scholarly journals Raman Microspectroscopic Imaging of Binder Remnants in Historical Mortars Reveals Processing Conditions

Heritage ◽  
2019 ◽  
Vol 2 (2) ◽  
pp. 1662-1683 ◽  
Author(s):  
Thomas Schmid ◽  
Petra Dariz
Keyword(s):  
Solid Solution ◽  
Raw Materials ◽  
Solid Solution Series ◽  
Crystal Lattices ◽  
Distribution Maps ◽  
Solution Series ◽  
Crystal Orientations ◽  
Cement Mortars ◽  
Amorphous Compounds ◽  
Compositional Variations

Binder remnants in historical mortars represent a record of the connection between the raw materials that enter the kiln, the process parameters, and the end product of the calcination. Raman microspectroscopy combines high structural sensitivity with micrometre to sub-micrometre spatial resolution and compatibility with conventional thin-sectional samples in an almost unique fashion, making it an interesting complementary extension of the existing methodological arsenal for mortar analysis. Raman spectra are vibrational fingerprints of crystalline and amorphous compounds, and contain marker bands that are specific for minerals and their polymorphic forms. Relative intensities of bands that are related to the same crystalline species change according to crystal orientations, and band shifts can be caused by the incorporation of foreign ions into crystal lattices, as well as stoichiometric changes within solid solution series. Finally, variations in crystallinity affect band widths. These effects are demonstrated based on the analysis of three historical mortar samples: micrometric distribution maps of phases and polymorphs, crystal orientations, and compositional variations of solid solution series of unreacted clinker grains in the Portland cement mortars of two 19th century castings, and the crystallinities of thermal anhydrite clusters in a high-fired medieval gypsum mortar as a measure for the applied burning temperature were successfully acquired.

scholarly journals Rinkite–nacareniobsite-(Ce) solid solution series and hainite from the Ilímaussaq alkaline complex: occurrence and compositional variation

2014 ◽  
Vol 62 ◽  
pp. 1-15
Author(s):  
Jørn G. Rønsbo ◽  
Henning Sørensen ◽  
Encarnacion Roda-Robles ◽  
François Fontan ◽  
Pierre Monchoux
Keyword(s):  
Solid Solution ◽  
Electron Microprobe ◽  
Compositional Variation ◽  
Solid Solution Series ◽  
Alkaline Complex ◽  
Full Extension ◽  
X Ray ◽  
Solution Series ◽  
Compositional Variations ◽  
A Minor

In the Ilímaussaq alkaline complex, minerals from the rinkite–nacareniobsite-(Ce) solid solution series have been found in pulaskite pegmatite, sodalite foyaite, naujaite and naujaite pegmatite from the roof sequence, and in marginal pegmatite, kakortokite and lujavrite from the floor sequence. The electron microprobe analyses embrace almost the full extension of the solid solution series and confirm its continuity. The solid solution series shows similar compositional variations in the roof and floor sequences: Rinkite members of the series are found in the less evolved rocks in the two sequences, whereas nacareniobsite-Ce members occur in the most evolved rocks and pegmatites in the two sequences. The REE (+Y) content varies from 0.83 atoms per formula unit (apfu) in rinkite from pulaskite pegmatite to 1.31 apfu in nacareniobsite-(Ce) from naujaite pegmatite. The main substitution mechanisms in the solid solution series investigated in this work are 2Ca2+ = Na+ + REE3+ and Ti4+ + Ca2+ = Nb5+ + Na+. The increased contents of Nb5+ and REE3+ are only to a minor degree compensated through the F1– = O2– substitution. The chondrite normalised REE patterns of the minerals develop in a similar way in the two sequences, showing relative La-enrichment and Y-depletion from the less to the most evolved rocks. Hainite has not previously been found in the Ilímaussaq complex. It was here identified in a pulaskite pegmatite sample by a combination of X-ray diffraction giving the unit cell dimensions a = 9.5923(7) Å, b = 7.3505(5) Å, c = 5.7023(4) Å, α = 89.958(2)°, β = 100.260(1)°, γ = 101.100(2)°, and X-ray powder pattern and electron microprobe data giving the empirical formula (Ca1.62 Zr0.16Y 0.22) (Na0.87Ca1.11) (Ca 1.65 REE0.35)Na(Ti0.81Nb0.09Fe0.08 Zr0.02)(Si2O7)2O0.99F2.96. Based on published and the present data it is documented that minerals from the hainite-götzenite solid solution series show a compositional variation between the ideal end members (Y,REE,Zr)Na2Ca4Ti(Si2O7)2OF3 and NaCa6Ti(Si2O7)2OF3.

