Laboratory Techniques and Processes

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ACTIVITY 3 - LABORATORY TECHNIQUES AND PROCESSES

Correct laboratory techniques must be practiced and through this, laboratory “habits” are
acquired.

Effective and efficient techniques depend on one’s skill and know-how of the laboratory
processes.

HANDLING SOLIDS

Solids should be shaken or loosened so that they can easily be scooped or poured from
their containers. A convenient way to withdraw the right amount of solid is to tap or rotate
the container gently while pouring ( Figure 3.1). Often, a scoop or spatula is used for
withdrawing small amounts of solids from the reagent bottle. Use only clean spatulas.

Figure 3.1 Figure 3.2 Figure 3.3

Some bottles have flat caps that can be placed upside down on the desk, thus
preventing contamination.

Always allow hot objects to cool before placing them on the balance pan if they
are to be weighed. Heat makes air currents rise, and this causes errors in the
weighing.

HANDLING LIQUIDS

When preparing acid solutions, always add acid to water slowly while stirring. Never add water
to acid.

A liquid can be conveniently poured from one vessel to another by directing its flow
with a stirring rod (Fig. 3.4) or by placing the neck of the reagent bottle against the rim of
the receiving vessel (Fig. 3.5).

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Figure 3.4 Figure 3.5

Test tubes containing liquids should be heated along the side and swirled constantly to
avoid sudden eruptions. The test tube being heated should be pointed away from
one’s self or anyone else. (Fig. 3.6)

Figure 3.6

When liquids are heated, bumping (the sudden release of vapor caused by super-
heating) can be avoided by putting solid objects such as boiling chips, bits of broken glass,
or a stirring rod in the container and placing the flame directly below the objects.

For accurate measurement of liquid volumes, pipets and burets are used, while an
approximate measure of liquid volumes is obtained by reading the volume in a graduated
cylinder. With eyes at the liquid level, the volume is read at the bottom of the meniscus (the
curved, darker region at the surface). The volume markings sometimes found on flasks
and beakers are for estimates only.

When using a pipet, the liquid (drawn up with a suction bulb and held to the exact level by
placing a finger over the end) is transferred to the designated container by allowing it to
drain out to the last drop with the tip of the pipet touching the inside. The pipet is not
shaken to get the last drop out.

When only a small amount of liquid is needed for the study, dispensing 1.00 mL or less of
a liquid is best done with droppers. Drop volume depends on the density of the liquid, the

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size of the tip, and the pressure applied on the rubber teat of the dropper. (Liquids of
different densities give different drop volume sizes.)

Proper use and handling of droppers involve always using clean dry droppers, filling
droppers with just enough of the liquid that will be used, using separate droppers for
each kind of liquid, and not turning them upside down to avoid contamination from the
rubber bulb. It is suggested to stand them on the tip in a beaker or a small bottle
when they are not in use.

To wash droppers, fill them with water and dispense by applying pressure on the
rubber bulb. Do this several times until the dropper is clear. Sometimes, there is
a need to detach the rubber bulb and wash them. Droppers may be washed with
detergent or soaked in an acid cleaning solution without the rubber bulb before
rinsing well. Droppers should be dry before keeping them.

DILUTION

Dilution is a process of decreasing the concentration of a solution by mixig it with water. Diluted
liquid reagents are prepared by adding a certain amount of concentrated solution to a specific
volume of water.

The dilution formula is generally expressed as: C1V1 = C2V2

where : C1 is the original concentration of the solution


V1 is the volume of the concentrated solution
C2 is the final concentration of the dilute solution
V2 is the final volume of the solution

PRECIPITATION

Precipitation is a chemical reaction of two liquid substances resulting in the formation of solid
particles. The solid is called the precipitate.

SEPARATION PROCESSES

FILTRATION is the standard method of separating a precipitate from a liquid. It is done by


pouring the mixture in a funnel lined with filter paper. The filter acts as a fine sieve. It permits
the liquid to pass through but the solids are left on it. The liquid that passes through the filter
paper is called the filtrate and the solid retained is the residue.

The filter paper should be fitted in the funnel well, so that air is not drawn between the
paper and funnel, for a rapid filtration. This is done by folding the paper properly ( in
either of two ways - Figure 3.7 or 3.8 ), inserting it in the funnel or moistening with
water and pressing the wet paper gently to make an airtight seal around the top of
the funnel wall (Fig. 3.9). A precipitate on the filter can be washed by pouring water
over it through a glass rod.

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Figure 3.7 Folding a Filter paper (Cone)

Figure 3.8 Folding a Filter paper (Fluted)

The assembled apparatus for filtration is shown in Figure 3.3.

