ACTIVITY NO.

COMMON LABORATORY TECHNIQUES AND APPARATUS

I. COMMON LABORATORY TECHNIQUES

The Common Laboratory Techniques describe procedures for safety conducting

an experiment. Be sure to read each technique carefully before the laboratory session
for completing a safe and successful experiment.

A. Handling Liquid Chemicals

1. Opening a Reagent Bottle.

Grasp the reagent bottle with one hand and using the other hand, hold the
glass stopper between fingers and lift (Fig.A.1a). Never lay the stopper from a
reagent bottle on the laboratory bench. Impurities may be picked up and thus
contaminate the solution when the stopper is returned to the reagent bottle. Flat
top glass stopper should be laid upside down on the laboratory bench.

Fig.A.1. Removing a glass stopper from a reagent bottle.

2. Transferring Liquids to Another Container.
To transfer a liquid from one container to another, hold a stirring rod
against the lip of the container holding the liquid and pour it down the rod which
should touch the inside wall of the receiving vessel (Fig.A.2). Try not to transfer
 more reagent than is needed, and do not return unused chemicals to the reagent
bottle.

Fig.A.2. Transferring a liquid from a reagent bottle.

3. Reading the Volume of a Liquid
For exacting the measurements of liquids in graduated cylinders, pipettes,
burettes, and volumetric flask, the solution’s volume is read at the bottom of the
meniscus. Read with the eye horizontal to the liquid’s surface (Fig.A.3). A clear
or transparent liquid is read more easily by positioning the top edge of a black
mark (made on a white card) just below the level portion of the liquid. The black
background reflects off the bottom of the lower meniscus and better defines the
liquid’s level. Substituting a finger for the black mark on the white card will work,
but it is not as effective.
 Fig. A.3. Reading the volume of the liquid.

4. Testing for the Odor and Taste of Chemicals

Chemicals should not be tasted nor tested for odor unless specially
directed to do so. Working with toxic vapors must be done in a ventilating hood.
To test the odor of a substance, waft a bit of vapor towards the nose as shown in
Fig A.4. Do not inhale the vapor directly from the test tube. Never hold your face
directly over vapors!

Fig.A.4. Testing for odors.

5. Heating Liquids
a. Test tube. The test tube should be no more than one-third full. Move the
test tube circularly in and out of the flame, heating the liquid from the top
to bottom. Never fix the flame’s position at the base of the test tube. Never
 point the test tube to anyone as sudden ebullition (a sudden violent
outburst of the liquid) may take place. See Fig. A.5a

Fig. A.5a. Heating; liquid in a test tube.

Warning:

Remember not to point the hot or heated test tube toward yourself
or anyone else.

b. Erlenmeyer Flask. An Erlenmeyer flask less than one-fourth full may be

heated directly over a flame. Hold it with a piece of tightly folded paper or
flask tongs laboratory bench; allow to cool by setting the flask on a wire
gauze. See Fig. A.5b.

Fig. A.5b. Heating liquid in an Erlenmeyer Flask.

c. Beaker (or flask). Support the beaker (or flask) on wire gauze. To avoid
bumping (sudden formation of superheated liquid near the flame) place a
glass stirring rod (or use boiling chops) in the beaker. Position the flame
 directly under the tip of the stirring rod (Fig.A.5c). Place a second
supporting ring around the top of the beaker (or flask) to prevent it from
being accidentally knocked off.
d. In hot water Bath. This is used to heat a small quantity of solution in a test
tube that needs to be held at a constant temperature over period of time
(Fig. A.5d). if the solution is to be heated in a beaker or Erlenmeyer flask,
use a larger as water bath filled to about ¼ -full, and heat to the desired
temperature.

Fig. A.5c.Heating liquid in a Fig. A.5d. Heating liquid in a

Beaker. Hot water bath.

