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CHM Lab 4

This laboratory exercise aimed to determine the melting points of pure and impure benzoic acid using a Fisher-John melting point apparatus. The observed melting point range for the impure benzoic acid was 120-121°C, indicating it was not completely pure as the standard melting point for pure benzoic acid is 121-123°C. The experiment highlighted the importance of melting point determination in assessing the purity and identity of chemical compounds.

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0% found this document useful (0 votes)
59 views8 pages

CHM Lab 4

This laboratory exercise aimed to determine the melting points of pure and impure benzoic acid using a Fisher-John melting point apparatus. The observed melting point range for the impure benzoic acid was 120-121°C, indicating it was not completely pure as the standard melting point for pure benzoic acid is 121-123°C. The experiment highlighted the importance of melting point determination in assessing the purity and identity of chemical compounds.

Uploaded by

Treshon Persaud
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Download as DOCX, PDF, TXT or read online on Scribd
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University of Guyana

Faculty of Natural
Sciences
Department of Chemistry

Organic Chemistry for


Biological Sciences
Course Code: CHM 2206
Laboratory Exercise #4

Lecturer:Professor. R.Jagessar
Date Submitted:

Group Members
Ganda Soodo-1030292
Christael Greaves-1038813
Lewnessa Cato-1038749
Letetia Richard-1039767
Satram Mohamed-1041469
Title: Determination of melting points of chemical compounds

Aim/Objective: To determine the melting point of impure and pure benzoic acid

Theory:

A compound melting point is an important physical property since it helps to determine a

substance's identification and purity (OLABS, n.d). The melting point of a substance is the

temperature at which it transitions from solid to liquid; these phases are in equilibrium

(Helmenstine, 2021). Pure crystalline substances have higher melting points and can be

completely melted at temperatures ranging from 0.5 to 1 oC. When a substance is impure, its

freezing points drop and its melting point range expands significantly. A melting point range

more than 5 degrees Celsius suggests an impure composition. The degree of purity of a known

substance can be evaluated by comparing its melting point to that of a pure sample (OLABS,

n.d).

Safety Precautions:

● Avoid inhaling dust from the benzoic acid sample.

● After finishing handling, carefully wash your hands, face, and any exposed flesh.

● Put on safety equipment such as gloves, clothes, goggles, and face shields.

● While utilizing this product, refrain from eating, drinking, or smoking.

● If it gets on the skin, wash it off with water, take off any contaminated clothing, and get

help from a medical professional.

● Container should be tightly sealed and stored in a ventilated environment.

● If benzoic acid gets into the eyes, wash with plenty of water for several minutes

(Regulatory Affairs Thermo Fisher scientific, 2012).


Materials:

● Fisher John melting point apparatus

● Spatula

● Benzoic acid

● Coverslips

Diagram:
Procedure:

1. A clean coverslip was placed on the hot stage.

2. Using the spatula, a few crystals of benzoic acid were placed on the coverslip.

3. Another clean coverslip was placed over the benzoic sample.

4. The apparatus was turned on.

5. The rate of temperature increase was set to 100°C.

6. When the thermometer was observed at 100°C, the rate of temperature increase was

decreased to 20°C.

7. The sample was closely observed under the magnifying lens.

8. The temperature at which the first crystal began melting was recorded along with the

temperature at which the last crystal became liquid.

9. The coverslips were disposed of, the heat was turned off and the apparatus was left to

cool off.

Result:

Observed Melting Point for benzoic acid using both melting point apparatus = 120oC-121°C.

Discussion:

The sublimate that was gathered weighed 0.51 grams. The following formula was used to

calculate the percentage recovery: weight of the impure benzoic acid/weight of the sublimate

* 100 = 10.2%
Only 0.51 grams, or 10.2%, of the 5.00 grams of benzoic acid that were sublimated were

recovered. This can be a result of the sublimation technique's limitations. Sublimation must take

place in a vacuum at low pressure for a better recovery percentage. Recrystallization is more

selective than sublimation, although sublimation requires that the compound be volatile and the

impurities be nonvolatile.

The range of melting points for pure benzoic acid and the sublimate are displayed in Table 1.

