Kari Strand, prof.

Oulu Mining School / Kaivannaisalan tiedekunta

Quantitive evaluation of minerals
in sediments and rocks / (room/huone PR 242)

Sedimenttien ja kivien Thule Institute / Thule-instituutti

kvantitatiivinen mineraaliarvio (room/huone IT 231)

Special issues in geology /

Geologian erityiskysymyksiä
773608S
5 op.
24 h lectures / 24 t luentoja
exercise / harjoitustyö
written exam / kirjallinen
kuulustelu

Part 2 / Osa 2 Oulun yliopisto

 ‒ Sedimentary studies and mineralogical
Examples of compositions
research results ‒ Detrital zircon constraints on the
tectonostratigraphy
using quantitative ‒ Characterizing REE minerals
mineral ‒ Distribution of gold based on mode of
evaluation and occurrence
‒ Fractures and fluids in geothermal
mineral systems
indentification ‒ Specific mineral search and trace mineral
search

2 Oulun yliopisto
 ‒ Close-up of slightly conglomeratic
Sedimentary sandstone from the Satakunta formation
showing lamella rich in quartz (black to
studies and white grains) alternating with
compositionally more immature fine-
mineralogical grained lamella.

compositions

3 Oulun yliopisto
 ‒ The Satakunta formation (traditionally
Petrology and referred to as the Satakunta sandstone) is
provenance a Mesoproterozoic sequence in a fault-
bounded basin within the
Palaeoproterozoic Svecofennian Domain,
resembling typical red beds with ferric
oxides.
‒ Compositional variations of the
sandstones and associated sediments
were studied to consider the subdivision
that could represent different basin
stages of the formation.
‒ In addition, the provenance and
especially the presence of rapakivi
detritus were scrutinized. We propose a
basin evolution model starting from c.
1.60 Ga and ending at 1.27 Ga.
4 Oulun yliopisto
 ‒ The samples for mineralogical study were
Petrology and selected to represent different lithological
provenance of the types and to verify the composition of
parts that appeared to be rich in quartz.
Mesoproterozoic The total number of studied samples was
Satakunta 24. The modes of the samples were
determined using a Mineral Liberation
formation, SW Analyzer (MLA), a combined scanning
Finland electron microscope (SEM) and anenergy
dispersive spectrum (EDS) analyser at
the Outokumpu Mineral Technology
Laboratory of GTK. In XMOD (X-ray
modal) analysis, minerals are identified
according to the spectrum produced by
X-rays. The procedure is rapid and
reliable, and it takes 10 to 15 minutes to
gain 6000 spectra from one thin section.

5 Oulun yliopisto
 The Satakunta formation is composed of arkosic
arenite and subarkose

(A) Results from old petrographic studies on outcrop samples.

(B) The modal composition of drill core samples determined using a Mineral Liberation Analyzer (MLA).
Lithic clasts cannot be distinguished from mineral grains by MLA, but because their frequency is low,
6 Oulun yliopisto
the analysed ratio Q/(Q+F) on the QF side approximates the composition in a QFL plot.
 Modes of the drill core samples analysed by MLA

7 Oulun yliopisto
 MLA chart showing the
interrelationship of
mineral grains

8 Oulun yliopisto
 A study of heavy minerals
in the Satakunta formation

‒ In the fractions CAR, magnetite constitutes most of the grains in the outcrop sample,
whereas muscovite, epidote and biotite are the most common minerals in the drill core
sample. In the fractions 3.3M, magnetite, epidote and almandine prevail in the outcrop
sample, and epidote and grossular in the drill core sample. In fractions 3.3–4, zircon and
apatite are prominent in the outcrop sample, and titanite and zircon in the drill-core sample.
9 Oulun yliopisto
 Heavy minerals from different fractions

10 Oulun yliopisto
 Zircon separations ‒ The pre-processing of the samples at the
Geological Survey of Finland included
for U-Pb dating crushing, separation with a shaking table
(only for the outcrop sample) and
CARPCO magnetic separation. The
concentrates were handled with a heavy
liquid (specific gravity 3.3), Franz
magnetic separation and another heavy
liquid separation (specific gravity 4.05).
‒ Age determinations for zircons were
carried out at the LA-MC-ICP/MS
laboratory of the Department of
Geosciences, University of Oslo.
‒ Large amount of the mounted grains were
unsuitable for age determination due to
being metamictic or cracked.

11 Oulun yliopisto
 Probability density plots (curves) and histograms (blue columns) showing the age
distribution of detrital zircons.

12 Oulun yliopisto
 ‒ The detrital zircon age data imply an
Provence study exclusively Svecofennian provenance for
summary the Satakunta formation.
‒ The coverage of the heavy mineral data is
better than the dated detrital zircons.
Both the reviewed previous data and our
results exclude rapakivi as a major
source. No topaz or other minerals
indicative of rapakivi granites was found
in the heavy mineral fractions of the two
samples analysed by MLA.
‒ To conclude that nothing in the new or
reviewed information points to rapakivi
Hematite forms a network-like texture provenance.

