CCFS 2012 - Technology

CCFS links three internationally recognised concentrations of analytical geochemistry infrastructure: GEMOC’s Geochemical Analysis Unit (Macquarie University) and the associated Computing Cluster, the Centre for Microscopy, Characterisation and Analysis (UWA/Curtin) and the John de Laeter Centre of Mass Spectrometry. All are nodes for the NCRIS AuScope and Characterisation Capabilities, and have complementary instrumentation and laboratories. In addition, Curtin and UWA share a leading facility for paleomagnetic studies.

Facilities:

CCFS/GEMOC INFRASTRUCTURE, LABORATORIES AND INSTRUMENTATION

CMCA TECHNOLOGY DEVELOPMENT AND INSTRUMENTATION

JOHN DE LAETER CENTRE

WESTERN AUSTRALIA PALAEOMAGNETIC AND ROCK-MAGNETIC FACILITY

CCFS/GEMOC INFRASTRUCTURE, LABORATORIES AND INSTRUMENTATION

CCFS/GEMOC INFRASTRUCTURE, LABORATORIES AND INSTRUMENTATION

The new femtosecond laser system in action.

The analytical instrumentation and support facilities of the Macquarie University Geochemical Analysis Unit (GAU) represent a state-of-the-art geochemical facility.

The GAU contains:

• a Cameca SX-100 electron microprobe

• a Zeiss EVO MA15 Scanning electron microscope

• four Agilent ICPMS (industry collaboration; two 7500cs; two 7700cx)

• a Nu Plasma multi-collector ICPMS

• a Nu Plasma high resolution multi-collector ICPMS

• a Thermo Finnigan Triton TIMS

• a custom-built UV laser microprobe, usable on the Agilent ICPMS

• three New Wave laser microprobes (one 266 nm, two 213 nm, each fitted with large format sample cells) for the MC-ICPMS and ICPMS laboratories (industry collaboration)

• a Photon Machines Excite Excimer laser ablation system

• a Photon Machines Analyte198 Femto-second laser ablation system

• a PANalytical Axios 1kW XRF with rocker-furnace sample preparation equipment

• a LECO RC412 H₂O-CO₂ analyser

• an Ortec Alpha Particle counter

• a New Wave MicroMill micro-sampling apparatus

• a ThermoFisher iN10 FTIR microscope

• selFrag electrostatic rock disaggregation facility

• clean labs and sampling facilities provide infrastructure for ICPMS, XRF and isotopic analyses of small and/or low-level samples

• experimental petrology laboratories include four
piston-cylinder presses (pressures to 4 GPa), hydrothermal apparatus, controlled atmosphere furnaces, Griggs apparatus and a multi-anvil apparatus for pressures
to 27 GPa

The Gemoc Facility For Integrated Microanalysis (FIM) And Micro-Gis Development

Within CCFS, GEMOC is continuing to develop a unique, world-class geochemical facility, based on in-situ imaging and microanalysis of trace elements and isotopic ratios in minerals, rocks and fluids. The Facility for Integrated Microanalysis now consists of four different types of analytical instrument, linked by a single sample positioning and referencing system to combine spot analysis with images of spatial variations in composition (“micro-GIS”). All instruments in the FIM have been operating since mid-1999. Major instruments were replaced or upgraded in 2002-2004 through the $5.125 million DEST Infrastructure grant awarded to Macquarie University with the Universities of Newcastle, Sydney, Western Sydney and Wollongong as partners. In late 2009 GEMOC was awarded an ARC LIEF grant to integrate the two existing multi-collector inductively-coupled-plasma mass spectrometers (MC-ICPMS) with 3 new instruments: a femtosecond laser-ablation microprobe (fs-LAM); a high-sensitivity magnetic-sector ICPMS; a quadrupole ICPMS. The quadrupole ICPMS was purchased and installed in 2010; a Photon Machines femtosecond laser system was installed in
June 2012; and a Nu Attom ICPMS to be installed in January 2013.

