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FACULTY OF EARTH SCIENCE

EGT10203 GEOCHEMISTRY
FEBRUARY 2021/2022

LAB REPORT:
MAJOR, MINOR AND TRACE ELEMENTS
IN IGNEOUS ROCK

Prepared by,

No. Name Matric No.


1) AIMAN ATHIRAH BINTI HASBULLAH E21A0446
2) FELSON BIN PETRUS E21A0481
3) LOSHINI A/P VIJAYASEGARAN E21A0501
4) UMMI AISYAH BINTI AZHARI E21A0686
Objective
To determine the distribution of major, minor and trace elements in igneous rock
sample using appropriate geochemical instruments.
1.0 Introduction
Carbon, hydrogen, oxygen, nitrogen, and sulphur are major elements that make up
more than 1% of the weight of coal. Carbon's relative percentage grows with rank,
while oxygen and hydrogen's relative percentages drop. Minor elements are elements
that constitute 1.0 to 0.01 percent of a coal by weight. Common minor elements in
coal are sodium, magnesium, aluminum, silicon, phosphorus, potassium, calcium,
titanium, manganese, and iron. Most of the minor elements are associated with the
minerals in coal, although phosphorus also is associated with the organic coal matrix
while trace elements are, also called minor element,which is a chemical element
whose concentration is very low. They are classified into two groups essential and
non-essential. Other than that, Igneous rocks form when magma (molten rock) cools
and crystallizes, either at volcanoes on the surface of the Earth or while the melted
rock is still inside the crust. All magma develops underground, in the lower crust or
upper mantle, because of the intense heat there, Igneous rocks can have many
different compositions, depending on the magma they cool from. They can also look
different based on their cooling conditions. For example, two rocks from identical
magma can become either rhyolite or granite, depending on whether they cool quickly
or slowly. Analytical lab instrumentation includes those used within spectroscopy,
mass spectrometry, electrochemical analysis, thermal analysis, separation analysis,
microscopy, and the various hybrid technologies such as GC-MS and HPLC-MS.
Examples of analytical instruments include mass spectrometers, chromatographs such
as GC and HPLC, titrators, spectrometers ( AAS, X-ray, and fluorescence), particle
size analyzers, rheometers, elemental analyzers ( salt analyzers, CHN analyzers),
thermal analyzers, and more. Advantages using spectroscopy is it can be used solids,
liquids and gases but the disadvantage is it cant be use for metals and alloys.
Advantages using electrochemical analysis is because of their simplicity, low cost and
speed but it cannot be recycle and it can be leak.
2.0 Experimental Apparatus and Methods
a) Methods for major elements analysis
1.From the time of collection to the time of analysis, keep chemical or biological
changes to a minimum of samples. Rock samples should be kept in airtight containers
and in a glass bead. Sediment samples should also be stored with as little space as
possible to maintain the anaerobic environment.
2.Label or tag each rock sample container with a unique field identification code.
3.Write the project name or project identification number on the label then write the
collection date and time on the label.
4.Attach the label or tag so that it does not contact any portion of the sample that will
be removed or poured from the container.
5.Then, start the experiment with XRF methods. A controlled X-ray tube is used to
incinerate a rock sample with high-energy X-rays.
6.An electron from one of the atom's exterior atomic orbitals is displaced when an
atom in the rock sample is blasted with an X-ray of adequate energy.
7.The particle regains stabilization once an electron from one of the atom's higher
energy orbital shells fills the vacancy left in the inner orbital shell.
8.By emitting a fluorescent X-ray, the electron descends to a lower energy state. The
particular difference in energy between two subatomic particles of the electron is
equivalent to the energy of this X-ray. The basis of XRF analysis is the monitoring of
this energy.
b) Methods for minor elements analysis.
For the major elements analysis, we using Inductively coupled plasma (ICP-AES)
methods in igneous rock.
1.From the time of collection to the time of analysis, keep chemical or biological
changes to a minimum of samples. Rock samples should be kept in airtight containers
and in a pressed powder disc. Sediment samples should also be stored with as little
space as possible to maintain the anaerobic environment.
2.Label or tag each rock sample container with a unique field identification code.
3.Write the project name or project identification number on the label then write the
collection date and time on the label.
4.Attach the label or tag so that it does not contact any portion of the sample that will
be removed or poured from the container.
5.Follow the sample preparation instructions above. If required, allow the sample to
cool. Add a suitable stabiliser for mercury measurement.
6.To acquire a final concentration of the sample, dilute the sample stock solution with
a suitable solvent.
7.For programme and wavelength, analyse according to the manufacturer's
recommendations. calculate and report result based on the size of the initial sample.
c) Methods for trace elements analysis.
For the trace elements analysis, we using Atomic Absorption Spectrometry (AAS)
methods in igneous rock.
1.From the time of collection to the time of analysis, keep chemical or biological
changes to a minimum of samples. Rock samples should be kept in airtight containers
and in a pressed powder disc. Sediment samples should also be stored with as little
space as possible to maintain the anaerobic environment.
2.Label or tag each rock sample container with a unique field identification code.
3.Write the project name or project identification number on the label then write the
collection date and time on the label.
4.Attach the label or tag so that it does not contact any portion of the sample that will
be removed or poured from the container.
5.Require the three main components a light source, the cell (rock sample), a means
of measuring the light.
6.The sample is atomised once it has been turned to a gas with flame aspiration. The
radiofrequency beam is then passed across it. Some of the radioactivity will be
absorbed by the rock sample.
7.After vapourisation, the sample is ready for preparation for measurement.
8.The amount of light absorbed by AAS is related to the number of atoms in the
element being analyzed.
3.0 Results

