Acid-Base Titrations Background B-1

Acid-Base Titrations Background

Part 1 Standardization of ~0.1 M NaOH(aq):
In Part 1 of today's experiment, you will prepare an approximately 0.1 M solution of
NaOH(aq) by diluting a 6 M solution of NaOH(aq). You will then accurately determine the
exact concentration of your ~0.1 M NaOH(aq) solution by a process known as standardization.
To "standardize" means to accurately determine the concentration of a solution, so that solution
may be used for another measurement. You can think of it as calibrating a solution. Crystalline
potassium hydrogen phthalate (abbreviated KHP) will be used as the primary standard acid. By
titrating a NaOH solution against a measured mass of KHP, you can accurately determine the
concentration of the NaOH solution. Then, it is possible to titrate solutions of acids having
unknown concentrations with the NaOH solution (whose concentration has now been
determined) to find the respective unknown acid molarities.
Potassium hydrogen phthalate (KHP) is a weak, monoprotic (one acidic H, denoted by
H*) organic acid that reacts with aqueous sodium hydroxide according to the reaction:

In order to detect the equivalence point (the endpoint when the reactants are exactly neutralized),
an indicator dye, such as phenolphthalein, is added to the reaction mixture. The endpoints of
your titrations will be signaled by the phenolphthalein color change. The indicator, in this case,
is sensitive to the relative amount of hydroxide ion in solution which increases quickly once the
KHP reactant is used up.
Part 1 Calculations:
To calculate the exact concentration of your ~0.1 M NaOH(aq) solution, the following
logic stream can be used. The stockroom will provide you with a stock solution of KHP(aq),
whose concentration is known and labeled on the bottle. Be sure to record this concentration,
with proper units, in the data section of your notebook!


Acid-Base Titrations Background B-2
Part 2 Determination of the Unknown Concentration of Sulfuric Acid:
By now, you'll know the exact concentration of your ~0.1 M NaOH(aq). In Part 2 of
today's experiment, you'll titrate your ~0.1 M NaOH(aq) solution against a solution of sulfuric
acid (H
2
SO
4
) whose concentration is unknown.
2NaOH(aq) + H
2
SO
4
(aq) ! Na
2
SO
4
(aq) + 2H
2
O(l)
Once again, phenolphthalein will be used to indicate the equivalence point of the titration; the
point where enough NaOH(aq) has been added to completely consume the H
2
SO
4
(aq) and any
further addition of NaOH(aq) quickly raises the pH of the solution.
Part 2 Calculations:
Although the balanced chemical equation is different from Part 1, the logic to determine
the unknown H
2
SO
4
(aq) concentration is nearly the same, albeit in reverse.


Sample Buret Readings Using a Meniscus:
In order to obtain data with good precision, you must develop good techniques with a
buret, a specially designed piece of volumetric glassware. Your instructor will cover the proper
use of a buret with you. You must read the buret to the proper level of precision (significant
figures) as with all volumetric glassware. Below is an example of a section of a buret. Note that
each of the three different examples are properly recorded to two decimal places with the last
digit estimated with an educated approximation (commonly called the doubtful digit).

initial volume = V
i
= 20.24 mL volume = 20.82 mL final volume = V
f
= 21.40 mL
Understand that the graduations of a buret are backward from a graduated cylinder, and burets
are meant to measure the volume dispensed. Record the initial volume, record the final volume,
and subtract the two values (V
f
V
i
) to calculate the total volume dispensed.

Acid-Base Titrations Background B-3
Pre-Lab Homework
1. If 26.25 mL of 0.1850 M NaOH solution reacts with 25.00 mL of H2SO4, what is the
molarity of the acid solution?

2. Standarization of a sodium hydroxide solution against potassium hydrogen phthalate
(KHP) yielded the accompanying results.

Mass KHP /g 0.7987 0.8365 0.8104 0.8039
Volume NaOH /mL 38.29 39.96 38.51 38.29
Calculate
a. the average molarity of the base
b. the standard deviation of the molarity of the base

3. A sample of battery acid is to be analyzed for its sulfuric acid content. A 1.00 mL sample
weighs 1.239 g. This 1.00 mL sample is diluted to 250.0 mL and 10.00 mL of this diluted
acid requires 32.44 mL of 0.00498 M Ba(OH)
2
for its titration. What is the mass percent
of H
2
SO
4
in the battery acid? (Assume that complete neutralization of the H
2
SO
4
occurs,
i.e. , that both H atoms are ionized)

Acid- Base Titrations Procedure P-1
Acid-Base Titrations Procedure

Purpose:
In the first part of this experiment you will prepare and standardize a solution of sodium
hydroxide to use in this week's experiments and also to use in next week's experiment (so don't
throw it away).