PROGRESS IN 2012

1. Facility for Integrated Microanalysis

a. Electron Microscope; Electron Microprobe: The Zeiss EVO MA15 SEM carried the electron imaging workload, providing high-resolution BSE and CL images for TerraneChron® (http://www.gemoc.mq.edu.au/TerraneChron.html) and all other research projects, including diamonds and diamondites, and PGM in chromitites. In 2012 a new Oxford Instruments AZtec Synergy combined Energy Dispersive System and Electron Back-Scatter Diffraction detector were installed on the Zeiss SEM. This combined capability for elemental and crystal orientation mapping has enabled new research directions in the study of deformation processes in mantle and crustal rocks. The SX100 serviced the demands for quantitative mineral analyses and X-ray composition maps for all projects including analysis of chromites; analysis of base metal sulfides and platinum group minerals; minor and trace element analysis of metals. A MQSIS 2013 Faculty of Science Infrastructure Fund grant was awarded for the upgrade of the integrated Energy Dispersive Spectrometer system on the SX100.

Dr Masahiko Honda (ANU/RSES), and ANU honours student Hanling Yeow with Dan Howell using the Photon Excite Excimer laser ablation system

b. Laser-ablation ICPMS microprobe (LAM): In 2012 the LAM laboratory was used by thirteen Macquarie PhD thesis projects, twelve international visitors, four Honours students, and several in-house funded research projects and industry collaborations. Projects included the analysis of trace elements in the minerals of mantle-derived rocks, in sulfide minerals and in a range of unusual matrices. U-Pb analysis of zircons was again a major activity with geochronology projects (including TerraneChron applications: http://www.gemoc.mq.edu.au/TerraneChron.html) from Australia (NSW, WA, SA), New Zealand, Algeria, Colombia, Indonesia, Mongolia, Papua New Guinea, Russia, and west Africa. Method development was also undertaken for the U-Pb dating of apatite. The LAM laboratory also routinely provides data for projects related to mineral exploration (diamonds, base metals, Au) as a value-added service to the industry.

c. MC-ICPMS: The continued increase of TerraneChron® activities (see http://www.gemoc.mq.edu.au/TerraneChron.html) involving the measurement of Hf isotopes, coupled with the growing demand for in-situ analysis of other radiogenic isotope systems (e.g. Re-Os analysis in sulfide and PGM; Nd-Sm and Rb–Sr in perovskite) and stable isotope analysis, created severe competition for instrument time on the LAM MC-ICPMS.

Major applications during 2012 using in situ techniques continued to centre on the high-precision analysis of Hf in zircons to trace lithosphere evolution and magma-mixing histories in granitic rocks, and Re-Os dating of single grains of Fe-Ni sulfides and alloys in mantle-derived rocks. In-situ Hf isotopes were measured in zircons from Australia (NSW, WA, SA), New Zealand, Algeria, Colombia, Indonesia, Mongolia, Papua New Guinea, Russia, and west Africa. Re-Os studies were undertaken on xenoliths from eastern China, Siberia, Mongolia, Spain, USA, South Africa and northern Africa, and sulfide and platinum group minerals in chromitites from Cuba, Spain, Turkey.

Photon engineer Ben Staal with the new Photon Machines Analyte198 Femto-second laser ablation system.

d. Laboratory development: The clean-room facility established in 2004 continued to be used primarily for isotope separations for analysis on the Triton TIMS and Nu Plasma MC-ICPMS. Routine procedures have been established for Rb-Sr, Nd-Sm, Lu-Hf and Pb isotopes, as well as U-series methods (U, Th and Ra). Further developments of methods were undertaken for whole-rock Re-Os isotopes of basaltic rocks. A project was initiated to adapt convnetional techniques for Rb-Sr and Nd-Sm isotope separation to the nano-scale to process small sample sizes.

e. Software: GLITTER (GEMOC Laser ICPMS Total Trace Element Reduction) software is our on-line interactive program for quantitative trace element and isotopic analysis and features dynamically linked graphics and analysis tables. This package provides the first real-time interactive data reduction for
LAM-ICPMS analysis, allowing inspection and evaluation of each result before the next analysis spot is chosen. Its capabilities include the on-line reduction of U-Pb data. The use of GLITTER has greatly increased both the flexibility of analysis and the productivity of the laboratory. Sales are handled by Access MQ and GEMOC provides customer service and technical backup. During 2012 a further 16 full licences of GLITTER were sold bringing the total number in use to 202 worldwide, in forensics and materials science, as well as earth science applications.
Dr Will Powell continued in his role in GLITTER technical support and software development through 2012. The current GLITTER release is version 4.4.3 and is currently available without charge to existing customers and accompanies all new orders (http://www.glitter-gemoc.com/).

