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Critical Assessment of the Mineralogical Collections At Examensarbete vid Institutionen för geovetenskaper Degree Project at the Department of Earth Sciences ISSN 1650-6553 Nr 391 Critical Assessment of the Mineralogical Collections at Uppsala University using Raman Spectroscopy Kritisk studie av de mineralogiska samlingarna vid Uppsala universitet med hjälp av Ramanspektroskopi Yuliya Zhuk INSTITUTIONEN FÖR GEOVETENSKAPER DEPARTMENT OF EARTH SCIENCES Examensarbete vid Institutionen för geovetenskaper Degree Project at the Department of Earth Sciences ISSN 1650-6553 Nr 391 Critical Assessment of the Mineralogical Collections at Uppsala University using Raman Spectroscopy Kritisk studie av de mineralogiska samlingarna vid Uppsala universitet med hjälp av Ramanspektroskopi Yuliya Zhuk ISSN 1650-6553 Copyright © Yuliya Zhuk Published at Department of Earth Sciences, Uppsala University (www.geo.uu.se), Uppsala, 2017 Abstract Critical Assessment of the Mineralogical Collections at Uppsala University using Raman Spectroscopy Yuliya Zhuk The technique of Raman spectroscopy was applied in order to identify and characterize the number of minerals in the mineralogical collection at the Department of Earth Sciences. The collection was broadened with five rare carbonates borrowed from the collection of the Swedish Museum of Natural History in Stockholm. In total, 66 specimens were examined. The characteristics of interest included possible presence and nature of defects and impurities, degree of crystallinity, residual stresses, possible treatment by natural heat sources (e.g. radionuclides) or chemicals (e.g. polishing agents), and fluorescence. Raman spectroscopy was chosen as examination method because of its distinctive advantage over traditional techniques – a non-destructive probing of pristine materials and minimum or no preparation. Besides, Raman spectroscopy performs very well in collecting the needed characteristics, in terms of its sensitivity, as well ability to probe miniature grains in a matrix with a high spatial resolution. A portable system was used to identify the presence of impurities and the fingerprint of the host rock in the majority of the examined carbonates. The rare carbonate burbankite showed distinct fluorescence bands, which likely can be explained by its complicated chemical composition. The Raman system was used for gemmological purposes and helped to identify the purity of the gems. Diamond and two rubies showed to be free from impurities, but red corundum showed a broad peak, which may represent traces of natural heat treatment, which in turn could be caused by regional metamorphism or even by a radiation source. Furthermore, the correlation between the signal intensity of the fluorites’ bands and the chemical composition of the minerals were studied. The experiment showed that blue fluorite fully misses the peak T2g while purple and grey fluorites showed a well- developed and easily recognizable peak at this location. Thus, it was discovered that the presence and intensity of this peak is directly dependent on the fluorite’s colour, i.e. on the host species, which are incorporated in the crystal structure, such as metals, rare earth elements (REE) or even organic substances. Moreover, residual tensile stress was identified in colourless quartz. The tensile stress was estimated to be in the interval between 0.23 and 1.0 GPa. The Raman system was used to identify different end-members of the garnet family. Raman spectroscopy showed to have high analytical power and helped to estimate the ratio between the end- members in eight garnet samples. In one case, fluorescence was linked to the presence of REEs in the structure of almandine. One sample of calcite showed to be incorrectly placed in the collection. This work will now form a solid foundation for the mineral characteristics handbook. Keywords: Raman spectroscopy, gemmology, geology, mineralogy, Mineralogical Collection Degree Project E1 in Earth Sciences, 1GV025, 30 credits Supervisor: Peter Lazor Department of Earth Sciences, Uppsala University, Villavägen 16, SE-752 36 Uppsala (www.geo.uu.se) ISSN 1650-6553, Examensarbete vid Institutionen för geovetenskaper, No. 391, 2017 The whole document is available at www.diva-portal.org Populärvetenskaplig sammanfattning Kritisk studie av de mineralogiska samlingarna vid Uppsala universitet med hjälp av Ramanspektroskopi Yuliya Zhuk Ramanspektroskopitekniken applicerades för att identifiera och karakterisera antalet mineraler i den mineralogiska samlingen vid Institutionen för geovetenskaper. Samlingen breddades med fem sällsynta karbonater som lånades från Naturhistoriska riksmuseets samling i Stockholm. Sammanlagt analyserades 66 prover. Egenskaperna av intresse inkluderade eventuell förekomst av och karaktären hos defekter och föroreningar, graden av