Sequential combustion separation of soil organic carbon fractions for AMS measurement of 14C and their application in fixation of carbon

  • Xia Yu
  • Weijian ZhouEmail author
  • Yunqiang Wang
  • Peng Cheng
  • Yaoyao Hou
  • Hua Du
  • Xiaohu Xiong
  • Ling Yang
  • Ya Wang
  • Yunchong Fu


A temperature stepped-combustion method for separating soil organic carbon (SOC) fractions and their 14C ages was developed to investigate SOC fixation and stability in soils. After acid-leaching, SOC was sequentially oxidized, and extracted from three temperature intervals: (1) 25–400 °C, (2) 400–600 °C, and (3) 600–900 °C. The acid-soluble carbon and SOC released below 600 °C are labile components, with relatively younger 14C ages, while the SOC released above 600 °C is stable with older 14C ages. We applied this method in a grassland, maize cropland and forest nursery cropland, to assist in understanding the stability of carbon in soils under different land use conditions.


14C ages Labile-stable SOC Reclaimed cropland Temperature stepped-combustion 



This work was jointly supported by National Natural Science Foundation of China (41730108, 41773141, and 41573136); National Research Program for Key Issues in Air Pollution Control (DQGG0105-02); the Strategic Priority Research Program of the Chinese Academy of Sciences (XDA23010302); CAS “Light of West China” Program (XAB2016A01); Youth Innovation Promotion Association CAS (2017452); State Key Laboratory of Loess and Quaternary Geology, Institute of Earth Environment, CAS (SKLLQG1724); Supported by the International Partnership Program of Chinese Academy of Sciences, Grant No. 132B61KYSB20170005. Dr. Cheng Peng would like to express sincere thanks to the Belt &Road Center for Earth Environment Studies and CAS Key Technology Talent Program. We thank anonymous reviewers and the Editor for their insightful comments, which significantly improved this paper. Funding was provided by National Nature Science Foundation of China (Grant No. NSFC41730108), State Key Laboratory of Loess and Quaternary Geology (Grant No. LQ1301).

Compliance with ethical standards

Conflict of interest

The authors declare that they have no conflict of interest.