Special Supplies Things to borrow and return on the same day:
1 liter polyethylene bottle
500 mL polyethylene bottle (return after next week's experiment)
25 mL volumetric pipet
pipet pump or pipet bulb
buret and brush
The volumetric pipet and buret are fragile and expensive.
Treat them with care and respect.

Procedure:
Clean glassware and proper lab techniques are essential for success in this experiment.
Your instructor will provide guidance and suggestions.
Part 1a. Preparation of the ~0.1 M NaOH Solution
Using the 6 M NaOH solution and deionized water available in the lab, prepare one liter
of approximately 0.1 M NaOH solution. You will need to calculate the necessary quantities
ahead of time and be prepared to show your instructor how you will prepare this solution. Your
instructor will go over how to safely handle, pour, and measure the 6 M NaOH(aq). Prepare
your approximately 0.1 M NaOH solution in the 1 liter polyethylene bottle which you have pre-
rinsed several times with deionized water. Although there are usually no volumetric graduations
on the plastic bottle, adding deionized water to the top (before the bottle tapers) will result in ~1
liter of solution. Given that this solution will be standardized in Part 1b, an accurate volume of
solution is not critical. Cap the bottle and be certain that this solution is thoroughly mixed.
Rinse the 500 mL polyethylene bottle with deionized water and discard the rinse water.
Use approximately 20 mL portions of your ~0.1 M sodium hydroxide solution to rinse the 500
mL polyethylene bottle three times, discarding each NaOH(aq) rinse in the proper waste
container. Then, fill this bottle with your ~0.1 M NaOH solution. Put the 500 mL bottle away in
your drawer to use in the next experiment.
For today's experiment, use the remaining ~0.1 M NaOH solution from the 1 liter
polyethylene bottle. (When you finish today, rinse out the 1 liter bottle and return it so the next
class can use it.) At this point you only know that the concentration of the sodium hydroxide
solution is approximately 0.1 M. Next, you will determine the exact concentration of the
solution by standardization.