2. X-Ray Fluorescence Analysis

In November 2012 a PANalytical Axios 1 kW X-ray Fluorescence Spectrometer was installed. This instrument is a wavelength spectrometer system and replaced the Spectro XLAB2000 energy-dispersive X-ray spectrometer, which was installed in November 2000. The new instrument will be used to measure whole-rock major element compositions on fused glass discs and trace-element concentrations on pressed-powder pellets. An upgrade of the sample preparation infrastructure is planned for early 2013.

Navigating the halls with the new PANalytical Axios 1 kW X-ray Fluorescence Spectrometer, installed in November 2012.

3. Whole-rock solution analysis

An Agilent 7500cs ICPMS produces trace-element analyses of dissolved rock samples for the projects of GEMOC researchers and students and external users, supplementing the data from the XRF.

The ICPMS dedicated to solution analysis continued to be used for the further development of ‘non-traditional’ stable isotopes with the refinement of separation techniques and analytical protocols for Mg isotopes in garnet and for the separation and analysis of Li isotopes in granitic rocks.

4. Diamond preparation and analysis

The GEMOC laser-cutting system (donated by Argyle diamonds in 2008), was used during 2012 to cut thin plates of single diamond crystals as part of the on-going research into diamond genesis. The plates are used for detailed spatial analysis of trace elements, isotopic ratios and the abundance and aggregation state of nitrogen. The nitrogen measurements are made using the ThermoFisher iN10FTIR microscope, which allows the spatial mapping of whole diamond plates at high resolution with very short acquisition times.

5. selFrag – a new approach to sample preparation

GEMOC’s selFrag instrument was installed in May 2010 and was the first unit in Australia. This instrument uses high-powered electrical pulses to disaggregate rocks and other materials along the grain boundaries. It removes the need to crush rocks for mineral separation, and provides a higher proportion of unbroken grains of trace minerals such as zircon. Since its installation selFrag, usage has continued to grow and in 2012 it was used for a range of applications including zircon separation, the analysis of grain size and shape in complex rocks, and the liberation of trace minerals from a range of mantle-derived and crustal rocks. Method development also continued in 2012 on the CNT Hydroseparator for the separation of small volumes of ultrafine material (e.g. alloys in chromitites). See p. 122-123.

6. Computer cluster

A 64-core ARC-funded computer cluster (Enki) came online in 2010, with the capability to run massively parallel high-resolution geodynamics simulations in 3D at a global scale. Further funding in 2011 was used to expand the cluster into a 160-core machine. Updated rack storage and power supplies have been completed, and the upgraded machine is currently in full operation.

The cluster is running some of the most cutting-edge simulation software packages, including CitcomS – enabling 3D spherical mantle simulations, and Underworld – a lithosphere and mantle deformation computational framework designed for massively parallel simulations. It has supported four Honours student projects, as well as two ongoing PhD projects, and underpins at least four successful ARC Discovery projects.

Internal capacity in this kind of computing is necessary as externally available clusters (e.g. At AC3/Intersect, or at NCI) are specifically for “production” runs only – not for research and development of experimental codes. However, many of these codes have absolute minimum resolution requirements which can only be met by a large cluster. For example, CitcomS requires at least 12 nodes to run, or 96 for a fully resolved simulation, which is often necessary for the testing of new modules. This cannot be done on a desktop machine, and since testing is not allowed on the public machines, the in-house cluster is essential to the development of the next generation of simulation tools.

CMCA TECHNOLOGY DEVELOPMENT AND INSTRUMENTATION

The University of Western Australia’s Centre for Microscopy, Characterisation and Analysis (CMCA) is a $40M core facility providing analytical solutions across a diverse array of scientific research. The world-class facilities and associated technical and academic expertise are the focus of micro-analytical and characterisation activities within Western Australia, while strong links and collaborations have earned the CMCA an excellent national and international reputation. The CMCA incorporates the Western Australian Centre for Microscopy, and is a node of the NCRIS Characterisation capabilities, the National Imaging Facility (NIF) and the Australian Microscopy and Microanalysis Research Facility (AMMRF). It is also associated with the NCRIS-funded Australian National Fabrication Facility (ANFF) and AuScope, which have made a substantial contribution to facilities run by CMCA.