13 Oulun yliopisto
 Basin forming processes ‒ A probable model with a constant
relative uplift of the rift margins
during basin development is
outlined.
‒ The initial basin evolution is
directly related to the ‘rapakivi
stage’ some 1600–1550 Ma ago.

14 Oulun yliopisto
 Basin history and tectonic model ‒ A basin evolution model starting
at c. 1600 Ma and ending with the
intrusion of the diabase dykes
some 1270 Ma ago.
‒ The first basin stages are
connected to progressing
extension of the upper crust in
relation to bimodal (rapakivi-type)
magmatism and the late basin
stages involve the development
of a narrow rift basin following
the trend of the margins of the
current Satakunta formation.
‒ The MLA technique is an
excellent tool for petrography,
quantitative analysis of the most
common minerals in sandstone,
and especially for the recognition
of detrital heavy minerals.
15 Oulun yliopisto
 ‒ Cathodoluminescence images were used to
Detrital zircon study the morphology of the zircon grains and
to select the ion probe spots prior to analyses.
constraints on the U–Pb dating of zircon grains was carried out on
tectonostratigraphy the SHRIMP I, II and RG mass spectrometers at
the Australian National University.
‒ Absolute age constraints are a key requirement
to understand links between global tectonics,
sedimentation and changing surface
environments in the Neoarchean and
Paleoproterozoic
‒ Zircon ages cover all major igneous source
terrains on the Kaapvaal craton and thus
constitute a representative cross section of
craton structure.

16 Oulun yliopisto
 ‒ Maximum depositional ages have been
determined for the Duitschland Formation
(2424 ± 12 Ma – youngest single grain
age), Timeball Hill Formation (2324 ± 17
Ma – youngest single grain age),
Hekpoort Formation (2247 ± 10 Ma –
weighed mean peak age), Daspoort
Formation (2265 ± 20 Ma – weighed mean
peak age), and Magaliesberg Formation
(2214 ± 11 Ma – youngest 2-grain cluster).
‒ Maximum depositional ages and zircon
populations show clear younging trends
up through the succession that reflect a
progressively thicker sedimentary cover
and increasing internal recycling.

17 Oulun yliopisto
 ‒ Detrital zircon geochronology is
increasingly being applied to sedimentary
rock successions, with the aim to
establish maximum depositional ages
(MDA) and to reconstruct provenance of
deposits.
‒ Combined with thorough sedimentary
studies, this allows identification of
unconformities and establishing the
tectonostratigraphic evolution of
siliciclastic-dominated basins.

18 Oulun yliopisto
 Detrital zircon constraints in Finland

19 Oulun yliopisto
20 Oulun yliopisto
 Mineral separation

21 Oulun yliopisto
 Heavy mineral ‒ Recent drilling at Muhos, northern
Finland has revealed an exceptionally
data in the thick thick Quaternary sediment cover,
overlying the unmetamorphosed
till sequence at Neoproterozoic Muhos Siltstone
Muhos, northern Formation in the Oulujoki River Valley.
‒ Geochemistry of the fine fraction and
Finland heavy minerals of the sand fraction were
studied from all four till units and the
Muhos Formation siltstone samples.
‒ Coarse and fine fractions were separated
by dry-sieving. The fine fraction was
analysed by XRF and AAS. The
mineralogical composition of the heavy
fraction was studied by FESEM-EDS and
SEM-EDS (QEMscan).

22 Oulun yliopisto
 ‒ Sediment sequence at Muhos drill-core
consists of four till beds (Mu-1 – Mu-4) and
sand/silt/clay interlayers.
‒ Optically Stimulated Luminescence (OSL)
dating from the sand layer between till beds
Mu-2 and Mu-3 yielded ages of 107 and 110 ka.
Two samples from the sand layer between till
beds Mu-3 and Mu-4 gave ages of 137 and 146
ka. The till beds Mu-3 and Mu-4 deposited
during the Saalian glaciation and till beds Mu-1
and Mu-2 most likely deposited during middle
and late Weichselian glacial events.
‒ The lowest till bed Mu-4 can be divided into
three subunits. On the basis of clast content,
geochemistry of till fines the ice movement
direction was from the NW or NNW during the
deposition of the lowermost brown and red till
units.
‒ The composition of the upper grey unit of till
bed Mu-4 shows that the ice flow direction was
from the WNW.
‒ Petrographical composition of till beds Mu-3
and Mu-2 indicates that the ice flow again was
from the NW whereas the petrographical
composition of the uppermost till bed Mu-1
suggests that the ice flow during this
deposition phase was from the WNW.
23 Oulun yliopisto
 Samples
processing and
analysing

