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RUNNING HEAD: Lab #6: QUALITATIVE ANALYSIS

Bryan Hatch
CHEM101L
Excelsior College
Oleg Maksimov

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LAB #6: QUALITATIVE ANALYSIS

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Abstract

In this lab I will demonstrate identifying elements by using the flame and
chemical tests. The flame test identifies elements by burning metal salts and
observing the color the flame. The chemical test identifies elements based
on the color of the precipitate created when the element is exposed to
solutions. Based on my results for the unknowns I tested my flame test was
using H2O and my chemical test contained Hg.

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Lab #5: Atomic Emission Spectrum


Introduction
Spectrometers can be used to identify elements based on the energy
of the emissions from their electrons. This identification process is simpler to
perform as well as less expensive. When elements are exposed to flame, the
heat from the flame adds energy to the element, this energy is released in
the form of light as the elements electrons return to their grounded state.
The light given off changes the color of the flame allowing for us to identify
the element in question.
The chemical test exposes elements to solutions of differing pH and
reactivity. Based on the color of the precipitate formed, the element can be
identified. Some elements require additional energy input in order to be
identified and one way to input additional energy is by heating the solution.
These two tests are examples of qualitative analysis. Qualitative analysis is
the process of determining the composition of a sample (Woodfield, 2014).

Method and Materials


Materials required
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Centrifuge
Hot plate
Bunsen Burner
Ignition source (lighter, torch spark, etc.)
Cobalt glass lens
Na solution
K solution

LAB #6: QUALITATIVE ANALYSIS


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Ag solution
Hg solution
Pb solution
NaCl solution
NH3 solution
pH4 solution
Deionized water
Platinum wire
Test tubes
Test tube stand
50ml graduated cylinder
Tweezers or Needle-nose pliers
Rubber gloves
Lab apron
Face shield
Dry chemical fire extinguisher
Vent hood

Experimental Procedure
To perform this procedure, begin by placing the Bunsen burner in the
center of the lab table under the vent hood. Connect the burner to the gas
source and open the isolation valve. Throttle open the flow control valve on
the burner a small amount and light the burner. Adjust the flame to the point
where the entire flame is a shade of blue. Close the isolation valve but do not
adjust the flow control valve.

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Don the gloves, face shield, and apron and retrieve the K, Na, Ag, Pb,
and Hg solutions from the storage container. Using the 50ml-graduated
cylinder, measure out 20ml of Na solution and pour it into a test tube,
measure out 10ml of Na solution and pour it into another test tube. Rinse the
graduated cylinder. Measure out 10ml of K solution and add it to the test
tube of 10ml Na. Measure out 20ml of K solution and pour it in a separate
test tube. Rinse the graduated cylinder. Measure out 20ml of deionized water
and pour it into a separate test tube. At this time there should be 4 test
tubes each with 20ml of fluid. Return the Na and K solution bottles to the
storage container.
Cut the platinum wire into 4 pieces each being 6-8 inches in length.
Fold each piece in half and twist the halves together. There should now be 4
twisted pieces of wire 3-4 inches in length. Open the gas isolation valve to
the burner and light the burner. Adjust the flow control valve as necessary for
the flame to be a blue hue. Using needle-nose pliers or tweezers pick up a
piece of wire and dip it into the Na test tube. Remove the wire from the tube
and hold it over the flame. Observe the color and record on Table 1. Properly
dispose of the wire. Repeat the process for each test tube being sure to use a
new piece of wire for each tube to prevent cross contaminating the sample.
Record all observations in Table 1.
At the front of the class are the Unknown element test tubes and
wire pieces. Take one test tube and piece of wire back to the lab table.
Document the unknown number in Table 1. Repeat the same steps to

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observe the flame color. Document the results in Table 1. Discard all
solutions in their appropriate waste containers and properly dispose of the
wire. Shut the gas isolation to the burner and disconnect the burner from the
gas source.
Measure out 10ml of Pb, Ag, and Hg each and pour into 1 test tube. Be
sure to rinse the test tube between each solution and after the last solution.
Place the test tube in the stand and place the hot plate below the tube. Add
a several drops of NaCl reagent to the test tube and document your
observations in Table 2. Place the test tube in the centrifuge and spin for
1minute. Return the tube to the stand and energize the hot plate. Once the
test tube is heated, spin in the centrifuge for another minute. Decant the
liquid into a new test tube. The decanted liquid is Pb; this is the test for Pb.
The Pb must be heated for the test to be successful. Dispose of the Pb in the
appropriate waste container.
Add 10ml of deionized water to the test tube with precipitate and
stir/swirl the test tube to mix up the precipitate. De-energize and remove the
hot plate. Add several drops of NH3 to the test tube and record the
observations in Table 2. Spin the test tube in the centrifuge for 1 minute and
decant the liquid into a new test tube. The solid precipitate is Hg. Dispose of
the Hg in the appropriate waste container.
We already know the Ag is the only element left in the test tube. To
confirm this add several drops of the pH4 solution and record observations in

