Exercise No.

1:
Introduction: The Chemical
Laboratory
Introduction

Safety is the state of being “safe” form French word sauf, the condition of being
protected from harm or other non-desirable outcomes. Safety precautions are
the most important instructions that you will receive in this course. Failure to
observe them may cause serious injury to the intention of leading you to believe
the laboratory is a dangerous place; it is only when those working in
laboratories become careless that accidents happen. If the following
precautions are observed, the laboratory will be a safer place for you than the
street you cross on your way to class.
The following safety precautions are implemented in the laboratory to avoid
any accident happened.
1. Goggles or other protective eye equipment approved by OSHA (Occupational
Safety and Health Administration) must be worn at all times when in the
laboratory unless otherwise specified by the instructor. Contact lenses or
regular glasses cannot be substituted for approved eye protective
equipment.
2. Shoes or similar adequate foot covering must be worn while in the
laboratory. Avoid wearing easily combustible or especially loose fitting
clothing. Long hair may catch fire if passed near a laboratory burner, and
hair nets or a change in hair style should be used to minimize the danger
presented by very long hair.
3. Protective laboratory aprons or coats are generally required. Note the
location of fire extinguishers and other protective equipment such as eye-
washing fountains, showers, and fire blankets.
a) In the case of minor fire, wet paper towels are efficient for smothering the
fire. Use other measures as appropriate and inform the instructor any time
that you have a fire.
b) If your clothing catches fire, the fire should be smothered with a blanket or
a heavy coat or you should immediately use laboratory showers. If you are
some distance from a shower, it is better to roll to the floor to prevent
 2 ESci 115b: Chemistry for Engineers

flames from reaching your head. Rolling over and over may also help
extinguish flames if a blanket or showers are not immediately available.
c) If chemicals of any kind get in your eyes, wash with water for several
minutes, preferably at an eyewash fountain. Always report such incidents
to the instructor.
d) If chemicals are spilled on your hands or any other part of your body, wash
at once with water. Inform your instructor whenever such chemicals
produce an irritation.
e) If chemicals are spilled on your clothing, advise your instructor at once. It
may be possible to use sodium hydrogen carbonate or other substance to
prevent damage to your clothing.
f) If you are burned or injured in any way, be certain to inform the instructor.
You may be directed to consult a student health service or your own
physician in some instances.
4. Do not taste anything in the laboratory. Do not eat or drink anything in the
laboratory.
5. Always read instructions carefully. If you are in doubt, ask your instructor. Be
especially careful in the following instances.
a) When heating any material in a glass container be certain that it is
borosilicate glass (e.g. Pyrex or Kimax).
b) When heating materials in a test tube, point the open end of the tube away
from yourself and others. Tilt the test tube and heat near the top of the
liquid first. Never heat the bottom of a test tube that contains liquids.
c) Be especially careful when inserting glass tubes or thermometers through
rubber or cork stoppers. Lubricate the tube with water, glycerine, or other
lubricant, grasp the item to be inserted securely near the stopper, and
protect your hands with a towel to avoid cutting your hands.
NEVER TRY TO FORCE GLASS TUBING OR THERMOMETERS THROUGH
STOPPERS.
d) Do not use mouth suction in filling pipets; use a pipet bulb for this purpose.
Ask your instructor to demonstrate the correct technique if you are
uncertain.
e) Exercise great care in noting the odor of gases or liquids. Use a fume food
whenever noxious fumes are being produced.
6. Do not work in the laboratory alone. In classes with experienced students,
your instructor may permit a group of students to work unsupervised, but
you should never work alone. In general, no persons other than class
members are allowed in a chemistry laboratory without explicit permission
of an instructor.

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7. Never perform unauthorized experiments.

8. Keep tabletops clean; what looks like a drop of water may be a strong acid or
base solution that could damage clothing or books, or injure students.
9. If you find it necessary to obtain liquid chemicals from a stockroom, a plastic
bucket should be used to carry such containers of liquids between the
stockroom and the laboratory.
10. Unless specifically directed to do so, never return chemicals to reagent
bottles or other containers. If you have an excess of a reagent, discard it.
11. Many of the reagents used in organic chemistry are flammable. Care should
be taken with such substances, particularly if they are liquid. Do not bring
such liquids near flames. Do not pour flammable liquids down a sink since
they tend to accumulate can be ignited in the pipes and cause an explosion.
Special instructions will be given in specific experiments for disposal of
organic liquids.
Common laboratory operations are used daily by chemist. Because of their
daily use, chemists have to become masters in using in the various laboratory
operations. Some laboratories require various laboratory equipments, such as
glassware or electrical devices; while others require little to no equipment. See
Figure 2, for some of the laboratory apparatus and equipment. Some common
laboratory operations include volume measurement, weighing, heating,
evaporation, precipitation, decantation, filtration and centrifugation.
A. Volume Measurement
Volume is the amount of space taken by an object, while capacity is the
measure of an object’s ability to hold a substance. Medicine droppers, beakers
and Erlenmeyer flasks that have volume readings on them indicate approximate
volume only, whereas precision equipment such as volumetric flasks, pipets,
and burets and even graduated cylinder give more accurate readings. The
measuring glassware selected depends on the degree of accuracy needed for a
particular determination. The lab glassware comes in variety of sizes; the
capacity of each at a given temperature is stamped on by the manufacturer,
together with the etched lines for precise measure.
The correct way to read the volume of a liquid is to hold or position the
glassware in a vertical position at eye level and look at the meniscus of the
liquid. The meniscus is curved, with rather flat part in the center (Figure 1). By
noting the position of this flat part relative to the calibration marks on the
glassware, you can determine the volume of a liquid. It is important to keep the
glassware clean because dirt may chemically contaminate an experiment and
the presence of dirt in the glassware may throw off accurate determination of
volume. (Glassware that is dirty does not drain properly, so that the delivered
volume is not equal to that indicated by the calibration marks).

