Chemical and mineralogical characterization of micro-inclusions in diamonds

Secondary-ion mass spectrometry (SIMS), electron probe analysis (EPMA), analytical scanning electron microscopy (SEM) and infrared (IR) spectroscopy were used to determine the chemical composition and the mineralogy of sub-micrometer inclusions in cubic diamonds and in overgrowths (coats) on octahedral diamonds from Zaire, Botswana, and some unknown localities.

The inclusions are sub-micrometer in size. The typical diameter encountered during transmission electron microscope (TEM) examination was 0.1-0.5 µm. The micro-inclusions are sub-rounded and their shape is crystallographically controlled by the diamond. Normally they are not associated with cracks or dislocations and appear to be well isolated within the diamond matrix. The number density of inclusions is highly variable on any scale and may reach 10^(11) inclusions/cm^3 in the most densely populated zones. The total concentration of metal oxides in the diamonds varies between 20 and 1270 ppm (by weight).

SIMS analysis yields the average composition of about 100 inclusions contained in the sputtered volume. Comparison of analyses of different volumes of an individual diamond show roughly uniform composition (typically ±10% relative). The variation among the average compositions of different diamonds is somewhat greater (typically ±30%). Nevertheless, all diamonds exhibit similar characteristics, being rich in water, carbonate, SiO_2, and K_2O, and depleted in MgO. The composition of micro-inclusions in most diamonds vary within the following ranges: SiO_2, 30-53%; K_2O, 12-30%; CaO, 8-19%; FeO, 6-11%; Al_2O_3, 3-6%; MgO, 2-6%; TiO_2, 2-4%; Na_2O, 1-5%; P_2O_5, 1-4%; and Cl, 1-3%. In addition, BaO, 1-4%; SrO, 0.7-1.5%; La_2O_3, 0.1-0.3%; Ce_2O_3, 0.3-0.5%; smaller amounts of other rare-earth elements (REE), as well as Mn, Th, and U were also detected by instrumental neutron activation analysis (INAA). Mg/(Fe+Mg), 0.40-0.62 is low compared with other mantle derived phases; K/ AI ratios of 2-7 are very high, and the chondrite-normalized Ce/Eu ratios of 10-21 are also high, indicating extremely fractionated REE patterns.

SEM analyses indicate that individual inclusions within a single diamond are roughly of similar composition. The average composition of individual inclusions as measured with the SEM is similar to that measured by SIMS. Compositional variations revealed by the SEM are larger than those detected by SIMS and indicate a small variability in the composition of individual inclusions. No compositions of individual inclusions were determined that might correspond to mono-mineralic inclusions.

IR spectra of inclusion- bearing zones exhibit characteristic absorption due to: (1) pure diamonds, (2) nitrogen and hydrogen in the diamond matrix; and (3) mineral phases in the micro-inclusions. Nitrogen concentrations of 500-1100 ppm, typical of the micro-inclusion-bearing zones, are higher than the average nitrogen content of diamonds. Only type IaA centers were detected by IR. A yellow coloration may indicate small concentration of type IB centers.

The absorption due to the micro-inclusions in all diamonds produces similar spectra and indicates the presence of hydrated sheet silicates (most likely, Fe-rich clay minerals), carbonates (most likely calcite), and apatite. Small quantities of molecular CO_2 are also present in most diamonds. Water is probably associated with the silicates but the possibility of its presence as a fluid phase cannot be excluded. Characteristic lines of olivine, pyroxene and garnet were not detected and these phases cannot be significant components of the inclusions. Preliminary quantification of the IR data suggests that water and carbonate account for, on average, 20-40 wt% of the micro-inclusions.

The composition and mineralogy of the micro-inclusions are completely different from those of the more common, larger inclusions of the peridotitic or eclogitic assemblages. Their bulk composition resembles that of potassic magmas, such as kimberlites and lamproites, but is enriched in H_2O, CO_3, K_2O, and incompatible elements, and depleted in MgO.

It is suggested that the composition of the micro-inclusions represents a volatile-rich fluid or a melt trapped by the diamond during its growth. The high content of K, Na, P, and incompatible elements suggests that the trapped material found in the micro-inclusions may represent an effective metasomatizing agent. It may also be possible that fluids of similar composition are responsible for the extreme enrichment of incompatible elements documented in garnet and pyroxene inclusions in diamonds.

