Characterization of Structure in Biogenic Amorphous Calcium Carbonate: Pair Distribution Function and Nuclear Magnetic Resonance Studies of Lobster Gastrolith
Abstract
Total X-ray scattering and pair distribution function analysis are combined with nuclear magnetic resonance spectroscopy to identify key differences in structural properties between biogenic and synthetic samples of amorphous calcium carbonate (ACC). Biogenic samples studied are gastroliths taken from the American lobster and are composed of hydrated ACC containing minor impurities. X-ray pair distribution functions reveal that the short- and medium-range structure found in synthetic ACC also occurs in gastrolith ACC, notably with atomic pair correlations extending up to ∼10 Å. The 13 C NMR spectra of gastrolith ACC show a distribution of carbonate environments as seen in synthetic hydrated ACC. However, 1 H NMR spectroscopy reveals that a mobile H 2 O component and hydroxyl groups found in synthetic hydrated ACC are absent in the gastrolith ACC. This difference may arise from differences in local conditions of ACC formation. The 31 P NMR results indicate that inorganic phosphate is the principal form of the minor phosphorus. Gastrolith that was allowed to age shows the presence of calcite and vaterite, as well as residual ACC. 31 P NMR also reveals trace amounts of monetite (CaHPO 4 ) in aged samples, raising the possibility that fresh gastrolith ACC may contain a minor component of amorphous calcium phosphate. The findings suggest that important differences in the hydrous components between synthetic and biogenic hydrated ACC influence stability of the amorphous phase and its transformation to crystalline forms, thereby extending the foundation for advanced materials applications in engineered systems.
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The NMR line width for ACC is 3.5 ppm FWHM.
“The observed chemical shift also corresponds well with amorphous calcium carbonate (ACC), however the NMR line width for ACC is considerably more broad, 3.5 ppm FWHM [32-34].”
From Mechanochemical formation of highly stable amorphous calcium carbonate in calcium silicates: Potential long-term storage of CO2 in cement (2024) · cites this paper as [33]
The observed 13C chemical shift corresponds well with amorphous calcium carbonate (ACC).
“The observed chemical shift also corresponds well with amorphous calcium carbonate (ACC), however the NMR line width for ACC is considerably more broad, 3.5 ppm FWHM [32-34].”
From Mechanochemical formation of highly stable amorphous calcium carbonate in calcium silicates: Potential long-term storage of CO2 in cement (2024) · cites this paper as [33]
In biogenic ACC from lobster gastrolith, NMR signals for structural water and hydroxyl associated with 13C are absent, although synthetic ACC contains them.
“Reeder et al. [33] noted that although synthetic ACC contains significant structural water and hydroxyl associated with 13 C, these NMR signals are absent in biogenic ACC derived from lobster gastrolith.”
From Mechanochemical formation of highly stable amorphous calcium carbonate in calcium silicates: Potential long-term storage of CO2 in cement (2024) · cites this paper as [33]
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- Authors
- Reeder, R. J., Tang, Y., Schmidt, M. P., Kubista, L. M., Cowan, D. F., & Phillips, B. L.
- Affiliations
- Stony Brook University (US)
- The Lobster Conservancy, Friendship, Maine 04547, United States
- Corresponding author
- Reeder, Richard J.
- Venue
- Crystal Growth & Design
- Publisher
- American Chemical Society (ACS)
- Published
- 2013-04-19
- Volume
- 13
- Issue
- 5
- Pages
- 1905-1914
- ISSN
- 1528-7483 (ISSN-L)
- 1528-7505
- OpenAlex
- W2015765084
- Cited by
- 70
- References
- 42
- Citations by year
- 2026: 2 · 2025: 6 · 2024: 7 · 2023: 4 · 2022: 4 · 2021: 6 · 2020: 2 · 2019: 4 · 2018: 8 · 2017: 3 · 2016: 5 · 2015: 6 · 2014: 7 · 2013: 5
- FWCI
- 2.93
- Type
- journal article
- Language
- en
- Open access
- closed
- Locations
- Crystal Growth & Design (publishedVersion)
- Topics
- Physical Sciences › Materials Science › Biomaterials › Calcium Carbonate Crystallization and Inhibition
- Physical Sciences › Environmental Science › Environmental Engineering › Microbial Applications in Construction Materials
- Physical Sciences › Materials Science › Materials Chemistry › Crystallization and Solubility Studies
- Keywords
- amorphous calcium carbonate, Homarus americanus, hydroxyl groups, phosphate impurity, monetite, calcite, vaterite, amorphous calcium phosphate, amorphous phase stability, biomineralization
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