Geological Laboratory Experiences On Different Subjects Involving

Rock/Mineral Sample

An Apprenticeship report submitted to Geological department of ASTU on the

experience of laboratory work in which students participated and conducted an
experiment

By: Jitu Tola

Adama science and technology

University
Addis ababa,Ethiopia
Oct,2022
Abstract

In the geological laboratory of Ethiopia which is under the mining ministry of Ethiopia
we have experimented (practiced) on different applications of our field of studies. The
main objective of the study was to ensure that the students had a practical knowledge
which will enable them to operate on the demanded level of expectancy where they
will enroll later on in the workspace. Among a few of the major studies we practiced
on included;Heavy metal separation,thin section preparation,practical evidence of
rock samples,viewing of rock samples on microscope,grinding of the samples using
heavy machines and usage of chemicals on the prepared rock powders. Throughout
the study heavy machinery i.e; jaw crushers,electro separators.microscopes and
chemical processors were used.Samples were separated into ferro and non
ferromagnetic materials using simple handmade equipment. They were then further
separated using electro separating machines where they were then viewed on
microscopes to identify the different ores they contained within. Rock samples were
cut into slabs and polished for thin section preparations. By the process of pulverizing
rock samples were crushed till they were powder by jaw crushers which were mixed
with chemicals to produce certain kinds of products.Generally the apprenticeship was
effective in guiding and preparing the students into upcoming internship programs
through practical knowledge and experiments.

Key words; Heavy metal separation,thin section preparation,rock

sample,microscopes,pulverizing,geochemical and rock analysis.
ACKNOWLEDGMENTS

I would like to express my utmost gratitude to the staff members of the geological
laboratory of Ethiopia, especially to the lab assistants who showed their unwavering
devotion and dedication in guiding and teaching us throughout this apprenticeship
program.

I would also like to thank in advance my fellow friends and members of the geological
department of AASTU who have guided me in some shape or form.
INTRODUCTION

Background

Geology is a field of studies which includes different sections of expertise, like that of
field work,office work and of laboratory work.Even though laboratory work isn’t
considered as a very demanding role as compared to the last two ,it's one of the
fundamental foundations in the study and analysis of geology.

Mines that are dug by field miners are brought back to the laboratory and studied
which then leads to identify and determine the important mineral(economically
significant)from the unimportant ones ,which will also help determine the allocation of
more mine fields in a given specific area. This process in return will help ease the
work of field workers by simplifying their research area by confining them to a specific
location.
In a process of heavy metal separation a ferrous metal i.e; cast and wrought iron or
carbon steel ,is separated from nonferrous metal distinguishing a more ironic metal
from a less ironic metal. These are skyscrapers,automobiles,buildings,tools and
appliances.

A petrographic thin section is helpful for analysis of reservoirs,but petrographic

techniques are useful throughout research and analysis in mineralogy. It provides
invaluable insight and details into mineral compositions and rock formations. By
tapping a thin cover class over a thin slice of a rock,thin section preparation has
multiple purposes i.e; investigating optical properties of minerals in the
rock,petrographic analysis to classify rocks and textural analysis to describe how a
rock is formed. They are also used for fluid or melt inclusion studies,Raman and FTRI
analysis and can also be analyzed in an SEM or electron microprobe. Then used by
the construction industry to build structures of bridges.
Geochemical analysis in geology on the other hand is used to understand
extraterritorial materials such as moon rocks or martian soil samples. It also provides
an essential role in our understanding of the processes that produce economic
concentration of minerals whether by hydrothermal, magnetic, metamorphic, hydraulic
or weathering agents.

From a different point of view it can be concluded that a laboratory work is considered
to be effective in any area of field it is conducted in. It deepens and fixes theoretical
knowledge and develops the skills of independent experimentation. The work includes
preparing an apparatus,equipment and reagents necessary for
experiment,diagramming and planning the experiment,carrying out the experiment
itself and writing the laboratory report. it deepens and fixes theological knowledge and
develops the skills of independent experimentation.

SIGNIFICANCE OF THE STUDY

Through the analysis presented in this report,the study and work of laboratory
personnel has proved to be an effective and productive section as equally as any
other areas of expertise. By playing its role in part of the work it is required of ,it
contributes its fair share of burden. It is very important to remember that laboratory
work is the founding core of any kind of study and appreciate the contribution it brings
forth. This apprenticeship has met its goals at informing certain students by bringing
forth new information that has been missed out at our lectures through practical
knowledge. In addition to this it has also incited some students in hopes of joining this
work force after graduation. Hence the information which is stated in this report may
be helpful at informing researchers who might have interest in this course of study.