CMCA capabilities:

• CAMECA IMS 1280 and CAMECA NanoSIMS 50 ion microprobes

• JEOL JXA 8530F electron microprobe, with Cathodoluminescence imaging (CL)

• Transmission Electron Microscopes (JEOL 3000F, 2100 and 2000FX), with EDS and energy-filtered EELS analysis capabilities

• Scanning electron microscopes (Zeiss 1555, 2 JEOL 6400, Philips XL30)

• X-ray powder diffraction (Panalytical Empyrean)

• NMR spectroscopy (2 Bruker Avance and 2 Varian spectrometers)

• Optical and confocal microscopy

• Micro-CT (to be installed 2012)

• Bioimaging, flow cytometry, cell sorting, and laser micro-dissection

• X-ray crystallography

• GC and HPLC mass spectrometry

• Biological sample cryo-preparation and ultramicrotomy

THE AMMRF FLAGSHIP ION PROBE FACILITY

The CMCA at UWA is home to two state-of-the-art ion microprobes that are integral to the goals of the CCFS. The CAMECA IMS 1280 and NanoSIMS 50 are flagship instruments of the Australian Microscopy and Microanalysis Research Facility (AMMRF). The AMMRF Flagship Ion Probe Facility offers state-of-the-art secondary ion mass spectrometry (SIMS) capabilities to the Australian and international research communities, allowing in-situ, high-precision isotopic and elemental analyses, secondary ion imaging, and depth profiling on a wide range of samples.

The IMS 1280 large-geometry ion probe, installed in 2009, was co-funded by the University, the State Government of Western Australia, and the Federal Government’s Department of Innovation, Industry, Science and Research (DIISR) under the ‘Characterisation’ (AMMRF) and ‘Structure and Evolution of the Australian Continent’ (AuScope) capabilities of the National Collaborative Research Infrastructure Strategy (NCRIS). The CAMECA IMS 1280 is optimised for in-situ stable isotope analyses (e.g. S, O, C) at a spatial resolution of 10 to 30µm and a precision of ~0.1-0.4 per mil.

The NanoSIMS 50, installed in 2003, was funded through the Federal Government’s NCRIS-precursor, the Major National Research Facility scheme (NANO-MNRF). The CAMECA NanoSIMS 50 is designed to provide elemental and isotopic imaging on a wide range of materials with a spatial resolution down to 50 nm – albeit, with considerably less sensitivity than the IMS1280.

Both instruments are relatively rare – there are only about 30 of each in the world – and until recently UWA was the only institution in the world to have both side by side.

The instruments are managed by the Western Australia Ion Probe Management Committee, which also manages the two SHRIMP II ion probes located at Curtin University. Access to the Ion Probe Facility is subsidised for publicly-funded researchers within Australia via a merit-based competitive application scheme, where projects are assessed by a scientific committee of international experts.

The Ion Probe Facility is a key characterisation component within the ARC Centre of Excellence for Core to Crust Fluid Systems. To ensure the highest levels of quality and throughput, the CCFS has provided funding for a Research Associate position within the Ion Probe Facility, to facilitate direct scientific and technical interaction for all CCFS users and projects.

PROGRESS IN 2012

In 2012, the Ion Probe Facility at CMCA-UWA has embraced a wealth of projects in the context of CCFS (see CMCA Research highlight p. 75). These have included a wide range of topics, from the characterisation of mantle metasomatism (O isotopes in zircon and garnet; E. Rubanova, E. Belousova, Q. Xiong, J. Huang), the origin of diamonds (O isotopes in garnet and C isotopes in diamond; E. Rubanova), magmatic processes and crustal growth (O isotopes in zircon; S. Li, E. Belousova, M. Sun), the origin of ore deposits (S isotopes in sulfides; M Fiorentini). Altogether, these projects account for ~30% of the availble analysis time on the CAMECA IMS 1280. In addition, the NanoSIMS has also been applied to the measurement of element diffusion across mineral interfaces, trace element transportation along grain boundaries, and S isotopes (D Wacey, M Fiorentini).

Standards development:

High-precision isotope measurement with SIMS requires calibration against known standards to correct for instrumental mass fractionation between analysis sessions. This varies significantly between materials, such that each new material analysed by SIMS necessitates the development of new standards. Standards are in constant development at CMCA and currently include diamond (C isotopes), lawsonite, pyroxene, garnet and olivine (O isotopes), tourmaline and serpentine (B isotopes), pentlandite, pyrrhotite and chalcopyrite (S and Fe isotopes).

