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Title: Synthesis and structure of synthetically pure and deuterated amorphous (basic) calcium carbonates

Abstract

It is generally believed that H 2O and OH - are the key species stabilizing and controlling amorphous calcium carbonate “polyamorph” forms, and may in turn control the ultimate crystallization products during synthesis and in natural systems. Yet, the locations and hydrogen-bonding network of these species in ACC have never been measured directly using neutron diffraction. In this paper, we report a synthesis route that overcomes the existing challenges with respect to yield quantities and deuteration, both of which are critically necessary for high quality neutron studies.

Authors:
 [1];  [2];  [3];  [3];  [3];  [4];  [2];  [2];  [2];  [2]
  1. Univ. of Tennessee, Knoxville, TN (United States)
  2. Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Spallation Neutron Source
  3. Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Chemical Sciences Division
  4. Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Materials Science and Technology Division
Publication Date:
Research Org.:
Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)
Sponsoring Org.:
USDOE Office of Science (SC), Basic Energy Sciences (BES) (SC-22)
OSTI Identifier:
1347339
Grant/Contract Number:
AC05-00OR22725; AC02-06CH11357
Resource Type:
Journal Article: Accepted Manuscript
Journal Name:
ChemComm
Additional Journal Information:
Journal Volume: 53; Journal Issue: 20; Journal ID: ISSN 1359-7345
Publisher:
Royal Society of Chemistry
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY

Citation Formats

Wang, Hsiu-Wen, Daemen, Luke L., Cheshire, Michael C., Kidder, Michelle K., Stack, Andrew G., Allard, Lawrence F., Neuefeind, Jörg, Olds, Daniel, Liu, Jue, and Page, Katharine. Synthesis and structure of synthetically pure and deuterated amorphous (basic) calcium carbonates. United States: N. p., 2017. Web. doi:10.1039/C6CC08848A.
Wang, Hsiu-Wen, Daemen, Luke L., Cheshire, Michael C., Kidder, Michelle K., Stack, Andrew G., Allard, Lawrence F., Neuefeind, Jörg, Olds, Daniel, Liu, Jue, & Page, Katharine. Synthesis and structure of synthetically pure and deuterated amorphous (basic) calcium carbonates. United States. doi:10.1039/C6CC08848A.
Wang, Hsiu-Wen, Daemen, Luke L., Cheshire, Michael C., Kidder, Michelle K., Stack, Andrew G., Allard, Lawrence F., Neuefeind, Jörg, Olds, Daniel, Liu, Jue, and Page, Katharine. Fri . "Synthesis and structure of synthetically pure and deuterated amorphous (basic) calcium carbonates". United States. doi:10.1039/C6CC08848A. https://www.osti.gov/servlets/purl/1347339.
@article{osti_1347339,
title = {Synthesis and structure of synthetically pure and deuterated amorphous (basic) calcium carbonates},
author = {Wang, Hsiu-Wen and Daemen, Luke L. and Cheshire, Michael C. and Kidder, Michelle K. and Stack, Andrew G. and Allard, Lawrence F. and Neuefeind, Jörg and Olds, Daniel and Liu, Jue and Page, Katharine},
abstractNote = {It is generally believed that H2O and OH- are the key species stabilizing and controlling amorphous calcium carbonate “polyamorph” forms, and may in turn control the ultimate crystallization products during synthesis and in natural systems. Yet, the locations and hydrogen-bonding network of these species in ACC have never been measured directly using neutron diffraction. In this paper, we report a synthesis route that overcomes the existing challenges with respect to yield quantities and deuteration, both of which are critically necessary for high quality neutron studies.},
doi = {10.1039/C6CC08848A},
journal = {ChemComm},
number = 20,
volume = 53,
place = {United States},
year = {Fri Feb 17 00:00:00 EST 2017},
month = {Fri Feb 17 00:00:00 EST 2017}
}

Journal Article:
Free Publicly Available Full Text
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Cited by: 2works
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  • It is generally believed that H 2O and OH - are the key species stabilizing and controlling amorphous calcium carbonate “polyamorph” forms, and may in turn control the ultimate crystallization products during synthesis and in natural systems. Yet, the locations and hydrogen-bonding network of these species in ACC have never been measured directly using neutron diffraction. We report a synthesis route that overcomes the existing challenges with respect to yield quantities and deuteration, both of which are critically necessary for high quality neutron studies.
  • Spectroscopically pure C/sub 6/H/sub 5/CD/sub 3/ was synthesized from phenyllithium and CD/sub 3/Br. The preparation of CD/sub 3/Br is briefly described. The phenyllithium is transferred under an atmosphcre of dry nitrogen to an autoclave cooled to -80 deg C. The CD/sub 3/Br is rapldly added, and the autoclave is brought slowly to room temperature, with agitation. It is then maintained at 100 deg C for 10 hr and cooled. The contents are hydrolyzed and extracted with ether. A first distillation leads to C/sub 6/H/sub 5/CD/sub 3/ contaminated with benzene from the hydrolysis of excess phenyllithium. Two new fractionations are mademore » with a column containing 40 theoretical plates. The compound obtained boils at 108 deg C under normal pressure, corresponding to C/ sub 6/H/sub 5/CD/sub 3/ of at least 99.5% purity. The infrared spectrum is given. (J.S.R.)« less
  • Aluminum scaling can be a problem following HF acidizing. In this paper, a series of synthetic aluminum scales was prepared and identified. The aluminum compounds of a field scale were identified with similar procedures. Recent field work showed that the use of acetic acid in the HF acidizing sequences significantly decreased scaling. The role of acetic acid is discussed on the basis of laboratory support of these field data.
  • Precipitation, crystal structure, and thermal decomposition behavior of the rare-earth basic carbonates were investigated. Precipitates were produced from hydrolysis of rare-earth cations in hot urea solutions. The light rare earths formed were crystalline with regular geometric shapes, whereas heavy rare earths produced amorphous, spherical monodisperse particles. Crystalline phases belong to ancylite-type orthorhombic symmetry. Unit-cell volume was related to interatomic distance. Thermal decomposition of the crystalline precipitates occurred in two major distinct steps to produce oxide, whereas heavy rare earths decomposed continuously with several distinct effects to produce oxide powder.
  • Peanut-shaped CaCO{sub 3} aggregates, featured of two dandelion-like heads built up from rod-like subunits, have been synthesized via a facile precipitation reaction between Na{sub 2}CO{sub 3} and CaCl{sub 2} at ambient temperature in the presence of magnesium ions and ethanol solvent. The as-prepared products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and inductively coupled plasma atomic emission spectrometry (ICP-AES). The results show that a high magnesium concentration and ethanol solvent are necessary for the formation of the unusual peanut-like aggregates. In addition, a multistep phase transformation process from amorphous calcium carbonate (ACC) to a mixture of ACCmore » and calcite and ultimately to calcite and aragonite was observed in the formation process of the unusual structures. A possible mechanism for the formation of the unusual peanut-shape aggregates has been proposed and discussed.« less