Around 118 degrees Celsius, the sublimate began to melt; by 121 degrees Celsius, it had entirely

melted. At 113 degrees Celsius, the pure benzoic acid started to melt; at 120 degrees, it had

entirely melted.

The melting point range of the sublimate should only vary by 1-2 °C in order to be regarded as a

pure product. The sublimate was still impure and included contaminants because the temperature

difference was only 3 °C . The typical melting temperature of 121–123 °C was not detected

because of the impurities that were still present in the sublimate. The melting point range for

pure benzoic acid was 113–120 °C. It could not be regarded as a pure substance either.

Due to the 7°C discrepancy in the melting point range, it cannot be regarded as a pure substance.

This resulted from environmental contaminants contaminating the pure benzoic acid. The

melting point range decreases and widens due to contaminants. At the molecular level, they alter

the consistency and order of the crystal lattice. The pollutants do not properly fit into the clean

lattice that would normally exist. The lattice is weakened by this disruption, which makes it more

easily broken. At lower temperatures, the weakened structure melts more rapidly. The disruption

also results in molecular non-uniformity, with molecules nearest to impurities melting first and

melting more slowly the further away they are from the impurities, where the crystal lattice is

generally undisturbed.
A vacuum is necessary for sublimation to be more successful; only a small number of

compounds can sublimate, and the compound must be volatile while the impurities are

nonvolatile. These are some of the constraints of sublimation. Alternative techniques for figuring

out a substance's melting point include the Fisher-Johns Melting Point Apparatus and the Mel-

Temp Melting Point Apparatus, both of which use small, rounded glass coverslips and long, thin

melting-point capillaries.

Conclusion:

It can be determined from this experiment that the melting point range of the benzoic acid was

120-121°C, which would suggest that the organic compound is pure because the standard

melting point of pure benzoic acid is sharp at 121-123°C.

Question:

1. Indicate the type of melting point apparatus used to determine the melting point of the

two compounds (impure and pure benzoic acid).

Answer:

Fisher-John Melting point apparatus.

2. Will the melting point range of impure benzoic acid and recrystallized benzoic acid be

the same? Explain.

When benzoic acid is impure, it can contain other compounds or impurities that will lower the

melting point range and make it broader. Impurities can also cause the melting point range to

shift to a lower temperature or cause the melting point to be depressed.


Recrystallization is a common technique used to purify benzoic acid. During recrystallization,

the impurities are removed from the sample, resulting in a pure compound with a higher melting

point range that is narrower and more well-defined. Therefore, the melting point range of impure

benzoic acid will likely be lower and broader than the melting point range of recrystallized

benzoic acid, which will be higher and narrower.

3. Report both the literature and observed values for the melting point range for pure

benzoic acid. (Observed values will be provided by the lecturer).

Answer:

● Observed melting point values are 120oC-121oC.

● Literature melting point values are 121–123 °C.

4. Why it is advantageous to report the melting point range and not just a melting point.

A pure compound has a sharp and well-defined melting point. Reporting a melting point range

instead of a single point provides more information about the purity of the compound. If the

melting point range is narrow, it indicates that the sample is likely pure. If the melting point

range is broad, it suggests the presence of impurities.

Many compounds have a range of melting points rather than a single melting point. By reporting

a melting point range, it can be easier to identify an unknown compound or confirm the identity

of a known compound. The melting point range can be compared to published values to identify

the compound.

5. Why is it important and a must to determine the melting point of a compound?

Determining the melting point of a compound is an essential part of its characterization and

identification. The melting point of a compound is the temperature at which the solid and liquid
phases of a substance are in equilibrium. The melting point can provide important information

about the purity, identity, and physical properties of a compound.

Reference

Helmenstine, A, M. (2021, February 16). Melting point definition in chemistry. ThoughtCo.

https://www.thoughtco.com/definition-of-melting-point-604569

OLABS. (n.d). Melting point of an organic compound.

https://amrita.olabs.edu.in/?brch=7&cnt=1&sim=33&sub=73

Regulatory Affairs Thermo Fisher scientific. (2012, May 1st) . Safety data sheet.

https://www.fishersci.com/store/msds?

partNumber=A65500&productDescription=BENZOIC+ACID+ACS+500G&vendorId=VN0003

3897&countryCode=US&language=en

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