Microcharacterisation Facility

Qualitative and quantitative analysis of materials using state-of-the-art instrumentation including JEOL Hyperprobe, iTrax Core Scanner, XRF and XRD.

PANalytical Empyrean Powder X-ray Diffractometer
PANalytical Empyrean Powder X-ray Diffractometer

Equipment

  • Rigaku XtaLAB Synergy-S single crystal X-ray diffractometer with dual Cu/Ag Kα source (XRD)
  • PANalytical Empyrean powder X-ray diffractometer with Cu Kα source (XRD)
  • JEOL Field Emission Electron Probe Microanalyser System 8530F (Hyperprobe)
  • Cox Analytical iTrax Core Scanner
  • PANalytical Axios 1KW X-ray Fluorescence Spectrometer (XRF)
  • Inductively Coupled Plasma Mass Spectrometry (ICP-MS)
    • With Laser Ablation (LA-ICP-MS)

Rigaku XtaLAB Synergy-S Single Crystal X-ray Diffractometer

Rigaku XtaLAB Synergy-S Single Crystal X-ray Diffractometer

X-ray Diffraction is a non-destructive analytical technique that provides detailed information about the internal lattice of crystalline substances.

Our XtaLAB Synergy-S single crystal diffractometer is equipped with:

  • Cu and Ag Kα X-ray sources, providing data collection to an accuracy of up to 0.80 or 0.35 Å, respectively.
  • Pilatus 200K hybrid photon detector
  • Oxford Cryostream, which allows measurement temperatures from 90 K to room temperature under a mixed dry air/nitrogen flow.

Our service includes:

  • Data collection and structure determination.
  • Single-crystal X-ray diffraction measurements for precise determination of a unit cell, including cell dimensions and positions of atoms within the lattice. Bond-lengths and angles are directly related to the atomic positions.

Sample requirements:

  • Suitable for small molecule crystals or extended structures, with small protein crystals being possible.
  • Optimum sample is an untwinned crystal with a size of 50-150 microns, with smaller sizes possible.
  • Oxygen/moisture sensitive samples are possible.
  • Power diffraction is possible on special request if you have insufficient sample to use the powder diffractometer.

PANalytical Empyrean Powder X-ray Diffractometer

Our PANalytical Empyrean diffractometer is equipped with:

  • Cu Kα X-ray source
  • PIXcel 1D detector
  • Add-on modules allowing high temperature measurements up to 1000°C as well as X-ray reflectivity measurements for thin films.

Please note: This is a self-use instrument that requires safety training before access can be given. Please contact the X-ray technician at the bottom of this page to request training.

Instrument capabilities:

  • Powder X-ray diffraction for phase identification of materials including minerals and Rietveld refinement for crystal structure determination.
  • Crystallinity measurement.
  • Clay minerals or 3 stage XRD scan - i) air dried, preferred orientation ii) glycolated and iii) heat treated samples.
  • XRD for non-ambient, high-temperature phase shift measurements - the collection of data up to 1000°C.
  • X-ray reflectivity for thin films.

Sample requirements:

  • Approximately 1g of sample is normally required, however, samples as small as 50 mg can be possible using a Si-based zero background holder.
  • Ambient sample conditions, therefore oxygen/moisture sensitive samples would need special sample preparation by the user.
     

JEOL Field Emission Electron Probe Microanalyser System 8530F (Hyperprobe)

This microanalysis system focuses a narrow collimated beam of electrons onto a solid sample to quantify its major and trace element chemistry. It can characterise chemical contrasts across zones of only tens of nanometres – the highest resolution technique available for this purpose.

This capability is especially suited to micro-geochemical studies within natural minerals, as well as manufactured surfaces, coatings, bone and ceramics.

The “Field-Emission Electron Microprobe Analyser FE-EPMA” is an advance on EPMA technology that uses high-vacuum, precision beam focusing and more reliable energy sources to produce a collimated beam of electrons at only nanometres in diameter. This opens the door to a level of non-destructive spot and spatial analysis of solid materials at scales not previously possible.