  1. 1.
    Singh M, Sarkar B, Sarkar S, Churchman J, Bolan N, Mandal S, Menon M, Purakayastha T, Beerling DJ (2017) Stabilization of soil organic carbon as influenced by clay mineralogy. Adv Agron 148:33–84CrossRefGoogle Scholar
  2. 2.
    Dungait JAJ, Hopkins DW, Gregory AS, Whitmore AP (2012) Soil organic matter turnover is governed by accessibility not recalcitrance. Global Change Biol 18:1781–1796CrossRefGoogle Scholar
  3. 3.
    Rumpel C, Amiraslani F, Koutika LS, Smith P, Whitehead D, Wollenberg E (2018) Put more carbon in soils to meet Paris climate pledges. Nature 564:32–34PubMedCrossRefGoogle Scholar
  4. 4.
    Fromm SF, Schwab VF, Trumbore SE, Tichomirowa M (2019) Parent material and depth effects on the age of radiocarbon in chemical fractions for Central German soils. Geophysical Research Abstracts 21Google Scholar
  5. 5.
    Leinweber P, Schulten HR (1995) Composition, stability and turnover of soil organic-matter-investigations by off-line pyrolysis and direct pyrolysis mass-spectrometry. J Anal Appl Pyrol 32:91–110CrossRefGoogle Scholar
  6. 6.
    Lin ZB, Zhang RD (2012) Dynamics of soil organic carbon under uncertain climate change and elevated atmospheric CO2. Pedosphere 22:489–496CrossRefGoogle Scholar
  7. 7.
    Zhou XQ, Chen CR, Wang YF, Smaill S, Clinton P (2013) Warming rather than increased precipitation increases soil recalcitrant organic carbon in a semiarid grassland after 6 years of treatments. PLoS ONE 8:e53761PubMedPubMedCentralCrossRefGoogle Scholar
  8. 8.
    Parton WJ, Schimel DS, Cole CV, Ojima DS (1987) Analysis of factors controlling soil organic-matter levels in great-plains grasslands. Soil Sci Soc Am J 51:1173–1179CrossRefGoogle Scholar
  9. 9.
    Stavi I, Gusarov Y, Halbac-Cotoara-Zamfir R (2019) Collapse and failure of ancient agricultural stone terraces: on-site geomorphic processes, pedogenic mechanisms, and soil quality. Geoderma 344:144–152CrossRefGoogle Scholar
  10. 10.
    Mueller CW, Rethemeyer J, Kao-Kniffin J, Loppmann S, Hinkel KM, Bockheim J (2015) Large amounts of labile organic carbon in permafrost soils of northern Alaska. Global Change Biol 21:2804–2817CrossRefGoogle Scholar
  11. 11.
    Wang H, Stumpf AJ, Kumar P (2018) Radiocarbon and stable carbon isotopes of labile and inert organic carbon in the critical zone observatory in Illinois, USA. Radiocarbon 60:989–999CrossRefGoogle Scholar
  12. 12.
    Rovira P, Vallejo VR (2007) Labile, recalcitrant, and inert organic matter in Mediterranean forest soils. Soil Biol Biochem 39:202–215CrossRefGoogle Scholar
  13. 13.
    Bu XL, Gu XY, Zhou XQ, Zhang MY, Guo ZY, Zhang J, Zhou XH, Chen XY, Wang XH (2018) Extreme drought slightly decreased soil labile organic C and N contents and altered microbial community structure in a subtropical evergreen forest. For Ecol Manag 429:18–27CrossRefGoogle Scholar
  14. 14.
    Yao SH, Zhang YL, Han Y, Han XZ, Mao JD, Zhang B (2019) Labile and recalcitrant components of organic matter of a Mollisol changed with land use and plant litter management: an advanced C-13 NMR study. Sci Total Environ 660:1–10PubMedCrossRefPubMedCentralGoogle Scholar
  15. 15.
    Xie WH, Jia GM, Chen FQ (2013) The soil labile organic carbon fractions at the different ages of tea in three gorges reservoir area. Adv Mater Res 864–867:2645–2648CrossRefGoogle Scholar
  16. 16.
    Dou F, Wright AL, Hons FM (2008) Sensitivity of labile soil organic carbon to tillage in wheat-based cropping systems. Soil Sci Soc Am J 72:1445–1453CrossRefGoogle Scholar
  17. 17.
    Li J, Wen YC, Li XH, Li YT, Yang XD, Lin Z, Song ZZ, Cooper JM, Zhao BQ (2018) Soil labile organic carbon fractions and soil organic carbon stocks as affected by long-term organic and mineral fertilization regimes in the North China Plain. Soil Till Res 175:281–290CrossRefGoogle Scholar
  18. 18.
    Figueiredo CCd, Farias WM, Melo BAd, Chagas JKM, Vale AT, Coser TR (2019) Labile and stable pools of organic matter in soil amended with sewage sludge biochar. Arch Agron Soil Sci 65:770–781CrossRefGoogle Scholar
