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O
ct
•prepasahion

P.
Pharmocutical
permangant
Definition
Bodium
heniy -thiosuphak Molas
scondany yllabus
identificotion,

erpessing diferent

-
Ca
and
It
hydvoxids
ANALYSIS
,tuphuric
which ond
Anayci CHAPIER-1
normal standadk
is and tchniqves
concantration,

deteminaion, ,Chydro
the fandadization

oric
re
involves

branch acid,pstascium
solutions- -
Dafinahion

aronium hio\c
of
ths anay
priman
we
of acid Oxalic

0-1
quantification

prOCUJ

pharmgcetiol of and
,rdjum
sulphate,
various and
acid Methadi scop,
OF
ll

ii) ii) i) O
Sprcifed Quontiltive
) Tt
Manval,
It and
Ph
determination
Qualttive
Semi
of derhify of is
Sample
-
conc
ik puificahion

subifanLJ.
sUbfanca
the
of
quautithive
chemical

linit determinathion
ornount
functional andlyiu qualitative
araly thee
is
ar

of [oR

of
deermration
in and
of
identificotion

analysis typu subtfarcs

y
gaup
sdte înstvUmuntal Substons

int
of It ?-(diff.
and
m

impurity
on sampe.
involves

tests Or peSert
elemens
quanthitotive

above
It and and by
a

inyoles using
quarhifkatio tchniques

present in purification
th
th In hods.
So|"
amp.
thu

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© ©
Diagnocus deerminahan
o
ldentification

Qualt Magor
anoUnt Scop
and effrctie,
Ca
Dutbierts-for
finishad
finishd
Control

to of amount

tha
role Pharmaceutial
of
to
Moe

of
Now
pure ot f safe fmaliysu
diagnose
impurity
componunts
presenco
compounda
produts
rau in
re
of
to and
producion

th th
componanS

impurities matesials,

ensUe
the plaut
andlycia
amoUnt
pu*
to
we
aust in the
ot
absenca

drug)
ond detc
intermdiate,
de}vin

th
qrouth.

of qualiiy
play
of esseial
th dniq,
any
of
ll
e

Clasti i) i)
food
It
forensic
Dairy
cal
Ph
Biologica!
Non-
Tt
Instrumunjal

t
involves detominahion

InatrU
furthw is produd
Titratjon
Sampl

cf Sonpl

sel
ar

Mantal

tibations
diuidd
tuo
not "In study
deleminatian

Graundy
typu

-
usod
Io thiA

-
m

and

for sereral iutu kyeach

checas

the
a

anclyci ty ete.
pus.

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Ca METHOD of ANALYSIS

Instrumutal DI#. TECHNIQUES OF ANALYSIS Non- Instrumnta

chromatogaphy othirs |Biologica

Electo <pacto
Mthods
re
analytical anayhcal (ELISA
Gas
Chromatoqaphy
tConducorahy
iR sprcbocopy HPLC
Pokntionay Atonje enjs sjn S.
we
TL
s. HPTLC
Atomic abioptin
Tuvbdimny
toloridr
ll

vü) vi) v) iv) uit Thuy fnd

t Melthods
percenage Pr-fomality Molarit
Mole Molalitiy Concentration,
pesant These
Ph
Parts

out
Solto

fraction

pt Solute
in
aK
of
nllion
or or expe t
calculoahion
any those
expr
o Molal
Molas
Solvent

sstd
ar

concration
and
mi
formol
(ppm) Nor
xed
sdution. sing(
concantoaion. MethodA
basially
Mol
by
conceanvation.

mole

Concantation
concontration.
with concartration)

-folljng
lamount
m

pocontage

th
which

sdvet.

o ae
amount
tom
a

Solute
Solution
amountaf

drug USd
(Conc)

- of to

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ü) •
i)
in
Mole
Molaliti M=
solvent.
dissolved
Tt substancu denotel Molarity

Tt
denoted

kg s Also

It
No.
Ca
Volumu

flso
is
of
defind

(sclue) is of Li deino by known

in by Mole
knDn
the Of (2) Capitad

as,
sMall fundamntal soluion
as
of
re
as,
MIasUe

no. as Mole
of
eight No. solute
(M molar

= (1L)
of moal
0.
Solution.

of molecula MaSs

of moles moles
th of con
we
qien (uni)
nslu
Concotin
solvent a controtion

amount Sdute
weiqht Unit
of of
of which

(In
solua selute
solute
9/A dsoved

kg of and
)
and
ll

pesent
No. Of ii)
Ph
Grom
find tquivalext

of of soluk
It and Nommality

solute tquivalevt vobu No. is

out
Grom

in of defind
deroed Also

raim
S0o
nonmalut
of dissolve
known
solution
ar

49 equivalert

m Weiqht Molecular

as, by
tquivalent
per
of f
in apital
as
L) No.
sol4.
(Hhsoy
of weiqut
itie
Normal

E
m

of
subsfance

(N
ueight
Mal..
of gram
94q
Concentration,

Solution.
a

of
(aOy
equialen

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V) •
iv)
TF
Mole
in
prcertog
Mole
Moles tf is
qram
formality

moles Ong
Ca
frochion

Tt It
denoteod

NO.
of is Lie
formula

of Litte is
of
solute
vole,
Mole Moles
solute
define
as defind

of
formula
of weight
re
frodion
of and
of to a,
olule solution solution.

solute soluent.
wejqt
u,
X
+ the the of
mdes
(solut) the
we
lo0
total
roatio
of jonjc
no.
of soute
solven Conpounds

no. of disolved

no.
of
of
ll

vii) O O vi)
7.
7 7,
Ph

of
Percentage
Pavts
Oh
Dass Mass by by
weight
eight
pr
Voluma
million

of of Also
solution solute
It nillion (alkulation
ar

pavts
is of Volung
of ofSdute knouwn

Volum

st
solute
th (Ppm) Voluma
velgt solue
ast
6
parts
of of
percontage

cf of of
m

Le.
subsfancu.
test Sf of by solute
Solution
Solate
le.
Tt solutian.
solution

quautity is of solutian
solute vol.
x
used
of 100
a

sdute conartatian'.
x
X soluion. 100
Conch for 100
in
ey

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i) i) i)
.
Tt
ty
Sandardizahon
STANDARD

or
Concontation

Primay Pimany
Icnoun Secondaky

and
Sodium
chumicalk is
Ca
do pepared which

concantration.