24 Oulun yliopisto
 ‒ For heavy mineral analysis of the sand fraction (0.06–
Heavy minerals ‒
0.6 mm) was used.
10–20 g of material were weighted from each sample
to separate heavy minerals by using Na-
heteropolytungstate, LST (d=2.82 g/ml). Magnetite
was separated using a hand magnet.
‒ A total of 200 mineral grains were systematically
identified and the percentages of the different mineral
species from a total of 200 grains were calculated
from the heavy mineral frac-tion of every sample by a
Barite grain from till rapid SEM scan (QEMscan, Zeiss ULTRA plus,
bed Mu-4 resolution 1.0 nm/15 kV).
‒ Minerals were identified using the MinIdent-
programme.
‒ Heavy minerals in the siltstone mainly consist of
apatite, tourmaline, pseudorutile, garnet, amphibole
and sphene.
‒ Barite grains were abundant also in till beds Mu-4
Ilmenite grain from till and Mu-3 as independent minerals and their number
increases towards the base of the sediment
bed Mu-1 sequence in the 3D-observations by the SEM.
‒ Amphiboles (hornblende, tschermakite, edenite,
tremolite/actinolite) are the most common heavy
minerals in the 0.06–0.6 mm fraction of all the till
beds, except in the upper grey unit of till bed IV
where the content of mica is 50%.
25 Oulun yliopisto
26 Oulun yliopisto
27 Oulun yliopisto
 ‒ In this study heavy minerals in central Arctic
Provenance sediments were used to determine those
most prominent provenance areas and their
analysis of the changes related to the Late Pleistocene
central Arctic history of glaciations in the Arctic.
‒ Provenance changes were then used to infer
Ocean sediments variations in the paleoceanographic
environment of the central Arctic Ocean,
such as variations in the distribution of sea
ice, icebergs controlled by the Arctic Ocean
Quaternary Science Reviews circulation.
Volume 147, 1 September 2016, Pages 210–220 ‒ Four critical end-members including Victoria
and Banks Islands, the Putorana Plateau, the
Special Issue: Anabar Shield, and the Verkhoyansk Fold
PAST Gateways (Palaeo-Arctic Spatial and Temporal Belt were identified from the Amerasian and
Gateways) Eurasian source areas, and their
proportional contributions were estimated in
relation to Late Pleistocene ice sheet
dynamics and ocean circulation.

28 Oulun yliopisto
 Geological map of the Arctic Ocean and
‒ Colors of arrows corresponded to
surrounding territories.
provenance end-members. Red
arrow is Banks and Victoria Islands
including the MacKenzie River
drainage sources, blue arrows
correspond to Putorana Plateau
source, green arrow shows input
from Anabar massif, yellow arrow
is Verkhoyansk Fold Belt source.
‒ The studied sediment core is
situated beneath the merging area
of sea-ice transported by the
Transpolar Drift (TPD) and the
Beaufort Gyre (BG) and should
record changes in sedimentary
supplies mostly from the Eurasian
margin and from the northern North
American margin.

29 Oulun yliopisto
 ‒ The >63 mm fraction was poured into a small
Heavy mineral separating funnel consisting of heavy liquid
sodium heteropolytungstate (LST Fastfloat)
analysis with a density of 2.82 g/cm3.
‒ The heavy mineral grains in the medium sand
fraction (0.63 mm - 0.2 mm) from 35 samples
were analyzed with the electron microprobe
(JEOL JXA-8200) at the Center of Microscopy
and Nanotechnology, University of Oulu, using
an accelerating voltage of 16 kV, a beam
current of 15 nA and a beam diameter of 10
µm.
‒ In total 17 analyzed oxides and elements
expressed in wt.% F, Na2O, Al2O3, MgO, SiO2,
Cl, K2O, CaO, TiO2, V2O3, Cr2O3, MnO, FeO,
Smith, D.G.W., Higgins, M.D., 2003. MinIdent NiO, ZnO, Zr2O, P2O5 are used for minerals
for windows, version 3.00 Professional, determination. Heavy minerals were identified
database 1.0. Can. Mineral. 41, 548-552.
using MinIdent-Win 4.0 computer software
(Smith and Higgins, 2003).

30 Oulun yliopisto
 Results ‒ The heavy minerals are presented here
by dividing them into two major groups.
‒ The first group of major silicates
consists of Amphiboles (Ca-amphiboles
and MgeFe-amphiboles), Pyroxenes
(clinopyroxenes and orthopyroxenes),
Epidote, Garnets (Ca-garnets, Fe-
garnets, Mn-garnets), Phyllosilicates,
Zircon, andTitanite.
‒ The second group includes Dolomite,
Phosphates (apatite, fluorapatite), Fe-
oxides (magnetite, goethite, hematite),
Ilmenite, Oxides (anatase, rutile,
chromite, ulvospinel), and Others
(kyanite, andalusite, sillimanite,
cordierite, staurolite, and
cummingtonite).

31 Oulun yliopisto
 Mineral compositional
plots

Ternary diagram with composition fields of Fe-Mg-garnets

from the heavy mineral fraction.

