Completion date: 9/30/11

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Non-Destructive Soil Inventory using Inelastic Neutron Scattering: An Application to Nitrogen Controls on Soil Carbon Storage Theme 2: Principal Investigator(s): Ruth D. Yanai Affiliations/Institutions: SUNY ESF Email: rdyanai@syr.edu Mailing address: 210 Marshall Hall, 1 Forestry Dr., Syracuse, NY 13210 Collaborators and affiliations: Lucian Wielopolski, Sudeep Mitra, Brookhaven National Laboratory; Matt Vadeboncoeur, University of New Hampshire, Steve Hamburg, Environmental Defense Fund; April Melvin, Christy Goodale, Cornell University; Ben Rau & Dale Johnson, University of Nevada Completion date: 9/30/11 Inelastic neutron scattering has the potential to non-destructively sample soils for carbon and other nutrients. Coring with a motorized diamond-tipped cylindrical bit can offer much faster access to deep soil samples than digging soil pits, but this method overestimates exchangeable cations and underestimates rock volume, depending on the soil type. Soil respiration measurements in response to nitrogen addition can reveal differences in carbon fluxes too small to be detected as changes in soil pools. Funding support for this project was provided by the Northeastern States Research Cooperative (NSRC), a partnership of Northern Forest states (New Hampshire, Vermont, Maine, and New York), in coordination with the USDA Forest Service. http://www.nsrcforest.org

Project Summary Forest soils can be difficult to sample because of spatial variability, rock content, coarse root systems, and inaccessibility. Traditional methods of soil characterization require excavation, transport, drying, sieving, weighing, and laboratory analysis. Quantitative soil pits are destructive and labor intensive. We demonstrated the use of inelastic neutron scattering to non-destructively measure elements in soils, using a prototype instrument not yet commercially available. We also tested the use of rotary coring, which uses easily obtained equipment and is relatively quick, enabling more samples to be collected than with soil pits, for the same time and cost. We found that rotary coring was appropriate for describing soil carbon and nitrogen. Unfortunately, we found elevated exchangeable cation concentrations in cored soils, presumably due to the grinding of rock and soil during excavation. Coring may still be attractive compared to soil pits, because greater numbers of samples can better characterize spatial heterogeneous forest soils. Although we could not use inelastic neutron scattering to measure the effects of added N on soil carbon storage, we measured soil carbon respiration after N addition in ten northern hardwood stands differing in age and site fertility. We did not find significant effects in the first year of treatment, but we will continue measurements in future years.

Soil Sampling Background Forest soils are notoriously heterogeneous, with both horizontal and vertical spatial variation contributing uncertainty to most sampling approaches. The most accurate method for estimating nutrient pools in soils is probably the quantitative soil pit, but estimates at the stand level are not very precise if the number of pits is small, each pit being time-consuming to excavate. Less destructive approaches to soil sampling, such as inelastic neutron scattering or power coring, could improve estimates of soil nutrient contents due to the speed and efficiency of obtaining many measurements at depth and over a large area.

Inelastic Neutron Scattering (INS) The INS prototype includes a neutron generator, an array of three NaI detectors, and electronics for nuclear spectroscopy. A miniature sealed-tube accelerator produces 14 MeV neutrons. Inelastic neutron scattering occurs when fast neutrons are captured by a carbon nucleus in the soil and reemitted at lower energy along with gamma rays of characteristic energy (4.43 MeV). The gamma radiation is measured by spectroscopy, which indicates the number of carbon atoms detected. Other elements can be detected by gamma radiation at other characteristic energy levels.

INS Results The INS method estimated soil C contents of 4.2 kg C m -2, compared to 5.4 kg C m -2 estimated by soil pits. If repeated, a change of 5% would be statistically detectable. However, results are not readily reproducible due to the uneven topography of the forest floor, which affects the geometry of the area sampled by the INS approach. The prototype INS system is difficult to transport in the field, and was not operable during most of the project period. (a) INS and (b) TNC spectra acquired for 1 h at Bartlett Experimental Forest. The lowest line was counted for 0.5 h, due to a computer error.