6. Evaporation of liquids
a. Nonflammable liquids may be evaporated in an evaporating dish with a
gentle, direct flame (Fig. A.6.a) or over a steam bath (Fig. A.6.b), which is
more efficient rather than rapid boiling. Avoid inhaling the vapors.
b. Flammable liquids may be similarity evaporated substituting a heating
mantle for the Bunsen flame. The use of fume hood or an improvised hood is
suggested if large amounts are evaporated in a laboratory with inadequate
ventilation; consult with your laboratory instructor.
 Fig.A.6.a. Evaporation of nonflammable Fig.A.6.b. Evaporation of non-
liquid over a low, direct flame. flammable liquid over a steam bath.

B. Handling Solid Chemicals

Transferring a Solid Reagent
First, read the label on the bottle twice to be sure of using the correct
reagent. If the bottle has a glass stopper, place it with the topside down on the
bench (Fig. B.1). If it has a screw cap, remove and set it on the bench, inner
inside facing up.

Hold the bottle with the label against your hand, tilt, and roll rock and
forth. Try not to dispense more reagent than needed. Do not insert a spatula or
other object into the bottle unless your O specifically tells you to. If too much
reagent is taken, do not return excess to the bottle but rather share it with
other students. Recap when finished.

Fig. B.1. Transferring solid reagent.

C. Handling Precipitates

Decantation. A liquid can be decanted (poured off the top) from a solid if the solid
clearly separates from the liquid in a reasonably short period of time. Allow the solid to
settle to the bottom of the beaker or test tube. If beaker is used, it may be tilted to allow
the solid to settle at the side below the spout of beaker then transfer the liquid (called
the (supernatant or decantate) with the aid of a clean stirring rod to a receiving vessel
(Fig. C.1). Do this slowly so as not to disturb the solid.

Fig. C.1. Decantation

Centrifugation. A centrifuge (Fig. C.2a) spins at velocities of 5,000 to 25,000 revolutions

per minute. A liquid-solid mixture in a small test tube or centrifuge tube is placed into the
sleeve of the rotor of the centrifuge. By centrifugal force, the solid is forced to the
bottom of the test tube or centrifuge tube and compacted. The clear liquid, called the
supernatant, is then easily decanted without any loss of the solid. The following
precautions are observed in operating a centrifuge:

a) Never fill the centrifuge tubes to a height more than 1 cm from the top.

b) Label the centrifuge tubes avoid confusion.

c) Always operate the centrifuge with even number of centrifuge tubes containing
equal volumes of liquid placed opposite one another in the centrifuge. This
balances the centrifuge and eliminates excessive vibration and wear. If only
 one tube needs to be centrifuged, then balance the centrifuge with a tube
containing the same volume of solvent (Fig. C.2b).

d) Never attempt to manually stop centrifuge, let the rotor come to rest on its
own.

Fig. C.2a. Centrifuge Fig. C.2b. Centrifugation

Gravity Filtration. Gravity filtration has the advantage that it is simple and economical. It
is most effective when the amount of solid is to be isolated is small. If a large amount of
solid or a gelatinous solid is to be isolated, this method is not used because the filter
paper may become clogged. In this case, vacuum filtration is most suitable.

1. General Procedures for Filtration

a. Allow the precipitate to settle to the bottom of the container.

b. Wet the filter paper with a small amount of water or a liquid in which the
precipitate is insoluble.

c. Decant (pour off) the bulk of the solution into the funnel using a stirring rod. This
step ensures the filtration will not be slowed by the precipitate clogging the filter
paper prematurely since most of the solution will have already filtered through.

d. Mix the precipitate with the remaining solution and dump the resulting precipitate
slurry into the funnel. Simultaneously, spray a stream of solution from a wash bottle
to rinse out any slurry adhering to the walls of the container. (See Fig C.1.)
 Remember: the liquid or solution used for washing the precipitate must be one in
which the precipitate is insoluble.

