Dear Frank, This is going to be a fairly radical suggestion but should narrowing down the source of your problem. You can try to run procedure duplicates using methods other than Indiana Zinc such as equilibration using Pt-on-alumina catalyst [1] or reduction employing Tanweer's Mn protocol [2]. And then there is always the acetylene method. This should at least tell you if the degree of uncertainty is caused by your current sample preparation. Another way of going about would be to prepare sample duplicates sticking to your current routine and have the samples double-checked on another IRMS. All the best, Wolfram [1] Scrimgeour, C.M. et al.; J. Biol. Mass Spectrom., 22, 383-387 (1993) [2] Tanweer, A., amd Han. L.-F., Isotopes Environ. Health Stud., 32, 97-103 (1996) ***************************************************** Dr. W. Meier-Augenstein Lecturer/Research Fellow University of Dundee, Dept. of Anatomy & Physiology, Small's Wynd, DUNDEE DD1 4HN, United Kingdom Tel.: +44-(0)1382-34/5124, /4968 +44-(0)468 -314563 Fax: +44-(0)1382-34/5514 e-mail: [log in to unmask] URL: http://www.dundee.ac.uk/AnatPhys/wma/wolfram.htm *****************************************************