Special Issue "Advances in Mineral Analytical Techniques"

A special issue of Minerals (ISSN 2075-163X).

Deadline for manuscript submissions: closed (31 May 2016)

Special Issue Editors

Guest Editor
Dr. Cristiana L. Ciobanu

School of Chemical Engineering, University of Adelaide, Adelaide, SA 5005, Australia
Website | E-Mail
Interests: ore-forming processes; nanoscale characterisation of ore minerals; microanalysis
Guest Editor
Prof. Dr. Nigel J. Cook

School of Chemical Engineering, University of Adelaide, Adelaide, SA 5005, Australia
Website | E-Mail
Phone: +61405826057
Interests: ore minerals; trace element analysis; ore deposit geology

Special Issue Information

Dear Colleagues,

Compositional heterogeneity and crystal-structural modifications in minerals, if understood at different scales of observation, are paramount for interpretation of petrogenetic processes down to the site where fluid–rock interaction or mineral transformation takes place. The significant advances in microanalytical techniques made in recent years present incredible opportunities for mineral and rock characterization, in turn, providing key information to constrain geological events. This includes compositional and crystal structural information at ever-better spatial resolution, and lower-and-lower concentrations, as well as microscopic techniques, which permit observational data collected in situ at scales from that of nanometres to microns to be correlated with one another.

This Special Issue, "Advances in Mineral Analytical Techniques", will review the techniques themselves but also highlight the new opportunities for petrogenetic interpretation, especially in the field of mineral deposits and their genesis. Manuscripts already committed to the special issue include those covering focussed ion beam–scanning electron microscopy, transmission electron microscopy, trace element microanalysis and U-Pb geochronology via laser-ablation inductively-coupled plasma mass spectrometry (LA-ICP-MS), de-convoluting mineral and fluid inclusions from complex LA-ICP-MS signals in host quartz, and TESCAN Integrated Minerals Analyser (TIMA) methodology.

Manuscripts covering the background and methodology of these and other new, or rapidly-developing analytical approaches, their application to problem-solving, or illustrative case studies, are welcomed. We particularly welcome manuscripts that illustrate innovate, integrated use of different techniques in combination with one another.

Dr. Cristiana L. Ciobanu
Prof. Dr. Nigel J. Cook
Guest Editors

Manuscript Submission Information

Manuscripts should be submitted online at www.mdpi.com by registering and logging in to this website. Once you are registered, click here to go to the submission form. Manuscripts can be submitted until the deadline. All papers will be peer-reviewed. Accepted papers will be published continuously in the journal (as soon as accepted) and will be listed together on the special issue website. Research articles, review articles as well as short communications are invited. For planned papers, a title and short abstract (about 100 words) can be sent to the Editorial Office for announcement on this website.

Submitted manuscripts should not have been published previously, nor be under consideration for publication elsewhere (except conference proceedings papers). All manuscripts are thoroughly refereed through a single-blind peer-review process. A guide for authors and other relevant information for submission of manuscripts is available on the Instructions for Authors page. Minerals is an international peer-reviewed open access monthly journal published by MDPI.

Please visit the Instructions for Authors page before submitting a manuscript. The Article Processing Charge (APC) for publication in this open access journal is 1400 CHF (Swiss Francs). Submitted papers should be well formatted and use good English. Authors may use MDPI's English editing service prior to publication or during author revisions.

Keywords

  • advanced analytical techniques
  • laser-ablation inductively-coupled plasma mass spectrometry
  • trace element microanalysis
  • U-Pb geochronology
  • transmission electron microscopy
  • focussed ion beam–scanning electron microscopy
  • nanoscale mineral characterisation
  • ore mineralogy

Published Papers (7 papers)

