Skip to main content
SpringerLink
Log in

Pitfalls of acid leaching method for determining organic and inorganic carbon contents in marine sediments

  • Published:
Acta Oceanologica Sinica Aims and scope Submit manuscript

Abstract

Organic and inorganic carbon contents of marine sediments are important to reconstruct marine productivity, global carbon cycle, and climate change. A proper method to separate and determine organic and inorganic carbons is thus of great necessity. Although the best method is still disputable, the acid leaching method is widely used in many laboratories because of its ease-of-use and high accuracy. The results of the elemental analysis of sediment trap samples reveal that organic and inorganic carbon contents cannot be obtained using the acid leaching method, causing an infinitely amplified error when the carbon content of the decarbonated sample is 12%±1% according to a mathematical derivation. Acid fumigation and gasometric methods are used for comparison, which indicates that other methods can avoid this problem in organic carbon analysis. For the first time, this study uncovers the pitfalls of the acid leaching method, which limits the implication in practical laboratory measurement, and recommends alternative solutions of organic/inorganic carbon determination in marine sediments.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Log in via an institution

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Institutional subscriptions

Similar content being viewed by others

References

  • Bai Yazhi, Liu Jihua, Zhang Hui, et al. 2013. The analysis of organic carbon and total nitrogen in marine sediments. Marine Environmental Science (in Chinese), 32(3): 444–447, 459

    Google Scholar 

  • Bisutti I, Hilke I, Raessler M. 2004. Determination of total organic carbon-An overview of current methods. TrAC Trends in Analytical Chemistry, 23(10-11): 716–726

    Article  Google Scholar 

  • Black H D, Anderson W T, Alvarez Zarikian C A. 2018. Data report: organic matter, carbonate, and stable isotope stratigraphy from IODP Expedition 346 Sites U1426, U1427, and U1429. In: Tada R, Murray R W, Alvarez Zarikian C A, et al., eds. Proceedings of the Integrated Ocean Drilling Program, Volume 346. College Station, TX: Integrated Ocean Drilling Program, 2–3

    Google Scholar 

  • Blattmann T M, Zhang Yanwei, Zhao Yulong, et al. 2018. Contrasting fates of petrogenic and biospheric carbon in the South China Sea. Geophysical Research Letters, 45(17): 9077–9086, doi: https://doi.org/10.1029/2018GL079222

    Article  Google Scholar 

  • Brodie C R, Leng M J, Casford J S L, et al. 2011. Evidence for bias in C and N concentrations and ´13C composition of terrestrial and aquatic organic materials due to pre-analysis acid preparation methods. Chemical Geology, 282(3–4): 67–83

    Article  Google Scholar 

  • Byers S C, Mills E L, Stewart P L. 1978. A comparison of methods of determining organic carbon in marine sediments, with suggestions for a standard method. Hydrobiologia, 58(1): 43–47, doi: https://doi.org/10.1007/BF00018894

    Article  Google Scholar 

  • Castro C G, Chavez F P, Pennington J T, et al. 2018. Temporal variability of downward fluxes of organic carbon off Monterey Bay. Deep Sea Research Part II: Topical Studies in Oceanography, 151: 89–101, doi: https://doi.org/10.1016/j.dsr2.2018.07.001

    Article  Google Scholar 

  • Chen Jianfang, Wiesner M G, Li Hongliang, et al. 2015. Biogeochemical fluxes and biological pump composition in the South China Sea. Bulletin of Mineralogy, Petrology & Geochemistry (in Chinese), 34(5): 911–919

    Google Scholar 

  • Chen Jianfang, Zheng Lianfu, Chen Ronghua, et al. 1998. Fluxes and constituents of particulate matter in the South China Sea in comparison with sediment accumulation rates. Acta Sedimentologica Sinica (in Chinese), 16(3): 14–19

    Google Scholar 

  • Cheng Sihai, Lei Zhisheng, Chen Daohua. 2010. Determination of carbonate in marine sediment by element analyzer. Chemical Analysis & Meterage (in Chinese), 19(5): 29–31

    Google Scholar 

  • Froelich P N. 1980. Analysis of organic carbon in marine sediments. Limnology & Oceanography, 25(3): 564–572

    Article  Google Scholar 

  • Galy V, Bouchez J, France-Lanord C. 2007. Determination of total organic carbon content and δ13C in carbonate-rich detrital sediments. Geostandards and Geoanalytical Research, 31(3): 199–207, doi: https://doi.org/10.1111/j.1751-908X.2007.00864.x

    Article  Google Scholar 

  • Gibbs R J. 1977. Effect of combustion temperature and time, and of the oxidation agent used in organic carbon and nitrogen analyses of sediments and dissolved organic material. Journal of Sedimentary Research, 47(2): 547–550

