CHATER THREE

3-1- Introduction:
The analysis chemistry of silicate rocks and mineral include
in divere range of techniques empoying awid variety of
physical phenomena. Although the concepts on which many
of these techniques are based appear to have little in
common adegree of uniformity does embrace each in terms
of the under lying analytical principles . Thus the desired
geol is to measure asignal relating to the concentration of an
elemental constituent of asample this analyte signal
invariably possesses abacround component, the magnitude
of which usually limits the lowst concentration that can be
satis factory analysed (the direction limit). The precision with
which the signal can be measured depends on avarity of
factors,both fundamental and instrumental in origin . These
include counting staistical errors , sigal to background
ratios , instrumental noise, drift and sensitivity.

3-2-Methods:
3-2-1-Field Methods:
This methods were studed regional geology , minerals ,
topographic feature and Structure feature. This methods are
consist:

3-2-1-1-Profile Method :
This method divide the area to 13 profile , the distance
between any point in profile about (200m) and the distance
between any profile to ather about (500m).where tooken
from any point in profile chip sample and rock sample and
details studies . Any poit in profile have different
coordinates.
3-2-1-2-Geological Mapping:
The work in this stage include delineate geological boundary
for any type of rocks in area of the study with observation of
structures .

3-2-1-3-Rock Samples :
The sample from this type taken in any point in profile by
cracking fresh source rocks by hammer describtion hand in
besement. This sample cutting thin section and veiwing it
under polarized microscope in Alneelain University .

3-2-1-4-Chip Samples :
The sample from this type taken in any point in profiles by
cracking rocks by hammer . This sample taken about 2 kg in
any sample pag.

3-3-Laboratory Methods:
This methods studed in Lab by different type of method ,
This Methods are consist:

3-3-1-Petrographyic study:
Thin section from varioun rock type were prepared at
Alneelain University laboratories . They have been studed
under Microscope . To determine the mineralogical
coposition , texture , micro stucture and alteration
representative fresh samples for chemical analysis.

3-3-2- Samples Preparation for Chemical

Analysis:

This partion is crush the sample by crusher and pulverizing

using ethier aring mill and plate pulverizer.

3-3-3- Analytical Techniques

3-3-3-1- Atomic – Absorption Spectroscopy (AAS)

In Atomic Absorption Spectroscopy, an element in its

atomic form is introduced into a light beam of appropriate
wavelength causing the atom to absorb light (atomic
absorption ) and enter an excited state.

At the same time there is a reduction in the intensity of the

light beam which can be measured and directly correlated
with the concentration of the elemental atomic species
this is carried out by comparing the light absorbance of the
unknown sample with the light absorbance of known
calibration standards.

Atypical atomic absorption spectrometer consists of an

appropriate light an absorption path ( usually a flame but
occasionally an absorption cell ) , a monochromator (to
allow of light of appropriate wavelength) and a detector (
potts, 1992).

The most common form of atomic absorption

spectroscopy is called flame atomic absorption . In This
technique , a solution of the element of interest in drawn
through a flame in order to generate the element in it is
atomic form At the same time , light from a hallow
cathode lamp is passed through the flame and atomic
absorption occurs . The flame temperature can be varied
by using different fuel and oxidant combinations , for
example, a hotter flame is required for those elements
which resist atomization by tending to form refractory
oxides. In This research the A .A.S used manufacturer by
Agilent Perking Elmer A.A.S Device model G.B.C. 932,
U.S.A.1996.
3-3-3-2-Spectrophotometer

The spectrophotometer comes equipped with all the

diode-array advantages fast scanning , excellent
sensitivity , virtually absolute wavelength reproducibility ,
exceptional ruggedness and reliability , minimum
maintenance and open sample area , and significant
improvements in optical performance . Better than two
nanometer resolution , wavelength range of

190 to 1100 nm and less than 0 . 03% stray light is

standard .Spectrophotometer used in this study to
determine the AL₂O₃% , SiO₂% . In This research the
spectrophotometer used manufacturer by CECIL
Instruments Cambridge England SR.NO.121 595.

Preparation of ‘A’ Solution

An amount of 0.05 gm sample and standard is

Decomposed in a Nickel Crucible with NaOH and leached
with distilled water to 500 ml as follows :

1– 5ml 30% NaOH solution ( 9-11 pellet).

2– Weight accurately 0.05gm of sample.

3–Cover and heat the crucible to dull redness for about 5

minutes-remove each crucible from the heat and sort the
melt around the sides.

4– Evaporate (melt) on gas burner .

5 – Add about 50 ml of distilled water to each crucible ,

cover and allow to stand over night .
6– Transfer the content from the crucible to a lliter
volumetric flask (previously rinsed with 50% HCL )
containing about 400 ml of distilled water and 20 ml of 50%
HCL, through a plastic funnel.

7– Each solution diluted to mark with distilled water, mix

well.

8– Keep the solution in polyethylene bottle as ‘A’ solution.

2.3.1.2 Preparation of ‘B’ Solution

An amount 0.05gm of the sample is digested in

concentric HCL ,HF ………….. acids in Teflon Bombs as
follows :

1– ….. 0.05 gm of sample power and standard in Teflon

Bombs.

2– ………….. conc. Hydrofluoric acid (40%AR).

3– Add 3 ml conc. Nitric acid (69.72% AR).

4– Add 3 ml conc. Hydrochloric acid (35.5%).

5– Cover the Teflon Bombs and keep them in an oven at 110

⁰C for about 1 hour .

6– Cool the oven for about 1 hour.

7– Dilute the mixture with 50 ml saturated boric acid.

8– Transfer the mixture in 100 ml a volumetric flask and

dilute it with distilled water to the mark as ‘B’ solution .

9– Keep the ‘B’ solution in polyethylene bottle.

2.3.6 Reagent preparation

The reagent used prepared has been according to

the procedure given in Rapid Analysis of Silicate, Carbonate
and phosphate Rocks (Leonard Shapiro, 1965).

Calculation:

Factor {SiO₂ in standard Χ Wt of standard} ÷

Absorbance of standard

SiO₂% in sample ₌ {Factor Χ absorbance OF THE SAMPLE }

÷ Sample weight

Factor ={ Al₂O₃ in standard Χ Wt of standard} ÷

Absorbance of standard

Al₂O₃ % in sample = {factor Χ absorbance of the sample } ÷

Sample weight

2.3.3 Infrared Spectroscopy (IR)

Infrared absorption Spectroscopy is a rapid, economical

and nondestructive physical method universally applicable
to structural analysis.

The technique is so versatile that it can be used both as a

source of the physical parameters of crystal lattice
determination, and as means of eliciting purely empirical
qualitative relationships between specimens. It is an
intrinsically simple technique that deserves to be more
widely used in clay mineralogy and soil science. Infrared
principles Spectroscopy is the study of light as a function of
wavelength that has been emitted, reflected or s-riched
attered from a solid, liquid, in this study IR was used to
identify the clay mineral in one profile.

The IR spectra were collected at room temperature

by means of Niclot 700 spectrometer for wave numbers
ranging from 4000 cm¯¹ to 350 cm¯¹ (Indian institute of
science (IIT), Bomby ).