Applicability of calcimetry in low-calcium carbonate sediments


  • Cecilia Cantera Departamento de Ciencias Geológicas, Facultad de Ciencias Exactas y Naturales, Universidad de Buenos Aires
  • Ivana Laura Ozán Consejo Nacional de Investigaciones Científicas y Técnicas – UBA. Instituto de Geociencias Básicas, Aplicadas y Ambientales de Buenos Aires.

Palabras clave:

Non-calcareous sediments/soils, Pressure calcimetry, Detection/ Quantification limits, Losson- Ignition, Micromorphology


In Earth and Environmental Sciences, pressure calcimetry is probably the most efficient and fast method to determine calcium carbonate (CaCO3) content in rocks, sediments and soils. However, measurements of low-CaCO3 samples can be less reliable by calcimetry, depending on the instrument used. This problematic is particularly relevant for sediments and soils with low content of CaCO3, very common in past and present lakes, soils and hydromorphic systems (e.g., peatbogs, mires, wetlands), where CaCO3 analysis contribute to understand water table changes, groundwater oscillation, ecology and wind-related processes, among others. In this context, this work presents a simple protocol to obtain accurate CaCO3 determinations through pressure calcimetry in low-CaCO3 samples (<4%), even though their CaCO3 content falls below the limit of detection of the instruments. Calibration curves were first established with a CaCO3 standard to calculate the critical value, detection limit and quantification limit, using two different pressure calcimeters. By considering these thresholds, a set of four natural samples with low-CaCO3 content were measured by pressure calcimetry and also analyzed by Loss-on-Ignition and micromorphology. Results with 1 g of sample were lower than the detection limit. Accordingly, a gradual increase of sediment mass was applied until obtaining results above the quantification limit. The amount of CaCO3 per g was thus inferred. Both calcimeters showed comparable results and high consistency with micromorphological observations. The CaCO3 content calculated by Loss-on-Ignition showed slightly lower values, likely due to the loss of structural water and dehydroxylation of some minerals exposed to high temperature, affecting calculations of both organic and inorganic carbon.


Bernal, E., and Guo, X. (2014). Limit of detection and limit of quantification determination in gas chromatography. Advances in gas chromatography, 3(1): 57-63.

Bockheim, J.G., and Douglass, D.C. (2006). Origin and significance of calcium carbonate in soils of southwestern Patagonia. Geoderma, 136(3-4): 751-762.

Currie, L.A. (1995). Nomenclature in evaluation of analytical methods including detection and quantification capabilities (IUPAC Recommendations 1995). Pure and Applied Chemistry, 67(10): 1699-1723.

Currie, L.A. (1999). Nomenclature in evaluation of analytical methods including detection and quantification capabilities:(IUPAC Recommendations 1995). Analytica Chimica Acta, 391(2): 105-126.

Dean, W.E. (1999). The carbon cycle and biogeochemical dynamics in lake sediments. Journal of Paleolimnology, 21(4): 375-393.

Doberschütz, S., Frenzel, P., Haberzettl, T., Kasper, T., Wang, J., Zhu, L., Daut, G., Schwalb, A., and Mäusbacher, R. (2014). Monsoonal forcing of Holocene paleoenvironmental change on the central Tibetan Plateau inferred using a sediment record from Lake Nam Co (Xizang, China). Journal of Paleolimnology, 51(2): 253-266.

Elfaki, J.T., Gafei, M.O., Sulieman, M.M., and Ali, M.E. (2016). Assessment of calcimetric and titrimetric methods for calcium carbonate estimation of five soil types in central Sudan. Journal of Geoscience and Environment Protection, 4: 120-127.

Engleman, E.E., Jackson, L.L., and Norton, D.R. (1985). Determination of carbonate carbon in geological materials by coulometric titration. Chemical Geology, 53(1-2): 125-128.

Folk, R.L., Andrews, P.B., and Lewis, S.W. (1970). Detrital sedimentary rock classification and nomenclature for use in New Zealand, New Zealand. Journal of Geology and Geophysics, 13: 937-968.

