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Elemental Scientific prepFAST Geo-Chem Fire Assay … prepFAST-GeoChem-Fire Assay.pdf · Elemental...

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1 Elemental Scientific prepFAST: Geo-Chem Fire Assay Precious Metals by ICPOES Features: • Autocalibrate from a single stock standard • Autodilute sample digests (50% acid) • Automate hazardous labor intensive steps • Fluoropolymer sample pathway • High speed analysis (<1 min/sample) • Reduce cost per analysis • Routine walk up and analyze solution for ICP and ICPMS Brief The prepFAST inline autodilution system autocalibrates and autodilutes 50% Aqua Regia samples for the precise and accurate determination of precious metals. Seamless integration of prepFAST with ICP software eliminates a hazardous manual dilution step that requires both time and additional reagents/tubes. Authors: Austin Schultz, Kyle Uhlmeyer and Paul Field (fi[email protected]) Figure 1. prepFAST automatically generates a 0.2 (25x), 0.5 (10x), 2.5 (2x) and 5.0 (1x) calibration curve from a 5 ppm Au, Ir, Os, Pd, Pt, Rh, and Ru (5% HCl/5% HNO 3 ) stock standard solution. Precise and accurate syringe based inline autodilution is illustrated through excellent linearity of all calibration curves. Element 0.99 0.99 0.99 0.99 0.99 0.99 Os Autocalibraon from 5 - 0.2 ppm Os 228.226 0.2ppm Element R 2 Ru 0.99998 Rh 0.99998 Pd 0.99998 Os 0.99998 Ir 0.99995 Pt 0.99996 R 2 = 0.99998 0.5ppm 2.5ppm 5.0ppm
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Page 1: Elemental Scientific prepFAST Geo-Chem Fire Assay … prepFAST-GeoChem-Fire Assay.pdf · Elemental Scientific prepFAST: Geo-Chem Fire Assay ... • High speed analysis (

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Elemental Scientific prepFAST: Geo-Chem Fire AssayPrecious Metals by ICPOES

Features:

• Autocalibrate from a single stock standard

• Autodilute sample digests (50% acid)

• Automate hazardous labor intensive steps

• Fluoropolymer sample pathway

• High speed analysis (<1 min/sample)

• Reduce cost per analysis

• Routine walk up and analyze solution for ICP and ICPMS

Brief

The prepFAST inline autodilution system autocalibrates and autodilutes 50% Aqua Regia samples for the precise and accurate determination of precious metals. Seamless integration of prepFAST with ICP software eliminates a hazardous manual dilution step that requires both time and additional reagents/tubes.

Authors: Austin Schultz, Kyle Uhlmeyer and Paul Field ([email protected])

Figure 1. prepFAST automatically generates a 0.2 (25x), 0.5 (10x), 2.5 (2x) and 5.0 (1x) calibration curve from a 5 ppm Au, Ir, Os, Pd, Pt, Rh, and Ru (5% HCl/5% HNO3) stock standard solution. Precise and accurate syringe based inline autodilution is illustrated through excellent linearity of all calibration curves.

Element   R2  

Ru   0.99998  

Rh   0.99998  

Pd   0.99998  

Os   0.99998  

Ir   0.99995  

Pt   0.99996  

Os Autocalibration from 5 - 0.2 ppm

Os 228.226

0.2ppm

Element   R2  

Ru   0.99998  

Rh   0.99998  

Pd   0.99998  

Os   0.99998  

Ir   0.99995  

Pt   0.99996  

R2 = 0.99998

0.5ppm

2.5ppm

5.0ppm

Page 2: Elemental Scientific prepFAST Geo-Chem Fire Assay … prepFAST-GeoChem-Fire Assay.pdf · Elemental Scientific prepFAST: Geo-Chem Fire Assay ... • High speed analysis (

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AbstractFire assay is one of the oldest known techniques for purifying precious metals. Typically Ni (Au, Ir, Os, Pd, Pt, Rh, and Ru) or Pb (Au, Pt and Pd) are used to scavenge precious metals from their matrix during fusion. The resultant sulfide bead and extracted precious metals are then digested in strong mineral acids (50% Aqua Regia). Using prepFAST, sample digests (50% Aqua Regia) can simply be placed on the autosampler rack with a blank and a 5 ppm multi-element (Au, Ir, Os, Pd, Pt, Rh, and Ru) stock standard. The prepFAST system will automatically generate a 0.2 (25x), 0.5 (10x), 2.5 (2x) and 5.0 (1x) calibration curve and analyze samples at a rate of nearly 90/hr.

