Sodium Fusion Test (Lassaignes Test)

-Qualitative test for halogens, sulfur, and nitrogen

Sodium

-very strong reducing reagent that is able to break up the carbon chain of
organic compounds
-convert the atoms that are covalently bonded to the carbon chain into
inorganic ions
Nitrogen to cyanide (CN-)

Sulfur to sulfide ions (S2-)

Cl, Br, I to ions (Cl-, Br-, I-).

, , , , , , 2,
HYPOTHESIS

The compounds to be tested are (1) p-chloroaniline

(C6H6ClN), which is expected negative for sulfur,
but positive for both nitrogen and halogen:
chlorine and (2) sulfanilic acid (C6H7NO3S), which
is expected positive for both sulfur and nitrogen,
but negative for halogen.
(1) To conduct the Sodium Fusion Test on
the given compounds and subject them
to Sulfur, Nitrogen, and Halogen tests

(2) To check the consistency of the

experimental results to the theoretical
results
MATERIALS and REAGENTS

(10) 5ml test tubes 0.5 g Na metal

1g p-chloroaniline
(2) 50 ml beaker 1 g sulfanilic acid
(2) filter paper 2g Ferrous sulfate
(1) burner 1ml 2% sodium
nitroprusside
(1) test tube holder 1ml 10% potassium
(1) wire gauze fluoride
(1) iron ring 5ml 2M ammonium
hydroxide
5ml 2M nitric acid
10ml 6M sulfuric acid
0.5 ml 0.1M silver nitrate
A. SODIUM FUSION

5-ml test tube

Test tube holder

Burner

Figure 1: Sodium Fusion Set-up

A. SODIUM FUSION

Na *VAPORS*

test tube (10x75mm)

A. SODIUM FUSION

REMOVE FLAME Remove flame

Na
IMMEDIATELY + 0.3g p- when reaction
choloraniline subsides
*gently*

Then HEAT to REDNESS for 3 minutes

A. SODIUM FUSION
NOTE: The tube will shatter on contact
Holding a clean with the water, releasing any unreacted
with sodium.
on free hand
Na

*red hot*

+ 10 mL water
A. SODIUM FUSION

Allow excess Sodium to

react, and when reaction has
subsided

Na
BOIL the solution in the
beaker for 2 minutes. *FILTER*

***repeat using sulfanilic acid sample

B. QUALITATIVE TESTS
1. Sulfur Test
(use p-chloroaniline and sulfanilic acid fusion solutions)

Place 5 fusion
Na
solution Add 2 drops of
2% aq. Sodium
nitroprusside
solution.
Place 3 water

**observe**
B. QUALITATIVE TESTS
1. Nitrogen Test
(use p-chloroaniline and sulfanilic acid fusion solutions)

Add a pinch of
FeSO4 to 1 ml
of fusion Na 5 drops 10% *boil* (5
solution in a KF solution seconds)

6M H2SO4 to
dissolve
insoluble iron 2 drops 5%
hydroxides and ferric chloride
make it acid to solution
litmus
B. QUALITATIVE TESTS
2. Nitrogen Test
(use p-chloroaniline and sulfanilic acid fusion solutions)

If result is ambiguous,
DEEP Na filter the mixture,
BLUE
Positive wash it with distilled
water, and examine
residue for blue
coloration
B. QUALITATIVE TESTS
3. Halogen Test
(use p-chloroaniline and sulfanilic acid fusion solutions)

Na

Bunsen Burner
B. QUALITATIVE TESTS
3. Halogen Test
(use p-chloroaniline and sulfanilic acid fusion solutions)

10 drops of
fusion solution
Na

If (+) for N or S
add 2M
HNO3
Cool to room
temperature
B. QUALITATIVE TESTS
3. Halogen Test
(use p-chloroaniline and sulfanilic acid fusion solutions)

Na AgBr vs. AgI

4 drops 0.1 M
AgNO3
Add: 2M
solution
NH4OH (stir)

**Heavy-curdy type precipitate = AgI= insoluble

presence of Halogens AgBr= slightly
soluble
AgCl = white; AgBr = pale yellow; AgI =yellow
 Sample Sulfur Test Nitrogen Test Halogen Test
(Theoretical)
P-chloroaniline Negative Positive Positive

Sulfanilic acid Positive Positive Negative

Table 1: Experimental Results

P-chloroaniline Sulfanilic Acid

FUSION TEST SOLUTIONS
S
ODIUM


, , , , , , 2,
p-chloroaniline

sulfanilic acid
NaCl + NaCN

Na2S + NaCN
Na NaSCN

+ 2 +
Sulfur Test

2 + 2 5
4[ 5]
(violet)
 Sulfur
Nitrogen
sulfanilic acid Halogen
Nitrogen Test

Fe4[Fe(CN)6]3
Prussian Blue
FeSO4 + 2NaOH Fe(OH)2 + Na2SO4
(dark green precipitate)

Fe(OH)2 + 6NaCN Na4Fe(CN)6 + 2NaOH

(sodium ferrocyanide)
3Na4Fe(CN)6 + 2Fe2(SO4)3 Fe4[Fe(CN)6]3 + 6Na2SO4
(Prussian blue complex)

