3. Analytical Sediment Chemistry on Board the JOIDES Resolution: A Comparison of Shipboard and Shore-Based Sample Preparation Protocols1

C.L. Ziegler2 and R.W. Murray2


We measured the chemical composition of 100 samples from the 250-m sediment sequence retrieved from Ocean Drilling Program Site 1256 in the Guatemala Basin using a newly developed microwave-assisted acid digestion protocol followed by inductively coupled plasma–atomic emission spectroscopy (ICP-AES) analysis. We compared these data gathered onshore to the results from the flux fusion prepared samples analyzed by shipboard ICP-AES during the leg and published in the Leg 206 Initial Reports volume, as well as to 35 randomly selected samples that were prepared by flux fusion at Boston University and analyzed by ICP-AES. Comparison of the newly developed acid digestion protocol to shore-based flux fusion demonstrates that the microwave-assisted acid technique yields a complete digestion, and because this procedure includes boric acid, it is safe for use with HF acid as boric acid neutralizes excess HF. The precision for nearly all elements in shore-based acid digestions is better than 3% of the measured values, including for elements such as Ni, Cr, and V, which are typically difficult to measure in biogenic-rich sediments. The shore-based flux fusions, while better than shipboard reported precision values (as expected), has precision better than 3% of their respective measured values for all major elements (Si, Al, Ti, Fe, Mn, Ca, Mg, Na, and K) and several trace elements (Ba and Sr). Results for P, Cr, Ni, V, Sc, and Zr are better than 5% of their measured values. Not only does the newly developed acid digestion provide better analytical results than the typical flux fusion method, the shore-based acid procedure also exhibits downhole lithologic and chemical characteristics similar to the shipboard flux fusion prepared results. These results confirm that the current shipboard methods are adequate for first-order geochemical interpretations and that the microwave-assisted acid digestion holds great potential to be the primary technique of preparing sediments on future Integrated Ocean Drilling Program expeditions.

1Ziegler, C.L., and Murray, R.W., 2007. Analytical sediment chemistry on board the JOIDES Resolution: a comparison of shipboard and shore-based sample preparation protocols. In Teagle, D.A.H., Wilson, D.S., Acton, G.D., and Vanko, D.A. (Eds.), Proc. ODP, Sci. Results, 206: College Station, TX (Ocean Drilling Program), 1–26. doi:10.2973/odp.proc.sr.206.009.2007

2Department of Earth Sciences, Boston University, Boston MA 02215, USA. Correspondence author: rickm@bu.edu

Initial receipt: 3 May 2005
Acceptance: 20 September 2005
Web publication: 1 February 2007
Ms 206SR-009