  19. 19.
    Li S, Zhang SR, Pu YL, Li T, Xu XX, Jia YX, Deng OP, Gong GS (2016) Dynamics of soil labile organic carbon fractions and C-cycle enzyme activities under straw mulch in Chengdu Plain. Soil Till Res 155:289–297CrossRefGoogle Scholar
  20. 20.
    Sun HM, Jiang J, Cui L, Feng WT, Wang YG, Zhang JC (2019) Soil organic carbon stabilization mechanisms in a subtropical mangrove and salt marsh ecosystems. Sci Total Environ 673:502–510PubMedCrossRefGoogle Scholar
  21. 21.
    Helfrich M, Flessa H, Dreves A, Ludwig B (2010) Is thermal oxidation at different temperatures suitable to isolate soil organic carbon fractions with different turnover? J Plant Nutr Soil Sci 173:61–66CrossRefGoogle Scholar
  22. 22.
    Sutton R, Sposito G (2005) Molecular structure in soil humic substances: the new view. Environ Sci Technol 39:9009–9015PubMedCrossRefGoogle Scholar
  23. 23.
    Cambardella CA, Elliott ET (1992) Particulate soil organic-matter changes across a grassland cultivation sequence. Soil Sci Soc Am J 56:777–783CrossRefGoogle Scholar
  24. 24.
    Yang YS, Guo JF, Chen GS, Yin YF, Gao R, Lin CF (2009) Effects of forest conversion on soil labile organic carbon fractions and aggregate stability in subtropical China. Plant Soil 323:153–162CrossRefGoogle Scholar
  25. 25.
    Dias FPM, Hubner R, Nunes FD, Leandro WM, Xavier FAD (2019) Effects of land-use change on chemical attributes of a ferralsol in Brazilian Cerrado. CATENA 177:180–188CrossRefGoogle Scholar
  26. 26.
    Tirol-Padre A, Ladha JK (2004) Assessing the reliability of permanganate-oxidizable carbon as an index of soil labile carbon. Soil Sci Soc Am J 68:969–978CrossRefGoogle Scholar
  27. 27.
    Jiang JY, Li ZW, Xiao HB, Wang DY, Liu C, Zhang XQ, Peng H, Zeng GM (2018) Labile organic matter plays a more important role than the autotrophic bacterial community in regulating microbial CO2 fixation in an eroded watershed. Land Degrad Dev 29:4415–4423CrossRefGoogle Scholar
  28. 28.
    Wang H, Hackley KC, Panno SV, Coleman DD, Liu CL, Brown J (2003) Pyrolysis-combustion 14C dating of soil organic matter. Quat Res 60:348–355CrossRefGoogle Scholar
  29. 29.
    Wang SL, Burr GS, Wang PL, Lin LH, Nguyen VJQG (2016) Tracing the sources of carbon in clay minerals: an example from western Taiwan. Radiocarbon 34:24–32Google Scholar
  30. 30.
    Benbi DK, Brar K, Toor AS, Singh P (2015) Total and labile pools of soil organic carbon in cultivated and undisturbed soils in northern India. Geoderma 237–238:149–158CrossRefGoogle Scholar
  31. 31.
    Lefevre R, Barre P, Moyano FE, Christensen BT, Bardoux G, Eglin T, Girardin C, Houot S, Katterer T, van Oort F, Chenu C (2014) Higher temperature sensitivity for stable than for labile soil organic carbon—evidence from incubations of long-term bare fallow soils. Global Change Biol 20:633–640CrossRefGoogle Scholar
  32. 32.
    Wang S-L, Burr GS, Chen Y-G, Lin Y, Wu T-S (2013) Low-temperature and temperature stepped-combustion of terrace sediments from Nanfu, Taiwan. Radiocarbon 55:553–562CrossRefGoogle Scholar
  33. 33.
    McGeehin J, Burr GS, Jull AJT, Reines D, Gosse J, Davis PT, Muhs D, Southon JR (2016) Stepped-combustion 14C dating of sediment: a comparison with established techniques. Radiocarbon 43:255–261CrossRefGoogle Scholar
  34. 34.
    Mcgeehin J, Burr GS, Hodgins G, Bennett SJ, Robbins JA, Morehead N, Markewich HJR (2004) Stepped-combustion 14C dating of bomb carbon in Lake sediment. Radiocarbon 46:893–900CrossRefGoogle Scholar
  35. 35.
    Wang YQ, Han XW, Jin Z, Zhang CC, Fang LC (2016) Soil organic carbon stocks in deep soils at a watershed scale on the Chinese loess plateau. Soil Sci Soc Am J 80:157–167CrossRefGoogle Scholar
  36. 36.
    Wang YQ, Shao MA, Liu ZP (2013) Vertical distribution and influencing factors of soil water content within 21-m profile on the Chinese Loess Plateau. Geoderma 193:300–310CrossRefGoogle Scholar
  37. 37.