Soil Coring Methods We compared samples collected with rotary cores and soil pits at four sites (four soil types): NH (Spodosols), NY (Inceptisols), NV (Mollisols), and CA (Alfisols). Cores were sampled to depths of 52-90 cm. The corer had a 9.5 cm diameter diamond-tipped bit powered by a rotary motor. Cores were extracted in segments of 8-20 cm. Concentrations of exchangeable sodium (Na), magnesium (Mg), potassium (K), and calcium (Ca) were measured in pits and cores at all sites. For two sites (NH, NY), we also modified the coring method to quantify the amount of soil introduced to samples during the insertion and removal of the cores.

Soil Coring Results Estimates of soil mass were 26% higher in cores than pits at the NY site (P < 0.0001). Estimates of rock mass were lower in cores than pits by 67% at the NH site (p<0.0001) and by 45% at the CA site (p=0.002). Cores are more biased against rocks than are soil pits because they are not able to sample at points with rocks larger than the bit. There was no difference between pits and cores at the NV site or the NY site, where the rocks are shale. Soil pit and core rock mass (kg ha -1 ) at the four sites. The lines represent a 1:1 relationship.

The difference between pits and cores in exchangeable cation concentrations was often significant. Concentration of K in cores was significantly higher than in the pits at all four sites. Concentrations of Na were higher in cores at the NV, NY, and NH sites, though Na concentrations were higher in the soil pits than cores at the CA site. Concentrations of Ca were higher in cores at the CA site, but higher in the pits at the NV site. Concentrations of Mg were higher in CA cores than pits. Soil Coring Results Exchangeable soil pit K concentrations (mg g -1 ) plotted against soil core K concentrations at the four study sites. The lines represent a 1:1 relationship.

Soil Respiration Background The northeastern United States has been receiving dramatically elevated atmospheric nitrogen deposition for many decades. This chronic fertilization could result in increased forest growth and carbon sequestration. Soil carbon storage is expected to increase as a result of N pollution, but changes in soil pools are difficult to measure, as discussed above. Instead, we studied carbon fluxes. We measured soil respiration (the loss of carbon from soils by root respiration and microbial respiration, or decomposition) in sites with N addition treatments. We distinguished the response of root respiration from that of decomposers by creating plots free of tree roots by trenching.

Soil Respiration Methods Soil respiration was measured every three to four weeks from May to October using an IRGA system (LI-8100). In each stand, 5 points were measured in each of four plots (control, N, P, and N+P treatments. Stands were in the Bartlett Experimental Forest (BEF), Hubbard Brook Experimental Forest (HB) and Jeffers Brook (JB), in stands of different ages at each of the three sites. One trench (1.8 x 1.8 m, 50 cm depth) was dug per plot in BEF and JB in 2010 to sever and exclude roots from future measurement.

Soil Respiration Results There was not a significant effect of N fertilization on soil respiration in the first year of treatment (P = 0.42 for N; P = 0.37 for NP). There was also no effect of fertilization on soil microbial respiration, as measured in trenched plots (P = 0.61 for N; P = 0.43 for NP). Soil respiration responses to fertilization were unaffected by forest age (P > 0.22) or site (P > 0.39) in both untrenched and trenched plots.

Soil respiration difference between control and fertilization plot (umol m -2 s -1 ) 3.0 2.0 1.0 1 st +N 2 nd +N Untrenched plot 4.0 3.0 2.0 1 st +NP BEF young (C1) BEF young (C2) BEF mid (C4) 2 nd +NP Untrenched plot BEF young (C1) BEF young (C2) BEF mid (C4) 0.0-1.0 1.0 0.0-1.0 BEF mid (C6) BEF old (C7) BEF old (C9) JB mid BEF mid (C6) BEF old (C7) BEF old (C9) JB mid -2.0-2.0 JB old HB mid JB old HB mid -3.0 3.0 May Jun early Jul late Jul Aug Sep Oct Trenched plot -3.0 3.0 HB old May Jun early Jul late Jul Aug Sep Oct Trenched plot HB old 2.0 2.0 1.0 1.0 BEF young (C2) BEF young (C2) 0.0 0.0 BEF mid (C6) BEF old (C7) BEF mid (C6) BEF old (C7) -1.0-1.0 JB mid JB mid -2.0-2.0 JB old JB old -3.0 May Jun early Jul late Jul Aug Sep Oct -3.0 May Jun early Jul late Jul Aug Sep Oct Effect of fertilization on soil respiration at BEF (Bartlett Experimental forest), JB (Jeffers Brook), and HB (Hubbard Brook). On the left are N treatments minus controls; on the right are NP treatments minus controls. Yellow lines show fertilizer additions. Points represent 5 collars in untrenched plots and 1collar in trenched plots.