These
sandavda
sfandada
of which

-
aboate, not
sfandads
to hese SOLUT

o
aud further and hove
through
kequjed
ae typus
re
IONS
make
OYalic
oxalic
thy those
which
accutoel ak
?
furthw highly use thoca
have olution
solution
acid
acid, is
we
for
stundordizion.
acurotely hiqhly
puk
Soluions
lcnoun
silver standardizaian

whjch standard.

veaqurts
ee.. nitratt (pu
ll

- ota -

ii)
) less less thuy they Highly Highly
Ph
per Sulphuric subsanu. analyaik.
0s Secondary

HCI
manganate
sabe puk sduble
pUe,
primary
(Hydvocori

and minly less

Usedfor
sjardards
acid less
ar

mor sfable These hon

(
Atandard

-
KMuo), used -toxic reacive
(Hyso),

eactive
ae
gcid) and
for
standardixation

and
m

hOse
quadittive
solutionu. and
ero
sandardizud

ele. Potassium
than eco
Soluion sfablQ
-friendly
a

1
stan of which

by

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) iv) u) )
* Pepavahion
VARIOUS

PREPARATION

folloing Nomot Sfandadizahion

tissolued
Sulphun) Sodjunm Sodium Oxaic Molecula Molar
Aydrochlovie
Ca
thiosulpháli
Hydroxida acd soluhin
solhian
pr-
MO
acid weiqt in

It
LAR
onpounds iqhed Tt
ocid solvent)<
AND
prpaation s AND

of
Molarity
re
total
V) sfandasd the
VI)
any SANDARDIAlioN

PstassjuM NORMAL
procus
Mas
Ceric
Compound.

"v of
pamangabati
we
of
Sulpkae

olutes
ca
slandard
in
al which
SOLOTIONS

elemnt
dnig)

sal of
ll

O
* tor
)
for
No
prepavahion
Ph
prepasatin Oxaljc

(
N= Jo00

nd o. IN
No.
N
V
|26q aad
OKalk dissolved
af
of =
sol
(nt)
Gr.
eq
of dissolwed

valuma of
ar

sfodavdi
dssol
dissolved

(o.
COOH
COoH
ocd
(L) 0.M)
ve S39
Jooo
ito
N) (126
atiom
Onalic
Oxalic
in Oxalic
m

md 9
looo Oxale I000

(o solvnt.
(aad
acd Mol.
mN. Mol.
m.
sfaud Rosicat
(26
a

ocd
cot
q/nol. ueig
auda) So,
into 1269

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O
tuo for
foL - I)
- - -

tipaion
Standardizohon
IN eutt. corcovdant
Repesi
pink Used
|bipkjalac)

Sfandardization 1
peparatin
Mol.
phen o.l (404) [Link] M: Sodium

till,
N: color
ibation
wt
Ca
M=
al
phthalein
dussolved

4q in wt tdicate
(ndi dissolved
Hydvoxid
with
and with
of
og/mol,Acidity
NaoH
lo00 0.2042

in cator.
indator qm throub

dssolved
m([Link]
(end
phuolpahalein
Y09 0.1
01N |potassium
re
of
x
(
M
NaOH
Potassium

point) (tihation)
49 NaoH
NaOH
Oxalje
(9ppr0x)
faint
in Y09
No0H

solh
1000 biptha in
we
acid
pink (Naot
m! acdily (n NaoH loo0
0
fochon)
CSm]
olor
m.
in
poiut
end so,
lo00
ll
ml.
and for iv) fo O ii)
in
mathyl By HC) pieparation

o.t Sfand
Ph
Sodium
o2q Jooo pale using (32) Mol. Hydrochloric

M Na, otang
rdization

: wt
of m
dissolve
S,03
tiosulphote
yllo) (THAM)
of (mass)
Sm
Sodum of
dsalve
of SH,o,Mol. indicator HCI
(0-
ocad
of
ar

erdpoint:

sy disillud 1000
(asam
,
0-
Son M
arbonai
Using Ol 36-46
--faint
N
BromoCHesol

M m Hu
(HCI
26 water.
9q of ot of of add sol^ g/Rasjty
m

potassium q/nd

n sodiuM Sodjum
Rd sodjum dstilud

248-18 8s Aid
l00
end indi
m add
a

thiosulphai arbona
thiosuphati

iodát point. ator

in
wali.
waer.
of wter
con

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O vi) O V)
preparation pepaation

fo to in
sfandavdization Sfandardizatian
Indicator Mol.
Potasum
dstillad
olor Sulphuric
fdd
tdd loo wt
o.0
, By
Ca
0.02
ed_point. m),
2

M (6
eNd wate. app0x
M
pernanqonate ucing of m) of (98
Aid
methyl
pont
IS3X
1N of 01M

-pink
3m
re
Hsou
Sodjum
In
O.02 HSoy
ed H
of Soy
1
> Color.
indiabr,
ito
Hysoy Casbonate
kMaOy
m loso
we
in, is
lôoom) to00 aint m
phinophnalein
-1s8 ol
of
m
walaL pink (02qm
water.

of
ll

-(0.| vin)

(6S -(o. potastjum

Ph
dissolue
Ceric add
N gm
thus
M
?.2
of of armmoniUm

in Ky
pemaugana

(san volUno qm
water.
ar

applying
mirte
of
ammonium
Upto
Sulphate

of qentle
m

Bom)
SulphaG
hat, kMnOy

of
a

Hysoy about
Nwhal
is
Salt.
and

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•
Us on YouTube
Syllalbuc
prcentage
Errors Aauracy
valua digits
ldentifying

