Organic Chemistry Report n7

NATIONAL UNIVERSITY OF CALLAO 2016
Faculty of Environmental Engineering and Natural Resources
Course: Organic Chemistry.
Practice No.: 7
Qualification: Recrystallization.
Schedule: 90-G (MONDAY)
Teacher: Álvarez López, Santos Pio.
Date of realization: 30/05/16
Date of delivery: 06/06/16
Members:
* Laura Oré, Erick Smith. 1519510052

* Mateo Tagle, Diego Alberto. 1519510097
* Oropeza Misari, Jhunior Luis. 1519520298
* Tejeda Berrios, Cynthia Julissa. 1519530015
RECRYSTALLIZATION Page 1
NATIONAL UNIVERSITY OF CALLAO
INDEX
Content
SUMMARY..........................................................................................................................................3
INTRODUCTION..................................................................................................................................4
GOALS................................................................................................................................................5
THEORETICAL FRAMEWORK...............................................................................................................6
Crystallization.................................................................................................................................6
Separation method of homogeneous material systems.................................................................6
Types of crystallization...................................................................................................................6
a) Dry crystallization...............................................................................................................6
b) Wet crystallization..............................................................................................................6
Recrystallization.............................................................................................................................6
EXPERIMENTAL DEVELOPMENT.........................................................................................................6
Materials........................................................................................................................................6
Recrystallization process................................................................................................................8
CONCLUSIONS..................................................................................................................................10
RECOMMENDATIONS.......................................................................................................................11
APPENDIX.........................................................................................................................................11
BIBLIOGRAPHY.................................................................................................................................12
SUMMARY
Recrystallization is used for the purification of solid compounds and is based on the
differences in solubility of solids in different solvents and the fact that they are much more
soluble in hot solvents than in cold ones. The solid is soluble if it is not observed in the
mixture. Increasing the temperature increases the solubility, saturating the solution, but
when it cools again the concentration is so great that crystals will form, in which different
molecules will not fit. The impurities remain in the solution. The technique consists of the
following steps:
* Dissolve the substance in the solvent at boiling temperature.

* Treat with activated charcoal to remove absorbable impurities.
* Filter the hot solution to remove insoluble impurities.
* Let the solution cool so that the crystals of the substance can settle.
* Filter the cold solution to separate the crystals from the supernatant solution
(known as liquor or mother liquid).
* Wash the crystals to remove the adhered mother liquor.
* Dry the crystals to remove traces of the solvent.
Choosing the right solvent is very important. An ideal solvent is one that: is not very
volatile, is not flammable, is cheap, does not react with the solute, dissolves a large
amount of the substance to be purified at high temperature and little at room temperature,
does not dissolve either cold or hot. impurities or do it only cold.
INTRODUCTION
In this report you will find step by step the entire process carried out by the recrystallization
technique of an organic compound. In this case we will use Activated Carbon, which in this
report is explained in detail with images based on our experience and the process we did
in the laboratory, observing changes in the types of changes that the compound
underwent both in appearance and in mass after going through everything. the re-
crystallization process.
GOALS
 Know and recognize recrystallization to separate impurities in liquids.
 Identify the characteristics and factors involved in the recrystallization process.
 Learn to choose the right solvents for good recrystallization.
 Acquire skill and knowledge about the recrystallization technique.
THEORETICAL FRAMEWORK
Crystallization
It is a chemical process by which, from a gas, a liquid or a solution, ions, atoms or
molecules establish bonds to form a crystalline network, the basic unit of a crystal.
Crystallization is used quite frequently in Chemistry to purify a solid substance.
The most important part of the crystallization process is the growth of the crystals. The
shapes or different sizes that the crystals acquire are due to different conditions, such as
the solvent used or the concentration of the different compounds used. Crystals grow by
forming layers of molecules around an initial crystal.
Separation method of homogeneous material systems

