Lect.4. General Chemistry Laboratory Reem.S.

Najm

Lect.4.

Titration
Titration: a sulfuric acid with sodium hydroxide.

Purpose:
To determine the concentration of a sulfuric acid solution by titration.

Please Read:
The section titled “Volumetric Glassware” on your lab page. You may
also wish to review the section titled “Accuracy and Precision”.

Introduction:
Titration is the process, operation, or method of determining the
concentration of a substance in solution (the analyses) by adding to it a
standard reagent of known concentration (the titrant) in carefully
measured amounts until a reaction of definite and known proportion is
completed, as shown by a color change or electrical measurement, and
then calculating the unknown concentration.
In this experiment, sulfuric acid is titrated with sodium hydroxide. The
equation is.
2NaOH + H2SO4 → Na2SO4 + 2H2O
The titration is done in the presence of phenolphthalein, an indicator that
is colorless in acid solution but turns pink in basic solution.
For the titration to give an accurate result, one must stop adding titrant
exactly at the equivalence point, when the indicator changes color.
At the equivalence point, all of the analyses has reacted, and only a tiny
excess of titrant has been added, just enough to change the color of the
indicator.

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Lect.4. General Chemistry Laboratory Reem.S.Najm

Lect.4.

Safety and Waste Disposal:

The solutions of H2SO4 and NaOH are fairly dilute, and not dangerous, but they are
mild irritants. If you spill them on yourself, rinse well with water.
NaOH will cause a slippery “soapy” feeling; rinse until it is gone. Spills on benches,
etc., should be cleaned up with paper towels. Waste solutions can be poured down the
sink.

Procedure:
1. Obtain a buret, a buret clamp, a 10.00 mL pipet, and a pipet bulb from the supply
area.
2. Make sure your 50 mL graduated cylinder is dry, then fill it with H2SO4 solution
(get it close to the 50 mL mark, but it doesn’t have to be exact). Clamp the cylinder to
your ring stand so it won’t tip over and spill.
3. Draw 2-3 mL of the H2SO4 solution into your pipet and rinse it. Discard the
rinsing's. Use the pipet to dispense 10.00 mL of sulfuric acid.
solution into each of three 250 mL Erlenmeyer flasks. Be careful not to draw the
solution into the pipet bulb.
4. Add about 10 mL of distilled water and 2 drops of phenolphthalein to each flask.
5. Make sure your 150 mL beaker is dry, then fill it to the 80 mL mark with NaOH
solution. Record its concentration on your data sheet Use
(5-10 mL) of NaOH solution to rinse out your buret. Discard the rinsings.

6. Fill the buret with sodium hydroxide solution, then clamp the buret to the ring
stand. With a second beaker under the buret, open the stopcock to fill the buret tip.
There should be no air bubbles. Make sure the liquid level is below the 0.00 mL mark.
Titrations.

7. Read the initial volume on the buret to the nearest 0.01 mL, between the marks, and
record the value. Remember, the buret reads from the top down. Titrate your first
sample of sulfuric acid. It's easier to see the pink color of the indicator if you put a
sheet of white pape under your flask. When the pink color starts to persist, slow the
rate at which you add sodium hydroxide. The idea is to stop adding sodium hydroxide
exactly at the endpoint, when the pink/purple color remains for at least 15 seconds. At
the endpoint, read the final volume on the buret to the nearest 0.01 mL and record the
result.

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Lect.4. General Chemistry Laboratory Reem.S.Najm
Lect.4.

8. Repeat the titration on the other two samples. You should use nearly the same
volume of NaOH for each titration. Before starting a titration, make sure there is
enough NaOH in the buret to complete it.
If not, add additional NaOH and record the initial volume on your data sheet. If the
range between the highest and lowest volume of NaOH is greater than 0.50 mL,
perform additional titrations until there are three that agree within 0.50 mL. Your data
sheet has space for more runs, if needed.