Part 1b. Standardization of the ~0.1 M NaOH Solution
Pour 80-85 mL of the KHP(aq) stock solution into a clean, dry, labeled beaker from your
drawer. You will pipet the KHP(aq) from this beaker and NOT from the stock bottle. A total of
Acid- Base Titrations Procedure P-2
75 mL will be used for the titrations and you need a little extra to rinse your pipet, so 80-85 mL
should suffice. Do not waste the KHP solution and DO NOT pour any excess back into the stock
bottle. Excess KHP(aq) should be discarded in the proper waste container.
Use a 25.00 mL volumetric pipet to precisely deliver a 25.00 mL aliquot of the standard
KHP solution into a 200 or 250 mL Erlenmeyer flask. (You may need to practice with the pipet
and water until you can carry out this operation well.) Then add about 25 mL of deionized
water, measured with a 100 mL graduated cylinder, washing down the sides of the flask in the
process. The exact volume of H
2
O added is not important because the addition of H
2
O will not
change the moles of KHP present in the flask. Next, add 2 drops of phenolphthalein indicator
solution. Don't forget this indicator or the titration will not work and you will spend much
longer in the lab than you had anticipated!
Rinse a buret twice with approximately 10 mL of the ~0.1 M NaOH solution and drain
the solution through the buret tip into a waste beaker. Then, using a funnel, fill the buret with the
~0.1 M NaOH solution. Make sure there are no air bubbles in the tip of the buret or just above
the stopcock. If bubbles are present, open the stopcock, let the ~0.1 M NaOH(aq) run through to
push out any bubbles, and then refill the buret. Run base solution (NaOH) out of the buret until
the meniscus level is just below the 0.00 mL graduated mark. Pay special attention to where the
buret is marked 0.00 mL and where it is marked 50.00 mL as it is typically marked opposite of a
graduate cylinder (0.00 mL is at the top). Remove the funnel to prevent clinging solution from
dripping down and changing your readings later. Read the bottom of the meniscus to determine
the initial volume of the base. If you have trouble viewing the bottom of the meniscus, you may
obtain a buret viewing card from the stockroom. Record the initial volume to the nearest 0.01
mL in your notebook. Be sure to keep all of the significant figures when you record the value.
You are now ready to titrate!
The most efficient way to do this experiment is to add base from the buret to the KHP
solution fairly slowly the first time, swirling the flask and contents, as you add the base. As you
approach the endpoint, the area in the KHP solution where the drops of NaOH(aq) fall will turn
pink; then the pink color will disappear as the solution becomes mixed. From this point on, add
the ~0.1 M NaOH(aq) dropwise, with constant swirling. Occasionally wash down the sides of
the flask with a little deionized water from your wash bottle. The endpoint is reached when one
drop (or less) of the ~0.1 M NaOH solution causes the solution to become permanently pale pink
throughout. Don't worry too much about getting exactly to the one drop, this time. This is your
"quick and dirty" trial. Record the final volume, again recording the reading to the nearest 0.01
mL. The difference between the initial and final volumes is the volume of NaOH solution
needed to reach the endpoint of the reaction.
Repeat the titration two more times using a clean Erlenmeyer flask each time. After the
first titration, the rest should go more quickly since you now have some idea of how much base
is required for each aliquot of KHP solution. The base may be added quickly until you are
within 2 or 3 mL of the end point. Then, change to slow dropwise addition. Be sure you read
the buret by estimating each reading to the nearest 0.01 mL. It is a good idea to record the
volumes when you are close to the endpoint so that if you add a little too much you have a value
of the volume just before that happened. Be sure to record all of your data, in your table, in your
notebook, as you collect it. This data will be used to calculate the exact concentration of your
standard sodium hydroxide solution.
Acid- Base Titrations Procedure P-3
Part 2. Determine the Concentration of Unknown Sulfuric Acid
Obtain a sulfuric acid solution of unknown concentration. Pour 80-85 mL of the
H
2
SO
4
(aq) stock solution into a clean, dry, labeled beaker from your drawer. You will pipet the
H
2
SO
4
(aq) from this beaker and NOT from the stock bottle.
You must record the unknown ID number/letter in your notebook!
If you do not record it, your instructor will not know the true value,
so you cannot receive any credit for accuracy. Don't let that happen!
A total of 75 mL will be used for the titrations and you need a little extra to rinse your pipet, so
80-85 mL should suffice. Do not waste the H
2
SO
4
solution and DO NOT pour any excess back
into the stock bottle. Excess H
2
SO
4
(aq) should be discarded in the proper waste container.
Pipet a 25.00 mL aliquot of your unknown sulfuric acid solution into a clean 250 mL
Erlenmeyer flask. Titrate this H
2
SO
4
(aq) solution with your standardized NaOH solution, using
the same buret. Use phenolphthalein as the indicator, as described previously. Repeat this
titration two more times. Record your data as you collect it, with the correct number of
significant figures!

Waste Disposal:
Dispose of excess 6 M NaOH(aq) into the waste container. DO NOT pour excess back
into the stock bottle!
Dispose of all 0.1 M NaOH(aq) rinses (1 liter polyethylene bottle and buret) into the
waste container.
Dispose of excess KHP(aq) and H
2
SO
4
(aq) into the waste container. DO NOT pour
excess back into the stock bottle!
Dispose of all titrated solutions (KHP + NaOH and H
2
SO
4
+ NaOH) into the waste
container.

Spills and Glassware:
Use wet paper towels to wipe up small spills.
Large spills of acid (KHP or H
2
SO
4
) or base (NaOH) should be immediately reported to
your instructor.
Rinse the pipet and buret and other glassware with deionized water before returning
them.

Calculations:
Follow the flow charts presented in the Background, making sure to properly convert
units as needed, and account for reaction stoichiometry. Show all units! Watch significant
figures!

Conclusion:
Report the average molarity of your NaOH(aq) solution. Is it close to your goal of
0.1 M? Report the average molarity of your H
2
SO
4
(aq) solution, with its ID number/letter.
Comment of the precision of your KHP and H
2
SO
4
titrations as shown by their standard
deviations. What are possible sources of error that may have, or could affect your precision? In
your opinion, do you trust your results/calculations and was the lab successful?