Instructions Observations
Volumetric Analysis, Part A: The Standardization of a
Sodium Hydroxide Solution
Step #3: Prepare the Primary Standard Acid
Calculate the mass of potassium hydrogen phthalate (KHP)
that will require 15 mL of the NaOH solution (use 0.1 M for
the approximate NaOH concentration). Include this
calculation in your prelab.
Measure this mass of KHC8H4O4 on a tared piece of
weighing paper and transfer it to a 250 mL Erlenmeyer
flask. Complete the preparation of all three samples while
you are occupying the balance. Dissolve the KHC8H4O4 in
about 50 mL of previously deionized water and add 2
drops of phenolphthalein. Make sure that the KHP has
completely dissolved in the deionized water before
titrating.
Step #4: Prepare a Clean Buret
Wash a 50-mL buret with deionized water. Rinse the
buret with three 5-mL portions of the diluted NaOH
solution, making certain that the solution wets the entire
inner surface. Have the instructor approve your buret
and titration setup before continuing.
Step #5: Fill the Buret
Using a clean funnel, fill the buret with the NaOH solution.
Record this initial. Place a Kim-wipe beneath the
Erlenmeyer flask. Make sure that there are no air bubbles
in the tip of the buret.
Record the number on the bottle of NaOH solution. You
should be sure to use solution from this same bottle for
the entire experiment. Make sure that you can read the
buret. If not, move the buret in the red buret clamp or get
a step stool.
Step #6: Titrate the Primary Standard Acid
Slowly add the NaOH titrant to the first acid sample. Swirl
the flask after each addition. Initially, add the NaOH
solution in 1- to 2-mL increments. As the stoichiometric
point nears, the color fade of the indicator occurs more
slowly. Occasionally rinse the wall of the flask with DI
water from your wash bottle. Continue addition of the
NaOH titrant until the endpoint is reached. The endpoint
in the titration should be within one-half drop of a slight
pink color. The color should persist for 30 seconds. After
10–15 seconds, read and record the final volume of NaOH
in the buret. If there are drops of NaOH on the side of the
flask, use a wash bottle of deionized water to rinse the
sides of the flask (do not add too much extra water).
Step #7: Repeat the Analysis with the Remaining Standard
Acid Samples
Perform at least two additional trials of the KHP titration.
You need to have at least two titrations with a faint pink
endpoint.
As long as the buret is at least half full (~25 mL), there is
no need to refill the buret after the first trial. However,
make sure there is enough NaOH solution in the buret to
complete any additional trials.
Step #8: Do the Calculations (lab report)
Potentiometric Analysis, Part A: Molar Concentration of
a Weak Acid Solution
Step #1: Obtain a Standardized NaOH Solution
Use the stock NaOH solution found in the white bottles at
the front of the lab. Make sure to use the same bottle
that you used for the first part.
Step #2: Prepare the Buret with the Standardized NaOH
Solution
Use the syringe attachment to contain your titrant instead
of the buret from the first experiment. Make sure that
both stopcocks are closed. Fill the syringe with the NaOH
solution from the previous part.
Step #3: Prepare the Weak Acid Solution for Analysis
Perform one trial in this part of the experiment. Place a
magnetic stirbar to the beaker that you will use so the
solution can be stirred during the titration.
You will be told in lab how much unknown acid solution
you will need. Dispense into a clean 250 mL beaker.
Record the information listed on the stock bottle so you
can compare this with your calculated results. Record
which unknown sample you have.
Use deionized water to rinse the pH electrode before
putting it into the acid solution.
Step #4: Titrate the Weak Acid Solution & Step #5: Titrate
Beyond the Stoichiometric Point
Press the “Play” button on the bottom left of the
LabQuest screen. Open the top stopcock and the
LabQuest will begin to collect data. Titrate the sample
until you reach at least a pH of 11.75; you want to see the
titration curve leveling out. After the titration is
complete, close the top stopcock and insert a photo of
the titration curve into your prelab. Save your data.
Step #6: Plot the Data (Lab Report)
In Excel, create the following table of numbers using your
experimental data from the LabQuest (do not worry
about error for each point). The first two columns of this
table will come from the LabQuest file on Courseworks.
The first two columns are cumulative, while the third and
fourth will be the calculated difference between two
adjacent rows.