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Research

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Open AccessArticle
Analysis of Au-Ag Mineralization in the Caribou Base-Metal VMS Deposit, New Brunswick; Examination of Micro-Scale Inter- and Intra-Sulphide Distribution and Its Relation to Geometallurgy
Minerals 2016, 6(4), 113; https://doi.org/10.3390/min6040113
Received: 3 March 2016 / Revised: 8 October 2016 / Accepted: 10 October 2016 / Published: 21 October 2016
Cited by 2 | PDF Full-text (11566 KB) | HTML Full-text | XML Full-text
Abstract
The Caribou Zn-Pb-Cu-Ag volcanogenic massive sulphide deposit located in northeast New Brunswick represents a significant base-metal resource in the Bathurst Mining Camp. Zinc, Pb and Cu are the primary resources that are being extracted from this deposit; however, Au and Ag are important [...] Read more.
The Caribou Zn-Pb-Cu-Ag volcanogenic massive sulphide deposit located in northeast New Brunswick represents a significant base-metal resource in the Bathurst Mining Camp. Zinc, Pb and Cu are the primary resources that are being extracted from this deposit; however, Au and Ag are important by-products that could help offset costs. This study used mineral liberation analysis supported further by in situ laser ablation inductively-coupled plasma-mass spectrometry methods to document variations in Au and Ag distribution between and within sulphide minerals. The variations in Ag and Au distribution provide critical inputs to the optimization of mineral processing design. The greatest influence on Au recovery at Caribou is the proportion of Au hosted in arsenopyrite and pyrite; consequently, considerable Au will report to the tailings. Silver recovery at Caribou is highly affected by the proportion of Ag hosted in galena and tetrahedrite-tennantite. Proximal to the vent complex, Ag values are primarily hosted in galena, whereas further from the vent complex, Ag values are likely primarily hosted in tetrahedrite-tennantite. Galena Ag values will report mostly to the Pb concentrate, while tetrahedrite-tennantite Ag values will report to the Cu concentrate. Full article
(This article belongs to the Special Issue Advances in Mineral Analytical Techniques)
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Open AccessArticle
Focused Ion Beam and Advanced Electron Microscopy for Minerals: Insights and Outlook from Bismuth Sulphosalts
Minerals 2016, 6(4), 112; https://doi.org/10.3390/min6040112
Received: 2 August 2016 / Revised: 27 September 2016 / Accepted: 11 October 2016 / Published: 20 October 2016
Cited by 9 | PDF Full-text (12097 KB) | HTML Full-text | XML Full-text | Supplementary Files
Abstract
This paper comprises a review of the rapidly expanding application of nanoscale mineral characterization methodology to the study of ore deposits. Utilising bismuth sulphosalt minerals from a reaction front in a skarn assemblage as an example, we illustrate how a complex problem in [...] Read more.
This paper comprises a review of the rapidly expanding application of nanoscale mineral characterization methodology to the study of ore deposits. Utilising bismuth sulphosalt minerals from a reaction front in a skarn assemblage as an example, we illustrate how a complex problem in ore petrology, can be approached at scales down to that of single atoms. We demonstrate the interpretive opportunities that can be realised by doing this for other minerals within their petrogenetic contexts. From an area defined as Au-rich within a sulphosalt-sulphide assemblage, and using samples prepared on a Focused Ion Beam–Scanning Electron Microscopy (SEM) platform, we identify mineral species and trace the evolution of their intergrowths down to the atomic scale. Our approach progresses from a petrographic and trace element study of a larger polished block, to high-resolution Transmission Electron Microscopy (TEM) and High Angle Annular Dark Field (HAADF) Scanning-TEM (STEM) studies. Lattice-scale heterogeneity imaged in HAADF STEM mode is expressed by changes in composition of unit cell slabs followed by nanoparticle formation and their growth into “veins”. We report a progressive transition from sulphosalt species which host lattice-bound Au (neyite, lillianite homologues; Pb-Bi-sulphosalts), to those that cannot accept Au (aikinite). This transition acts as a crystal structural barrier for Au. Fine particles of native gold track this progression over the scale of several hundred microns, leading to Au enrichment at the reaction front defined by an increase in the Cu gradient (several wt %), and abrupt changes in sulphosalt speciation from Pb-Bi-sulphosalts to aikinite. Atom-scale resolution imaging in HAADF STEM mode allows for the direct visualisation of the three component slabs in the neyite crystal structure, one of the largest and complex sulphosalts of boxwork-type. We show for the first time the presence of aikinite nanoparticles a few nanometres in size, occurring on distinct (111)PbS slabs in the neyite. This directly explains the non-stoichiometry of this phase, particularly with respect to Cu. Such non-stoichiometry is discussed elsewhere as defining distinct mineral species. The interplay between modular crystal structures and trace element behaviour, as discussed here for Au and Cu, has applications for other mineral systems. These include the incorporation and release of critical metals in sulphides, heavy elements (U, Pb, W) in iron oxides, the distribution of rare earth elements (REE), Y, and chalcophile elements (Mo, As) in calcic garnets, and the identification of nanometre-sized particles containing daughter products of radioactive decay in ores, concentrates, and tailings. Full article
