ELEMENTAL

Sodium fusion
ANALYSIS

INTRODUCTION
Elemental Analysis
-used for identification of unknown
compounds
-chief aspect in experimental organic
chemistry

Sodium fusion
-also known as Lassaignes test
-useful method for qualitatively
determining the presence of sulfur,
nitrogen or halogens in organic
compounds
-property of sodium to be a very
strong reducing agent makes it
possible to break the organic
compounds carbon chain into
inorganic ions

Sodium fusion
-the filtrate from the fused solution of
the unknown compound and sodium
metal is used to conduct the
confirmatory tests for the presence
of sulfur, nitrogen or halogens

EXPERIMENTAL
Set-up
The set-up for sodium fusion was
done as shown in the figure:

Pea-sized sodium was placed in a

small test tube. The test tube was
heated until sodium vapor was
observed to condense on the wall of
the test tube.
The flame was removed and about
0.3g of p-chloroaniline was added.

The test tube was heated gently to

initiate the reaction with sodium. The
flame was removed when the reaction
subsided then it was heated to
redness for 3 minutes

The red-hot tube was dropped in a 50mL beaker containing 10-mL of

distilled water

Solution was filtered and the filtrate

was used as the test solution

(The procedure was repeated using

sulfanilic acid)

Qualitative Analysis
Sulfur test

Five drops of fusion solution and 3

drops of water were placed in a 5-mL
test tube
2 drops of 2% aqueous sodium
nitroprusside solution was added

The formation of a deep blue-violet

color was observed

Nitrogen test
A pinch of FeSO4 was added to 1-mL of
the fusion solution
5 drops of 10% solution of KF was
added
Mixture was boiled for 5 minutes and 2
drops of 5% solution of ferric chloride
was added
6M H2SO4 was added to dissolve the
iron hydroxides and to acidify the
solution
Formation of a deep-blue precipitate
indicated the presence of nitrogen

Halogen test
Ten drops of the fusion solution was
placed in a test tube
If the sample was positive for nitrogen
or sulfur, acidify with 2M HNO3
Gently boil to eliminate HCN or H2S
that might be present and cool to
room temperature
0.1M AgNO3 was added to the solution
n hydroxides and to acidify the
solution
A heavy and coagulated precipitate
indicated the presence of halogens

Halogen test
Differentiating Chlorine, Bromine and
Iodine
The observed colors indicate the following
precipitates: AgCl (white), AgBr (pale yellow), and
AgI (yellow)
Differentiating Bromine and Iodine
Add 0.5-mL of dilute 2M NH4OH to the
precipitate
Determining if is soluble by stirring with a
glass rod
If the precipitate is soluble, AgBr is
present in the solution. Otherwise, AgI is
present.

RESULTS
The fusion solutions obtained from the two
compounds, p-chloroaniline and sulfanilic acid,
were subjected to confirmatory tests and the
obtained data is shown in the table.
Sample

Sulfur Nitrogen
Test
Test

Haloge
n Test

p-chloroaniline

Sulfanilic acid

Sulfur
To test for the presence of sulfur, sodium
nitroprusside was added to the fusion
solution. Deep blue-violet coloration in the
solution indicates the presence of sulfur
given as:

Na2Sn+ Na2[Fe(CN)5NO]
Na4[Fe(CN)5NOS]
(violet in color)

Nitrogen
To test for the presence of nitrogen, FeSO4
was added into the fusion solution giving
the following reaction:

2NaCN + FeSO4 Fe(CN)2 + Na2SO4

Fe(CN)2 + 4NaCN Na2Fe(CN)6

Afterwards, addition of KF was done to

intensify the blue coloration of the solution.
Finally, FeCl3 was added to form NaCl which
is a blue precipitate.

3Na4Fe(CN)6 + 4 FeCl3 Fe4[Fe(CN)6]5

Halogens
Test for the presence of halides involves the
addition of HNO3 to the solution and heating
if afterwards. This is to expel HCN or H2S in
the sodium fusion.

