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1EPI/MS - Aqua Regia-ICP and ICPMS, INAA

A 30 g sample is analyzed by INAA and with an aqua regia digestion followed by ICP analysis.

 

INAA

INAA is an analytical technique dependent on measuring gamma radiation induced in the sample by irradiation with neutrons. The primary source of neutrons for irradiation is usually a nuclear reactor. Each activated element emits a "fingerprint" of gamma radiation which can be measured and quantified. 

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-2 s-1.  After a 7-day period, 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.

ICP/MS
Digested samples are diluted and analyzed by Perkin Elmer Sciex ELAN 6000, 6100 or 9000 ICP/MS. One blank is run for every 68 samples. An in-house control is run every 33 samples. Digested standards are run every 68 samples. After every 15 samples, a digestion duplicate is analyzed. Instrument is recalibrated every 68 samples.

Code 1EPI/MS (Au + 23 ) Elements and Detection Limits (ppm)

Element

Detection Limit

Upper Limit

Reported By

Element

Detection Limit

Upper Limit

Reported By

Ag *

0.2

10,000

INAA

K

0.01%

20%

ICP

As

2

10,000

INAA

Mn

2

20,000

ICP

Au

5 ppb

30,000 ppb

INAA

Mo

2

10,000

ICP

Ba

100

100,000

INAA

    Na   0.01%

50% 

INAA 

Bi

0.1

1,000

ICP/MS

Ni

1

 10,000

 ICP

Ca

0.01%

50%

ICP

 Pb

2  

 5,000

 ICP

Cd

0.5

5,000

ICP

 S

 0.001%

 20%

 ICP

Cs

2

10,000

INAA

 Sb

 0.2

 10,000

 INAA

Cu

1

10,000

ICP

 Se

 0.1

 1,000

 ICP/MS

Fe

0.02%

75%

INAA

 Te

 0.1

 1,000

 ICP/MS

Ga

1

10,000

ICP/MS

Tl

0.1

1,000

ICP/MS

Ge

0.1

1,000

ICP/MS

W  

4  

10,000

 INAA

     Hg 0.01 1,000    INAA      Zn         1 10,000      ICP

 

Code 1EPI/MS Enhanced (Au + 23) Elements and Detection Limits (ppm)

Element

Detection Limit

Upper Limit

Reported By

Element

Detection Limit

Upper Limit

Reported By

Ag *

0.2

10,000

INAA

K

0.01%

20%

ICP

As

0.5

10,000

INAA

Mn

2

20,000

ICP

Au

2 ppb

30,000 ppb

INAA

Mo

2

10,000

ICP

Ba

100

100,000

INAA

   Na  0.01%  50%

INAA

Bi

0.1

1,000

ICP/MS

Ni

1

10,000

ICP

Ca

0.01%

50%

ICP

Pb

2

5,000

ICP

Cd

0.5

5,000

ICP

S

0.01%

20%

ICP

Cs

2

10

INAA

Sb

0.2

10,000

INAA

Cu

1

10,000

ICP

Se

0.1

1,000

ICP/MS

Fe

0.02%

75%

INAA

Te

0.1

1,000

ICP/MS

Ga

1

10,000

ICP/MS

Tl

0.1

500

ICP/MS

Ge

0.1

1,000

ICP/MS

W

4

10,000

INAA

Hg

1

10,000

INAA

Zn

1

100,000

ICP

 

 

 

 

  


 




Notes:  

Extraction of each element by Aqua Regia Digestion is dependent on mineralogy.

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

Assays are recommended for values which exceed the upper limits.

 

Reference:

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


Activation Laboratories Ltd. | 41 Bittern Street, Ancaster, Ontario, L9G 4V5, Canada | TF: +1.888.228.5227
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