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EXPERIMENT 1: GRAVIMETRY
GRAVIMETRIC ANALYSIS OF A CHLORIDE SALT
OBJECTIVE:
To illustrate typical techniues use! in gra"imetric analysis by uantitati"ely !etermining the
amount o# chlori!e in an un$no%n&
APPARATUS:
2'0(mL) 100 mL bea$ers Bunsen burner %eighing paper
#ilter paper "acuum a!apter "acuum tubing
#ilter #las$ "acuum pump #unnel support
glass #unnel %ash bottle stirring ro!s
*ing stan!) ring) + gau,e %ire Buchner #unnel
CHEMICALS-
0&' g o# un$no%n chlori!e sample
0&2' . Ag/0
3
1&0 . 2/0
3
acetone
!istille! %ater
INTRODUCTION:
3uantitati"e analysis is that aspect o# analytical chemistry that is concerne! %ith !etermining
ho% much o# one or more constituents are present in a particular sample o# material& T%o
common metho!s use! in analytical chemistry are gra"imetric an! "olumetric analysis&
4ra"imetric analysis !eri"es its name #rom the #act that the constituents being !etermine! can
be isolate! in some %eighable #orm& 5olumetric analysis) on the other han!) !eri"es its name
#rom the #act that the metho! use! to !etermine the amount o# a constituent in"ol"es
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measuring the "olume o# a reagent& 6sually) gra"imetric analysis in"ol"es the #ollo%ing
steps-
1& 7rying an! then accurately %eighing representati"e samples o# the material to be
analy,e!&
2& 7issol"ing the sample in an appropriate sol"ent
3& Precipitating the analyte in the #orm o# a substance o# $no%n composition by a!!ing a
suitable reagent&
8& 9solating the precipitate by #iltration&
'& :ashing the precipitate to #ree it #rom contamination&
1& 7rying the precipitate to a constant %eight&
7& Calculating the %eights an! the percentage o# the sample an! precipitate&
Chlori!e ion may be uantitati"ely precipitate! #rom solution by the a!!ition o# sil"er ion
accor!ing to the #ollo%ing ionic euation-
Ag
;
<a= ; Cl
(
<a= > AgCl <s= <1=
Sil"er chlori!e is uite insoluble <?0&0001 g o# AgCl !issol"es in 100 mL o# 2
2
0 at 20
o
C=@
there#ore) the a!!ition o# sil"er nitrate solution to an aueous solution containing chlori!e ion
precipitates AgCl uantitati"ely& The precipitate can be collecte! on a #ilter paper) !rie!) an!
%eighte!& Arom the %eight o# the AgCl obtaine!) the amount o# chlori!e in the original
sample can then be calculate!&
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This eBperiment also illustrates the concept o# stoichiometry& Stoichiometry is the
!etermination o# the proportions in %hich chemical elements combine an! the %eight
relations in any chemical reaction& 9n this eBperiment stoichiometry means speci#ically the
mole ratio o# the substance entering into an! resulting #rom the combination o# Ag
;
an! Cl
(
&
9n the reaction o# Ag; an! Cl( in euation <1=) it can be seen that 1 mole o# chlori!e ions
reacts %ith 1 mole o# sil"er ions to pro!uce 1 mole o# sil"er chlori!e&
PROCEDURE:
A. Mass by sub!a"#$%:
1& 6sing a %eighing paper %eigh about 0&1 to 0&2 g o# your un$no%n sample on a top
loa!ing balance& <remember to tare the paper mass=
2& Trans#er the sample #rom the paper into a %eighing bottle an! %eigh it accurately&
3& A#ter trans#erring the sample #rom the %eighing bottle care#ully into a clean 2'0 mL
bea$er) %eighs the empty bottle alone accurately&
B. P!&"#'#a#$%:
1& Label the bea$er C1& A!! bet%een 1'0 mL o# !istille! %ater an! 1 mL o# 1 . 2/0
3
to
the bea$er&
2& *epeat %ith sample numbers 2 an! 3 an! label the bea$ers 2 an! 3) respecti"ely& Stir each
o# the solutions %ith three !i##erent glass stirring ro!s until the entire sample has
!issol"e!& Lea"e the stirring ro!s in the bea$ers&
3& :hile stirring one o# the solutions) a!! to it about 20 mL o# 0&2' . Ag/0
3
solution
slo%ly in !rops& Place a %atch glass o"er the bea$er&
8& Co"er the bea$ers an! %atch glasses %ith #oil $ '!$&" (!$) *#+,-.
'& :arm the solutions +&%*y %ith your hot plate an! $eep it %arm #or approBimately 30
minutes& D$ %$ b$#* ,& s$*u#$%.
C. F#*!a#$%:
1& 0btain a #ilter paper <three o# these %ill be nee!e!=&
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2& Alute the #ilter paper then #it it into the #unnel.
3& Be certain you mass the paper accurately a#ter it has been #ol!e! an! torn) not be#ore&
8& Ait it into a glass #unnel& Be certain that you open the #ilter paper in the #unnel so that one
si!e has three pieces an! one si!e has one piece o# paper against the #unnel((not t%o
pieces on each si!e&
'& :et the paper %ith !istille! %ater to hol! it in place in the #unnel& Completely an!
uantitati"ely trans#er the precipitate an! all the %arm solution #rom the bea$er onto the
#ilter using a rubber policeman an! a %ash bottle to %ash out the last traces o# precipitate&
The le"el o# solution in the #ilter #unnel shoul! al%ays be belo% the top e!ge o# the #ilter
paper& :ash the precipitate on the #ilter paper %ith t%o or three ' mL portions o# %ater
#rom the %ash bottle&
<Check for completeness of precipitation by adding a few drops of the AgNO
3
solution to the
clear filtrate. If it clouds you must re-filter&=
1& Ainally) pour three ' mL portions o# a"&$%& through the #ilter&
/EEP THE ACETONE A0AY FROM OPEN FLAMES BECAUSE IT IS HIGHLY
FLAMMABLE.
7& *emo"e the #ilter paper@ place it on a numbere! %atch glass@ an! store it in your loc$er
until the neBt perio!&
D& *epeat the abo"e processes %ith your other t%o samples) being sure that you ha"e
numbere! your %atch classes so that you can i!enti#y the samples&
E& /eBt) %hen the AgCl is thoroughly !ry) %eigh the #ilter papers plus AgCl an! calculate
the %eight o# AgCl&
10& Arom the !ata obtaine!) "a*"u*a&:
i= .ass o# chlori!e in original sample)
ii= Percentage o# chlori!e in your original sample)
iii= A"erage percent chlori!e) stan!ar! !e"iation an! relati"e stan!ar! !e"iation&
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RESULTS SHEET
Trial 1 Trial 2 Trial 3
.ass o# %eighing bottle) g
.ass o# %eighing bottle
; sample) g
.ass o# sample) g
.ass o# #ilter paper) g
.ass o# #ilter paper ; AgCl) g
.ass o# AgCl) g
.ole o# Cl
(
.ass o# Cl
(
) g
F o# Cl
(
A"erage o# F o# Cl
(

Stan!ar! !e"iation
1UESTIONS:
1& Aluminum metal reacts %ith !ilute sul#uric aci! to pro!uce aluminum sul#ate an!
hy!rogen gas& :hat %eight o# aluminum %ill react %ith 7&D'8 g o# sul#uric aci!G
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2& A 2&'100 g sample o# a sul#ur(containing compoun! is analy,e! by precipitating the
sul#ur as barium sul#ate& 9# 1&17'1 g o# BaS0
8
is #orme!) %hat is the percentage o# sul#ur
in the sampleG