OBJECTIVES
General objective;-

The general objective of these studies was to strengthen students in their knowledge
and practical ability enabling them to be effective performers in their respective field of
study.

Specific objective

To be able to separate ferro metals from non ferrous metals

To be able to identify minerals and ores found in these respective metals and use the
appropriate microscope for each kind
To follow the steps and procedures needed to form a thin section preparation and
make samples to analyze.
To use the different machineries to their respective purposes effectively

LITERATURE REVIEW
Heavy minerals

Most sands are composed of 99% of light minerals such as quartz(s.g. 2.65) and
feldspar(s.g. 2.54-2.76). Therefore sands are mainly distinguished on the basis of
their variable heavy mineral content. Heavy minerals are high density siliciclastic
components. They comprise minerals that have specific gravity greater than the two
main framework components of sand and sandstones,quartz(s.g. 2.65) and
feldspar(s.g. 2.54 - 2.76). In practical ,heavy minerals are those with specific gravity
greater than 2.8 to 2.9 ,the limit being dependent on the density of the liquid used to
separate them from the volumetrically more abundant light minerals.Heavy minerals
are usually volumetrically insignificant. However, there are a large number of heavy
mineral species, each of them having their own story to tell. Therefore geologists
often need heavy minerals to get as much information out of the studied rock as
possible.

Fig 1;Heavy minerals including gold on a gold pan.The concentrate is panned from river
sediments of Lapland,Finland.

Heavy minerals are useful to study the provenance of sand, sandstone and the
history of sedimentary rocks.”provenance” is a fancy word used by geologists to talk
about the place where the sand grain broke out of its parent rock and began its
journey as a sediment particle.How do we study provenance? We take a look at the
heavy mineral fraction and make sure what its composition is. i,e; it contains
garnet,staurolite and kyanite.Its then safe to assume that this sand is a weathering
product of metamorphic terran because this mineral assemblage is very topical to
metamorphic rocks.

Fig;2 A closer look at the pfeiffer beach sand. Main heavy mineral species are
garnet,epidote,zircon,magnetite,spinel,spirolite…etc.

Many diamond-bearing kimberlite pipes are discovered by studying heavy mineral

fractions of a sand. We need to look for pyrope (which is a heavy mineral) for
example.This is a rare Mg-bearing garnet that is associated with diamonds in
kimberlite pipes. Its presence in the river sand may give us a hint that kimberlite
pipes. Its presence in the river sand may give us a hint that a kimberlite pipe may be
nearby. To hunt down its location, we have to go upstream and take many samples
until pyrope and some other index minerals found in abundance in kimberlite pipes
suddenly disappear. Heavy minerals have other applications in the forensic, oil and
gas industry.
Heavy minerals sometimes get concentrated as a heavy mineral sand and there
were, ofcourse , no bromoform involved. It was moving water either in a stream or
beach that did the job. Sometimes the sand is so concentrated in heavy minerals that
it has a real economic value as an ore. Sand collectors also love these black sand
deposits. Such heavy mineral concentrates are called placers.

Gold planning is an activity used to separate gold flakes and nuggets from these
placers. However, gold is not the only mineral that is mined from placers. These
minerals also include cassiterite (tin ore),ilmenite (titanium), magnetite (iron), rutile
(titanium), monazite (rare earth), chromite (chromium), zircon (zirconium),etc.
Australia is a particularly well-known heavy mineral source, but heavy mineral
deposits occur in many places.

Table;1 some common and uncommon minerals and their properties

Mineral Density Stability in Stability in Provenance

weathering diagenesis

Anatase 3.82… High High Felsic igneous rocks,

3.97 hydrothermal veins,
alteration product of
titanite or ilmenite.

Andalusite 3.13… High Low Metamorphic rocks.

3.16

Amphibole 3.02… Low Low Igneous and

3.50 metamorphic rocks.

Apatite 3.10… Low High Igneous and

3.35 metamorphic rocks.

Cassiterite 6.98… High Felsic plutonic rocks,

7.07 hydrothermal
deposits.

Chloritoid 3.51… Moderate Moderate Metamorphic rocks.

3.80
Chromite 4.43… High Mafic and ultramafic
5.09 igneous rocks.

Clinopyroxene 2.96… Low Low Igneous and

3.52 metamorphic rocks.

