Analiyticq Date:

Expt. No.:-
Ltroclnuctio Page No.:4.

Detinition
Analytical techniaues are the methods used for the qualilative
and quantitative _determination ot Concerration ot a_compound
y sing various techniquues ike titrations,spect0Scopies.
chromadDaxaphy and qrovimetric analysis.
Tntmduction
*Analytica chenmistay plays a vital xole in Hoe development DE
Science
I t playaa vial role in many Tesearch areas in chemistmy,
liochennisry,bioloqu,qenloqyphysics_and other scien.ces
At lbranches of chemistny drou on the ideaS and techniqes
o analytical chemistmy.
The interdisciplinay nature of chenaical analysis makes ita.
vital tool in caenital anayais) medical,industdal,government
and acodemic laboratories

Nature of -Analytical chemistn

*Analytical chernisty deals with methods for de he chemi
ca coroposition of samples
ualitative Analysis lidentitication) providesitormoction about the
in the sample (an analyte
idertiy o Specieso x functional qroups
conbe iaentified)
onalute
uatita-tive Analysis provides numerical intormation ot
9uaitate the eract amount or concerntration).
-Analutical metbods are o two ypes
i classical methods
iyInstmmental nethods
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 Date:

Expt. No.: Page No.:a

Classical methods: let chemical meth ods sudh.as precipibation,

extraction. diotillation, boiling ox rneltinq points, qravinet.xic and
titrimetric measurements

Instrumental metbods:Analutical measuremernts Cconductiviby,

electande potertial,light abaorption or emission,mass-to-charge
natio,fuOre.ccence etc)are made usinq instoxumentation
classityina quantitative Ahalytical meth.ode:
Gravinmetmic methods: Detemine the mas& of the _analyte or some
Compound chemicalty related o it
*Yolunetric methods the volume ota solution cotaining aufficient
eoqent o eact coaple.te ly with the analyte is measurd
*Spectmscopic methods Based on _measurement othe interacton
beween eledomaqnetic mdiatton and analyte atoms or molecu

*Chromatoqraphic boethodeiSeparation techniques and auarstitation

is based on calilorattion cumve
Eledoanalytical oethods:Involve themeasurement o elecixical
poperties such as voltage Cure,Tesistance and quartity
oeleciical chorqe

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Co mplexoieric libratioLS
Date:
Expt. No.: 4 . ML Page No.: -

Calcnav AOmns ot
Aim
To ectinmate the amount ot Coalcium io ailk powder by
complezom-
etaic titrationusinq thylenediamine etra ace-tic acid (EDTA)-
Theoy
Calcium comprises l5-2.0/ ot Dur body weight.It is reauired loy
the londy to pmduce stong oornes and teeth and qa of the cale
ium ot DuY body js_prsent in oones_and teeth: Milk is aheternge
npus mlatuw of pmteias,sugar,fatikaminsand minecals.Miik
lond miIk produchs ae gome btthe natural sources ot calcium.
Inthis ezpeximent, tue will_estimate the omount of coalcium pres
ent in milk lay complezomebic titration usinq the weti- Enon che
atiq liqand Ehylene diamine tetraacetic acid (EDIA).EDTA Teat
cSith Calcium ond with many other metalions to form ven+
Sable complexes Milk will be analyzed for its Calcium content
uSing EDTA, which reacts to torm CaEDTA Ihe calcium in the
milk reacts quantitativey with EDIA at pH=lo to torm NenY
stable cormplei.EDTA Litraions invalves the use ot an indicatorsu
cas Eiochrome olack-T.This is a netal ion indicadtor whose Calo
ur changes when it binds to a metal ionfor an indicator to be.
setul, it must bind metal less strongly than does EDTA.Asmal
aoourt D£ Mis_added to the Indicator to -fonm a wine ed-
ColDuredcomple As tDIA is added, it reacts irst mith ree calc
ium,and then with the small amount ot the Mg-In complez.As the
nal oa.ces of calcium io the milk is being Compleed,the slight_
eicess of EDTA Comverts the wine Yed- colbuted magnesium comple
ed indicortor irnto the ree blue anion By using ammonical loueffex
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 Date:

Expt. No. Page No.: 4 .

the pH t the solution a-1o) is maintained

+
Ca EDTA lCa-EDTA)
Ca-EDTA +EBT+MaS0 >lMa-EDTA)J+Ca-EBI
Blue colbured comple: Colourless Complez wine-red colour
hoceduNT
step-1: æparastion ot Mgso
solution:
|laleigh 3amsoMaso, and dissolve in 100m owater in a valuna
eic lask.

