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ACID-BASE TITRATION

1. Objectives
a. Prepare acid standard solution
b. Determine the normality of the acid/base using a standard solution
c. Determine the equivalence point using titration curve

2. Basic of theory
Acid-Base Titration
In a titration, the concentration of one solution is determined by
quantitatively observing its reaction with a solution of known
concentration. The solution of known concentration is called a standard
solution. The aim of a titration is to find the point at which the number of
moles of the standard solution is stoichiometrically equal to the original
number of moles of the unknown solution. This point is referred to as the
equivalence point. At the equivalence point, all the moles of hydrogen ions
that were present in the original volume of one solution have reacted with
an equal number of moles of hydroxide ions from the other solution.
Precise volume measurements are needed when you perform a titration.
Chemists use special glass apparatus (burette) to collect these
measurements. As well, an acid-base indicator is needed to monitor
changes in pH during the titration. A transfer pipette (bottom) measures a
fixed volume of liquid, such as 10.00 mL, 25.00 mL, or 50.0 mL. A
burette (top) measures a variable volume of liquid. In a titration, a pipette
is used to measure a precise volume of standard solution into a flask. The
flask sits under a burette that contains the solution of unknown
concentration. After adding a few drops of indicator, you take an initial
burette reading. Then you start adding the known solution, slowly, to the
flask. The end-point of the titration occurs when the indicator changes
colour. The indicator is chosen so that it matches its equivalance point.

Titration Step by Step
Rinsing the Pipette
A pipette is used to measure and transfer a precise volume of liquid. You
rinse a pipette with the solution whose volume you are measuring. This
ensures that any drops that remain inside the pipette will form part of the
measured volume.
1. Pour a sample of standard solution into a clean, dry beaker.
2. Place the pipette tip in a beaker of distilled water. Squeeze the suction
bulb. Maintain your grip while placing it over the stem of the pipette.
(If your suction bulbs have valves, your teacher will show you how to
use them.)
3. Relax your grip on the bulb to draw up a small volume of distilled
water.
4. Remove the bulb and discard the water by letting it drain out.
5. Rinse the pipette by drawing several millilitres of solution from the
beaker into it.
6. Rotate and rock the pipette to coat the inner surface with solution.
Discard the rinse.
7. Rinse the pipette twice in this way. It is now ready to fill with standard
solution.

Filling the Pipette
1. Place the tip of the pipette below the surface of the solution.
2. Hold the suction bulb loosely on the end of the glass stem. Use the
suction bulb to draw liquid up just past the etched volume mark.
3. As quickly and smoothly as you can, slide the bulb off and place your
index finger over the end of the glass stem.
4. Gently roll your finger slightly away from end of the stem to let
solution drain slowly out.
5. When the bottom of the meniscus aligns with the etched mark, press
your finger back over the end of the stem. This will prevent more
solution from draining out.
6. Touch the tip of the pipette to the side of the beaker to remove any
clinging drop. The measured volume inside the pipette is now ready to
transfer to an Erlenmeyer flask or a volumetric flask.

Transferring the Solution
1. Place the tip of the pipette against the inside glass wall of the flask. Let
the solution drain slowly, by removing your finger from the stem.
2. After the solution drains, wait several seconds, then touch the tip to the
inside wall of the flask to remove any drop on the end. Note: You may
notice a small amount of liquid remaining in the tip. The pipette was
calibrated to retain this amount. Do not try to remove it.

Adding the Indicator
1. Add two or three drops of indicator to the flask and its contents. Do not
add too much indicator. Using more does not make the colour change
easier to see. Also, indicators are usually weak acids. Too much can
change the amount of base needed for neutralization. You are now
ready to prepare the apparatus for the titration.



Rinsing the Burette
burette is used to accurately measure the volume of liquid added during a
titration experiment. It is a graduated glass tube with a tap at one end.
1. To rinse the burette, close the tap and add about 10 mL of distilled
water from a wash bottle.
2. Tip the burette to one side and roll it gently back and forth so that the
water comes in contact with all inner surfaces.
3. Hold the burette over a sink. Open the tap, and let the water drain out.
While you do this, check that the tap does not leak. Make sure that it
turns smoothly and easily.
4. Rinse the burette with 5 mL to 10 mL of the solution that will be
measured. Remember to open the tap to rinse the lower portion of the
burette. Rinse the burette twice, discarding the liquid each time.