S4:InternalStandard

S3:Diluent

S2:Carrier

Sample

Vacuum

V2:P7+ Load1. Fill Loop

Carrier

Waste

To ICPMS

V1:P6 Load

Carrier

S4:InternalStandard

S3:Diluent

S2:Carrier

Sample

Vacuum

V2:P7+ Inject2. Dilute Sample

Waste

To ICPMS

V1:P6 Load

S4:InternalStandard

S3:Diluent

S2:CarrierRinse

Vacuum

V2:P7+ Load3. Inject Sample Clean V2

Carrier

Waste

To ICPMS

S4:InternalStandard

S3:Diluent

S1:Rinse

Sample

Vacuum

V2:P7+ Inject4. Clean V1

Waste

V1:P6 Load

S4:InternalStandard

S3:Diluent

S2:Carrier

Sample

Vacuum

V2:P7+ Load5. Tune

Tune

Waste

To ICPMS

V1:P6 Load

Carrier

To ICPMS

Figure 2. The prepFAST system schematic illustrating 1) sample loading during spray chamber rinse and 2) sample injection dilution and internal standardization.

Figure 3. Mixing inline eliminates the need to premix/dilute samples in discrete tubes prior to analysis. This cost effective approach improves sample throughput, saves time, and reduces labware and reagent consumption. After in-valve dilution, the sample is injected (400 µL/min) at the user's desired flow rate.

Manual vs. Inline Sample Dilution

Page 3: Elemental Scientific prepFAST Geo-Chem Fire Assay … prepFAST-GeoChem-Fire Assay.pdf · Elemental Scientific prepFAST: Geo-Chem Fire Assay ... • High speed analysis (

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Figure 4. A 5ppm Au, Os, Ir, Pt, Pd, Rh, and Ru sample prepared in 50% Aqua Regia simulates a fire assay digestion. The concentrated mineral acid solution is diluted 20x inline for 700 replicate sample analysis of 0.25 ppm of precious metals. prepFAST inline autodilution illustrates not only a rapid throughput at 88 samples per hour, but also very accurate reproducible results for a 50% Aqua Regia matrix.

Sample Stability

0.00  

0.10  

0.20  

0.30  

0.40  

0.50  

0   60   120   180   240   300   360   420   480  

Concen

tra)

on  Fou

nd  (p

pm)  

Time  (Minutes)  

Rh  concentra)on  in  700  samples  over    8  hours.  RSD  ≤  2%  

50% Aqua Regia20x Inline autodilution

88 sample/hr

Figure 5. Recovery based on the 700 analysis of 0.25 ppm precious metal is both quantitative (101 to 106%) and precise (<3%).

Recovery

102%   105%   101%   104%   104%   102%   106%  

0%  

50%  

100%  

150%  

200%  

Au  267.595   Ir  224.268   Os  228.226   Pd  340.458   Pt  265.945   Rh  343.489   Ru  240.272  

Percen

t  Recovery  

Element  

Recovery  101%  -­‐  106%  

Page 4: Elemental Scientific prepFAST Geo-Chem Fire Assay … prepFAST-GeoChem-Fire Assay.pdf · Elemental Scientific prepFAST: Geo-Chem Fire Assay ... • High speed analysis (

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SC-2 DX prepFAST System

7277 World Communications Drive | Omaha, NE 68122 USA

Phone: 1.402.991.7800 | Fax: 1.402.991.7799

Email: [email protected]

Web: www.prepFAST.com | www.icpms.com Elemental Scientific

Benefits:

• Reduce cost per analysis through inline sample dilution Cut sample time in half

Reduce the amount of diluent (by 20x)

Reduce the number of vials (by half)

Eliminate hazardous (50% Aqua Regia) manual sample dilution step

• Simply place rack with digested samples on the autosampler and run

14071


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