Chem Lab Manual

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Table of Contents

Laboratory Safety and Laboratory Guidelines

Common and Special Laboratory Equipment

Materials and Other Requirements

Common Laboratory Operations and Techniques

Experiment 1 …………………………………………………………………………..10
Properties of Matter

Experiment 2 …………………………………………………………………………. 12
Chemical Changes

Experiment 3 …………………………………………………………………………. 15
Classification of Matter

Experiment 4 ………………………………………………………………………….17
Chemical Nomenclature: The Language of Chemistry

Experiment 5 ………………………………………………………………………….22
Water of Hydration

Experiment 6 ………………………………………………………………………….25
Gases

Experiment 7 ………………………………………………………………………….27
Oxygen

Experiment 8 ………………………………………………………………………….29
Heat and Volume Effects

Experiment 9 ………………………………………………………………………….31
Flame Test

Experiment 10 ………………………………………………………………………..32
Electromotive Series

Experiment 11 ………………………………………………………………………...33
Oxidation – Reduction Reactions/ Some Aspects of Corrosion

Experiment 12………………………………………………………………………….35
Colligative Properties

1
GENERAL INSTRUCTIONS TO THE STUDENTS
Apparatus

 Check each piece of apparatus, which you find in your locker from the duplicate
list furnished to you by your instructor. Sign your name and submit to your
instructor. The instructor signs the checklists and gives one copy to you for your
safekeeping.
 Provide your locker with reliable padlock. You are responsible for all the
apparatus issued to you. Towards the end of the semester you have to replace or
give a deposit for any piece which you have lost or broken. If you have partners,
each of you will share equally any loss or breakage of apparatus kept in your
lockers and those borrowed from the stockroom. A clearance duly signed by the
laboratory attendant is a requirement for taking the final examination. NO
CLEARANCE, NO FINAL EXAMINATION.
 General apparatus, e.g., Bunsen burner, thermometer, iron stand, clamps, etc.
and special apparatus may be borrowed from the laboratory attendant.
 Borrowing of apparatus from the stockroom should be done during the first
30 minutes of the laboratory period.

Materials and Other Requirements

You have to provide yourself with the following materials and supplies besides the apparatus in the
laboratory locker and the stockroom:

Group Individual
Masking/paper tape Tissue paper Vials with cover (5 pcs) Lab notebook
Pair of scissors Rags Medicine dropper (3-5 pcs) Lab manual
Aspirator Marking pens Rubber tubing (2 ft) Lab gown
Wire gauze Filter paper Newspaper/scratch paper Hand towel
Wash bottle Tray Stirring rod Mask
Liquid detergent Match Corks/rubber stoppers Goggles
Test tube brush Test tube holder Padlock with keys

Laboratory Work

Laboratory work is an integral and essential part of any chemistry course. Chemistry is an
experimental science – the compounds and reactions that are met in the lecture and classroom work
has been discovered by experimental observation.

The purpose of laboratory work is to provide an opportunity to observe the reality of compounds and
reactions and to learn something of the operations and techniques.

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Safety is Top Priority
 All students are required to wear a lab gown during each experiment. This will be
strictly enforced to avoid accidents caused by chemical spills and the like.
 Safety glasses, goggles or eye shields must be worn during the experiment.
Contact lenses should not be worn.
 Shorts, skirts, sandals, slippers are not allowed in the laboratory. Secure long hair.

 Never taste, smell, or touch a chemical solution unless specifically directed to do


so. Individual allergic or sensitivity responses to chemicals cannot be anticipated. If
any chemical comes in contact with any other parts of your body or clothes, wash
thoroughly with plenty of water.
 Procedures involving the liberation of volatile or toxic flammable materials shall be
performed in a fume hood (e.g., H2S, HCN).
 Never heat a flask or apparatus that is not opened to the atmosphere.
 Always pour waste acid, used KMnO4, organic solvents and solutions of heavy
metals into their respective disposal jars, never into the sink.
 Replace the cover of every container immediately after removal of reagent. Deposit
insoluble refuse such as pieces of paper, wood, glass cork in the waste basket,
never into the sink or on the floor
 All accidents, injuries, breakages and spillages, no matter how minor, must be
reported immediately to the instructor.

 Eating, drinking, smoking and playing inside the laboratory are strictly prohibited.
Your hands may be contaminated with “unsafe” chemicals.
 Unauthorized experiments, including variations of those in the laboratory manual,
are strictly prohibited. If your chemical intuition suggests further experimentation,
consult with your instructor first.
 Unauthorized person(s) shall not be allowed in the laboratory.
 Maintain a wholesome, businesslike attitude. Horseplay and other careless acts are
prohibited.
 The tabletop must be cleared of unnecessary materials. Put all bags and books in
designated areas.
 Solids, water and other liquids spilled on your tabletop must be cleaned up as soon
as possible
 No electronic equipment (laptops, ipod, mp3s, cellphone, etc.) will be switched on
while working in the lab.