Filling the Burette
1. Assemble a retort stand and burette clamp to hold the burette. Place a
funnel in the top of the burette.
2. With the tap closed, add solution until the liquid is above the zero mark.
Remove the funnel. Carefully open the tap. Drain the liquid into a
beaker until the bottom of the meniscus is at or below the zero mark.
3. Touch the tip of the burette against the beaker to remove any clinging
drop. Check that the portion of the burette that is below the tap is filled
with liquid and contains no air bubbles.
4. Record the initial burette reading in your notebook.
5. Replace the beaker with the Erlenmeyer flask that you prepared earlier.
Place a sheet of white paper under the Erlenmeyer to help you see the
indicator colour change that will occur near the end-point.

Reading the Burette
1. A meniscus reader is a small white card with a thick black line on it.
Hold the card behind the burette, with the black line just under the
meniscus. Record the volume added from the burette to the nearest 0.05
mL.
(McGraw-Hill Reyerson. 1996. Chemistry 11.pdf)

Calculation of [H
+
] in the titration of a strong acid with a strong base or
vice versa strong base with a strong acid is not difficult at all. This
calculation can be done with dividing the number of moles of acid (or
base) who lived with the volume of the solution. Calculation will be more
complicated when the combination of a weak acid and a strong base, or
involving strong acid and weak base. [H
+
] will depend not only on the
acidic or basic living, but also hydrolysis of the salt formed. Plots of [ H
+
]
or pH vs . the amount of acid or base added is called a titration curve. Let
us describe the titration curve when the initial volume of acid Va , MA
acid concentration , and Vb base added volume and concentration is MB.

A. TITRATION BETWEEN STRONG ACID AND STRONG BASE
1. Before the equivalence point :
Since the dissociation of water can be abandoned , the number of moles
of H
+
is equal to the amount of residual acid living
[ H
+
] = ( MaVa - MbVB ) / ( Va + Vb )

2. At the equivalence point :
Dissociation of water can not be ignored here .
[ H
+
] = Kw = 10
-7


3. After the equivalence point :
The number of moles of excess base is equal to the number of moles of
hydroxide ions. [ OH
-
] can be obtained by dividing the number of
moles by the volume of solution . [ OH
-
] obtained is converted into
[H
+
] .

[ OH
-
] = ( MbVb - MaVa ) / ( Va + Vb )

[ H
+
] = Kw / [ OH
-
] = ( Va + Vb ) Kw / ( MbVb - MaVa )

Symmetric curve near the equivalence point because Vb Va .10 x 10
-
3
dm
3
titration of a strong acid , for example HCl 0.1 mol dm
- 3
with a
strong base , for example NaOH 0.1 mol dm
- 3
resulted in a typical
titration curve. On early stage ,slow pH changes . PH changes rapidly
near the equivalence point ( Vb = 10x10
- 3
dm
3
). Near the equivalence
point, the pH changed only by the addition of multiple units a few drops
of bases

B. TITRATION BETWEEN WEAK ACID AND STRONG BASE
The result would be different if a weak acid is titrated with a strong
base. Titration of 10 x 10
-3
dm
3
acid acetate 0.1 mol dm
- 3
with NaOH
0.1 mol dm
3
is a typical example.
1. The starting point : Vb = 0. pH in the early stages is greater than in
the previous case.
[ H + ] = MA
is the dissociation constant of acetic acid .
2. Before the equivalence point : until the equivalence point , the pH
change is rather slow .
3. At the equivalence point ( Vb = 10 x 10
-3
dm
3
) : at this point the
only sodium acetate CH
3
COONa there . [ H
+
] can be obtained in a
similar way to when we discuss the hydrolysis salt
4. After the equivalence point, [H
+
] is determined by the concentration
of NaOH, not by CH
3
COONa. pH changes slowly before the
equivalence point is the result of the buffer. Before the equivalence
point, there is a solution of sodium acetate ( salt of weak acid and
strong base ) and acetic acid ( a weak acid ) . Due to the presence of
sodium acetate , sodium equilibrium dissociation acetate

CH
3
COOH H
+
+ CH
3
COO
-

shifted to the left , and [ H
+
] will decrease .

As the approach of [ CH3COO - ] = c
S
[ HA ] c
0
.
c
S
is the concentration of salt , then

[ H
+
] c
S
/ c
0
= Ka , [ H
+
] = ( c
0
/c
S
) Ka
When acid is added to this solution , the equilibrium will shift to the
left because there is an acetate ions will be neutralized acid added .

CH
3
COOH H
+
+ CH
3
COO
-

Conversely, when a base is added , the acetic acid solution will
neutralized.
So, CH3COOH + OH - H2O + CH3COO -
[ H + ] is almost unchanged
(Yashito Taekuchi. 2006. Buku Teks Pengantar Kimia terjemahan.
Tokyo : Iwanami Shoten.)

