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Author(s): | N. Lawler & A. Armstrong |
Reviewer(s): | C. Bennight, E. Jackson, H. Barnes |
Management Approval: | D. Houpt |
Current Version: | V371T | July 2017 | Reviewed X374 | March 2018 |
Previous Versions: | V1.2 | 6/10/2017, V1.1 | 1/6/2014 (IODP-II) |
Domain: | Chemistry; XRD lab |
System: | ICP-AES Elemental Analysis |
Keywords: | Element oxide, ICP, solids |
In This User Guide
Contents
Manual Information
In This User Guide
Introduction
Apparatus, Reagents, & Materials
Laboratory Apparatus
General Laboratory Equipment
Rock Grinding
LOI/Bead-Making
Dissolution/Dilution
Reagents
Materials
Grinding Samples
LOI/Sample Bead
Preparing Rock Samples
Cutting Samples to Size
Notes about altered samples:
Polishing Samples on Diamond Wheel
Apparatus and Materials
Cleaning Samples
Apparatus and Materials
Drying Samples
Apparatus and Materials
Crushing Samples in the X-Press
Grinding Samples in the Shatterbox
Apparatus and Materials
Cleaning the Grinding Vessels
Determining LOI
Loss on Ignition
Advice on LOI Procedures (from Exp. 366 Methods)
Pre-ignition Weighing
Apparatus and Materials
Weighing Crucibles
Weighing Sample
Igniting Samples
Post-Ignition Weighing
Uploading LOI Data To LIMS
Cleaning the Quartz Crucibles
Making the Sample Bead
Weighing the Sample
Fusing the Sample into a Bead
Using the Beadmaker
Cleaning Platinum Crucibles
Polishing the Platinum Crucibles
Using the LOI Furnace to Make Sample Beads
| Table of Contents |
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Introduction
Inductively Coupled Plasma Atomic Emission Spectroscopy, ICP-AES, 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-AES 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 a safe and ideal method (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-AES machine.
The complete process (from sample table to ICP-AES 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 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.
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