Personnel:

Dr Laure Martin was appointed to the position of Research Associate within the CMCA to facilitate the use of the ion probes by the CCFS. With a considerable background in geological SIMS analysis, Dr Martin has already made valuable contributions to the development of standards and analytical protocols, while providing assistance in sample preparation, data acquisition, and data processing. In addition to this service role, Dr Martin also carries out her own research on the evolution of fluids in subduction zones and mineral/fluid interaction in metamorphic rocks, both key subjects within CCFS.

Laure Martin and Ekaterina Rubanova with the Cameca IMS1280 ion probe.

The Ion Probe Facility also employed Dr Rong Liu as a Senior Research Officer.

CMCA Research highlights:

In 2012, a wealth of innovative CCFS research projects passed through the doors of the Ion Probe Facility at CMCA, illustrating the strong collaborative environment within the CCFS.
Examples include:

4D lithospheric evolution and controls on mineral system distribution: The Western Superior-Yilgarn comparison (Yongjun Lu, Foundation project)

The O isotope analysis of zircon samples using the CAMECA IMS 1280, show that terrane boundaries appear to control the location of mineralization within the Wabigoon subprovince. The zircon Hf-O isotopes also indicate that the supracrustal recycling and juvenile crustal growth in the Wabigoon subprovince mainly developed at ca. 2.7 Ga. By contrast, the proceeding 3.1-2.9 Ga felsic magmatism mainly represents crustal reworking of deep crust without supracrustal input.

Fluid processes in the deep mantle: geochemical studies of diamonds and related minerals (Ekaterina Rubanova)

Carbon isotope analyses in diamond and oxygen isotope analyses in coexisting garnets have been undertaken to provide a better understanding of diamond formation processes in the mantle. The analytical results confirm that diamonds have complex mantle-residence histories and were involved in mantle metasomatic processes. These data combined with other geochemical analyses are contributing to the study of mantle fluid systems.

Textural and spatial variability in multiple sulfur isotope biosignatures (David Wacey, John Cliff, Mark Barley)

The CAMECA IMS1280 has been used to analyse some of Earth’s oldest sedimentary sulfides from the 3.5 Ga Dresser Formation of Western Australia. Here we have measured all 4 stable sulfur isotopes, and while the δ³⁴S and Δ³³S values appear to be similar to previous bulk analyses, the Δ³⁶S values have a much greater spread than previously reported. This could be significant for understanding the sources of sulfur on the early Earth but more work is now needed to test the robustness and further develop SIMS Δ³⁶S data.

Multiple sulfur isotope measurements (James Farquhar, John Cliff)

One highlight of 2012 included the two-month visit of Professor James Farquhar (University of Marlyand) as a UWA Gledden Senior Fellow, working with Dr John Cliff on the development of multiple S isotope measurements. A part of this work will be published in the Proceedings of the National Academy of Sciences (in press). Not only does the work provide fresh evidence of sulfate reduction at 2.6 Ga, but also provides evidence of two distinct sulfur pools in the Archaen oceans.

Isotopic standards development (John Cliff, Laure Martin)

Due to the strong ‘matrix effect’ inherent in SIMS analysis, each new material requires a chemically (and isotopically) homogeneous standard of known composition with which to calibrate the instrument. In addition, new standards extend our capabilities into hitherto unexplored isotope systems. Recent standards development has included diamond (C isotopes), lawsonite, pyroxene, garnet and olivine (O isotopes), tourmaline and serpentine (B isotopes), pentlandite, pyrrhotite and chalcopyrite (Fe, Cu and S isotopes).

NanoSIMS development (Matt Kilburn, Rong Liu)

The NanoSIMS 50 was also involved in isotope development work. In February, Francois Hillion, the R&D manager from CAMECA visited the lab to work on improving the precision of isotope ratio measurements. David Wacey and Professor Martin Brasier (University of Oxford) performed δ³⁴S measurements on ediacaran pyrite microfossils, and Dr Chen Lei (Chinese University of Geoscience – Wuhan) visited to analyse Au in sulfide minerals. High-resolution imaging was employed by Marco Fiorentini and Zoja Vuckmanovic to detect element segregation along twin-boundaries in sulfide minerals.

