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LEARNING OBJECTIVES

The objectives of this experiment are to ...


- to understand the titration curve for a diprotic base.
- to understand the difference between the equivalence point and end point of titration.
- to use the end point to calculate the percent of Na2CO3 in an unnown sample
of soda ash.
BACKGROUND
!odium carbonate is an important industrial chemical. "t is used in the manufacture of soap#
$lass# paper and as a source of alalinit%# that is# as a base. &bout half the sodium carbonate used
in the 'nited !tates is manufactured b% the !olva% process. "n this process# which is carried out
at ()C# carbon dioxide is bubbled throu$h a concentrated sodium chloride solution which is
saturated with ammonia. !odium h%dro$en carbonate precipitates from the solution and is
isolated*
CO2+$, - N.3+$,- .2O+l, - Na
-
+aq, - Cl
-
+aq, Na.CO3+s, - N./
-
+aq, - Cl
-
+aq,
0hen heated to 3((
o
C# the sodium h%dro$en carbonate decomposes to form sodium carbonate#
carbon dioxide# and water.
2Na.CO3 Na2CO3 - CO2 - .2O
The crude product obtained from this thermal decomposition is called soda ash# which is
primaril% Na2CO3# althou$h it also contains unreacted Na.CO3 and other impurities.
The total acid neutrali1in$ capacit% of a soda ash sample# its alalinit% value# can be stated in
terms of percent sodium carbonate. "n doin$ so# an% sodium h%dro$en carbonate present in the
sample is converted to its equivalent neutrali1in$ capacit% in terms of sodium carbonate. That is#
a 2((3 Na.CO3 sample is represented as a 4(3 Na2CO3 sample in terms of its acid
neutrali1ation capacit%. "t is not uncommon to $roup compounds of similar behavior to$ether
and state the composition in terms of one of them. 5or example# the potassium content of
fertili1er is stated as percent 62O# althou$h the potassium compounds actuall% present ma% be
phosphates# nitrates or carbonates. "n this case the relatin$ factor is the amount of potassium in a
sample of fertili1er.

Experiment
Chemistry 21
Experiment !
&N&78!"! O5 !O9& &!.
2
Carbonate ion and h%dro$en carbonate ion are both sufficientl% basic to be quantitativel%
determined b% reaction with stron$ acid in a titration procedure. The neutrali1ation of carbonate
ion proceeds in two steps*
CO3
2-
- .
-
:-; .CO3
-
+h%dro$en carbonate or bicarbonate,
and
.CO3
-
- .
-
:-; .2CO3 +carbonic acid,
Note that althou$h we t%picall% represent carbonic acid as .2CO3# in aqueous solution there is
virtuall% no .2CO3 present. To be accurate we should represent .2CO3 as CO2 - .2O. Thus# the
titration of .CO3
-
with .
-
is most accuratel% represented b% the equation*
.CO3
-
- .
-
CO2 - .2O
5or convenience# we will adopt the normal convention of representin$ carbonic acid as .2CO3 .
The titration curve shown above has two breas as evidence of the two-step neutrali1ation
process. Note that the breas are not as sharp as those obtained when a stron$ base is titrated
with a stron$ acid. The first equivalence point# occurrin$ at a p. of about <# is not as well
defined as the second# and consequentl% is not as useful for hi$hl% accurate anal%tical wor. &t
the midpoint of the first brea the principal species in solution is .CO3
-
. The second
equivalence point which corresponds to the formation of .2CO3 is more distinct and thus is more
useful for quantitative wor.
The species in solution that determine the shape of the titration curve are the products of the
stepwise titration# the h%dro$en carbonate ion and carbonic acid. =oth are wea acids with the
followin$ dissociation equilibria and dissociation constants*
.CO3
-
:-; .
-
- CO3
2-
6a2 > /.? x 2(
-22
.2CO3 :-; .
-
- .CO3
-
6a2 > /.4 x 2(
-?
Notice that the two 6a values differ b% about four orders of ma$nitude. "t is this relativel% lar$e
difference that allows us to see both equivalence points on the titration curve. =ecause .CO3
-
is
a much weaer acid than .2CO3 +or one could sa%# because CO3
2-
is a much stron$er conju$ate
2
base than .CO3
-
, nearl% all the carbonate ion in the sample will be converted to .CO3
-
+at the
first equivalence point, before the second step of the neutrali1ation be$ins formin$ .2CO3
SA"ET# $RECAUTIONS
!afet% $o$$les must be worn in the lab at all times. &n% sin contacted b% chemicals should be
washed immediatel%.
BE"ORE $ER"OR%ING T&IS E'$ERI%ENT
2. !tandardi1ed .Cl has been provided.
2. The unnown soda ash sample has also been dried for two hours at 22(
o
C.
&s stated above# althou$h soda ash is mostl% Na2CO3# it contains some Na.CO3. @iven the fact
that the two equivalence points show up on the titration curve# it should be possible to anal%1e
for the percent Na2CO3 in the sample b% usin$ the first equivalence point +the reaction is
CO3
2-
- .
-
.CO3
-
,. "n $oin$ from the first to the second equivalence point the h%dro$en
carbonate reacts to form carbonic acid +.CO3
-
- .
-
.2CO3,. There are two sources of .CO3
-
*
the .CO3
-
formed from the CO3
2-
in the first step of the titration and the .CO3
-
from an%
Na.CO3 present in the ori$inal sample. "n principle we can calculate the amount of .CO3
-