Implications and applications in the Northern Forest region The rotary coring method is useful for sampling soils for C and N analysis. However, we observed elevated exchangeable cation concentrations in cored samples relative to soil pits in the four soil types tested. Since this method provides a convenient way to collect soil samples at depth, the benefits of capturing spatial heterogeneity may outweigh the possible biases introduced by grinding, especially when the goal is to detect change over time.

Future directions Our original goal was to use INS to measure soil C response to N additions. We demonstrated the use of INS to measure soil C prior to N addition, but we could not use this method to measure C response to treatment. Now we are using other methods to measure ecosystem response to N additions, associated with an NSF-funded collaborative project on Multiple Element Limitation in Northern Hardwood Ecosystems. We will continue to monitor soil respiration in response to additions of N and P, as well as other responses, including microbial N transformations, tree biomass accumulation, litter production, foliar resorption, root production, and sap flow. http://www.esf.edu/melnhe

List of products Peer Reviewed Publications Wielopolski, L., R.D. Yanai, C.R. Levine, S. Mitra, and M.A Vadeboncoeur. 2010. Rapid, nondestructive carbon analysis of forest soils using neutron-induced gamma-ray spectroscopy. For. Ecol. Manag. 260(7): 1132-1137. http://dx.doi.org/10.1016/j.foreco.2010.06.039 Levine, C.R., R.D. Yanai, M.A. Vadeboncouer, S. Hamburg, A. Melvin, C. Goodale, B. Rau, and D. Johnson. Assessing the suitability of using rotary corers for sampling cations in rocky soils. Soil Science Society of America Journal. In review. Rothfuss Dair, B., C.R. Levine, M. Fisk. Soil nitrogen and carbon transformations in field and laboratory manipulations of nitrogen and phosphorus availability. In preparation. Bae, K., R.D. Yanai, T.J. Fahey, M. Fisk. Nutrient availability affects soil respiration and belowground carbon allocation in New Hampshire northern hardwoods. In preparation. Bae, K., R.D. Yanai. Effects of N and P addition on soil microbial respiration and root respiration. In preparation, after another year of observation. Other Publications Levine, C.R. 2011. Assessing the suitability of rotary corers for sampling exchangeable cations in rocky soils. MS thesis, State University of New York, College of Environmental Science and Forestry, Syracuse, NY.

List of products (continued) Conference Presentations Rothfuss Dair, B. C.R. Levine, M.C. Fisk. Nitrogen and phosphorus co-limitation of microbes in soil microcosms. July 11, 2011. Ecological Society of American Annual Meeting, Austin, TX. Levine, C.R., R.D. Yanai, S.P. Hamburg, L. Wielopolski, and S. Mitra. New techniques in soil sampling: Methods to improve long-term ecological research. August 4, 2010, Ecological Society of America Meeting, Pittsburg, PA. Levine, C.R., R.D. Yanai, S.P. Hamburg, L. Wielopolski, and S. Mitra. New techniques in soil sampling: Methods to improve long-term ecological research. April 13, 2010. SUNY-ESF Spotlight on Research. Syracuse, NY. Levine, C.R., R.D. Yanai, S.P. Hamburg, T.K. Refsland, L. Wielopolski, and S. Mitra. New techniques in soil sampling: methods for long-term ecological research. January 28, 2010. New York Society of American Foresters Winter Meeting, East Syracuse, NY. Levine, C.R., R.D. Yanai, S.P. Hamburg, T.K. Refsland, L. Wielopolski, and S. Mitra. New techniques in soil sampling: methods for long-term ecological research. October 31, 2009. Rochester Academy of Science Meeting, Rochester, NY. Levine, C.R., R.D. Yanai, S.P. Hamburg, T.K. Refsland, L. Wielopolski, and S. Mitra. New techniques in soil sampling: methods for long-term ecological research. Sept 12, 2009. LTER All Scientists Meeting, Estes Park, CO.