-
diferenca

It ,
-
Ca
trorr Methods)

tiror
to Rules and
ERRORS
is Inttoduchion

= th
CHAPTER-2D

siqnifiant
= Sfondad
batueen
defind
-for Precision,

of
obseved
Standavd
re
.

refining

mininizing ,
Valus
the as,
Sfancdavd
digts, SoUrC
Value

- t
Sigifiant
value.
we
-
sndad sigifiant
eJ
0bsevved
,
is
Obievved
RoUnding
Typu,
value
er
the rors

Valuty value.
/te fiqura,
figut.
-of
ll
lo0

- -
During Due
Du Duo Dus It rror SoUYce
Ph
Dua
in (lack) during

to
Sampling

to
Can

to to to
Parocolamol

Sampla.
onapovt ror
wrong
an of
any ncowect
inpropr of bb error
= observation

inbroper Icnooiedqe
ocUSd be
ar

-
type
nethod

and observahio
alibation
Sample
ocCURd

Calculahan.
S00
handlinq
stoage of by Yomg ng
m

selechian. awd pRpasation

anals),
npurii) due =So
(sfandad

focus.
nd in find.
Cue to leo
a

cqupmint.
data
prcent . impropY

to duu
)

102.
to

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Personal
follouing
hece

eg minimi
i)
due
ii) ii) i) lype
Sustenjc Gross)
These
OceUrS
Random
Syiteni
erors fo
to
Ca
Incorrect
sed.
error Calculation.
erors
T† of
wrong
errors
during -Errors trrors
typu:
hese ero enor
on total is
forimula (Indeerminak)
maindy
be
(Dteminate)
Thos :
ae
re
proceduk
Con analycu
furthir
Detemi

erros
Used be hose

of
or by
dividsd prerented
nate
thee
we
wich
by instrumunt.
error,
ervors LReagent
Insrumetal prsonal
onalyst,
analy
into thodic
typu

-
wshjch
OcCurs

st
ll
1i) O
eq) of Ainayst
dictablg
InstuMnal
krowledga

analyst)
duu

of
Random
Ph
Error thesQ
OCUrS

to
ocurs
has Eros impuities wrong deset
. personal
e
typu and
ror
tT
Vondomly;

no evror
So These
ar

mehod
in may
may
dua
of eliminatidon
Conrol dffieult
ndeterinae
It SoMtimes,
impioper
mistakes

in ocUIs instrumunt

and
to eror
(tengent
whjch
Tt
bt
m

over
to
occUrs
temp
may (dentify
uwhich thoce
dul anayst
sampling
dw or
and theu errors
CaUse
CateleAJ

nd not are
eYrors, t0 due
- to
a

My Color

to
pevention choose
eIYOYS
(unpk blind lack nUs
humidity
typ
possible
wich
nes.
)
.

of Of

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3) 2) i)
Covthol
in with Slank
instvumantt
hose By instruments Calibrahion

following
whch METHODS
Stardard
reag,onts
using
Ca
deemination
or detertnination dekumnats
trrors

without In we Calibration

or
aibration,

In
and
thi, reading and
chck
of mathods

an F
thi, appasaus
nstumunts
re
(
apparatus MINIMIZING

Sonmpla analyciu
solvends ervors
bu
stondard we and tho is
:
minimzd

to (gsares which
mnimisad
value. tu /appavatvs
and is
corvectness
we
idetify

puformad
by proces
solution
minimza
occur ERRORS

Using

inpritia
ee-). by
MaUring

are dus Of by
them.
ll
to
5)
errors
4) Used
two
ot
Ph
Parollel Indeperndent
CoMpOt

A-Substance
analuçis anadysis
MO
tinM
for
and normal

In In
deterination

to deferent-2
onalycis

miniiza and
of this,
Of this muhods
ar

find
ony ony
, deterninahion.

thun
we we
malhod
error
hem. and
substonc
mhod substonces
m

putorm puform
mathody
COmpare

sane and compared

hoice
minimiz
and
the
th
a

thee
tinus but o Mor
by
hun
find
ditterer
than thum. to with

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Example
They Repeated
2) Neay 1)Accuracy-
O
|Precision-
Seven US ACCURALY

CoNch
each
to of
-
These
Can of true about
Ca
Valud

any
closenessS
stdens

of
other.
Ong deCRaSey true th Value

ae
dg tablet
(repeatcd) measuted
thu
ondlysit.
the
the
pufoym
It Valu.
thos
AND

Of f orrechness)
re
-
pecent
the is cloceness)

Mltiple is
have
valud defind Valu procses PRECISION

chanA definud
this
in to
of to
we
experimn
masUe obsU
as, or of
it. of uasUKnut
the as, which
at
vation correctness observahion

errot:

the is
sfandard
it
to thu is tel
ll

fccurocy
Precision Nou,

a) )
Ph
500 O499
the 490 490 Y90

ie. ie.
g mg mg
teplatss
closens i.e.
stardad
mg Mg
ar

Poracalomol

Accuracy

value
prcim

q9g Hu
m

(S00
mq (err
valul

,
a

stardand Is
Vale

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O ) -
insiqnificonts)
Significants.
Keroes

A|
Rules 0ccuracy

and
I whjch SIGNIEICANT

observation

siqu These
Ieoding is
Ca
Non
botween
ficonts.
-Zero
fo .00 sed majndy

kdentifing

-,
ae
to USed

(e tuo
digits
(3) based
and
those
f1GuRES
re
digits
1001 defina
00s
non-Z0
123,
siqnifiant
Ot teAults.
to
ak
siqnificaut
on numbus

non- 123, expess

th
1.001
we
O·002-(0) considerrd decimal

signifian
34s
,
2.048)
dugits dugits
figura
deqree

the
or
or
digits
et( cystem

ae as of
ll

) (6)
-lhi Substactio,
-fo )
Rules
in Rounding Ohers
Ph
addihian l0 Trajling

decjal.

for
2.4S69
fixed Tt
or -
siqnificant,if
2.02.3o09

tqUired
-
l0 270
Relairing
mah Zroes
or diqits
ctf
ar

digits
when /fnding
eq4
2.4S69
siauian
on- occurs,

we
m

siqnifionts ony zeroe,

tequlttd
200 ofter
fiqures

at
a

2.457
decimal.
anyuer

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 CAREWELL PHARMA - A FAMILY OF LEARNING
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REDOX TiTRATION UNIT-4

A
SYLLARUS:

M
a) Concepts of OX\dation and
ond reduchion
b) Types oF ledox tittations (principles and appli aicos)

R
,
Ceimey Jodimetvy ,
lodomtry, Bromatomery, bicOMatry.