Titration is a method for determining the concentration of acid or base by
the used of standard solutions. Standard solution can be either acid or base
of known concentration carefully. Standard solution of acid is needed to
establish the concentration of base and base standard solution is needed to
determine the concentration of the acid. State with the same amount of
acid equivalent to the number of equivalents of base is called the
equivalence point. The pH changes during the titration and the titration is
terminated when the pH of the equivalence point has been reached.
To determine the equivalence point, the indicators that have used stretch
change in pH of the equivalence point included. Very difficult to
determine exactly at the end of the titration equivalence point, because the
indicator is not only a color change at the equivalence point alone, but
rather in the area called stretch change color. Therefore, usually titration is
terminated at a particular pH called end point titration.
For titration of strong acid-strong base, the equivalent point occurs at pH =
7 so used indicators that have a pH from 6.0 to 7.6 as Bromkresil Blue. For
titration of weak acid-strong base, the equivalent is more than 7 points so
used indicators that have a pH from 8.2 to 10.0 as Penolptalein. A graph
obtained from the titration is called titration curve.
(Kasmadi . 2012 . Kimia Dasar II . Semarang: Unnes press)

3. Apparatus and Reagent
Analytical Balance
Volumetric Flask 100
mL
Erlenmeyer 100 mL
Buret 50 mL
Stative and clamps
Volumetric pipet 10
mL
pH meter
Oxalic acid crystals
Distilled water
NaOH 0,2 M and 0,1
M solution
HCl 0,1 M solution
CH
3
COOH 0,1 M
solution
PP indicators

4. Procedure























5. Observation
a. Mass of Oxalic acid = 1,2607 gram
Volume of solution = 100 mL
Molarity of Oxalic acid = 0,1 M
Normality of Oxalic acid = 0,2 M

b. Volume of Oxalic acid = 10 mL
Volume of NaOH(1) = 18,7 mL
Volume of NaOH(2) = 21,4 mL
Average volume of NaOH = 20,05 mL

c. Volume of HCl = 10 mL
Volume of NaOH(1) = 10,2 mL
Volume of NaOH(2) = 10,4 mL
Average volume of NaOH = 10,3 mL

d. Relationship of the volume of titrant with pH in acid-base titration
No
Volume of
NaOH added to
10 mL of 0,1M
HCl
pH
1 0 1
2 1 1
3 2 1
4 3 1
5 4 3
6 5 10
7 6 10
8 7 10
9 8 10
10 9 10
11 10 10
12 11 10
13 12 10
14 13 10
15 14 10

No
Volume of NaOH
added to 10 mL of
0,1M CH
3
COOH
pH
1 0 3
2 1 3
3 2 3
4 3 3
5 4 4
6 5 4
7 6 5
8 7 6
9 8 6
10 9 8
11 10 10
12 11 10
13 12 10
14 13 10
15 14 10

6. Data Count
a. Preparaation of primary standard solution of H
2
C
2
O
4
(COOH)
2
.
2
H
2
O
mass of Oxalic acid: 1,2607 gram
Mr of Oxalic acid: 126,07
Volume of solution: 100 mL = 0,1 L
n(COOH)
2
= 2
M =



=



= 0,1 M

N = M . n
= 0,1 . 2
= 0,2 N

b. Determine the concentration of NaOH
n(COOH)
2
= 2
n(NaOH) = 1
M (COOH)
2
= 0,1 M
V (COOH)
2
= 10 mL
V NaOH = 20,05 mL

n(COOH)
2
. M(HCl) . V(COOH)
2
= n(NaOH) . M(NaOH) . V(NaOH)
2 . 0,1 . 10 = 1 . M(NaOH) . 20,05
M(NaOH) =


M(NaOH) = 0,09 M

N(NaOH) = M(NaOH) . n(NaOH)
= 0,09 . 1
= 0,09 N

c. Determination of the concentration of HCl using secondary standard
solution of NaOH
n(HCl) = 1
n(NaOH) = 1
M NaOH = 0,09 M
V HCl = 10 mL
V NaOH = 10,3 mL

n(HCl) . M(HCl) . V(HCl)

