A Comparison of SEM-EDS with ICP-AES for the Quantitative Elemental Determination of Estuarine Particles

Stephen M. Haley, Alan D. Tappin and Mark F. Fitzsimons

School of Earth, Ocean and Environmental Sciences, University of Plymouth, Plymouth PL4 8AA, U.K.

Presented at: 6th European Meeting on Environmental Chemistry (EMEC6), Belgrade, Serbia and Montenegro, 6-10 December, 2005.

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Brief Summary

The physico-chemical behaviour of estuarine suspended particulate matter (SPM) is an area of increasing interest, as particles can regulate the speciation and destiny of contaminants and nutrients in the aquatic environment. This study compared the use of Inductively Coupled Plasma –Atomic Emission Spectrometry (ICP-AES) with Scanning Electron Microscopy-Energy Dispersive X-ray Spectrometry (SEM-EDS) in quantifying the elements Al, Fe, Mg, Si, Zn, Mn, Ca, K and Ti in an estuarine Certified Reference Material (CRM).

Sample preparation for ICP-AES analysis involved LiBO2 fusion in order to release Al. SEM-EDS analysis required the production of polished resin stubs containing the CRM. The analysis of 15 scans from the ICP-AES, and 100 individual particles by SEM-EDS, revealed no significant difference between the medians for Al, Fe, Mg, Ca and K. Good correlation was generally observed between the instrument and reference values. Significant differences were observed between the medians of Mn and Ti, while the Si value was not established as a reliable reference. Trace Zn was not determined by SEM-EDS and the instrument performed poorly on Mn and Ti, which were also present at trace levels.

The ICP-AES values correlated closely with CRM values throughout, except for K, which it undervalued substantially. Qualitative elemental mapping techniques were performed on the SEM-EDS. The results were mainly illustrative but showed potential for further development.

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