LxperlmenL number:

3
LxperlmenL:
CravlmeLrlc Analysls of a Chlorlde SalL
uA1L:

26 leb. 2014
name:
AmLeshwar Slngh Sandhu
Lab arLner:
lmad Sadeq
Croup number:
8
SecLlon:
l8l M



!"#!$%&
1o use Lhe sLeps of CravlmeLrlc analysls Lechnlque and measure Lhe chlorlde ln an
unknown, glven quanLlLy of salL.
'(&$#)
1. LquaLlon of lormaLlon of Sllver Chlorlde:
!"
!
!!"!
!!"
!
!!"!
! !"#$
!!!
Lq. 1
1hls equaLlon means LhaL !"
!
has an exLra e
-
ln lLs valence shell Lo reach
sLablllLy. Whereas, !"
!
has deflclency of one e
-
Lo compleLe lLs valence shell
elecLrons and reach sLablllLy. 1herefore, !"
!
and !"
!
share one e
-
Lo flll Lhelr
valence shell elecLrons and aLLaln sLablllLy. 1hus, Lhe resulL ls Lhe formaLlon
of a sLable compound !"#$.
2. !"#$ ls hlghly lnsoluble ln waLer. 1hus, lL forms preclplLaLe as colloldal
parLlcles. k
sp
ls Lhe solublllLy producL of Lhe consLlLuenL lons. lor example:
!"#$
!!!
! !"
!
!!"!
!!"
!
!!"!
Lq. 2
k
sp
= !"
!
!!"!
! !"
!
!!"!
Lq. 3
Low solublllLy ln aqueous soluLlons occurs when Lhe k
sp
has a lower value.
1hls, also means when Lhe preclplLaLe formed ls maxlmum Lhe solublllLy was
low ln Lhe aqueous soluLlon.
3. reclplLaLlon ls carrled ouL slowly ln Lhe presence of nlLrlc acld Lo prevenL
lnLerference from oLher anlons of weak aclds. 1hus, Lhe preclplLaLe formed ls
free of co-preclplLaLes.
4. 8y heaLlng and sLlrrlng Lhe soluLlon genLly durlng preclplLaLlon prevenLs Lhe
formaLlon of preclplLaLe as colloldal parLlcles. 1he preclplLaLe formed ls
proper crysLal. unllke Lhe colloldal parLlcles Lhls, preclplLaLe can be collecLed
uslng a fllLer seLup.
3. 1here are Lwo cases as follows:
o ln Alr:
1he phoLodecomposlLlon of sllver chlorlde (preclplLaLe) leads Lo Lhe
formaLlon of flnely dlvlded sllver and chlorlne gas:
!"#$
!!!
! !"
!!!
!
!
!
!"
!!!!
Lq. 4
1he analyLlcal resulLs are low ln Lhls case. As Lhe chlorlne gas produced as
shown ln Lq. 4 escapes Lhe soluLlon.
o When excess sllver chlorlde ls presenL ln soluLlon:
When excess sllver lon presenL ln Lhe soluLlon lL reacLs wlLh chlorlne gas and
forms sllver chlorlde. 1hus analyLlcal resulLs wlll have a hlgher value.
Lq. 3 shows Lhe preclplLaLlon of sllver chlorlde when Lhere are sllver lons
presenL ln Lhe soluLlon.
!!"
! !
!!!
!
!
!
!!!"
!
!"
! !!"#$
!
!!"#
!
!
!"
!!!
!
!"
Lq. 3
6. 8ecause Aqcl has very small amounL of solublllLy ln waLer. 1he maxlmum loss
can be accounLed for uslng k
sp
formula as:
1he k
sp
for Aqcl ls [1] !!!!!"
!!"
!"#
!

1he loss ln moles when washed wlLh 100 ml or 0.1 L of waLer wlll be:
!!!!!"
!!"
!"#
!
! !!!! ! !!!!!"
!!!
!"#
1hus, Lhe maxlmum preclplLaLe loss ln mass:
!"## ! !"#$% ! !! !! !" !"#$
!"## ! !!! !!"
!!!
!"# !
!"#!!" !
!"#
! !!! !!"
!!
!
7. lons such as CC
3
2-
and cn
J
cOO
-
form co-preclplLaLes wlLh sllver and lncrease
Lhe mass of Lhe preclplLaLe slgnlflcanLly.