Elements Method
Major XRF(X-ray fluorescence)
Minor ICP(Inductively coupled plasma) spectroscopy
Trace Atomic absorption spectroscopy(AAS)
Table 1
1. For the major elements, the method used is the XRF (X-ray fluorescence). This is
because it is relatively non-destructive chemical analysis of rocks,mineral and
many more. It work on wavelength-dispersive spectroscopic principles that are
similar to an electron microphone. The relative ease and low cost of sample
preparation, and the stability and ease of use of x-ray spectrometers make this one
of the most widely used methods for analysis of major and trace elements in
rocks,mineral and sediment.
2. For the minor elements, we used the ICP (Inductively coupled plasma)
spectroscopy. The ICP-MS allows determination of elements with atomic mass
ranges 7 to 250(Li to U), and sometimes higher. Some masses are prohibited such
as 40 due to the abundance of argon in the sample. Other blocked regions may
include mass 80 (due to the argon dimer), and mass 56(due to ArO), the latter of
which greatly hinders Fe analysis unless the instrumentation is fitted with a
reaction chamber. Such interferences can be reduced by using high resolution
ICP-MS(HR-ICP-MS) which use two or more stlits to constrict the beam and
distinguish between nearby peaks. This comes at the cost of sensitivity. For
example, distinguishing iron from argon requires a resolving power of about
10,000, which may reduce the iron sensitivity by around 99%.
3. For the trace elements, we used the Atomic absorption spectroscopy(AAS). This
is because, AAS provides a high degree of accuracy. AAS is also a highly
sensitive method of analysis, where in a given material, it can measure parts per
billion of gram.
4.0 Discussion
Major elements are elements that constitute more than 1 percent of the coal by weight:
carbon, hydrogen, oxygen, nitrogen, and sulfur. Minor elements are those that make
up 1.0 to 0.01 percent of the weight of a coal. Sodium, magnesium, aluminium,
silicon, phosphorus, potassium, calcium, titanium, manganese, and iron are all
common minor elements in coal. The rest of the elements in the periodic table are
found in concentrations of less than 100 parts per million. These are called trace
elements. X-ray fluorescence spectrometry (XRF) is one of the most versatile
methods for analyzing major and trace elements of rock samples. It was discovered
that most igneous rocks are made up of just 10 major elements (O, Si, Al, Mg, Fe, Ca,
Ti, Na, K, P), with minor amounts of Mn and H2O (typically less than 1%). Igneous
rock chemical compositions are normally expressed as a weight percent (wt%) of each
element as an oxide. For those with lithophile affinity, the distribution of minor and
trace elements in igneous rocks is mostly regulated by their ionic radii or size. Minor
and trace elements with radii comparable to those of major elements can be used to
replace these elements in igneous rock common minerals

5.0 Conclusion
In conclusion, there are many instruments for geochemical analyses of elemental
distribution in rock samples. For the major elements analysis, we can use X-ray
Fluorescence (XRF) methods in igneous rock while for the trace elements analysis,
we using Atomic Absorption Spectrometry (AAS) methods in igneous rock. By using
those analytical instrument we can distribute those element into their each type (major,
minor and trace elements).
References
1) National Geographic (2019) igneous rock ,
https://www.nationalgeographic.org/encyclopedia/igneous-rocks/
2) Encycloplodias (2005) Geochemical analysis,
https://www.encyclopedia.com/science/encyclopedias-almanacs-transcripts-and-
maps/geochemical-analysis
3) Carleton.edu (March, 2007) geochemical instrumentation and
analysishttps://serc.carleton.edu/research_education/geochemsheets/workshop.html#L
istofParticipants
4) Thermofisher Scientific (2020) What is XRF
https://www.thermofisher.com/blog/ask-a-scientist/what-is-xrf-x-ray-fluorescence-
and-how-does-it-work/
5) Wikipedia (2022) Inductively coupled plasma mass spectrometry
https://en.wikipedia.org/wiki/Inductively_coupled_plasma_mass_spectrometry#:~:tex
t=Inductively%20coupled%20plasma%20mass%20spectrometry%20(ICP%2DMS)%
20is%20a,ions%2C%20which%20are%20then%20detected.
6) Taylor & Francis Online (2011) Major and minor concentration
https://www.tandfonline.com/doi/full/10.1080/10942912.2010.506621
7) Kerry Taylor Smith (2019) What is Trace elemental analysis
https://www.azomining.com/Article.aspx?ArticleID=1511#:~:text=Trace%20element
al%20analysis%2C%20or%20TEA,toxicology%2C%20forensics%20and%20food%2
0safety.
8) De Gruyter (2017) Analytical Techniques for Trace Element Determination
https://www.degruyter.com/document/doi/10.1515/psr-2017-8002/html?lang=en

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