    Google Scholar 

  • Harris D, Horwáth W R, Van Kessel C. 2001. Acid fumigation of soils to remove carbonates prior to total organic carbon or carbon-13 isotopic analysis. Soil Science Society of America Journal, 65(6): 1853–1856, doi: https://doi.org/10.2136/sssaj2001.1853

    Article  Google Scholar 

  • Hedges J I, Stern J H. 1984. Carbon and nitrogen determinations of carbonate-containing solids. Limnology and Oceanography, 29(3): 657–663, doi: https://doi.org/10.4319/lo.1984.29.3.0657

    Article  Google Scholar 

  • Jones G A, Kaiteris P. 1983. A vacuum-gasometric technique for rapid and precise analysis of calcium carbonate in sediments and soils. Journal of Sedimentary Research, 53(2): 655–660, doi: https://doi.org/10.1306/212F825B-2B24-11D7-8648000102C1865D

    Article  Google Scholar 

  • Keil R. 2017. Anthropogenic forcing of carbonate and organic carbon preservation in marine sediments. Annual Review of Marine Science, 9(1): 151–172, doi: https://doi.org/10.1146/annurev-marine-010816-060724

    Article  Google Scholar 

  • King P, Kennedy H, Newton P P, et al. 1998. Analysis of total and organic carbon and total nitrogen in settling oceanic particles and a marine sediment: an interlaboratory comparison. Marine Chemistry, 60(3–4): 203–216

    Article  Google Scholar 

  • Komada T, Anderson M R, Dorfmeier C L. 2008. Carbonate removal from coastal sediments for the determination of organic carbon and its isotopic signatures, δ13C and Δ14C: comparison of fumigation and direct acidification by hydrochloric acid. Limnology and Oceanography: Methods, 6(6): 254–262, doi: https://doi.org/10.4319/lom.2008.6.254

    Google Scholar 

  • Li Liangge, Xu Jinshu. 1987. A comparison of major methods of determination of organic carbon in marine sediments. Tropic Oceanology (in Chinese), 6(1): 46–51

    Google Scholar 

  • Li Jiabiao, Ke Changzhi, Kang Shouling, et al. 2008. GB/T 12763.8-2007 Specifications for oceanographic survey—Part 8: Marine geology and geophysics survey (in Chinese). Beijing: Standards Press of China, 22–28

    Google Scholar 

  • Lorrain A, Savoye N, Chauvaud L, et al. 2003. Decarbonation and preservation method for the analysis of organic C and N contents and stable isotope ratios of low-carbonated suspended particulate material. Analytica Chimica Acta, 491(2): 125–133, doi: https://doi.org/10.1016/S0003-2670(03)00815-8

    Article  Google Scholar 

  • Nelson D W, Sommers L E. 1982. Total carbon, organic carbon, and organic matter. In: Sparks D L, Page A L, Helmke P A, et al., eds. Methods of Soil Analysis. Madison: Agronomy Society of America and Soil Science Society of America, 539–579

    Google Scholar 

  • Passow U, Carlson C A. 2012. The biological pump in a high CO2 world. Marine Ecology Progress Series, 470: 249–271, doi: https://doi.org/10.3354/meps09985

    Article  Google Scholar 

  • Peng Yajun, Wang Yujue, Liu Dongyan, et al. 2015. Acid treatment effects on the carbon stable isotope values of marine sediments. Haiyang Xuebao (in Chinese), 37(12): 85–92

    Google Scholar 

  • Qiu Lingjia, Huang Guolin, Su Yu, et al. 2015. An overview on current measurment methods of total organic carbon. Guangdong Chemical Industry (in Chinese), 42(9): 107–108, 96

    Google Scholar 

  • Roberts A A, Palacas J G, Frost I C. 1973. Determination of organic carbon in modern carbonate sediments. Journal of Sedimentary Petrology, 43(4): 1157–1159

    Google Scholar 

  • Ryba S A, Burgess R M. 2002. Effects of sample preparation on the measurement of organic carbon, hydrogen, nitrogen, sulfur, and oxygen concentrations in marine sediments. Chemosphere, 48(1): 139–147, doi: https://doi.org/10.1016/S0045-6535(02)00027-9

    Article  Google Scholar 

  • Schubert C J, Nielsen B. 2000. Effects of decarbonation treatments on δ13C values in marine sediments. Marine Chemistry, 72(1): 55–59, doi: https://doi.org/10.1016/S0304-4203(00)00066-9

    Article  Google Scholar 

  • Schwartz V. 1995. Fractionated combustion analysis of carbon in forest soils—New possibilities for the analysis and characterization of different soils. Fresenius’ Journal of Analytical Chemistry, 351(7): 629–631, doi: https://doi.org/10.1007/BF00323339

