General Chemistry: Lab 4: Thermodynamics II

General Chemistry
Laboratory Resources
Chem 152
Lab 4: Thermodynamics II
The Temperature Dependence of the Solubility Product (Ksp), Heat of

Solution (Hºsoln), and Entropy of Solution (Sºsoln)
Procedure Overview
Part A
 Obtain KCl stock solution in a beaker
 Using a 50 mL volumetric flask and the digital pipettor, dilute the stock solution with DI water,
according to your prelab calculations, making the five required KCl standard solutions and
transferring the solutions to the test tubes
 Using a 50 mL volumetric flask and the digital pipettor, dilute the KCl/KHP solution with DI
water, according to the instructions, and transfer the solution to a test tube
 Take the test tubes containing the standard solutions and diluted KCl/KHP solution to the
photometer station
 Use the beaker of DI water to calibrate the instrument according to the outlined procedure
 Analyze each of the standards and the sample, recording the intensity reading for each once it
stabilizes
Part B
 Set up the buret and ring stand, then rinse the buret with tap and DI water
 Obtain NaOH in a beaker and rinse the buret twice with small portions of NaOH
 Fill the buret with NaOH, making sure any air bubbles are removed from the tip
 Record the initial level of NaOH in the buret
 Weigh out KHP – record the mass
 Transfer the KHP to an Erlenmeyer flask, add a stir bar and DI water, and stir until dissolved
 Add the phenolphthalein indicator and titrate to the faint-pink endpoint
 Record the final volume of NaOH in the buret
 Calculate the concentration of NaOH
 Refill the buret and repeat for a second titration; if the two calculated values for [NaOH] are
more than 5% different, perform a third titration to obtain reproducible agreement
Part C
 Refill the buret with NaOH and record the initial level in the buret
 Use the digital pipettor to deliver 1 mL of one of the saturated KHP solutions to a flask,
recording the exact temperature for that solution
 Add DI water, a stir bar, and phenolphthalein indicator
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 Titrate to the faint-pink endpoint

 Record the final volume of NaOH in the buret
 Repeat for all six saturated KHP solutions, recording the exact temperature for that solution
 Use the digital pipettor to deliver 3 mL of the KHP/KCl solution to a clean flask and titrate it as
you did the other solutions
 Repeat the titrations of both room temperature solutions two more times for a total of three
titrations of each
Materials
To be checked out from the stockroom:
Digital pipettor
Digital thermometer
10 mL buret
Magnetic stir bar
Note: You are required to leave your UW Student ID card with the stockroom while you have items
checked out.
From your lab drawer:

125 mL Erlenmeyer flask
(2) 50 mL volumetric flasks
(2) 100 mL beakers
(6) small test tubes
Test tube block
Spatula
Plastic buret funnel
Grease pencil
1-L waste bottle
Provided in the lab:

Flame photometers (1/section)
0.0050 M potassium chloride (KCl) stock solution
Solid potassium hydrogen phthalate (KHP)
(7) Saturated KHP solutions
~0.1 M sodium hydroxide (NaOH) solution
Phenolphthalein indicator solution in dropper bottles
Digital pipettor tips
Balances and weighing paper
Magnetic stirrer
White cards with black tape for reading burets
Kimwipes
Plastic wash bottle of deionized water
pH paper for waste solutions
Sodium bicarbonate and 1 M HCl for neutralizing waste
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PROCEDURE
A. Flame emission determination of K+ concentration in the 0.50 M KCl + KHP (sat)
solution
I. Preparation of K+ calibration standards from the 0.0050 M KCl stock solution