    Duval ME, Galantini JA, Martinez JM, Limbozzi F (2018) Labile soil organic carbon for assessing soil quality: influence of management practices and edaphic conditions. CATENA 171:316–326CrossRefGoogle Scholar
  38. 38.
    Cheng P, Zhou WJ, Wang H, Lu XF, Du H (2013) 14C dating of soil organic carbon (SOC) in Loess-Paleosol using sequential pyrolysis and accelerator mass spectrometry (AMS). Radiocarbon 2–3:563–570CrossRefGoogle Scholar
  39. 39.
    Purdy CB, Burr GS, Meyer R, Helz GR, Mignerey ACJR (2006) Dissolved organic and inorganic 14C concentrations and ages for coastal plain aquifers in southern Maryland. Radiocarbon 34:654–663CrossRefGoogle Scholar
  40. 40.
    Xiong XH, Zhou WJ, Cheng P, Wu SG, Niu ZC, Du H, Lu XF, Fu YC, Burr GS (2017) Δ14 CO2 from dark respiration in plants and its impact on the estimation of atmospheric fossil fuel CO2. J Environ Radioact 169–170:79–84PubMedCrossRefGoogle Scholar
  41. 41.
    Stuiver M, Polach AH (2006) Reporting of C-14 data—discussion. Radiocarbon 19:355–363CrossRefGoogle Scholar
  42. 42.
    Kuzyakov Y, Mitusov A, Schneckenberger K (2006) Effect of C3–C4 vegetation change on δ13C and δ15N values of soil organic matter fractions separated by thermal stability. Plant Soil 283:229–238CrossRefGoogle Scholar
  43. 43.
    Zhou ZJ, Zeng XZ, Chen K, Li Z, Guo S, Shangguan YX, Yu H, Tu SH, Qin YS (2019) Long-term straw mulch effects on crop yields and soil organic carbon fractions at different depths under a no-till system on the Chengdu Plain, China. J Soil Sediment 19:2143–2152CrossRefGoogle Scholar
  44. 44.
    Huo L, Pang HC, Zhao YG, Wang J, Lu C, Li YY (2017) Buried straw layer plus plastic mulching improves soil organic carbon fractions in an arid saline soil from Northwest China. Soil Till Res 165:286–293CrossRefGoogle Scholar
  45. 45.
    Fontaine S, Barot S, Barre P, Bdioui N, Mary B, Rumpel C (2007) Stability of organic carbon in deep soil layers controlled by fresh carbon supply. Nature 450:277-U210CrossRefGoogle Scholar
  46. 46.
    Sanderman J, Baisden WT, Fallon S (2016) Redefining the inert organic carbon pool. Soil Biol Biochem 92:149–152CrossRefGoogle Scholar
  47. 47.
    Goh KM, Rafter TA, Stout JD, Walker TW (1976) The accumulation of soil organic matter and its carbon isotope content in a chronosequence of soils developed on aeolian sand in New Zealand. J Soil Sci 27:89–100CrossRefGoogle Scholar
  48. 48.
    Reimer PJ, Brown TA, Reimer RW (2004) Discussion: reporting and calibration of post-bomb 14C data. Radiocarbon 46:1299–1304CrossRefGoogle Scholar
  49. 49.
    Naegler T, Levin I (2006) Closing the global radiocarbon budget 1945–2005. J Geophys Res Atmos 111:D12311CrossRefGoogle Scholar
  50. 50.
    Angst G, Mueller KE, Eissenstat DM, Trumbore S, Freeman KH, Hobbie SE, Chorover J, Oleksyn J, Reich PB, Mueller CW (2019) Soil organic carbon stability in forests: distinct effects of tree species identity and traits. Global Change Biol 25:1529–1546CrossRefGoogle Scholar
  51. 51.
    Torn MS, Trumbore SE, Chadwick OA, Vitousek PM, Hendricks DM (1997) Mineral control of soil organic carbon storage and turnover. Nature 389:170–173CrossRefGoogle Scholar

Copyright information

© Akadémiai Kiadó, Budapest, Hungary 2019

Authors and Affiliations

  1. 1.State Key Laboratory of Loess and Quaternary Geology, Institute of Earth EnvironmentChinese Academy of SciencesXi’anChina
  2. 2.Shaanxi Key Laboratory of Accelerator Mass Spectrometry Technology and ApplicationXi’an AMS CenterXi’anChina
  3. 3.University of Chinese Academy of SciencesBeijingChina
  4. 4.Interdisciplinary Research Center of Earth Science FrontierBeijing Normal UniversityBeijingChina
  5. 5.CAS Center for Excellence in Quaternary Science and Global ChangeXi’anChina
  6. 6.Open Studio for Oceanic-Continental Climate and Environment ChangesPilot National Laboratory for Marine Science and Technology (Qingdao)QingdaoChina
  7. 7.Institute of Global Environmental ChangeXi’an Jiaotong UniversityXi’anChina

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