What is in this Container: A Capstone Experiment

Joshua Ong, Elizabeth De Tienne

April, 22, 2015

Introduction:

This experiment will use many processes to determine the identity of a chemical. This is because

an unknown material has been identified by the Environmental Protection Agency, and a fine will be

issued if it is not identified in three hours under the Chemical Specific Right-to-Know Act. To the labs

advantage, the chemical inventory list has only 12 chemicals lists for the stock room. Using a wide range

of processes, the identity of the container will be found.

A density experiment will be conducted through water displacement. Density is the

measurement of a certain amount of mass per volume. Mass can be measured on a scale, and volume is

measured by the displacement of water. Density can be used to identify substances.

Freezing point depression is a colligative property. This phenomenon occurs because the liquid

solution has a lower vapor pressure than the solid state. The freezing point depression is directly

correlated to how many molecules of substance are added, rather than identity. If the initial molar mass

and molality are recorded the molar mass can be solved for from this colligative property.

An emission analysis of aqueous solutions will be used to identify the sample in certain

situations. Emission spectroscopy is preferable to absorption spectroscopy in colorless aqueous solution

such as the group 1A metals. In this experiment the sample will be excited by heat using a Bunsen

burner. The wave length of the emitted light is characteristic of a particular metal. A spectrophotometer

will record the wavelength and intensity. The unknown sample will then be compared to the spectra of

water samples containing known metal ions to identify it.

Absorption spectroscopy will be used to identify the sample in certain situations. Absorption

spectroscopy is a process of measuring light intensity before and after it passes through an aqueous

solution. Refraction and diffraction will be nullified by using a blank solution, a solution containing no
absorbing species. First serial dilutions will be prepared of the unknown sample so that samples with

known higher and lower concentrations than the sample are collected. The amount of light absorbed is

directly proportional to concentration. The absorption spectras lambda max -the maximum absorbance

line- will then be compared to the spectra of water samples containing known metal ions to identify it.

In completing this lab the identity of the material in the stock room will be determined. The

molarity can also be determined in the titrations. This lab is a summary of all semester two experiments,

testing our knowledge of acids and bases, transition metals, solubility, and colligative properties.

Experiment:

Receive materials: unknown chemical, .1 M hydrochloric acid solution, pH 4 and pH7 buffer

solutions, .1 M sodium hydroxide solution, , .1 M silver nitrate solution, , .1 M barium chloride

solution, .1 M Iron (III) nitrate solution, , .1 M sodium chloride solution, , .1 M potassium

chloride solution, distilled water, MeasureNet spectrophotometer, cuvetttes, nichrome wires, ,

MeasureNet pH probe and drop counter, , MeasureNet temperature probe,conductivity

detector, Styrofoam cup calorimeter and lid, volumetric flasks, kimwipes, crucible, lid, and

ordinary lab glassware. (You may only need some of these materials in the experiment.)

Place the unknown sample and 50ml of distilled water in a 100ml beaker; stir the 100 ml beaker.

If it is soluble proceed to step 6. If it is insoluble identify what the original state your unknown is,

it should be a solid or liquid.

If it liquid proceed to step 5. 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.
After the experiment, calculate the density of the unknown to be 2.70 g/mL. Note: the mass of

water is one gram per mL.

If it is a liquid, confirm it is hexane 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.

After the experiment calculate the density of the unknown to be .655 g/mL. Note: the mass of

water is one gram per mL.

Gather the conductivity detector (LED light and wire), distilled water, the unknown chemical,

and a petra dish.

Add the chemical and water into the petra dish. The amount of water used should be much

more than chemical used, to allow the chemical to ionize in solution.

Place the wire of the LED light into the solution.

Judge if the LED if off (proceed step 7), shining dimly (proceed step 9), or shining brightly

(proceed step 11).

If it liquid proceed to step 8. If it is a solid confirm it is urea through experimentally calculating

its freezing point depression. (lab 17)

Prepare the measureNet system using Appendix A-1. Set the minimum temperature to -10C

and the max temperature to 25C.

Prepare 300mL of distilled water into a 600ml beaker, and then fill the beaker to 500ml with ice.

(This is called the ice bath)

Gather the 25 x 200 mm test tube, ring stand, clamp, rubber stopper, and temperature probe.

Insert the rubber stopper and temperature 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. Note: the

temperature probe needs to be covered in at least 2cm of solution.

Prepare an aqueous solution by adding 20 mL of water to 1 gram of unknown sample. Record

this.

Secure the test tube onto the ring stand, immersed in the ice bath. Press start in the

workstation, stir continuously.

Once the solution is frozen press stop. Press file options, f3, save your file name (e.g.001), and

press enter. Press display to view the previous scan.

Clean all chemicals into the sink wash and dry thoroughly. Repeat all of step 7 in another trial.

If it is a liquid, confirm it is ethanol 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.

After the experiment calculate the density of the unknown to be .655 g/mL. Note: the mass of

water is one gram per mL.

Use the pH probe to determine if the solution is acidic or basic. If it is acidic proceed to step X. If

the solution is basic continue to confirm it is ammonia. Record the starting molarity and liters

used in the experiment. Use appendix F to titrate the unknown with .1 M hydrochloric acid.

Repeat step 9 in a second trial.

After the experiments calculate the moles used to react with hydrochloric acid. Calculate the

pKb to be 1.8x10^-5.