1. Obtain 15 mL of 0.00500 M KCl from the dispenser bottle.
2. Using a clean 50 mL volumetric flask and a digital pipettor, prepare 50 mL of
7.5 x 10-5 M KCl from 0.00500 M KCl solution. Transfer the solution to a clean test tube clearly
labeled with the concentration of KCl (i.e. 7.5 x 10-5 M KCl).
3. Similarly prepare the following standards and appropriately label each tube:
a. 1.50 x 10-4 M KCl
b. 2.25 x 10-4 M KCl
c. 3.00 x 10-4 M KCl
d. 3.75 x 10-4 M KCl.
II. Dilution of 0.50 M KCl + KHP (saturated) solution
The saturated solution is too concentrated for the flame photometer and must be diluted by a factor
of 2,500!
1. Using the digital pipettor, withdraw 1 mL of clear solution from the 0.50 M KCl + KHP (sat)
solution and transfer this to a clean 50 mL volumetric flask.
2. Add DI water to the mark. Cap the flask and mix by inverting several times. Take 1 mL of this
solution and add it to a second clean 50 mL volumetric flask. Add DI water to the mark and mix.
The original sample is now diluted by a factor of 50 x 50 = 2500. Transfer this solution to a
clean and appropriately labeled test tube. Discard the remainder of these solutions in the 1L
waste bottle.
3. Notify your TA when all of your samples are ready for analysis. Then continue to Part B until
the instrument is available.
III. Measurements using the flame photometer
1. To calibrate the instrument, place the sample inlet tube into the beaker of blank solution
(deionized water) provided next to the flame photometer; fill if necessary using the deionized
water tap. The blank solution will be aspirated into the flame. Turn the 'blank' knob until the
intensity reading on the digital display reads "0." DO NOT adjust the 'fuel' knob.
2. Next, aspirate the highest concentration standard solution (3.75 x 10-4 M) by placing the
sample inlet tube directly into the test tube and turn the 'fine sensitivity' knob until the intensity
reading on the digital display reads "375." You should aspirate for approximately 10 seconds to
get a stable reading. The flame photometer is now calibrated.
3. Aspirate the lowest concentration standard and record the intensity. Proceed to the next
higher concentration and record the intensity; repeat until all of the calibration standards have
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been measured. Make a rough plot of your data in your notebook. Do your values make sense?
For example, the 7.5 x 10-5 M standard should read an intensity of approximately 75 units.
4. Aspirate and record the intensity of the 1:2500 diluted sample of the 0.50 M KCl + KHP (sat)
solution.
B. Standardization of the ~0.1 M NaOH (aq)

1. Use a buret clamp to secure the 10-mL buret to a ringstand. Make sure the clamp holds the
buret securely so the buret does not slip out and break. Thoroughly rinse the buret with tap
water and then deionized water. The final deionized water rinse should drain evenly from the
inside surfaces of the buret and leave no droplets behind. If necessary, repeat the deionized
water rinsing until the buret drains cleanly.
2. Obtain approximately 80 mL of 0.1 M NaOH solution in a 100-mL beaker. Label the beaker
NaOH. Rinse the buret twice with ~ 3 mL of the NaOH solution, draining the rinsings into the 1
L waste bottle, then fill the buret with this solution. Make sure the tip is filled with solution. Air
bubbles can be removed by opening the stopcock so that the flowing solution forces out any air
bubbles. Adjust the amount of solution in the buret so that the level is between 0 and 0.5 mL on
the scale. It is not necessary that the initial level read exactly 0 mL, but it must be at or below
the start of the scale.
3. Record the initial level of the buret, keeping your eye level with the bottom of the meniscus. Be
sure to get an accurate reading to  0.02 mL.
4. Rinse the 125 mL Erlenmeyer flask twice with deionized water.
5. Weigh out 0.13  0.02 grams of KHP on a sheet of weighing paper; record the exact mass.
Transfer this sample into the Erlenmeyer.
6. Add ~ 20 mL of deionized water to the Erlenmeyer add a stir bar and stir using the magnetic
stirrer until all the KHP has dissolved.
7. Add 2-3 drops of phenolphthalein indicator solution to the Erlenmeyer.
8. Titrate the KHP solution to a faint-pink endpoint. Add NaOH solution dropwise near the
endpoint. When the solution reaches a permanent faint-pink color, record the volume from the
buret.
9. Repeat the titration on another sample of KHP. If the two titrations do not agree within 3%
perform a third KHP titration.
10. Use your 1 L bottle to collect your waste solutions.
C: Titration of KHP Samples