A
Titration with potassium iodole.

Definition :

H
Oxidation - reduction
P
t is also knouon titration
•Redox fitration thoce tittotion in which
LL

the unenown (redudng ogents by Using knou (moUn

Of ONdising agnts O]
OR

determin tu UNRNOwn oxjdisng aqens by Using

E

ICnown amount of reducing 0gets. oridising agcn

W

RE DOX Titrat
E
R

RED OX

Oxid ation
A

Reduction Reduing

Titrand
C

• Redox ttttations ae basmd

tha tedox reocton, in

which both Oxidatlon
.

teducton take placos

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CoNCEPTS OXIDATION ANO REDUCT1ON

Ihen ORidation
and reducion roact lons

A
,
toqether hey ae termed as
0s (Redox) reoctiorn.
(Pedox)

M
fe2t
Loxidatian

R
Reduction
. In this

A
reachon, feet Is
Oridlzud and t is tedvcod

Oxidatiorn +(e)
Reducion : c + e
H
P
LL

OXIDATION

reoction, in which foss of electroDs take

pla cas and Oxidotlon stae (valency) increasu
E

involves : fkamples :
W

- Addition
of Oygen
- Rermoval of tydroqen S +
th0
E

- Loss Of electons (LEO)

R

REDVCTION
A

reacion, in which of electons take

dkereases
.
places and th valency
C

\nvdlves:
- Rermoval
oval
of Oxygen CUO +
2H
Additton of ttydtoqen C2H
t 2H C2Hy
Gain ot electons (GEO) + e fet
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Those substorces which invalves in Oxdotion -vedurtion (redox)

eoction t are knðun oxidising /reduin aqerts.

A
Oxidising Aqents

M
TheSe thos substacQs
and oxldisa .
which reduce) kdf (qan elechrons)
others Oxldants.

R
) Potassiu dichromae (k,G,0;), Potassium pemarganae (kMnou)

A
Potasslum Iodale (kLb2), tydroqen paroxido (H0) ele.

H
Reducing Agerts : P
Thoso aye those substaes wch Oxdi ad )Hes itself (l0ss
electron)
and reduce ohers. Also as reducavts.
,
LL

ferroUs triosulphae ferraus sulphate, oralic 0dd

acid ete

Oxidation ( Redving Aqets)

E

2+
W

L
Reducion(Oxldising Aqents)
E
R

REDOX INDICATORS

ae redox
A

indicators which
These those

itration.
C

These ae of follouinqs
indicaor
0D Extunal
O Inteeno! indicator
Instrument indicafor
0 self indicafor

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O
Inteal indicator : Also knoun Redox Indiolors.

these those indicotor whjch exhibit diffeent color

in Oxidised reducod form. -mixed in titan d)

A
eg). ferrojn [ Pale - blueoy Red,]
,
Starch iodide [Slue, o|orles

M
self indicator ? Thece those io which titrant iself

R
act as an Indiator and changes t Color of
titand ofer end
erd point. ) Potsjum per mangorate (kMMo)

A
lodis C Broun] pink color

) External Indicoato : Thecu

H those indicators which ore
P
not added ittond Instead the fi drops of

Solution is taken peiodi cally and ixed with

LL

Indicator Solutian and chck th colo change.

) Potassium fericyanide kfe C(N]

E

muthod USe potenhiormuker

(IN) Instumenal technique : In this
determi naion
W

ond Conductomater instruMent for the

point. t is USod whwn three an
end above
of
E

nôt work ) Potntiomey.

R

Of REDOX TITRATION
TYPES
A

They are of following types :

C

Brormtormetry
(eimeHy
Todimetny Dichtomehry
Most inp.
(M) Titation uit pofasium Todate

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[ODMETRY AND TODoMETRY

A
Tho se ase those ttraton whieh invdlves jodine.
In this itlation, lodine is Used an onldising agerts .

M
[ODIMETRY

R
.
It is one type of redox ttation which involves
t
direct

A
titration uwith T:
I, (lodin).
is mainly based on reacion In which lodine
the
Converted iodide.
H
P
1)
LL

Principle: act as OXidising aqents

stundord Solution oF odine) (In) is vsad

for tthe detenaion Of teducing 0gents SUch as
E

Sodium thiosulphate (NazSz0;), rserioUs aci4 (HAs0) ett..

W

End poin deke mned by using as

i:
sfach indiator
Color changus form blue to ccdorless.
E
R

Procadure

.firsHy talke jodin () in cONcal fiack and

A

mixed with potassium iodide (k1), hen make voluna,

C

by adding wate.
Now, dd sforch as an indiatoy Nouw
this storch solution

make iodine - stach Solutian which blue

Color. I,-Studh Complex Blue color.

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•
Now, ths Solution is then itraed against sodium

thiosulphae (Nass,0i) reducin agents thot is flled în burette.

A
Iz + 2Na,S,0, 2NaT + NazsyOs
(odine Sod. thiosulproke odlum (0dide

M
NOw, during titration, when

R
Sodium thiosulphae from Ti-slardn complex
th blue color

sjavt dis appcuing and at end point t becd (coloress

A
Applications:

•It is USed for the demination

H of sulphur dioxtde
P
and reducing agerts.
LL

IODOME TRY
E

• I+ is type of
one redox titation whi ch involves
W

(indivec) ttration with

1t is based the reaction in uwhich iodide (I)
E

is conNerted I, (1odin) shich further titrated.

