EXPT 6: ELEMENTAL ANALYSIS

II. OBJECTIVES

1. To prepare a sodium fusion test so as to be used in determining the presence of sulfur, nitrogen and
halogens.

2. To perform several qualitative tests to determine the presence of sulfur, nitrogen, and halogen in a
solution.

III. THEORETICAL FRAMEWORK

Characterization of an unknown organic compound includes the analysis of elements other than carbon,
hydrogen, and oxygen, which are most often present in organic compounds. These are the nitrogen,
sulfur, and the halogens (chlorine, bromine, and iodine). Detection of these elements in organic
compounds is usually done by sodium fusion. In this process, an unknown organic compound is fused
with metallic sodium at high temperature. The reaction converts them to the water-soluble inorganic
compounds; NaCN, Na2S, NaX (X = Cl, Br, and I). Inorganic qualitative analysis can be conducted to
determine the presence of the corresponding ions.

Organic compound containing C, H, O, N, S, X (up: Na) → (down: heat) NaCN, Na2S, NaX

IV. MATERIAL SAFETY DATA

COMPOUNDS/REAGENT: PHYSICAL PROPERTIES: HAZARDS:

1. Sodium metal -PHYSICAL STATE & IRRITANT:
APPEARANCE: solid (metal =skin & eye contact
solid), odorless, silvery in color =ingestion
-MOLECULAR WEIGHT: 22.99 =inhalation
g/mole FLAMMABILITY:
-SOLUBILITY: insoluble in cold =flammable
water, hot water
-CORROSIVITY: not available
2. p-chloroaniline -PHYSICAL STATE & IRRITANT:
APPEARANCE: solid (crystals =skin & eye contact
solid), sweetish odor, colorless =ingestion
-MOLECULAR WEIGHT: 127.57 =inhalation
g/mole FLAMMABILITY:
-SOLUBILITY: easily soluble in =may be combustible at high
diethyl ether, acetone. Soluble temperature
in hot water. Partially soluble in
cold water
-CORROSIVITY: not available
3. Sulfanilic acid -PHYSICAL STATE & IRRITANT:
APPEARANCE: solid (crystalline =skin & eye contact
solid), odorless, colorless =ingestion
-MOLECULAR WEIGHT: 173.19 =inhalation
g/mole FLAMMABILITY:
=may be combustible at high
temperature
 -SOLUBILITY: partially soluble in
cold water. Insoluble in
methanol, diethyl ether
-CORROSIVITY: non-corrosive in
presence of glass
4. Ferrous sulfate -PHYSICAL STATE & CORROSIVE/IRRITANT:
APPEARANCE: solid, odorless, =skin & eye contact
grayish-white to yellowish in =ingestion
color =inhalation
-MOLECULAR WEIGHT: 151.9 FLAMMABILITY:
g/mole + H2O =non-flammable
-SOLUBILITY: soluble in cold
water
-CORROSIVITY: not available
5. Sodium nitroprusside -PHYSICAL STATE & IRRITANT:
APPEARANCE: solid (crystals =skin & eye contact
solid), odorless, red in color =ingestion
-MOLECULAR WEIGHT: 297.95 =inhalation
g/mole FLAMMABILITY:
-SOLUBILITY: easily soluble in =non-flammable
cold water. Solubility in water:
43 g/100ml water @ 16 deg C
-CORROSIVITY: not available
6. Ferric chloride -PHYSICAL STATE & IRRITANT:
APPEARANCE: solid, odorless, =skin & eye contact
colorless =ingestion
-MOLECULAR WEIGHT: 162.21 =inhalation
g/mole FLAMMABILITY:
-SOLUBILITY: soluble in cold =non-flammable
water
-CORROSIVITY: non-corrosive in
presence of glass
7. Potassium fluoride -PHYSICAL STATE & CORROSIVE/IRRITANT:
APPEARANCE: solid =skin & eye contact
(deliquescent solid), odorless, =ingestion
white in color =inhalation
-MOLECULAR WEIGHT: 58.1 FLAMMABILITY:
g/mole =non-flammable
-SOLUBILITY: easily soluble in
hot water. Soluble in cold water.
Very freely soluble in boiling
water. Soluble in Hydrogen
fluoride, liquid ammonia.
Insoluble in alcohol unless water
is present
-CORROSIVITY: corrosive in
presence of glass
8. Ammonium hydroxide -PHYSICAL STATE & CORROSIVE/IRRITANT:
APPEARANCE: liquid, ammonia- =skin & eye contact
like odor, colorless =ingestion
-MOLECULAR WEIGHT: 35.05 =inhalation
g/mole FLAMMABILITY:
-SOLUBILITY: easily soluble in =non-flammable
water
-CORROSIVITY: extremely
corrosive in presence of zinc, of
copper. Corrosive in presence of
aluminum. Non-corrosive in
presence of glass, of stainless
steel (304) and (316)
9. Nitric acid -PHYSICAL STATE & CORROSIVE/IRRITANT:
APPEARANCE: liquid, =skin & eye contact
acrid/disagreeable and choking =ingestion
odor, colorless to light yellow =inhalation
-MOLECULAR WEIGHT: N/A FLAMMABILITY:
-SOLUBILITY: easily soluble in =non-flammable
cold water, hot water. Soluble in
diethyl ether.
-CORROSIVITY: extremely
corrosive in presence of
aluminum, of copper. Non-
corrosive in presence of glass, of
stainless steel (304) and (316), of
brass
10. Sulfuric acid -PHYSICAL STATE & CORROSIVE/IRRITANT:
APPEARANCE: liquid (thick oily =skin & eye contact
liquid), odorless (but has a =ingestion
choking odor when hot), =inhalation
colorless FLAMMABILITY:
-MOLECULAR WEIGHT: 98.08 =non-flammable
g/mole
-SOLUBILITY: easily soluble in
cold water. Sulfuric is soluble in
water with liberation of much
heat. Soluble in ethyl alcohol
-CORROSIVITY: extremely
corrosive in presence of
aluminum, of copper, of
stainless steel (316). Highly
corrosive in presence of stainless
steel (304). Non-corrosive in
presence of glass
11. Silver nitrate -PHYSICAL STATE & IRRITANT:
APPEARANCE: solid (crystals =skin & eye contact
solid), odorless, colorless/white =ingestion
 -MOLECULAR WEIGHT: 169.87 =inhalation
g/mole FLAMMABILITY:
-SOLUBILITY: easily soluble in =non-flammable
cold water, hot water. Soluble in
diethyl ether. Very slightly
soluble in acetone
-CORROSIVITY: non-corrosive in
presence of glass

