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G.

Alur
 Recrystallization
1 gram of salicylic acid

Put in a 125 mL erlenmeyer


Added 5 mL of aquades.
Heated the mixture until it is homogeneous while shaken.
Added slowly every 10 mL of water (± 70mL) until the crystals have dissolved
Calculated V aquades needed
Add a few drops of distilled water to make it completely homogeneous.
Add to it 1-2% of the weight of salicylic acid (if the solution is colored)
Bring to a boil while stirring for a while.
Filtered in a hot state

Filtrate Residue

Heated up
Cooled at room temperature
Filtered with a buchner funnel enclosed by a vacuum pump.

Residue Filtrate
Dried by inserting it into the desiccator
Weighed its mass
Tested the melting point and compared with the melting point of the original substance

Observation result
 Making aspirin.
2.5 grams of salicylic acid.

Put in a 125 mL erlenmeyer.


3,75 CH3COOH anhydride added.
Put in a water bath (temperature 55-60 ℃) while stirring.
Cooled at room temperature.
Plus 3 drops of concentrated H2SO4.
Plus 37.5 mL of distilled water.
Heated until homogeneous.
Filtered with a buchner funnel equipped with a vacuum pump.

Residues Filtrate

Added 7.5 mL 96% ethanol and 25 mL aquades.


Heated up.
Filtered with a buchner funnel equipped with a vacuum pump.
Dried out

Residues Filtrate

Weighed its mass Tested with FeCl3


Tested the melting
point

Observation result Observation result


H. Observation Data
G.
Conclusion

 To get pure salicylic acid use a solvent that dissolves well in hot conditions, but
only slightly soluble in cold conditions. Usually polar compounds are
recrystallized in less polar solvents or vice versa.
 The principle in recrystallization experiments is the difference in solubility of
substances dissolved in one solvent.
 The percentage of salicylic acid crystalline mass obtained by the experiment was
53.2%. When the salicylic crystal melting point is tested, melting at 160 ° C.
This is consistent with the literature, salicylic acid is a crystalline powder that
melts at 158⁰ - 160 ° C (Dewi et al, 2016: 19).
 Making aspirin (acetyl salicylic acid) can use the Fischer esterification reaction
between salicylic acid and acetic acid anhydride, and sulfuric acid as a catalyst.
Esterification reaction is carried out by reacting acids and alcohols with mineral
acids as a catalyst, the process is an equilibrium that is accelerated by hydrogen
ions (Feiser & Feiser, 1957)
 In the experiment of making aspirin, aspirin produced 46.65%. When tested with
FeCl3 the results are inconsistent with the reaction. this is because the aspirin
obtained is not pure aspirin. The dissimilarity with the theory could be because
the ingredients of making aspirin namely salicylic acid and acetic acid anhydride
are not pure compounds so the results of making aspirin are slightly different
from the theory. When the melting point is tested at 136 ℃ where the aspirin
melting point is theoretically 133.3 ℃ - 133.6 ℃.
H. dokumentasi
No Proses Gambar Keterangan
1 rekristalisasi 1 gram asam
salisilat

2 rekristalisasi 1 gram asam


salisilat dan air
yang dipanaskan

3 Rekristalisasi Setelah larutan


dipanaskan

4 Rekristalisasi Penyaringan asam


salisilat dalam
keadaan panas
menggunakan
corong buchner
dan vacuum power
5 Rekristalisasi Larutan setelah
disaring

6 Rekristalisasi Setelah didiamkan


beberapa menit,
kristal terbentuk

7 Rekristalisasi Kristal setelah


dikeringkan di
dalam desikator

8 rekristalisasi Kristal diuji titik


lelehnya. Didapat
titik leleh kristal
sebesar 160℃
9 Pembuatan 2,5 gram asam
aspirin salisilat
ditambahkan asam
asetat anhidrat

10 Pembuatan 2,5 gram asam


aspirin salisilat
ditambahkan asam
asetat anhidrat
setelah dipanaskan
dalam penangas
air.
11 Pembuatan Residu pada
aspirin penyaringan yang
pertama

12 Pembuatan Residu + 7,5 ml


aspirin etanol + 25 ml
aquades,
menghasilkan
larutan tidak
berwarna
13 Pembuatan Aspirin zetelah
aspirin dikeringkan
menggunakan
desikator

14 Pembuatan Massa aspirin yang


aspirin didapatkan

15 Pembuatan Suhu ketika aspirin


aspirin mencapai titik
lelehnya yaitu 136

16 Pembuatan Aspirin + FeCl3 ,


aspirin menghasilkan
larutan berwarna
kuning ( aspirin
murni )

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