The origin of the fluid trapped in the micro-inclusions is still uncertain. It may have been formed by incipient melting of a highly metasomatized mantle rocks. More likely, it is the result of fractional crystallization of a potassic parental magma at depth. In either case, the micro-inclusions document the presence of highly potassic fluids or melts at depths corresponding to the diamond stability field in the upper mantle. The phases presently identified in the inclusions are believed to be the result of closed system reactions at lower pressures.

Chemical and mineralogical characterization of portuguese ceramic tiles in the historic center of São Luís do Maranhão (Brazil): an approximation of the mineralogy and firing temperature of the raw materials

Nesse trabalho, foram caracterizados, pela primeira vez, azulejos históricos portugueses do Centro Histórico de São Luís (CHSL) do Maranhão. A caracterização foi realizada através dos ensaios de microscopia ótica, difração de raios X (DRX) e análise química, visando ao uso dessa informação para a determinação das possíveis matérias-primas utilizadas na sua fabricação, bem como a provável temperatura de queima desses materiais. Os resultados mostraram que a microestrutura desses materiais é constituída por poros de tamanhos variados, apresentando incrustações de calcita e grãos de quartzo de tamanhos inferiores a 500 µm, distribuídos numa matriz de cor rosa-amarelo, onde foram identificadas, por DRX, as fases minerais calcita, gelhenita, wollastonita, quartzo e amorfo. A partir da informação obtida, é possível inferir que as matérias-primas originais estiveram constituídas, provavelmente, por mistura de argilas caoliníticas (Al₂O₃•2SiO,₂•2H₂O), ricas em carbonatos de cálcio e quartzo ou misturas de argilas caoliniticas, quartzo e calcita. Essas matérias-primas originais não atingiram a temperatura de cocção de 950ºC.

Metamorphism and Fluid Inclusion Studies of Charnockites and Associated Rocks from the Madurai Granulite Block , Southern India with Special Reference to Graphite Mineralization

The present research is aimed at studying the charnockites and associated rocks of the Madurai Granulite Block (MGB), especially in terms of their field settings, texture, mineralogy, and mineral chemistry analyzing their petrogenesis with the help of thermobarometrical studies and geochronological constraints. The mechanism of charnockitization by the influx of CO2 rich fluids and its relation to the graphite mineralization is actually a matter of discussion and study. The objectives of the present study are, to delineate petrological and structural relationship of charnockites and associated gneissic rocks, to study the field and petrogenetic aspects of graphite mineralization in the MGB, to establish and re-evaluate the P-T conditions of formation of the rocks with the aid of thermbarometric computations and to compare with the earlier studies, characterization of graphite with XRD, Raman spectroscopy and isotope studies together with a search in to its genesis and its relation to the high-grade metamorphism of the terrain, to evaluate the role of CO2 bearing fluids in the processes of charnockitization as well as in the genesis of graphite within the high-grade terrain and to delineate the metamorphic geochronology of selected rocks using ‘monazite dating’ technique with EPMA.

Physicochemical and mineralogical characteristics of soil/saprolite cores from a field research site, Tennessee

Site characterization is an essential initial step in determining the feasibility of remedial alternatives at hazardous waste sites. Physicochemical and mineralogical characterization of U-contaminated soils in deeply weathered saprolite at Area 2 of the DOE Field Research Center (FRC) site, Oak Ridge, TN, was accomplished to examine the feasibility of bioremediation. Concentrations of U in soil–saprolite (up to 291 mg kg–1 in oxalate-extractable Uo) were closely related to low pH (ca. 4–5), high effective cation exchange capacity without Ca (64.7–83.2 cmolc kg–1), amorphous Mn content (up to 9910 mg kg–1), and the decreased presence of relative clay mineral contents in the bulk samples (i.e., illite 2.5–12 wt. %, average 32 wt. %). The pH of the fill material ranged from 7.0 to 10.5, whereas the pH of the saprolite ranged from 4.5 to 8. Uranium concentration was highest (about 300 mg kg–1) at around 6 m below land surface near the saprolite–fill interface. The pH of ground water at Area 2 tended to be between 6 and 7 with U concentrations of about 0.9 to 1.7 mg L–1. These site specific characteristics of Area 2, which has lower U and nitrate contamination levels and more neutral ground water pH compared with FRC Areas 1 and 3 (ca. 5.5 and

