14C measurements provide a useful test for determining the degree to which chemical and physical fractionation of soil organic matter (SOM) are successful in separating labile and refractory organic matter components. Results from AMS measurements of fractionated SOM made as part of several projects are summarized here, together with suggestions for standardization of fractionation procedures. Although no single fractionation method will unequivocally separate SOM into components cycling on annual, decadal and millennial time scales, a combination of physical (density separation or sieving) and chemical separation methods (combined acid and base hydrolysis) provides useful constraints for models of soil carbon dynamics in several soil types.

Temperate forests of North America are thought to be significant sinks of atmospheric CO2. We developed a below-ground carbon (C) budget for well-drained soils in Harvard Forest Massachusetts, an ecosystem that is storing C. Measurements of carbon and radiocarbon (14C) inventory were used to determine the turnover time and maximum rate of CO2 production from heterotrophic respiration of three fractions of soil organic matter (SOM): recognizable litter fragments (L), humified low density material (H), and high density or mineral-associated organic matter (M). Turnover times in all fractions increased with soil depth and were 2-5 years for recognizable leaf litter, 5-10 years for root litter, 40-100+ years for low density humified material and >100 years for carbon associated with minerals. These turnover times represent the time carbon resides in the plant + soil system, and may underestimate actual decomposition rates if carbon resides for several years in living root, plant or woody material. Soil respiration was partitioned into two components using 14C: recent photosynthate which is metabolized by roots and microorganisms within a year of initial fixation (Recent-C), and C that is respired during microbial decomposition of SOM that resides in the soil for several years or longer (Reservoir-C). For the whole soil, we calculate that decomposition of Reservoir-C contributes approximately 41% of the total annual soil respiration. Of this 41%, recognizable leaf or root detritus accounts for 80% of the flux, and 20% is from the more humified fractions that dominate the soil carbon stocks. Measurements of CO2 and 14CO2 in the soil atmosphere and in total soil respiration were combined with surface CO2 fluxes and a soil gas diffusion model to determine the flux and isotopic signature of C produced as a function of soil depth. 63% of soil respiration takes place in the top 15 cm of the soil (O + A + Ap horizons). The average residence time of Reservoir-C in the plant + soil system is 8±1 years and the average age of carbon in total soil respiration (Recent-C + Reservoir-C) is 44±1 years. The O and A horizons have accumulated 4.4 kgC m-2 above the plow layer since abandonment by settlers in the late-1800's. C pools contributing the most to soil respiration have short enough turnover times that they are likely in steady state. However, most C is stored as humified organic matter within both the O and A horizons and has turnover times from 40 to 100+ years respectively. These reservoirs continue to accumulate carbon at a combined rate of 10-30 gC m-2 yr-1. This rate of accumulation is only 5-15% of the total ecosystem C sink measured in this stand using eddy covariance methods.

The sealed tube zinc reduction method for converting CO2 to graphite for AMS 14C measurements was originally developed for rapid production of graphite in biomedical tracer experiments. The method was usually thought to have low precision and a high background. We have modified the zinc reduction method originally outlined in Vogel [J.S. Vogel, Radiocarbon 34 (3) (1992) 344] by carefully controlling the amounts of reagents (zinc, titanium hydride and Co or Fe catalyst) and now routinely obtain a precision of 2-3‰ and a relatively low background of ∼50,000 14C years when analyzing for 14C at the Keck Carbon Cycle AMS facility at UC Irvine. Fractionation of carbon isotopes does occur during graphitization and depends on the graphitization yield, which can be affected by the amounts of reagents used and other conditions. The δ13C of our zinc-reduced graphite is usually lighter by 2-3‰ than the CO2 from which it is made, but this is corrected for in our system by simultaneous measurement of 13C/12C along with 14C/12C by the spectrometer. This method is suitable for 14C enriched samples, as well as natural abundance 14C samples, especially those with modern 14C contents. With improved precision and background, we believe that many disciplines can benefit from this technique because of its low cost and rapid production of graphite. © 2007 Elsevier B.V. All rights reserved.