-
R

21 Tz + 2e

Todid Todin.
A

Priniple:
C

Sjodard solution of sodium thiosulphae

IO tnis, a
Solution is Used for te delermination liberattd
.
iodine from potassium iodide (kL)

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Then this iodin (T) make complex with Starch soluton

and apptar blue color.

A
Procoqure:

M
• firsHy take Potassium jodido (k) in ftask in excess
amount, hen add Onldising ogerts ( Mno) which reacts

R
with inth presence Of qcidic udium, ushich
ibesated lodine.

A
2kI + Mno, t 3H,S04 + 2kHSOy t
Mangn
Oxide
H Toding MnsOy + 2H,0
P
•Then add stauch solution an indicator which forms
stayc -I Complex of blye Color
LL

• then this T is tihated agoi nst stangad thiosulphale

solution (reducing acqes) filled in burette which converts
E

jodinu solution into jodide

4hen ate
W

Na,s,03
color chaqes from blue to
(olorlecs indicotes end point.
E

T: t 25,0
R

Todide
L libratrd
A

Application: from
C

•This metthod is maurdy used

for boh wel as idising cqets, dua

dejomiation to itT sunsaiu.

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CERIMETRY
. In
this titration Ceic sulphake ( o) lon) uSAd as an

A
oxidising agents shch is basically Used for th
determination

M
ferous ions (fez*), Cut ele.. by using
feroin indicator.

cett

R
+
t fet

A
GROMATO METRY

• In this, Potassíum bromale

H
is USed as Oxidising agerts
P
•
It estimated by adding pstassium todide and dil.
Hydochloric ocid (H).
LL

OICHROMETRY

• In this, potassivm dicomae (K;r;0) is uSAd a strong axtdislng

E

- Igent.
USAd -for determiration of Iron SAs.
W

TITRATION wITH PoTA SSIvM 10DATE

polassiUm iodak (tio:) Ued tittant and a

this,
E

• In
. librivm
oxidising agests. fqui Consfovt
R

NERNST EQUATI ON F:e°- RTA2303, loa)

log(k
A

•
1+ is telation béhwRen E
Elethrode poterial
where
C

potentia 0f a non sfadard E°= stohdard electode poteial

lectrocnejcal cell and R= UnjveNsal qas Constant
Concertrotion of Solution. T= Absolule tempraore
n = N0. Of e trans fe

f= faraday constant.
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ELECTROCHEMICAL METHODS

A
Of ANALY SIS UNIT-5

M
•SYLLARUS:

a) Conductomehy: Introduction,

R
Conduchivity call, Conductometric

titaions, appliations.

A
H
.
Elecdrocni cal Methods P
These are thos methods wich inyolves the
interaction belueen the electvicity and charical veacions.
LL

These methods majndy

Elechrode
USLd
for measUrement of
electric paramater Iiko
like CUrrent,
E

potenial, chaqe by using

W

humical interociand ( conc of ions). Solutioms

It is bassd on that, thest

E

Chemjca solutions diecty /indivectly reach with elecrodes.

R

Also USed forDr

detRchion Of end point of titrations.
A

Methods:
C

0 onductometry
Potentiomehry elecohenmicol cal

Polaogaphy

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CONDUCTOMETRY

A
•
It is the measuremert Of Condvctivity) of
o

M
mobility (movemen)
due the of aions and anions
ouards tecpechively electrodes.

or

R
•
It is basi cally usd te measure ment of
Conducaxo by using instvumen conductometer.

A
H
Conducanco:
• It is the aöl lity of solution to pass the
P
electric CUrrent. t denoted by G:
LL

Conductanre [G] = Ur Siemens s)

Resistanco (R)
(ohm!)
iNJeKSaly proportionol to the resisfanco.

-
E

•
It is
depends on
W

oncentration of ions,
Mobility/mouement of ions
E

-tempeature Of Solution.
R

• The main principle of condvcohelvis thatthe

present a
A

ions in Solution in chemial cells are

responsible for the ftbw of elecric Current.
C

SO, when these ions Moves towards anode 4 cathode

(-)
the (onductanco sfarts.

Hy - Move
Moe

tbwards
touwads
anoda.(+)
Cathode(-)

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TERMS RELATED TO CONDUTOMETRY

. Conductonce
/ Conductivity follous ohm's law.

A
) Ohm's lauw
Itstates that the strength of current (1)

M
possing thyough Corducor i s direcHy
proportional to potertial differexe inversely to resistaxe
(R)

R
I E
I
R R

A
resistance : The

H
speific ReSistance (R) OF i the Condvctar
(P) dinecHy proportional to
the leng» (2) and
P
inNrsely proportional to is area of vOSS sechon (a).
spsor
LL

Ra, Ro Rx
E

(u) Specific conductivit (k): H is the ioverse of specific resisance

k(Kappa) =
W
E

JNSTRU MENTATlON
R

•
The instrument USed for measurement Of Conductance
A

are Jcnown Condvclomeers

based On the wheatstone bidge circuit.

C

•
It

of:
=
• It Consistc Condvctanca
Resistanco
Conducivity cells Con fains electodes]

Beakor
nial ino device
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RaNaa
Conductivity

meler

A
-Burette

M
aibrabr Conduchiity
Digital -Analyk
Cell
display Range Solutian
selector

R
(Aid)
pouer Suwltkh

A
A) pouer supply magnehie (stirrer

H
CONDUCTOMETER

•Instrumeation for Conduco mtu/ Conducomeric titration

P
Conduciviy colls
LL

•It (s mode with qlos vessels in whi ch two

electrodes are pre sents at o define distance ie. lem,
E

Gnd thesQ electrodos are Used MeasUre conductanco.