(This article belongs to the Special Issue Advances in Mineral Analytical Techniques)
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Open AccessArticle
Mapping of Sulfur Isotopes and Trace Elements in Sulfides by LA-(MC)-ICP-MS: Potential Analytical Problems, Improvements and Implications
Minerals 2016, 6(4), 110; https://doi.org/10.3390/min6040110
Received: 7 July 2016 / Revised: 17 August 2016 / Accepted: 22 August 2016 / Published: 20 October 2016
Cited by 18 | PDF Full-text (8556 KB) | HTML Full-text | XML Full-text
Abstract
Constraints on accurate quantitative trace element and sulfur (S) isotope analysis of sulfide minerals, especially pyrite, by laser-ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) remain imperfectly understood at the present time. Mapping of S isotope distributions within a complex sample containing several minerals [...] Read more.
Constraints on accurate quantitative trace element and sulfur (S) isotope analysis of sulfide minerals, especially pyrite, by laser-ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) remain imperfectly understood at the present time. Mapping of S isotope distributions within a complex sample containing several minerals requires an evaluation of the matrix effects and accuracy. Here, we apply LA-Q(quadrupole)-ICP-MS and LA-MC(multiple collector)-ICP-MS methods to analyze trace elements and S isotopes in sulfides. Spot analysis of S isotopes was conducted to evaluate the influence of matrix effects. The matrix effects from siderite and magnetite are deemed to be negligible in mapping analysis at the precision of this study. Both Fe and S were used as internal standard elements to normalize trace element concentrations in pyrite. Fe proved to be the better choice because the normalized counts per second ratio of trace elements with Fe is much more stable than if using S. A case study of a sulfide sample from the Chengmenshan Cu deposit, Jiangxi Province, South China, demonstrates the potential of combined S isotope and trace element mapping by LA-(MC)-ICP-MS. The results suggest that this deposit underwent multi-stage ore formation. Elements, including Au and Ag, were hosted in early-stage pyrite but were re-concentrated into multi-component sulfide assemblages during a late-stage hydrothermal event, which also led to crosscutting veins containing pyrite largely devoid of trace elements, except Se. Combining in situ S isotope and trace element analysis on the same sample represents a powerful tool for understanding ore-forming processes. Full article
(This article belongs to the Special Issue Advances in Mineral Analytical Techniques)
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Open AccessArticle
Nano-Tomography of Porous Geological Materials Using Focused Ion Beam-Scanning Electron Microscopy
Minerals 2016, 6(4), 104; https://doi.org/10.3390/min6040104
Received: 18 July 2016 / Revised: 23 September 2016 / Accepted: 28 September 2016 / Published: 10 October 2016
Cited by 14 | PDF Full-text (16650 KB) | HTML Full-text | XML Full-text | Supplementary Files
Abstract
Tomographic analysis using focused ion beam-scanning electron microscopy (FIB-SEM) provides three-dimensional information about solid materials with a resolution of a few nanometres and thus bridges the gap between X-ray and transmission electron microscopic tomography techniques. This contribution serves as an introduction and overview [...] Read more.
Tomographic analysis using focused ion beam-scanning electron microscopy (FIB-SEM) provides three-dimensional information about solid materials with a resolution of a few nanometres and thus bridges the gap between X-ray and transmission electron microscopic tomography techniques. This contribution serves as an introduction and overview of FIB-SEM tomography applied to porous materials. Using two different porous Earth materials, a diatomite specimen, and an experimentally produced amorphous silica layer on olivine, we discuss the experimental setup of FIB-SEM tomography. We then focus on image processing procedures, including image alignment, correction, and segmentation to finally result in a three-dimensional, quantified pore network representation of the two example materials. To each image processing step we consider potential issues, such as imaging the back of pore walls, and the generation of image artefacts through the application of processing algorithms. We conclude that there is no single image processing recipe; processing steps need to be decided on a case-by-case study. Full article
(This article belongs to the Special Issue Advances in Mineral Analytical Techniques)
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Open AccessArticle