1. Fill the buret with the standardized NaOH solution. Record the initial level of the buret, keeping
your eye level with the bottom of the meniscus. Be sure to get an accurate reading to  0.02
mL.
2. Note: Bring both your Erlenmeyer flask and pipettor to the ice and water baths so you
can quickly dispense from the pipettor after withdrawing your sample. Use your digital
thermometer to measure the temperature of each solution. You will obtain a 1 mL sample
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from one of the following six KHP solutions provided in the lab: 0 ˚C (ice bath), room
temperature (~22 ˚C), 35 ˚C, 45 ˚C, 55 ˚C, and 65 ˚C. Prepare to use the digital pipettor by
adjusting the volume setting to 1 mL (1000 µL) and placing a clean plastic tip on the end.
Before you immerse the tip of the digital pipettor in the solution, depress the button to the first
stop. Taking care to not disturb the KHP solid at the bottom of the flask, insert the tip into the
solution and release the button slowly to draw up 1 mL of the solution. Dispense the 1 mL
sample into a clean 125 mL Erlenmeyer flask by depressing the button to the second stop.
Discard the plastic tip in the trash.
3. Add ~ 20 mL of deionized water to the Erlenmeyer flask. Add 2-3 drops of phenolphthalein
indicator. Add a magnetic stir bar, place on a magnetic stirrer, and begin stirring.
4. Read the initial volume in the buret.
5. Titrate to the first permanent faint pink color. You may need to refill the buret for the higher
temperature solutions. Remember to go drop by drop as you approach the endpoint. As you
approach the endpoint, the pink color will spread out much more than observed earlier. Do not
over titrate. If you think you over titrated, repeat the titration. Record the volume corresponding
to the phenolphthalein endpoint.
6. Refill the buret with NaOH and titrate (steps 2 - 5) the remaining KHP solutions listed in step 2.
7. Repeat the titration of the room temperature solution 2 more times to obtain a total of 3
titrations of that sample.
8. For the seventh solution, room temperature KHP with KCl added (~22 ˚C), obtain a 3 mL
sample using the pipettor, dispense into the Erlenmeyer flask, and titrate according to steps 3 -
5 above. Repeat this titration 2 more times to obtain a total of 3 titrations for that sample.
9. Use your 1 L bottle to collect your waste solutions.
Waste Disposal
All solutions must be between 5 and 12 pH units before being poured down the sink with water. You
can lower the pH by adding 1M HCl, or raise it by adding small amounts of sodium bicarbonate.
Before You Leave the Lab

1. Upon completing the work (includes all requested calculations and plots), show your work to your
TA.
2. Clean your lab bench and have your TA check your equipment drawer, lab bench, and lab
notebook.
3. Obtain your TA’s signature in your lab notebook and turn in the duplicate copies of your lab
notebook pages associated with this experiment.
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Information to Enter in your Notebook during the Lab

 Concentration of stock KCl solution
 Volumes of stock KCl solution required to make 50 mL of each standard solution in
Part A.
 Details of the dilution of the KHP/KCl solution so that you can account for the dilutions when
calculating the K+ concentration of the solution for the post-lab report
 Intensity reading from the photometer for each standard KCl solution and the diluted KHP/KCl
solution
 Mass of KHP for each KHP-NaOH titration in Part B
 Initial and final volume readings from the buret for each KHP-NaOH standardization titration in
Part B
 Calculation of NaOH concentration for each KHP titration showing that your data is reproducible
(within 3% of each other)
 The actual temperature for each KHP and KHP/KCl solution you titrate in Part C
 Initial and final volume readings from the buret for each KHP titration in Part C
 Any other notes or observations that will help when you work on your post-lab report or need to
explain your results
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What is the goal of this experiment?

What are the main steps involved in the experiment?

General Chemistry

The Temperature Dependence of the Solubility Product (Ksp), Heat of

 Titrate to the faint-pink endpoint

From your lab drawer:

Provided in the lab:

I. Preparation of K+ calibration standards from the 0.0050 M KCl stock solution

B. Standardization of the ~0.1 M NaOH (aq)

C: Titration of KHP Samples

Before You Leave the Lab

Information to Enter in your Notebook during the Lab

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