Experiment 2

Elemental Analysis by Sodium Fusion

Larrie Antoni B. Adaptar, Bianca Chellyne A. Aguilar,
and Joan Pauline D. Agustin Date Performed: February 5, 2020
Group 1, Chemistry 33— LB2A, Jamie Sy Date Submitted: February 12, 2020

Abstract
Elemental analysis serves the purpose of determining a compound’s identity and
elemental, sometimes isotopic, composition. It is a fundamental step in the
development of new compounds and reagents and serves as a key player in the
advancement of material science. This experiment aims to distinguish a positive
result from a negative result in qualitative analysis; and determine whether an
unknown compound contains nitrogen, sulfur, and halogens. Separate fusion
solutions from sodium metal, p-chloroaniline, sulfanilic acid, chlorobenzene, and an
unknown element were prepared. Three qualitative tests were performed to test the
presence of nitrogen, sulfur, and halogens; while sulfanilic acid only tested positive
for sulfur. A white precipitate was observed in chlorobenzene, indicating the presence
of chlorine. Since the test results reflect the elements found on the structure of these
compounds, sodium fusion was proven to be a viable method of determining the
presence of sulfur, nitrogen, and halogens attached to organic molecules.

Keywords: organic compounds, qualitative analysis, elemental analysis, sodium fusion, heteroatoms

I. Introduction covalent bonds. In the sodium fusion test, the

molecule is broken down into its ionized form
The discovery of organic compounds derived
through controlled decomposition. The ions
from natural products continues to be a
that were formed after the decomposition will
forefront topic of research in pharmaceutics,
then be treated with different reagents to
chemistry, and medicine. Progress in these
confirm the presence of their constituting
fields is partly in response to the threat of
elements through a color change. The
antibiotic-resistant bacteria and the need for
presence of an element after the addition of
newer and more effective medicine that
reagent reflects its presence in the original
addresses the changing needs of the health of
unknown organic compound (Nechamkin,
the general public (Miceli, 1936). With this,
1951). This test is especially useful in the
qualitative analysis plays a crucial role in the
elemental determination of nitrogen, sulfur,
characterization of newly discovered or
and halogens as the physical changes are
isolated organic compounds. These tests allow
evident (Vinson & Gabrowsky, 1977).
for the non-numerical identification of some
elements present in a sample through
In this experiment, p-chloroaniline, sulfanilic
observable precipitation, color change, and the
acid, and chlorobenzene was separately mixed
like. Qualitative analysis achieves this without
with molten sodium to determine which
the need for expensive equipment. Although
heteroatom is attached to the carbon chain.
its results are less accurate, it is often
Sodium is used in the decomposition of the
cheaper, faster and more convenient to
covalent bonds as it is a strong reducing
conduct (Velcárcel, Cárdenas, & Gallego,
agent, is highly reactive, and is capable of
2000).
breaking the organic compound’s carbon
chain. As a result, the organic compounds will
Among organic compounds, carbon and
be converted into inorganic ions which will be
hydrogen predominate in its constitution but
detected by the reagents in the subsequent
heteroatoms like sulfur, nitrogen, and halogens
tests. Three separate tests were conducted for
attach to the carbon chain in different
each of the compounds stated above to test
permutations, thus altering the molecule and
for sulfur, nitrogen and halides.
its properties (Wang & Tarter, 1983). One
reliable method to determine the presence of
In order to determine the presence of
these atoms qualitatively is through Sodium
heteroatoms in organic compounds, the
Fusion or more commonly called the
experiment aims to: (1) differentiate positive
Lassaigne’s test (Gower & Rhodes, 1969).
results from negative results using compounds
Organic compounds are held together by weak

Chemistry 33: Elemental Analysis by Sodium Fusion

1
of known elemental composition. And (2) The boiled solution was then filtered. The color
determine whether an unknown compound of the solution is observed and recorded. The
contains nitrogen, sulfur, chlorine, bromine, or fusion is repeated two more times for the other
iodine. Additionally, the experiment is limited reagents: sulfanilic acid and chlorobenzene.
only to the use of p-chloroaniline, sulfanilic
acid, and chlorobenzene (compounds of Elemental analysis was carried out through
known composition) as a negative control to three tests. The results between p-
set the basis for the results of the test. chloroaniline, sulfanilic acid, and
chlorobenzene were compared to determine
II. Methods which among the following solutions contain
halogens, sulfur, and nitrogen.
The procedure is divided in two parts: Sodium
Fusion and Elemental Analysis through
Qualitative Tests. The first part, Sodium
Fusion, was performed by placing a pea-sized
lump of sodium in a test tube. Prior to this, the
sodium was immersed in hexane to remove
the oil. The test tube is heated to melt the
sodium lump. When it appeared similar to
liquid mercury, the tube was removed from the
heat.