Ternary plots showing pyroxene compositions, expressed

32 in Mg (enstatite), Ca (wollastonite) and Fe (ferrosilite). Oulun yliopisto
 Estimated relative
contribution of four identified
provenance end-members
versus sample depth

33 Oulun yliopisto
 QUANTITATIVE ‒ QEMSCAN analysis coupled with whole
CHARACTERIZATION OF THE rock, REE, Zr and Nb, and electron
microprobe analyses were utilized to
REE MINERALS BY QEMSCAN identify and quantify the mineralogy of
FROM THE NECHALACHO HEAVY the deposit, and define the REE
RARE EARTH DEPOSIT, THOR distribution among minerals.
LAKE PROJECT, NWT, CANADA ‒ QEMSCAN mineralogical data is
TASSOS GRAMMATIKOPOULOS – SGS extremely valuable in assessing the
WILLIAM MERCER – AVALON RARE METALS INC.; mineralogy of the ore. The data have
CHRIS GUNNING - SGS; been implemented in defining the
SARAH PROUT - SGS mineralogy of the ore body, support
metallurgical testwork, predict recoveries
SGS MINERALS SERVICES and grades, and finally calculate reserves
TECHNICAL PAPER 2011-07 of the deposit.
‒ Unlike these better known metals
however, the rare earths have little
tendency to become concentrated into
commercial ore deposits.

34 Oulun yliopisto
 ‒ The most commonly occurring deposits
What are REEs of REEs contain a sub-group of elements
referred to as the “light rare earth
elements” (LREEs), which include
lanthanum, cerium, praseodymium,
neodymium, and samarium.
‒ Less commonly, deposits of REEs
contain the much more valuable sub-
group of elements referred to as the
“heavy rare earth elements” (HREEs),
which include europium, gadolinium,
terbium, dysprosium, holmium, erbium,
thulium, ytterbium and lutetium.

35 Oulun yliopisto
 REE MINERALS ‒ QEMSCAN analysis coupled with
whole rock, REE, Zr and Nb, and
electron microprobe analyses were
utilized to identify and quantify the
mineralogy of the deposit, and define
the REE distribution among minerals.
‒ The sample matrix predominantly
consists of biotite, feldspars, quartz,
muscovite/clays, minor chlorite and
amphibole, magnetite and hematite
and carbonates. REE include in
decreasing order of abundance
allanite (3.6%), monazite (1.5%),
synchysite (0.9%), columbite (0.9%),
fergusonite (0.6%), bastnaesite (0.4%),
and zircon (11.0%). The majority of the
HREE are carried by fergusonite and
zircon, and the LREE by monazite,
allanite, synchysite and bastnaesite.
36 The Nechalacho rare metal deposit is located in NWT, Canada Oulun yliopisto
 REE Applications ‒ In the 1980s, China
started production of
HREEs from unique
laterite clay deposits.
China now produces
approximately 95% of
the world’s rare earths.

37 Oulun yliopisto
 GEOLOGICAL SETTING ‒ The Aphebian Blatchford Lake
Complex, intrudes Archean
Yellowknife Supergroup
metasedimentary rocks and
comprises of early ultrabasic and
basic rocks through to
leucoferrodiorite, quartz syenite
and granite, finally to a peralkaline
granite and a late syenite.
‒ Nepheline syenite underlies Thor
Lake Syenite and was recognised
in drilling of the Lake Zone
mineralization.
‒ Recent studies have indicated that
the mineralization is hosted in
metasomatized and hydrothermally
altered nepheline syenite
underlying the Thor Lake syenite.

38 Oulun yliopisto
 DEPOSIT GEOLOGY AND ‒ The Nechalacho deposit is characterized
MINERALIZATION by near-complete replacement of the
primary mineral assemblageincluding K-
feldspar, plagioclase, biotite and
amphibole, by chlorite, magnetite, biotite,
zircon, bastnaesite, monazite, allanite and
fergusonite. Where the rare earth grades
are higher, the presence of visible high
grade zircon is striking.
‒ The Nechalacho REE mineralization is
hosted in a tabular hydrothermal
alteration zone, exposed over an area in
excess of one km2 and averaging about
100-200m in thickness.

39 Oulun yliopisto
 ‒ The Bulk Mineral Analysis, or BMA, and
Zircon and the Particle Mineral Analysis, or PMA
Fergusonite were used for the analyses.
‒ A representative back scattered electron
microscope image illustrates the
complexity of the ore. It shows
fergusonite and zircon among various
silicates, carbonates and Fe-oxides.
‒ By comparing the chemical analysis and
the mineral distributions, the zones of
enriched LREE and HREE a mineralogical
distinction was demonstrated. Zones of
enriched HREE have higher abundances
of fergusonite (Ce,La,Y) NbO4.
‒ Fergusonite was a target mineral because
it carries significant HREE.

40 Oulun yliopisto
 HREE and LREE distribution among the minerals

Fergusonite and zircon carry most of the HREE, whereas monazite, allanite, synchysite,
41
bastnaesite carry most of the LREE. Oulun yliopisto
 HREE and LREE distribution among the minerals

It is possible that zircon was a primary cumulate phase in the deposit and carried most of the
42
REE. Alteration of zircon might have released REE that were hydrothermally transported Oulun yliopisto

and deposited as REE minerals (allanite, bastnaesite etc.).

