Acid-Base Chemistry

Standardization of a NaOH Solution

For the next part of the green crystal lab, you will need a standardized solution of NaOH. In this
experiment, you will be standardizing (determining the normality) of the base solution. The accuracy of
these analyses will depend on the care you use in doing this experiment. Titrations can be done very
precisely and accurately. You should strive for both in your work.
You will determine the concentration of your NaOH solution by using it to titrate an accurately
weighed sample of a solid acid salt, potassium hydrogen phthalate (abbreviated KHP). This process is
called standardization, and the KHP is referred to as the primary standard.
Primary standard substances must have certain properties. They should be available in a state of
known purity, should be easy to dry and should not pick up moisture from the air, and should have a high
gram equivalent weight. There are several good primary standard acids. We will be using KHP, which is
available in purity of 99.95% or better, is easily dried and stable at 110oC, and has a molecular weight of
204.22 g/mole. Only one of the hydrogen dissociates, so its gram molecular weight is also its gram
equivalent weight. Therefore one mole of KHP will exactly neutralize one mole of NaOH.

Equipment and Chemicals:

solid KHP two 250-ml Erlenmeyer flasks 250-ml beaker

50-ml buret NaOH solution ~ approx. 0.1 N buret clamp
buret funnel bottle of phenolphthalein indicator ring stand

Procedure:

1. Samples of dry KHP are available in the drying ovens. Weigh out approximately 0.5 - 0.8 grams. This
sample must be weighed accurately so you will be weighing by difference. Weigh the plastic
container holding the KHP, measuring to milligram accuracy on the top-loader balances. Remove a
small sample and put this sample directly into a 250-ml Erlenmeyer flask. Reweigh the plastic
container. The weight lost should equal the mass of KHP transferred to the flask. Each person will
perform two titrations, so you will need to repeat this weighing procedure, but move on to the next
step before doing the second weighing! [Don't tie up the balances - let others use the balance while
your first sample is being dissolved!]

2. Add approximately 50 ml of distilled water to the Erlenmeyer flask. (Why is the exact volume of
water added not important?) Shake each flask gently to help the solid dissolve. If a hot plate / stirrer
is available, put the heat on a very low setting (#1), add the stir bar, and stir the solution.

3. While you are waiting for the KHP to dissolve, go ahead and prepare your buret. Fill a 250-ml beaker
with tap water and rinse your buret at least twice. Be sure to let water run through the tip as well.
Rinse one more time with distilled water. Check to see if any water droplets adhere to the inside of
the buret. If beading occurs, your buret needs to be cleaned with a soap solution. If you must wash
your buret with a soap solution, be sure to thoroughly rinse all soap residue from the burets -
including a distilled water rinse.
4. Using a small buret funnel, pour about 10 ml of the NaOH solution into the buret. This wash serves
to remove any water from the buret. Be sure to let some of the base solution drain through the tip.
Empty the buret of this wash solution. DO NOT WASTE THE NaOH SOLUTION BECAUSE YOU
WILL NEED TO USE IT FOR LATER LABS AS WELL. IF YOU RUN OUT OF BASE
SOLUTION, YOU WILL NEED TO RESTANDARDIZE A WHOLE NEW BATCH!!!

5. Fill the buret slightly above the zero mark at the top of the buret (about 1 inch above the markings).
Allow the base solution to drain, filling the tip. Check to make sure that the bottom of the meniscus
sits on the 0.00-ml line for your first titration.

6. Hopefully the solid KHP has completely dissolved at this point. Since it takes some time for the solid
to dissolve, it may be a good idea to go ahead and weigh out your other samples. (You and your
partner are doing a total of four titrations - each of you are doing two apiece.) Vary the amount of
KHP used for each sample by at least 0.050 grams.

7. When the KHP has completely dissolved add 5 - 7 drops of the phenolphthalein indicator to the acid
solution.

8. Titrate the solution in the Erlenmeyer flask with the NaOH solution to the first permanent pink color,
being sure to stir constantly. [If the automatic stirrers are available, you may use them.] (A permanent
color means one that lasts at least 30 seconds. CO2 from the air will lower the pH of the solution
slightly, so the pink color may fade after about one minute.) Whatever you do, do not overshoot
the endpoint! A dark magenta color means you have gone too far! It also means you will need to do
at least one additional trial!

Some tips on how to avoid overshooting the endpoint:

a. Constant stirring will help the solutions mix better, and will allow the base to react with
the acid quicker.
b. You can tell when you are approaching the endpoint because where the drops of base enter
the solution, there will be a pink area. This area will enlarge and become more persistent
as you get closer to the equivalence point.
c. The stopcocks are designed to be turned in either direction. Positioning the stopcock
perpendicular to the barrel completely stops the flow. If you will practice quickly turning
the stopcock 180o, you can actually master the skill of adding 1/2 drops. One drop is only
0.05 ml, so you can theoretically increase the volume by only 0.025 ml!

9. Record the total volume of NaOH solution used. Record the initial buret volume reading as well as
the final buret volume reading. Remember that the scale is inverted - as the volume goes down, the
marking increase. If you started at the 0.00-ml mark and the final volume reading has the meniscus
sitting on the 24.50-ml mark, you have used 24.50 ml of NaOH solution. All buret readings should
be read to the nearest 0.00-ml mark. The hundredth reading is the approximation - estimate it as
either .00-ml or .05-ml.

10. Repeat the titration with your other sample.

11. The reason for the four trials is for accuracy as well as precision. You need at least three trials that
agree to within 0.004. If only one trial deviates from the average normality by more than 4%, it may
be discarded. If more than one trial shows too much deviation, though, you will need to perform an
additional titration.
 Data Table

Mass of KHP used: Trial #1 Trial #2 Trial #3 Trial #4

Initial mass of container (in grams) ___________ __________ __________ _________

Final mass of container (in grams) ___________ __________ __________ _________

Mass of KHP (in grams) ___________ __________ __________ _________

Titrations:

Final buret reading (in ml) ___________ __________ __________ _________

Initial buret reading (in ml) ___________ __________ __________ _________

Volume of NaOH used (in ml) ___________ __________ __________ _________

Calculated Data

1. Number of moles (equivalents)

of KHP weighed out _____________ ____________ ____________ _________

2. Number of equivalents of NaOH

used to neutralize the KHP _____________ ____________ ____________ _________

3. Volume of NaOH used to reach

the endpoint (in liters) _____________ ____________ ____________ _________

4. Normality of NaOH solution _____________ ____________ ____________ _________

5. Average normality of NaOH solution _____________

6. Deviation from average ____________ ___________ ___________ _________

7. Average deviation _____________