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Ultratrace 5 - INAA + 4-Acid Digestion/ICP-MS

Ultratrace 5 is a combination of INAA with a 4-acid digestion ICP/MS. Some of the resistate elements are provided by INAA.

 

ICP/MS

A 0.25 g sample is digested at 260°C with four acids beginning with hydrofluoric, followed by a mixture of nitric and perchloric acids, heated using precise programmer controlled heating in several ramping and holding cycles which takes the samples to dryness. This leach is partial for magnetite, chromite, barite, spinels, zircon and massive sulphides.

 

Digested samples are diluted and analyzed by Perkin Elmer Sciex ELAN 6000, 6100 or 9000 ICP/MS. One blank is run for every 40 samples. In-house control is run every 20 samples. Digested standards are run every 80 samples. After every 15 samples, a digestion duplicate is analyzed. Instrument is recalibrated every 80 samples.

 

INAA

A 30 g aliquot, if available, is encapsulated in a polyethylene vial and irradiated with flux wires and an internal standard (1 for 11 samples) at a thermal neutron flux of 7 x 1012 n cm-2s-1. After a 7-day decay to allow Na-24 to decay the samples are counted on a high purity Ge detector with resolution of better than 1.7 KeV for the 1332 KeV Co-60 photopeak. Using the flux wires, the decay-corrected activities are compared to a calibration developed from multiple certified international reference materials. The standard present is only a check on accuracy and is not used for calibration purposes. From 10-30% of the samples are rechecked by re-measurement. For values exceeding the upper limits, assays are recommended.

 

One standard is run for every 11 samples. One blank is analyzed per work order. Selected duplicates are analyzed when enough material is submitted.

 

 

Code Ultratrace-5 Elements and Detection Limits (ppm except where noted)

Element

Detection Limit

Upper Limit

Reported By

 

Element

Detection Limit

Upper Limit

Reported By

Ag*

0.05

100,000

INAA& ICP/MS

 

Mn

1

10,000

ICP/MS

As

0.5

10,000

INAA

 

Mo

0.05

10,000

ICP/MS

Au

2ppb

30,000ppb

INAA

 

Na

0.01%

20%

INAA

Ba

1

100,000

INAA& ICP/MS

 

Nb

0.1

500

ICP/MS

Be

0.1

1,000

ICP/MS

 

Nd

0.1

10,000

ICP/MS

Bi

0.02

2,000

ICP/MS

 

Ni*

0.5

100,000

INAA& ICP/MS

Br

0.5

5,000

INAA

 

Pb

0.5

5,000

ICP/MS

Ca

0.01%

50%

ICP/MS

 

Pr

0.1

1,000

ICP/MS

Cd

0.1

1,000

ICP/MS

 

Rb

0.2

5,000

ICP/MS

Ce

0.1

10,000

ICP/MS

 

Re

0.001

100

ICP/MS

Co

0.1

5,000

INAA

 

Sb

0.1

10,000

INAA

Cr

1

100,000

INAA

 

Sc

0.1

1,000

INAA

Cs*

0.05

5,000

INAA& ICP/MS

 

Se*

0.1

10,000

INAA& ICP/MS

Cu

0.2

10,000

ICP/MS

 

Sm

0.1

100

ICP/MS

Dy

0.1

5,000

ICP/MS

 

Sn

1

200

ICP/MS

Er

0.1

1,000

ICP/MS

 

Sr

0.2

1,000

ICP/MS

Eu

0.05

100

ICP/MS

 

Ta*

0.1

10,000

INAA& ICP/MS

Fe

0.01%

50%

INAA

 

Tb

0.1

100

ICP/MS

Ga

0.1

500

ICP/MS

 

Te

0.1

500

ICP/MS

Ge

0.1

500

ICP/MS

 

Th*

0.1

10,000

INAA& ICP/MS

Gd

0.1

5,000

ICP/MS

 

Tl

0.05

500

ICP/MS

Hf

0.1

5,000

INAA

 

Tm

0.1

1,000

ICP/MS

Hg

10ppb

10,000ppb

ICP/MS

 

U*

0.1

10,000

INAA& ICP/MS

Ho

0.1

1,000

ICP/MS

 

V

1

1,000

ICP/MS

In

0.1

100

ICP/MS

 

W

1

10,000

INAA

K

0.01%

5%

ICP/MS

 

Y

0.1

10,000

ICP/MS

La

0.1

10,000

ICP/MS

 

Yb

0.1

5,000

ICP/MS

Li

0.5

400

ICP/MS

 

Zn*

0.5

100,000

INAA& ICP/MS

Lu

0.1

100

ICP/MS

 

Zr

1

5,000

ICP/MS

Mg

0.01%

10%

ICP/MS

 












































Notes:    
Extraction of each element by 4-Acid Digestion is dependent on mineralogy.  

Unaltered silicates and resistate minerals may not be dissolved.

*  Element reported by multiple techniques if one or more techniques may not be total.

 

Reference
Hoffman, E.L., 1992. Instrumental Neutron Activation in Geoanalysis. Journal of Geochemical Exploration, volume 44, pp. 297-319.

 


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