You are on page 1of 11

Experiment 32 Procedure Proposal

Andrew Nguyen
Collin Teng
Lab Section #32
March 29th, 2016

Introduction
An inspector from the Environmental Protection Agency was doing a laboratory
stockroom check, when the inspector found a container in the laboratory stockroom with
unknown chemicals inside of it. We must determine what is within the container, the list of
chemicals from the stockroom are:
1. Aluminum (s)
2. Sodium hydrogen carbonate (s)
3. Barium chloride (s)
4. Ammonia (aq)
5. Formic acid (aq)
6. Sodium hydroxide (s)
7. Hydrochloric acid (s)
8. Iron (III) chloride (aq)
9. Ethanol (l)
10. Hexane (l)
11. Urea (s)
12. Potassium sulfate (s)
We must use a series of techniques to determine what is within the container. Some of
these techniques we will be using will be from the first semester of lab. We will need to
differentiate between different states of matter, perform both absorption and emission
spectroscopy. We must also need to be able to check solubility and watch for precipitants that
will form. We should be able to calculate different densities of different materials and we
must be able to use different colligative properties and know how to find pH. After we
eliminate all possible items on the list, we must make sure that the compound we found was
in fact the compounds identity.

Experimental
Necessary Reagents and Chemicals:
0.1 M Hydrochloric acid solution
pH 4 or pH 7 buffer solutions
0.1 M Sodium hydroxide solution
0.1 M Silver nitrate solution
0.1 M Barium chloride solution
0.1 M Iron(III) nitrate solution
0.1 M Sodium chloride solution
0.1 M Potassium chloride solution
Distilled water
Necessary Equipment:
MeasureNet spectrophotometer, cuvettes, and nichrome wires
MeasureNet pH probe and drop counter
MeasureNet temperature probe
Conductivity detector
Styrofoam cup calorimeters and lid
Volumetric flasks
Kimwipes
Crucible and lid
Ordinary lab glassware
Procedure
In order to determine the identity of the substance in the container the different properties of
each possible compound must be identified and tested. Then they must be matched up and
tested with the unknown using the following flowchart. Also refer to the list of chemicals and
their properties for further comparisons.

Aluminum:
1. Phase: Solid
2. Density: 2.7
g/cm
3. Solubility:
Insoluble
4. Conductivity:
36 m/Ohmmm
5. Melting point:
660 C
6. Boiling Point:
2500 C
Barium Chloride

1. Phase: Solid
2. White
,odorless and orthorhombic
crystal
3. Solubility:
Soluble
4. Emission
Spectrums: 740, 841, and
873
5. When added
to an SO42(aq) and C2O42(aq)
a precipitate forms
6. Very toxic
Formic Acid
1. Solubility:
Soluble
2. pH: Acid
3. Pungent
Penetrating Odor
4. Conductivity
tests: Weak Electrolyte
Hydrochloric acid

Sodium Hydroxide Carbonate:


1. Phase: Solid
2. Solubility:
Highly Soluble
3. pH level:
Basic
4. Similar to
Baking Soda
5. White
Crystalline compound

Ammonia:
1. Solubility:
Soluble
2. Electrical
Conductivity: Weak
Electrolyte
3. pH: Basic
4. Pungent Smell

Sodium Hydroxide
1. Solubility:
soluble
2. pH: Basic
3. Strong Base

Iron (III) Chloride


1. Odorless
2. White Crystal
3. Very

Corrosive
4. Electrical
Conductivity: Strong
5. Absorbance:
None

1. Solubility:
Soluble
2. Conductivity:
High
3. Absorbance:
None
4. Yellow when
solid

6. Emission:
None
Ethanol
1. Has the ability
to intoxicate but at the same
time might give you alcohol
poisoning
2. Solubility:
Soluble
3. Conductivity:
none
4. Phase: Liquid
5. Density: .789
Urea

Hexane
1. Solubility:
insoluble
2. Phase: Liquid

Potassium Sulfate
1. Phase: Solid
2. Reacts With
alcohol to form urethanes
3. White ball
like crystal
4. Solubility:
Solid
5. Conductivity:
None

1. White Crystal
2. Purple Flame
test
3. Solubility:
Soluble
4. Conductivity:
High
5. Absorbance:
None
6. Emission: 765
and 771
7. When BaCl2 is
is added a precipitate forms

1.

Check for Solubility

Pour about 4 drops or .5 g of sample into a test tube filled with distilled water and shake the
test tube. If no visible precipitant or the solution becomes miscible then the test can be
deemed as soluble. If precipitant is visible or the solution is immiscible then the compound
can be deemed as not soluble.

2.

Perform Electrical Conductivity Test

Clean and dry a watch glass. Pour about 15 drops of the aqueous unknown solution to the
watch glass. Simultaneously immerse the conductivity detector electrodes into the solution or
liquid on the watch glass. Then record the relative brightness of the LED bulb to further
refine your results

3. Test for pH Value


Calibrate a pH probe with the pH 7 buffer solution. Then dip the pH probe in the solution and
stir the solution until pH stops changing. Refine your choices according to the pH constrains.