Figure 3 Test for Sulfur

To perform the test for sulfur, 5 drops of the

fusion solution was placed in a 10 mL test tube
containing 3 drops of water. Two drops of 2%
aqueous Na2[Fe(CN)5NO] were then added.
The change in color of each fusion solution
was observed and recorded.

Figure 1. Melted lump of sodium metal

The first reagent, p-chloroaniline was added to

the ignition tube. When the reaction subsided,
the tube is returned to the flame and heated
for 10 minutes. While hot, the test tube was
dropped in a 150 mL beaker containing 20 mL
water, breaking the test tube upon impact. It
was then set aside for a few minutes until any
reaction that occured subsides. The solution is Figure 4 Test for Nitrogen
then boiled for 5 minutes.
Test for nitrogen was carried out by adding a
small amount of FeSO4 to a test tube
containing 10 drops of the fusion solution. Five
drops of 10% KF were added before boiling
the solution for 10 seconds. Afterwards, 2
drops of 5% FeCl were added. The solution
was acidified with 6 M H2SO4. Blue litmus
paper was used to determine the acidity of the
solutions.

Figure 2. Filtering the solution

Chemistry 33: Elemental Analysis by Sodium Fusion

2

Sample Confirmatory tests
S* N* X*
p-chloroaniline - + +
sulfanilic acid + +
chlorobenzene - - + absence of a purple to deep blue-violet color.
Figure 5 Test for Halogens
To determine the presence of halogens, 2 M
HNO3 was added to 10 drops of the fusion
solution. The solution was boiled for 5 minutes.
Subsequently, 4 drops of 0.1 M AgNO3 were
added. The color of the three fusion solutions
were compared and recorded. The solution is
then centrifuged at 3000 rpm for 15 minutes.
The decantate was discarded while 2 M NH3
was added to the precipitate.
III. Results
A. Sodium Fusion
The p-chloroaniline, sulfanilic, and
chlorobenzene solutions displayed a light
brown color upon boiling, due to the presence
of insoluble black particles and glass shards.
However, after respectively filtrating the fusion
solutions, the filtrates were clear in color.
B. Qualitative Tests
A positive result for the sulfur test is indicated
by an observable purple solution. For the
nitrogen test, the appearance of a blue
coloration confirms the presence of nitrogen in
the organic compound. Whereas for the
halogen test, a white, pale yellow, or yellow
precipitate determines the presence of a
certain halogen (Co & Salindo, 2012). The
results for the elemental analysis of the fusion
solutions through qualitative tests for sulfur,
nitrogen, and halogen are as follow.
Table 1. Results for the Qualitative Tests
Chemistry 33: Elemental Analysis by Sodium Fusion
Note: + indicates the observed presence of the
element while - indicates its observed
absence. S*- sulfur, N*- nitrogen, X*- halides
The fusion solution of p-chloroaniline showed
a clear white liquid upon performing the test for
- sulfur. This indicates that the solution has no
presence of which, as determined by the
For the nitrogen and halogen tests, the
presence of blue and white precipitate was
observed respectively. Thus, signifying that the
solution generated a positive result for both.
The fusion solution for sulfanilic acid, on the
other hand, tested positive for sulfur and
nitrogen. Purple liquid and greenish blue
precipitate were accordingly detected upon
performing the said tests. However, a yellow
liquid was produced for the halogen test. The
absence of precipitate indicates a negsative
result for the halogen test.
Whereas, for chlorobenzene, the sulfur and
nitrogen tests displayed negative results as a
yellow liquid and pale-yellow precipitate were
respectively observed. Moreover, for the
halogen test, a clear liquid with minimal white
precipitate was observed. This is evidence that
the organic compound contains halogen.
IV. Discussion
Sulfur ( S), nitrogen ( N ), and halogens (
X =Cl , Br ,∨I ) are covalently bonded to
organic compounds and in order to detect
such, it is fundamental to convert these into
their ionic forms through sodium metal and
heat, since bond breaking is an endothermic
process. Through heating sodium metal along