It allows you to separate substances that form a homogeneous material system, for
example: drinking water is a solution formed by water and salts dissolved in it. The three
best known methods are: Evaporation or capitalization, chromatography and distillation.
The crystallization operation is the process by which a component is separated from a
liquid solution by transferring it to the solid phase in the form of crystals that precipitate. It
is a necessary operation for any chemical product that is commercially presented in the
form of powders or crystals, whether sugar or sucrose, common salt or sodium chloride.
Types of crystallization
a) Dry crystallization
The solid melts at high temperature. It then cools and when it solidifies, crystals
form. Certain solids come into contact with a cold surface and crystals form on it.
b) Wet crystallization.
A saturated solution of a certain solid that was said to crystallize is prepared, for
example common salt. The solvent, water for example, evaporates and the
dissolved solid crystallizes little by little.
Recrystallization
The crystallization process is repeated in a solution that had already undergone this
process. The waters that remain still contain dissolved solute that can crystallize. For a
faster crystallization process, apply a crystallization nucleus.
EXPERIMENTAL DEVELOPMENT
Materials
- Baguette
- Beakers
- Spatula
- Funnel
- Test tube
- Balance
- Moon object holder
- Benzoic Acid
Recrystallization process
 Having everything ready and clean, we proceed to weigh the substance, which in
our case was benzoic acid. Of which 0.5g will be weighed.
 This substance is placed in a 25 or 50ml beaker where 15 ml of water is added and

we proceed to dissolve it in a bath that is at a temperature of 60 to 80°C, stirring at
all times with the help of a baguette. for an interval of 15 minutes.
 Once dissolved, it is quickly filtered while hot, which we do very carefully so as not
to lose sample and this is where the short stem funnel, filter paper and a beaker
are used where the already filtered substance will be deposited.
 Now the glass containing the substance is placed in an ice water bath for 15
minutes.
 After the previous step, once the crystals have been obtained, we filter again with the help
of filter paper. At the end, the glass containing the crystals is rinsed with 5ml of water so
as not to lose substance.
 Now we proceed to dry the crystals obtained in an oven at a temperature below 80°C for
an interval of 20 to 30 minutes.
 During this time interval, the waste can be filtered again, but due to time constraints we
were unable to do so.
CONCLUSIONS
- Through recrystallization we were able to obtain a purer substance of oxalic acid.
- We also came to the conclusion that if we want a pure substance we can do the
recrystallization process with all the steps followed in the laboratory.
RECOMMENDATIONS
- You must have pure substances that have zero impurities in their entirety.
- Be very cautious when heating these substances as harmful toxic odors may
emanate.
- Try not to lose part of the sample when filtering.
APPENDIX
1.- What is the dissolution temperature of the compound under study in the solvent
used?
The dissolution temperature was 55° C.
2.- Can any solvent be used in the recrystallization process?
No, the solvent and solute must be polar or nonpolar. Benzoic acid dissolves in water
since both are polar. On the other hand, the two (solvent and solute) should not react and
finally we must ensure that it is volatile enough to be able to eliminate it from the crystals.
3.- What waste is eliminated in the practice carried out?
The extracted waste is concentrated in activated carbon, since activated carbon plays the
role of extracting waste and impurities from substances in the recrystallization process.
4.- Can a solid that is soluble in a certain cold solvent be recrystallized in said
solvent? Because?
Yes, it can be recrystallized because both substances have the same affinity. In the case
of what was done in the laboratory, both substances are polar. But for example, benzoic
acid cannot dissolve in benzene since it is nonpolar.
BIBLIOGRAPHY
* http://quimica.laguia2000.com/general/ cristalizacion#ixzz4AZD8o6OV
* https://es.m.wikipedia.org/wiki/Cristalizaci%C3%B3n
* http://metodosdeseparaciondemezclas.bligoo.com.mx/ cristalizacion
* http://ocw.unizar.es/ocw/ciencias-experimentales/tecnicas-basicas-de-laboratorio-
quimico/teoria/Re cristalizacion_teoria.pdf
* http://www.quimicaorganica.net/recritalizacion.html
* http://www.bodycote.com/es-ES/services/heat-treatment/annealing-normalising/
recrystallisation.aspx

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NATIONAL UNIVERSITY OF CALLAO 2016

Faculty of Environmental Engineering and Natural Resources

Course: Organic Chemistry.

Schedule: 90-G (MONDAY)

Teacher: Álvarez López, Santos Pio.

Date of realization: 30/05/16

Date of delivery: 06/06/16

* Laura Oré, Erick Smith. 1519510052

* Dissolve the substance in the solvent at boiling temperature.

 Know and recognize recrystallization to separate impurities in liquids.

 Identify the characteristics and factors involved in the recrystallization process.

 Learn to choose the right solvents for good recrystallization.

 Acquire skill and knowledge about the recrystallization technique.

Separation method of homogeneous material systems

- Moon object holder

 This substance is placed in a 25 or 50ml beaker where 15 ml of water is added and

- Try not to lose part of the sample when filtering.

The dissolution temperature was 55° C.

2.- Can any solvent be used in the recrystallization process?

3.- What waste is eliminated in the practice carried out?

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