Experiment # 1

Melting Point Determination and Identification

of an Unknown Substance
Melting Point Definition

Melting Point (Range): temperature range at which a solid changes to a

liquid?

Pure substances typically have a narrow range: also described as

“sharp” M.P.
The difference <1o or between 1-2o.

Ice is melting (0 oC)

Effect of impurities on Melting Point:

Soluble impurities:
Lowers the melting point:
- Starts melting at a temperature lower than that of the
pure substance (ice starts to melt at < 0 oC, salt in ice)
Broadens slowly continues to melt as the temperature rises
- difference 4-5 degrees or even greater.
Insoluble impurities
Typically, these do not affect the melting point,
ex. Trans- cinnamic acid + charcoal
Right amount of
sample
Experiment:

Fill the melting point capillary

- Thin-walled, fragile, sealed at one end
- Sample must be dry, finely powdered
- Fill with a small amount: to a column height of about 1/8 in. long
- Put the right amount of sample
- Tap gently to pack it well- careful
- Place it in the apparatus and measure
Determine the melting point of:

1. Melting point of known substances:

trans- cinnamic acid m.p. = 133oC
Urea m.p. = 133oC
- Heat rapidly to within 10oC of known M.P.
- Continue heating slowly: about 1oC per minute
- Report two temperatures:
- Sample starts to melt
- Sample is completely melted

Softening or shrinking of the sample is NOT to be

considered melting- you must be able to see liquid!
3. Determine the melting points of mistures:

- Mixtures of trans- cinnamic acid and urea

trans- cinnamic acid: urea
1:1
1:4
4:1
– observe the lowering and broadening of the melting
range.
2. Melting Point of Unknown substance:
Do m.p. determination twice:

First reading: heat rapidly, Approximate m.p. range,

Cool down the apparatus to at least 10oC below the approximate
M.P.,
Second reading: heat slowly (about 1oC per minute): use a new
sample, in a new tube!
Concept of mix melting point to reconfirm the identification of an
unknown (Do not do it in lab).

Determine its identity by comparison with the given list

of possibilities.
What to perform in the lab?

• Determine m.p. of Urea

• Determine m.p. of trans-cinnamic acid
• Determine m.p. of mixture of trans-cinnamic acid + urea in 1:1, 1:4
and 4:1 ratios
• Determine the melting point of one of the unknown given in letter
A,B,C,D ……… and identify it by comparing its m.p. with the given
melting points of different substances in the book. Confirm your
unknown with your TA before you leave the lab.
( Do not do mix m.p. and trans- cinnamic acid + charcoal mixture)
Prelab Questions:

1. Why should the melting point sample be finely powered?

2. How can melting point be used to determine the purity of a
substance?
3. What type of error might be expected if melting point capillaries
tubes are not thin-walled?
Post-lab Questions:

1. You are given two sample tubes, each containing a white power:
your task is to determine if these powders are pure substances and
two samples of same substance.
Briefly describe your strategy for completing your task.
2. Is melting point alone sufficient to establish the identity of a given
unknown substance? Explain briefly.