Name: Renz Marion C.

Dela Cruz Date Performed: 18 April 2012

Lab Partners: Jayson Palomar, John Carl Camayang, Almira de Villa, Leony Lyn Castellano

Experiment 2: Recrystallization and Melting Point Determination of Benzoic Acid

I. Objective
Performing recrystallization of benzoic acid in water by gravity filtration
From the determination of the melting point, the purity of the recrystalized benzoic acid
is determined

II. Schematic Diagram of the Procedure

Recystalization

Add boiling water in

0.25 tech grade benzoic Filter hot sol'n through
small amounts if some
acid in 25-ml E-flask + fluted filter paper into
solids remain dissolved. +
7mL water for boiling w/ another E-flask
pinch of charcoal then
1-2 min. duration. containing 3mL hot H2O.
heat until boiling.

Allow filtrate to cool
slowly w/out
disturbance. Collect
recrystallized benzoic
acid by filtration.
Wash crystal w/ min. cold
water for removing
adhering mother liquor.
Spread filter paper on
watch glass and air dry.
Wash crystal w/ min. cold
water for removing
adhering mother liquor.
RECORD! Weight and
%recovery.

Melting Pt. Determination

Tap lightly sealed end of

Pulverize smpl. by placing
crystals on watch glass and
crushing using spatula or t-
tube end.
Mound pulverized smpl. and
tube on tabletop. Put more
press open end of melting
samples on tube until it
pt. capillary tube into smpl.
reaches 2-4 mm height.
against watch glass surface.
Determine melting pt.

25 mL oil in 50 mL beaker. 2nd melting pt tube w/ smpl

Insert thermometer through
cork placing it on top of
thermometer. Attach
melting pt. tube w/ smpl. by
thin rubber strips.
In low flame, heat gently at
can be attached to other
rate of 3 deg C/min. Record
side of thermometer. Heat
temp when liquid droplet
oil bath strongly unti temp.
forms (start) and last trace
is 10-15 deg C below
of solid liquefied. (end)
melting pt.
 III. Table of Reagents/Products
Reagent/Product Structure Physical Hazards Disposal
Properties
Benzoic Acid Solid. Acidic. Hazardous in case of Organic Waste Jar
Boiling Point: 249.2C skin contact (irritant),
Melting Point: 122.4C of eye contact
Specific Gravity: 1.2659 (irritant), of ingestion,
Very slightly soluble in of inhalation. Slightly
cold water. hazardous in case of
skin contact
(permeator).

IV. Set-ups

Figure 1. Gravity Filtration Set-up Figure 2. Melting Pt. Determination Setup

V. Waste Disposal
Unrecrystallized benzoic acid must be recovered by allowing the mother liquor to air-dry and be
submitted to the instructor. Used oil may be stored in the locker and may be used in other
melting pt. expts. Dispose used capilliary tubes in solid waste containers.