W

ElQtro des are Of Patinum (pt) and

Coated with platinum black 10 avoid (polaisatia)
E

and to incoease urface area.

R

Surface
elecrode distanc
beweon elecode slcm.
A

It is OF three types:
C

0 low CoNCertroahion Conlains

Jan In which too
electrodes dipped in solution and
eletrodesae modeupup of plai nur.
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G Preipitale type It is Uced for those which confajn

preci pitae solution. I ontains magnetic
stirrer, due

A
to tbis precipilate does no stick or

surfaco of elecrode.

M
) Dipped type (ompletely dipped in solvtion
solution due to It
compressed size.

R
A
elecirodes
Pt Pt
electrodes

Analyt
H -Mognehie
P
sirer
Analyk
solution 4HHH
LL

O louw onCn type @ Precipitation type dipped type

E

|CONDUCOMETRIC TITRATION

the determination of end poinH of

W

is

trtahon by means Of Conductivity measU remente

condu cto metrie itahon.

E
R

Priniple :
.
that, titahon (on)
A

Jt is based On prìniple during

lon is replocod by oters whjch difer n ionic Conductand.

C

to this, qraph OCCUrs beween change In conductaw

volum of titrat had

AMaap chaqes uwhich helps in
and
detchion of end point.
to no. .
Conductivity donqes oCUYS due change in of ions mobility

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Procodure:

fircty calibrok tne inctu ment A

titrant filled i burette ad

A
conductivit cell immersed in anayk solution.

• NOu, tihant added dropwise ino Solution nokd tu reading

M
A sharp chanqes in Condvcanco Impliesthe end
end point and
thu obseved value MUst be plothed qraphially.t*

R
the equvalente point Can be obajned from the point of

A
Inserti on two (ines.
th

Types:
H
P
Used for acid -base neutral tityahions.

0 Strong Add with Strong Acid witn

LL

a strong Base
E

(onducanu
W

Conductane

or
End point
fquivaleneo
polnt tnà poin
E

vol. of titrant (NooH)

vol. of tittont (NH,oH)
R

Ha
w h
NaH
H with NHyoH
A

Hcl+ NaOH
HI +
NHyoy
C

+
Nat +
tho

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)weoak acd with o strong Baso

eq) Acetic aad with sodium hydroxi de

A
Conducanc

Ed point

M
CH, Co0 +Nat +
H0
Vol. of titraut (Na0H)

R
() weak aid uwith weok base

A
e Acetic acád with
ammonjum hydroxide

CHh (o0H +
NH0H1 H End poin
P
LL

Appli caions:

Used to check water pollution in lake, rivers

]t is
E

ond ofher bater reservajr.

sparingly soluble (sals
W

check solubility Of
Also

ttace antibioics.
E

Used to check (alkainity of fresh water

purity Of distilled ond e -ionised water can defrmloed.

R
A
C

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POTENTIOMETRY CHAPTER

UNIT5
2

A
srLLABUS :

M
Electrochemical cell, consuchon ond
asd working of refence
(standard ydroqen . siler chlovide elechrode and Calomel elecrode)

qloss elochrode)
ad indicator electrodes ( metal elechrodes ard

R
melhods to dejervine ehd point of potentiomeric

A
tration and opplicahions.

H
Potertiomery:
. techrique whae potutial of an elecrode is ysed
It is
P
to Measure the Concavtrahion of onalte /solution.
Rosicall, it t measurement Of
OF elechode potential ie.
LL

using electrochcal cels

dìfferences in voltagk befueen the electrod b

Principle :
E

bosed on the principle that in this we (masuve the

ohich is dopends
W

elecvode potential, dea

the OF

indicator electrodes.
poteutal diffunu voltagk bs refrenco and

. Thls potentialis measured ajculated by Nent fquation.

E

elechrode

€
R

2303 RT lag Elechode poterial

k
k: fuilibrium constant for
A

the half- cel) recfion as

ushere, equlibrium law.
C

€: stondard redvchion potential

R G0s onstant
kelvin temperature
T: in the balf reachons
n=NO. Of elecvans ttansferred
faraday of Eechnicty
f=
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ELECTROCHEMICAL CELL

Thesa thoco cells whch the physical /chemal

COnverts

enerqy

A
enerqy into electrical helpsn
and helpsin themeasurement
of clectode potential.

M
• 1F helps in the generation of voltoge)Cie. electromotive forceJ
ent
and Current bu usin9 chenicl reochonc

R
fach electrochermjal cell is omposed of to half-cells.

A
Voltmeker

electrode
H
Salt bridqe (Ke)
elecrode
P
Oridgti -depo ition of copper

fnode -Cathode (4)

LL

(-) Ruducian
Half-cell tHalf- col|
ZnsOy
Cyt+so
E

• Flectro chemi a
cells, also known dielectric or galvaniC cell.

•
At anode
W

+ 2e Oxidahion Loss of elechron]

.
ahode.
E

At
( Reducion Gajn of electron:]
R

Salt bridqe elecrical confact Made behueen botn

A

- cells.
the half
-
it majntain te jonic disbalanca ondneutralisa i
C

COmplek th cirwit

Na+ a,kg k+
+
Nac)

Fcell = festferensa t Eindiaor + Ejunetiae: ectomotive focs

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Electtodes
They are moinly USAd
to measUYe the voltagR theye

A
ae majnly two types Of elecvodes USAd in potenfiomtny

0 Reference lstand ard electrode

M
stardad hydroqen
Silver cNoride elecrode

R
alomel electrode

2) IndiCalor electrode

A
Metal elecrode

t Glass electrode

- H
P
O Referenco electrode Thesa aie thos electrode which haue

known elecrode potential

LL

oIt is complelely independent of concentroion of

analyk solution

for the detemiration analyt

of the anayk by
E

maintaining the fixed potential.

W

-Nomal
sfondard tydroqen Electode (SHEJ NHE

with a within a
IF ontajns qlass tube platinumwire sealed
E

plainum foil Coatd with pt. block to Increa sa surfaco area.