 MODERN GOLD ‒ Modern gold deportment studies include
DEPORTMENT AND ITS physical, chemical and mineralogical
assessments, combined to obtain a full
APPLICATION understanding of the nature and
TO INDUSTRY variability of gold in a resource.
LOUIS L. COETZEE, ‒ The distribution of gold, based on
SALOMON J. THERON, speciation, grain size and mode of
GAVIN J. MARTIN, occurrence (liberation, exposure, and
JUAN-DAVID VAN DER MERWE,
mineral association) can be quantitatively
TRACEY A. STANEK - SGS
determined by means of automated
Scanning Electron Microscopic
SGS MINERALS SERVICES Techniques (QEMSCAN/MLA).
TECHNICAL PAPER 2011-04
‒ The most efficient gold extraction
processing route is directly related to the
inherent mineralogical features of the
gold ore being processed.

43 Oulun yliopisto
 Gold deportment study ‒ It is crucial to accurately characterize the
includes mineralogical nature of the ore to be
processed; i.e. characterization of the
precious metal phases (gold deportment)
and gangue minerals.

Gold deportment
testwork options.
44 Oulun yliopisto
 ‒ Advances in automated mineralogy, by
Distribution of Scanning Electron Microscopy,
revolutionized this field of study as the data
gold based on became comprehensive and quantitative.
‒ Two main factors influence representivity
mode of namely (1) biased sample collection and (2)
the ‘‘nugget effect” caused by sparse and
occurrence inconsistently distributed gold grains.
‒ The most common metallurgical tests
employed are direct cyanidation, gravity
separation and diagnostic leaching.
‒ It is found that a combination of
mineralogical and metallurgical tests
provides the most cost- and time-efficient
means to fully characterize gold-bearing
samples.
‒ A composite sample mass of about 10–50 kg
is used for a full gold deportment study.
45 Oulun yliopisto
 MINERALOGICAL ‒ X-ray Diffraction (XRD), optical
COMPOSITION microscopy and QEMSCAN Bulk Modal
Analysis (BMA) are employed to obtain
the detailed quantitative mineralogical
composition of each sample.
‒ Optical microscopy is employed to
identify carbonaceous components (e.g.
kerogen) not easily identified by XRD or
BMA.
‒ Polished sections are prepared from the
different size fractions and analysed by
QEMSCAN Specific Mineral Search (SMS)
in order to determine the sulphide
liberation, mineral association and size
distribution.

46 Oulun yliopisto
 Certain characteristics ‒ Gold mineral type and proportions (e.g.
native gold vs. aurostibite or Au-tellurides).
need quantitatively
‒ Gold-containing particle characteristics (e.g.
extracted particle composition, particle size
distribution and particle SG).
‒ Gold exposure (% of gold grains exposed
vs.% of gold grains locked in gangue
particles).
‒ Gold mineral associations (especially
mineral associations of locked gold grains).
‒ Gold grain size distribution.
‒ An estimate of the amount of sub-
microscopic gold (solid solution or
‘‘invisible” gold). The estimate is obtained by
calculating the particulate gold grade and
subtracting it from the measured head grade.

47 Oulun yliopisto

Cyanidation can be used to
determine
the following
Cyanidation/Carbon
in Leach = CIL
Cyanidation is the most commonly used
technique for extracting gold from ore by
converting the gold to water soluble
aurocyanide metallic complex ions.
Very fine (normally <10 µm in size)
particulate gold, locked in sulphide or other
gangue, may not be exposed to cyanide
solutions at ‘‘normal” grinds (e.g. 80%
passing 75 µm). This may require finer to
ultra-fine grinding (e.g. 80% passing 20 µm
or 80% passing 10 µm) to expose the
particulate gold.
48
‒ To quantify the gold that can be extracted via
direct cyanidation (i.e. free and exposed gold), a
sub-sample is cyanided.
‒ To quantify the gold that is pregrobbed, but which
should be recoverable via CIL processing, a
second sub-sample is cyanided in the presence of
activated carbon.
‒ To quantify the gold liberated by mild oxidative
pre-treatment (occluded in carbonates, pyrhotite,
magnetite, etc.), the CIL residue is subjected to
hot HCl followed by CIL dissolution of the acid-
treated residue.
‒ To quantify the gold occluded within sulphide
minerals, the residue from the previous step is
subjected to a severe oxidative pre-treatment
using hot HNO3 followed by CIL dissolution of the
acid-treated residue.
‒ To quantify the gold associated with
carbonaceous material such as kerogen, the
subsequent residue sample is subjected to
complete oxidation via roasting, followed by CIL
dissolution of the calcine product. The gold
remaining in the final residue is assumed to be
occluded within silicate gangue.
Oulun yliopisto
 GOLD SPECIATION ‒ Gold predominantly occurs as native
metal, often alloyed with silver. Since
native gold has such a high specific
gravity (16.0–19.3) it can be recovered by
gravity concentration, provided the gold
grains are liberated and coarse enough
(>10 µm).
‒ Other naturally occurring gold minerals
include alloys with antimony, tellurium,
selenium, bismuth, mercury, copper, iron,
rhodium and platinum.
‒ There are no naturally occurring gold
oxides, silicates, carbonates, sulphates
or sulphides.