with organic compounds, sodium converts the
present elements into sodium salts as shown
by the reactions below.
Na+CN → NaCN
Na+S +C+ N → NaSCN
2 Na+ S → Na₂ S
Na+ X → NaX ( X =Cl , Br ,∨I )
In accordance with this, p-chloroaniline when
heated with the sodium metal, formed NaCl
and NaCN . The sulfanilic acid, on the other
hand, formed Na₂ S and NaCN , while the
chlorobenzene fusion formed NaCl . For
compounds containing both sulfur and
nitrogen, such as sulfanilic acid, when fused
with sodium generally produces NaSCN .
Given this, another test would have been
3
employed as the Lassaigne’s Test is limited to
detecting the presence of such elements
individually. But due to fusion with excess
sodium metal, it is possible to form the said
test on compounds such as sulfanilic acid.
Such occurrence is described by the reaction
below.
NaSCN +2 Na→ NaCN + Na ₂ S
Consequently, the solutions were filtered. The
filtrate, which can also be called Lassaigne’s
or sodium extract, should be colorless. Since
the extract is to be subjected to qualitative
tests, it is necessary for the solution to be clear
of impurities in order for the color changes to
be easily observable. Remaining residue or
insoluble solid would also interfere with the
potential detection of precipitate.
For the sulfur test, as drops of sodium
nitroprusside ( Na₂ ¿) are added to the fusion
solution, formation of a deep blue to purple
color confirms the presence of sulfur. The
change in coloration is caused by the reaction
between sodium sulfide ( Na₂ S) and sodium
nitroprusside, producing sodium
sulfonitroprusside ( Na ₄ [Fe(CN )₅ NOS ]), a
compound violet in nature. The said chemical
reaction is presented below.
Na₂ S+ Na ₂[Fe(CN ) ₅ NO ]→ Na ₄ [Fe (CN )₅ NOSAgNO
Among the three organic compounds, only
sulfanilic acid solution exhibited a purple liquid; interfere with the detection of silver halide
thus, confirming the presence of sulfur in
which and the absence of sulfur in p-
chloroaniline and in chlorobenzene. These
results comply with theoretical data.
In the nitrogen test, a positive result is
described by a blue coloration and precipitate.
This is due to the formation of the blue
complex ferric-ferrocyanide ( Fe[ Fe(CN )₆ ]₃
). The reaction chain is initiated by the
production of NaOH from unreacted sodium
and water, thus making the sodium extract
mostly basic. As ferrous sulfate ¿) is added,
the solution develops a brown-green color due
to insoluble ferrous hydroxide. Ferrous ions
from the ferrous hydroxide ( Fe(OH )₂)
consequently react with sodium cyanide (
NaCN ) from the organic compound to create
sodium ferrocyanide. The chemical reactions
involved are presented below.
FeSO ₄+2 NaOH → Fe(OH )₂+ Na ₂ SO ₄
Fe(OH ) ₂+6 NaCN → Na ₄ Fe (CN )₆+2 NaOH
Chemistry 33: Elemental Analysis by Sodium Fusion
The ferric ( Fe ³ ⁺) ions produced from aerial
oxidation and those from FeCl ₃ react with the
acid to form ferric salt ( Fe ₂( SO ₄)₃ ). The
sodium ferrocyanide ( Na ₄ Fe(CN )₆ ) then
reacts with the ferric salt to generate the blue
ferric-ferrocyanide complex.
3 Na ₄ Fe(CN )₆+ 2 Fe ₂(SO ₄)₃ → Fe ₄ [Fe (CN )₆]₃+6 N
Sulfuric acid ( H ₂ SO ₄ ) was added to dissolve
iron produced from the reaction between
excess ferric ( Fe ³ ⁺) ions and air (O ² ⁻)., KF
was further added to allow the color change to
be more evident.
Both p-chloroaniline and sulfanilic acid provide
positive results. The blue and greenish blue
precipitates confirm the presence of nitrogen in
the organic compounds, as clarified by the
mentioned process. Chlorobenzene, on the
other hand, tests negative for nitrogen. These
results comply with theoretical data.
For the halogen test, nitric acid ( HNO ₃) is
firstly added to the fusion solution and then
boiled. This is to expel any HCN or H ₂ S that
form, given the possibility that nitrogen and
sulfur are both contents of the compound as
well. Reaction of HCN and H ₂ S with
] ₃ forming AgCN and Ag₂ S must be
prevented due to the formation of white and
black precipitate, respectively. This would
precipitate.
Formation of precipitate after HNO ₃ addition
would correspondingly imply that the test is
