Titrations
of Acetic Acid, Formic Acid, Unknowns X and Y
Nov 17, 2015
Generally
we do acid-base titrations with NaOH solution in the burette,
and the acid in a 250 ml Erlenmeyer flask or 400 ml
beaker. You will use beakers so that you can use a pH
probe and a magnetic stirrer.
Be sure
to coat the inside of your
burette with
the standardized 0.10xx M NaOH solution and rinse before filling
the
burette. You'll need to clear bubbles
from
the burette tip; sometimes they're hiding where you can't see
them. Once you’ve
filled the burette with NaOH solution and cleared bubbles from
the
tip,
you should not have to do this again; just refill the burette
after
each
titration and don’t let the burette get emptied. Don’t
bother trying to start at exactly the
0.00 ml mark on the burette. You should
never use a titration that
consumes more than 50 ml of titrant. Before you start, think
about how much titrant
each titration will consume.
Spread the acid bottles selected by your instructor across an unused bench top. Get a 25 ml pipette and a 5 ml pipette for each acid bottle. Coat the inside of the pipette with acid solution and rinse before you use it. DON’T MIX THE PIPETTES! If you have forgotten how to use a pipette bulb, practice on water first before you pipette acid solution in to the beaker. In the past you may have used a 250 ml Erlenmeyer flask for titrations, but since you will be using a pH probe today, you should use a beaker and a magnetic stirrer.
Do a quick and dirty titration of 5 ml of each acid so that you have an idea where the end point will be. That way you can do the big titrations faster, and you’ll know were the buffer region is. You can always add more DI water to the titration if the volume is too small for the pH probe. Make a rough estimate of how much water you add. Remember to add 2 drops of phenolphthalein to each titration before you start.
Set up the Vernier LabPro to record data during the big titrations. (Instructions for the LabPro are below.) Plan your titration! You want to record more points as you pass through the buffering region and again during the endpoint region--but you don't want to waste time recording lots of unneeded points. While passing through the buffering region (where pH = pKa) and also while passing through the endpoint, add just 0.20 ml of titrant at a time and read the pH after each addition of titrant. You want readings close together in these regions so that you can make an accurate graphical estimate of the pKa and the end point volume..
Compare the shape of the
titration
curve to the curves in Harris’s textbook. Your
instructor may tell you to repeat
a titration if your curve doesn’t make sense.
Write your results
on
the
board. Compare the results among
groups;
if one group gets values for acetic acid that are rather different
from
everyone else’s, then that group should check their calculations
and
repeat the
titration. Write on the board results
for formic acid, X, and Y; check to make sure all groups get
consistent
results.
On each acid bottle the concentration is given in grams of
solute/liter
of solution. (Don't mistake this for solution density!)
Using this
information and the titration data, compute the molecular weight
of acetic acid, formic acid, X,
and Y. X and Y are both monoprotic
acids
listed in
Appendix G of Harris’s textbook. Use the molecular weight and the
pKa to determine identity of
the unknown acids.
Setting up LabPro:
Obtain a LabPro and supply it with power using the AC Adapter. Using the USB cable, connect one end to the LabPro and the other to one of the USB ports on the left side of a laptop. Connect the pH probe to the one of the channels in the side of the LabPro and then open up Logger Pro (located on desktop). Once this program opens it should display a table on the left-hand side and a graph on the right. Open up the Experiment menu and select Data Collection. Under the Collection tab, select Events with Entry from the pull-down menu. This will allow you to label the column as volume of base added, or something to that effect. There is also a spot for the units, mL, or whatever is appropriate. A modified table on the left should have two columns, one for the volume and one for the pH.
You will need to calibrate the pH probe using pH 4 and pH 7 buffers. If the pH probe is not calibrated, your value of the pKa will be wrong.
To adjust the scale on the graphs,
right-click on the graph and select Autoscale
from the menu. You can also select a
value
on the axis and type over it with the value you want. Get
the
axes right so that the titratio curve will be big and easy to read
on
the computer screen.
To start recording readings:
Click
the Collect button at the top right of the screen
in
Logger Pro. At this point the Keep
button should also become active. The
current readings for the pH probe should
be shown right above the table and graphs.
Once the readings have had a chance to stabilize, click the
Keep button and enter “0” in the
blank. Now add two or three mL of
titrant at a time to the beaker, allow
the reading to stabilize, and click Keep
once again to enter the amount of titrant added.
Around
the endpoint, add titrant 0.2 mL at a
time. Be sure to take seven or eight
data
points beyond
the
endpoint so that you see the shape of the entire curve.
Once your last data point has been collected,
click Stop to end data
collection. You MUST click Stop before you can print and
save
the data to a drive.
You may then print out the table and graphs separately by opening up the File menu and selecting Print Data Table and Print Graph, respectively. A menu will come up in which you can add a footer if you would like.
To save your data, open up the File menu and select Export as Text. This will allow you to save the data as a text file to open in Excel. Then, open up Excel and select the Open command. Change the file type in the pull-down menu to Text Files and find your file and open it. A window will appear which helps to import the data into Excel. Make sure the Delimited option is selected, then click Next twice, and then Finish. The data should appear exactly as it was in your table in Logger Pro. Alternatively, you can highlight the data in Logger Pro, select Copy, switch to Excel, and finally select Paste. However, do not forget to save your data from Logger Pro.