Pb-Isotopic Study of Galena by LA-Q-ICP-MS: Testing a New Methodology with Applications to Base-Metal Sulphide Deposits
Minerals 2016, 6(3), 96; https://doi.org/10.3390/min6030096
Received: 31 May 2016 / Revised: 26 August 2016 / Accepted: 2 September 2016 / Published: 15 September 2016
Cited by 4 | PDF Full-text (3932 KB) | HTML Full-text | XML Full-text | Supplementary Files
Abstract
In situ laser ablation quadrupole inductively coupled plasma mass spectrometry was used to measure Pb isotopes in galena. Data acquisition was optimized by adjusting spot size, energy density, and ablation time to obtain near steady-state low relative standard deviation (%RSD) signals. Standard-sample bracketing [...] Read more.
In situ laser ablation quadrupole inductively coupled plasma mass spectrometry was used to measure Pb isotopes in galena. Data acquisition was optimized by adjusting spot size, energy density, and ablation time to obtain near steady-state low relative standard deviation (%RSD) signals. Standard-sample bracketing using in-house Broken Hill galena as external reference standard was used and offline data reduction was carried out using VizualAge for Iolite3. Using this methodology, galena grain in polished thin sections from selected massive sulphide deposits of the Bathurst Mining Camp, Canada, were tested and compared to previously published data. Absolute values and errors on the weighted mean of ~20 individual analyses from each sample compared favourably with whole-rock Pb-Pb isotope data. This approach provides a mean to obtain rapid, accurate, and moderately (0.1% 2σ) precise Pb isotope measurements in galena and is particularly well suited for exploratory or reconnaissance studies. Further refinement of this approach may be useful in exploration for volcanogenic massive sulphides deposits and might be a useful vectoring tool when complemented with other conventional exploration techniques. Full article
(This article belongs to the Special Issue Advances in Mineral Analytical Techniques)
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Open AccessArticle
Matrix-Matched Iron-Oxide Laser Ablation ICP-MS U–Pb Geochronology Using Mixed Solution Standards
Minerals 2016, 6(3), 85; https://doi.org/10.3390/min6030085
Received: 18 May 2016 / Revised: 11 August 2016 / Accepted: 16 August 2016 / Published: 23 August 2016
Cited by 21 | PDF Full-text (8715 KB) | HTML Full-text | XML Full-text | Supplementary Files
Abstract
U–Pb dating of the common iron-oxide hematite (α-Fe2O3), using laser-ablation inductively-coupled-plasma mass-spectrometry (LA-ICP-MS), provides unparalleled insight into the timing and processes of mineral deposit formation. Until now, the full potential of this method has been negatively impacted by the [...] Read more.
U–Pb dating of the common iron-oxide hematite (α-Fe2O3), using laser-ablation inductively-coupled-plasma mass-spectrometry (LA-ICP-MS), provides unparalleled insight into the timing and processes of mineral deposit formation. Until now, the full potential of this method has been negatively impacted by the lack of suitable matrix-matched standards. To achieve matrix-matching, we report an approach in which a U–Pb solution and ablated material from 99.99% synthetic hematite are simultaneously mixed in a nebulizer chamber and introduced to the ICP-MS. The standard solution contains fixed U- and Pb-isotope ratios, calibrated independently, and aspiration of the isotopically homogeneous solution negates the need for a matrix-matched, isotopically homogenous natural iron-oxide standard. An additional advantage of using the solution is that the individual U–Pb concentrations and isotope ratios can be adjusted to approximate that in the unknown, making the method efficient for dating hematite containing low (~10 ppm) to high (>1 wt %) U concentrations. The above-mentioned advantage to this solution method results in reliable datasets, with arguably-better accuracy in measuring U–Pb ratios than using GJ-1 Zircon as the primary standard, which cannot be employed for such low U concentrations. Statistical overlaps between 207Pb/206Pb weighted average ages (using GJ-1 Zircon) and U–Pb upper intercept ages (using the U–Pb mixed solution method) of two samples from iron-oxide copper-gold (IOCG) deposits in South Australia demonstrate that, although fractionation associated with a non-matrix matched standard does occur when using GJ-1 Zircon as the primary standard, it does not impact the 207Pb/206Pb or upper intercept age. Thus, GJ-1 Zircon can be considered reliable for dating hematite using LA-ICP-MS. Downhole fractionation of 206Pb/238U is observed to occur in spot analyses of hematite. The use of rasters in future studies will hopefully minimize this problem, allowing for matrix-matched data. Using the mixed-solution method in this study, we have validated a published hematite Pb–Pb age for Olympic Dam, and provide a new age (1604 ± 11 Ma) for a second deposit in the same province. These ages are further evidence that the IOCG mineralizing event is tied to large igneous province (LIP) magmatism in the region at ~1.6 Ga. Full article
(This article belongs to the Special Issue Advances in Mineral Analytical Techniques)
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Review