If the solution is acidic continue to confirm it is formic acid. Use appendix F to titrate the

unknown with .1 M hydroxide acid. Record the starting molarity and liters used in the

experiment. Use appendix F to titrate the unknown with .1 M hydroxide. Repeat step 10 in a

second trial.

After the experiments calculate the moles used to react with hydroxide. Calculate the pKa to be

1.8x10^-4.
To confirm the unknown solution is iron (III) chloride an absorption spectroscopy will be

performed, it is not proceed to step 12. See appendix D for how to perform an absorption

spectroscopy. Note: standard solutions of the unknown solution are not prepared as the

concentration does not need to be calculated. It should be found that iron (III) chloride has an

absorbance spectrum from 200 800nm. The lambda max highest consistent point of graph-

can be found to be at 456.57.

Next use the pH probe to determine if the solution is acidic (proceed to step 13), basic (proceed

to step 14), or neutral (proceed to step 15).

If the solution is acidic continue to confirm it is hydrochloric. Use appendix F to titrate the

unknown with .1 M hydroxide acid. Record the starting molarity and liters used in the

experiment. Use appendix F to titrate the unknown with .1 M hydroxide. Repeat step 10 in a

second trial.

After the experiments calculate the moles used to react with hydroxide. Calculate the

equivalence point to be 7.

If the solution is basic continue to confirm it is sodium hydroxide or sodium hydrogen carbonate.

Record the starting molarity and liters used in the experiment. Use appendix F to titrate the

unknown with .1 M hydrochloric acid. Repeat step 9 in a second trial.

After the experiments calculate the moles used to react with hydrochloric acid. Calculate the

pKb to be 2.1x10^-8 for sodium hydrogen carbonate or an equivalence point of 7 for sodium

hydroxide.

If the solution is not acidic or basic an emission spectrum will be performed to confirm the

sample is barium chloride or potassium sulfate. Clean a nichrome wire by placing 5ml of 6M HCL

in a 50-ml beaker. Measurements do not need to be exact or measured.

Swish the nichrome wire in the beaker for 30-40 seconds.

Rinse the wire with 30-50 ml of distilled water, and pour the used acid into the waste container.

Measurements do not need to be exact or measured.

Review appendix E to prepare the MeasureNet system for recording data.

Pour a small amount of distilled water into a watch glass.

Quickly put a heated nichrome wire onto the distilled water and aim the gases into the Bunsen

burners intake.

Using the graph determine the peaks. If there are two peaks at 550 nm confirm it is barium

chloride. If there are two peaks at 770 nm confirm it is potassium sulfate.

 Results:

Trial A freezing pt. depression:

Depression (change in temp) = Depression constant * molality

Depression constant for water 1.86 C/molal

freezing pt. depression mL of water initial temp final temp mass of unknown
20.0 20.78 C -1.86 1.00

Trial B freezing pt. depression:

freezing pt. depression mL of water initial temp final temp mass of unknown
20.00 2-.16 -1.69 1.00

Trial 1
25

20

15

Temp (C) 10

0
0 50 100 150 200 250 300
-5
Time
 Trial 2
25

20

15

Temp (C) 10

0
0 50 100 150 200 250 300
-5
Time

density lab:

D = m/v

grams of
Density ml of water substance

Trial A titration:

pH= pKa+ log(A-/HA)

pH= pKb+ log(HA/A-)

titration initial molarity mL used to titrate

Trial B titration:
titration initial molarity mL used to titrate

Emission Lab

emission peaks

Absorption

absorbance peaks
Discussion:

This experiment used several different processes to determine the identity of a chemical. This is

because an unknown material was identified by the Environmental Protection Agency, and a fine can be

issued if it is not identified in three hours under the Chemical Specific Right-to-Know Act. To the labs

advantage, the chemical inventory list has only 12 chemicals lists for the stock room. Using three

processes, the identity of the container was found.

I believe the experiment was accurate and precise. The solubility and conductivity of the

unknown, although measured qualitatively, was very accurately determined. This is because the

qualitative experiment observations adhere to a strict dichotomy. The solubility will either mix into

solution or will not. The conductivity can be compared by first touching the wire together to see how a

full circuit emits light, compared to an ionized solution. Finally urea was confirmed through freezing

point depression. The molar mass was determined within a 5 gram derivation in two trials.

There are some errors that could have been altered to make this experiment more accurate.

Without more examples of weak and strong electrolytes, it may be hard to differentiate between them.

The freezing point depression also doesnt flatten for a long period of time, and may be hard to identify.

Conclusions:

In completing this lab the identity of the material in the stock room will be determined. This lab

is a summary of all semester two experiments, testing our knowledge of acids and bases, transition

metals, solubility, and colligative properties. The experiment also requires one to identify if a materials

phase, testing conductivity, and testing absorption and emission spectroscopies.

 Three processes were used to identity of the container was found. The identity was first mixed

to see if it was miscible in water. When unknown number 8 was mixed in water, the compound was

found to be water soluble. The unknown was next, in solution, tested to see if it was an electrolyte.

Because the solution produced no LED light, it was determined to be a nonelectrolyte. Finally a freezing

point depression was performed to confirm the unknown was urea. The average molar mass was

calculated to be 52 grams. The actual molar mass is 60 grams.

Bibliography:

http://physics.nist.gov/PhysRefData/ASD/lines_form.html

Atwood, Stanton, Zhu. Experiments in General Chemistry. Australia: Cengage Learning, 2010. Print.

4500
Emission KCl
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Intensity2000

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 Emission BaCl2

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Absorption Fe(NO3)3 400 ppm

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