30AL Soil Project
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CHEM 30AL : General Chemistry Laboratory II
Soil Project Lab Report
Unknown #12
Arnav Jhawar, Maggie Clark, Jessica Gonzalez
TA: David Deluca
Section: 1E
CHEM 30AL
Soil Project Lab Report
Group Responsibilities
Arnav Jhawar :
-
Performed extraction, identification, and analysis of the inorganic
molecules within the solution created from the unknown.
-
Conducted various tests, including Beer’s law, metal ion tests, and
assisted in the analysis of the organic material on day 3 of the lab.
-
Assisted and contributed to the creation of the presentation slides,
presented and contributed to the report.
Maggie Clark :
-
In charge of the extraction, identification, and analysis of the organic
molecules within the solution, created from the unknown.
-
Assisted in tests needed for organic analysis (TLC, mass spectroscopy,
acid-base separation, UV spectrum, and melting point analysis).
-
Assisted and contributed to the creation of the presentation slides,
presented and contributed to the report.
Jessica Gonzalez :
-
In charge of the extraction, identification, and analysis of the organic
molecules within the solution, created from the unknown.
-
Assisted in tests needed for organic analysis (TLC, mass spectroscopy,
acid-base separation, UV spectrum, and melting point analysis).
-
Assisted and contributed to the creation of the presentation slides,
presented and contributed to the report.
CHEM 30AL
Soil Project Lab Report
Abstract
This project aimed to examine and understand the different substances
present in a soil sample of unknown origin, labeled as sample 12. Through a
series of experiments, we successfully identified and measured the amounts
of both organic and inorganic compounds within the sample. The organic
compounds
found
were
naphthalene,
a
neutral
substance,
and
m-nitroaniline,
a
basic
substance.
On
the
other
hand,
the
inorganic
compounds discovered were nickel (II) chloride (NiCl
2
) and cobalt (II) sulfate
(CoSO
4
). To separate the organic and inorganic components, we utilized
vacuum filtration after dissolving the sample in a mixture of hexane and
ethyl acetate because one is polar and the other is non polar. We also
employed an acid-base extraction to further separate the organic neutral
and organic basic compounds from each other. For identification purposes,
we utilized UV-vis, IR, and mass spectroscopy, and the compounds were
purified through multiple liquid-liquid extractions. To assess the compound’s
purity, we conducted TLC and melting point analyses. Similarly, for the
inorganic compounds, we used UV-vis spectroscopy and specific tests to
determine
their
presence.
To
obtain
quantitative
data,
we
performed
colorimetry, a method that measures the intensity of color, based on which
we analyzed Beer's Law. Calculations showed that the percentages by mass
of the compounds in the sample were as follows: 1.4% naphthalene, 0.7%
m-nitroaniline, 7.14% nickel chloride, and 4.48% cobalt sulfate.
CHEM 30AL
Soil Project Lab Report
Design and Discussion of the experimental procedure
Separating the Organic and Inorganic:
1.
We weighed approximately 25 g of the unknown mixture and
recorded the appearance and exact weight.
2.
Dissolved the unknown mixture in a nonpolar organic solvent- which
was a mixture of hexane and ethyl acetate.
3.
We Gently stirred the solution with a glass stirring rod.
4.
Poured the solution into a vacuum filtration setup.
5.
Collected the filtrate and stored it in a separately labeled beaker
“organic compound.” Green/yellow color.
6.
Dissolved the residue in water and stored it in a separate beaker
labeled “inorganic compound.” Red/brown color.
Organic:
1.
We ran an initial TLC test using a mixture of hexane and ethyl acetate
at the bottom of the jar and found that the organic layer was most
likely Naphthalene (neutral) and
m-
nitroaniline (basic).
2.
Placed solution into a separatory funnel to perform liquid-liquid
extraction with HCl to protonate the basic part of the organic layer
because it was now neutral.
3.
This made the
m-
nitroaniline move into the aqueous layer and make
CHEM 30AL
Soil Project Lab Report
the organic layer neutral. For only the 1st extraction we collected an
aqueous layer in the beaker.
4.
Repeated 5 times so the neutral organic layer was pure. For the other 4
extractions, aqueous was waste.
5.
Added drying agent to neutral organic and air dried to get white
precipitate. This is Naphthalene.
6.
Added a base to aqueous to deprotonate the
m-
nitroaniline, add until
ph>7, some precipitate forms, this was the
m-
nitroaniline.
7.
Conducted a liquid-liquid extraction with the aqueous solution from
#6 with ethyl acetate to dissolve the precipitate. Repeated three times.
8.
took an ethyl acetate layer, added a drying agent, air dried, and got a
yellow precipitate. This was
m-
nitroaniline.
9.
Ran TLC, melting point, UV vis, IR spec, and mass spec on both the
basic and neutral.
Inorganic: DAY 1
1.
The inorganic solution was not pure, so an initial liquid-liquid extraction
with ethyl acetate was necessary to wash the solution. 3 washes were
done to purify. There was still some organic in this aqueous solution
that needed to be washed out.
2.
Solution was ready to run metal tests.
CHEM 30AL
Soil Project Lab Report
3.
Culture Tube #1: A small amount of the inorganic solution was added.
Ammonium hydroxide was added and nothing happened.
Dimethyloxirane was added and the solution turned a bloody red. This
indicates that we have Nickel. There was only one Nickel option that
could be in the unknown, so we could conclude that we had
NiCl
2
4.
Culture Tube #2: A small amount of the inorganic solution was added.
Potassium Nitrate added and nothing happens. The culture tube was
placed into a heating bath and yellow precipitate formed. This indicates
that we have Cobalt. We had to determine if we had CoCl
2
or CoSO
4
5.
Culture Tube #3: A small amount of the inorganic solution was added.
BaNO
3
was added and white precipitate formed. This indicates that
there is SO
4
-2
6.
Culture Tube #4: A small amount of the inorganic solution was added.
AgNO
3
added and white precipitate forms. This indicates that there is
SO
4
-2
and Cl
-
are present. By inductive reasoning, we determine that we
must have
CoSO
4
Inorganic: DAY 2
1.
Added 4.017 g of NiCl
2
to 50 mL of water. This was the stock solution.
2.
Made 3 standard solutions. Solution #1: 15 mL of stock in 25 mL
volumetric flask, diluted to the mark with water. Solution #2: 20 mL of
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