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Open AccessReview
Trace Element Analysis of Minerals in Magmatic-Hydrothermal Ores by Laser Ablation Inductively-Coupled Plasma Mass Spectrometry: Approaches and Opportunities
Minerals 2016, 6(4), 111; https://doi.org/10.3390/min6040111
Received: 31 July 2016 / Revised: 15 August 2016 / Accepted: 16 August 2016 / Published: 20 October 2016
Cited by 27 | PDF Full-text (15671 KB) | HTML Full-text | XML Full-text
Abstract
Laser ablation inductively-coupled plasma mass spectrometry (LA-ICP-MS) has rapidly established itself as the method of choice for generation of multi-element datasets for specific minerals, with broad applications in Earth science. Variation in absolute concentrations of different trace elements within common, widely distributed phases, [...] Read more.
Laser ablation inductively-coupled plasma mass spectrometry (LA-ICP-MS) has rapidly established itself as the method of choice for generation of multi-element datasets for specific minerals, with broad applications in Earth science. Variation in absolute concentrations of different trace elements within common, widely distributed phases, such as pyrite, iron-oxides (magnetite and hematite), and key accessory minerals, such as apatite and titanite, can be particularly valuable for understanding processes of ore formation, and when trace element distributions vary systematically within a mineral system, for a vector approach in mineral exploration. LA-ICP-MS trace element data can assist in element deportment and geometallurgical studies, providing proof of which minerals host key elements of economic relevance, or elements that are deleterious to various metallurgical processes. This contribution reviews recent advances in LA-ICP-MS methodology, reference standards, the application of the method to new mineral matrices, outstanding analytical uncertainties that impact on the quality and usefulness of trace element data, and future applications of the technique. We illustrate how data interpretation is highly dependent on an adequate understanding of prevailing mineral textures, geological history, and in some cases, crystal structure. Full article
(This article belongs to the Special Issue Advances in Mineral Analytical Techniques)
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