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Dr. C.Thangavelu
Assistant Professor of Chemistry
Periyar E.V.R. College (Autonomous)
Tiruchirappalli 6! !".
To
The Registrar
#harathi$asan %ni&ersity
Tiruchirappalli 6! !'.
(ir)
Sub: Ph.D., Third year Annual Progress report for Mr. B.Balanaga arthi ! Reg.
Ref* "#$%&'Ph.D. ('Che)istry'Part*ti)e'+uly $"(('Date: ",*"-*$"((
+ere,ith - ha&e enclose$ the Thir$ year Annual Progress report of Mr. B.Balanaga arthi)
Part.time Ph./.) Research (cholar ,ho ,or0s ,ith my gui$ance for your recor$s an$ for ta0ing
further action in this regar$.
Than0ing you)
1ours faithfully
(/r. C. Thanga&elu)
Enclosure*
2. Thir$ year Annual Progress Report !2".!2'
. Reprint copy of Pu3lishe$ 4ournals $uring this perio$
T+-R/ 1EAR A55%A6 PR78RE(( REP7RT
(u3mitte$ 3y
Mr.B.BA.A/A0A 1ART231
Do4toral Resear4h S4holar 5Part*ti)e6
P7ST ! 0RAD8AT9 : R9S9ARC2 D9PARTM9/T 7; C29M3STR<
P9R3<AR 9.=.R C7..909 5A8T7/7M78S6
T3R8C23RAPPA..3*#$" "$&,
TAM3. /AD8, 3/D3A.
>or done so far
(. .iterature Survey
- too0 the literature sur&ey for the purpose of choosing the pro3lem $ue to
corrosion in in$ustries. 9any in$ustries are using car3on steel as constructing
materials. - foun$ &arious corrosion an$ corrosion control metho$s to control the rate
of corrosion. -n ,hich i ha&e choose a metho$ ,hich can a3le to control the rate of
corrosion 3y the a$$ition of some eco.frien$ly su3stances as a corrosion inhi3itor.
From that i got some i$ea to formulate some ne, inhi3itor formulation. The forme$
ne, formulation must gi&e some higher -nhi3ition Efficiency (-E) an$ it shoul$ not
affect the en&ironment much. +ere i formulate$ such a type formulation to control the
corrosion rate. For that i ha&e choose Phosphonic aci$ an$ some a$$iti&es ,ith a
transporting cation li0e :n
;
.
2. Preparation of Materials
Car3on steel samples ,ith the composition (C !.2<<= ) ( !.!26 =) (i
!."'6 =)9n 2.2>=) P !.!"6 =) Cr !.>>?=) 9o !.> =) 5i !.!<'?=) Al
!.!'2?=) Cu. !.!"'=) Ti. !.!2'@=) V !.!"2"=) P3. !.!!!6= an$ rest -ron
@?.?=) ,ere use$ for ,eight.loss stu$y an$ electrochemical measurements)
specimen of the siAe 2.! cm B !. cm B '.! cm ,ere cut) polishe$ to mirror finish 3y
ta3le grin$ing ,heels) $egrease$ ,ith Trichloroethylene.
a6 Solution preparation
Preparation of the Sto4 solutions
Sodiu) Chloride Solution
(o$ium Chlori$e stoc0 solutions ,ere prepare$ 3y $issol&ing @.<@2 g of
(o$ium Chlori$e in triple $istille$ ,ater an$ ma0e it up to 2 liter. A hun$re$.fol$
$ilution gi&es eBactly 6! ppm of chlori$e solution.
Sodiu) salt of Phosphoni4 a4id
2 g of /iethylenetriamine penta(methylene phosphonic aci$) (/TP9P) ,as
$issol&e$ in ,ater 3y using triple $istille$ ,ater an$ ma$e up to 2!! m6 in a stan$ar$
measuring flas0. 2 m6 of this solution ,as $ilute$ to 2!! m6 to get 2!! ppm of /TP9P
Sodiu) 2ydro?ide solution 5(/6
A3out 22 g of so$ium hy$roBi$e ,as $issol&e$ in >! m6 of triple.$istille$
,ater in or$er to ma0e a solution of normality slightly greater than 2 5. -ts eBtra
strength ,as $etermine$ 3y titrating ,ith a stan$ar$ solution of oBalic aci$) using
phenolphthalein as in$icator. Then eBactly 2 5 5a7+ into a >! m6 stan$ar$
measuring flas0 an$ ma0ing up to the mar0 ,ith triple $istille$ ,ater.
@in4 Sulphate solution
EBactly '.' g of :inc sulphate ,as $issol&e$ in triple.$istille$ ,ater an$ ma0e
it up to 2 litre. A hun$re$ fol$ $ilution yiel$s eBactly 2! ppm of :n
;
ion
concentration.
