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EXPERIMENT 5

Qualitative Analysis: Unknown Anions


First Practical Exam

Outcomes
After completing this experiment, the student should be able to:
1. Demonstrate their understanding of qualitative analysis.
2. Determine anion in an unknown using chemical methods.
3. Confirm their results with confirmatory qualitative tests.

Introduction
Students will use qualitative methods learned in previous experiment to determine anions in
two unknowns. Teaching Assistant/Instructor will provide two unknowns. Each will contain
one unknown anion.

Safety Precautions
Handle all the chemicals in this experiment with care. Avoid getting AgNO3 on skin or clothing; it
will stain dark-brown or black. Be especially careful when handling concentrated sulfuric acid,
H2SO4. It is one of the strongest and most corrosive concentrated acids. If any skin contact occurs,
wash with large amounts of water. If instructed to sample odors, do not inhale deeply, gently waft the
fumes toward your nose. Wear your safety glasses at all times which is required for all
experiments in which you use chemicals.

Materials and Equipment


Dropping bottles of 2 unknowns, conc. H2SO4, 6 M H2SO4, 6 M HNO3, 6 M HCl , 0.1 M Fe(NO3)3,
chlorine water,1 M BaCl2, 0.2 M FeSO4, AgNO3 solution, saturated KNO2, hexane, copper wool or
fine Cu wire, and 10 mL graduated cylinder.

Apparatus
Test tubes, test tube rack, test tube holder, stirring rods, pH paper, Bunsen burner, lead acetate paper,
centrifuge, 10-mL graduated cylinder, ring stand and clamp, boiling water bath, ice water bath and
spatula.

Hazardous Waste Disposal


All of the aqueous solutions may be washed down the drain with a large volume of water. The
hexanes or other organic solvents should be collected in a container for organic wastes.

Experimental Procedure
You may use flowchart on next page or procedure used in previous experiment to determine
anion in your unknown.

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Flow sheet for the identification of unknown anions


CO32

SO42

PO43

SCN

Cl

Br

NO3 CH3COO

In test tube: 10 drops


unknown
add 6M H2SO4
dropwise

Gas evolution
(bubbles):
unknown is CO32

No gas: negative test


Groups 2, 3 or 4
present

In new test tube, 10


drops unknown, add
10 drops BaCl2

White precipitate:
positive
PO43 or SO42

Confirming test:
add 6 drops 6M HCl

Precipitate
dissolves:
PO43

No precipitate:
negative
Groups 3 or 4
present

In new test tube: 10


drops unknown, add
10 drops AgNO3

Precipitate does
not dissolve:
SO42

Positive: white or
yellow(ish)
precipitate

Negative (no ppt)


Unknown is NO3 or
CH3COO

White ppt:
Unknown is SCN or
Cl

Yellow(ish) ppt:
Unknown is Br or I

Confirming test for


NO3 (brown ring)

New test tube: 10 drops


unknown+1 mL DW
add 2 drops Fe(NO3)3

Do confirmatory test
as given in previous
experiment for I and
Br

Confirming test for


Ac (ester smell)

Dark red solution:


unknown is SCN

Violet hexane layer:


I
confirming test I

No colour:
unknown is Cl
confirming test for
Cl-

Brown hexane layer:


Br
confirming test Br

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FIRST PRACTICAL EXAM


Identification of Unknown anions
Name:___________________________________________________
REPORT:

UNKNOWN 1

ID ___________________

Unknown Code: ____________

Write down your observations in the boxes given in the following table. You must submit this sheet to your instructor before leaving the lab.
CO32

SO42

PO43 SCN

Cl

Br

NO3

CH3COO

Group Test

Group
Test

Observation

Confirmatory Test (if any)


Conclusion

Test

Observation

Conclusion

Anion
Present

1
Acid-volatile

2
Barium
precipitate
3
Silver
precipitate
group
4
Soluble
group

Unknown anion is: _____________________________

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FIRST PRACTICAL EXAM

Identification of Unknown anions


Name:___________________________________________________
REPORT:

UNKNOWN 2

ID ___________________

Unknown Code: ____________

Write down your observations in the boxes given in the following table. You must submit this sheet to your instructor before leaving the lab.
CO32

SO42

PO43 SCN

Cl

Br

NO3

CH3COO

Group Test

Confirmatory Test (if any)

Group
Test

Observation

Conclusion

Test

Observation

Conclusion

Anion
Present

1
Acid-volatile

2
Barium
precipitate
3
Silver
precipitate
group
4
Soluble
group

Unknown anion is: _____________________________

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