Complete elimination of carbonates: a critical step in the accurate measurement of organic and black carbon in sediments.

Accurate measurement of organic carbon (OC) and black carbon (BC) in sediments requires the complete removal of coexisting inorganic carbonates from the sample before instrumental analysis. The removal of carbonates from sediments is achieved with acidification, which causes the dissolution and decomposition of carbonates with accompanying effervescence. This effervescence, or the lack of it, is commonly used as an indicator for the presence or absence of carbonates. We have found that the lack of effervescence endpoint used with the direct acidification method (adding aliquots of acid to samples) is not a reliable indicator for complete removal of carbonates from sediment samples. The ineffectiveness of the lack of effervescence endpoint, we believe, is caused by the presence of carbonates with dissolution rates much slower than those of calcite, resulting in much slower rates of visible effervescence. We propose and demonstrate a method for determining the amount of acid required for complete elimination of all carbonates using Lake Michigan (USA) sediment samples. Based on our experiences with the lack of effervescence endpoint, we recommend that in any scheme for analysis of OC and/or BC, a minimum of two samples be treated with three different levels of acidification, with the lowest level being the same as that planned for all the OC and/or BC analyses. There can be no significant differences among the OC and BC contents measured using the three different levels of acidification.