Forman, S.L., Tripaldi, A., and Ciccioli, P.L. (2014). Eolian sand sheet deposition in the San Luis paleodune field, western Argentina as an indicator of a semi-arid environment through the Holocene. Palaeogeography, Palaeoclimatology, Palaeoecology, 411: 122-135.

Gialanella, S., Girardi, F., Ischia, G., Lonardelli, I., Mattarelli, M., and Montagna, M. (2010). On the goethite to hematite phase transformation. Journal of Thermal Analysis and Calorimetry, 102(3): 867-873.

Gómez, C., Lagacherie, P., and Coulouma, G. (2008). Continuum removal versus PLSR method for clay and calcium carbonate content estimation from laboratory and airborne hyperspectral measurements. Geoderma, 148(2): 141-148.

Heiri, O., Lotter, A.F., and Lemcke, G. (2001). Loss on ignition as a method for estimating organic and carbonate content in sediments: reproducibility and comparability of results. Journal of Paleolimnology, 25(1) :101-110.

Horváth, B., Opara-Nadi, O., and Beese, F. (2005). A simple method for measuring the carbonate content of soils. Soil Science Society of America Journal, 69(4): 1066-1068.

ISO 11843-2:2000. (2000). Capability of detection ? Part 2: Methodology in the linear calibration case. In International Organization for Standardization. Corrigendum: ISO 11843-2/Cor1:2007: 24.

Kassim, J.K. (2013). Method for estimation of calcium carbonate in soils from Iraq. International Journal of Environment, 1(1): 9-19.

Li, N., Sack, D., Sun, J., Liu, S., Liu, B., Wang, J., Gao, G., Li, D., Song, Z., and Jie, D. (2020). Quantifying the carbon content of aeolian sediments: Which method should we use? Catena, 185: 104276.

Loeppert, R.H., and Suarez, D.L. (1996). Carbonate and gypsum. Methods of soil analysis: Part 3 Chemical Methods, 5: 437-474.

Martínez, J.M., Galantini, J.A., Duval, M.E., López, F.M., and Iglesias, J.O. (2018). Estimating soil organic carbon in Mollisols and its particle-size fractions by loss-on-ignition in the semiarid and semihumid Argentinean Pampas. Geoderma Regional, 12: 49-55.

Mocák, J., Bond, A.M., Mitchell, S., and Schollary, G. (1997). A Statistical Overview of Standard (IUPAC and ACS) and New Procedures for Determining the Limits of Detection and Quantification: Application to Voltammetric and Stripping Techniques. Pure Applied Chemistry, 69: 297-328.

Mocák, J., Janiga, I., and Rábarobá, E. (2009). Evaluation of IUPAC limit of detection and iso minimum detectable value electrochemical determination of lead. Nova Biotechnologica, 9(1): 91-100.

Moore, D.M., and Reynolds Jr, R.C. (1997). X-ray Diffraction and the Identification and Analysis of Clay Minerals. Second edition. Oxford University Press (OUP). 332 pp.

Munsell Color (1994). Munsell Soil Color Charts. Macbeth Division of Kollmargen Instruments Corporation. New Windsor, New York. 28 pp.

Ozán, I.L., Méndez, C., Oriolo, S., Orgeira, M.J., Tripaldi, A., and Vásquez, C.A. (2019). Depositional and post-depositional processes in human-modified cave contexts of west-central Patagonia (Southernmost South America). Palaeogeography, Palaeoclimatology, Palaeoecology, 532: 109268.

Rowell, D.L. (1994). Soil Science: Methods and Applications. Prentice Hall, Harlow. 368 pp.

Santisteban, J.I., Mediavilla, R., Lopez-Pamo, E., Dabrio, C.J., Zapata, M., Garcia, M., Castan, S., and Martínez-Alfaro, P.E. (2004). Loss on ignition: a qualitative or quantitative method for organic matter and carbonate mineral content in sediments? Journal of Paleolimnology, 32(3): 287-299.