49 Oulun yliopisto
 SEM Backscattered
electron images and
accompanying
QEMSCAN particle
maps of a few gold
mineral containing
particles

50 Oulun yliopisto
 ‒ High Definition Mineralogy is valuable for
QUANTITATIVE the identification and characterization of
TRACE precious or trace mineral components in
an ore, metallurgical product or soil
MINERAL sample.
‒ These components, including gold,
ANALYSIS uranium, and platinum group minerals, or
contaminant heavy metals such as lead,
mercury or arsenic, commonly occur in
the range of 1 to 100 parts per million,
and are normally very costly and time
consuming to locate.

Fine-grained platinum group minerals

(PGM) occur as attachments and
inclusions in silicate minerals.
51 Oulun yliopisto
 High Definition Mineralogy
analysis provides ‒ identification of precious mineral
components,
‒ particle and grain size distribution,
‒ elemental deportment,
‒ mineralogical associations
‒ locking characteristics.

52 Oulun yliopisto

High Definition
Mineralogy can provide
significant input into
strategic decisions at
the acquisition,
exploration,
prefeasibility, feasibility
and operational levels
53 Selected Core Sample
‒ map the bulk mineralogy and ore textures
throughout a deposit and export this data
to 3D imaging software
‒ provide a detailed snapshot of
metallurgical recovery
‒ provide closure and environmental
monitoring: the composition of waste
rock, tailings and soils, and can be used
to detect deleterious minerals containing
As, Pb, Se etc.
Polished Thin Section False-colour Image with mineral list
Oulun yliopisto
 Quantitive clay mineral
analysis
Mineral d/hkl Glycollation effect Heating effect up to 550°C

Smectite
(001) expands to 17 Å No change
15 Å (001)

Illite
10 Å (002) Slight shift No change
3.3 Å (006)

Kaolinite
7.15 Å No change Destroyed
3.58 Å (002)

Chlorite
14.1 Å (001) Mg
Increase in intensity (Mg)
14.1 Å (001) Fe No change
Structure collapses (Fe)
7.15 Å (002)
3.54 Å (004)

54 Oulun yliopisto
 Clay Mineral Analysis ‒ Clays mineral is analyzed with an X-
Ray Diffractometer - XRD (e.g.
Siemens D5000) apparatus with
copper radiation (40 kV, 40 mA) at
angles ranging from 2° to 32° 2θ
(0.02° 2θ per second) immediately
after the sample treatments.
‒ The four principal clay mineral
groups have basal spacings at 7.15
Å (kaolinite, chlorite), 10 Å (illite), 15
Å (smectite) and 14.1 Å (chlorite);
mixed-layer minerals give
intermediate or higher values.
Usually, study of chlorite content is
done by calculate the quantities of
kaolinite and chlorite from the joint
peak at 7.15 Å.

55 Oulun yliopisto
 ‒ The samples can be centrifuged for 2
Treatments for minutes to suspend the clay minerals (<2
µm).

XRD samples ‒ The suspension is to be removed from the

centrifuge tube and placed in another tube.
‒ The samples were concentrated by
centrifugation for 15 minutes, after which
the water is to be decanted.
‒ For the oriented samples the clay material
is then injected on the slide with a drop of
distilled water.
‒ One slide is to be dried for 2 hours at 60°C
and analyzed with XRD equipment. The
second slide is to be solvated with
ethylene glycol for at least 2 hours at 60°C
in a vacuum. This treatment expands
smectite to a basal spacing of 17 Å. The
third slide is to be first heated to 60°C for 2
hours and then to 550°C for 2 hours and
analyzed. Kaolinite and certain chlorites
disintegrate at a temperature of 550°C.
‒ The X-ray identification of the clay minerals
can be then studie from X-ray
diffractogrammes.
56 Oulun yliopisto
 ‒ MacDiff software version 4.2.5. by
Quantitive analysis Petschick (2001) can be used to quantify
the clay minerals from the glycollated
of mineral from samples, which subsequently were used
to calculate percentages by using
XRD diffractorams weighing factors (Biscaye, 1964).
‒ Peak correction with quartz, smoothing
of counts and subtraction of the base
line were done before the analysis. Since
no internal standards were available, the
precise accuracy of this procedure is not
known, but the quantitative analyses
justify interpretations of fluctuations
around ± 2 %.
‒ The applications of MacDiff range from
routine analysis in sedimentology,
especially clay minerals, over analysis of
X-ray diffractogrammes of all types of
rocks and minerals all the way to phase
analysis of various crystalline
substances