positive for halogen. A white precipitate would
indicate the presence of chloride as AgCl is
white in nature. A pale yellow precipitate would
determine the presence of bromide since
AgBr is pale yellow. While, a yellow
precipitate would then indicate that iodide is
present as AgI is a yellow compound. The
reactions are listed below.
NaCl+ AgNO ₃→ AgCl+ NaNO ₃
NaBr+ AgNO ₃ → AgBr+ NaNO ₃
NaI + AgNO ₃ → Agl+ NaNO ₃
The experiment showed that p-chloroaniline
and chlorobenzene are positive for halogen.
Slightly white liquid with minimal white
precipitate was observed for both compounds.
Furthermore, no precipitate was observed for
sulfanilic acid. These results comply with
theoretical data.
V. Conclusion and Recommendations
Elemental analysis of newly discovered
organic compounds is a fundamental step in
the possible development of new medicines,
reagents for industrial use, and the
advancement of material science. The sodium
fusion aims to quantitatively detect the
4
presence of heteroatoms (sulfur, nitrogen and
halogens) in organic compounds by breaking
the covalently bonded organic molecule into its
inorganic ions through a strong reducing
agent. The ions are then mixed through a
specific series of reagents to confirm the
presence of the element that it is being tested
for.
In this experiment, chloroaniline tested positive
for chlorine and nitrogen Likewise, sulfanilic
acid was positive for sulfur and nitrogen.
Lastly, chlorobenzene tested positive for
chlorine. As the test results of the experiment
reflected the elements that can be found on
the structure of these compounds, it can then
be said that the sodium fusion test can be a
viable qualitative method of determining the
presence of sulfur, nitrogen, and halogens
attached to organic molecules.
For future studies, it is suggested to expand on
the analysis of other elements that are
commonly found on organic molecules through
the lead acetate test and carbon disulfide test.
In this method, errors in the result may be
caused by the likelihood of: (1) the sodium and
the reagents spewing out of the test tube
during heating, (2) reagents combusting while
being heated. In addition, shards of glass from
the ignition tube poses a safety hazard.
Therefore, it is also suggested to explore safer
alternatives in the analysis through the use of
a Non-breakable Sodium Ignition Apparatus
(NOSIA) in place of a fragile ignition tube
(Singh, 2015).
Co, F.K., & Salindo, E.S. (2012). Experiment
#6 elemental analysis. Retrieved from:
https://www.scribd.com/doc/86737439/Exp-6-
Sodium-Fusion-PDF
Gower, R. P., & Rhodes, I. P. (1969). A review
of techniques in the Lassaigne sodium-fusion.
Journal of Chemical Education, 46(9), 606.
Miceli, A. S. (1936). Improved sodium fusion
technic for volatile or difficultly decomposable
liquids. Journal of Chemical Education, 13(11),
515.
Nechamkin, H. (1951). Sodium-fusion tests on
plastics. Journal of Chemical Education, 28(2),
97.
Singh, M. (2015). Extra elements detection in
organic compounds by nonbreakable sodium
ignition apparatus (NOSIA). Green Chemistry
Letters and Reviews, 8(1), 1-7.
Velcárcel, M., Cárdenas, S., & Gallego, M.
(2000). Qualitative analysis revisited. Critical
Reviews in Analytical Chemistry, 30(4), 345-
361.
Vinson, J. A., & Grabowski, W. T. (1977).
Organic qualitative analysis. An improved
sodium fusion procedure and a new test for N
and S. Journal of Chemical Education, 54(3),
187.
Wang, C. Y., & Tarter, J. G. (1983).
Determination of halogens in organic
compounds by ion chromatography after
sodium fusion. Analytical Chemistry, 55(11),
1775-1778.
VII. Appendices

VI. References

Amrita (2011). Detection of elements:

Lassaigne’s test. Retrieved from: Figure 1A. Structure of
https://vlab.amrita.edu/? p-chloroaniline
sub=2&brch=191&sim=344&cnt=1

BYJUS (n.d.). Lassaigne’s test- test for

nitrogen, sulphur, halogens. Retrieved from:
https://byjus.com/jee/lassaigne-test/

Chemistry 33: Elemental Analysis by Sodium Fusion

Figure 2A. Structure of sulfanilic acid

Figure 3A. Structure of chlorobenzene

Chemistry 33: Elemental Analysis by Sodium Fusion