Mineralogical and chemical characterization of some vermiculites from the mozambique belt of tanzania for agricultural use

Vermiculite minerals are locally available in the Mozambique Belt of Tanzania but are not currently commercially exploited. In part this may be due to lack of any precise characterization. This study was carried out as a first step to assess the suitability of these vermiculites for crop production by characterization of their mineralogical and chemical compositions. X-ray diffraction and scanning electron microscopy combined with an energydispersive X-ray system were used to establish the mineralogy. Electron microprobe analysis and inductively coupled plasma-mass spectrometry were used to study the chemical compositions and to identify any possible issues related to chemical composition that might affect their use if applied as soil conditioners. The samples were characterized as vermiculites and hydrobiotites with a wide variety of accessory minerals. Accessory minerals that might be of some concern are galena, fibrous amphiboles and sepiolite. The total levels of Ni in all vermiculites, and Cr in some, were also found to be high relative to common European standards and this might limit their potential as soil conditioners. It is clear that a field assessment of the bioavailability of various elements would be necessary before decisions relating to potential agricultural use could be made. © 2009 The Mineralogical Society.

Preparation and Characterization of Graphite-Epoxy Composite Modified with Zinc Hexacyanoferrate and Their Electrochemical Behaviour in Presence of Substituted Anilines

The growth of zinc hexacyanoferrate (ZnHCF) hybrid film on the surface of graphite-epoxy composite (GEC) electrodes was demonstrated by cyclic voltammetry. Surface morphology of the hybrid film was investigated by using scanning electron microscopy. The effect of the type of monovalent cations on the redox behaviour of hybrid film was also studied. This effect indicated that the radius of the hydrated cation mainly determines the ion permeability of the film.The electrochemical behavior of the substituted anilines (procaine and sulfamerazine) in 1 M KCl of the modified GEC electrode showed a decrease of the cathodic currents while increasing the concentration of these analytes. The developed sensor also showed excellent stability for long time usage, higher sensitivity and cost-effective fabrication.

Processing and mechanical characterization of titanium-graphite hybrid laminates

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Ceramic raw materials from the State of Maranhao, Brazil. Part 1: chemical and mineralogical characterization and technological properties of clays from Sao Luis, Rosario, Pinheiro and Mirinzal

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Ceramic raw materials from the State of Maranhão, Brazil. Part 1: chemical and mineralogical characterization and technological properties of clays from São Luis, Rosário, Pinheiro and Mirinzal

Nesse trabalho, foram caracterizadas algumas argilas coletadas nos municípios de São Luís, Rosário, Pinheiro e Mirinzal. A caracterização foi realizada através dos ensaios de difração de raios X, massa específica real, capacidade de troca de cátions (CTC), área superficial, distribuição granulométrica, análise química, análise térmica (TG-DTA) e limites de Atterberg. Ensaios tecnológicos de retração linear, antes e após a queima, absorção de água e tensão de ruptura a flexão, em três pontos, foram realizados em corpos de prova prensados uniaxialmente a 20 MPa e tratados termicamente em 850, 950, 1050, 1150 e 1250ºC. Os resultados obtidos permitiram identificar duas argilas de queima branca, constituídas de quartzo, caolim, feldspato e anatásio, com excelentes propriedades para uso em cerâmica branca. As restantes são queima vermelha e possuem composição mineralógica de quartzo, caolim, feldspato, montmorilonita, hematita e goetita. Estas últimas apresentaram valores moderados de plasticidade e são adequadas para aplicações em cerâmica vermelha.