For Economic Reasons


 Always turn off the burner as soon as you are finished using it.
 Get only the amount of the reagent, which you need in the experiment. Use spatula
for solid reagents and pipet for liquid ones.
 Never return any excess reagent to a bottle, unless specifically directed, to avoid
contamination

Before leaving the room, see to it that:


 Your locker is locked
 Your assigned water and/or gas outlet(s) are turned off
 The tabletop and the floor near your working area are clean and dry

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Collecting Data

 Record all data as they are being collected on the laboratory notebook. Data on
scraps of paper (such as mass measurements in the balance room) will be
confiscated.
 Record the data in ink as you perform the experiment.
 If a mistake is made in recording data, cross out the incorrect data entry with a
single line (do not erase, white out or obliterate) and clearly enter the corrected
data nearby. If a large section of data is deemed incorrect, write a short notation
as to why the data are in error, place a single diagonal line across the data, and
note where the correct data are recorded.

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Assessment:
Evaluation of the students’ progress will be based on performance laboratory experiments; written
reports of laboratory work and exams. The distribution is as follows:

Exams 40%
Performance/ Attendance 10%
Written Laboratory report 40%
Pre-laboratory write-up/ Data notebook 10%

Laboratory Course Policies:


1. Arrive on time. The overview and description of the lab exercise, and the questions you need
to answer in your written reports are usually given at the start of each session. These could be
valuable to the success of you laboratory course.
2. Note all laboratory safety policies at all times. You are required to wear lab coats and safety
glasses while in the lab. You must wear your protective gear at all times that any lab work is
underway. Failure to observe safety precautions may result in your being dismissed from the
laboratory class.
3. Request all chemicals and materials that you may need from the stock room at least 30 mins.
ahead of the scheduled experiment. At this stage in your studies, you are expected to be able
to work independently and responsibly.
4. Written reports of laboratory work are due at the start of the following lab session. Reports that
are late will be penalized for each day of late submission.
5. Laboratory techniques, including your preparedness and participation in each laboratory
activity, good note-keeping and ability to work well with your partner will be graded
accordingly.
6. Read and plan you work before every laboratory class. Prepare a pre-laboratory write-up at
the start of the lab period and prior to starting your laboratory work. You will not be allowed to
perform the experiment without a pre-lab write up. The pre lab should include the following
sections: Experiment #, Title of Experiment, Date, Objectives of the Experiment’ Theoretical
Framework, Materials and Methods, Expected Outcome. Sign and Date each pre-lab write-up.
During the conduct of the experiment, record all your raw data in the same notebook.
7. Written Reports should be written on a short-sized bond paper and will have the following
components: Name, Laboratory partner/s, Discussion of Results, Calculation/s, Question/s,
and Answer/s, Conclusion/s, Comment on you and your partner’s contribution towards the
successful completion of the laboratory activity.

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COMMON LABORATORY OPERATIONS AND TECHNIQUES

1. BUNSEN BURNER

A. Lighting the Burner

a. Examine the parts of the Bunsen burner. Make a sketch of the burner, label and state the
function of its parts.

b. Attach the rubber tubing from the burner to the gas outlet on the lab bench. Bring the lighted
match or striker up 4-5 cm above the barrel while opening the gas valve.
c. Adjust the gas supply so as to have a flame of not more than 8 cm high. Close the air holes of
the burner and observe the appearance of the flame.

Hold the porcelain dish on this flame for a moment. What is deposited on the porcelain dish?

d. Open the air holes until the flame is pale blue and has two or more distinct cones. A slight
buzzing or roaring sound is characteristic of the hottest flame from the burner. Too much air
may blow the flame out. Adjust the air intake until the roaring stops. What is the effect on the
flame upon opening of the air holes?
Does this type of flame have the same effect on the porcelain dish? Why?

Spray powdered charcoal on the flame and note its effect.

What makes the flame luminous?


e. When the best adjustment is reached, three distinct cones are visible. Always use this kind of
flame unless directed otherwise.
f. Extinguish the flame when it is not being used, by closing the gas valve.

B. Determining the Flame Temperatures

a. Wet a piece of cardboard and hold it vertically through the center of the flame, with the lower
end of the cardboard resting against the top of the burner.
b. Remove the cardboard as soon as it shows a tendency to char. From the scorched portions
note the relative temperature of the different parts of the flame.
c. Draw a sketch of the flame to illustrate the different regions.

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2. GLASS MANIPULATION

A. Cutting

a. Place the glass tubing flat on the table. Make a single scratch with a sharp triangular file 30cm
from one end of the glass tubing.
b. Grasp the glass tubing with both hands and place the thumbs one cm beside the scratch.
Position the thumbs such that they are opposite the scratch.
c. Break the glass tubing by applying a gentle pressure. If it does not yield to gentle pressure,
make a deeper scratch.
d. The edges of the cut glass tubing are sharp and should be polished by rotating it at the non-
luminous portion of the burner’s flame. This is to prevent the sharp edges of the glass from
ruining corks and rubber tubing as well as cutting your fingers.