Sodiu) Tungstate solution
2 g of (o$ium Tungstate ,as $issol&e$ in triple $istille$ ,ater an$ ma$e it up
to 2!! m6 in a stan$ar$ measuring flas0. 2 m6 of this solution ,as $ilute$ to 2!!
m6 to get 2!! ppm of (o$ium tungstate.
Sodiu) 0lu4onate solution
2 g of so$ium gluconate ,as $issol&e$ in triple $istille$ ,ater an$ ma$e it up
to 2!! m6 in a stan$ar$ measuring flas0. 2 m6 of this solution ,as $ilute$ to 2!! m6
to get 2!! ppm of (o$ium gluconate.
Sodiu) potassiu) tartrate solution
2 g of so$ium potassium tartrate ,as $issol&e$ in triple $istille$ ,ater an$ ma$e
it up to 2!! m6 in a stan$ar$ measuring flas0. 2 m6 of this solution ,as $ilute$ to
2!! m6 to get 2!! ppm of (o$ium potassium tartrate.
Sodiu) )olybdate solution
2 g of so$ium moly3$ate ,as $issol&e$ in triple $istille$ ,ater an$ ma$e it up
to 2!! m6 in a stan$ar$ measuring flas0. 2 m6 of this solution ,as $ilute$ to 2!!
m6 to get 2!! ppm of (o$ium moly3$ate.
Trisodiu) 4itrate solution
2 g of triso$ium citrate ,as $issol&e$ in triple $istille$ ,ater an$ ma$e it up to
2!! m6 in a stan$ar$ measuring flas0. 2 m6 of this solution ,as $ilute$ to 2!!
m6 to get 2!! ppm of triso$ium citrate.
2ydro4hlori4 a4id 5(/6
<@ m6 of analar +Cl is ta0en in a 2 litre stan$ar$ measuring flas0 an$ ma$e it
up to 2 litre 3y using triple $istille$ ,ater.
b6 >eight ! loss te4hniAues
Car3on (teel specimen in Triplicate ,ere immerse$ in 6! ppm Cl
.
,ith an$
,ithout inhi3itor. After the immersion perio$ is o&er specimens ,ere ta0en out)
rinse$ in running tap ,ater an$ 0ept in a $esiccators. The corrosion pro$ucts ,ere
cleane$ ,ith Clar0Cs solution. Then Deight loss $etermine$ in or$er to calculate
the -nhi3ition Efficiency an$ Corrosion Rate (CR) using the follo,ing formulae.
D
o
D
i
-. E E F 2!! ..................................
D
o
Dhere)
D
o
E Deight loss in a3sence of an inhi3itor)
D
i
E Deight loss in presence of an inhi3itor
>"' B 6oss in Deight (mg)
CR E ...................................... mpy
(/) ?.<6 B A ($m
) B -P (hours)
/ /ensity of the specimen (A (urface Area of the specimen in $m
) -P
-mmersion Perio$ in hours
46 Prote4tive fil) analyses 5;T*3R , S9M and A;M6
The analysis is ma$e to analyse the protecti&e film forme$ on the metal
surface. +ere &arious surface analysis ma$e to confirm the protecti&e film
formation. FT. -R stu$y lea$s to confirm that the formation of protecti&e film 3y
shifting in freGuency. For that the FT.-R stu$y ,as ta0en an$ shifting of freGuency
has 3een foun$ an$ that confirm the formation of protecti&e film on the surface.
The (canning Electron 9icroscope ((E9) micrographs ha&e 3een ta0en an$
that also confirm the surface morphology of the metal. #y that ,ay it can 3e
confirme$ that the formation of protecti&e film.
The Electrochemical -mpe$ance stu$y is use$ to stu$y a3out the formation of
protecti&e film on the metal surface.
To analyAe the 5ano film forme$ on the metal surface can 3e confirme$ 3y
Atomic Force 9icroscopy. From the Values of P.V) A&erage Roughness (Ra) an$
R9( roughness confirms the formation of 5ano film on the metal surface.
d6 Type of inhibitor
The inhi3itor is the small amount of su3stance) ,hich is a$$e$ to the system
a3le to protect the corrosion from metal. There are three types of inhi3itors ano$ic)
catho$ic an$ miBe$ respecti&ely. The inhi3itors use$ for this stu$y is ano$ic
inhi3itor) ,hich can 3e confirme$ 3y the Electrochemical stu$ies li0e
PolariAation.
e6 Synergis) Para)eter:
The synergism parameter can 3e calculate$ 3y using the eGuation in$icate$ the
synergistic effect eBisting 3et,een the inhi3itors. (
-
&alue is foun$ to 3e greater
than 2 suggesting that the synergistic effect 3et,een the inhi3itors.
(
-
E 2. -
2;
H 2. -C
2;
-
2
-nhi3ition efficiency of the inhi3itor 2)
-