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MINERALOGY

The Application of Recent Developments in EDS


Hardware and Software to Process Mineralogy
Application Note

Introduction
Improvements in Energy Dispersive X-ray Spectroscopy (EDS) hardware (detector and pulse processing
electronics) and software over the last decade have delivered many advances in terms of data quality,
acquisition speed and ease of use. Here, we look at the specific advantages that these developments
have brought to the field of process mineralogy.

INCAMineral
Oxford Instruments’ automated mineralogy software,
INCAMineral, operates on a standard scanning electron
microscope (SEM) equipped with Oxford Instruments’
hardware. As such, other analysis tasks may be performed
on the sample without removing it from the chamber. The
software is integrated with the AZtec® and INCA® analysis
suite allowing it to be retrofitted to existing systems.
Fig. 1. X-MaxN 150 mm2 Silicon Drift Detector.

X-MaxN Silicon Drift Detectors


INCAMineral uses Oxford Instruments’ large area X-MaxN
Silicon Drift Detectors (SDD) (Fig. 1). This range of detectors
requires no liquid nitrogen for cooling. By using a detector
with a large detection area, it is possible to collect a greater
proportion of the X-rays which are generated by the
interaction of the electron beam with the sample. This is
due to the larger area creating a larger capture angle for Traditional 10 mm2 SDD: small capture angle = few counts
X-Max 150 mm2 SDD: larger angle = 15x more counts.
the incoming X-rays (Fig. 2). More X-rays can therefore be
collected per unit time. As such, it takes less time to collect Fig. 2. Schematic showing the advantage of using large area
detectors: NB. The detector is much closer to the sample in practice.
a given number of X-rays in order to make a statistically
valid characterisation of the particle under the beam. It also
means that beam currents can be reduced thereby increasing
the spatial resolution of measurements but still making
determinations of composition possible in a reasonable time
period.

Up to 4 X-MaxN detectors may be used simultaneously to


give a total possible detection area of 600 mm2. This enables
exceptionally high count rates and is particularly suited to the
rapid creation of detailed maps of geological samples (Figs. 3 Fig. 3. Four X-MaxN 150 mm2 detectors installed on a single SEM
& 4). to give a total acquisition area of 600 mm2.

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MINERALOGY
The Application of Recent Developments in EDS
Hardware and Software to Process Mineralogy
Application Note

INCAMineral and X-MaxN


The combination of INCAMineral with an X-MaxN detector allows data of an exceptionally high quality to be recorded. This
is down to the way that X-rays are measured and counted by the system. All counts are recorded into a spectrum which
undergoes a complete pulse pile up correction (removing pile up peaks and re-allocating the counts to the correct peak),
background correction and deconvolution of any overlapping peaks. This correction enables accurate quant measurements to
be performed at the highest count rates (Fig. 5). The quantification of the spectrum is then performed after these corrections
have been completed. By performing a full quantification of each particle instead of attempting to match each particle to
a reference spectrum, unexpected phases and phases which do not perfectly match a reference spectrum can be dealt with
very effectively. Classifications can be set based upon any combination of chemical and/or morphological measures enabling
very subtle variations between phases to be clearly delineated or enabling grouping of phases together with equal ease.
Classification schemes may be created prior to a run and used to classify in real time or afterwards so that they may be built
based upon acquired data.

The accelerating voltage may be chosen by the user. As a full quantification including the corrections described above and auto-
identification (if selected) of all elements is performed for each particle, the microscope conditions can be varied to optimise the
run.

Various automated analysis modes may be employed to solve different50 µm


problems. Liberation mode analyses particulated
samples – typically multiple size fractions – in order to determine how well liberated all of the identified minerals are and which
other minerals they are associated with. Individual grains within particles are differentiated from each other based upon their
grey-level threshold as viewed in a back-scattered electron (BSE) image. Analysis areas are then automatically determined by the
software such that each grain is sampled. EDS data may be collected from grains belonging to all grey level thresholds or only
from selected thresholds (e.g. bright phases – high-value, dense metals). It is also possible to set up the system to only acquire
data from particles which contain grains belonging to a specific threshold (e.g. to calculate association for rare phases such as
gold). Modal analysis may also be undertaken. In this mode, solid samples (e.g. a polished rock section) are analysed. The
same detection logic as liberation samples, based upon BSE imaging, is used.

1mm     
Fig. 4. Montaged large area autophasemap of a geological sample Fig. 5. Quant Data collected from orthoclase at 10 kcps and 250 kcps
obtained with multiple SDDs. Sample courtesy of Juliane Hennig, Data collected at both high and low count rates gives the same
Royal Holloway, University of London. correct quant results. Pile-up is automatically corrected, so there is no
degradation in data quality at high count rates.

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GSR
MINERALOGY
The Application of Recent Developments in EDS
Hardware and Software to Process Mineralogy

Mineralogical Data Processing


Application Note

Once acquisition is complete, data is processed with GrainAlyser to determine the minerals processing parameters of the
sample. Size fractions may be combined and weighted and industry standard plots may be quickly generated depending on
the type of analysis undertaken (see Fig. 6 to Fig. 9). A number of parameters are calculated for all datasets, these are: The
bulk elemental makeup of the sample, the mean composition of all phases, the deportment of each detected element, and full
morphological data for all grains and particles (each field of view for a modal sample is considered as an individual particle).
A series of plots are also immediately available including phase abundance, size distribution and association. For particulated
samples run in liberation mode, liberation plots may be output. MS Excel reports may also be output for each analysis type with
all of the calculations already made or alternatively as raw data thereby allowing the user to process the data in their own way.

Examples of GrainAlyser Graphical Output – Sphalerite Ore Case Study


Here, a sphalerite ore has been analysed to determine its liberation parameters. An accelerating voltage of 20 kV was used with
a high beam current. The X-MaxN150 mm2 detector was operated at a livetime of 0.1 s per grain enabling approximately 6000
grains per hour to be analysed. All spectra were processed and corrected as described above. A number of examples of the
graphical output are shown here.

Fig. 7. Individual grain phase image.

Fig. 6. Phase view of sphalerite ore sample.

Fig. 8.
Liberation plot for various forms of sphalerite.

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Fig. 9. Phase abundance within ore.

Conclusions
We have shown that the combination of up to four X-MaxN SDDs with the AZtec and INCA
nanoanalysis suite enables powerful analysis of geological materials and high throughput. Comprehensive
quantitative processing algorithms ensure the accuracy of quant data and are utilised throughout the
software. INCAMineral takes advantage of X-MaxN to automatically determine key mineralogical
measures such as liberation, association, grade recovery and phase abundance quickly and easily.
Classifications are performed on the fully quantified data and as such can be easily tailored to any sample.

www.oxford-instruments.com/mineral

The materials presented here are summary in nature, subject to change, and intended for general
information only. Performances are configuration dependent. Additional details are available. Oxford
Instruments NanoAnalysis is certified to ISO9001, ISO14001 and OHSAS 18001. AZtec and X-Max are
Registered Trademarks of Oxford Instruments plc, all other trademarks acknowledged. © Oxford Instruments
plc, 2015. All rights reserved. OINA/EDS/AN/INCAMineral/1115.