DIRECT ELECTROCHEMISTRY AND SURFACE CHARACTERIZATION OF GLUCOSE-OXIDASE ADSORBED ON ANODIZED CARBON ELECTRODES

The glassy carbon electrode (gce) and highly oriented pyrolytic graphite (hopg) were electrochemically anodized at a potential of +2.0 V (vs. Ag/AgCl) to create active sites and to improve the adsorption of glucose oxidase (GOD) and flavin adenine dinucle

Petrologic and geochemical characterization of São Jorge island volcanism, Azores

The island of São Jorge (38º 45’ 24’’ N - 28º 20’ 44’’W and 38º 33’ 00’’ N - 27º 44’ 32’’ W) is one of the nine islands of the Azores Archipelago that is rooted in the Azores Plateau, a wide and complex region which encompasses the triple junction between the American, Eurasia and Nubia plates. São Jorge Island has grown by fissural volcanic activity along fractures with the regional WNW-ESE trend, unveiling the importance of the regional tectonics during volcanic activity. The combination of the volcanostratigraphy (Forjaz & Fernandes, 1975; and Madeira, 1998) with geochronological data evidences that the island developed during two main volcanic phases. The first subaerial phase that occurred between 1.32 and 1.21 Ma ago (Hildenbrand et al. 2008) is recorded on the lava sequence forming the cliff at Fajã de São João, while the second phase started at 757 ka ago, is still active, and edified the rest of the island. This second phase edified the east side of the island that corresponds to Topo Volcanic Complex, in the period between 757 and 543 ka ago, while the west side named Rosais Volcanic Complex, started at 368 ka ago (Hildenbrand et al. 2008) and was still active at 117 ka ago. After the onset of Rosais, volcanic activity migrates to the center of São Jorge edifying Manadas Volcanic Complex. The volcanism on São Jorge is dominantly alkaline, with a narrow lithological composition ranging between the basanites/tefrites through the basaltic trachyandesites, in spite of this the two volcanic phases show distinct mineralogical, petrographic and geochemical characteristics that should be related with different petrogenetic conditions and growth rates of the island. Abstract viii During the first volcanic phase, growth rates are faster (≈3.4 m/ka), the lavas are slightly less alkaline and plagioclase-richer, pointing to the existence of a relative shallow and dynamic magma chamber where fractional crystallization associated with gravitational segregation and accumulation processes, produced the lavas of Fajã de São João sequence. The average growth rates during the second volcanic phase are lower (≈1.9 m/ka) and the lavas are mainly alkaline sodic, with a mineralogy composed by olivine, pyroxene, plagioclase and oxide phenocrysts, in a crystalline groundmass. The lavas are characterized by enrichment in incompatible trace element and light REE, but show differences for close-spaced lavas that unveil, in some cases, slight different degrees of fertilization of the mantle source along the island. These differences might also result from higher degrees of partial melting, as observed in the early stages of Topo and Rosais volcanic complexes, of a mantle source with residual garnet and amphibole, and/or from changing melting conditions of the mantle source as pressure. The subtle geochemical differences of the lavas contrast with the isotopic signatures, obtained from Sr-Nd-Pb-Hf isotopes, that São Jorge Island volcanism exhibit along its volcanic complexes. The lavas from Topo Volcanic Complex and from the submarine flank, i.e. the lavas located east of Ribeira Seca Fault, sample a mantle source with similar isotopic signature that, in terms of lead, overlaps Terceira Island. The lavas from Rosais and Manadas volcanic complexes, the western lavas, sample a mantle source that becomes progressively more distinct towards the west end of the island and that, in terms of lead isotopes, trends towards the isotopic composition of Faial Island. The two isotopic signatures of São Jorge, observed from the combination of lead isotopes with the other three systems, seem to result from the mixing of three distinct end-members. These end-members are (1) the common component related with the Azores Plateau and the MAR, (2) the eastern component with a FOZO signature and possibly related with the Azores plume located beneath Terceira, and (3) the western component, similar to Faial, where the lithosphere could have been entrained by an ancient magmatic liquid, isolated for a period longer than 2Ga. The two trends observed in the island reinforce the idea of small-scale mantle heterogeneities beneath the Azores region, as it has been proposed to explain the isotopic diversity observed in the Archipelago.