Step-a1 shandardisation of EDTA

The burette is_cleaned and washed with distilled and illed with
EDTA Aaltion.Take ioml of Mgs0 solition.Add 1oml of auter soluli
aM on and -2 drops t EeT indicator the contents of the soltion
changes to wine ed colour and eolution ia titaated aqainst EDTA
solution.The colour of the solution chanqesiom wine red to blue
Note down the volume ot EDTA and repeat the titrationfor
ConCureny
Step-3: tstimation o Calcium in milk
Part -IBlank Titrationi
Pipette Out oml of standardized EDTA icto a clean Conical flask
and dilute to 1ooml, add 6dops of BN koH and 4drops of
Eriochmme black-T indicator andtitrate it against Maso om
the buette till the blue colour changes -o pink

PortaBlankTitration
pette out 1oml of EDTA indo a clean conical flask,add 5m milk
dilute it to 1oom and bdrops ot aN KOH along with 4drops_of|
dilute i to 10om
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CALCULATIONS:

Aep-I: Pcparotion of Mgs O4 solution

Molavidy of Mgs4 Mol t ) V )

23)
24 6.50 O049
0e- M

step-a: stond avdi sation of EDTA:

BAxetie ReadinG (na)

No Vel: ot Mas nal2 Tnitialla)Einal Cnml) Vol:of EDTA Lm)
O 3mN i03 m
om m
lom Oml 0 3 m O3m
Oml o 3 O 3
Molovity o EDTA (MEDTA)= ? Molavity of Mgso, (MMgso,) =o.0
No o moóles oEDTA (nEpTA) 1 No o molés 'of Mgs0,
(Maso
Volume ot FDTA (VÇ DTA) 10.3m= Volume o Maso (Vmas o= 1om

MEDTA Ve DTA Mg so MgSo

EDTA

MMasoMga EDTA 0-0411x10

MEDTA
maro

VEoTA MEOTA O04°* EDTA O.0484M

masoa 0 3

Step-T: tstirmation of alcium in ilk

fet Blank Titraion:
Burette Readina lml)_
Vol. ot TDTA ( l )
Inilialtm) |final m)_ Vol of Mgs0 Mpol
1O4 m
Om l04m 0,4 m
10r o4m
 Date:-
Expt. No.:- Page No.:5

aiochome Black-T indicator.litrate aqainst Mq50 ron the bu

ette illthe blue colour changes tn pink.
Result
Amount ot Capresent in one litre =Melaoity ot Ca x40 1.2269L
Amount Dt Cain ppm= 1236ppm
 Part-T
ank Titralion:

Burette Reading (m)

SNo Val: of EPTA (nd) Tnitial Cm) final Cna)Val of MgsoLol)
Om F2m F2m
2 lOm
Om 4 2m :2 m
2m 2m
3 10m Om
Molavity of EDTA (MeoTA) 0. 0484M
=
Molarity of a3*(Mc*)-9|
No. of moles of.EDTA (nEoTA) 4 no. of mole e of Ca =
Volume of tDTA (VEDTA) (10.4-2)
= Volume oF Ca (Vc*) 5m
3.2m

MEDTAVeDTA Mc, Vc*

wowuam

EDTA

Mc MEDTAgoTA nct 0.0484 x3.2 x

EDTA V Ix5
M O.0309 M

Voume o Mgso (V, m)= 10.4 m

Voume of Maso4 (V,ml) = 2 m
Voume euiyalent ot EbTA tha.t hos oraple s,ed wth metal ions rom
Voume
milk
(V-V) =
(1o4-72)m =3.2
Amount of Capres ent in ore i e o milk Molarity of x 4o >o03ohM
40
2 36 3/L
Amount o Ca prsent in
pem= f236 9=123% ppm