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15.

Determination of H
3
PO
4
or citric acid using volumetric and pH-metric
titrations
Titration of the polyproton acids, for example phosphoric acid H3PO4 or citric is not trivial. Although
often listed together with strong mineral acids hydrochloric, nitric and sulfuric!, the phosphoric acid
is relatively wea", with p#a$%&.$', p#a&%(.&) and p#a3%$&.3'. That means titration curve contains
only two inflection points and phosphoric acid can *e titrated either as a monoprotic acid or as a
diprotic acid. +n the first case acid has to *e titrated against indicator changing color around pH 4.(
for example ,romocresol -reen or .ethyl Orange!, in the second case / against indicator changing
color around pH 0.1' for example Thymolphthalein!. Phenolphthalein should not *e used, as it
starts to change color around pH 2.&, when phosphoric acid is titrated in a*out 0'3.
+f the sample is pepsi, one cannot
titrate it classically using dyes as
indicators, procedure no. $ *elow!. 4or
pehametric titration of pepsi using
).$. 5aOH, student should measure
exactly ') m6 of this *everage to a
*ea"er, degas it mixing vigorously few
minutes, add water to the total volume
$') m6 of and then titrate procedure
&!.
Titration curve calculated for 0.1M solution of phosphoric acid titrated with 0.1M solution of strong
base.
As explained a*ove, during titration of phosphoric acid can *e used either .ethyl Orange or
,romocresol -reen and detect first end point around pH 4.(, or Thymolphthalein and detect second
end point around pH 0.1. 7ecision which indicator should *e used can *e *ased on the approximate
concentration of phosphoric acid and titrant and on personal preferences / some find it easier to
detect change of the .ethyl Orange from red to yellow or ,romocresol -reen from yellow to *lue
color than the appearance of a *lue hue of Thymolphthalein. 8e will however use *oth the end
points pH 4.( and 0.1!9 the results of them will *e averaged : see *elow.
7ifferent case is citric acid HOO;/;H&/;OH!;OOH!/;H&/;OOH!, with p#a$%3.$', p#a&%4.(( and
p#a3%1.4). Here, the titration curve exhi*its only one inflection, at pH%0.&'.
+f the sample is citron <uice, measure
exactly 4 m6 of it to a *ea"er, add water
to the total volume $') m6 and then
titrate procedure &!.
+t is clear that for citric acid one should
use Thymolphthalein the reasons are the
same as for H3PO4!, *ut here the third
inflection is detected, influencing the
stoichiometry factor, here e=ual to three,
used in calculation of the final result.
Titration curve calculated for 0.1M solution of citric acid titrated with 0.1M solution of strong base
4aculty of ;hemistry, >niversity of 8roc?aw, Analytical ;hemistry 7ept., =uantitative analysis. Tas" $' / p. $
Thus, the classical volumetric titration of polyproton acids re=uires first determination of the titration
curve, to "now the stoichiometry of the neutrali@ation reaction. The curve can *e easily determined
*y titrating a sample of acid using strong *ase and simultaneous measurement of pH. One has to
note the volume of titrant added together with respective value of pH as read on the device.
AB
Procedure $ volumetric titration!
$. 7ilute the sample in the volumetric flas" to the mar" with distilled water and sha"e carefully.
&. Pipette &) lu* &' m6 H3PO4 sample from teacher! or ') m6 pepsi! or 4 m6 citron <uice! into
Crlenmayer flas".
3. 7ilute with distilled water to $') m6 total volume.
4. only if sample is pure H3PO4!D Add &/4 drops of ,romocresol -reen preferred! or .ethyl
Orange and titrate with 5aOH solution till the color change completely from yellow to *lue red to
yellow with .ethyl Orange!. 5ote the volume of titrant. Eepeat points &/4. ;alculate the average
titrant volume.
'. *oth acids! Perform ps. &/4 two or three times, *ut using Thymolphthalein and titrating till the
*lue color appears.
Eesult calculation
7epending on the indicator used reaction isD
either H3PO4F5aOHG5aH&PO4FH&O or H3PO4F&5aOHG5a&HPO4F&H&O
However, for citric acid only the following reaction is useful in =uantitative analysisD
;3H'O;OOH!3F35aOHG ;3H'O;OO5a!3F3H&O
;onse=uently, the stoichiometric ratio of sodium hydroxide and phosphoric acid is either $D$ or &D$,
*ut that for citric acid is 3D$..
;alculate the mass of phosphoric acid in the initial sample independently for these two series and,
finally, calculate the arithmetic average of these two results. +f the sample contains citric acid, s"ip
point 4 and calculate the results from the mean of &/3 titrations using Thymolphthalein only.
Procedure & pH/metric titration !
AttentionD this part can *e performed simultaneously with procedure $ or separately.
$. 7ilute the sample in your volumetric flas" to the mar" with distilled water and sha"e carefully.
&. Pipette &) lu* &' m6 H3PO4 sample from teacher! or ') m6 pepsi! or 4 m6 citron <uice! into
Crlenmayer flas".
3. 7ilute with distilled water to $') m6 total volume.
4. Place the *ea"er on magnetic stirrer, insert the magnet in it, as well as pH/electrode. As" the
assistant to control the correctness of the installation and some advices.
'. .easure and note pH. Eepeat this adding small portions of the titrant *ase few drops each!,
noting also the actual volume of titrant added total!. 4inish titration when pH exceeds ca. $&.
Processing the results
>sing a computer data/sheet, plot the titration curve o*tained and determine as exactly as possi*le
the volume of titrant corresponding to the inflection points two for phosphoric acid, one for citric
acid!. ;alculate the respective contents of acids in the initial sample, independently for every
inflection.
For more aspiring studentsD The preciseness of determination of the inflection point can *e very
improved if calculating the second derivative of the titration curve. As" your teacher for details if
want to try this procedure.
ECPOETD should contain all the results o*tained the titration curves +n form of plots only! and a
short interpretation.
HourcesD 8i"ipedia, httpDBBwww.titrations.infoBacid/*ase/titration/phosphoric/acid &)$&/)&/$)! and others, also
text*oo"s.
AB 4or EeaderIs informationD the curves shown here in 4igures were calculated using the following formulaD
4aculty of ;hemistry, >niversity of 8roc?aw, Analytical ;hemistry 7ept., =uantitative analysis. Tas" $' / p. &
( )
5 3 4 2 3 2 3 2
0 a a1 a1 a a1 a2 a1 a 2 a a1 a2 a3 a1 a 2 a3 w a1 w a1 a2 w a1 a 2 a3 w
titr 2 3 2
titr w a1 a1 a2 a1 a2 a3
v [H ] c [H ] K [H ] K 2 c [H ] K K [H ] K K 3 c [H ]K K K [H ] K K K [H ] K [H ] K K [H ]K K K K K K K
v
(c [H ] [H ] K )([H ] [H ] K [H ]K K K K K )
+ + + + + + + + + +
+ + + + +
+ + +
=
+ + + +

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