9. Perform the calculations and answer the questions on your data sheet.

10. Rinse all glassware three times with tap water. Follow with a final rinse of
distilled water. Use the procedures in steps 3 and 5, using distilled water, to rinse your
pipet and buret. The buret should be put away with its top down and the stopcock
open. Calculations The calculations for titrations are essentially theoretical yield
calculations, worked with volumes and concentrations of solutions, rather than masses
and molar masses of compounds. As in all theoretical yield calculations, one must
have the balanced equation for the reaction.

2 NaOH + H2SO4 → Na2SO4 + 2 H2O .

The first step in any theoretical yield calculation is to determine the number of moles
of one of the reactants, the one for which you know both the volume and
concentration. In this case, you know both quantities for NaOH.
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reaction
This is a simple neutralization reaction:

H2SO4 + 2NaOH → Na2SO4 + 2H2O sample size.

Depending on the titrant concentration (0.2 M or 0.1 M), and assuming.

50 mL burette, aliquot taken for titration should contain about

(0.34-0.44 g) (0.17-0.23 g) of sulfuric acid (3.5-4.5 or 1.7-2.3 mill moles).

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Lect.4. General Chemistry Laboratory Reem.S.Najm

Lect.4.

End point detection

Equivalence point of strong acid titration is usually listed as exactly 7.00. In the case
of sulfuric acid second step of dissociation is not that strong, and end point is shifted
up by tenths of the pH unit - but we are still very close to 7. Thus the best indicator of
those listed on pH indicators preparation page is bromothymol blue.

However, as we have discussed on the acid-base titration end point detection page,
unless we are dealing with a diluted solution (in the range of 0.001 M) we can use
almost any indicator that gives observable color change in the pH 4-10 range. In
effect we can safely use the most popular phenolphthalein and titrate to the first
visible color change.

Color change of phenolphthalein

during titration - on the left,
colorless solution before end point,
on the right –pink. Solution after
end point .

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Lect.4. General Chemistry Laboratory Reem.S.Najm

Lect.4.

Example 11 :

The titration of 0. 25 mL of an unknown concentration H2SO4 solution

requires 83.6 mL of 0.12 M LiOH solution. What is the concentration of
the H2SO4 solution (in M)? I keep getting 0.40 mol instead of the correct
0.20 mol.
Answer:
The reaction is:
H2SO4 + 2LiOH → 2H2O + Li2SO4.
1 mole H2SO4 requires 2 moles of LiOH. So we know the molarity
and volume of LiOH solution so we can find number of moles of LiOH
needed:

0.0836 L of LiOHx0.12molofLiOH\ 1LofLiOH = 0.010 mol of LiOH.

Now that we know the number of moles of LiOH needed we can find
number of moles of H2SO used: 0.010 mol.
ofLiOH x1molofH2SO4\2molofLiOH = 0.005 mol of H2SO4.

Finally, we know that concentrarion is number of moles per volume, so

we find the molarity of H2SO4 by dividing the mol number to its volume,
25.0 mL which is 0.025L:
0.005
M = ‫=ـــــــــــــــــــــــ‬0.2M.
0.025
H2SO4 + 2LiOH → 2H2O + Li2SO4.
0.010 mol of LiOH x1molofH2SO42molofLiOH = 0.005 mol of H2SO4.
Finally, we know that concentrarion is number of moles per volume, so
we find the molarity of H2SO4 by dividing the mol number to its volume,
25.0 mL which is 0.025L:
M = 0.0050.025=0.2M.

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Lect.4. General Chemistry Laboratory Reem.S.Najm

Lect.4

Example 12
student titrates(40 ml) of an H2SO4 solution of unknown concentration
with a (0.55M) NaOH solution . the volume of base solution needed to
reach the equivalence point (24.64ml), what the normality concentration
of H2SO4 solution ?

Answer:
V H2SO4=40 ml C H2SO4 =? V, NaOH=24.64ml C NaOH=0.55M
N=M x no. of H+\1mole
N= 0.55Mx2= 1.1N
(N1.V1)acid = (N2.V2)base
1.1x24.64
N1=‫=ــــــــــــــــــــــــــــ‬0.68N concentration of H2SO4
40

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