formed from the CO3
2-
b% nowin$ the moles of .
-
required to reach the first equivalence point.
=% subtractin$ this amount of .CO3
-
from the total .CO3
-
determined in the second step of the
titration we could then calculate the amount of .CO3
-
ori$inall% present in the sample.
.owever# we cannot carr% out these calculations ver% accuratel% because the first equivalence
point is not ver% distinct. That is# because the p. chan$e at the first equivalence point is not ver%
dramatic# we have trouble accuratel% specif%in$ the exact volume of acid required to reach the
first equivalence point. To avoid this problem we will use the more distinct second equivalence
point and report the acid neutrali1in$ abilit% of the soda ash sample in terms of percent Na2CO3
+even thou$h a small part of the neutrali1in$ abilit% of the sample reall% comes from Na.CO3,.
"n other words we will assume that the number of moles of Na2CO3 in the soda ash sample
equals one-half the number of moles of stron$ acid required to reach the second equivalence
point.
&lthou$h less precise# acidAbase indicators can be used to measure p.. "nstead of measurin$ the
p. and determinin$ the equivalence point# we can use acidAbase indicators and determine the end
point of a titration where the indicators chan$e color. These are a $roup of wea acids and bases
that are hi$hl% colored or$anic d%es. Their chan$e in color depends on the p. and serves as the
end point of a titration# provided that their chan$e in color occurs at the equivalence point of the
titration. 0e will use phenolphthalein# to detect the first end point. Bhenolphthalein is pin
above p. 2(.( and colorless below p. <.3 and this chan$e occurs at the first equivalence point.
Ceth%l oran$e will be used to detect the second end point. Ceth%l oran$e is %ellow above p.
/./ and red below p. 3.2.
3
E'$ERI%ENTAL $ROCEDURE
Titr(ti)n )* (n Un+n),n S)-( Ash S(mp.e
2. =oil distilled water to expel an% dissolved carbon dioxide. Cool to room temperature.
9issolve approximatel% (.2( $ +record the exact mass, of the unnown soda ash in about
<( m7 of boiled# distilled water. Brepare several more samples in the same manner.
2. &dd three drops each of phenolphthalein and meth%l oran$e to the soda ash sample. The
solution should be pin.
3. &dd a drop each of phenolphthalein and meth%l oran$e to a 2( m7 sample of p. < buffer.
Bhenolphthalein is colorless and meth%l oran$e is %ellow at p. <. This is the color of the
solution at the first end point.
/. &dd a drop each of phenolphthalein and meth%l oran$e to a 2( m7 sample of p. / buffer.
Bhenolphthalein is colorless and meth%l oran$e is oran$e at p. /. This is the color of the
solution at the second end point.
4. The first titration is done to determine the two end points. !tart recordin$ the volume of
.Cl added and the color chan$e. Bin color will $raduall% turn to oran$e. &t the first end
point# phenolphthalein will become colorless and the sample will chan$e from oran$e to
%ellow close to the color in p. < buffer. Continue addin$ .Cl from the buret at re$ular
intervals until the color of the meth%l oran$e indicator chan$es from %ellow to oran$e
close to the color in p. / buffer. Cae sure to reduce volume additions when %ou start
seein$ more rapid color chan$e. Decord this data in Excel.
F. Depeat procedure on the next sample. 8ou ma% immediatel% titrate to the 2
nd
end point.
?. Bart of %our score will be based on the precision and accurac% of the measurements %ou
mae. 0ithin 43 3 error# %ou will receive 4 /)n0s points. 4 points will be deducted if
%ou have 3error lar$er than 2(3. "f it appears %ou do not have a hi$h de$ree of precision
%ou ma% want to consider performin$ more trials +assumin$ some soda ash remains,.
DATA ANAL#SIS
Determin(ti)n )* the per1ent N(2CO in the Un+n),n S)-( Ash S(mp.e
Calculate the percent Na2CO3 in each unnown soda ash sample and obtain the avera$e value
from the anal%ses. 8ou ma% want to set up an Excel spreadsheet beforehand.
Coles of Na2CO3 in sample
>
used .Cl of moles
2
2

