METHOD TITLE: DETERMINATION OF TRACE

ELEMENTS IN GEOLOGICAL
MATERIALS USING ICPAES
FOLLOWING AN AQUA REGIA
DIGESTION

SOP NUMBER ME-ICP41

Related Digestion Code GEO-AR01

Amend. Approved
Date Description of Amendment Appendix
No. By
0 23-Feb-06 Issue A (1/0), (2/0) K. Bunten
1 16-Mar-06 Added ME-ICP41s Method K. Bunten
Updated Method title. Removed
2 29-Aug-06 K. Bunten
ME-ICP41s Method
Removed standard GEO QC from Milder
3 03-Jun-09
table in the section 9.3 Mascaraqui

Reviewed By:
Kelly Ocaña and Milder Mascaraqui
Date: 03-Jun-09

Copy number:
THIS IS A CONTROLLED COPY UNLESS OTHERWISE MARKED.

Ref: ME-ICP41 (SOP) Issue: A Amendment: 3 Date: 03-Jun-09 Page 1 of 8

1. SCOPE
This procedure is suitable for the determination of aqua regia soluble trace elements in
exploration samples such as soils, sediments and weakly mineralised rock or drill
samples. Major rock forming elements and the more resistive minerals are only
partially dissolved.
Refer to Digestion Code: GEO-AR01 for a more comprehensive discussion of
expected element recoveries and mineral solubilities.
2. PRINCIPLE
The sample, in a polypropylene test tube, is digested with 75 % aqua regia in a
digestion block operating at 115°C. After dilution a suite of 34 elements is determined
using ICPAES.
3. SAFETY
3.1 Adequate safety equipment must be worn when handling concentrated acids.
Safety glasses, rubber gloves and lab coats should be worn. Refer to the
relevant MSDS for further details.
3.2 Preparation of the acid mixture and sample digestion must be carried out in a
mechanically ventilated and scrubbed fume cupboard.
4. ELEMENTS REPORTED
4.1 Elements determined by ICPAES in this package are summarised in GEMS.
4.1.1 In Webview, Select in Order: ‘Lab’ or ‘QC’ Tab, In Method Info Box; Type,
‘ME-ICP41’, <Enter>, In Method Detail Window, click, ‘Analytes’
4.1.2 In StarLIMS, Select in order: ‘Static Tables’, ‘Method’, ‘Methods’,
‘Department’, ‘Spectroscopy’, ‘ICP-AES’, ‘ME-ICP41’
5. REAGENTS
5.1 Refer to Digestion Method GEO – AR01 (SOP).
6. APPARATUS
6.1 Refer to Digestion Method GEO-AR01 (SOP)
6.2 Inductively coupled plasma atomic emission spectrometer (ICPAES) equipped
with a solid-state detector (CCD or similar)
7. DIGESTION PROCEDURE
7.1 Refer to Digestion Method GEO – AR01 (SOP)
8. INSTRUMENT PARAMETERS
8.1 The ICPAES daily setup procedures are detailed in document ICP/SETUP
(Radial) (SOP).
8.2 The ICPAES operating parameters are detailed in document ICP/OP (SOP).
8.3 The spectral lines used to determine elemental concentrations and inter-
element corrections required for method ME-ICP41 are included in document
ICP/LINE (SOP).

Ref: ME-ICP41 (SOP) Issue: A Amendment: 3 Date: 03-Jun-09 Page 2 of 8

 8.4 Maintenance procedures for the ICPAES are outlined in document
ICP/MAINTENANCE (SOP).
9. QUALITY CONTROL
9.1 Batch Quality Control samples are weighed, digested and analysed with the
unknown samples. The number of QC samples, blanks and duplicates are listed
in GEMS after the creation of an instrument run.
9.2 Instrument Calibration solutions are prepared from purchased multi-element
stock solutions. See document ICP/CAL-QC (SOP) for solution preparation
details.
9.3 Quality Control solutions are purchased from a different source to the
Calibration solutions. Details of these solutions and their preparation details are
found in ICP/CAL-QC (SOP). General positioning details for these samples are
shown below.