Fig. C.1. Transferring a precipitate

 Wet a rubber policeman or glass rod with wash liquid and use it to help
transfer any precipitate still clinging to the container walls.
 Use was bottle to rinse out whatever precipitate remains.
 Typically 5- to 10 mL of a wash solution are drawn through the funnel to
wash the precipitate. This may be repeated several times to ensure that only
pure precipitate remains.
 Allow air to be drawn through the filter paper several minutes to dry the
precipitate partially.

e. Usually precipitates are washed or rinsed to remove impurities, unless the filtrate is
the desired component.

f. Lift a corner of the filter paper with a spatula and then use the corner to pry up the
rest of the kilter paper. Carefully transfer the filter paper and precipitate to a
previously weighed watch glass. Allow the precipitate to air dry, or oven dry (if
melting point is above 70⁰C).

2. Folding a Filter Paper

 Fold the filter paper in half (Fig. C.2). then refold to within about 10 ⁰ of a 90 ⁰ fold,
tear off the corner unequally, and open. The tear enables a close seal to be made across
the paper’s folded portion when placed in a funnel.

Fig. C.2 technique in folding a filter paper

D. Inserting a Glass Tubing into a Stopper

To insert glass tubing (including thermometers, long-stemmed funnels, thistle tubes,

etc.) through a rubber stopper, first lubricate the tube and stopper with water or
glycerol. Hold the tubing with a cloth near the end to be inserted, and push with a
twisting motion. (If you twist a long-stemmed funnel or thistle tube by the large end, it
is easily broken.)

Fig. D Inserting a glass tube into a stopper.

E. Operating the Bunsen burner

 The Bunsen burner, used for most laboratory heating, produces a cone-shaped
flame, as illustrated in Figure E. Ordinary beakers, crucibles, and other objects to be
heated are placed just above the hottest portion of the flame. This allows most heat
to spread about them. Do not place in the cold inner cone of the flame, which
consists of unburned gas. For maximum temperature, have the gas full pressure, and
with the air vents open, adjust the needle valve or the air to produce short blue flame
of many short cones that are about 0.5 cm high. The object to be heated is placed
about 1 cm above the grid.

Fig. E Operating the Bunsen burner

II. A. COMMON LABORATORY APPARATUSES

This section details common laboratory apparatus and their appropriate use.
Knowing the proper use will help ensure safe laboratory practices.
 B. USES OF COMMON LABORATORY APPARATUSES

1. Balance – for measuring mass

2. Beaker – to hold, mix, and heat liquids
3. Bunsen burner – as heat source in the absence of flammable materials
4. Buret – for dispensing accurate volume of a liquid
5. Clay triangle – to support a crucible during heating
6. Crucible – for holding chemicals during heating to very high temperatures
7. Crucible tongs – to hold crucibles
8. Erlenmeyer flask – to hold mix chemicals. The small neck is to facilitate mixing
without spilling
9. Evaporating dish – to heat liquids for evaporation
10. Funnel – for Filtration; also to transfer liquids or fine-grained materials into
containers with small openings.
11. Graduated Cylinder – to measure a precise volume of a liquid
12. Mortar and pestle – to crush and grind materials
13. Ring clamp – used with a ring stand to hold glassware, such as beaker or funnel
14. Ring stand – to support laboratory glassware, water bath, etc.
15. Spatula – to transfer solids
16. Stirring rod – for stirring and mixing
17. Test tube – to hold and mix liquids
18. Test tube holder – to hold test tube during heating
19. Test tube rack – to hold several tubes at one time
20. Thermometer – to measure temperature
21. Utility/ iron clamp – to secure glassware to a ring stand
22. Volumetric flask – to prepare solutions of accurate volume
23. Volumetric pipet – to measure small amounts of liquid very accurately; draw in or
suck the liquid using an aspirator (never use your mouth)
24. Wash bottle – to rinse parts of glasswares and to add small quantities of water
25. Watch glass – to hold solids while weighing or to cover a beaker
26. Wire gauze – to support a container, such as beaker, on a ring stand during
heating