Anda di halaman 1dari 9

1

Health Science Chemistry I


CHEM-1180
Laboratory Experiment No. 13
Acid-Base Titration
(Revised 01/20/2014)


Titration is defined as the process of determining the concentration of a solution by comparing it to the
known concentration of another solution. In an acid-base titration, the point at which moles of acid are
equivalent to moles of base is the equivalence point. This is expressed algebraically as:

na(mol) = nb(mol) (Equation 1)

In the titration of acetic acid, the active ingredient in vinegar, all reactants and products are colorless
and the equivalence point is invisible. A small amount of added acid-base indicator allows
visualization of the equivalence point. Phenolphthalein, the indicator used in this experiment, is
colorless in an acidic solution and turns pink when the acid is neutralized and the solution turns
slightly basic. (When a weak acid is titrated with a strong base such as NaOH, the solution at the
equivalence point is slightly basic due to hydrolysis of acetate ion.) The point at which the indicator
turns color is the endpoint. The visual endpoint may not exactly correspond to the equivalence point,
but selecting the correct acid-base indicator gives the closest match between the endpoint and the
invisible equivalence point.

The concentration of a base titrating solution can be determined in one of two ways:

1. By using the base solution to titrate a standard acid solution of precisely known concentration, such
as commercially available 0.100 M HCl.
2. By using the base solution to titrate a known amount of a primary standard, a solid acid that can
be weighed easily and that reacts with base in a known stoichiometric manner.

We will do the second procedure and use a solid acid primary standard to standardize the NaOH
solution. Requirements for a primary standard acid are:

It must exist in very pure form, preferably as a crystalline solid.
It must be chemically stable, must not react with atmospheric oxygen or absorb water from the air.
It must have a high formula mass to minimize the effect of weighing errors.
It must react in a known manner with the solution to be standardized.

A commonly used primary standard for standardizing base solutions is the monoprotic weak acid
potassium hydrogen phthalate, HKC8H4O4, also called acid potassium phthalate. Its name may be
abbreviated as KHP where P stands for phthalate, not phosphorus. The formula mass of KHP is
204.2234 g/mol. Verify this for yourself as an exercise. KHP reacts with sodium hydroxide in a one
to one molar ratio according to the equations:
KHC8H4O4(aq) + NaOH(aq) NaKC8H4O4(aq) + H2O(l) (Equation 2)
or
KHP(aq) + NaOH(aq) NaKP(aq) + H2O(l) (Equation 3)



2

Equation 1 is the starting point of this exercise since moles of acid equal moles of base at the
equivalence point. In this case, moles of the solid acid, symbolized by na, are calculated from the mass
of KHP weighed out (between 0.6 and 0.7 g) and the KHP formula mass, 204.223 g/mol as shown in
Equation 4.


a
mass acid(g)
n (mol)
formula mass(g / mol)
(Equation 4)

At the endpoint, moles of acid equal moles of base, but moles of base solution, nb(mol), also equal the
base concentration times the volume of solution used (Equation 5).

na(mol) = nb(mol) = Mb(mol/L) x Vb(L) (Equation 5)

You will make up an approximately 0.1 M NaOH solution from stock 6 M NaOH. You will then use
this base solution to titrate a known mass of the standard acid and calculate the actual molarity of the
base, Mb, using Equation 6. Then you will use the base solution to titrate an unknown acid solution
(vinegar) and determine its molarity, Ma, using Equation 7. Base volumes will be measured with a
buret marked in 0.1 mL intervals and read to 0.01 mL. The unknown acid will be dispensed with a 5
mL pipette. For keeping track of significant figures, assume that the delivered pipette volume is
precise to 0.01 mL, that is, that the pipette delivers 5.00 mL of solution.