Corundum 3.98… Silica-poor igneous

4.02 rocks, pelitic
metamorphic rocks,
hornfels,
metamorphosed
carbonates, mafic
igneous rocks.

Epidote 3.12… Low Low Mostly metamorphic

3.52 rocks, less in igneous
rocks.

Garnet 3.59… Moderate Moderate Mostly metamorphic

4.32 but igneous also.

Ilmenite 4.70… Igneous and

4.79 metamorphic rocks,
sometimes
hydrothermal veins.

Source; Heavy minerals - sandatlas

Heavy mineral separation

It is very uncomfortable to do if only one grain out of a hundred or less is what we are
looking for. We therefore seek methods to somehow separate heavy minerals from
the bulk of the sand. Obvious way to do that is to use some heavy liquids Which have
a density greater than that of quartz(2.65 g/cm3) but lighter than most minerals.
The most common physical separation methods are washing, high-intensity magnetic
separation, separation by gravity concentration, and separation by floatation, which
makes use of the different surface properties.(Gasik, 1992).some of the specific
methods include; panning,sieving,magnetic separation,measuring the density of the
mineral and use of electro separating machinery to further classify them.

Flow chart; steps in separation process of heavy minerals

Heavy minerals are separated from the light quartz and feldspar by immersion in a
heavy liquid (2.8g/ml). The separation is carried out in a separation funnel. Heavy
minerals sink to the bottom, while lighter minerals float to the surface, The residue of
heavy minerals is drained by opening the tap at the bottom of the separation funnel.
The obtained heavy minerals are mounted on microscope slides for microscopic
identification. Identification occurs on the basis of optical properties under a polarizing
microscope.

Microscopes and their respective merits

Microscopes are great instruments used to see the details of objects/specimens,

purposely used by geologists.These microscopes are used in petrology and optical
mineralogy to identify rocks and minerals. They are highly advanced machineries
specifically designed for examining and researching rocks and minerals. There are
mainly types of microscopes used in geological laboratories,among this are ;-

A petrographic microscope is a type of optical microscope used in petrology and

optical mineralogy to identify rocks and minerals in thin sections. The microscope is used
in optical mineralogy and petrography, a branch of petrology which focuses on detailed
descriptions of rocks. The method is called "polarized light microscopy" (PLM).
Petrographic microscopes are constructed with optical parts that do not add unwanted
polarizing effects due to strained glass, or polarization by reflection in prisms and mirrors.
These special parts add to the cost and complexity of the microscope. However, a
"simple polarizing" microscope is easily made by adding inexpensive polarizing filters to a
standard biological microscope, often with one in a filter holder beneath the condenser,
and a second inserted beneath the head or eyepiece..The two Nicol prisms (occasionally
referred to as nicols) of the petrographic microscope have their polarizing planes oriented
perpendicular to one another. When only an isotropic material such as air, water, or glass
exists between the filters, all light is blocked, but most crystalline materials and minerals
change the polarizing light directions, allowing some of the altered light to pass through
the analyzer to the viewer. Using one polarizer makes it possible to view the slide in
plane polarized light; using two allows for analysis under cross polarized light. A
particular light pattern on the upper lens surface of the objectives is created as a
conoscopic interference pattern (or interference figure) characteristic of uniaxial and
biaxial minerals, and produced with convergent polarized light. To observe the
interference figure, true petrographic microscopes usually include an accessory called a
Bertrand lens, which focuses and enlarges the figure. It is also possible to remove an
eyepiece lens to make a direct observation of the objective lens surface.
An optical microscope, also referred to as a light microscope, is a type of microscope
that commonly uses visible light and a system of lenses to generate magnified images of
small objects. Optical microscopes are the oldest design of microscope and were
possibly invented in their present compound form in the 17th century. Basic optical
microscopes can be very simple, although many complex designs aim to improve
resolution and sample contrast.
The object is placed on a stage and may be directly viewed through one or two
eyepieces on the microscope. In high-power microscopes, both eyepieces typically show
the same image, but with a stereo microscope, slightly different images are used to
create a 3-D effect. A camera is typically used to capture the image (micrograph).
The sample can be lit in a variety of ways. Transparent objects can be lit from below and
solid objects can be lit with light coming through (bright field) or around (dark field) the
objective lens. Polarized light may be used to determine crystal orientation of metallic
objects. Phase-contrast imaging can be used to increase image contrast by highlighting
small details of differing refractive index.A range of objective lenses with different
magnification are usually mounted on a turret, allowing them to be rotated into place and
providing an ability to zoom-in. The maximum magnification power of optical microscopes
is typically limited to around 1000x because of the limited resolving power of visible light.
While larger magnifications are possible no additional details of the object are resolved.
Alternatives to optical microscopy which do not use visible light include scanning electron
microscopy and transmission electron microscopy and scanning probe microscopy and
as a result, can achieve much greater magnifications.