R

• This
at as platinom electrode.

whjch mmersed in IM HCU to th qas E

A

Salt budq
majntain tne conc of H* lons. pt wtre
C

The tHydrogen (H) qas in pure

fom js Cortinvousl bubbled in IM HO
the acdjc solution at T- 298k Bubblei of
qas
and pRSSUre = Lam. pt fol Coajed

• It is atachd with aother half cell with analyk so1k

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hen t 0ct
+

A
QH* 2e (oxidation]

When

M
(reduchon)

R
- Silver
) Silver CWoride electrode

A
USed in pH maters as
te internal rekerenco electode.
Constwchiarn:
•
|f conojns a
Ag4 (siver chloride)
silver wire Coaled with

H
P
• The electrode Ag wire
is immersed in solution oF
potassiom chloride [kc] having JM OF
T ion.
LL

• It is tepresented as
-Ag oire
COvered wilh
E

•
there is a reachion blw tq (civer mal ) -Ikc/Agel so14
W

and Agcu (ilver hloride) porous junchin Jtit

Aq +
AgI
Agd t e
or Ag +e Aq6)
E
R

() Calomel electrode

It offen employed as secordory sfadard reference electrode.

A

,
pt. wjre
•A plainUM jre immersed in liquid muUry
i
C

is covered with olomel (i.t. Hq2(44) to salt

•
The to is fled with 1M saturaed solution
bidqt Saturated
OF potasum chlortde (ke). kei so

which kq solution ic
The narow alass tube in
con Connect thiy Hqai,) Hg.
illed hs a Salt bridg wCh
electvodo t0 diffesent
elecrodeS. -rcuny
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It Can be represented as:

A
Worling teochions for half- cell of calomel electrode is

M
Hqt
2+
20 24
Hq2 +(2e
2H9

R
2 Indicaor Etectrodes : -

A
These USed in pair with refeene electrode and
connected with voltmeter.

H
.•
It is USed to detming the Concentration of analyk in
the sample solution.
P
() Metay elecvode -PH
LL

Tt qenerae elechric (potential) as a result of redoxX

reachion on the Surfaca Of metal.

• Plainum or qold melals are Used in indiao electrode.
E

wires to /pH
) Glass tectode
W

Muer

he me0sUre ment Of pH for ay

qiven solution bo done easily
E

Can

USing a qlass elechrode.

a
R

bulb kl soluthia
•
It indudes thn- walled

tubi at top.
a qloss electhad
he bottom and iglAgcl
A

• The bulb is Alled wilh 0-)M HU

elecrode
C

•
4 silver (Ag) wie, (overed with Agd is
present af the louwer end oF qlass tube. 0.] M HCJ

•
It is tepre sentcd as :
thnwalled
Ag4 IM HQ H* (TEST SÔUTION)
glas tub
Aq,

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TpoteNTIOMETER

It is instrument which is Used in poteniomhry

A
|t consists of:
0 Hectrodes References

M
Indicator
2) Vessels

(0) TitraHon burette

R
9 Magntic stirer PH METER Bunettc

A
Sfandond so"
Referenca elecvode

Indicakor
elecrode H
P
LL

Sample /tes
Solution

Mogntie stirrer
E
W

0 Electtodes Tt Conains both referena and indicaot.

Vessels Tt contains
Tt Sample/ analyk solution, whoosa
E

CoNcenfrahin to ba
be msured..
(?) TitatHon byret It conjajns standard 0lution whjch is
R

Used for itraion.

A

titration. tn
.
If is redox end point pH=?
C

stirrer It incEACLA the reaction

9 Magnuhic

Hl t NaOH

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End Point Dection

The erd point or the equivalent point an be iocated

A
using various mthods.
.There is a Aharp change in elecroe potertial
potetial when

M
equivalenxe point (end point) is reochsd.

of ttant
• End point should be reOchd ar) tqval quartity

R
and titrand.

A
) pH MasUremet In this, pH meter to Masue
is vLed

solution, throvqhout th titratin.

H
the pH Of
•A shap/ siqificant (mp) change in pH Can be th
P
, cprially in add- basa titrahion.
endpoint of tic

t potential
LL

) Graphical mthods involves plotting the

difference (voltage) aqcinst ths volumu of titrant
addd.
Y-axis
E

aurve
•A SMmooth |s
drauw Toining al th End léquivalexe
W

poins
. Voltage
point
The endpoint coresponds emt
E

to -axis
X

the ctee pes} (higlu

volun of tittant
Magvtude ) slope on t
R

qraph.

Aid -Base te
A

(m) Tittation In this, endpoint is dekced

Ustng pH mukr. th
p
at equivalenca
C

poin is close to
(v) Rodox the end pout is detem nud by montoing
Changu (voltage du to tho ttansfer
in thu of
eletvons buen the anayk and ittant.
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O Complexomutric tittauons :" n thu, the endpoint is typically

deectedusing indicators electrodes Sensitive
or

A
fo mtal ons

M
APPUcATION S

R
USed in clirical chestvy for th analyss oF

ts Na, k, Ca,

A
electvoty SUch H and ( and dissolved

qasu SUch

• Vsed for th
H
determnatjan of (erdpoint)of an ad bas
P
itrotion
ervivonmuntal chunisty for analyí oF CN,
LL

N, NOg, ln oater and waste water.

USed in
aqriultu foe anlycis of NH,I,a,NO3, k,
E

soils, plat mateials, feuilizurs ek..

W

It alto Uced in food processing deportuntr in

E

-
8alt confenf in daiy pOducs
R

Ca in dairy products and but

k in
fuut guicA
A

-
f in dinkina wars and ofha dinks
C

NO
ad NO2 in mat presentive.
Also USAd in assay of NaboZpam and oth sulpha dgs.

