Skip to main content

Analysis of carbon in sediments using fast neutron activation analysis (FNAA)


Purpose: Measurement of carbon in cores of undisturbed sediments may provide valuable information on historical trends in sea primary production and carbonate precipitation which can be related to climate changes. Since core sediments are usually subjected to a different analysis, it is important to preserve the sample. A non-destructive technique for carbon measurement in sediments based on fast neutron activation analysis (FNAA) has been developed, which might replace the loss-on-ignition (LOI) as a conventional method for carbon analysis.

Materials and methods: The method was tested on sediment samples collected from the Western Black Sea at depths up to 22 m. A surface sample and a core cut in centimeter intervals were freeze-dried. Samples weighing between 60 and 300 g were irradiated with the portable neutron generator. Gamma rays from 12C(n,n'γ)12C nuclear reaction were counted between 2000 and 4000 s by LaBr3:Ce detector. Standards for direct comparison and construction of the calibration line were prepared as mixtures of different amounts of quartz sand and graphite powder. The FNAA results for total carbon (TC) were verified by LOI at 1000 °C. LOI at 450 °C and treatment with 1 M HCl were used to separate inorganic carbon (IC) and organic carbon (OC), respectively, followed by the FNAA measurements.

Results and discussion: Climate effects on physical and biological marine processes are evident as historical changes in carbon flux to sediments. Carbon in sediments is found in the form of the OC produced by photosynthetic organisms and as IC produced by calcifying organisms and precipitated as calcite. The FNAA is usually applied to samples weighing more than 1 kg. The method was optimized to reduce the minimum weight of the sample to 60 g, after subsequent adaptation of the setup geometry. Carbon content measured in cores and surface sediment was between 2.8 and 6.1 wt%. OC constituted up to 84% of TC measured in the core. The FNAA measurements were in good agreement with LOI analysis.

Conclusions: The results have shown that FNAA can be used for the non-destructive determination of carbon in sediments in samples weighing ≥ 60 g. FNAA is non-destructive, robust, and fast in comparison to conventional methods for carbon determination such as LOI. The disadvantage is a relatively high MDL of 1%.

This is a preview of subscription content, access via your institution.

Fig. 1
Fig. 2
Fig. 3
Fig. 4


  1. Bates NR, Mathis JT (2009) The Arctic Ocean marine carbon cycle: evaluation of air-sea CO2 exchanges, ocean acidification impacts and potential feedbacks. Biogeosciences 6:2433–2459

    Article  CAS  Google Scholar 

  2. Bhatti JS, Bauer IE (2002) Comparing loss-on-ignition with dry combustion as a method for determining carbon content in upland and lowland forest ecosystems. Commun Soil Sci Plant Anal 33:3419–3430

    Article  CAS  Google Scholar 

  3. Bonvin D (2000) X-ray fluorescence spectrometry in the iron and steel industry. In: Meyers RA (ed) Encyclopedia of analytical chemistry. John Wiley & Sons Ltd, Chichester, pp 9009–9028

    Google Scholar 

  4. Cartapanis O, Galbraith ED, Bianchi D, Jaccard SL (2018) Carbon burial in deep-sea sediment and implications for oceanic inventories of carbon and alkalinity over the last glacial cycle. Clim Past 14:1819–1850

    Article  Google Scholar 

  5. Chmura GL, Anisfeld SC, Cahoon DR, Lynch JC (2003) Global carbon sequestration in tidal, saline wetland soils. Glob Biogeochem Cycles 17:1111

    Article  CAS  Google Scholar 

  6. Clais P, Sabine C, Bala G, Bopp L, Brovkin V, Canadell J, Chhabra A, DeFries R, Galloway J, Heimann M, Jones C, Le Quéré C, Myneni RB, Piao S, Thornton P (2013) Carbon and other biogeochemical cycles. In: Stocker TF, Qin D, Plattner GK, Tignor M, Allen SK, Boschung J, Nauels A, Xia Y, Bex V, Midgley PM (eds) Climate change 2013: the physical science basis, Contribution of Working Group I to the Fifth Assessment Report of the Intergovernmental Panel on Climate Change, Cambridge University Press, Cambridge and New York, pp 465–570

  7. Dean WE (1974) Determination of carbonate and organic matter in calcareous sediments and sedimentary rocks by loss on ignition: comparison with other methods. J Sediment Petrol 44:242–248

    CAS  Google Scholar 

  8. Eastern (2013) Carbon analysis with X-ray fluorescence. Eastern Applied Research Inc. Accessed 16 September 2019

  9. Frangipane G, Pistolato M, Molinaroli E, Guerzoni S, Tagliapietra D (2009) Comparison of loss on ignition and thermal analysis stepwise methods for determination of sedimentary organic matter. Aquat Conserv Mar Freshwat Ecosyst 19:24–33