JOHN DE LAETER CENTRE

The John de Laeter Centre houses a suite of mass spectrometry instruments and is a collaborative research venture involving Curtin University, the University of Western Australia, CSIRO and the Geological Survey of WA. It hosts over $25M in infrastructure in key facilities supporting research in: geosciences (geochronology, thermochronology and isotope studies); environmental science and global change; isotope metrology; forensic sciences; economic geology (minerals and petroleum); marine sciences; nuclear sciences. The components are organised into nine major facilities.

The Advanced Ultra-Clean Environment (ACE) Facility: This consists of a ~400m² class 1000 containment space that houses four class 10 ultra-clean laboratories, a class 10 reagent preparation laboratory and a −18 °C class 10 cold clean laboratory, located at Curtin University. The extremely low ultimate particle counts are achieved with successive ‘spaces within spaces’ and HEPA (99.999% high efficiency particle arresting) filtration at each stage.

Inductively-Coupled Plasma Mass Spectrometry (ICPMS) Facility: This facility is located at UWA and consists of:

• TJA (VG/Fisons) PlasmaQuad 3 Quadrupole ICP-MS. The system has a high sensitivity interface to facilitate ultra-low detection limits.

• TJA (VG/Fisons) Laserlab high resolution 266 nm (Frequency quadrupled Nd-YAG) laser. The laser system is adapted with a high-resolution interface to facilitate the ablation of craters down to 10 μ in diameter.

• GBC Optimas 8000 Time of Flight ICP-MS

• Leco Renaissance Time of Flight ICP-MS

• A wide range of chromatographic and thermal dissociation interfacing is also available.

Argon Isotope Facility: This is located at Curtin and is equipped with a MAP 215-50 mass spectrometer with a low-blank automated extraction system coupled with a NewWave Nd-YAG dual IR (1064 nm) and UV (216 nm) laser, an electron multiplier detector and Niers source. Laser analysis allows for high spatial resolution up to 10 μm beam size for UV laser and 300 μm for IR laser. Larger sample sizes (>8-10 mg) are accommodated by an automated Pond-Engineering low-blank furnace. The extraction line has a Nitrogen cryocooler trap and three GP10 getters that allow gas purification. An Argus VI Mass Spectrometer and a Photon Machines Laser have been ordered for the JdL facility.

A joint ANU-John de Laeter Centre for Mass Spectrometry (JdL) Argon Facility has been established following a successful ARC bid. A total of ~$988,200 will be expended with the ARC contribution being $420,000. A management committee comprising two Facility Directors (Dr Marnie Forster, RSES, and Dr Fred Jourdan, JdL), Director JdL (Professor Brent McInnes), Mr Michael Avent (School Manager, RSES) and Professor Gordon Lister (RSES and named Project Manager and Chief Investigator on the ARC grant) has been set up and approved by all Collaborating and Partner Organisations.

The new instrument allows the JDLC Argon isotope facility to carry out specialised work on rare extra-terrestrial sample materials, such as micrometer-size grains recovered from the Itokawa asteroid (see below) by the Japanese spacecraft Hayabusa. Dr Jourdan was awarded the grains because of the international standing of his laboratory in the study of meteorites and asteroid impacts, as well as the new Argus instrument established in the John de Later Centre for Isotope Research.

A new Thermo Argus VI multi-collector noble gas mass spectrometer was installed in November 2012 with funding from a 2012 ARC LIEF grant. This new instrument is a low volume (~700 cc) instrument providing excellent sensitivity and is particularly suited to the isotopic analysis of small samples of the noble gases, and in particular, Argon. The muti-collector design gives it the ability to measure all five Ar isotopes simultaneously leading to reduced analysis time and greater productivity.

Curtin University has been selected by the Japanese Space Agency to undertake Ar-Ar dating of two rare and precious grains that it recovered from the asteroid Itokawa using the Hayabusa spacecraft. The Japanese mission was the first to bring back samples from an asteroid, and the argon analysis at Curtin will determine its formation age and contribute new knowledge about the history of the solar system.

