Lourdes Patricia L.

Carreon Zaborah Eunice Bobadilla, Nerissa Unielle Quenga, Bernadette Toledo

November 22, 2011

RECRYSTALLIZATION AND MELTING POINT DETERMINATION OF BENZOIC ACID I. Objectives
  To recrystallize benzoic acid in distilled water To determine the melting point to examine the purity of recrystallized benzoic acid

II. Schematic Diagram of Procedure
A. Recrystallization

0.25 g tech grade benzoic acid in 25 mL Erlenmayer flask

+7 mL water and boil for 1-2 mins while stirring

dissolve all remaining solids by adding boiling water

+pinch of charcoal and gently heat to boiling

filter sol'n through fluted filter paper into another Erlenmayer flask with 3 mL hot water

collect recrystallized benzoic acid by filtration

wash crystals with minimum amount of cold water

spread filter paper on a watch glass and allow to air dry

transport crystals to previously weighed vial

report weight of crystals and % recovery

B. Melting Point Determination

dry crystals on watch glass and crush with metal spatula

press the open end of the melting point capillary tube into the sample against the surface of watch glass

tap sealed end of tube on the tabletop

25 mL oil in dry 50 mL beaker

determine melting point

introduce more samples into tube until the sample fill about 2-4 mm height

insert thermometer through a cork

attach melting point tube containing the sample to thermometer

heat oil bath until temperature is 1015°C below known melting point

record temperature reading when all solid is liquefied

record temperature as soon as a droplet of liquid forms in tube

heat using very low flame (oil bath temperature rises at 3°C per minute)

allow oil batch to cool and make another trial using fresh sample

III. Table of Reagents/Products Reagent/Product Structure Physical Properties Hazards
Hazardous in case of skin contact (irritant), of eye contact (irritant), of ingestion, of inhalation. Slightly hazardous in case of skin contact (permeator). The substance is toxic to lungs, the nervous system, mucous membranes. Repeated or prolonged exposure to the substance can produce target organs damage.

Benzoic acid

MOLECULAR WEIGHT: 122.121 g/mol MELTING POINT: 123°C BOILING POINT: 249°C DENSITY:1.316 g/cm3 APPEARANCE: white crystals or powder

IV. Set-up Gravity Filtration Set-up

V. Waste Disposal  Unrecrystallized benzoic acid – allow mother liquor to self dry and submit to instructor  Used oil – store in locker  Used capillary tubes – solid waste containers VI. Data Sheet

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