>
7 in .Cl of Golume .Cl of Colarit%
2
2

Cass of Na2CO3 in sample > Coles of Na2CO3 in sample Colar mass of Na2CO3
3 Na2CO3 in sample > 2((
ash soda of mass "nitial
sample in CO Na of Cass
3 2

/
5or example# assume %ou have dissolved (.24( $ sample of soda ash into <( m7 of deioni1ed
water. "t too 23.2 m7 of (.2(( C .Cl to titrate the solution to the second equivalence point.
To calculate the 3 Na2CO3 in the soda ash sample*
Coles of Na2CO3 in sample
>
used .Cl of moles
2
2

>
mole (.(((FF( (.(2327 C 2(( . (
2
2
=
Cass of Na2CO3 in sample > (.(((FF( mole 2(4.H<</ $Amole > (.(?(( $
3 Na2CO3 in sample >
3 ( . 2< 2((
$ (.24(
$ (.(?((
=
4
ANAL#SIS O" SODA AS&
D(t( Sheet
%).(rity )* the st(n-(r-i2e- &C. 333333333%
An(.ysis )* Un+n),n S)-( Ash
'nnown "dentification I JJJJJJJJJ
Color Chan$e at the 2
st
End Boint > JJJJJJJJJJtoJJJJJJJJJJJJ
Color Chan$e at the 2
nd
End point > JJJJJJJJJJtoJJJJJJJJJJJJ
Trial 2 Trial 2 Trial 3 Trial / Trial 4
"nitial mass of soda ash +$,
Golume of titrant +.C7,
added. +2
nd
End Boint,
+m7,
Coles of Na2CO3 in sample +mole,
Cass of Na2CO3 in sample +$,
3 Na2CO3 in sample +3,
&vera$e Bercent Na2CO3 JJJJJJJJJJJJ
&ctual Bercent Na2CO3 JJJJJJJJJJJJ +instructor use onl%,
3error JJJJJJJJJJJJJ +instructor use onl%,
F
&nal%sis of !oda &sh
Bre 7aborator% &ssi$nment
NameJJJJJJJJJJJJJJJJJJJJJJJJ
!ectionJJJJJJJJJJJJJJJJJJJJJJJ
9ateJJJJJJJJJJJJJJJJJJJJJJJJJ
2. 0rite an outline of the procedure for this experiment.
2. "n one experiment# %ou have dissolved (.2H< $ of soda ash into <( m7 of deioni1ed water.
"t too 2H.< m7 of (.(HH< C .Cl to titrate the solution to the second equivalence point.
0hat is the percent Na2CO3 in the soda ashK !how %our wor.
3. 9istin$uish between the equivalence point of a titration and the end point of a titration.
?

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