Organic Geochemistry Facility: This facility is located within Applied Chemistry at Curtin and the instruments used for biomarker, petroleum and water studies include:

• GCMS (Gas Chromatograph Mass Spectrometer)

• GC-HRMS-MS (Gas Chromatograph-High Resolution Mass Spectrometer)

• Py-GC-MS (Pyrolysis-Gas Chromatograph-Mass Spectrometer)

• LCTOFMS (Liquid Chromatograph-Time of Flight-Mass Spectrometer)

• LC-MS-MS (Liquid Chromatography-Mass Spectrometry-Mass Spectrometer)

• HPSEC-DAD (High Performance Size Exclusion Chromatograph-Diode-Array Detection)

• GCIRMS (Gas Chromatograph-Isotope Ratio-Mass Spectrometer)

• TD-GC-IRMS (Thermal Desorption-Gas Chromatograph-Isotope Ratio-Mass Spectrometer)

• EA-IRMS (Elemental Analysis-Isotope Ratio-Mass Spectrometer)

Sensitive High Resolution Ion Micro Probe (SHRIMP):
The facility at Curtin has two automated SHRIMP II ion microprobes capable of 24-hour operation, together with a preparation laboratory. The equipment allows in-situ isotopic analysis of chemically complex materials with a spatial resolution of 5-20 microns. The main application of the SHRIMP instruments at Curtin is for U-Th-Pb geochronology of mineral samples. Zircon and other U-bearing minerals, including monazite, xenotime, titanite, allanite, rutile, apatite, badelleyite, cassiterite, perovskite and uraninite are the main minerals studied, where multiple growth zones commonly require high spatial resolution analyses.

Stable Isotope Ratio Mass Spectrometry (SIRMS) Facility: The West Australian Biogeochemistry Centre (WABC) at UWA is associated with the WA John de Laeter Centre of Mass Spectrometry and provides a range of analytical and interpretive services to researchers both within UWA and in the broader scientific community. The WABC currently operates three isotopic ratio mass spectrometers (IRMS) plus a considerable range of further analytical instrumentation (GC, HPLC, CE autoanalyser) routinely used in biogeochemical studies. A fourth IRMS (especially for small-sample δ¹³C and δ¹⁸O and carbonate analysis) is now being commissioned. Our IRMS are coupled with a variety of sample preparation modules to facilitate analysis of a broad range of sample matrices. Consequently, a wide range of applications of stable isotopes is supported by this facility.

Thermal Ionisation Mass Spectrometry (TIMS) Facility:
The TIMS facility at Curtin incorporates a Thermo Finnegan Triton™ and a VG 354 multicollector mass spectrometer. The Triton is equipped with a 21-sample turret and 9 faraday cups, enabling a precision of 0.001% on isotopic ratios. As well as geological applications within the broad field of isotope geochronology (Re/Os, U/ Pb, Pb/Pb, Sm/Nd, Rb/Sr) the TIMS instruments can be applied to a variety of subject areas involving isotope fingerprinting, such as mantle geodynamics, forensics and the environmental impact of human activities. The TIMS instruments are also widely used in chemical metrology for the calibration of isotopic standards, and the calculation of isotopic abundances and atomic weights.

AuScope GeoHistory and (U-Th)/He Facility: The laboratory at Curtin hosts the prototype of the Alphachron™ automated helium microanalysis instrument now marketed by Australian Scientific Instruments in Canberra. (U-Th)/He thermochronology involves the measurement of ⁴He generated by the radioactive decay of U and Th in minerals. Helium is an inert gas that is quantitatively retained by minerals at low temperature, but is gradually lost from the mineral lattice by diffusion at elevated temperatures. Some minerals are more retentive to helium than others (e.g. zircon = 200 °C vs apatite = 75 °C), a unique characteristic that, when integrated with other techniques such as U-Th-Pb and Ar-Ar dating, can be used to produce complete time-temperature histories through a temperature interval from 900 °C to 20 °C. The JDLC (U-Th)/He Facility provides thermal-history analysis of metallogenic and petroleum systems by integrating several age-dating capabilities along with 4D thermal modelling. The Facility is also involved in fundamental collaborative research in the fields of orogenic tectonics, volcanology and quantitative geomorphology. The facility has grown in 2012-13 to integrate a new Alphachron™ machine coupled to a RESOlution Excimer laser + Agilent 7700 mass spectrometer. This “RESOchron” instrument enables the development of in-situ U-Pb and (U-Th)/He dating on single crystals of U-bearing minerals and immensely increases our application potential. In addition, laser ablation trace element analysis and U-Pb geochronology is now routinely undertaken in this facility, supporting industry, government and University projects.

Installation of the ELA-ICP-MS instruments in the AuScope AGOS GeoHistory Facility at Curtin University. Left to right: Fred Fryer (Agilent), Brad McDonald, Noreen Evans, Brent McInnes, Mike Hamel (Resonetics).