    Article  Google Scholar 

  10. Freibauer A, Rounsevell MDA, Smith P, Verhagen J (2004) Carbon sequestration in the agricultural soils of Europe. Geoderma 122:1–23

    Article  CAS  Google Scholar 

  11. Heiri O, Lotter AF, Lemcke G (2001) Loss on ignition as a method for estimating organic and carbonate content in sediments: reproducibility and comparability of results. J Paleolimnol 25:101–110

    Article  Google Scholar 

  12. Komada T, Anderson MR, Dorfmeier CL (2008) Carbonate removal from coastal sediments for the determination of organic carbon and isotopic signatures, δ13C and Δ14C: comparison of fumigation and direct acidification by hydrochloric acid. Limnol Oceanogr Methods 6:254–262

    Article  CAS  Google Scholar 

  13. Lal R, Follett RF, Stewart BA, Kimble JM (2007) Soil carbon sequestration to mitigate climate change and advance food security. Soil Sci 172:943–956

    Article  CAS  Google Scholar 

  14. Leong LS, Tanner PA (1999) Comparison of methods for determination of organic carbon in marine sediment. Mar Pollut Bull 38:875–879

    Article  CAS  Google Scholar 

  15. Mitsch WJ, Bernal B, Nahlik AM, Mander Ü, Zhang L, Anderson CJ, Jørgensen SE, Brix H (2013) Wetlands, carbon, and climate change. Landsc Ecol 28:583–597

    Article  Google Scholar 

  16. NOAA-ESRL (2019) Mauna Loa Observatory, Hawaii. Accessed 14 May 2019

  17. Obhodas J, Valkovic V, Sudac D, Matika D, Pavic I, Kollar R (2010) Environmental security of the coastal sea floor in the sea ports and waterways of the Mediterranean region. Nucl Instrum Method: Phys Res Sect A 619:419–426

    Article  CAS  Google Scholar 

  18. Pribyl DW (2010) A critical review of the conventional SOC to SOM conversion factor. Geoderma 156:75–83

    Article  CAS  Google Scholar 

  19. Sabine CL, Feely RA, Gruber N, Key RM, Lee K, Bullister JL, Wanninkhof R, Wong CS, Wallace DWR, Tilbrook B, Millero FJ, Peng TH, Kozyr A, Ono T, Rios AF (2004) The oceanic sink for anthropogenic CO2. Science 305:367–371

    Article  CAS  Google Scholar 

  20. Schumacher BA (2002) Methods for the determination of total organic carbon (TOC) in soils and sediments. U.S. EPA, Washington, pp 1–23

    Google Scholar 

  21. Simakov SP, Pavlik A, Vonach H, Hlavâc S (1998) Status of experimental, and evaluated discrete y-ray production at E,=14.5 MeV: final report of research contract 7809/RB, performed under the CRP on measurement, calculation and evaluation of photon production data. IAEA, Nuclear Data Section, pp 1-62

  22. Solomon S, Plattner GK, Knutti R, Friedlingstein P (2009) Irreversible climate change due to carbon dioxide emissions. Proc Natl Acad Sci 106:1704–1709

    Article  Google Scholar 

  23. Sundquist ET, Burruss RC, Faulkner SP, Gleason RA, Harden JW, Kharaka YK, Tieszen LL, Waldrop, MP (2008) Carbon sequestration to mitigate climate change. U.S. Geol Surv Fact Sheet 2008-3097.

  24. Valkovic V, Sudac D, Obhodas J, Eleon C, Perot B, Carasco C, Sannié G, Boudergui GK, Kondrasovs V, Corre G, Normand S, Woo R, Bourbotte JM (2013) The use of alpha particle tagged neutrons for the inspection of objects on the sea floor for the presence of explosives. Nucl Instrum Method: Phys Res Sect A 703:133–137

    Article  CAS  Google Scholar 

  25. Yakubova G, Kavetskiy A, Prior SA, Torbert HA (2019) Tagged neutron method for carbon analysis of large soil samples. Appl Radiat Isot 150:127–134

    Article  CAS  Google Scholar 

Download references


This research was partially financed by the IAEA RER7009 project “Enhancing Coastal Management in the Adriatic and the Black Sea by Using Nuclear Analytical Techniques” and partially by the Croatian Science Foundation—Youth Careers Development Project (ESF-DOK-1-2018).

Author information



Corresponding author

Correspondence to Jasmina Obhođaš.

Additional information

Publisher’s note

Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.

Responsible editor: Marta Castellote

Rights and permissions

Reprints and Permissions

About this article

Verify currency and authenticity via CrossMark

Cite this article

Vinković, A., Obhođaš, J., Sudac, D. et al. Analysis of carbon in sediments using fast neutron activation analysis (FNAA). J Soils Sediments 20, 2741–2748 (2020).

Download citation


  • Carbon
  • FNAA
  • Loss-on-ignition
  • Sediment
  • The Black Sea