Mineralogical characterization of clays used in the structural ceramic industry in west of S. Paulo State, Brazil

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Computer techniques towards the automatic characterization of graphite particles in metallographic images of industrial materials

The automatic characterization of particles in metallographic images has been paramount, mainly because of the importance of quantifying such microstructures in order to assess the mechanical properties of materials common used in industry. This automated characterization may avoid problems related with fatigue and possible measurement errors. In this paper, computer techniques are used and assessed towards the accomplishment of this crucial industrial goal in an efficient and robust manner. Hence, the use of the most actively pursued machine learning classification techniques. In particularity, Support Vector Machine, Bayesian and Optimum-Path Forest based classifiers, and also the Otsu's method, which is commonly used in computer imaging to binarize automatically simply images and used here to demonstrated the need for more complex methods, are evaluated in the characterization of graphite particles in metallographic images. The statistical based analysis performed confirmed that these computer techniques are efficient solutions to accomplish the aimed characterization. Additionally, the Optimum-Path Forest based classifier demonstrated an overall superior performance, both in terms of accuracy and speed. © 2012 Elsevier Ltd. All rights reserved.

Geochemical and radioactivity characterization of rocks from the Rio Preto (Go) Project

The Rio Preto Project, developed by the extinct Brazilian nuclear state company, Nuclebrás, during the late 70s and early 80s, consisted of basic geological mapping and radiometric characterization by aerogeophysical gamma-ray spectrometry, without channel discrimination, of a surface area of 650 km2 located to the west of the Chapada dos Veadeiros National Park on the northeastern of Goiás State, Brazil, including the confluence area of Claro and Preto Rivers. Additionally, the natural radioelements U, Th and 40K were determined by gamma-ray spectrometry in 300 rock samples from cores of the Rio Preto Project area. The tests were conducted at LABIDRO-Isotopes and Hydrochemistry Laboratory of the Departament of Petrology and Metallogeny (DPM) of the Institute of Geosciences and Exact Sciences, UNESP, in Rio Claro, SP, Brazil. This paper reports the results of petrographic characterization and chemical analyses of major oxides (SiO2, TiO2, Al2O3, Fe2O3, MgO, MnO, K2O, Na2O, CaO and P2O5) for all samples used to determine the natural radioelements present in the region. The organic matter content results obtained by colorimetry are also reported for selected cores of different lithotypes in order to investigate the possible relationship between graphite and the radioelements uranium and thorium. Finally, uranium content and 234U/238U activity ratio data for selected samples of schists and gneisses of the Lower Member of the Ticunzal Formation suggest the influence of weathering processes in the area. © 2012 Sociedade Brasileira de Geofísica.

Geochemical and mineralogical analyses of clay-rich intervals in ODP Sites 166-1006 and 166-1007

The western flank of the Great Bahama Bank, drilled during ODP Leg 166 at seven sites, represents a prograding carbonate sequence from late Oligocene to Holocene [Eberli et al., Proc. ODP Init. Reports 166 (1997)]. The signatures of the detrital input and of diagenetic alteration are evident in clay enriched intervals from the most distal Sites 1006 and 1007 in the Straits of Florida. Mineralogical and chemical investigations (XRD, TEM, SEM, ICP-MS) run on bulk rocks and on the clay fractions enable the origin and evolution of silicate parageneses to be characterized. Plio-Pleistocene silt and clay interbeds contain detrital clay assemblages comprising chlorite, illite, interstratified illite smectite, smectite, kaolinite and palygorskite. The greater smectite input within late Pliocene units than in Pleistocene oozes may relate either varying source areas or change in paleoclimatic conditions and weathering intensity. The clay intervals from Miocene-upper Oligocene wackestone sections are fairly different, with prevalent smectite in the fine fraction, whose high crystallinity and Mg contents that point towards an authigenic origin. The lower Miocene section, below 1104 mbsf, at depths where compaction features are well developed, is particularly characterized by abundant authigenic Na-K-clinoptilolite filling foraminifer tests. The authigenic smectite and clinoptilolite paragenesis is recorded by the chemical trends, both of the sediment and the interstitial fluid. This diagenetic evolution implies Si- and Mg rich fluids circulating in deeper and older sequences. For lack of any local volcaniclastic input, the genesis of zeolite and the terms of water rock interaction are discussed. The location of the diagenetic front correlates with that of the seismic sequence boundary P2 dated as 23.2 Ma. This correspondence may allow the chronostratigraphic significance of some specific seismic reflections to be reassessed.