= n(NaOH) . M(NaOH) . V(NaOH)
1 . M(HCl) . 10 = 1 . 0,09 . 10,3
M(HCl) =


M(HCl) = 0,0927 M

N(HCl) = M(HCl) . n(HCl)
= 0,0927 . 1
= 0,0927 N
7. Discussion
a. In this experiments, we make of standard solution of oxalic acid
crystals that have Mr = 126.07 and the mass is 1.2607 grams dissolved
in distilled water in the measuring flask to 100 mL. From the
experiment, we obtained the molarity is 0.1 M and the normality is 0.2
N, where the normality obtained from the formula:
M (Oxalic acid) x Valence of oxalic acid
b. Molarity of NaOH required to determine a primary standard solution
of oxalic acid of known concentration is 0.1 M. Solution of oxalic acid
is titrated with NaOH until the color changes to bright pink and stop
the titration process. From here obtained average volume of NaOH
solution is 20,05 mL. This volume then used to determine the molarity
of the NaOH solution formula:
n . M
H2C2O4
. V = n . M
NaOH
. V
from the formula, obtained M
NaOH
is 0,09 M and the Normality is 0,09
N
c. In this experiment, Oxalic acid was replaced with 10 ml of HCl. This
experiment was not different from the previous experiment. Titrating
until the color changes to bright pink and stop the titration after a
change of color. From the observations, obtained the average volume
of NaOH is 10,3 mL. Then, we can determine the Molarity of HCl
from the formula:
n . M
HCl
. V

= n . M
NaOH
. V
from the formula, obtained M
Hcl
is 0,0927 M and the Normality is
0,0927 N
d. In make titration curve is done trhough 2 tricks which is measure pH
with universal indicator and by use of count. By use of our universal
indicator cant know definitely gets what the pH because of range it
just of 1 until 10 only. Then of arithmethic pH we can acuurate lessing
in determine pH of solution. On linking that does to be gotten
equivalence dot to titration among strong acid and strong base is 7,
while pH of titration between weak acid and strong base is more than 7
which is 10

8. Conclusion
a. acid-base titrations are based on acid-base neutralization reaction
b. Primary standard solution is a solution of known concentration as a
determinant of the concentration of another solution. Secondary
standard solution is a solution of known concentration determined by
the concentration of the primary standard solution.
c. Equivalence point is the condition in which the analyte (solution
which exist in erlenmeyer) reacts with the titrant (solution which exist
in the burette)
d. The normality of (COOH)
2
= 0,2 N, The normality of NaOH = 0,09 N
and The normality of HCl = 0,0927 N

9. Suggestion
a. We must known the material of the experiment before doing the
experiment.
b. Carefully when doing the titration experiment to determine the
equivalence point.
c. Carefully when using the apparatus and reagent.

10. Reference
Team of Basic Chemistry. 2014. Manual Labwork Basic chemistry.
Semarang: Universitas negeri semarang.
Yashito Taekuchi. 2006. Buku Teks Pengantar Kimia terjemahan. Tokyo :
Iwanami Shoten.
McGraw-Hill Reyerson. 1996. Chemistry 11.pdf.
Kasmadi. 2012. Kimia Dasar II. Semarang: Unnes press

11. Answer
1. Preparaation of primary standard solution of H
2
C
2
O
4
(COOH)
2
.
2
H
2
O
mass of Oxalic acid: 1,2607 gram
Mr of Oxalic acid: 126,07
Volume of solution: 100 mL = 0,1 L
n(COOH)
2
= 2
M =



=



= 0,1 M

N = M . n
= 0,1 . 2
= 0,2 N

2. Determine the concentration of NaOH
n(COOH)
2
= 2
n(NaOH) = 1
M (COOH)
2
= 0,1 M
V (COOH)
2
= 10 mL
V NaOH = 20,05 mL

n(COOH)
2
. M(HCl) . V(COOH)
2
= n(NaOH) . M(NaOH) . V(NaOH)
2 . 0,1 . 10 = 1 . M(NaOH) . 20,05
M(NaOH) =


M(NaOH) = 0,09 M

N(NaOH) = M(NaOH) . n(NaOH)
= 0,09 . 1
= 0,09 N

3. Determination of the concentration of HCl using secondary standard
solution of NaOH
n(HCl) = 1
n(NaOH) = 1
M NaOH = 0,09 M
V HCl = 10 mL
V NaOH = 10,3 mL

n(HCl) . M(HCl) . V(HCl)

= n(NaOH) . M(NaOH) . V(NaOH)
1 . M(HCl) . 10 = 1 . 0,09 . 10,3
M(HCl) =


M(HCl) = 0,0927 M

N(HCl) = M(HCl) . n(HCl)
= 0,0927 . 1
= 0,0927 N

4. Titration Curve









5. pH = 7
6. pH = 4
pH = 14 pOH
pOH = 10
pOH = - log [OH
-
]
10 = - log [OH
-
]
[OH
-
] = 10
-10

[OH
-
] =


10
-10
=


10
-20
=


Ka = 10
-5

7. pH = 9
8. [OH
-
] =


[OH
-
] =


= 7,45 x 10
-6

pOH = - log [OH
-
]
= - log 7,45 x 10
-6

= 5,127
pH = 14 5,127
= 8,87