66 63.156 6.3156E-08 1.761 8.473 5.68E+13 1.83E+12 1.25E+11 1.00$ 125,017,313,323.28$ Zr 90 1.322 1.322E-09 0.037 0.177 1.19E+12 3.82E+10 2.62E+09 13.17$ 34,464,562,951.58$ Nb 93 0.06 6E-11 0.002 0.008 5.39E+10 1.73E+09 1.19E+08 -$ -$ Mo 98 0.103 1.03E-10 0.003 0.014 9.26E+10 2.98E+09 2.04E+08 7.76$ 1,582,174,903.30$ Ru 102 0.08 8E-11 0.002 0.011 7.19E+10 2.31E+09 50.00$ 115,587,534,584.95$ Rh 103 0.068 6.8E-11 0.002 0.009 6.11E+10 1.96E+09 1,080.00$ 2,122,187,134,979.58$ Pd 106 0.351 3.51E-10 0.010 0.047 3.15E+11 1.01E+10 785.50$ 7,967,174,238,545.59$ Sn 118 0.584 5.84E-10 0.016 0.078 5.25E+11 1.69E+10 1.16E+09 7.21$ 8,334,962,634.93$ Hf 180 0.049 4.9E-11 0.001 0.007 4.40E+10 1.42E+09 9.70E+07 -$ -$ W 184 -0.039 0.00E+00 0.00E+00 -$ -$ Os 192 0.05 5E-11 0.001 0.007 4.49E+10 1.44E+09 360.00$ -$ 520,143,905,632.25$ Ir 193 0.022 2.2E-11 0.001 0.003 1.98E+10 6.36E+08 580.00$ -$ 368,724,235,325.97$ Pt 195 0.103 1.03E-10 0.003 0.014 9.26E+10 2.98E+09 1,147.50$ -$ 3,415,394,920,357.77$ Au 197 0.141 1.41E-10 0.004 0.019 1.27E+11 4.07E+09 1,206.00$ -$ 4,913,799,476,507.87$ Valu/lb Total 519,960.47$ PGM Total 511,131.88$ Rh/Pd/Pt/Au 93.2% 484,698.84$18,418,555,770,390.80$ 19,758,497,890,509.70$ 19,423,011,445,934.00$