Sherrod, L.A., Dunn, G., Peterson, G.A., and Kolberg, R.L. (2002). Inorganic carbon analysis by modified pressure-calcimeter method. Soil Science Society of America, 66: 299–305.

Stetson, S.J., and Osborne, S.L. (2015). Further modification of pressure-calcimeter method for soil inorganic carbon analysis. Soil Science and Plant Analysis, 46(17): 2162-2167.

Stoops, G. (2003). Guidelines for Analysis and Description of Soil and Regolith Thin Sections. Soil Science Society of America, Madison. 185 pp.

Stoops, G., Marcelino, V., and Mees, F. (2010). Interpretation of Micromorphological Features of Soil and Regoliths. Elsevier, Amsterdam. 720 pp.

Sun, H., Nelson, M., Chen, F., and Husch, J. (2009). Soil mineral structural water loss during loss on ignition analyses. Canadian Journal of Soil Science, 89(5): 603-610.

Tatzber, M., Stemmer, M., Spiegel, H., Katzlberger, C., Haberhauer, G., and Gerzabek, M.H. (2007). An alternative method to measure carbonate in soils by FT-IR spectroscopy. Environmental Chemistry Letters, 5(1): 9-12.

Tripaldi, A., and Forman, S.L. (2007). Geomorphology and chronology of Late Quaternary dune fields of western Argentina. Palaeogeography, Palaeoclimatology, Palaeoecology, 251(2): 300-320.

Tripaldi, A., and Forman, S.L. (2016). Eolian depositional phases during the past 50 ka and inferred climate variability for the Pampean Sand Sea, western Pampas, Argentina. Quaternary Science Reviews, 139: 77-93.

Tripaldi, A., and Zárate, M.A. (2016). A review of Late Quaternary inland dune systems of South America east of the Andes. Quaternary International, 410: 96-110.

Tripaldi, A., Ciccioli, P.L., Alonso, M.S., and Forman, S.L. (2010). Petrography and geochemistry of late Quaternary dune fields of western Argentina: Provenance of aeolian materials in southern South America. Aeolian Research, 2(1): 33-48.

Tripaldi, A., Zárate, M.A., Forman, S.L., Badger, T., Doyle, M.E., and Ciccioli, P. (2013). Geological evidence for a drought episode in the western Pampas (Argentina, South America) during the early–mid 20th century. The Holocene, 23(12): 1731-1746.

Toms, P., King, M., Zárate, M., Kemp, R., and Foit, F. (2004). Geochemical characterization, correlation, and optical dating of tephra in alluvial sequences of central western Argentina. Quaternary Research, 62(1): 60-75.

Vogelgesang, J., and Hädrich, J. (1998). Limits of detection, identification and determination: a statistical approach for practitioners. Accreditation and quality assurance, 3(6): 242-255.

Wang, Q., Li, Y., and Wang, Y. (2011). Optimizing the weight loss-on-ignition methodology to quantify organic and carbonate carbon of sediments from diverse sources. Environmental Monitoring and Assessment, 174(1): 241-257.

Wang, J.P, Wang, X.J., and Zhang, J. (2013). Evaluating loss-on-ignition method for determinations of soil organic and inorganic carbon in arid soils of Northwestern China. Pedosphere, 23(5): 593-599.

Zárate, M.A., and Tripaldi, A. (2012). The aeolian system of central Argentina. Aeolian Research, 3(4): 401-417.

Zolitschka, B., Brauer, A., Negendank, J.F., Stockhausen, H., and Lang, A. (2000). Annually dated late Weichselian continental paleoclimate record from the Eifel, Germany. Geology, 28(9): 783-786.

Zougagh, M., R??os, A., and Valcárcel, M. (2005). Direct determination of total carbonate salts in soil samples by continuous-flow piezoelectric detection. Talanta, 65(1): 29-35.


2022-10-03 — Actualizado el 2022-12-21

Cómo citar

Cantera, C., & Ozán, I. L. (2022). Applicability of calcimetry in low-calcium carbonate sediments. Latin American Journal of Sedimentology and Basin Analysis, 29(2), 83-95. Recuperado a partir de



Trabajos de investigación