X-Ray Analysis Facilities

Analyse the elemental composition and mineral structure of geological and environmental samples using X-Ray fluorescence (XRF) and X-Ray diffraction (XRD).

The lab houses two separate, purpose-built instruments for analysing geological and environmental samples: 

  • an X-ray Diffractometer (XRD), which determines the crystallographic structure and mineralogy of a sample; and
  • an X-ray Fluorescence spectrometer (XRF), which determines its elemental chemical composition.

These facilities support in-house research, as well as academic and commercial services.

Details of each instrument, along with information on access, specifications, sample requirements, and costs, are given below.

 

Contact and location

Contact

Gus Calderxray.geos@ed.ac.uk +44 (0) 131 650 8534XRF/XRD Laboratory manager

Location

Address: XRF/XRD Laboratory, Grant Institute, School of GeoSciences, University of Edinburgh, James Hutton Road, EDINBURGH EH9 3FE

Please note that parking on campus is strictly by permit only, and parking spaces are subject to availability. Commercial and external users should contact our staff about parking arrangements.

X-Ray Diffraction Facility

X-ray diffraction (XRD) is a technique that provides detailed information about the crystallographic structure, chemical composition, and physical properties of materials. A primary use of XRD analysis is the identification of materials based on their diffraction pattern. 

Our facility includes a state-of-the-art Panalytical Empyrean XRD equipped with iCore and dCore optics for powder diffraction, GIXRD and Microdiffraction. 

Technical information for users of the facility including the Panalytical Empyrean and associated analysis software and support equipment. 

Multipurpose Panalytical Empyrean X-Ray Diffractometer:

  • X-Ray Diffraction equipment for both quantitative and qualitative identification of crystalline materials.
  • The instrument is fitted with a Panalytical iCore as the primary optic, a dCore for the incident beam and a 1Der detector for maximum sensitivity and resolution.
  • The Empyrean is also capable of Grazing Incidence XRD (GIXRD), XRR (X-Ray Reflectrometry), and Microdiffraction. 
  • Software used for interpretation includes Highscore Plus and DiffracPlus with the ICDD and COD databases.
  • Quantification can be carried out with a variety of software including Highscore Plus, TOPAS and Siroquant. 
  • Analysis of clay speciation may be carried out by using dedicated clay separation, glycolation and heating facilities. 

Support equipment

The facility also has the necessary support equipment including:

  • Rock cutting and grinding equipment
  • Micronising mill
  • Spray dryer
The Malvern Panalytical website has some useful information on their XRD instruments.Malvern Panalytical
The Bruker website has information on TOPAS software for Rietveld AnalysisBruker
The Mineralogist Crystal Structure Database is an interface that includes every structure published in the American Mineralogist, The Canadian Mineralogist, European Journal of Mineralogy and Physics and Chemistry of Minerals, as well as selected datasets from other journals. Mineralogist Crystal Structure Database

Prices may vary depending on work involved - 24hr and 48hr turnaround available. 

For the wider University and all external users:

Please contact the facility to discuss availability, as well as analytical requirements and charging information.  

For staff and students in the School of GeoSciences:

Pricing and access to the facility must be completed through a job request form, which can be found on the X-Ray Diffraction and X-Ray Fluorescence Facility intranet pages.


X-Ray Fluorescence Facility

X-ray fluorescence can be used for qualitative or quantitative analysis of a range of materials. Our facility is equipped with a Rigaku Primus IV wavelength-dispersive sequential X-ray spectrometer and a Rigaku NEX-DE energy dispersive XRF.

We also have dedicated sample preparation laboratories, supported by sawing, crushing, and grinding facilities.

Technical information for users of the facility including instrument specification, and requirements necessary for sample preparation.

Quantitative whole-rock analysis may be obtained for most elements heavier than oxygen, with abundances in the range 1 ppm to 100 wt.%, depending on instrument sensitivity at the wavelength of the analytical line and availability of calibration standards.

Instrument Specification

  • Instrument: Panalytical PW2404 wavelength-dispersive sequential X-ray spectrometer.
  • Automated Sample changer: Panalytical PW2540 VRC 168-position X-Y sample changer.
  • X-ray Tube: 3kW Rh-anode, end-window tube.
  • Analysing Crystals: LiF 200, LiF 220, Ge 111-C, InSb 111-C, PE 002-C, PX1, PX6, TlAp 100 coated.
  • Detectors: Flow, Scintillation, Duplex, Xe-sealed.
  • Collimators: 700µm, 300µm, 150µm.
  • Collimator masks: 6mm, 27mm, 37mm.
  • Tube Filters: Brass 100µm, Brass 300µm, Pb 1000µm, Al 750µm.

Sample Requirements

Powders used for XRF analysis must be very finely ground using either tungsten carbide or agate grinding apparatus. Normally at least 10-12g of powder should be available for major and trace element analysis. 

Major-element concentrations are measured on 40mm-diameter fused glass discs. 1.0000g of sample powder is mixed with a borate flux using a 10:1 (flux: sample) dilution and fused in Pt-5%Au crucibles at 1050°C. 

Please note the following important points: 

  • A 40mm-diameter glass disc cannot be made using less than 1.0000g of powder. 
  • Samples containing sulphides or more than 100ppm of As, Sb, Pb or Sn must not be fused in Pt crucibles. 
  • Samples containing free carbon or organic material must be pre-ignited at 400°C in porcelain crucibles prior to fusion. 
      

Trace-element concentrations are measured on pressed powder pellets. Approx.10-12g of powder is required to make a 40mm-diameter pellet. It is also possible to make 30mm-diameter pellets (using 8g of powder) and 13mm-diameter pellets (using 1g of powder) for some analytical applications. 


Availability

  • Access is subject to availability. 
  • School staff and students are normally given priority. Pricing and access the facility must be completed through an SRF request form. 
  • For the wider University, and for external users: work is taken on only by prior arrangement. 
  • Our preparation laboratories are bookable in advance.

Costs

  • All analytical work will involve costs. Sufficient funding should be in place before work starts. Prices may vary depending on work involved. 
  • Prospective users should contact the facility to discuss requirements and costs involved. 
  • Staff and students within the School of GeoSciences must complete a technical request form.

Training and assistance

  • Undergraduate students, postgraduate students, and research staff prepare their own samples for analysis after instruction. 
  • Students and research staff generally do not set up or calibrate the instrument but may be required to load and run samples, or to make standards for non-routine analysis. 
  • Our preparation laboratories are bookable in advance. The sawing, crushing, and grinding facilities are also bookable, but a 'Permit to Work' system is in operation for health and safety reasons. Access is only allowed to permit holders who have received the appropriate training.

Sample preparation

  • There are requirements for sample preparation before analysis at the facility. See 'Equipment specification and sample requirements' section above on this page.
  • A sample preparation service is offered to academic staff in the School of GeoSciences. Samples (as powders) must be accompanied by a request detailing the type of material and analysis required.

For the wider University and all external users:

Please contact the facility to discuss availability, as well as analytical requirements and charging information.  

For staff and students in the School of GeoSciences:

Pricing and access to the facility must be completed through a job request form, which can be found on the X-Ray Fluorescence Facility intranet pages.

 


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