UNIVERSITY

BASIC OPERATIONS TECHNOLOGY

FROM PERU

PRACTICE Nº2
BASIC OPERATIONS

I. GOALS
• Carry out a study and recognition of some basic operations techniques, frequently used in
laboratory work.
• Carry out the separation of a homogeneous or heterogeneous mixture.

II. THEORETICAL PRINCIPLES

In nature and in preparations made in the laboratory, mixtures of substances are found or obtained.
Therefore, the main basic laboratory operations are defined.

1. Precipitation:
It is a rapid process of obtaining a Precipitate from a solution. It can be carried
out by a chemical reaction, by evaporation of the solvent, by sudden cooling of a
hot solution, etc.

2. Decantation:
It consists of leaving a solution containing a precipitate at rest, so that all of it settles
at the bottom of the container under the influence of the force of gravity and the
supernatant liquid can be separated, leaving the precipitate at the bottom of the
container.

3. Filtration:
It is the simplest method to separate the components of a mixture and consists of
passing the solid-liquid mixture through a porous medium (filter paper) that retains
the solid particles and allows the liquid to pass through.

4. Centrifugation:
It consists of rotating the centrifuge using a motor. The test tube with the sample
is placed in the centrifuge; It is turned on and the tubes are rotated, which gives
the mixture a force greater than that of gravity where the solids are pushed to
the bottom, forming two phases (solid-liquid).

5. Spray:
This operation serves to reduce the size of some relatively large solid bodies. The
substances that are to be subjected to reaction must be pulverized, thus making
them better available to the action of the reagents. At the laboratory level, 1
mortars are used.

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6. Evaporation:
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It consists of passing a substance from a liquid state to a vapor state; it can be done
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at room temperature or at higher temperatures. It is generally used for the purpose

of concentrating a solution.

7. Sublimation:
Some solid organic compounds that are capable of directly passing into the vapor
state and then condensing to acquire the solid state again without transforming
into the liquid state, is very convenient for the separation and purification of
volatile solids such as iodine, ac. Benzoic, naphthalene.

8. Crystallization:
A compound that is solid at room temperature, is commonly isolated and purified
by crystallization, consists of the preparation of a saturated solution at a higher
temperature, when the solution cools the substance separates in crystalline form,
then the crystallized solute is separated from the mother solution.

9. Drying and calcination:

These are operations that consist of eliminating the moisture content of the precipitates obtained
by filtering a mixture, through the action of a heat source, such as ovens, stoves, muffles, etc.
• Drying: When the T (ºC) < 250ºC and is carried out in electric stoves.
• Calcination: When T (ºC) is between (250-1200ºC) and is carried out in
electric muffles.

10. Heavy:
It is an operation that consists of determining the exact value of the mass of a
substance, for which balances of different models and types are used.

11. Distillation:
Through this operation, a substance goes from the liquid state to the vapor state
(which is evaporation and occurs due to heating) and subsequently condenses
(produced by refrigeration). It is based on the difference in the boiling point of the substances to be
separated. The two most used types of distillation:
• Simple Distillation
• Fractional distillation.

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BASIC OPERATIONS TECHNOLOGY
FROM PERU

III. EXPERIMENTAL PROCEDURE

a) Materials:

- Glass of ppdo. 50ml

- Glass of ppdo. 150 ml (Heavy)
- Porcelain capsule
- Crucible tong
- Test tube
- Funnel
- Glass rod (Baguette)
- Universal support
- Filter paper (Heavy)
- Piceta

b) Reagents:

- Sodium Chloride (1 g.)

- Fine sand (2.5 g.)
- Distilled water

c) Equipment

- Electric iron
- Analytical or analytical precision balance
- electric stove

d) Procedure :

1. Separation of a compound by:

Precipitation, Decantation, Filtration, Washing and Drying

a) Add the NaCl and Sand to the 50 ml beaker and measure 15 ml of distilled water in a test tube,
add them to the 50 ml beaker and shake with the baguette until completely dissolved. Heat the
glass on the electric griddle, stirring periodically with the baguette. I watched. Let the solid that
does not dissolve settle.

b) Once the mixture has settled and cooled, it will be separated.

using two classic laboratory techniques.

b.1) First, DECANT, directing the solution with the help of the baguette onto
the funnel with previously prepared filter paper and tilting the glass. The
transferred liquid is collected in a 150ml ppdo glass (heavy).

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b.2) Secondly, the FILTRATION will be carried out. Once all the rest of the liquid has passed
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through the funnel (which was not separated with decantation, since thisDEL
process
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helps us
separate the largest amount but not all), all the solid is passed with the help of the
baguette (SAND ) to the funnel. The last particles of sand must be removed with a few
milliliters of distilled water.

OBSERVATION: Observe the sand that is in the funnel, it may still have some traces of
Sodium Chloride, wash the sand with a beaker, pour approximately 2 to 3 ml over the sand.
of water 5 or 6 times. This process is called PRECIPITATE WASHING.

After all these operations you will have separated on one hand a solution in the 150 ml
beaker (weighed) and the solid in the filter paper. Given which we will proceed to work
with both.

c) The liquid contained in the glass is placed on the electric stove, heating until a good amount of
liquid volume is reduced. Once there are a few milliliters left, lower the temperature and heat
gently until total dryness is achieved. This process is called EVAPORATION.
Observe and Interpret.

CAUTION : Care must be taken to ensure that it does not boil violently as it will produce
projections of DROPS that would have dissolved chloride, causing losses of the solid.

d) The sand is wet and as a necessary step it is DRYED. Transfer the paper with the sand to the
appropriate porcelain capsule and heat it on the electric stove with the help of the tongs,
leaving it for a few minutes until almost dry. Remove the porcelain capsule with tweezers and
place it on the table to allow gradual cooling.

When the solvent is water, drying is generally done at 120 ºC since water boils at 100 ºC and
thus its evaporation is certain.

We have separated the two substances that were originally in the form of a mixture.

e) Finally, weigh the glass where the liquid was dried and also weigh the filter paper with the dry
and cold sample.

Record the results in the following table.

Waste disposal:

• Do not pour sand or sodium chloride down drains. 4

• Sand can clog pipes with the difficulties that this would entail.
• Sodium chloride can be recovered.
IV. RESULTS:

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BASIC OPERATIONS TECHNOLOGY
FROM PERU

Final Mass (g)

Initial Mass (g)
Sand NaCl Filter paper Ppdo glass. Sand NaCl

% sand mass error

NaCl mass % error

OBSERVATIONS

V. QUESTIONNAIRE

1. What materials are used to filter a substance?

2. What state changes occur in the following operations: Recrystallization, simple distillation and
drying. Point out each one of them and describe it. ?

3. Establish the fundamental differences between the following separation methods:

a. Evaporation and drying
b. Decantation and crystallization
c. Precipitation and decantation

4. How would you proceed to separate the components of the following samples (mixtures): salt and
dirty water, oil plus water and more salt, gold and sand, and gasoline with kerosene?

5. If a test sample weighs 20 g and crystallizes, obtaining 14.5 g of pure substance. What is the
percentage purity of the test sample? If theoretically 17 g of pure substance should be obtained,
what absolute and relative error have you made?

6. What is the importance of the study of different separation methods? Cite some examples, apart
from those studied.
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