4. Absorption Spectroscopy
Record absorbance spectra of the unknown solution sample using the MeasureNet
spectrophotometer. See Appendix D Instructions for Recording an Absorbance Spectrum
using the MeasureNet Spectrophotometer. If there is no absorbance in the 200-850 nm bound
then the absorbance can conclude the fact that the solution is not Iron (III) Chloride

5. Test for Emission


See Appendix E Instructions for Recording an Emission Spectrum Using the MeasureNet
Spectrophotometer. Complete Steps 17 in Appendix E before proceeding below. Obtain 1
mL of the unknown water sample, and a nichrome wire. The nichrome wire must be cleaned
before it can be used to introduce samples into the flame. Place 5 mL of 6 M HCl in a 50-mL
beaker. Dip the nichrome wire into the 6 M HCl and swish the wire in the solution 128
Experiments in General Chemistry Featuring MeasureNet n Stanton et al. for 3040 seconds
to insure that it is thoroughly clean. Any ions that remain on the wire from a previous lab
students experiment could contaminate your experiment. See Appendix E Recording an
Emission Spectrum. Complete Steps 824 in Appendix E before proceeding below.
Calculations and Experimental Analysis to be Completed Outside of Lab 6. Excel
instructions for preparing an XY Scatter Plot are provided in Appendix B-5. Use these
instructions to plot emission spectra for each of the standard metal solutions and the
unknown water sample. Record the two most intense emission lines in the Lab Report for
each metal ion in the emission spectra of the known and unknown solution.

6.

Precipitant Check

Add 56 drops AgNO3(aq) or Fe(NO3)3(aq) to 2 mL of the unknown solution in a small test


tube. Shake the test tube to mix the substances. A precipitant must form in order to conform
the substance. If a precipitant does not form, then the unknown cannot be deemed as either
Barium Chloride or Sodium Hydroxide, respectively.

Results
Unknown # 4
Cross off any possibilities that arent from the flow chart.
Aluminum

Sodium
Hydrogen
Carbonate

Barium
Chloride

Ammonia

Formic Acid

Sodium
Hydroxide

Hydrochloric
Acid

Iron (III)
Chloride

Ethanol

Hexane

Urea

Potassium
Sulfate

Solubility Test: Unknown was Soluble


This will rule out Aluminium and Hexane as they are both
insoluble
Conductivity Test: Weak Electrolyte (Dim Light)
This will narrow down Sodium Hydroxide, Sodium
Hydrogen Carbonate, Potassium Sulfate, Barium Chloride,
Hydrochloric Acid, and Iron (III) Chloride because they are all strong
electrolytes.
It will also narrow down Urea and ethanol because they
both are non-electrolytes
pH: 10.93
The last two that are left are Ammonia and Formic Acid
and since the pH was basic that singles out Formic Acid and leaves
Ammonia

Trial A titration:
pH= pKa+ log(A-/HA)
pH= pKb+ log(HA/A-)

Equivalence Point: 5.84 pH at 561 drops


Half Equivalence Point: 9.40 pH at 280 drops

-log( K b = -log[ OH
-log( K b = pOH
14-9.40 = 4.6

K b of ammonia = 1.8 x 105

-log( K b =4.6
K b = 104.60
K b = 2.5 x 105

Discussion
There are many different scenarios where an experiment like this would be useful. Some
examples would be identifying an unknown in a crime field or even determining the identity
of a beaker left out in a formal lab setting. Basically whenever a compound is unknown or
needs to be narrowed down, this experiment would come into play. The results that were
found seemed to agree with each other. By testing the different properties of the compound
the list of possibilities were narrowed down to one compound that fit all of those properties.
There is always some source of human error, whether it be in the titration to confirm or the
determination process. With the titration there was a possibility for faulty equipment or
setting it up so that the drop counter did not measure accurately. With the determination
process the solubility test could have not have enough of the unknown which would make the
layers too minimal to notice or the conductivity light could have been strong instead of weak.
Even though there was possible source for error most of the data agreed with itself and the
result is accurate and precise.

Conclusion
By testing the compound for its various properties we were able to narrow down the
possibilities one by one until one remained. Then by process of elimination we were able to
safely assume that the compound that was given to us was Ammonia. But in order to make
sure our results are accurate a confirmation test was necessary. A titration curve was the best
way to confirm our results as each curve has different equivalence points and half
equivalence points. The unknown compound was undeniably Ammonia and the pungent
smell to ammonia and the unknown further confirmed the identity.

Bibliography
Stanton B., Zhu L., Atwood C. (2010) . Experiments in General Chemistry Featuring
MeasureNet 2nd Edition.
https://www.gliffy.com/publish/5557399/

You might also like