Chapter -2

FTIR ANALYSIS
2.1 FTIR
Four Transforms Infraed Spectroscopy ,also known as
FTIR Analysis or FTIR Spectroscopy is an analytical technique
used to identify organic ,polymeric and in the some cases ,
inorganic materials.The FTIR analysis method uses infrared light
to scan test samples and observe chemical preparties.
Figure 2.1 FTIR Spectrometer
2.2. FTIR work
The FTIR instrument sends infrared radiation of about
10,000 to 100 cm-1 through a sample ,with some radiation
absorbed and some passed through .The absorbed radiation is
converted into rotational and or vibrational energy by the
sample molecules. The resulting signal at the detector presents
as a spectrum ,typically from 4000 cm-1 to 400cm-
1 ,representing a molecular finger print of the sample .Each
molecule or chemical structure will produce a unique spectral
finger print ,making FTIR analysis a great tool for chemical
identification.
 Figure 2.2 FTIR SPECTROMETER with source
INTERFEROMETER and DETECTOR
2.3 Sample Preparation
All the collected samples were subjected to various
pretreatment in order to remove organic matter and certain
orther materials for improving the quality and for resolution of
the spectra the KBr pellet technique was used in the present
investigation All chemicals used were of spectroscopic grade.

Materials required for KBr pressed-pellet method are

Potassium Bromide (KBr),acetone ,die for making
pellets ,laboratory hydraulic press for creating pressure on
the confined sample ,small hand agate mortor and pestle
and mechanical vaccum pump. Wet grinding was carried out
by placing 30 to 50 mg of the sample in an agate mortar
along with 20 to 25 drops of ethanol .The ground samples
were dried in a hot air oven at 110 c to remove the moisture
content . Using the KBr pellet technique , each grain sized
sample was mixed with KBr at various ratios
viz .1:10,1:20,1:30 ,1:40 and 1:50 .The mixture was then
pressed into a transparent disc in an evacuable dye at
sufficiently high pressure . The samples in the ratio 1:30
(sample :KBr) was taken for further analysis ,since it gives rise
to maximum transmittance and observable peaks (Ramasamy
et al., 2006).This ratio was checked for 2 to 3 times for its
accuracy.

2.4 Instrument used and procedure

Using the X86 spectrometer , the infrared spectra for all the
samples were recorded in the region 4000-650 cm-1 at room
temperature . It scans the spectra 100 times in 1 minute . The
resolution of the instruments is 0.001cm-1 and the accuracy is +
4 cm-1 .At each and every time ,this instrument was calibrated
for its accuracy with the spectrum of a standard polystyrene
film .An optical layout of FTIR spectrometer.

2.5 FTIR used

FTIR Spectroscopy is an established technique for quality
control when evaluating industrially manufactured
material ,and can be often serve as the first step in the material
analysis process. A chage in the characteristic patternof
absorption bands clearly indicates a change in the composition
of the material or the presence of contamination .This
technique is useful for analyzing the chemical composition of
smaller particle , typically 10 -50 microns, as well as larger areas
on the surface.

FTIR analysis is used

 Identify and characterize unknown materials

(e.g .,films ,solids, power ,or liquids)
 Identify contamination on or in a material
(e.g.,particles ,fibers,power ,or liquid )
 Identify additives after extraction from a polymer matrix
 Identify oxidation ,decomposition ,or uncured momomers in
failure analysis investigations

2.6 FTIR Sample Introduction Techniques

Proper FTIR analysis is only as good as the ability to

introduce and observe the energy from a particular
matrix.Fortunately we have many sample preparation and
introduction techniques available in the laboratory to properly
analyze the sample.In the early days of infrared
spectroscopy ,the only available method of analysis was
transmission .For analysis by transmission ,the sample needed
to be made translucent to the laser and infrared energy ,by
directly inserting the sample in the optical path ,casting a thin
film on a selt crystal ,or mixing a power version of the sample
with a salt and casting.(https ://rtilab.com)

Chapter-5
5.1FTIR ANALYSIS
Result And Discussion
The FTIR spectra for all the soil samples were recored .A
selected representative FTIR spectrum of the soil samples
(S1,S2) as shown in figures 5.1.1 to 5.1.2 . The observed
waves numbers are analyzed and the minerals are assigned
using available literatures (John M. Hunt et al.,
(1950),Tuddenham and Lyon (1970),Stubican and Roy
(1961a&b),farmer and Russell,(1964),Russell et al., (1970),Joe L.
White (1971),Hlavay et al., (1978),Russell
(1987),Madejova(2003),Saikia et al.,(2003) and Ramasamy et al
(2003a,b,c,2004b,2005a,2006c,2009b,2010a,2011 ),P.Rajesh
(2013).The observed wave numbers from all the spectra are
given in the 5.1 and 5.2 two soil samples with their
corresponding mineral names.