kristallinitet, restspänningar, eventuella spår av naturlig värmebehandling (till exempel radionuklider) eller kemisk behandling (till exempel polermedel), och fluorescens. Ramanspektroskopi valdes som undersökningsmetod på grund av dess tydliga fördel över traditionella metoder – en icke-förstörande undersökning av rena material och minimal eller ingen förberedelse. Därutöver fungerar Ramanspektroskopi väldigt bra för undersökning av de efterfrågade egenskaperna, vad gäller dess känslighet och kapacitet vid sondering av miniatyrkorn i matriser med hög spatial upplösning. Ett portabelt system användes för att identifiera föroreningar och fingeravtryck av den omslutande bergarten i de flesta undersökta karbonatprov. Den sällsynta karbonaten burbankit visade på distinkta fluorescensband, som sannolikt kan tillskrivas dess komplicerade kemiska sammansättning. Ramansystemet användes i gemmologiskt syfte och kunde identifiera ädelstenarnas renhet. Diamant och två rubiner visade sig sakna föroreningar, men den röda korunden visade en bred topp, som kan indikera på spår av naturlig värmebehandling, som i sin tur kan ha orsakats av regional metamorfos eller till och med en strålningskälla. Därutöver studerades sambandet mellan signalstyrkan hos fluoriters band och mineralers kemiska sammansättning. Experimentet visade att blå fluorit fullständigt saknar toppen från T2g, medan de lila och grå fluoriterna hade välutvecklade och lättigenkännliga toppar vid denna position. Således upptäcktes att denna topps närvaro och intensitet är direkt beroende av fluroritens färg, det vill säga av elementen som är inkorporerade i kristallstrukturen, så som metaller, sällsynta jordartsmetaller eller till och med organiska substanser. Därutöver identifierades restdragspänning i den färglösa kvartsen. Spänningen uppskattades ligga i intervallet 0.23 – 1.0 GPa. Ramansystemet användes för att identifiera olika ändelement i granatfamiljen. Ramanspektroskopin hade hög analytisk förmåga och hjälpte till att estimera förhållandet mellan ändelementen i åtta granatprover. I ett fall kunde fluorescens bindas till förekomsten av sällsynta jordartsmetaller i almandinets struktur. Ett kalcitprov visade sig vara felaktigt placerat i samlingen. Detta arbete kommer nu utgöra en god grund för den mineralogiska samlingens handbok. Nyckelord: Ramanspektroskopi, gemologi, geologi, mineralogi, mineralogisk samling Examensarbete E1 i geovetenskap, 1GV025, 30 hp Handledare: Peter Lazor Institutionen för geovetenskaper, Uppsala Universitet, Villavägen 16, SE-752 36 Uppsala (www.geo.uu.se) ISSN 1650-6553, Examensarbete vid Institutionen för geovetenskaper, Nr 391, 2017 Hela publikationen finns tillgänglig på www.diva-portal.org Table of Contents 1 Introduction ....................................................................................................................... 1 2 Objectives ........................................................................................................................... 2 2.1 Scientific problems ...................................................................................................... 2 2.2 Testing hypotheses ...................................................................................................... 3 2.3 The broader value of the project .................................................................................. 4 3 Background ....................................................................................................................... 4 3.1 Physics of Raman spectroscopy .................................................................................. 4 3.2 Interaction between the incitation source and the geomaterial. ................................... 5 3.3 Common applications of Raman spectroscopy ........................................................... 7 4 Methodology ...................................................................................................................... 7 4.1 Materials ...................................................................................................................... 7 4.2 Portable Raman spectrometer ...................................................................................... 7 4.3 Experimental calibrations ............................................................................................ 8 4.3.1 Calibration procedure ........................................................................................... 9 4.4 PeakFit™ software .................................................................................................... 11 4.5 Crystal Sleuth search engine ...................................................................................... 12 5 Chapter I – Carbonates .................................................................................................
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