The Crystal Structure of Bi2PbMnO4(PO4)2, a Member of a New Solid Solution Series in the Bi–Pb–Mn–P Oxide System

2002 ◽  
Vol 165 (2) ◽  
pp. 324-333 ◽  
Author(s):  
Olivier Cousin ◽  
Marielle Huve ◽  
Pascal Roussel ◽  
Olivier Perez ◽  
Hugo Steinfink
Keyword(s):  
Crystal Structure ◽  
Solid Solution ◽  
Oxide System ◽  
Solid Solution Series ◽  
Solution Series

Rietveld refinement of the solid-solution series: (Cu,Mg)SO4·H2O

1995 ◽  
Vol 10 (3) ◽  
pp. 189-194 ◽  
Author(s):  
C. L. Lengauer ◽  
G. Giester
Keyword(s):  
Solid Solution ◽  
Rietveld Refinement ◽  
Powder Diffraction ◽  
Rietveld Method ◽  
Structure Refinement ◽  
Solid Solution Series ◽  
Cation Site ◽  
Tg Analysis ◽  
X Ray ◽  
Solution Series

The kieserite-type solid-solution series of synthetic (Cu,Mg)SO4·H2O was investigated by TG-analysis and X-ray powder diffraction using the Rietveld method. Representatives with Cu≥20 mol% are triclinic distorted () analogous to the poitevinite (Cu,Fe)SO4·H2O compounds. Cation site ordering with preference of Cu for the more distorted M1 site was additionally proven by the structure refinement.

ChemInform Abstract: The Solid Solution Series (GeTe)x(LiSbTe2)2(1 ≤ x ≤ 11) and the Thermoelectric Properties of (GeTe)11(LiSbTe2)2.

ChemInform ◽  
2013 ◽  
Vol 44 (50) ◽  
pp. no-no
Author(s):  
Thorsten Schroeder ◽  
Stefan Schwarzmueller ◽  
Christian Stiewe ◽  
Johannes de Boor ◽  
Markus Hoelzel ◽  
...  
Keyword(s):  
Solid Solution ◽  
Thermoelectric Properties ◽  
Solid Solution Series ◽  
Solution Series

Crystal chemistry of lamprophyllite-group minerals from the Murun alkaline complex (Russia) and pegmatites of Rocky Boy and Gordon Butte (USA): single crystal X-ray diffraction and Raman spectroscopy study

2021 ◽  
Vol 77 (2) ◽  
Author(s):  
Sergey M. Aksenov ◽  
Anastasia D. Ryanskaya ◽  
Yuliya V. Shchapova ◽  
Nikita V. Chukanov ◽  
Nikolay V. Vladykin ◽  
...  
Keyword(s):  
Solid Solution ◽  
Single Crystal ◽  
Raman Spectra ◽  
Crystal Chemistry ◽  
Solid Solution Series ◽  
X Ray Diffraction ◽  
Alkaline Complex ◽  
Oh Groups ◽  
X Ray ◽  
Solution Series

Specific features of the crystal chemistry of lamprophyllite-group minerals (LGMs) are discussed using the available literature data and the results of the single-crystal X-ray diffraction and a Raman spectroscopic studies of several samples taken from the Murun alkaline complex (Russia), and Rocky Boy and Gordon Butte pegmatites (USA) presented here. The studied samples are unique in their chemical features and the distribution of cations over structural sites. In particular, the sample from the Gordon Butte pegmatite is a member of the barytolamprophyllite–emmerichite solid solution series, whereas the samples from the Murun alkaline complex and from the Rocky Boy pegmatite are intermediate members of the solid solution series formed by lamprophyllite and a hypothetical Sr analogue of emmerichite. The predominance of O2− over OH− and F− at the X site is a specific feature of sample Cha-192 from the Murun alkaline complex. New data on the Raman spectra of LGMs obtained in this work show that the wavenumbers of the O—H stretching vibrations depend on the occupancies of the M2 and M3 sites coordinating with (OH)− groups. Cations other than Na+ and Ti4+ (mainly, Mg and Fe3+) can play a significant role in the coordination of the X site occupied by (OH)−. Data on polarized Raman spectra of an oriented sample indicate that the OH groups having different local coordinations have similar orientations with respect to the crystal. The calculated measures of similarity (Δ) for lamprophyllite and ericssonite are identical (0.157 and 0.077 for the 2M- and 2O-polytypes, respectively), which indicates that these minerals are crystal-chemically isotypic and probably should be considered within the same mineral group by analogy to the other mineralogical groups which combine isotypic minerals.

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