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POLAROGRAPHY CHAPTER-3
ÜNIT-5

A
SYLLARUS:

M
Pvinciple, Tlkoie equaion, construcion and wotking of
,
dropping merury ekcrode ard rototing platinum elechvode

R
applicotions.

A
Polarography :

H
H was invented by Jaroslau tHeuovsky -

electrochenmical hod of analysis which involvs

P
•Tt is on

bween electrode
tthe mQasurement Of (UNent) flowing
voltage applied, whjch helps
LL

in th solution when Some

the ConcevtraHon of a
concentrahon solute/analyt.
to detemine

:
E

Principle
on the pindple tht when voltag (Emf)
•It
.I is based
W

,
is applied between th elecrodes, geducion) taks place
Ondotion
and curent fiow.
E

MOWe

Current is measured) whjch is depends

• Nouw,
ths fowing
R

on tho oNentraion of (ions)/analye.

Two electrodes
A

Dropping Mercury flectvode, Dn

O
Polarizable Elechode
C

Non- polasizable electrode Calomel decrode

•The instrumen Called Polaiogrop) and th CUrve is

Called polaròqram which Is forrmud as cwrent-voltag (urve

(ciqmoid
hapa).

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.Polaroqrophic cuets;
It is o
current
wnih we have to masured le
a
Diffusjon Corrent
(id) = Whn voltaga Is applied in a sautiong

A
pacs wich
diffucion of ions/ analyte taes loca

M
qenwae current le. krown
kroun as diffusjon current.
Jeducing
•It is measured
b
by using |ilkovic equaien.
(urrent

R
jd = 607. n. DM,c

A
whre, id = diffusion curent
no. Of
H
electron
P
di ffusion coefficjent (cm/suc)

M= Mercur fouw rote (m9/sec)

LL

Me aury drop tim (s)

C =
(ontentrafion of anolyte /ions.
. Ac. to
tnis,
E

id KC
W

Tnstumenation
. polaroqraph. polasographic cell
E

knouun
It is also

•J indudes twol elecrodes

R

+Indicator ( polaisable elechrode) act as cathode (e.

murcury electrode)
A

e9) oME ( Dropping

electrode)
RPE (Rotating Platirum
C

RefereNO_ ( non-Polaisable elecrode) act

as anode (+)ve

• Sample solution
• Battery Connection

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DROPPING MeRCURY ELECTRODE

A
•
It is
th woHg elecvode which is Used in polawograph.
• In polavography. as indicator elecrode.

M
Constuchion:

R
•t is Made up of tree
- Caillay

A
- Mercuny reservoir vessels Mercury (H)
standing tub! with odjprent stopcock
• Small mer cury drop is ecelved
H
P
from th orifia of finu
qlass capiltlay tubt
LL

Capillay lenqth S-12 cm

inernal diameter 002 - 0oS mn
tlq teservoir
luterval blw dropst 1-S sac
E

adjusted.

wovking:
W

lar apillary
glas
•T† is polarisoble and
.Mercury (Hq) drops.
E

work as indi aor electrode.

athode
R

and referena lecrod od as

- veYSa.
Onode vC
A

• Anolyk sor is plocad biaker,supporting lecholy k

kCI is 0dded
C

pure N Ite qas is bubbled hough t soluion, to take

out
Then qradually ingesing voltag& is appled to polarogaphie cll,
and curent s recorded.
flowng
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Mercury (H) cotbede

Glass tubing

A
Indiapt
( DME)

M
exist
Nittogen

R
To poteiomter
inat
(tecondu
mode

A
S
Sample refrence
Glon E.

H
Solution
K)
Hq-drop agon (salh
P
(cimn) bidt
frited qlass disc
LL

oking:
• In thic
,
qrodvally ingeosin9 voltagt is aplied beturen

o
E

two elechrodes. palasoti

an

• Due to this, elechrolysis) (ditfusion of ionsj analk) of solution

W

takes place, which qenatates eurent bu fiouwi(ng of eochrons.

• Mercury conhinously aops) fiom the reçeviour through a
E

Capillay tvbe solufion. the nteval blw

th
-s
R

drops of Hg k
is 2-S second.
se
cond. T ac as cahode ve
anotho elechode le. referenco electrode ( standasd
A

Calomel elechrode) which ach as onode () ve

current flo)
C

NOw, thro vah bw thoss electrode and

daa or results are obaind thvovgh polaoqram
In the form of cUHent-voltaga cune
N qase poss to expel out Oygen (o].

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|ROTATING PLATINUM ELETRODE

. as
It is also Usud
used indiator elecvode in polardq roaphy.

A
•It is uCad
USed jn hgh pOsitive poterial Cabovt 0-4u)
wre

M
DME Ca) not b0 USAd.

6-7 mm

R
wwire

A
21-22mm
-

Scm

H
P mercury

Coppr wire
LL

-eury
plainum wire S-6 mm long9

0'S mm diamter
•The eletrode is consructed
E

from a stondard merwvy ual'.

W

•A wire is connected Dlu t yry

mrwry al opplied volg.
electrode is rofacd with a constant spud OF 600 Ypm.
E

o It's workig is similar ar (OME Dropping

cUny electrode
R

APPLICANONS Of POLAROGRAPHY
A

. Quowiahw
determjnation
If helps o the date mi nation
C

Of CONCenttahion of (druqs.)
Metal lons dssolved Ogqe, ett.
Qualtaive determnahion It helps in the determýnatian
Cu, Pb, Ar
el )
At
Of ttaa utal, ek
M
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A
It dso halps in
t deferjnaion of

M
ijomines estimahon of both fat- soluble 4 usate soluble
, , vianjnu.
otmones ThyroxiN insulin, adrenalno ek.

R
,
Anibioties Penicilin streptomycin and chloramphuri col ele.

A
• It is also USad in phuyical , inorqanie and
ard orqoNc
chistry for rsLrch
H work
P
also vSAd in th
fhe fields biochanjstry. pteutical
cheni stvy and ervironmunfal chumi str ete
LL
E
W
E
R
A
C

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