V. SCHEMATIC DIAGRAM/METHODOLOGY

A. SODIUM FUSION

1. Set-up the apparatus for sodium fusion *draw*

2. Place a piece of sodium (pea-size: 4mm diameter) in a small test tube (10x75mm). Heat test tube until
sodium vapor is observed to condense on the walls of the tube

3. Remove flame immediately. Add about 0.3g of p-chloroaniline

4. Heat the tube gently to initiate the reaction with sodium. Remove flame when reaction subsides. Heat
to redness for 3 minutes

5. Drop the red-hot tube into a 50mL beaker containing 10mL distilled water as you hold a clean wire
gauze with tongs. Immediately place the gauze on top of the beaker [NOTE!!! Tube will shatter ON
CONTACT W WATER, releasing any unreacted sodium]

6. Allow excess sodium to react. When reaction has subsided, boil the solution in the beaker for 2
minutes.

7. Filter and use the colorless, alkaline filtrate as test solution for part B.

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

SULFUR TEST

1. Place 5 drops of fusion solution and 3 drops of water in a 5mL test tube.

2. Add 2 drops of 2% aqueous sodium nitroprusside solution. Observe the formation of a deep blue-
violet color

NITROGEN TEST

1. Add a pinch of FeSO4 to 1mL of the fusion solution in a test tube.

2. Add 5 drops of a 10% solution of KF

3. Boil the resulting mixture for 5 seconds. Then add 2 drops of 5% solution of ferric chloride.
4. Add “sufficient” amount of 6M H2SO4 to dissolve the insoluble iron hydroxides. Make the solution acid
to litmus

HALOGEN TEST

OF THE FUSION SOL’N

1. Place about 10 drops of the fusion solution into a small test tube.

2. If the sample is positive for N or S, acidify the solution by adding 2M HNO3

3. Heat the resulting solution to a gentle boil for about 1 minute to expel any HCN or H 2S present. Cool
to room temperature.

TO THE FUSION SOL’N

4. Add 4 drops of 0.1M AgNO3 solution to the fusion solution.

5. Indicate the presence of halogens by taking note of a heavy curdy-type precipitate. [Faint turbidity =
negative test; White = AgCl ppt; Pale Yellow = AgBr; Yellow = AgI]

DIFFERENTIATE AgBr FROM AgI

6. Conduct solubility test using dilute ammonium hydroxide.

7. TO THE PRECIPITATE: Add 0.5mL of 2M NH4OH. Stir with a glass rod to determine whether the solid is
soluble. {NOTE!!! AgI= insoluble in this solution; AgBr = slightly soluble}

[NOTE! Can carry out a preliminary test for halogen on the original sample

1. Make a small loop 3mm in diameter on a piece of copper wire (about 6 in) at one end. Insert the
other end into a cork to serve as a holder

2. Heat the coil in the hot portion of a Bunsen flame (until there’s no color to the flame)

3. Allow wire to cool. Dip into a small portion of the original sample.

4. Heat the sample in the hot portion of the flame. [GREEN: indicates presence of halogen]

VI. OBSERVATIONS AND RAW DATA

A2. OBSERVATIONS

A3. OBSERVATIONS

A4. OBSERVATIONS

A5. OBSERVATIONS

A6. OBSERVATIONS

B-S2. OBSERVATIONS

B-N3. OBSERVATIONS
B-N4. Acidity of solution (litmus)

B-H2: OBSERVATIONS. Acidity:

B-H3. OBSERVATIONS

B-H5. Indicate presence of halogens

- Faint turbidity = negative test

- White = AgCl ppt

- Pale Yellow = AgBr

- Yellow = AgI

B-H7: Conduct solubility test to differentiate AgBr from AgI

- AgI= insoluble in this solution

- AgBr = slightly soluble

VII. DATA ANALYSIS