The concentration of the base titrating solution is calculated by combining Equations 4 and 5 into
Equation 6 and solving for the base concentration, Mb. Take into account the fact that the fact that
molar concentration is expressed as mol/L while the buret measures base solution volume in milliliters.


mass acid(g)
formula mass(g / mol)
= Mb(mol/L) x Vb(L) (Equation 6)

After you determine the exact NaOH solution molarity by titration with KHP, you will use that
concentration to determine the molarity of acetic acid in an unknown vinegar sample by solving for Ma
in Equation 7, derived by substituting n(mole) = M(mol/L) x V(L) into each side of Equation 1.

MaVa = MbVb (Equation 7)

Note: The standardization titrations do not necessarily have to be performed before the vinegar
titrations. Either set of titrations may be done first, whichever is more convenient, depending on the
availability of balances and KHP supply bottles in the laboratory.


Experimental

Preparation of NaOH Titrating Solution: Be sure your safety goggles are properly fitted to your
face. Make an approximately 0.1 M NaOH solution by dilution from 6 M NaOH stock solution as
follows: Dispense about 11 mL of 6 M NaOH into a 500 mL Florence flask. Fill the flask halfway
with distilled water and swirl the flask for 15 s to mix the contents thoroughly. When the solution
appears completely homogeneous, fill the flask to the bottom of the neck with distilled water for a total
volume of about 500 mL. Place a rubber stopper securely in the neck, support it with the palm of your
hand, invert the flask and swirl it for 5 s. Right the flask and repeat this step two more times to ensure

3

the solution is uniform. If you see swirls of inhomogeneity, the solution is not yet well mixed. Keep
the ~0.1 M NaOH sealed with the rubber stopper. Remember, the concentration of base in this
solution is not well known. Its actual concentration will be determined by titration. You will use this
solution for all subsequent titrations. Do not discard it until the end of the experiment.

NaOH is never used as a primary titration standard because the compound cannot be weighed
accurately. NaOH pellets exposed to the air immediately absorb water and carbon dioxide so their
purity is always in doubt. Moreover, NaOH solutions undergo slow conversion to sodium carbonate
unless they are carefully protected from atmospheric CO2.

Filling Buret with Base Solution: Obtain a 50 mL buret. If the buret is clean and dry, there is no
need to wash the buret or rinse it with tap water. Insert a stopcock and tip into the buret bottom. If
they do not fit tightly, match a different stopcock with your buret. Rinse the buret twice with 5 mL
portions of your 0.1 M NaOH solution, drain the solution through the tip and discard it. Support the
buret vertically with a buret clamp over a sink so the top of the buret is at or below your eye level. Fill
the buret with NaOH solution nearly to the top. Open the stopcock and run some base solution out
rapidly while tapping the stopcock to dislodge any bubbles hidden inside. Adjust the volume of base
so that it is at, or slightly below, the zero mark. It is not necessary to get the initial volume to exactly
zero. Record the initial volume of the NaOH solution to the nearest 0.01 mL. (Note: If the 50-mL
buret is filled to the very top graduation, the initial volume should be read as 0.00 mL, not 50.00 mL.)

NaOH Solution Standardization: Using small beakers or plastic weigh boats, weigh four 0.6 to 0.7 g
samples of KHP on an electronic balance to 0.001 g. Take advantage of the convenient electronic
balance tare function. Place a weighing container on the balance pan and push the Tare or T button.
The balance display will read 0.000 g, showing the balance considers the container to have no mass.
The mass of any material you put in the container will be displayed directly, eliminating the need for
two separate weighings and a subtraction step to get the mass of the chemical. (If the balance display
reads to only two decimal places, inform the instructor.)

Quantitatively transfer each weighed KHP sample to a labeled, clean, but not necessarily dry 125 or
250 mL Erlenmeyer flask. Pour the solid through a wide-stem funnel into the Erlenmeyer flask and
wash all traces of the chemical out of the weighing container and funnel with distilled water from your
wash bottle. Add about 50 mL of distilled water and two drops of phenolphthalein indicator to each
Erlenmeyer flask and swirl briefly. (The KHP will not dissolve completely until you add NaOH
solution.) Titrate each KHP solution with NaOH solution as follows:

For easy visualization of the endpoint, place a sheet of white paper on the ring stand base under the
titration flask. Record the initial buret reading. Lower the buret so the tip is inside the Erlenmeyer
flask and run base solution rapidly into the flask. If you are right handed, grip the neck of the
Erlenmeyer flask with the fingers of your right hand and swirl the solution rapidly to mix the acid and
base. Meanwhile operate the stopcock with your left hand. As the endpoint approaches, all the solid
KHP will dissolve. The color change from clear to pink will persist longer where the base enters the
solution. The final addition of base should be slow, one drop at a time to avoid overtitration. Rinse
the upper flask walls several times during the titration with a few milliliters of distilled water from
your wash bottle to ensure all the acid and base mix in the flask. Distilled water contains equal (and
almost negligible) amounts of hydrogen and hydroxide ion and will not affect the titration results. You
may also rinse the buret tip to remove hanging drops of base solution. Do not rinse excessively
because that will remove sodium hydroxide solution from inside the tip.


4

The titration endpoint occurs when the solution changes from colorless to a persistent pale pink color.
Sometimes less than half a drop of base brings this about. When you believe you are near the
endpoint, transfer less than one drop of base from the buret tip to the wall of the flask, rinse it down
with distilled water and swirl. Repeat this step until you reach the visible endpoint. Do several more
titrations until you have three that agree to within a few percent. Since your KHP masses are likely to
be different, check for consistency of your titrations by dividing the volume of base solution dispensed
by the KHP mass (no units are necessary). Write the calculated ratios with the correct number of
significant figures in the blank space to the right of the titration data. This volume/mass ratio should
be nearly constant for all titrations.

If you add base solution beyond what is needed to get the first pale pink color, you have overtitrated.
A pale pink endpoint is best; medium pink is acceptable. Deep pink means you have added too much
base. Do not use overtitrated results in your calculations. If you use more than 24 mL of base solution
for a titration, fill the buret before the next titration so you will not run out of base partway through the
next procedure.

Titration of Unknown Acid: Obtain an unknown vinegar solution and record its number on your data
sheet. Rinse a 5 mL pipette two times with a small amount of your unknown acid and discard the
rinsate down the drain. Pipette 5 mL aliquots of your unknown acid into four separate clean (but not
necessarily dry) Erlenmeyer flasks as follows: Fill the rinsed pipette by suction using a rubber bulb
until the acid solution level is about 2 cm above the upper stem fill line. Never pipette by mouth. Let
in small amounts of air with the bulb or your finger tip until the bottom of the meniscus just touches
the fill line. Move the pipette to an Erlenmeyer flask and drain the pipette into the flask with the
pipette tip held against the inside of the neck. Wait 2 s after the flow stops, touch the pipette tip to the
surface of the liquid and remove the pipette from the flask. Do not blow out the liquid remaining in
the tip. Volumetric pipets are calibrated to deliver, not to contain, the specified amount. Add two
drops of phenolphthalein indicator to each flask and titrate each solution with your standard NaOH
solution to a persistent pale pink endpoint. Repeat the titrations until you have three reliable results
(pale pink endpoints with base volumes that agree closely) from which to calculate the average
molarity of your acetic acid sample. (Since the volume of unknown acid solution you pipette is the
same each time, the NaOH solution volumes should be the same for each titration. There is no need to
calculate a base volume to acid ratio as before.)

Cleanup: When you finish titrating, remove the stopcock and rinse the buret, stopcock and tip
thoroughly with tap water. Sodium hydroxide solution corrodes glass and will etch the buret if
allowed to remain inside. After you rinse the buret, your instructor may tell you to place the buret in a
special buret cleaner. Return your pipette and unknown bottle to the stock room. Wipe up any spilled
KHP from the balance and surrounding area. Wipe your benchtop down with a wet sponge and wash
your hands before you leave the room.

Safety: The stock 6M NaOH solution is extremely corrosive and dangerous to the eyes. Chemical
splash goggles and a waterproof apron must be worn at all times during this and all chemistry
experiments, from the very beginning to the very end of the time you spend in the laboratory.