K-Ar Geochronology Facility: The K-Ar facility utilises the following instrumentation and techniques:

• VG3600 noble gas mass spectrometer

• Heine double vacuum resistance furnace

• Clay mineral separation laboratory utilising cryogenic disaggregation of rock samples

• XRD, SEM, TEM, particle size analysis for clay characterisation

• Vacuum encapsulation station for Ar-Ar dating of ultrafine samples

• Clays – illite: Dating the timing of diagenetic and deformation events

• Fault gouge dating (illite) – earthquake and hazard assessment

selFRAG: The purchase of a new selFrag installation, similar to the one at the Macquarie node, is being negotiated with Curtin’s administration. A lab is being prepared, and a technician is being sought. The instrument will be available to CCFS staff.

ARC LIEF success: An AZtec Electron Backscatter Diffraction Facility for State-of-the-Art Quantitative Microstructural Analysis

The microstructures recorded in rocks and minerals record essential information relating to growth, deformation and mass transfer processes in Earth’s crust and mantle, meteorites and moon. Quantification of these relationships is critical in interpreting the small-scale geochemical variations in minerals that underpin our understanding of large-scale tectonic and impact processes and the formation of ore deposits. In 2012 CCFS and JDLC researchers, led by Steve Reddy, were involved in a successful ARC LIEF application to develop a new state-of-the-art quantitative microstructural characterisation facility at Curtin University. This equipment will complement existing high-spatial resolution microanalytical equipment within Curtin’s Electron Microscopy Facility, to provide a cutting-edge platform for pure and applied research in the Geosciences for the next decade.

WESTERN AUSTRALIA PALAEOMAGNETIC AND ROCK-MAGNETIC FACILITY

The Western Australia Palaeomagnetic and Rock-magnetic Facility was established at the University of Western Australia by CCFS CI Z.X. Li in 1990, funded by a UWA start-up grant to the late Professor Chris Powell. It was subsequently upgraded through an ARC Large Instrument Grant in 1993 to purchase a then state-of-the-art 2G Enterprises AC-SQUID cryogenic magnetometer and ancillary demagnetisation and rock magnetic instruments. It was upgraded again in 2006 into a regional facility, jointly operated by Curtin University, UWA and the Geological Survey of WA through an ARC LIEF grant with a 4k DC SQUID system plus a Variable Field Translation Balance (VFTB). A MFK-1FB kappabridge was installed in 2011.

The facility is one of the three similar laboratories in Australia, with major instruments including:

2G cryogenic magnetometer upgraded (LE0668377) to a 4K DC SQUID system
MMTD80 (one) and MMTD18 (two) thermodemagnetisers
Variable Field Translation Balance (VFTB)
MFK-1FB kappabridge
Bartington susceptibility meter MS2 with MS2W furnace

A wide range of research topics have been investigated using the facility, including reconstructing the configuration and drifting history of continents all over the world from the Precambrian to the present, analysing regional and local structures and deformation histories, dating sedimentary rocks and thermal/chemical (e.g. mineralisation) events, orienting rock cores from drill-holes, tracing ancient latitude changes, palaeoclimates, and recent environmental pollution.

Program 1: Regional and Global Tectonic Studies

Palaeomagnetism and rock magnetism are employed to study tectonic problems ranging from global to microscopic scales. The WA research group plays a leading role in a worldwide effort to establish the configuration and evolution of supercontinents Pangaea, Gondwanaland, Rodinia, and pre-Rodinia supercontinents.

Program 2: Ore genesis studies and geophysical exploration

We carried out a major research program on the timing and genesis of the giant iron ore deposits in the Pilbara region, and obtained a systematic set of petrophysical parameters for rock units in the region that enables more reliable interpretations of geophysical survey results (gravity and magnetic).

Program 3: Magnetic signatures in sediments as markers of environmental change

Sediments in suitable environments can incorporate a large number of environmental proxies. A major strength of environmental-magnetism analyses, such as magnetic susceptibility and saturated isothermal magnetism, is that they provide a rapid and non-destructive method of obtaining information on changes in palaeoclimate and environment of sedimentation. In addition, rock magnetism can be used for monitoring and tracing industrial pollution.

Program 4: Magnetostratigraphy

We are conducting major research programs in the Canning Basin and in East Timor, both linked to petroleum resources.