What Is in this Container: A Capstone Experiment

Ema Condori-Teves
Ames Lab
27 March 2018
Introduction
At an Environmental Protection Agency, an inspector came across an unknown material

was found on the shelf of the laboratory stockroom during his inspection. In order to avoid a fine

for the violation of the Chemical Specific Right-to-Know Act, the inspector gives us three hours

to identify the unknown chemical in the container. The chemical inventory list for the stockroom

provides a list of 12 chemicals that the unknown solution in the container could be.

1. Aluminum (s), Al

2. Sodium hydrogen carbonate (s), NaHCO3

3. Barium chloride (s), BaCl2

4. Ammonia (aq), NH3

5. Formic acid (aq), HCOOH

6. Sodium hydroxide (s), NaOH

7. Hydrochloric acid (aq), HCl

8. Iron (III) chloride (aq), FeCl3

9. Ethanol (l), CH3CH2OH

10. Hexane (l), C6H12

11. Urea (s), (NH2)2CO

12. Potassium sulfate (s), K2SO4

To identify the unknown chemical, we must first generally categorize the chemical by breaking

down it major components to identify its composition. The use of a flowchart will be helpful in

determining the components for the unknown. This will be done by performing a series of

experiments that will help us sort the unknown into is corresponding components.
 To do this we will first determine its solubility in water, and then testing its electrical

conductivity to determine whether the substance is soluble or not. If the unknown happens to be

insoluble, determining its density will aide in determining its density. From there, we will have to

either determine its pH or perform an absorption spectroscopy. Substance composition can also be

determined by determining its freezing point depression, determining its density, or performing a

titration. In case of an absorption spectroscopy, an emission spectroscopy may be need to be

performed, as well as a pH test or a precipitate test. A flowchart can help better determine what

steps are needed and the appropriate order in which they must be completed.

Experimental

List of Chemicals/Equipment to be used:

 M Hydrochloric Acid Solution  Cuvettes and nichrome wires

 pH 4 and pH 7 buffer solutions  Measurenet pH probe and drop counter

 0.1 M Sodium hydroxide solution  Measurenet temperature probe

 0.1 M Silver nitrate solution  Conductivity detector

 0.1 M Barium chloride solution  Styrofoam cup calorimeter and lid

 0.1 M Iron(III) nitrate solution  Volumetric flasks

 0.1 M Sodium chloride solution  Kimwipes

 0.1 M Potassium chloride solution  Crucible and lid

 Distilled water  Ordinary lab glassware

 Measurenet spectrophotometer
 Determine the water solubility of the unknown. To do this you must add a few grams of

the unknown to distilled water in a small test tube or flask and stir or shake this solution. Once

you observe the reaction, determine whether the unknown in soluble or insoluble. Empty

contents of the flask or test tube into a waste container. If the unknown is insoluble, then confirm

the identity as Aluminum(s) by calculating its density. This may be done through the water

displacement method or any other density calculation. If the unknown is soluble then we will

proceed to test its conductivity.

To test the unknown’s solubility, we must add a few grams of the unknown substance to

a test tube with enough water to allow the chemical to ionize and then mix the contents
thoroughly and then pour the contents in the test tube to a watch glass. Then we can place the

conductivity detector electrodes into the solution in the watch glass and determine the brightness

or dimness of the LED light. If the LED does not light up and the substance is liquid, then you

can confirm that it is ethanol by calculating its density either using water displacement or another

method. If the LED does not light up, and the substance is solid, we can confirm the unknown is

urea by calculating the freezing point depression.

To calculate the freezing point you will need to prepare the measurenet accordingly and

set the minimum temperature to about -10˚C, and the maximum temperature to about 25˚C. Then

prepare an ice bath using a 500 ml beaker and set up the equipment necessary to determine the

freezing point depression. Then prepare an aqueous solution by adding about 20 mL of water to

1 g of the unknown. Then insert the temperature probe into the test tube and record the data

while stirring continuously until the prepared solution is frozen. Preform two trials of this.

If the LED light is weak, test for pH using a pH probe. If the pH tested indicates that the

solution is acidic, titrate the solution with 0.1 M Sodium hydroxide to confirm that it is formic

acid. To do this you must set up the measurenet station so that it records pH vs volume and set

up the equipment necessary to perform a titration. Run the titration twice for accurate results. If

the pH tested indicates that the solution is basic, confirm the solution is ammonia by titrating

with 0.1 M Hydrochloric acid using the same titration set up as explained above. Preform a

second trial of this as well.

If the LED is strong, then test for absorption spectroscopy. To do this you must set up the

measurenet system and spectrophotometer to record the spectroscopy and emission. It is

important to not forget to zero, and reference before recording the data for the sample cuvette

that was prepared with the unknown solution and water. Check to make sure graph is recorded
correctly. If the absorbance is between 250 nm and 800 nm the substance is iron (III) chloride. If

no absorbance is recorded, a test for emission spectroscopy must be done.

To perform an emission spectroscopy, you must set up the Measurenet system and

spectrophotometer to record spectroscopy and emission. To do this you must use the Bunsen

burner and clean it properly with distilled water using the spatter technique before sampling the

unknown. Next sample the prepared solution of the unknown with water and test it by spattering.

If there is no emission recorded, confirm that the solution is Hydrochloric acid by testing the pH.

To do this you will need to use the pH probe and confirm that the pH is less than 1.5.

If the emission intensity recorded is between 740 nm, 831 nm, and 873 nm, then confirm

that the unknown solution is barium chloride by adding 0.1 M silver nitrate to an unknown

solution and confirm a precipitate is formed. If the emission intensity is 765 nm or 771 nm then

confirm that it is potassium sulfate by adding 0.1 M barium chloride to the unknown solution and

a precipitate should form. If the emission intensity recorded is 589 nm then test for the pH using

the pH probe. If the pH tested is greater than 10 then you must confirm that it is sodium

hydroxide by adding 0.1 M iron (III) nitrate to the unknown solution and a precipitate should

form. If the solution is less than 10 pH then confirm that the unknown is sodium hydrogen

carbonate by titrating with the 0.1 M Hydrochloric acid. Remember to perform the titration

twice.

Results

Bibliography
Stanton, B., Zhu, L., & Atwood, C. H. (2010). Experiments in general chemistry featuring
measurenet: guided inquiry, self-directed, and capstone. Belmont, CA: Brooks/Cole,
Cengage Learning.