Steven J Hall1, Wenjuan Huang1, Kenneth E Hammel2,3. 1. Department of Ecology, Evolution, and Organismal Biology, Iowa State University, 251 Bessey Hall, Ames, IA, 50011, USA. 2. US Forest Products Laboratory, Madison, WI, 53726, USA. 3. Department of Bacteriology, University of Wisconsin, Madison, WI, 53706, USA.
Abstract
RATIONALE: Carbon dioxide isotope (δ13 C value) measurements enable quantification of the sources of soil microbial respiration, thus informing ecosystem C dynamics. Tunable diode lasers (TDLs) can precisely measure CO2 isotopes at low cost and high throughput, but are seldom used for small samples (≤5 mL). We developed a TDL method for CO2 mole fraction ([CO2 ]) and δ13 C analysis of soil microcosms. METHODS: Peaks in infrared absorbance following constant volume sample injection to a carrier were used to independently measure [12 CO2 ] and [13 CO2 ] for subsequent calculation of δ13 C values. Using parallel soil incubations receiving differing C substrates, we partitioned respiration from three sources using mixing models: native soil organic matter (SOM), added litter, and synthetic lignin containing a 13 C label at Cβ of the propyl side chain. RESULTS: Once-daily TDL calibration enabled accurate quantification of δ13 C values and [CO2 ] compared with isotope ratio mass spectrometry (IRMS), with long-term external precision of 0.17 and 0.31‰ for 5 and 1 mL samples, respectively, and linear response between 400 and 5000 μmol mol-1 CO2 . Production of CO2 from native soil C, added litter, and lignin Cβ varied over four orders of magnitude. Multiple-pool first-order decay models fitted to data (R2 > 0.98) indicated substantially slower turnover for lignin Cβ (17 years) than for the dominant pool of litter (1.3 years) and primed soil C (3.9 years). CONCLUSIONS: Our TDL method provides a flexible, precise, and high-throughput (60 samples h-1 ) alternative to IRMS for small samples. This enables the use of C isotopes in increasingly sophisticated experiments to test biogeochemical controversies, such as the fate of lignins in soil.
RATIONALE: Carbon dioxide isotope (δ13 C value) measurements enable quantification of the sources of soil microbial respiration, thus informing ecosystem C dynamics. Tunable diode lasers (TDLs) can precisely measure CO2 isotopes at low cost and high throughput, but are seldom used for small samples (≤5 mL). We developed a TDL method for CO2 mole fraction ([CO2 ]) and δ13 C analysis of soil microcosms. METHODS: Peaks in infrared absorbance following constant volume sample injection to a carrier were used to independently measure [12 CO2 ] and [13 CO2 ] for subsequent calculation of δ13 C values. Using parallel soil incubations receiving differing C substrates, we partitioned respiration from three sources using mixing models: native soil organic matter (SOM), added litter, and synthetic lignin containing a 13 C label at Cβ of the propyl side chain. RESULTS: Once-daily TDL calibration enabled accurate quantification of δ13 C values and [CO2 ] compared with isotope ratio mass spectrometry (IRMS), with long-term external precision of 0.17 and 0.31‰ for 5 and 1 mL samples, respectively, and linear response between 400 and 5000 μmol mol-1 CO2 . Production of CO2 from native soil C, added litter, and lignin Cβ varied over four orders of magnitude. Multiple-pool first-order decay models fitted to data (R2 > 0.98) indicated substantially slower turnover for lignin Cβ (17 years) than for the dominant pool of litter (1.3 years) and primed soil C (3.9 years). CONCLUSIONS: Our TDL method provides a flexible, precise, and high-throughput (60 samples h-1 ) alternative to IRMS for small samples. This enables the use of C isotopes in increasingly sophisticated experiments to test biogeochemical controversies, such as the fate of lignins in soil.