ICPAES
Reagent blank
Immediately ALSQC-ICP41/61 (ALSQC1)
after calibration IEC Solutions

On-going
calibration drift
checks (after a ALSQC-ICP41/61 (ALSQC1)
maximum of 60
samples)

9.4 Acceptable QC control limits are shown below.

Lower Limit Upper Limit

Conc.
QC (Per Analyte) (Per Analyte)
(ppm)
(%) (%)
ALSQC-ICP41/61 (initial) 10 90 110
ALSQC-ICP41/61 (ongoing) 10 80 120

10. ERROR ACTIONS

10.1 If the initial QC check fails after calibration, cease the analysis immediately.
10.2 If the initial QC check passes after calibration, continue to run the first set of
samples until the next ongoing QC check.
10.3 If the ongoing QC Check passes, continue running the next set of samples.
10.4 If the ongoing QC Check fails, recalibrate the instrument, check the QC and
rerun all samples up until the last successful QC check.

Ref: ME-ICP41 (SOP) Issue: A Amendment: 3 Date: 03-Jun-09 Page 3 of 8

 10.5 If the QC solution fails to fall within acceptable control limits after re-calibration,
the analysis must stop. The analyst must then determine the cause of the QC
failure and make the necessary adjustments. Analysis shall then recommence
from the solution immediately following the last successful QC check.
NOTE: If the adjustments require turning plasma off and taking apart and cleaning the
glassware (nebulizer, spray chamber, transfer tube, torch) then the data prior to QC
recalibration failure must be exported to GEMS while re-batching the leftover rack of
samples to another Instrument Run. Flagging "missed results" for rerun on an
incomplete Instrument Run can only be done in Starlims (See Appendix 2 “Procedure
for Flagging Incomplete Runs Containing Missed Results”).

11. REFERENCED DOCUMENTS

11.1 Aqua Regia Digestion – Geochemical Analysis GEO-AR01
11.2 ICPAES – Daily Setup Procedure ICP/SETUP (RADIAL)
11.3 ICPAES – Calibration and QC Solutions ICP/CAL-QC
11.4 ICPAES – Operating Parameters ICP/OP
11.5 ICPAES – Line Selection and Interferences ICP/LINE
11.6 ICPAES – Routine Maintenance ICP/MAINTENANCE

12. Appendix

Appendix 1 Flowchart ME-ICP41 (1/0)

Procedure for Flagging Incomplete
Appendix 2 ME-ICP41 (2/0)
Runs Containing Missed Results

Ref: ME-ICP41 (SOP) Issue: A Amendment: 3 Date: 03-Jun-09 Page 4 of 8

 Flow Chart ME-ICP41/61

! "# $ " % & $ "" ' $

(
) * " +
' ( +# *
(
" ) *# %) ' , * "
* (
# " * ** " )
-(. (
# & /01 %201 (

* #
" '* & * ) % & (
*" # " ' % " * '( 4 5
*" # " ' % & ( 5*
*" # " '* % ) " % + " '" #
" * # " '( &)
*" # * % & " *" ) ( (
' & 3 & * " *
# " '(

Ref: ME-ICP41 (1/0) (SOP) Issue: A Amendment: 3 Date: 03-Jun-09 Page 5 of 8

 Procedure for Flagging Incomplete Runs Containing Missed Results

SUMMARY
The file status for incomplete Runs indicates “Missed Results” on the approval list
(Available Runs for ICP-AES, ICP-MS). When the Run file is opened in Webview, no
results will be displayed and the cells will be coloured blue. The procedure to retrieve the
completed results in Starlims is described.
PROCEDURE
1. Log onto Starlims.

2. Go to Results Entry/Analytical Results and enter the Run number then press “OK”.

Ref: ME-ICP41 (2/0) (SOP) Issue: A Amendment: 3 Date: 03-Jun-09 Page 6 of 8

3. Click on “Resubmit” button.

4. All missed samples will show a status “logged” while samples that were run will show
a status “Done”. Highlight the “logged” samples by pointing the cursor on the very left
hand column while holding the left key. Highlighted cells will turn “red”. Click on
“Rerun” icon, it will then confirm if you want to rerun the samples… click “yes”. A
dialog box will pop up. Enter a reason for the rerun then click “OK”. Close the screen.

5. After closing the previous screen. It brings you back to the original screen. Click “QC
Rules” (say yes to all prompts). Starlims will then re-calculate the results for the
samples that were done and flag the “Missing results” for rerun. Close the file after and
exit Starlims.

Ref: ME-ICP41 (2/0) (SOP) Issue: A Amendment: 3 Date: 03-Jun-09 Page 7 of 8

6. Go back to Webview/Lab/Available Runs for ICP-AES, ICP-MS and open the Run.
Results should be displayed now while missed samples should be greyed out with
status “Rerun”. Approve as usual.

Ref: ME-ICP41 (2/0) (SOP) Issue: A Amendment: 3 Date: 03-Jun-09 Page 8 of 8