+ 10% Solution of KF (to make the color distinct)

+ 6M H2SO4 (to dissolve excess iron oxides)
 Sulfur
Nitrogen
sulfanilic acid
Halogen
Sulfur
Nitrogen
p-chloroaniline Halogen
Halogen Test
NaCl + AgNO3 AgCl(s) + NaNO3
(white ppt)

NaBr + AgNO3 AgBr(s) + NaNO3

(pale yellow ppt)

NaI + AgNO3 AgI(s) + NaNO3

(yellow ppt)
Prior to Silver Nitrate Test

+ 2M HNO3 +

To expel any HCN or H2S present

Without this step
CN- AgCN

S 2- Ag2S
Halogen Test
NaCl + AgNO3 AgCl(s) + NaNO3
(white ppt)

NaBr + AgNO3 AgBr(s) + NaNO3

(pale yellow ppt)

NaI + AgNO3 AgI(s) + NaNO3

(yellow ppt)
 Sulfur
Nitrogen
p-chloroaniline
Halogen
 Sample Sulfur Nitrogen Halogen
Test Test Test

p-chloroaniline - +(blue ) +(white )

sulfanilic acid +(violet ) +(blue ) -
Beilsteins Test for Halogen

Chloride Bromide Iodide

 PHOSPHORUS
-can be detected through its phosphine odor
during Na fusion (garlic-like)
-a black color will be produced upon placing the
filter paper on top of fusion tube (w/ moistened
AgNO3)
-1 mL of the fusion soln was treated with 3 mL
conc. HNO3 (aq), and was boiled
-After cooling, equal volume of ammonium
molybdate is added
-Mixture is warmed to 40-50 C.
-Presence of Phosphorus was seen as
ammonium molybdate separated from the
mixture as a yellow crystalline precipitate
1. Outline the procedures for
detecting the presence of oxygen
and phosphorus in organic
compounds.
OXYGEN
-Ferrox Test
-On a dry spot plate, grind one crystal of ferric
ammonium sulfate, FeNH4(SO4)2, and a crystal of
potassium thiocyanate, KSCN, using a glass rod
-Place 2 drops of unknown to separate test
tubes
-Use glass rod (with ground up crystals
attached to it) to stir the unknown
-dissolution of crystals in the unknown and
formation of reddish-purple color indicate a
positive result
SULFUR Oxidation Test

The organic compound is fused with a mixture of potassium nitrate and sodium
carbonate.
(If sulfur is present, it gets oxidized into sodium sulfate.)

3KNO3 3KNO2 + 3O
Na2CO3 + S + 3O Na2SO4 + CO2
(sodium sulfate)

Next, the fused mass is extracted with water. These contents are boiled and
filtered. The filtrate contains sodium sulfate. This is acidified with dilute
hydrochloric acid and added with a solution of barium chloride.
(If sulfur is present, a white precipitate forms.)

BaCl2(aq) + Na2SO4(aq) BaSO4 + 2NaCl(aq)

(white precipitate)

2. Discuss other methods of

detecting the presence of sulfur,
nitrogen, and halogen in organic
compounds.
NITROGEN Sodalime Time Test

A pinch of the organic compound is heated strongly with sodalime in a test tube.
(The evolution of ammonia indicates the presence of nitrogen.)

CH3CONH2 + [NaOH + CaO] CH3COONa + NH3

(acetamide) (sodalime)

*However, a large number of organic compounds such as nitro and diazo

compounds do not liberate ammonia under these conditions.

2. Discuss other methods of

detecting the presence of sulfur,
nitrogen, and halogen in organic
compounds.
HALOGENS Beilsteins Test

A copper wire flattened at one end is heated in the oxidizing flame of Bunsen
burner until it does not impart blue color to flame. The hot end of copper wire is
now dipped to the organic substance and is once again kept in flame.
(The reappearance of green or blue color indicates the presence of halogens in the
organic compound.)

*However, substances such as urea and thiourea do not contain halogens,

but is positive for this test. Also, it does not tell as to what halogen is present
in the organic compound.

2. Discuss other methods of

detecting the presence of sulfur,
nitrogen, and halogen in organic
compounds.
The Lassaignes Test, consisting of the Sodium Fusion and the
separate inorganic qualitative tests, produced results that
matched with the theoretical results stated
earlier, that is:

(1) p-chloroaniline being negative for sulfur, but positive for

both nitrogen and halogen chlorine

(2) sulfanilic acid being positive for both sulfur and nitrogen,
but negative for halogen.

Moreover, aside from the Lassaignes Test, the detection of the

presence of the elements sulfur, nitrogen, and halogens chlorine,
bromine, and iodine is possible through the Oxidation Test, the
Sodalime time Test, and the Beilsteins Test respectively.
ERROR ANALYSIS and
RECOMMENDATIONS

It is recommended that for the Halogens

Test, a preliminary Beilsteins Test
should be conducted first in order to save
time.
 Thank you!
Merry Christmas and a
Happy New Year!