Thin section preparation

In optical mineralogy and petrography, a thin section (or petrographic thin section)
is a thin slice of a rock or mineral sample, prepared in a laboratory, for use with a
polarizing petrographic microscope, electron microscope and electron microprobe.A
photograph of a rock in thin section is often referred to as a photomicrograph.

A thin sliver of rock is cut from the sample with a diamond saw and ground optically
flat. It is then mounted on a glass slide and then ground smooth using progressively
finer abrasive grit until the sample is only 30 μm thick. The method uses the Michel-
Lévy interference color chart to determine thickness, typically using quartz as the
thickness gauge because it is one of the most abundant minerals.

When placed between two polarizing filters set at right angles to each other, the
optical properties of the minerals in the thin section alter the color and intensity of the
light as seen by the viewer. As different minerals have different optical properties,
most rock forming minerals can be easily identified. Plagioclase for example can be
seen in the photo on the right as a clear mineral with multiple parallel twinning planes.
The large blue-green minerals are clinopyroxene with some exsolution of
orthopyroxene.Thin sections are prepared in order to investigate the optical properties
of the minerals in the rock. This work is a part of petrology and helps to reveal the
origin and evolution of the parent rock.

Thin section preparation

Thin sections used for petrological and mineralogical observations are made in
different sizes and using different techniques for curing, polishing and staining. Our
products are made by experienced cutters, using only the finest grinding powders,
adhesives, and diamonds. In addition, mineralogical preparations can sink in
aluminum rings or ankle carry rocks. Preparations are dedicated to the study of
mineralogical, petrological or fluid inclusion. The waiting period is dependent on the
quantity ordered preparations..
We make observations using a high-quality optical microscope in polarized light. For
petrological and mineralogical descriptions we include photographic documentation.
We also have excellent access to analytical equipment in the field of X-ray
microprobe analysis (EPMA and EDS), the qualitative and quantitative analysis we
include photographic documentation made in BSE.

In optical mineralogy and petrography, a thin section is a laboratory preparation of a

rock, mineral, soil, pottery, bones, even metal sample for use with a polarizing
petrographic microscope, electron microscope and electron microprobe. A thin sliver of
rock is cut from the sample with a diamond saw and ground optically flat. It is then
mounted on a glass slide and then ground smooth using progressively finer abrasive grit
until the sample is only 30 μm thick. The method involved using the Michel-Lévy
interference color chart. Typically quartz is used as the gauge to determine thickness as
it is one of the most abundant minerals.When placed between two polarizing filters set
at right angles to each other, the optical properties of the minerals in the thin section
alter the color and intensity of the light as seen by the viewer. As different minerals have
different optical properties, most rock forming minerals can be easily identified.

Ordinary thin section preparation

The ordinary thin section is recommended for transmitted light microscope observations.
The thickness of the rock sample is 30 microns and the thin rock sample is covered with
glass. The most important in ordinary thin section preparation is to have the most clear
observation using the microscope. That's why our ordinary thin sections are prepared
with full attention on no bubbles.

Polished thin sections preparation

To reach the best quality of polished thin sections we are using two methods of
polishing. The first one with no-water is dedicated for clay rich minerals rock samples
and the second one is dedicated for rock samples with no clay minerals. For the first
methodology we are using the oils and non-water diamonds polish and for the second
methodology we are using the water-diamonds fluids. Polished thin sections are
dedicated for EPMA and SEM research, for the best results of mineral analysis we are
suggesting to have a little thicker thin section but it is an optional version. Polished thin
section preparation is little longer than ordinary (regular) thin section.

Thin sections of fines, aggregates for concrete preparation

The preparation of a thin section made of aggregates, fines is easy using special epoxy
glue. For thin sections of concrete the epoxy has special fluorescent yellow dye.

