Acid Base Titration
Purpose: To determine the concentration of a solution of hydrochloric
acid using a primary standard (solid Na2CO3) and
a secondary standard (aqueous, standardized NaOH).
Procedure:
Preparation of a solution of hydrochloric acid
Each group of 4 students will prepare 1L of 0.1M HCl from concentrated
HCl (12M): Fill a 600 mL beaker to the 250 mL mark with de-ionized water.
In the hood, add 8.3± .2 mL of con HCl
(approximately 12M) to the beaker and stir. (Record the actual volume of
con HCl used.) At your desk, transfer the liquid into a 1L volumetric flask
using a funnel. Rinse the beaker once with de-ionized water and add the
rinse to the flask. Dilute to the 1L mark. Mix thoroughly.
The actual concentration of this solution to 3 significant figures is
the unknown in today’s lab.
Titration with a primary standard
-
Weigh out 0.25 ± .05 g of dry Na2CO3. Record
actual mass used to nearest .001 g. Transfer the solid to a 250 mL Erlenmeyer
flask, rinse the weigh paper into the flask with a small amount of de-ionized
water and dissolve the solid with 25 mL of de-ionized water. Add 3 drops
of bromcresol green once the solid is dissolved.
-
Clean and check the flow rate of a buret (as described in the handbook).
-
Rinse the buret 3 times with 5 mL of the 0.1M HCl solution to be titrated.
Discard the rinses. With the stopcock open and over a beaker, begin filling
the buret with 0.1M HCl solution. Have your lab partner close the stopcock
once the tip is draining and the volume is above the stopcock. This will
prevent bubbles from forming in the stopcock during the filling process.
Finish filling the buret to within a few mL of the zero mark. Record this
volume as the initial volume in the titration. (Note that this is NOT the
volume of liquid in the buret.)
-
Begin titrating the sodium carbonate solution with the hydrochloric acid
solution by adding small increments of the titrant from the buret. Swirl
the reaction mixture between additions. Use smaller increments of HCl as
you get closer to the expected endpoint (Pre-Lab question 2). The acid-base
indicator, bromcresol green, will eventually turn from blue, which indicates
an excess of Na2CO3, to yellow, which indicates an
excess of HCl. The endpoint will be when the solution remains green, which
indicates that the stoichiometric quantity of HCl has been added.
-
Once the solution is green, bring it to a gentle boil on a hot plate to
expel all dissolved carbon dioxide. Remove it from the hot plate to a wire
gauze, and rinse the inside surfaces with a small amount of de-ionized
water. If the solution stays green, the titration is complete. Record this
volume as the final volume of titrant. If it turns blue, allow it to cool,
and complete the titration by adding a few drops more of titrant. If the
solution is yellow, you have overshot the endpoint and must repeat the
titration.
Step 5 is necessary because one of the products of the titration
is carbon dioxide. The carbon dioxide will react with water to form carbonic
acid which can cause the reaction mixture to become acidic prior to the
addition of enough HCl to neutralize the Na2CO3.
If this happens, the indicator will change color early, and you will have
a "premature endpoint".
6. Flush the neutralized solution down the drain with
lots of water. Repeat the titration until you have 3 titrations whose molarity
are within ±.0006 of the average.
7. Rinse the buret thoroughly with tap water (3 times)
then 3 times with de-ionized water. Verify that the final rinse is neutral
by placing a drop from the buret on blue litmus paper. If it is still acidic,
the blue litmus will turn pink.
Titration with a secondary standard
-
Pipet 25 mL of the HCl solution into a 250-mL Erlenmeyer flask. Add 50
mL of de-ionized water and 3 drops of phenolphthalein.
-
Rinse the buret 3 times with 10 mL of the standard NaOH solution. Discard
the rinses. With the stopcock open and over a beaker, begin filling the
buret with the NaOH solution. Have your lab partner close the stopcock
once the tip is draining and the volume is above the stopcock. This will
prevent bubbles from forming in the stopcock during the filling process.
Finish filling the buret to near the zero mark. Record the precise concentration
of the standard NaOH solution and the Vinitial in your notebook.
