Harry, we recently ran sediments from Florida Bay for C/N on our Carlo Erba/Optima setup. the following is from an email sent to me by the person who prepped these samples. "FB seds are approximately 90-95% carbonate. I added 40mL of 2N HCl to 1 gram of sed., sonicated for 5min., sit overnight, and rinse until the pH is close to that of D.I. water , then dry in oven overnight, grind, and analyze. Apparently this "wash out" method (as it's called in the literature) results in loss of up to 50% of organic carbon due to loss of acid soluble fraction. However, the %C and N ratio generally stays the same." we also tried the "fuming acid" technique (adding acid to the boat itself), and seemed to get d13C numbers that were lighter by about 1.5 per mil as compared to the "wash out" method. Perhaps the lighter acid-soluble organic C is remaining in the silver cup versus being washed away in the other method... We haven't explored this much further yet. For what it's worth, the wash out method is more labor intensive--but the fuming acid took over a week to completely remove carbonate material from our sediments. good luck, Cyndi Cyndi Brock U.S. Geological Survey DFC, Bldg. 21, MS 963 Denver, CO 80225 office: 303-236-0278 lab: 303-236-7694 fax: 303-236-4930 email: [log in to unmask]