In addition, new large-area detection systems are used to detect elements formerly unseen at edges of the X-Ray detection spectrum as well as to provide better determination of trace-elemental compositions. Other enhancements to the technology enable high-speed quantitative 2D chemical mapping of samples. This has turned FE-EMPA into a one-stop shop for the finest-possible spot analysis.

Cox Analytical iTrax Core Scanner

The itrax Core Scanner is a unique laboratory analytical instrument that provides very high-resolution, non-destructive X-ray density and elemental analysis of a variety of solid samples.  

Its main use is to evaluate high-resolution environmental and chemical aspects of sediment and rock cores within hours to days.

Speleothem (cave limestone), coral and wood samples can also be analysed in high resolution. 

PANalytical Axios 1KW X-ray Flourescence Spectrometer (XRF)

The PANalytical Axios is a 1kW wavelength dispersive X-ray fluorescence (XRF) spectrometer equipped with an argon flow counter and solid state scintillation counter.

This system uses PANalytical's Axios high resolution, wavelength dispersive, X-ray fluorescence (WDXRF) spectrometer for elemental analysis.

Our service includes: 

  • Preparation and elemental analysis of fused glass discs.
  • Preparation and elemental analysis of pressed powders, liquid samples and thin films (in the future).
  • Element search and quantification.
  • Automated sample disc fusion and programmable fusion settings to optimise the preparation of the sample discs.
  • XRF instrument operates in continuous measurement mode reducing sample turnaround times.

Limitations of XRF:

  • Quantification of certain low mass and trace elements are not possible due to the limits of the instrument.
  • Samples must be dried powders and require a minimum of 4g mass before ignition.
  • Samples must be  safe to handle with bare hands.
  • Certain materials with high concentrations of certain elements may be unsuitable samples for this instrument, please see a technician to assess suitability.
  • Data collection generally requires between 1.5+ hours per
    sample.

Inductively Coupled Plasma Mass Spectrometry (ICP-MS)

The University of Auckland operates an Agilent 7700 ICP-MS that can be coupled to our deep-ultraviolet (193 nm) New Wave Excimer laser ablation system or LC-MS (for compound-specific elemental analysis).

The ICP-MS is equipped with collision cell technology (He) for reduction and elimination of spectral interferences on difficult to analyse elements.

Inductively Coupled Plasma Mass Spectrometry (ICP-MS) is a technique suitable for elemental analysis of a wide range of inorganic and organic materials, including geological, biological, medical, agricultural and environmental samples.

Its main advantage is that it can analyse a large number of elements in a single analytical run. Samples can be analysed in either a liquid (solution ICP-MS) or solid form (laser ablation ICP-MS) with typical detection limits in the (sub)parts per trillion (solutions) or parts per billion range (solids).

In addition to elemental analysis, the ICP-MS can be used for the determination of isotopic ratios of selected elements to a precision of ±0.2% for isotopic tracing and uranium-lead dating of minerals from rocks such as zircon.

Elements that can be analysed by ICP-MS include: Li, Be, B, Na, Mg, Al, Si, P, Ca, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, Ge, As, Se, Rb, Sr, Y, Zr, Nb, Mo, Ru, Rh, Pd, Ag, Cd, In, Sn, Sb, Te, Cs, Ba, rare earth elements (actinides), Hf, Ta, W, Os, Re, Ir, Pt, Au, Hg, Tl, Pb, Bi, Th and U.

Our services include:

  • Sample preparation including mounting of solids for laser ablation ICP-MS and digestion of samples for solution ICP-MS analysis
  • Elemental analysis of a wide range of sample types either by laser ablation or solution ICP-MS

We have previously developed and applied methods that include:

  • rocks and glasses in volcanic systems
  • geochronology of minerals
  • micro-fossil records of paleoclimatology and oceanography
  • meteorites and the origins of the Solar System
  • kai moana (paua, cockles, mussels) and aquaculture
  • fish otoliths and life histories
  • plant and wood material
  • animal/human teeth and migration
  • provenancing of archaeological artefacts
  • anti-cancer drugs

How we can help you

Bookings to use our equipment can be made through iLab or the relevant technician. We are also able to provide training to use the equipment requested. 

Our people

Technical contacts

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