!#$*&+"#&
Lach parLner performed Lhe followlng procedure of Lhe experlmenL lndlvldually. A
sample of salL #291 welghed as 0.1396 g and poured lnLo a 230 ml beaker. 1he color
of Lhe salL was whlLe and Lhe shape of Lhe salL crysLals was lrregular. 1he sample salL
# 291 and cruclbles were welghed as 0.1396 g and 31.3192 g wlLh analyLlcal balance.
1he cruclbles were welghLed uslng a Llssue Lo hold Lhem and an error of !0.0001 g
was accounLed. 100 ml of dlsLllled waLer and 1 ml of dlluLe 6M nNO
J
were added Lo
Lhe salL ln a 230 ml beaker. 1hen Lhe soluLlon was heaLed and sLlrred slowly. !usL
before Lhe heaLlng was sLarLed calculaLed amounL of AqNO
J
(30 mL) was added Lo
Lhe salL (lncludlng 3ml exLra). When Lhe soluLlon was almosL LransparenL, Lhe LesL Lo
check lf Lhe preclplLaLlon of sllver chlorlde was compleLe was performed by addlng
small amounL of AqNO
J
. lf more preclplLaLe formed Lhen, more AqNO
J
was added
unLll preclplLaLlon was compleLed. When Lhe preclplLaLlon was compleLe, soluLlon
was sLored ln Lhe drawer carefully wlLhouL much momenL of Lhe soluLlon.

LaLer, Lhe vacuum fllLraLlon was seLup and fllLer cruclbles were used Lo lllLer Lhe
soluLlon and Lhe preclplLaLe was collecLed. 3 ml of 0.01M nNO
J
was used Lo remove
Lhe remalnlng preclplLaLe from Lhe beaker and fllLered Lhrough Lhe cruclble. Also,
waLer was used Lo remove Lhe preclplLaLe clung Lo Lhe walls of Lhe beaker. **3 ml of
washlngs were collecLed and add a small amounL of ncl was added wlLh help of 1A.
lf llLLle or no LurbldlLy was observed, Lhe washlng was compleLe. lf cloudlness
appeared small amounL of 0.01M nNO
J
was fllLered Lhrough Lhe preclplLaLe. 1he LesL
was performed agaln and lf no LurbldlLy appeared Lhe washlng was compleLe. When
Lhe washlng was compleLe Lhen 3 ml AceLone was fllLered Lhrough Lhe preclplLaLe
and collecLed separaLe, as Lhls wasLe had Lo be LreaLed before dlsposal.
1he cruclble was noL placed ln oven due Lo prlor breakage. 1he mass of Lhe
preclplLaLe wlLh cruclble ls *31.7216. 1he lab coordlnaLor Lo compleLe Lhe
calculaLlons and formal reporL provldes Lhls mass.
** lease noLe - uue Lo Lhe breakage of Cruclbles prlor Lo placlng ln oven, furLher
experlmenL was noL performed and Lhe procedure ls wrlLLen based on observlng
parLners experlmenL.
$,%&#-.'/$0%
1. 1he sample number of Lhe salL was #291. 1he salL was of whlLe color and lL
conslsLed of flne crysLals.
2. A small amounL of AgnC3 was added Lo Lhe preclplLaLe Lo compleLe Lhe
preclplLaLlon. 1he LesL of washlng Lhe preclplLaLe was performed uslng no
more Lhan 3 ml 0.01M nNO
J
buL Lhe LesL of PCL Lo check Lhe washlng was
noL compleLed Lo Lhe breakage of cruclbles. reclplLaLe was losL due Lo
breakage.
3.
1he color of Lhe preclplLaLe was llghL vloleL. 1he color appeared
because cerLaln exposure Lo llghL ls lnevlLable. When Lhe soluLlon was
exposed Lo llghL sllver chlorlde spllLs up lnLo lLs consLlLuenL molecules
as shown ln Lq. 4 above. 1he flnely dlvlded sllver preclplLaLe acqulred
a vloleL color. Also, Lhe sllver preclplLaLe was opaque ln naLure. 1hus,
lL prevenLed furLher decomposlLlon unless Lhe soluLlon was sLeady.
1he shape of Lhe preclplLaLe was sllghLly powdery.