57 Oulun yliopisto
 Peak idenfication and
database (MacDiff)

58 Oulun yliopisto
 ‒ X-ray powder diffraction is the best available
QUANTITATIVE X-RAY technique for the identification and
DIFFRACTION ANALYSIS quantification of all minerals present in clay-
rich rocks (claystones, mudstones, and
Synthesis marls).
‒ Accurate quantitative mineral analysis is
CLAY MINERAL d (Å) important in petrological studies,
SMECTITE 4.5, 14.0 Å, expands to 14-17 Å after ethylene glycol, engineering, and industrial applications of
10 Å after heating rocks that contain clay minerals.
ILLITE 10.0, 5.0, 3.34, (2.82, 2.7), 1.99 Å
KAOLINITE 7.1, 3.54-3.57 Å (collapses after 550) ‒ Whereas mineral identification is relatively
CHLORITE 14.1-14.2, 7.1, 4.7, 3.54 Å simple and unambiguous if modern software
VERMICULITE 12.0-15.1 Å, 10.1 Å after heating, 10.4 after KCl and good mineral databases are available,
saturation accurate quantitative analysis of clays
CHLORITE-SMECTITE 12.5 after heating to 550 remains a formidable challenge.
CHLOR-VERMICULITE 14.3 Å,  10 Å after heating
ILLITE-SMECTITE 14.7 Å,  11.0 Å after heating, 12-15 Å after ethylene ‒ The main analytical difficulties in
glycol quantitative mineral analysis of rocks by X-
ray diffraction are related to the chemical
and structural characteristics of clay
minerals: variable chemical composition,
highly variable structures involving different
patterns of layer interstratification including
swelling interlayers.

59 Oulun yliopisto
 Clay-mineral assemblages in ‒ The Ocean Drilling Program Leg 188 Site
high-resolution Plio-Pleistocene 1165 was drilled on the Wild Drift on the
interval at ODP Site 1165, Prydz Continental Rise off Prydz Bay, East
Bay, Antarctica Antarctica to a total depth of 999.1 meters
below seafloor (mbsf).
‒ Study of this interval could show possible
intervals of expansions of the ice-sheet
across the continental shelves and express
the climatic evolution in Antarctica,
particularly during the middle Pliocene warm
period (3.15 to 2.85 Ma), which may provide
an indication of how the Earth responds to a
rise of its surface temperature.
‒ The results from the mid-Pliocene with the
increasing smectite content and decreasing
illite content may indicate warmer and
possibly interglacial conditions

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 Map from Leg 188 including Sites 1165–1167

61 Oulun yliopisto
 Clay mineral
distribution
from the last
5 Ma

62 Oulun yliopisto
 Provenance and sea-ice
transportation of Mid-
Pliocene and Quaternary
sediments, Yermak Plateau,
Arctic Ocean (ODP Site 911)
‒ The clay and heavy mineral analysis of
63
‒ The Mid-Pliocene Global Warmth period
at around 3 Myr is of special interest
because average global temperatures
were significantly warmer than they are at
present.
ODP Site 911 sediments is used to
investigate the sources and transport
mechanisms (sea ice and oceanic
currents) of sediments in the Arctic
Ocean during the Mid to Late Pliocene
(3.10–2.78 Myr) and upper Quaternary
(800 kyr to the present).
Oulun yliopisto
 Clays and heavy minerals in
‒ The time period between 3.10 and 3.00 Myr is
sediments
characterized by a decreasing smectite and
increasing illite content, which is interpreted
as reflecting cooling conditions.
‒ At the beginning of the Mid-Pliocene Global
Warmth period at 3.00 Myr, the smectite
content shows an abrupt increase.
‒ After 3.00 Myr the kaolinite and TOC values
start to increase, probably indicating high
rates of reworked glacially eroded matter.
‒ During the Pliocene, the fluctuating heavy
minerals might reflect changes in freshwater
input from the great Siberian rivers
‒ Based on the composition of the clay and
heavy mineral groups in this study, the most
likely transportation path is the Siberian
branch of the Transpolar Drift

64 Oulun yliopisto
 Amount of
individual clay
minerals
at Site 911

65 Oulun yliopisto
 Synthesis of sediment
transportation to Site 911A

66 Oulun yliopisto
 ‒ A study of the changes in sand grain
Quantitive surface microtextures and their frequencies can
texture analysis – Quartz provide important information on glaciers
sand grains influence as well as paleoenvironments
associated with fluvial, coastal and eolian
processes.

