Week 4 Melting point & Solubility 1211

Dr. Urmi Doshi

Experiment 3: Determination of Melting point (to examine

purity) and Solubility of the Unknown Organic acid
**** Obtain a new unknown organic acid sample and record the sample number in your
notebook *****
All the data tables and text in orange should be copied and completed in your
NOTEBOOK

Melting point
(Read pages 27-29, 65-67 of the lab manual)
(Report sheet is on p.85 of the lab manual)
There are 3 steps:
1. Quick estimate of the expected melting point range
2. Record the actual melting point of the unknown acid and the standard sample
3. Confirm melting point by repeating step 2

1. Quick estimate of the expected melting point range

a. Filling the Capillary tube
Read p.67 of lab manual.
Fill a thin wall capillary tube sealed at one end with a small
amount of sample (fill up to inch depth). Tap the tube gently
with fingers to or a file to firmly pack the sample at the bottom of
the tube.

b. Placing the sample in the melting point device

Place the capillary tube in the sample tube holder.
Make sure you can see the capillary tip through the eye viewer.

Week 4 Melting point & Solubility 1211

Dr. Urmi Doshi

c. Setting the plateau temperature

Plateau temperature is the temperature to which the melting point device will heat
QUICKLY
Press and hold the SET button
Use arrow keys to set the plateau temperature to 200 C
Release the SET button

d. Recording the melting temperature

Press START to begin heating.
The top red light is ON when the sample is heated quickly.
The middle red light becomes ON when the plateau temperature is reached.
Press START to begin heating. The ramp rate of heating should be set to 1C/minute.
The lower green light becomes ON when the sample is heated in the RAMPING mode
SLOWLY.
Observe the sample very CAREFULLY.
Record the temperature (T1) at which the sample begins to melt (i.e. when the edges
start to soften) AND
Record the temperature (T2) at which the sample has fully melted (i.e. when you see
only liquid in the tube).
Press the STOP button and allow the unit to cool down to ambient temperature before
using again.
Melting Point range : ___- ___ C. (example: T1= 215, T2 =217, Melting point range:
215-217 C)
Plateau Temperature: ________C

e. Select a standard sample with melting point near the melting point range of
your unknown acid
Record the melting point value of the standard sample printed on the bottle

Week 4 Melting point & Solubility 1211

Dr. Urmi Doshi

2. Record the actual melting point of unknown acid and the standard sample
a. Fill (as in 1.a) a fresh capillary tube with unknown acid and a second capillary tube
with the standard sample.
b. Insert both the tubes in the melting point device ONLY once the unit has cooled down
preferably at least 20 C below the plateau temperature.
c. Set the plateau temperature (as in 1.c) 20 C below the melting point of the unknown
acid or the standard sample, whichever is lower.
d. Record the melting temperature as in 1.d.
e. Observe both the samples carefully and record melting temperature for both the
samples:
T1 (temperature at which
edges start to soften)

Unknown acid
Standard sample

C
C

T2 (temperature at which
the crystals have
completely turned into
liquid)
C
C

Plateau Temperature: __________C

f. Press the STOP button and allow the unit to cool down to ambient temperature before
using again.

3.Confirm melting point by repeating Step 2

If in Step 2, the plateau temperature was set to very high or the ramp rate was high, the
sample will get heated rapidly resulting in a broad melting point range and inaccurate
melting point.
Based on the results of Step 2, lower the plateau temperature.
Repeat steps 2.a to 2.f and record the following:

Week 4 Melting point & Solubility 1211

Dr. Urmi Doshi

T1 (temperature at which
edges start to soften)

Unknown acid
Standard sample

C
C

T2 (temperature at which
the crystals have
completely turned into
liquid)
C
C

Plateau Temperature: __________C

Solubility
Determine Solubility of 0.1g of your new unknown organic acid in 2ml solvent
Solvent

De-ionized
water
1:3 Ethanol:DI
water
1:1 Ethanol:DI
water
3:1 Ethanol:DI
water
Ethanol

ml of Ethanol

ml of Deionized water

2.0

0.5

1.5

1.0

1.0

1.5

0.5

2.0

Room
temperature
Solubility
e.g. YES or
NO

Hot solvent
Solubility
e.g. YES or
NO

Solubility unknown organic acid in ___________________solvent (Choose the

solvent with the lowest % of Ethanol)