arLner's daLa:
hyslcal descrlpLlon CompleLeness of
preclplLaLlon
Washlngs wlLh nNO
J


hyslcal descrlpLlon
of preclplLaLe
WhlLe powder and
flne shaped crysLals
1he preclplLaLlon was
compleLed uslng 24
mL of AqNO
J

1he washlng was
successfully
compleLed.
1he preclplLaLe was
llghL purple and
powdery afLer drylng.





+.'.

values arLner's values
Sample mass !!!"#$ !!!!!!" ! !!!""# !!!!!!" !
8equlred AqNO
J
30 mL 29 mL
Mass of cruclble !"!!"#$ !!!!!!" ! !"!!""# !!!!!!" !
Cven LemperaLure n.A.* !!!!! ! !!!! !
1lme preclplLaLe ln oven n.A.* 30 mlnuLes
reclplLaLe coollng Llme n.A.* 3 mlnuLes
Mass of cruclble wlLh
preclplLaLe
!"!!"#$ !!!!!!" ! !!!!!"# !!!!!!" !
Mass preclplLaLe !!!"#! !!!!!!" ! !!!"# !!!!!!" !

*PLEASE N0TE: because the ciucible bioke piioi to placing in oven. Lab
cooiuinatoi pioviueu the ciucible with piecipitate mass to complete the
calculations anu foimal iepoit.
















+/%*"%%/$0
The aveiage value of the % !"
#
in solution is 66.7%, wheie as the tiue value is
S6.19%. Theie aie seveial ieasons why aveiage calculateu value is highei than
tiue value. Fiistly, the most significant cause of this eiioi coulu be auuition of
laige excess of $%&'( uuiing piecipitation. The piecipitate must have entiappeu
anions of weak acius fiom the solution. Thus, the mass of the piecipitate
incieaseu significantly uue to impuiities.

Seconuly, the iesult coulu be high because of impiopei washing of the
piecipitate uuiing filtiation. The anions of the weak acius might have been
piesent in the piecipitate even aftei washing. Also, uuiing the *!" test *if little
tuibiuity was obseiveu that means a small amount of $% is also accounteu foi in
the piecipitate. 0thei ieasons foi highei iesults coulu be unceitainty in weighing
salts anu measuiing volume of chemicals.


*PLEASE N0TE: because the ciucible bioke piioi to *!" test. Lab cooiuinatoi
pioviueu the ciucible with piecipitate mass to complete the calculations anu
foimal iepoit.

*$0*1"%/$0
1. The salt Sample #291 was useu foi the uiavimetiic Analysis.

2. The aveiage % Cl
-
was 66.7% anu the ieal value is S6.19%

S. The unceitainty foi weighing sample salt was !!! !!"
!!
, unceitainty foi
weighing the piecipitate is !!! !!"
!!
anu unceitainty foi oven
tempeiatuie is *N.A.

Paitnei's values foi unceitainties:

0nceitainty foi weighing sample salt = !!! ! !"
!!
, unceitainty foi
weighing piecipitate was !!! !!"
!!
anu the unceitainty foi oven
tempeiatuie was !!! !!"
!!


4. The piecision was 129 ppt

S. The ielative eiioi was 11%

Paitnei's ielative eiioi was - 26.4%




,/,1/$3#.!()
1. Aichei B.W., Buik R.C., White C.A., Wolff P.A. anu Levac S. 'uiavimetiic
Analysis of a Chloiiue Salt', CBEN 11u1: Chemistiy foi engineeis Laboiatoiy Lab
manual, Caileton 0niveisity, 0ttawa, Fall 2u1S, S4-S9.





































*PLEASE N0TE: because the ciucible bioke piioi to placing in oven. Lab
cooiuinatoi pioviueu the ciucible with piecipitate mass to complete the
calculations anu foimal iepoit.