    Article  Google Scholar 

  • Sun Xuan, Song Jinming, Yu Ying, et al. 2014. A rapid method for determing the total organic carbon and total nitrogen in marine sediments with an elemental analyzer. Marine Sciences (in Chinese), 38(7): 14–19

    Google Scholar 

  • Tan Yang, Wu Xueli, Hou Lijie. 2018. The effects of sample treatment methods on marine sediment organic carbon stable isotope. Marine Environmental Science (in Chinese), 37(5): 780–784

    Google Scholar 

  • Tripathi S, Tiwari M, Lee J, et al. 2017. First evidence of denitrification vis-à-vis monsoon in the Arabian Sea since Late Miocene. Scientific Reports, 7(1): 43056, doi: https://doi.org/10.1038/srep43056

    Article  Google Scholar 

  • Verardo D J, Froelich P N, McIntyre A. 1990. Determination of organic carbon and nitrogen in marine sediments using the Carlo Erba NA-1500 Analyzer. Deep Sea Research Part A. Oceanographic Research Papers, 37(1): 157–165, doi: https://doi.org/10.1016/0198-0149(90)90034-S

    Article  Google Scholar 

  • Walkley A, Black I A. 1934. An examination of the Degtjareff method for determining soil organic matter, and a proposed modification of the chromic acid titration method. Soil Science, 37(1): 29–38, doi: https://doi.org/10.1097/00010694-193401000-00003

    Article  Google Scholar 

  • Wang Yifan, Huang Depei, Cui Shuying. 1988. Determination of total carbon, organic carbon and inorganic carbon in marine sediments by 240C elemental analyzer. Marine Environmental Science (in Chinese), 7(2): 73–77

    Google Scholar 

  • Weliky K, Suess E, Ungerer C A, et al. 1983. Problems with accurate carbon measurements in marine sediments and particulate matter in seawater: A new approach. Limnology and Oceanography, 28(6): 1252–1259, doi: https://doi.org/10.4319/lo.1983.28.6.1252

    Article  Google Scholar 

  • Wu Jinping, Calvert S E, Wong C S, et al. 1999. Carbon and nitrogen isotopic composition of sedimenting particulate material at Station Papa in the subarctic northeast Pacific. Deep Sea Research Part II: Topical Studies in Oceanography, 46(11–12): 2793–2832

    Article  Google Scholar 

  • Yang Shouye, Li Congxian. 2006. Compositions of organic elements and carbonate in the late Cenozoic sediments of the Changjiang Delta: Implication for paleoenvironmental changes. Geochimica (in Chinese), 35(3): 249–256

    Google Scholar 

  • Zhang Weiyan, Jin Haiyan, Zhang Fuyuan, et al. 2009. Organic carbon distribution in the Yangtze River estuary-Hangzhou Bay and its adjacent sea area. Advances in Earth Science (in Chinese), 24(11): 1202–1209

    Google Scholar 

Download references

Acknowledgements

We acknowledge the helpful suggestions provided by Martin G. Wiesner of Universität Hamburg, Germany. We also thank Pengfei Ma, Shaohua Zhao, Xiaodong Zhang, Kui Duan, and Baozhi Lin from Tongji University for their participation in the cruise or experimental analysis.

Author information

Authors and Affiliations

  1. State Key Laboratory of Marine Geology, Tongji University, Shanghai, 200092, China

    Chen Ling, Zhifei Liu, Jingwen Zhang, Yulong Zhao, Yanwei Zhang & Adrian R. Fernandez

Authors
  1. Chen Ling
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. Zhifei Liu
    View author publications

    You can also search for this author in PubMed Google Scholar

  3. Jingwen Zhang
    View author publications

    You can also search for this author in PubMed Google Scholar

  4. Yulong Zhao
    View author publications

    You can also search for this author in PubMed Google Scholar

  5. Yanwei Zhang
    View author publications

    You can also search for this author in PubMed Google Scholar

  6. Adrian R. Fernandez
    View author publications

    You can also search for this author in PubMed Google Scholar

Corresponding author

Correspondence to Zhifei Liu.

Additional information

Foundation item: The National Natural Science Foundation of China under contract Nos 41530964, 41776047, 41876048 and 91528304.

Rights and permissions

Reprints and permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

Ling, C., Liu, Z., Zhang, J. et al. Pitfalls of acid leaching method for determining organic and inorganic carbon contents in marine sediments. Acta Oceanol. Sin. 39, 96–102 (2020). https://doi.org/10.1007/s13131-020-1631-z

Download citation

  • Received:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s13131-020-1631-z

Key words

Search

Navigation