CHEM 108

Experiment: Standardizing sodium hydroxide solution by titration of KHP

(K. Gorzelska update 2023)

Name _______________________ Name _______________________

Name: _______________________ Lab Section: _______ Date_______

OBJECTIVES In this experiment, you will determine a precise concentration of NaOH solution by titration of potassium
hydrogen phthalate (,KHC8H4O4 - abbreviated KHP) solution with a known concentration.

BACKROUND An unknown concentration of a solution is often determined by titration. Titration is a process in which
solution of known concentration (called standard solution) is added gradually to the solution with unknown concentration,
until the chemical reaction between the two solutions is complete. The titrant is usually (but not always) the solution of
known concentration that is delivered by a burette into a known quantity of the solution of unknown concentration. The
process of determining the unknown’s concentration is called standardization.

Solutions of sodium hydroxide are virtually impossible to prepare to a precise molar concentration because the
substance is hygroscopic. In fact, solid NaOH absorbs so much moisture from the air that a measured sample of the
compound is never 100% NaOH. Also, a solution of sodium hydroxide absorbs carbon dioxide from the air, and it
changes its concentration.

On the other hand, the acid salt potassium hydrogen phthalate, KHC8H4O4, can be measured out in a highly precise
mass amounts. It reacts with NaOH in a simple 1:1 stoichiometric ratio, thus making it an ideal substance to use to
standardize a solution of NaOH.

NaOH(aq) + KHC8H4O4(aq) → NaKC8H4O4(aq) + H2O(l)

In this experiment you will standardize unknown NaOH solution with the accuracy of 3 significant figures.

EQUIPMENT

- 50 mL burette check for leaks

- Erlenmeyer flask

- Solid potassium hydrogen phthalate (KHP) (primary standard reagent).

~ 0.1 M NaOH solution

- Phenolphthalein indicator,
 Wear safey glasses

Tie back and pin up long hair.

Cover as much of the exposed skin as possible. Wear footware that is fully covering your feet.

Both acids and bases are harmfull (corrosive) to human tissue. We will use a base (NaOH) in this lab and you must
know what to do in case you spill it. As you have heard in the first lab, both acids and bases can damage the skin and
eye tissue. The more concentrated the base (or an acid) is, the more hazardous it is.

If you do get any base in your eyes, flush it out immediately with lots of water for several minuters. There are eye
washes in the hallway outside the lab. If you get base on your skin (it will feel slippery) flush that area immediately
under running water for several minutes and then inform your instructor. If you spill an acid or a base all over you, use
the safety shower (in the hallway outside the lab).

If you spill a base on the lab bench or on the floor, clean it immediately. Neutralize base spills with some vinegar (a
dilute acetic acid).

PROCEDURE

Obtained primary standard potassium hydrogen phthalate, KHP, (also known as potassium biphthalate or potassium
acid phthalate) that was dried at 110°C for at least two hours. This has been done for you - you don’t need to dry the
KHP before you use it.

Accurately weigh about 0.4 grams of dried potassium hydrogen phthalate (KHP) (MW = 204.23 g/mole) into an
Erlenmeyer flask and dissolve it in ~ 50 mL of distilled water.

Set up a ring stand and the burette clamp.

Use ~ 100 ml beaker to obtain about 50 ml the NaOH solution to be standardized.

Fill burette with NaOH. Unless absolutely necessary don’t use a funnel (– it is easy to overfill the burette when the stem
of the funnel extends into the burette). CAUTION: Sodium hydroxide solution is caustic! Avoid spilling it on your skin or
clothing

Check for the presence of bubbles (they like to hide below the stopcock). If present, open the stopcock fully (over a sink)
and jerk the burette upwards, then quickly close the stopcock and refill the burette.

Clamp the burette to the stand. Make sure it is not leaking.

Add 3 drops of the indicator (phenolphthalein) into the titration flask. Place the flask below the burette. Adjust the height
of the burette so that the tip of the burette is inside the flask ~ 2 cm below the rim.

Place a piece of white paper under the flask (It will help you to see the color change).

Record the initial volume of NaOH in the burette (with accuracy of 0.01 ml) - when reading volume, use the level of the
bottom meniscus. Please note that burettes are calibrated “to deliver”. Therefore, when “full” the volume on the burette
scale is zero.

You are now ready to begin the titration.

Start by rapidly adding about 12-15 ml of NaOH to the flask. At this stage of titration, the rapidly developing pink color
should equally rapidly disappear. Continuously swirl the titration flask.
Near the endpoint - after adding ~ 12-15 ml of the base, the pink color will persist longer and longer. At this point, adjust
the stopcock to deliver NaOH drop by drop, and do not add the next drop till all the color disappears. Use small
quantities of distilled water from the squirt bottle to rinse down the tip of the burette and sides of the flask (the base there
is “accounted for but did not react with the KHP). The end point of titration is reached when addition of a drop results in
the permanent very light pink color. If the color turns bright pink, you passed the end point of titration and you need to
start over.

Read the volume of NaOH left in the burette (to the 2nd place after decimal point!).

Determine the volume of NaOH used to titrate KHP (the volume at the end point minus the initial volume).

Calculate the concentration of NaOH solution (3 significant figures).

Fill the burette back up with NaOH solution and get a new KHP sample. Repeat the titration. If your first and 2nd titration
are within 3% of each other than you do not need to do a 3rd trial.

Drain the burette then rinse with distilled water.

DATA TABLE 1st titration 2nd titration 3rd titration

Mass of KHP ____________ _____________ _____________

Sample calculation of moles of KHP ___________________________________________________

# Moles of KHP ____________ _____________ _____________

Initial volume of NaOH in the burette ____________ _____________ _____________

(-estimate the second place after decimal!)

Final volume of NaOH in the burette ____________ _____________ _____________

Volume of NaOH used to titrate KHP ____________ _____________ _____________

Calculations

At the end point: # moles NaOH = # moles KHP, Molarity NaOH = # moles NaOH / volume of base used to titrate KHP
(in what units?)

Show sample calculation for 1st titration: ____________________________________________________

1st titration 2nd titration 3rd titration

NaOH [M] __________ __________ ___________

Average concentration of NaOH [M] ____________

 Pre- Lab Assignment
Experiment: Standardizing a Solution of Sodium Hydroxide

Name (please print) ______________________ Section ________ Date _____________________

1. (5 pts) Calculate the mass of sodium hydroxide needed to prepare 100. mL of a 0.10 M solution.

_____________

2. (5 pts) How many sodium ions are present in 100 ml of 0.1 M NaOH solution?

______________

3. (10pts) Calculate the mass of KHC8H4O4 (KHP) (MM = 204.23 g/mol) needed to react completely with 25.00 mL of a
0.100 M NaOH solution according to the following equation.

NaOH(aq) + KHC8H4O4(aq) → NaKC8H4O4(aq) + H2O(l)

____________

4. (5 pts) The reaction between NaOH and KHP is an example of this type of chemical reaction

____________________________________

5. (5 pts) It took 23.16 ml of KOH solution to titrate 0.412 g of KHP. Calculate molarity of the KOH solution.

____________________________________