Experiment 32: What is in this Container?

A Capstone Experiment
Introduction
An Environmental Protection Agency inspector was inspecting a

laboratory stockroom when he came upon a container that was filled with an

unknown material. In order for the stockroom and laboratory program to

avoid a fine (due to violation of the Chemical Specific Right-to-Know Act) the

unknown chemical must be determined within 3 hours. There are 12

chemicals on the inventory list that the unknown material could be:

1. Aluminum
2. Sodium hydrogen carbonate
3. Barium chloride
4. Ammonia
5. Formic acid
6. Sodium hydroxide
7. Hydrochloric acid
8. Iron(III) chloride
9. Ethanol
10. Hexane
11. Urea
12. Potassium sulfate

In order to identify the unknown chemical, we must categorize the

chemical first generally, then working to more specific until determine the

composition. Through the use of a flowchart, we will perform a series of basic

experiments to breakdown each component of our unknown.

First, we will determine solubility in water, then electrical conductivity

if the substance is soluble. If the substance is insoluble, density can be used

to determine identity. From there, we will either determine pH, perform

absorption spectroscopy, or confirm substance composition by determining

freezing point depression, density, or titration. If absorption spectroscopy

was used, a conclusion can be made or emission spectroscopy will be tested,

followed by a pH test or precipitate test. The flowchart below demonstrates

the order of steps and which steps are appropriate for each circumstance.
Experimental
Chemicals

A. 0.1 M Hydrochloric acid solution

B. pH 4 and pH 7 buffer solutions
C. 0.1 M Sodium hydroxide solution
D. 0.1 M Silver nitrate solution
E. 0.1 M Barium chloride solution
F. 0.1 M Iron (III) nitrate solution
G. 0.1 M Sodium chloride solution
 H. 0.1 M Potassium chloride solution
I. Distilled water

Equipment

A. MeasureNet spectrophotometer, cuvettes, and nichrome wires

B. MeasureNet pH probe and drop counter
C. MeasureNet temperature probe
D. Conductivity detector
E. Styrofoam cup calorimeter and lid
F. Volumetric flasks
G. Kimwipes
H. Crucible and lib
I. Ordinary lab glassware

Procedure

Place the unknown sample and 50ml of distilled water in a 100ml

beaker; stir the 100 ml beaker. If it is soluble, conduct an electrical

conductivity test. If it is insoluble identify what the original state your

unknown is, it should be a solid or liquid. If it is a solid, confirm it is aluminum

through calculating its density. To calculate its density record and fill a

graduated cylinder with distilled water. Add a recorded mass of your sample.

Then record the final mass. If it is a liquid, confirm it is hexane through

calculating its density by repeating the water displacement method.

To test electrical conductivity, dissolve the unknown chemical in

enough water to allow the chemical to ionize. Place the wire in the solution

and judge the LED light brightness. If it does not light up, and the substance

is solid, confirm that it is urea by calculating freezing point depression.

Prepare the MeasureNet system and set the minimum temperature to -10C
and the max temperature to 25C. Prepare an ice bath with water and ice in

a 600 mL beaker. Use a test tube, ring stand, clamp, rubber stopper, and

temperature probe to determine freezing point depression. Insert the

temperature probe into the rubber stopper, and the probe into the test tube.

Connect the test tube to the ring stand and make sure that it can become

immersed in the ice bath (Figure 1). Prepare an aqueous solution by adding

20 mL of water to 1 gram of unknown sample in the test tube. Press start in

the workstation, stir continuously. Once the solution is frozen press stop and

save file. Perform a second trial. If it does not light up, and the substance is

liquid, confirm that it is ethanol by calculating density using water

displacement.

If the LED light is weak, test for pH using the pH probe. If the solution is

acidic (> 7 pH) titrate with 0.1 M Sodium hydroxide to confirm that it is

formic acid. Use ring stand,

Figure 1: Ice bath-ring stand

set up for freezing point
depression
burette, and drop counter set up to titrate the unknown. Press start on the

workstation, stir continuously. Once the titration is complete, press stop and

save file. If the solution is basic (< 7 pH) titrate with 0.1 M Hydrochloric acid

using the same set up as used to titrate the acid to confirm that it is

ammonia. Perform a second trial of each titration.

If the LED light is strong, test for absorption spectroscopy. Set up

MeasureNet system and spectrophotometer to record spectroscopy and

absorbance. Enter station number, zero the system, sample the reference

cuvette, then sample a cuvette fill with a solution of water and the unknown.

If absorbance is between 250 nm and 800 nm, the substance is iron (III)

chloride.

If no absorbance is recorded, test for emission spectroscopy. Set up

MeasureNet system and spectrophotometer to record spectroscopy and

emission. Clean bunsen burner by placing a water glass of water near the air

intake and using a heated nichrome wire to spatter. Next, prepare a solution

of the unknown and water, pour approximately 1 mL of the solution onto the

watch glass, and spatter the solution while pressing sample at the moment

the heated wire touches the solution. If there is no emission, confirm that it is

hydrochloric acid by testing pH. Using the pH probe, confirm that the pH is

less than 1.5. If the emission intensity is 740 nm, 831 nm, or 873 nm,

confirm that it is barium chloride by adding 0.1 M silver nitrate to an

unknown solution and a precipitate should form. If the emission intensity is

765 nm and/or 771 nm, confirm that it is potassium sulfate by adding 0.1 M

barium chloride to an unknown solution and a precipitate should form.

If the emission is 589 nm, test for pH using the pH probe. If the solution

is greater than 10 pH, confirm that it is sodium hydroxide by adding 0.1 M

iron (III) nitrate to an unknown solution and precipitate should form. If the

solution is less than 10 pH, confirm that it is sodium hydrogen carbonate by

titrating the unknown with 0.1 M hydrochloric acid. Perform a second trial of

titration.

Results
Freezing Point Depression
Trial 1
mL of water Initial Final temperature Mass of unknown
temperature

Trial 2
mL of water Initial Final temperature Mass of unknown
temperature

Density
Density mL of water Mass of unknown

pH
Unknown Trial pH

Titration
Trial 1
Initial molarity mL used to titrate

Trial 2
Initial molarity mL used to titrate

Absorbance
Absorbance Peaks

Emission
Emission Peaks

Bibliography
Stanton, B., Zhu, L., & Atwood, C. H. (2015). General chemistry lab manual:

Chem 1215 and Chem 1225. Boston, MA: Cengage Learning.