Six minerals are identified through FTIR analysis.

Quartz,kaolinite,dehydrated halloysite ,glauconite, thiol-
thioether and terminal alkyne were identified only in soil
samples
Fi gure 5.1 FTIR analysis of soil sample 1
MINERAL IDENTIFICATION :

Table no:1

Feet 1 Wave Numbers Name of the minerals

3380 Quartz

3693 Kaolinite

3623 Dehydrated Halloysite

1636 Kaolinite

990 Glauconite

909 Kaolinite

775 Quartz
Thiol –Thioether
685
Figure 5.2 FTIR analysis of soil sample 2
Table no :2

Feet 2 Wave Numbers Name of the mineral

3362 Quartz

3619 Kaolinite

3690 Kaolinite

2100 Terminal alkyne

(Monosubtituted)
1636 Kaolinite
990 Glauconite
909 Kaolinite
775 Quartz
 THE OVER ALL OBSERVATION OF MINERALS THROUGH FTIR

z
1 FEET SOIL 2 FEET SOIL

1. Quartz Quartz

2. Kaolinite Kaolinite
Dehydrated
3. Halloysite --

4. Glauconite Glauconite
Thiol –Thioether
5. --
-- Terminal alkyne
6.
5.3 FTIR MINERALS
Quartz
The Silicate Minerals are of primary concern because of
their relatve abudance and importance. Quartz is a non –clay
mineral, which is common and invariably present in all the
samples. The Si –O bonds are the strongest bonds in the
silicate structure and can be readily recognized in the infrated
specta of such minerals by very strong bands in the region 900
to 1100 cm-1 stretcthing) as well as less intense bands in the
400 to 800 cm region .The presence of quartz in the samples
can be ascribed by the observation of the peaks In the ranges
460-420 and 510-514 cm due to Si- o asymmetrical bending
vibrations 693-695 cm due to Si-o symenntrical stretching
vibrations while the 1080-1084 and 1160-1164 cm absorption
region arises from si-o low AI for Si substitution .These
assihnments are in good agreement with the observation on
the quartz mineral ontainted by Hlavay et al (1978) with the
view of the keller and pickett (1949) the observed absorption
peaks in the ranges 1610-1614 and 1870-1875 cm indicate the
presence of quartz in present rock and sediment and
weathered from metamorphic origin

Clay minerals
The presence of the bonds at around 3623 and 3398 -
3400 cm-1 are due to the Kaolinite clay mineral. The intensity
of the bonds various from sample to sample indicates the
quantity. The obesvations made in the present study show that
broad absobtion bond at around 3398 cm-1 is due to OH
stretching vibration of water in the kaolinite strecture . if the
peaks are appeared around 3652 and 3620 cm -1, then the
presence of kaolinite is in ordered state .however, in this study
ordered state kaolinite was observed in 2 sediment sampling
sits (S1,S2) .However only one peak is observed (3621 –3625
cm-1) in the (S1,S2).

Glauconite
 Glauconite ,greenish ferric-iron silicate mineral with
micaceous structure ,characteristically formed on submarine
elevations ranging in depth from 30 to 1000 metres below sea
level .Glauconite is abundant only in sea –floor areas that are
isolated from large supplies of land –derived sediment.

Glauconite forms by three principal processes alteration

of the fecal pellets of bottom –dwelling organisms; modification
of particals of illitic and biotitic clays by seawater ;and direct
precipitation from seawater . particles of glauconite are
generally sand –sized or finer.

Other minerals
According to Russell (1987) ,the trithydrate aluminium
minerals gibbsite is identified by the observation of the peaks in
the range 667-670cm-1 .Appearing peaks at 2854 and 2924 cm-
1 in all the samples show the presence of organic carbon (Bain
and Fraser ,1984,Dios Cancela et al .,1996, song et
al ,.2001,Mohammed Hajaji et al .,2001 and Tung and
Tanner,2002).
Chrysotile is the serpentine mineral ,trioctahedral analogues of
kaolitine with very different morphologies (rusell, ) 1987 .These
minerals and are readily distinguished frm each other
particularly from the OH strectching region. This serpentine
mineral is identified in S40 sendiment samples by their
characteristic absorption bands at around 451 cm -1 the
appearance of peak in the region 1394-1398 cm -1 shows the
presence of cerussite in sediment . the presence of nacrite can
be confirmed by the appearance of the peaks in the ranges 914-
917 cm -1 in S1-S2 sediment samples .

CONCLUSION

Six minerals such as quartz,kaolinite,dehydrated

halloysite ,glauconite,thiol –thioether,terminal alkyne were
observed in the soil samples.Through this FTIR ,totally 6
minerals are identified.
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