Waste Disposal: All spent titration solutions are neutralized and may be safely rinsed down the drain
with water. Your instructor will tell you how to dispose of unused 0.1 M NaOH titrating solution.




5

Health Science Chemistry I
CHEM-1180
Laboratory Experiment No. 13
Acid-Base Titration
Data Page for Sodium Hydroxide Standardization Titrations


Standardization Titration # 1
Mass of KHP
Final NaOH Volume
Initial NaOH Volume
NaOH Titrating Volume
Endpoint Color

Standardization Titration # 2
Mass of KHP
Final NaOH Volume
Initial NaOH Volume
NaOH Titrating Volume
Endpoint Color

Standardization Titration # 3
Mass of KHP
Final NaOH Volume
Initial NaOH Volume
NaOH Titrating Volume
Endpoint Color

Standardization Titration # 4
Mass of KHP
Final NaOH Volume
Initial NaOH Volume
NaOH Titrating Volume
Endpoint Color

Standardization Titration # 5
Mass of KHP
Final NaOH Volume
Initial NaOH Volume
NaOH Titrating Volume
Endpoint Color

Standardization Titration # 6
Mass of KHP
Final NaOH Volume
Initial NaOH Volume
NaOH Titrating Volume
Endpoint Color




6

Health Science Chemistry I
CHEM-1180
Laboratory Experiment No. 13
Acid-Base Titration
Data Page for Unknown Vinegar Solution Titrations

Unknown Vinegar Solution Number:________________

Vinegar Titration # 1
Volume Acid Pipetted
Final NaOH Volume
Initial NaOH Volume
NaOH Titrating Volume
Endpoint Color

Vinegar Titration # 2
Volume Acid Pipetted
Final NaOH Volume
Initial NaOH Volume
NaOH Titrating Volume
Endpoint Color

Vinegar Titration # 3
Volume Acid Pipetted
Final NaOH Volume
Initial NaOH Volume
NaOH Titrating Volume
Endpoint Color

Vinegar Titration # 4
Volume Acid Pipetted
Final NaOH Volume
Initial NaOH Volume
NaOH Titrating Volume
Endpoint Color

Vinegar Titration # 5
Volume Acid Pipetted
Final NaOH Volume
Initial NaOH Volume
NaOH Titrating Volume
Endpoint Color


7

Health Science Chemistry I
CHEM-1180
Laboratory Experiment No. 13
Acid-Base Titration
Report
Clearly show the equations, setups and steps for each calculation.
1. For each of your three best standardization titrations, use Equation 4 to calculate the moles of
KHP weighed out. (3 points)

















2. For each of your three best standardization titrations, solve Equation 6 to calculate the molarity
of your NaOH titrating solution. (6 points)



















3. Calculate the average molarity of the NaOH titrating solution from your three best trials.
(2 points)


8

4. Calculate the average volume of NaOH solution used in your three most consistent titrations of
the unknown acetic acid (vinegar) solution. (1 point)




5. Write your Unknown Vinegar Solution Number here:__________
Use Equation 7 to calculate the molarity of your unknown acetic acid solution. (4 points)













6. Calculate the mass of sodium hydroxide in one liter of your NaOH titrating solution. (2 points)








7. Calculate the percent (w/v) concentration of your unknown acetic acid solution, that is, the
mass of acetic acid in 100 mL of solution. (2 points)


















9

Health Science Chemistry I
CHEM-1180
Laboratory Experiment No. 13
Acid-Base Titration
Prestudy

1. A 0.7483 gram KHP sample requires 14.98 mL of a NaOH solution to neutralize it using
phenolphthalein as an indicator. What is the molarity of the NaOH solution? (4 points)

















2. A 10.00 mL sample of acetic acid solution is titrated with 35.87 mL of 0.217 M NaOH solution.
Calculate the molarity of the acetic acid solution. (4 points)












3. Why is phenolphthalein the indicator of choice for the titrations in this experiment? (2 points)

Anda mungkin juga menyukai