Addition of silver nitrate (AgNO3) into the

sodium fusion resulted in the following
reactions:

NaCl(aq) + AgNO3 (aq) AgCl(s) + NaNO3 (aq)

(white precipitate)

NaBr(aq) + AgNO3 (aq) AgBr(s) + NaNO3 (aq)

(pale yellow precipitate)

NaI(aq) + AgNO3 (aq) AgI(s) + NaNO3 (aq)

(yellow precipitate)

P-chloroaniline
- With a formula of ClC6H4NH2
- It can be noted that only nitrogen and
chlorine, a halogen, are present in the
compound, indicating a negative result
for the sulfur test
Nitro
gen
Test

Halog
en
Test

Sulfu
Sample
r Test
pchloroa
niline
Sulfanili
c acid

Sulfanilic acid
- With a formula of C6H7NO3S
- It can be observed that there is no
halogen in sulfanilic acid, but the
presence of sulfur and nitrogen are
confirmed
Nitro
gen
Test

Halog
en
Test

Sulfu
Sample
r Test
pchloroa
niline
Sulfanili
c acid

CONCLUSION
Sodium fusion is a test to determine the
presence of some elements like sulfur,
nitrogen, and halides such as chlorine,
bromine, and iodine. This is possible by
turning these insoluble elements into
soluble sodium salts.

The presences of the mentioned elements

are determined through series of
qualitative tests mainly by forming
colored precipitates or products.
Flame test can also be done as a pretest
for halogen since a green flame result
indicates the presence of halogens.

RECOMMENDATION
Since the experiment employed only one
confirmatory test for the presence of
nitrogen, sulfur, and halogens, it is
recommended to use other methods for
confirming the elements mentioned.

ANSWERS TO GUIDE
QUESTIONS
1. Outline the procedures for detecting the presence of
oxygen and phosphorus in organic compounds.
A. Oxygen
Ferrox Test
-Grind one crystal of ferric ammonium
sulfate and a crystal of potassium cyanate
using a glass rod (do this in a dry spot
plate)
-Add 2 drops of the unknown in a separate
well
-Use the glass rod with attached ground up
crystals to stir the unknown
-A positive test indicates dissolution of

B. Phosphorus
-The unknown is fused with sodium
peroxide (Na2O2)
-Phosphorus present in the unknown is
converted to sodium phosphate
-Fused mass is extracted with water
-Aqueous extract is heated with
concentrated nitric acid and ammonium
molybate solution.
-Yellow precipitate of ammonium
phosphomolybate (NH3)3[PMo12O40]
indicates the presence of phosphorus.

2. Discuss other methods of detecting the presence of

sulfur, nitrogen and halogen in organic compounds.
A. Sulfur
Using the sodium fusion solution
Lead acetate solution is added to the
fusion solution. A positive test for sulfur is
indicated by the presence of a black
precipitate (PbS).
Oxidation test
The unknown organic compound is heated
with oxidizing fusion mixture (Na2CO3 +
KNO3). If sulfur is present, it will be
oxidized to sulfate. The fused mass is
extracted with water. It was made acidic by

B. Nitrogen
Addition of p-nitrobenzaldehyde
To the fusion solution, add pnitrobenzaldehyde solution. Afterwards,
add a basic solution of o-dinitrobenzene. A
positive test is indicated by a blue-violet
color.
Oxidation of benzidine with cupric ion
This reaction will not take place in the
absence of cyanide ion. The cyanide
complexes with cuprous ions so as to
increase the oxidation potential of the
system.

C. Halogens
Sodium Iodide in Acetone Test
To the unknown, add solution of sodium
iodide in acetone. Shake tube to
adequately mix the unknown and the
solution. If about 5 minutes has passed
and presence of precipitate is still not
evident, place test tube in a 50 water
bath. Formation of a white precipitate
indicates presence of halides.
Beilstein Test
Heat the tip of a copper wire in a burner
flame. Cool the wire slightly then dip it into
the unknown. Heat it once again. A green
flash is indicative of chlorine, bromine,

REFERENCES
Srivastava, A.K., (2007). Chemistry. Delhi: V.K. (India)
Enterprises

Chemical Tests for Unknowns. Retrieved from

http://cactus.dixie.edu/smblack/chemlabs/Chemical_Test
s_for_Unknowns.pdf

Detection of Phosphorus, Sulfur and Oxygen Retrieved

from
http://gradestack.com/Class-11th-Science-With-Math-/De
tection-of-Phosphorus-Sulphur-and-Oxygen/17562-3564-29
276-study-wtw

Organic Qualititative Analysis. Retrieved from

http://faculty.swosu.edu/william.kelly/pdf/qo2a.pdf

Test for Halides. Retrieved from

http://academics.wellesley.edu/Chemistry/chem211lab/Org
o_Lab_Manual/Appendix/ClassificationTests/halide.html