Sample preparation
A vital part of experimentation is sample preparation. It's usually done within 1 inch
diameter cores when studying the physical and mechanical properties of bulk samples
and/or subjecting them to various processes.(stanford university)
Geological samples include a wide variety of materials such as rocks, minerals, ores, soils,
sediments, fossil fuels (as crude oil and coal), and natural water. Sample preparation is a
critical step in the geochemical analysis, and complete sample dissolution is a prerequisite
for obtaining accurate and precise data for geological materials in most studies.
Geological samples such as rocks, minerals, ores, soils, ferromanganese crusts, and
nodules have to be finely powdered to pass a 230‐ mesh sieve before, preferably by agate
grinding machines to avoid contamination.
Important advancements are happening to various atomic, mass and nuclear analytical
techniques used in general to determine major, minor, trace and ultra-trace
elemental/isotopic concentrations in geological materials

Pulverizing
The use of a laboratory pulverizer is a must before sending any soil or test sample for
XRF, titration, ICP or other assay method; you need to pulverize or fine grind a dry
representative portion of the rock sample using what is commonly called in the
laboratory language of sample preparation a laboratory pulverizer. Any of these terms
are part of the jargon to describe the pulverizing machine used to bring the particle size
of your test sample down to low microns. Finer is better, and under 270 mesh (53 um) is
generally fine enough.

Geochemical Analysis
The process or geochemical analysis requires a thorough grounding in chemistry and
Earth sciences, as well as an understanding of the different ways elements can interact
in a given geologic situation. Geochemical analysis can be used to help predict where
petroleum, metals, water, and commercially valuable minerals may be located.

MATERIALS AND METHODS

Sampling and sample preparation
Accurate determination of elemental and isotopic compositions of geological
samples must be a prerequisite for successful mineral exploration,basic
geochemical and geochronological studies. During rock analysis,sample
digestion which involves steps from simple dilution to partial or total
digestion,is a crucial step and is the limiting factor many times for achieving
reproducible and accurate analytical results.sample preparation is a critical
step in the geochemical analysis,and complete sample discussion is a
prerequisite for obtaining accurate and precise data for geological materials in
most studies.
Sample matrix,analytes of interest,the analytical technique, and intended
purpose play a major role in selecting the optimum sample preparation
method. This review focuses on the recent advances,developments,and trends
in sample digestion methods, such as open-vessel acid digestion,closed
digestion,microwave digestion,alkali fusion, use of NH4F for both open and
closed digestions, sintering with Na2o2,fire-assay methods,infrared radiation
digestion,high-pressure asher digestion, and automated sample preparation
systems along with examples of some important and exciting applications in
geochemical and geochrono;ogical studies. Various sample decomposition
methods have been compared to bring out advantages and limitations for a
particular application.

Sample preparation for different analytical techniques

Due to a very broad number of analytes and techniques, the sample preparation
methods also vary depending up on the requirement. In the sample dissolution
process, the sample is treated to convert insoluble components to a soluble
chemical species using chemical exchange reaction. For example, CaCO 3 is
brought into soluble form with HCl by the following reaction:CaCO 3 + 2
HCl → CaCl2 + H2O + CO2 ↑

Calcium chloride is readily soluble in water. Sodium pyrosulfate fusion, for

example, converts zirconia (ZrO2) into zirconium sulfate [Zr (SO4)2], which is
soluble in acid solution by a simple reaction.

ZrO2 + 2 Na2S2O7 → 2 Na2SO4 + Zr (SO4)2

Grinding samples to pass through a 230‐ mesh sieve is generally recommended to

promote total acid dissolution and efficient fusions. Most geological materials
often contain refractory minerals that are resistant to acid attack and may require
several hours of heating with acids. Chromite is an example of a mineral phase
that is very difficult to digest. This is particularly true in the case of REE ores and
minerals because a significant fraction of these elements often reside in accessory
refractory minerals, which could be very difficult to decompose, and digestions are
often incomplete because of the refractory nature of the accessory minerals, such
as zircon. Low recoveries are often obtained when these elements are determined
due to incomplete dissolution of the zircon phase. When these sample solutions
are analyzed, they will yield potentially inconsistent results and very rarely
consistent results are obtained. These sample dissolution methods often use a
variety of combinations and a number of high-pure acids and other chemical
reagents involving a lot of manual labor. In routine analysis, digestion efficiency is
commonly evaluated only by the visual inspection of the final digests. A clear
 solution without suspended particles generally means a successful dissolution.

In general, the sample decomposition methods can be broadly classified into

three types: (i) open acid decompositions, (ii) closed acid
decompositions, and (iii) fusion decompositions. Very often,
during the analysis of rock and ore samples for precious metals,
samples are commonly heated at ∼600 °C to volatilize sulfur and
oxidize organic matter prior to acid attack, both of which may
otherwise co-precipitate the platinum group metals (PGE) and also
reduce Au irreversibly to its metallic form.