3. Start adding the NaOH to the HCl solution in the Erlenmeyer flask,
swirling the flask thoroughly between additions. Use smaller increments
of NaOH as the color of pink begins appearing in the flask. Add drop-wise
when the color seems to last a long time before disappearing. The endpoint
is the volume of NaOH needed for the color to remain a pale pink (not fuschia!)
Record this volume as the Vfinal. Phenolphthalein, the acid-base
indicator, will turn pink at a slight excess of hydroxide ion.
4. Flush the contents of the beaker down the drain
with lots of water. Rinse the buret thoroughly with tap water (3 times)
then 3 times with de-ionized water. Verify that the final rinse is neutral
by placing a drop from the buret on red litmus paper. If it is still basic,
the red litmus will turn blue.
PROCESSING THE DATA
Part I Titration with a Primary Standard
For each titration, calculate the molarity of the hydrochloric acid solution
using the volume of HCl needed to achieve the endpoint of the titration,
the mass of the sodium carbonate and a balanced equation for the reaction.
Determine the average and verify that you have three results that are within
.0006 of your average. Don’t forget to propagate the error through your
calculations!
Part II Titration with a Secondary Standard
Calculate the molarity of the hydrochloric acid, using the volume of NaOH
needed to reach endpoint, the molarity of the standard NaOH solution, the
volume of HCl pipetted and a balanced equation for the reaction. . Don’t
forget to propagate the error through your calculations!
Compare the molarity determined using a primary standard and the molarity
determined using a secondary standard. Which molarity do you think is the
most reliable and why? Use this molarity as your accepted value to calculate
the %error.
Pre Laboratory Assignment
-
Read section VIII of your Laboratory Handbook for information on
the use of volumetric glassware, making solutions and pipetting.
-
Prepare a table in your laboratory notebook to put your data in. Make sure
that you have thought about all of the data you will need and leave a place
for your observations. Show it to your instructor as you walk in the door.
Make sure that he/she signs it. (What kind of data do you need? Initial
and final buret readings. Mass of sodium carbonate and lots more!
-
Read Chapter 5, Section 6 (Section 9 in 4th Ed.) of the textbook to learn
more about titrations.
Post lab Questions:
-
Calculate the approximate concentration of a hydrochloric acid solution
prepared by diluting 100 mL of 12.3M HCl to 2.00 liter.
-
Calculate the approximate volume of 0.095 M HCl needed to neutralize 0.25g
of sodium carbonate. Hint: Write a balanced equation first.
-
Calculate the approximate volume of 0.0879 M NaOH needed to neutralize
25.0 mL of 0.095 M HCl. Hint: Write a balanced equation first.
-
Write an equation (including states) for the reaction between carbon dioxide
gas and water. Why is this reaction significant in this experiment?
-
A student failed to rinse a damp buret with a small amount of the acid
before filling it with acid. (p 23 lab handbook). Will more or less titrant
(acid) be required to neutralize the sodium carbonate?
Your report should be in the following format:
Purpose: What you are doing in the lab. The question you are
answering.
Procedure & apparatus: A description of the procedure. This
can be simply the statement: "As given in the lab handout." It should include
any modifications to the experiment.
Data: This section contains all observations, including tables
with measurements, etc.
Calculations: This section must show samples of all of the different
types of calculations. Include any graphs in this section. Show at least
one sample calculation for the Na2CO3 titration and
one calculation for the NaOH calculation. You may feel free to show the
entire square method.
Discussion and errors. A section that describes your results
and how good you think your results are. (For example: Although the
density of my metal is close to the literature value for gold my results
varied widely and the sample did not look like gold.) Although you
may have more, you must describe at least 4 sources of error.
The first line in this section could be "My data is good (or bad) because
……)
Another paragraph should be "My errors include..
1.
2.
Modifications: Describe at least one modification you would make
to improve the accuracy of the procedure. (Presumably it fixes one of the
errors you described.)
Conclusion: It is the answer to the problem posed in the purpose
In this case, " The concentration of the HCl was _____ from a ....
Answers to the post laboratory questions: Answers to the post
laboratory questions.