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LEONG, Jo-Celine M.

LUKBAN, Claudine Rosario B.

CHEM 31.1 – Experiment 06


Elemental Analysis
Experiment Performed on January 17, 2011

A. Sodium Fusion
1. Set-up apparatus
2. In test tube, add pea-size sodium (4mm diameter) and
heat until vapor condenses on walls of test tube.
3. Remove from flame. Add 0.3g p-choloaniline.
4. Heat tube gently for sodium re-reaction. Remove flame
when reaction subsides. Heat to redness for 3 mins.
5. Drop tube into 50mL beaker (with 10mL water). Cover
with wire gauze. Allow excess sodium to react. Boil
solution for 2 mins. Filter and use alkaline filtrate for
Part B.
6. Repeat with Sulfanilic Acid.

B. Qualitative Tests
SULFUR TEST:
1. In 5mL test tubes, add 5 drops fusion solution and 3
drops water.
2. Add 2 drops 2% aqueous sodium nitroprusside
solution.
3. Observe formation of deep blue-violet color.

NITROGEN TEST:
1. In test tube with 1mL fusion solution, add pinch of
FeSO4.
2. Add 5 drops 10% KF solution.
3. Boil mixture for 5 seconds, add 2 drops 5% ferric
chloride.
4. Add 6M H2SO4 to dissolve iron hydroxide. Make
solution acid to litmus.
5. Observe deep blue formation (N)
IF BLUE FORMATION NOT APPARENT:
6. Filter mixture, wash filter paper with water, examine
residue.

HALOGENS:
1. a. Place 10 drops fusion solution to small test tube.
b. IF POSITIVE FOR N or S, acidify solution by adding
2M HNO3.
c. Heat to gentle boil, for 1 min. Cool to room temp.
2. To fusion solution, add 4 drops 0.1 M AgNo3. HEAVY
CURDS = +Halogens (AgCl = white; AgBr = pale
yellow; AgI = yellow). NO CURDS = NO HALOGENS
3. TO DIFFERENTIATE AgBr FROM AgI, solubility test
with ammonium hydroxide:
a. To precipitate, add 0.5 mL 2M NH4OH; stir with
rod. Determine if solid is soluble.
b. AgI = INSOLUBLE; AgBr = SOLUBLE.
c. May use color flame test as preliminary test for
halogen. ***

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