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 4 ESci 115b: Chemistry for Engineers

Burets are constructed so that it is possible to measure volume more precisely

than a graduated cylinder. It is necessary for the meniscus to be at zero mark,
since the volume delivered from a buret can be obtained simply by taking the
difference between the initial and final readings. Make sure that no drop is left
hanging from the buret tip either before or after delivering liquid. After
delivering a volume, always touch the tip to the wall of the receiver.
Sometimes it is necessary to obtain several equal samples of an accurately
determined volume of liquid. This can be means of a pipet. A volumetric pipet
consists of an elongated glass tube having a delivery tip at the lower end and
an opening for suction at the upper end. The proper way to use a pipet is to
draw liquid up past the ring mark using a rubber bulb aspirator, detach the bulb,
and quickly place the a fingertip over the suction to hold the suction and then,
by slightly rolling the fingertip aside, allow excess liquid to drain out of the
delivery tip until the meniscus descends to the ring mark. The tip of the pipet is
then transferred to a receiving vessel, and the liquid is allowed to drain out,
Usually 10 seconds are counted off to permit the walls to drain properly, and
then the tip is touched to the receiver wall to get off the last drop. The pipet
should be held constantly in vertical position when pouring liquids directly from
bottles (or any vessel), a stirring rod is held against the mouth of the vessel so
as to permit liquid to flow down along without splashing into the receiver (see
Figure 5).
B. Weight Measurement
One of the most common operations in experimental chemistry is the
determination of mass or weight. Types of balance found in the laboratory are
platform balance, single-pan balance, top-loading balance and analytical
balance. The following are the rules in weighing substances.
1. Before you make any weighing, familiarize yourself with the type of balance
you will use.
2. If there is apparent difficulty in operating the balance consult your
instructor, do not make any adjustments.
3. Do not remove the balance from its location.
4. Do not interchange balance pans; the pan is calibrated for its particular
balance.
5. Never weigh chemicals directly on the balance pan; on the balance pan;
use a watch glass or weighing paper. Clean up any spills.
6. Weigh volatile or corrosive samples in stoppered containers.
7. Do not weigh objects that are not at room temperature.
8. Arrest the balance beam before removing the weighed object from the pan.
The container is weighed (tare weight), the sample is added and both are
weighed together (gross weight). The weight of the sample (net weight) is
obtained from the difference in the two weighings. See table 2.2 for the rules in
weighing substances.

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C. Heating of Liquids
1. In a test tube (see figure 6)
a) Hold the test tube with a test tube holder in a slanting position.
b) Point the mouth of the test tube away from you or anyone working
near you.
c) Move the test tube gently from side to side so that the heat will be
evenly distributed.
d) Avoid heating the glass above the liquid for the cooler liquid may
crack the hot glass when they meet.
e) Do not heat the test tube directly on the bottom as this may cause
the contents to spurt out.
2. In a beaker (see figure 7)
a) The beaker should be supported about 5-7 cm above the burner by an
iron ring on an iron stand or with a tripod.
b) A wire gauze is placed between the beaker and the iron ring (or
tripod) to prevent unequal heating.

D. Precipitation
When substances in a solution interact to form a solid that is soluble or only
very slightly soluble in the solvent, precipitation occurs. Separation of the solid
from the liquid can be carried out by decantation, filtration or centrifugation.

E. Decantation
Adequate separation of a solid and a liquid can be achieved by decantation,
especially if the solid is dense. Allow the mixture to stand until the solid or
precipitate has settled, then carefully pour off the liquid down a stirring rod,
leaving the solid behind. The liquid above the precipitate is called the
supernatant liquid. This means of separation seldom affords a convenient
method for a clean separation especially when the precipitate does not settle
easily. (See Figure 3).

F. Gravity Filtration
Filtration is a process of separating a solid-liquid mixture by passing through a
barrier with fine pores, such as the filter paper. The clear liquid passing through
the filter paper is called the filtrate. The precipitate remains on the filter paper.
(See Figure 4).

G. Centrifugation

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 6 ESci 115b: Chemistry for Engineers

Rapid separation of solids and liquids can be done in a centrifuge.