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Table 2. If the solution turns to a white precipitate then Ag is present in the


liquid. Dispose of the Ag in the appropriate container.
At the front of the class are the Unknown element test tubes. Take 1
test tube back to the lab table and document the number in Table 3. Repeat
the above procedure for the unknown and document the results in Table 3.
Dispose of the solutions in their proper storage containers. Properly wash all
lab equipment used and return to its proper storage location. Return the Ag,
Pb, and Hg to their proper storage containers. Place all used safety gear in
the proper waste or laundry container.

Results and Discussion


For my flame tests I was given unknown #5. When placed in the flame
there was no color seen. Based on the previous results I determined my
unknown to be H2O. This part of the lab is simple and has little room for error.
Areas that could produce error would be setting the burner flame too high.
This would add an orange/yellow color to any colors given off, creating false
readings. Another error is not properly cleaning the wire pieces prior to
placing them into the solutions to be tested. The small impurities on the wire
could give small flashes of color not from the test solution. Because the color
is ultimately determined by what the observer sees, each person could see
different colors, which could skew the results slightly. My results matched the

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published values except for K. I observed a faint pink/magenta color for K,


the published value for K was lilac (pink) (Clark, n.d.).
For my chemical test I was given unknown #16. When I added NaCl a
white precipitate was formed. I heated the solution and ran it through the
centrifuge and then decanted the liquid. The decanted liquid did not turn
white when removed from the heat, proving there was no Pb in the solution. I
then added NH3 and the solution turned grey/black, proving the presence of
Hg. I ran the solution through the centrifuge and decanted the liquid. I added
the pH4 solution to my liquid and saw no change; this proved that there was
no Ag in the solution. My unknown only contained Hg. This part of the lab
had more room for error due to there being more required materials. Adding
the reagents in the wrong order could give incorrect indication of elements.
Not sufficiently heating the solution would cause the Pb to not be soluble and
stay with the precipitate. This would cause the rest of the lab to give
incorrect indication.

Conclusion
In conclusion, the flame and chemical tests can be used to detect the
presence of different elements based on the reaction. The flame test detects
elements based on the color given off when the element is placed in the
flame. The chemical test detects elements based on the color of the
precipitate formed and which reagent formed the precipitate. These tests

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examples of qualitative analyses. Qualitative analysis is used to determine


the composition of a sample (Woodfield, 2014).

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Tables

Table 1
Color

Intensity

Na
Na/K
K
H2O
Unknown
Table 2
Precipitate Color
Test 1
Test 2
Test 3

Table 3
Unknown #

Precipitate Color

Test 1
Test 2
Test 3

Table 4
Color

Intensity

LAB #6: QUALITATIVE ANALYSIS

Na
Na/K

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Bright color with

Yellow
Yellow fading into
orange at the end

Pink/Magenta

H2O
Unknown #5

None
None

large flame
Bright color with
large flame
Bright color with
low flame
N/A
N/A

Table 5
Precipitate Color
Test 1

White

Test 2

Grey/Black

Test 3

White

Unknown #16

Precipitate Color

Test 1

White

Test 2

Grey/Black

Test 3

None Produced

Table 6

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References

Clark, J. (n.d.) Flame Tests. Retrieved from


http://chemwiki.ucdavis.edu/Inorganic_Chemistry/Descriptive_Chemistr
y/Elements_Organized_by_Block/1_sBlock_Elements/Group__1%3A_The_Alkali_Metals/2Reactions_of_the_Gr
oup_1_Elements/Flame_Tests
Woodfield, B. F., Asplund, M. C., Haderline, S. (2014) Identification of Cations
in SolutionFlame Tests. In A. Jaworski & T. Haugen (Eds.), Virtual
ChemLab General Chemistry Laboratory v.4.5 (pp. 169.170). Saddle
River, NJ: Pearson Education.
Woodfield, B. F., Asplund, M. C., Haderline, S. (2014) Identification of Cations
in SolutionAg+, Hg22+, Pb2+. In A. Jaworski & T. Haugen (Eds.), Virtual
ChemLab General Chemistry Laboratory v.4.5 (pp. 171,172). Saddle
River, NJ: Pearson Education.

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