Figure 3.9 Proper Filtering Technique

CENTRIFUGATION is the process by which centrifugal force produced by an electric motor


speeds up the rate of the settling of small particles. The solid that settles is called the residue
and the clear liquid that separates on top of the residue is termed centrifugate.
DECANTATION is the process of carefully pouring off the liquid from a solid-liquid mixture
into a clean receiver without disturbing the solids at the bottom. This is applicable when
the solid readily settles at the bottom of the container. The liquid is called the supernatant
liquid, or more specifically the decantate.

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Figure 4.0 Proper Pouring of the Decantate

EVAPORATION is the process of changing from a liquid or solid state into vapor or a
gas. It is usually done faster by heating.

OBJECTIVES
At the end of the activity, the students should be able to:
1. perform laboratory processes applying the proper laboratory techniques;
2. improve skill in doing laboratory processes; and
3. understand why it is necessary to apply the different laboratory techniques.

MATERIALS AND EQUIPMENT


balance funnel spatula
beaker glass rod test tube holder
Bunsen burner graduated cylinder test tubes
centrifuge hot plate thermometer
crucible tong iron clamp tripod
erlenmeyer flask iron ring vials
evaporating dish iron stand watch glass
filter paper match wire gauze

REAGENTS
1M barium chloride HCH3COO distilled water
1M calcium chloride HCl n-hexane
1M potassium iodide HNO3 sodium chloride solid
1M sodium carbonate NH4OH
1M sodium sulfate

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PROCEDURES

A. DILUTION

1. Calculate the amount of concentrated solution and the amount of water that are
needed to prepare 50 mL of the following dilute solutions:
(a) 3 M NH4OH (b) 3M HCl (c) 3M HNO3 (d) 1M HCH3COO

2. Have the calculations checked by the laboratory instructor.

3. Prepare the solution assigned to your group and submit it to the laboratory
instructor.

B. PRECIPITATION, CENTRIFUGATION AND DECANTATION

1. Measure 2.0 mL of 1M sodium carbonate solution and place it in a clean small test tube.
Add 1.0 mL of 1M calcium chloride solution. Shake and let it stand. Observe what
happens. Record the time it takes for the liquid to become clear.

2. Place the test tube in a centrifuge and switch on the device for one minute. Remove
the test tube from the centrifuge and observe the contents.

3. Separate the liquid from the solid by decantation. Collect the decantate in a test tube
labeled accordingly. Record the observations.

C. FILTRATION
1. Measure 2 mL of 1M barium chloride solution and place it in a clean small test tube. Add
1.0 mL of 0.1M sodium sulfate solution to it. Shake and observe what happens. Record
the time it takes for the liquid to become clear.
2. Fold a filter paper, fit it into a funnel, moisten with water and filter the contents of the
test tube in step # 1. Collect the filtrate in a test tube labeled accordingly. Record the
observations.

D. EVAPORATION

1. Weigh an evaporating dish.

2. Weighed 2.0 g NaCl into the evaporating dish and add 10 mL water. Stir it to dissolve.

3 . Heat the evaporating dish with the salt solution gently until all the liquid disappears
and a solid residue remains.

4. Cool and weigh. Record the data.

5. Calculate the % of the recovered salt.

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Name____________________________________ Rating _____________________
Course/Yr/Sec_____________________________ Teacher ___________________
Group No. ________________________________ Date ______________________

ACTIVITY 3 - LABORATORY TECHNIQUES AND PROCESSES

DATA AND OBSERVATIONS

A. DILUTION

Solutions Concentration of solution Volume of solution


Concentrated (M) Dilute ( M) Concentrated (mL) Dilute (mL)
NH4OH 15 3 50
HCl 12 3 50
HNO3 16 3 50
HCH3COO 17 1 50

B and C. PRECIPITATION, CENTRIFUGATION, DECANTATION AND FILTRATION


.
Observation Time for the
Reagents liquid to become
Before mixing After clear
Mixing-
Sodium
carbonate
Centrifugation-

Calcium
chloride Decantation-

Mixing-
Sodium
sulfate

Filtration-

Barium
chloride

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D. EVAPORATION

Weight of evaporating dish


Weight of evaporating dish + salt (NaCl)
Weight of salt (NaCl)
Weight of evaporating dish + residue
Weight of residue
% recovered salt

% recovered salt = __weight of residue_ (g)____ x 100


weight of dissolved salt (g)

QUESTIONS

A.1. What precaution should be followed in preparing dilute acid solutions? __________
_______________________________________________________________________
______________________________________________________________________

B.1. In what aspect/s are decantation , centrifugation and filtration similar? How do they
compare in effectivity?_ __________________________________________________
_______________________________________________________________________
_______________________________________________________________________
D.1. What was the purpose of evaporating the liquid of the salt solution?
_______________________________________________________________________
_______________________________________________________________________
What substance became the residue? ______________________________________

References: ______________________________________________________
______________________________________________________

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