Centrifugation is a technique which involves the application of centrifugal force
to separate particles from a solution according to their size, shape, density,
viscosity of the medium and rotor speed. More-dense components of the
mixture migrate away from the axis of the centrifuge (move to the outside),
while less-dense components of the mixture migrate towards the axis, move to
the center.
During operation make sure that the tubes are free from cracks and tightly
sealed. The rotor is properly balanced for effective separation. Allow to come to
complete stop before opening.

G. Evaporation
Molecules with kinetic energies suffiently above average may overcome the
attractive forces of neighboring molecules and escape from a liquid surface
into the gaseous or vapour state. This phenomenon is termed evaporation or
vaporization. The material that remains after evaporation is called residue.
Evaporation is usually carried out in an evaporating dish placed over a burner,
hot plate, or steam/water.

Learning Outcomes

1. To become aware with some of the safety precautions inside the

laboratory.
2. To become familiar with some of the common laboratory operations.

Figure 1 Meniscus

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Figure 2 Common Laboratory Apparatus and Equipment

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 8 ESci 115b: Chemistry for Engineers

Figure 3 Decantation Figure 4 Filtration

DECANTATION FILTRATION

Figure 5 Pipetting

PIPETTING

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Figure 6 Heating of Beaker Figure 7 Heating of Test Tube

Test tube
Test tube
holder

Bunsen
burner

HEATING OF BEAKER HEATING OF TEST TUBE

Materials

 20.0 mL grad. Cylinder 3M NaOH 3M FeCl3

 10.0 mL pipet Filter paper Evaporating dish
 Tripod aspirator Clay triangle
 50 mL beaker funnel Platform balance
 Stirring rod Hot plate Watch glass
 Crucible tong Wash bottle Medicine dropper

Procedure

A. Measuring Volume
a) Measure 200 ml water using a graduated cylinder and show it to your
instructor
b) Measure 7.50 ml of water using a pipet and show it to your instructor

B. Measuring Weight
Weigh out 10.0 g of sand and show it to your instructor

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 10 ESci 115b: Chemistry for Engineers

C. Precipitation
Measure 1.0 ml of 3 M ferric chloride (FeCl) and place it in a 50-ml beaker
Measure 90 mL of 3 M sodium hydroxide (NaOH) and mix this with the FeCl,
in the beaker. Observe the formation of a precipitate. Allow the precipitate to
settle and add NaOH drop by drop until no more precipitate forms Divide the
solution into two equal parts. Save this for parts E and F.

D. Decantation
Weigh an evaporating dish and record the weight. Decant the supernatant
liquid (from part C) into the evaporating dish (save this for part F) taking care
that no precipitate goes with the liquid Add 2.0 ml distilled water to the
precipitate left in the beaker. Save this for part F.

E. Filtration
Secure a piece of filter paper. Fold it in half along one diameter and then
quarters. Tear off a comer of the folded paper and open it into a shape of a
cone with and thickness on one side and three thickness on the other side,
Weigh the Filter paper and record the weight Insert the paper into the funnel
and moisten it with distilled water. Press the moist paper gently against the
funnel wall until there are no more air bubbles. Support the funnel on a
funnel rack then place the receiver (evaporating dish from part D) under the
funnel with the tip touching the wall of the receiver. Pour the mixture in the
beaker from part C) carefully down a stirring rod. Do not let the level of the
liquid in the funnel go above the top of the paper. Wash the solid that
remains in the beaker with a minimum amount of distilled water from a
wash bottle. Save the filtrate for part F Remove the filter paper, open it on a
watch glass, let dry and weigh.

F. Evaporation
The supernatant liquid from part D and the filtrate from part E both contain
dissolved sodium chloride which may be recovered by evaporating the water
from the solution. Place the evaporating dish on a hot plate (or burner).
When all of the water has evaporated, remove the evaporating dish, let cool
to room temperature and weigh.

Guide questions and instructions on how to prepare

and submit the laboratory

1. What are the following safety precautions in handling organic

chemicals?
2. State the proper way of heating liquids using test tube.
3. Which is a more accurate volume-measuring instrument, a graduated
pipet or a graduated cylinder?
4. Which is more efficient method of separating solids from liquids by
filtration or by decantation? Why?

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5. Write the balanced chemical equation involved in:

a) Precipitation __________________________________________
b) Evaporation ___________________________________________
6. What is the chemical composition of the
a) Filtrate ____________________________________
b) Residue ___________________________________
7. If the size of the precipitate is smaller than pores of the filter paper, the
paper cannot retain the precipitate. Give two separation methods that
may overcome this difficulty.

This guide questions will serve as your quiz and to be submitted along with
your lab report. The laboratory report sheets provided will be submitted by
the student after every exercise through email or courier.
See abridged for the schedule of submission.

Additional Resources

https://study.com/academy/lesson/what-is-a-meniscus-definition-uses-lab-examples.html (Date
Accessed: September 9, 2020

References

G. Calvez, A. Ramal, and F. Salas. ESci 115b: Chemistry for Engineers Laboratory Manual

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