Silicon-Oxygen Region Infrared and Raman Analysis of Opals: The Effect of Sample Preparation and Measurement Type

An extensive infrared (IR) spectroscopy study using transmission, specular and diffuse reflectance, and attenuated total reflection (ATR) was undertaken to characterise opal-AG, opal-AN (hyalite), opal-CT and opal-C, focussing on the Si-O fingerprint region (200–1600 cm<sup>−1</sup>). We...

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Main Authors: Neville J. Curtis, Jason R. Gascooke, Allan Pring
Format: Article
Language:English
Published: MDPI AG 2021-02-01
Series:Minerals
Subjects:
Online Access:https://www.mdpi.com/2075-163X/11/2/173
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spelling doaj-5fca62fd807e43deab2dbfa105b12d972021-02-08T00:04:38ZengMDPI AGMinerals2075-163X2021-02-011117317310.3390/min11020173Silicon-Oxygen Region Infrared and Raman Analysis of Opals: The Effect of Sample Preparation and Measurement TypeNeville J. Curtis0Jason R. Gascooke1Allan Pring2South Australian Museum, North Terrace, Adelaide, SA 5000, AustraliaCollege of Science and Engineering, Flinders University, Bedford Park, SA 5042, AustraliaCollege of Science and Engineering, Flinders University, Bedford Park, SA 5042, AustraliaAn extensive infrared (IR) spectroscopy study using transmission, specular and diffuse reflectance, and attenuated total reflection (ATR) was undertaken to characterise opal-AG, opal-AN (hyalite), opal-CT and opal-C, focussing on the Si-O fingerprint region (200–1600 cm<sup>−1</sup>). We show that IR spectroscopy is a viable alternative to X-ray powder diffraction (XRD) as a primary means of classification of opals even when minor levels of impurities are present. Variable angle specular reflectance spectroscopy shows that the three major IR bands of opal are split into transverse optical (TO) and longitudinal optical (LO) components. Previously observed variability in powder ATR is probably linked to the very high refractive index of opals at infrared wavelengths, rather than heterogeneity or particle size effects. An alternative use of ATR using unpowdered samples provides a potential means of non-destructive delineation of play of colour opals into opal-AG or opal-CT gems. We find that there are no special structural features in the infrared spectrum that differentiate opal from silica glasses. Evidence is presented that suggests silanol environments may be responsible for the structural differences between opal-AG, opal-AN and other forms of opaline silica. Complementary studies with Raman spectroscopy, XRD and scanning electron microscopy (SEM) provide evidence of structural trends within the opal-CT type.https://www.mdpi.com/2075-163X/11/2/173opalhyalitegeyseritemeniliteinfraredRaman
collection DOAJ
language English
format Article
sources DOAJ
author Neville J. Curtis
Jason R. Gascooke
Allan Pring
spellingShingle Neville J. Curtis
Jason R. Gascooke
Allan Pring
Silicon-Oxygen Region Infrared and Raman Analysis of Opals: The Effect of Sample Preparation and Measurement Type
Minerals
opal
hyalite
geyserite
menilite
infrared
Raman
author_facet Neville J. Curtis
Jason R. Gascooke
Allan Pring
author_sort Neville J. Curtis
title Silicon-Oxygen Region Infrared and Raman Analysis of Opals: The Effect of Sample Preparation and Measurement Type
title_short Silicon-Oxygen Region Infrared and Raman Analysis of Opals: The Effect of Sample Preparation and Measurement Type
title_full Silicon-Oxygen Region Infrared and Raman Analysis of Opals: The Effect of Sample Preparation and Measurement Type
title_fullStr Silicon-Oxygen Region Infrared and Raman Analysis of Opals: The Effect of Sample Preparation and Measurement Type
title_full_unstemmed Silicon-Oxygen Region Infrared and Raman Analysis of Opals: The Effect of Sample Preparation and Measurement Type
title_sort silicon-oxygen region infrared and raman analysis of opals: the effect of sample preparation and measurement type
publisher MDPI AG
series Minerals
issn 2075-163X
publishDate 2021-02-01
description An extensive infrared (IR) spectroscopy study using transmission, specular and diffuse reflectance, and attenuated total reflection (ATR) was undertaken to characterise opal-AG, opal-AN (hyalite), opal-CT and opal-C, focussing on the Si-O fingerprint region (200–1600 cm<sup>−1</sup>). We show that IR spectroscopy is a viable alternative to X-ray powder diffraction (XRD) as a primary means of classification of opals even when minor levels of impurities are present. Variable angle specular reflectance spectroscopy shows that the three major IR bands of opal are split into transverse optical (TO) and longitudinal optical (LO) components. Previously observed variability in powder ATR is probably linked to the very high refractive index of opals at infrared wavelengths, rather than heterogeneity or particle size effects. An alternative use of ATR using unpowdered samples provides a potential means of non-destructive delineation of play of colour opals into opal-AG or opal-CT gems. We find that there are no special structural features in the infrared spectrum that differentiate opal from silica glasses. Evidence is presented that suggests silanol environments may be responsible for the structural differences between opal-AG, opal-AN and other forms of opaline silica. Complementary studies with Raman spectroscopy, XRD and scanning electron microscopy (SEM) provide evidence of structural trends within the opal-CT type.
topic opal
hyalite
geyserite
menilite
infrared
Raman
url https://www.mdpi.com/2075-163X/11/2/173
work_keys_str_mv AT nevillejcurtis siliconoxygenregioninfraredandramananalysisofopalstheeffectofsamplepreparationandmeasurementtype
AT jasonrgascooke siliconoxygenregioninfraredandramananalysisofopalstheeffectofsamplepreparationandmeasurementtype
AT allanpring siliconoxygenregioninfraredandramananalysisofopalstheeffectofsamplepreparationandmeasurementtype
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