Sulphur by ICP OES

DETERMINATION OF SULPHUR IN SOILS, SOLIDS AND LEACHATES
BY INDUCTIVELY COUPLED PLASMA OPTICAL EMMISSION

SPECTROSCOPY (ICP OES)
1.0 Discussion
This method is used for the determination of Sulphur in Solid, Soil and Leachate samples. Solid
and Soil samples are digested prior to analysis. Molecules in the sample are converted to
individual atoms and ions using a high temperature argon plasma. Sample is introduced into the
plasma as a solution and is pumped using a peristaltic pump to a nebuliser where it is converted
to a fine spray and mixed with argon in a spray chamber. Here it is excited by the high
temperatures. ICP OES utilizes UV and visible spectrometry to image the plasma at the exact
wavelength of ionic excitation of the element of interest.
2.0 Interferences
 Spectral interferences are overcome by the flexibility to choose from many available
emission lines combined with spectral interferences correction software.
 Matrix interference can be overcome by sample dilution, matrix matching and the use of
internal standards.
3.0 Sample Preparation
3.1 Leachates:
Leachate samples are prepared as per SOP 128. These are a 1/10 dilution.
3.2 Solids/Sludge samples

1. Weigh 1g of sample (+/-0.010g) using the balance into a labelled glass beaker.
2. Add 50ml of acidified ultrapure water using a graduated cylinder.
3. Add 5ml (+/- 0.05ml) of concentrated nitric acid (Aristar Grade) and cover the beaker with
a clock glass.
4. Digest on the Clifton hotplate EE147 at temperature setting 6.5 or EE260 at the marked
setting until the sample has reduced to around 20ml.
5. Filter the sample through filter paper directly into a 50ml volumetric and wash through
several times using the 2% acidified ultrapure water.
6. Dilute to 50ml using 2% acidified ultrapure water.
7. Store samples in a 100ml plastic bottle and label with lab reference and dilution 1/50.
3.3 Soil Samples
Prior to digestion soil samples must be prepared as in SOP 207 (air dried at no greater than 30 C
and homogenized gently through the 2mm sieve.
1. Prepare a concentrated solution of Aqua Regia (3 parts Hydrochloric Acid to 1 part

Nitric acid) by adding 65ml of Nitric acid and 195ml Hydrochloric acid (both Aristar
grade) into a volumetric flask.
2. Prepare a 50% Aqua Regia Solution by adding 250ml of the concentrated Aqua
Regia solution above to 250ml Ultra pure water.
3. Weigh 1g (+/-0.010g) of dried, sieved soil into a labelled modblock tube.
4. Add 20ml of the 50% Aqua Regia Solution.
5. Set the Modblock to temperature 118 C (see GOP 248 for details).
6. Place the modblock tubes into the modblock and digest for 1 hour 30 minutes
7. Allow to cool and filter samples directly into a 100ml volumetric.
8. Rinse the Modblock tube several times with ultrapure acidified water to ensure all the
sample is rinsed through.
9. Make up to 100ml with ultrapure acidified water (1/100 dilution).
10. Store samples in a 100ml plastic bottle and label with reference number and 1/100.
11. Digest a soil QC with each batch of 20 soils digested. Weigh out 1g (+/- 0.01g) of soil
QC (CRM 039-050) and digest as above.
Digestion logbook must be filled out with all details of samples digested and the Balance
used.
4.0 Procedure for sample run
1. Analysts must be familiar with GOP 254 before commencing an experiment.

2. Turn chiller and fume hood on.
3. To open up the software double click on ‘ICP EXPERT II’.
4. To create an experiment click on ‘worksheet’ and then click ‘new’.
5. Click on ‘create from template’, then ‘ICTOESPPRP\Varian’, then
‘VAIMDB_Euro_database (000)’ and then ‘supplied worksheets’.
6. From the list in the middle section, scroll down and click on the previous run. Change
the date on the bottom of the screen to the correct date and then click worksheet in
the left hand section.
7. This will bring you into the experiment details. Click on ‘Sequence Editor’ and enter
the number of samples to be analysed. Click ‘yes’ to update changes.
8. Click on the ‘Sequence tab’ and enter the new sample reference numbers which are
jobbed for testing. Any dilutions are entered in the right hand column.
9. Dilutions are entered as follows – If working in multiplies of 10 1/1000 is the highest
dilution that can be entered in the ‘Dil Fact’ column. If you need to dilute this 1/1000
sample further e.g. 1/10000 it should be entered as 1 in ‘Act Wt’ column, 1000 in ‘Act
Vol’ column and 10 in ‘Dil Fact’ column. The same applies for multiplies of 50 e.g. if
you want to enter a dilution of 1/50000 it should be entered as 1 in ‘Act Wt’ column,
5000 in ‘Act Vol’ column and 10 in ‘Dil Fact’ column.
10. Ensure that the standards and samples are in the correct positions according to the
sequence editor.
11. Click on ‘Analysis’ tab.
12. Light the plasma by clicking on the ‘plasma on’ tab on the top of the screen
13. Highlight all the standards and samples by clicking on the rack number at the left-
hand side (Tube Column). They must be highlighted yellow to be analysed.
14. Once the plasma is lit and the sequence is set up click on the green arrow at the top
of the screen to begin analysis
15. Once the sequence is finished check all calibrations curves individually. There may
be calibration points that need to be deselected as they are not linear. Do not
deselect more than 2 points or the blank.
16. Check the internal standard results. They should be close to 1.0. Any great
difference needs to be investigated and the problem corrected e.g. the sample may
need diluting.
17. Check the QC results and enter onto the appropriate QC charts. SOP 402 must be
followed.
18. Any samples that are over range will show up as x------ and will need to be diluted
and re analysed.
19. To print off the experiment, click on’ File’, ‘Report settings’ and then ‘Print’.
20. Results for samples can be taken down directly and entered into the LIMS.
5.0 Wavelengths
Sulphur is analysed at wavelength 180.669 nm.

Sulphur by ICP OES

Uploaded by

Copyright:

Available Formats

Sulphur by ICP OES

Uploaded by

Document Information

Original Description:

Copyright

Available Formats

Share this document

Share or Embed Document

Sharing Options

Did you find this document useful?

Is this content inappropriate?

Copyright:

Available Formats

Sulphur by ICP OES

Uploaded by

Copyright:

Available Formats

DETERMINATION OF SULPHUR IN SOILS, SOLIDS AND LEACHATES

BY INDUCTIVELY COUPLED PLASMA OPTICAL EMMISSION

3.0 Sample Preparation

3.2 Solids/Sludge samples

3.3 Soil Samples

1. Prepare a concentrated solution of Aqua Regia (3 parts Hydrochloric Acid to 1 part

4.0 Procedure for sample run

1. Analysts must be familiar with GOP 254 before commencing an experiment.

Sulphur is analysed at wavelength 180.669 nm.

You might also like

Pfad - The Proxy pFad of © 2024 Garber Painting. All rights reserved.