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ME-MS61 - "Near Total" Digestion - ICP-OES & ICP-MS

ME-MS61 combines the 4-acid digestion (HF, HClO4, HNO3 and HCl) with analysis by ICP and ICP-MS. Resistate minerals are not digested.


4-Acid "Near Total" Digestion – ICP-OES Portion
A 0.25 g sample is digested 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 incipient dryness. After incipient dryness is attained, samples are brought back into solution using aqua regia.

With this digestion certain phases may be only partially solubilized. These phases include zircon, monazite, sphene, gahnite, chromite, cassiterite, rutile and barite. Ag greater than 100 ppm and Pb greater than 5000 ppm should be assayed as high levels may not be solubilized. Only sulphide sulfur will be solubilized.

The samples are then analyzed using a Varian ICP-OES.  QC for the digestion is 14% for each batch, 5 method reagent blanks, 10 in-house controls, 10 sample duplicates, and 8 certified reference materials.  An additional 13% QC is performed as part of the instrumental analysis to ensure quality in the areas of instrumental drift.

 

4-Acid "Near Total" Digestion – ICP-MS Portion
Additional elements are determined by ICP-MS on the multi-acid digest solution above.  The samples are diluted and analyzed on a 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.

 

Code ME-MS61 Elements and Detection Limits (ppm)

Element

Detection Limit

Upper Limit

Reported By

 

Element

Detection Limit

Upper Limit

Reported By

Ag

0.01

100

ICP&ICP/MS

 

Na

0.01%

10%

ICP

Al 

0.01%

50%

ICP

 

Nb 

0.1

500

ICP/MS

As 

0.2

10,000

ICP/MS

 

Ni

0.2

10,000

ICP/MS

Ba 

10

10,000

ICP/MS

 

P

10

10,000

ICP

Be

0.05

1,000

ICP/MS

 

Pb

0.5

10,000

ICP/MS

Bi

0.01

10,000

ICP/MS

 

Rb

0.1

10,000

ICP/MS

Ca

0.01%

50%

ICP

 

Re

0.002

50

ICP/MS

Cd

0.02

1,000

ICP/MS

 

S+

0.01%

10%

ICP

Ce 

0.01

500

ICP/MS

 

Sb 

0.05

10,000

ICP/MS

Co

0.1

10,000

ICP/MS

 

Sc

0.1

10,000

ICP

Cr 

1

10,000

ICP/MS

 

Se

1

1,000

ICP/MS

Cs

0.05

500

ICP/MS

 

Sn 

0.2

500

ICP/MS

Cu

0.2

10,000

ICP/MS

 

Sr

0.2

10,000

ICP/MS

Fe 

0.01%

50%

ICP

 

Ta 

0.05

100

ICP/MS

Ga

0.05

10,000

ICP/MS

 

Te

0.05

500

ICP/MS

Ge

0.05

500

ICP/MS

 

Th 

0.2

10,000

ICP/MS

Hf 

0.1

500

ICP/MS

 

Ti 

0.0005%

10%

ICP

In

0.005

500

ICP/MS

 

Tl

0.02

10,000

ICP/MS

K 

0.01%

10%

ICP

 

U 

0.1

10,000

ICP/MS

La 

0.5

10,000

ICP/MS

 

V

1

10,000

ICP/MS

Li

0.2

10,000

ICP/MS

 

W 

0.1

10,000

ICP/MS

Mg

0.01%

50%

ICP

 

Y 

0.1

500

ICP/MS

Mn 

5

100,000

ICP

 

Zn 

2

10,000

ICP/MS

Mo

0.05

10,000

ICP/MS

 

Zr 

0.5

500

ICP/MS

Extraction of each element by 4-Acid Digestion is dependent on mineralogy.
+ Sulphide sulphur and soluble sulphates are extracted.


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