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Inductively Coupled Plasma Optical Emission Spectroscopy, ICP-OES, is a method to perform elemental analysis on a sample in solution (ODP Technical Note 29). This manual covers hard rock sample preparation for ICP-OES analysis. Hard rock samples are prepared via the 'flux fusion' approach. This technique ensures complete dissolution of sample allowing a full elemental analysis. Solutions are stable which allows further analysis, and involves no HF making it . It is a safe and ideal method for shipboard analyses (ODP Technical Note 29).
Rock samples are crushed to a fine, talc-like powder using multiple cleaning, crushing and grinding procedures. After grinding, loss on ignition (LOI) is determined. Ignited material is fused with flux powder forming a glass sample bead. Fused beads are then dissolved in 10% HNO3 . This is further diluted and the resulting solution is processed by the ICP-OES machine.
The complete process (from sample table to ICP-OES machine) takes 3-4 days. Day 1 involves: polishing on the Diamond Wheel, cleaning, and drying samples overnight. Day 2: Crushing in the X-Press, grinding in the Shatterbox, a pre-ignition (for LOI) weight, and placing samples in the muffle furnace overnight. Day 3-4: Taking a post-ignition (for LOI) weight, and fusing the sample bead. The beads are handed off to the chemistry technicians to continue ICP analysis. Note that
Wait until there are about six or more samples so you can prepare a 'batch' of six or more at a time.
Note: ignited powders are most often used for ICP analyses (LOI determines the amount of alteration of the sample, generally, scientists use this to determine the 'freshness' of the ingenious rock being analyzed), however it is not always the case. Please speak to your scientist regarding their preference.Wait until there are about six or more samples so you can prepare a 'batch' of six or more at a time.
Apparatus, Reagents, & Materials
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- Compensated Dual Analytical Balance System System (Metler balances)
- Drying ovens at 110°C and 60°C
- Muffle furnace
- Sonicating bath
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- 0.172 mM LiBr wetting agent (0.15 mg ultrapure LiBr in 10 mL DI water)
- 400mg of drew sighed lithium metabolite flux (weighed on shore)
- 10% nitric acid (143 mL concentrated nitric acid/L of solution). Caution! always add acid to water.
- Isopropyl alcohol, laboratory grade
- Methanol, laboratory grade
- Acetone, laboratory grade
- DI water (18.2 M¿ laboratory water obtained from Chemistry Lab)
Materials
Grinding Samples
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- Cut to size (see Cutting Samples to Size).
- Polish (see Polishing Samples on Diamond Wheel).
- Clean (see Cleaning Samples).
- Dry (see Drying Samples).
- Crush (see Crushing Samples in the X-Press).
- Grind (see Grinding Samples in the Shatterbox).
Cutting Samples to Size
To cut samples for the X-Press, use the splitting room saw following these guidelines:
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