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Result Lab OC Ex2

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9 views

Result Lab OC Ex2

Uploaded by

Hoàng Lâm
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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RESULT

Part 1: Recrystallization of Benzoic acid

Figure 1: The mixture of benzoic acid and distilled water at the room temperature.

Figure 1 illustrates the 0.5032g insolubility of benzoic acid when we add 20mL distilled
water. This mixture is additionally placed at the room temperature around 21 – 23oC. Before
stirring or after stirring, the acid cannot dissolve in the water. It is to be measured based on the
identification sign is white precipitate of the benzoic acid which sediment under the liquid. After
swirling, there is a part of the precipitate floats to the surface of the solution, but it does not
dissolve.
Aluminum foil

Figure 2: The appearance of white crystals inside the solution.

The mixture after swirling will be token on the hot plate with a temperature 250oC to
dissolve the original impure benzoic acid. After heating the mixture until the original impure
benzoic acid is completely dissolved in the distilled water solution, the baker will be left to cool
outside for about 2 to 3 minutes. The baker will be soaked in cold water to accelerate up the
formation process and will take less time if the combination is kept at room temperature. This is
intended to boost the formation efficiency as well as increase the quantity of crystals. The
benzoic acid crystals, which we are gathering, may be higher in purity since the layer of
aluminum foil enclosed in a bag keeps airborne contaminants out of the solution.
Figure 3: The benzoic acid crystals after washing and drying

The process after the appearance of the acid crystals is collecting the crystals by the
filtration in a Buchner funnel apparatus and get all the crystals by the stirring rod. Putting the
crystals rinse with 1 to 2mL of cold water. It has two effects: remove the impurities and get all
the crystals out of the flask. Before the drying completely, we use the spatula to lift the crystals
out of the funnel. Dried pure benzoic acid will be transferred to the 0.06g weighing boat.

Calculation to determine the recovered benzoic acid:

mbenzoicacid after recrystallization −mweighingboat 0.4855−0.06


%recovered = x 100 %= x 100 %=84.56 %
mimpure benzoic acid 0.5032
Part 2: Recrystallization and identification the unknown compound

Unknown compound 3 Unknown compound 2 Unknown compound 1


+ ethanol + methanol + distilled water
Figure 4: The respective impure unknown compound in three different solutions:
ethanol, methanol, and distilled water.

Figure 4 shows the solubility of the unknown compound when adding alternately ethanol
and methanol; however, the compound does not dissolve in the distilled water in room
temperature. We determine in the table to show the comparison and acceptation of solution we
choose:

Room temperature
Unknown compound 1 (0.5022g) + 20mL distilled water Insoluble => accept
Unknown compound 2 (0.5149g) + 20mL methanol Fully dissolve -> soluble => reject
Unknown compound 3 (0.5077g) + 20mL ethanol 85% solubility => reject
Table 1: The comparison of three unknown compounds in difference of solutions.

The lower solubility solution in room temperature, the higher solubility in high
temperature, so, the unknown compound 1 mixed with distilled water is the best choice to do the
next step in this experiment depending on the comparison of Table 1.

Doing step-by-step like the experiment in Part 1, after stirring in the high temperature at
315oC, the solution fully dissolve, then, it takes time to cool and puts into the ice-water path. The
crystals do not appear when we put the soluble solution after heat; otherwise, we have the extra
step which is scratching the inner wall of a flask with a stirring rod to make the crystal
formation. The crystals are collected by filtration step just like the experiment in Part 1 in the
Buchner funnel apparatus. The variation must be carefully taken out all the crystals the beaker by
the stirring rod to ensure the maximum weight of the pure crystals.

Figure 5: The unknown crystals after washing and drying

The observation of the crystals after drying can determine by calculating the recovered of
this unknown compound:

munknownafter recrystallization −mweighingboat 0. 2983−0.06


%recovered = x 100 %= x 100 %=47.45 %
mimpure unknowncompund 0.50 2 2
To identify the unknown compound, the crystals will be crushed and then using the previous
technique in Experiment #1 to observe the melting points and pursue the compound by the given Table 2-
1: Melting points data for the possible unknown samples.

Figure 6: The observed melting points of the unknown compound.

According to the Table 2-1, the melting points range of the acetylsalicylic acid is 134 – 136 oC.
Hence, the unknown compound in this case is acetylsalicylic acid.

DISCUSSION

1. What properties should ideally be possessed by recrystallization solvent?

For choosing the solvent of the recrystallization process, the solvent should be higher dissolve the
solid in the high temperature, not the lower solubility of the solution in the room temperature.
Additionally, the dissolved solid will be cooled down and we take the observation of the purified crystals
formation.

2. Why are crystals wash with additional solvent when collected? Why cold solvent?

The crystals must be washed by the cold solvent (example: ice water) to ensure that there are
more purified crystals will be rinsed out. If using warm solvent, the crystals should be dissolved in
this washed solvent. Hence, the result will be deprivation.

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