67 Oulun yliopisto
 Implications of quartz grain
microtextures for onset
Eocene/Oligocene glaciation
in Prydz Bay,
ODP Site 1166, Antarctica
68
‒ SEM analysis of quartz grains at Site 1166
was used to characterize the glacial and
preglacial sediments by their diagnostic
textures.
‒ Angular edges, edge abrasion as well as
arcuate to straight steps, are the most
frequent features in glacial deposits. The
highest frequency of grains with round
edges is present in Middle-Late Eocene
fluvio-deltaic sands. However, angular
outlines, fractured plates with subparallel
linear fractures and edge abrasion
indicating glacier influence are also
present.
‒ Verify the transition from the East
Antarctic preglacial to glacial conditions
on the continental shelf from Middle/Late
Eocene to Late Eocene/Early Oligocene
time.
Oulun yliopisto
69 Oulun yliopisto
 Frequency of surface textures from selected samples of Site 1166

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 Quartz grain
microtextures and
heavy minerals -
synthesis

71 Oulun yliopisto
 Example of petrofacies interpretation ‒ Qp = polycrystalline quartz
‒ Qm = monocrystalline quartz
‒ P = plagioclase feldspar
‒ K = potassium feldspar
‒ Lss = siliciclastic sedimentary
‒ lithic fragment
‒ Lsc = carbonate sedimentary
‒ lithic fragment
‒ Lv = volcanic/metavolcanic
‒ lithic fragment
‒ Lm = metamorphic lithic
‒ fragment
‒ C = carbonate minerals
‒ M = mica flakes
‒ D = dense minerals
‒ Bio = biogenic grains

72
Q = Qm + Qp F=P+K L = Lss + Lsc + Lv + Lm Oulun yliopisto
 ‒ Dickinson, W.R., 1970. Interpreting detrital
Sandstone modes of graywacke and arkose. Jour. Sed.
composition and plate Petrol., 40:695-707
‒ Dickinson, W.R., Beard, L.S., Brakenridge,
tectonic setting G.R., Erjavec, J.L., Ferguson, R.C., Inman,
K.F., Knepp, R.A., Lindberg, F.A., and
Ryberg, P.T., 1983. Provenance of North
American Phanerozoic sandstones in
relation to tectonic setting. Geol. Soc. Am.
Bull., 94:222-235
‒ Ingersoll, R.V., Bullard, T.F., Ford, R.L.,
Grimm, J.P., Pickle, J.D. and Sares, S.W.,
1984. The effect of grain size on detrital
modes: a test of the Gazzi-Dickinson point-
counting method. Jour. Sed. Petrol.,
54:103-116

73 Oulun yliopisto
 1. Ore minerals in hornblendite dike and
Own learning diorite
exercise 2. Ore minerals in quartz pebble
conglomerate
3. Heavy minerals in sediment sample
4. XRD analysis for clay minerals

FESEM-EDS

EMPA

Center of Microscopy and Nanotechnology

University of Oulu
74 Oulun yliopisto
XRD
 Ore minerals in hornblendite dyke and
diorite

Thin section photos provided by Al-Tamini Tapu.

75 Oulun yliopisto
 Ore minerals in quartz pebble
conglomerate

Hematite-rich mature granule beds

Pyrite concentrations

Concentration of gold particles

along cross beds in pebbly quartz
76 arenite Oulun yliopisto
 Heavy minerals in
sediment sample

911-42X-1-79 911-45X-4-81
77 Oulun yliopisto
 XRD analysis for clay minerals
BS118-20cm
400

d=9,93889

d=7,07414

d=3,33338
d=14,13486
300

d=3,53126
d=3,55455
Lin (Counts)

d=4,96100

d=4,69861

d=4,24041
200

100

3 10 20 30

2-Theta - Scale
BS118-20N - File: BS118-20N.raw - Type: 2Th/Th locked - Start: 2.000 ° - End: 32.000 ° - Step: 0.020 ° - Step time: 1. s
Operations: Fourier 20.000 x 1 | Background 1.000,1.000 | Import
BS118-20K - File: BS118-20K.raw - Type: 2Th/Th locked - Start: 2.000 ° - End: 32.000 ° - Step: 0.020 ° - Step time: 1. s
Operations: Y Scale Add 60 | Fourier 20.000 x 1 | Background 1.000,1.000 | Import
BS118-20E - File: BS118-20E.raw - Type: 2Th/Th locked - Start: 2.000 ° - End: 32.000 ° - Step: 0.020 ° - Step time: 1. s
Operations: Y Scale Add 120 | Fourier 20.000 x 1 | Background 1.000,1.000 | Import

Diffractogram from Core BS118. Blue curve is ethylene glycol treatment,

78
red represents heated (550oC) and black is the normally air dried sample. Oulun yliopisto
 Some future ‒ Automated evaluations needed for
sediments, rocks and ore samples as well
perspectives as environmental monitoring.
‒ Key analytical tools used in quantitive
mineralogy studies include optical
microscopy, quantitative XRD,
QEMSCAN, EMPA, MLA as well as
portable (onsite) XDR/XRF and
hyperspectral applications.
‒ Quantitave mineralogical data is further
more valuable in assessing the
mineralogy of the ore. The data have
been implemented in defining the
mineralogy of the ore body, support
metallurgical testwork, predict recoveries
and grades, and finally calculate reserves
of the deposit.

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