Using the table created above, plot the data as outlined in
your lab manual (Step #6): pH (y-axis) versus volume (mL)
NaOH added (x-axis). However, do not worry about
drawing a smooth curve over the points.
You will observe the shape just by inspection.
Using the data table created above, make a graph of
[(DpH) / (Dvolume (mL) NaOH added)] (y-axis) versus
volume (mL) NaOH added (x-axis). Using this graph,
determine the equivalence point and the volume (mL) of
NaOH added at that point. You will do this by finding the
maximum peak on this graph and recording the volume
NaOH delivered at this point; you should mark this point
on your graph. This value will be used for “Volume of
NaOH dispensed (mL)” on the Report Sheet (Part A, #5).
Potentiometric Analysis, Part B: Molar Mass and pKa of
Solid Weak Acid
Step #1: Prepare the Unknown Solid Acid Samples
Perform one trial in this part of the experiment. Mass out
the “Unknown Solid Acid” in a 150 mL beaker and record
the exact mass in your data table. You will be told in lab
how much solid acid you will need. Record which
unknown sample you have. Add a stir bar so that the
solution can be stirred during the titration.
Step #2: Fill the Buret and Titrate
Use the same NaOH from the “Volumetric Analysis” since
it was just standardized.
Use the experimental apparatus from Part A (LabQuest,
pH probe and drop counter). Make sure that the syringe
has at least 40 mL of NaOH in it.
Select the “Play” button and “discard” your last run. Open
the top stopcock. Titrate the sample until you reach at
least a pH of 11.75; you want to see the titration curve
leveling out. After the titration is complete, close the top
stopcock and insert a photo of the titration curve into your
prelab. Save your data.
Step #3: Plot and Interpret the Data (Lab Report)
In Excel, create the following table of numbers using your
experimental data from the LabQuest (do not worry about
error for each point). The first two columns of this table
will come from the LabQuest file on Courseworks. The
first two columns are cumulative, while the third and
fourth will be the calculated difference between two
adjacent rows.
Step #4: Calculate the Molar Mass and the pK a of the
Weak Acid
This part will be done for the lab report and is analogous
to the calculations and graphs to the “Weak Acid Solution”
part of the experiment.
Using the table created above, plot the data as outlined in
your lab manual (Step #3): pH (y-axis) versus volume (mL)
NaOH added (x-axis). However, do not worry about
drawing a smooth curve over the points. You will observe
the shape just by inspection.
Using the data table created above, make a graph of
[(DpH) / (Dvolume (mL) NaOH added)] (y-axis) versus
volume (mL) NaOH added (x-axis).
Using this graph, determine the equivalence point and
the volume (mL) of NaOH added at that point. You will do
this by finding the maximum peak on this graph and
recording the volume NaOH delivered at this point; you
should mark this point on your graph. This value will be
used for “Volume of NaOH dispensed (mL)” on the Report
Sheet (Part B, #5).
Data tables:
PART A: Standardization of Sodium Hydroxide Solution.
Calculate the approximate mass of KHC8H4O4(molar mass = 204.23g/mol) needed for the
standardization of the NaOH solution
________ g KHC8H4O4
T1 T2 T3
Mass of KHP(g)
Moles of KHP (mol)
Initial buret reading
(mL)
Final buret reading
(mL)
Volume of NaOH
dispensed (mL)
Molarity of
NaOH(mol/L)
Average molarity of
NaOH (mol/L)
PART B: Molar Concentration of a Weak Acid Solution: Unknown Code_______________
Monoprotic, diprotic or triprotic?
Molar concentration of NaOH (mol/L)from Part A
Volume of weak acid solution (mL)
Volume of NaOH dispensed at the stoichiometric
point(mL)
Moles of NaOH to reach stoichiometric point
(mol)
Moles of acid (mol)
Molarity of weak acid solution (mol/L)
PART C: Molar Mass and the pKa of a Solid Weak Acid: Unknown Code_______________
Monoprotic, diprotic or triprotic?
Mass of solid acid (g)
Molar concentration of NaOH (mol/L) from Part A
Volume of NaOH dispensed at the stoichiometric
point (mL)
Moles of NaOH to reach stoichiometric point
(mol)
Moles of acid (mol)
Molar mass of acid (g/mol)
Volume of NaOH to half-equivalence point (mL)
pKa value(s) of weak acid