B. Bending

a. Take a piece of glass tubing about 30 cm long and hold it lengthwise over the flame.
b. To bend the glass tubing properly, it must be heated uniformly over a length of 5 to 8 cm. This
can be done using a flame spreader.
c. Roll the tube back and forth until it has become quite soft.
d. When it has become sufficiently soft, (i.e., the glass tubing begins to take a pink color and sag
gently) take it out of the flame.
e. Bend quickly to the desired angle (30° or 90°) and hold until it hardens. Try to get a good idea
of the angle before you begin to work so that you may work rapidly and secure the desired
bend at once.
f. Make one right angle and one 30O bent glass tubing.

NOTE: Reheating and re-bending produces unsightly and often frail apparatus.

C. Drawing Out

a. Roll the center of a 10cm glass tube over the flame until it softens. The tube must be
constantly rotated, to prevent the softened portion from sagging.
b. Quickly remove it from the flame, and while holding it in a vertical position, gently pull the ends
apart until the bore at the stretched portion is of the desired diameter.
c. Cut to the desired nozzle length and fire polish the tip.

D. Boring corks and rubber stoppers

a. Select a cork that will fit into the mouth of the flask or test tube.
b. Soften by rolling it between the tabletop and the palm of your hand. Select a sharp cork borer
one size smaller than the glass tube that will be inserted.
c. Place the cork on the desk and gently twist the borer in until it is halfway through the cork.
Then withdraw the borer and finish the hole from the other end of the cork.
d. Smoothen the hole in the cork with a round file.
e. If the hole is too small, enlarge it by carefully filing with a round file. Only small adjustment
should be made in this way.
f. Rubber stoppers are bored in the same manner as mentioned. Select a very sharp borer one
size larger than the hole to be made, and wet it with glycerin. Proceed as in boring the cork,
but do not apply too much pressure.

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E. Inserting a glass tubing through a cork/rubber stopper

NOTE: This operation is the most common cause of accidents in the laboratory.

a. Wet the cork and the glass tubing with water.


b. Place your hand on the tubing 2-3 cm away from the stopper. Protect your hand with a towel.
c. Simultaneously twist and push the tubing slowly and carefully through the hole.

3. CLEANING OF GLASSWARE

a. Clean all glassware with a soap or detergent solution. Use a brush if appropriate.
b. Once the glassware is thoroughly cleaned, rinse several times with tap water and then once or
twice with distilled water.
c. Roll each rinse around the entire inner surface of the glass wall for a complete rinse. Discard
each rinse through the delivery point of the vessel (e.g., beaker spout).
d. Invert the clean glassware on a clean paper towel or rubber mat to dry. Do not dry any
glassware over direct flame.
e. The glassware is clean if, following the final rinse, no water droplets adhere to the clean part of
the glassware.
f. If you must use a piece of glassware while it is still wet, rinse it with the solution to be used in
the manner described in step 5c below.

4. TRANSFERRING OF LIQUIDS/SOLUTIONS

a. When the liquid or solution is to be transferred from a reagent bottle, remove the glass stopper
and hold it between the fingers of the hand used to grasp the reagent bottle. Never lay the
glass stopper on the laboratory bench; impurities may be picked up and thus contaminate the
liquid when the stopper is returned.
b. To transfer a liquid from one vessel to another, hold a stirring rod against the lip of the vessel
containing the liquid and pour the liquid down the stirring rod, which, in turn, should touch the
inner wall of the receiving vessel. Return the glass stopper to the reagent bottle.
c. Do not transfer more liquid than is needed for the experiment; do not return any excess
liquid or unused liquid to the original reagent bottle.

5. MEASURING VOLUME OF LIQUID/SOLUTIONS

a. The eye should always be level with the meniscus when you are making a reading.
b. For measurements of clear or transparent liquids/solutions, the volume is read using the lower
meniscus. For colored liquids/solutions, the upper meniscus is used.

6. HEATING A LIQUID/SOLUTION IN A TEST TUBE

NOTE: Never fix the position of the flame at the base of the test tube and never point the test tube
to anyone. The contents may be ejected violently if the test tube is not heated properly.

a. The test tube should be less than one third full. Hold the test tube with a test tube holder at an
angle of about 45º with the cool flame. A cool flame is a nonluminous flame supplied with a
reduced amount of fuel.
b. Move the test tube circularly in and out of the flame, heating from top to bottom.

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7. PRECIPITATION

a. Place 2 mL of sodium chloride solution in a test tube and slowly add 2 mL of silver nitrate
solution. Write the balanced chemical equation for this reaction.

NOTE: Be careful in handling silver nitrate solution. This solution may leave dark stains on skin,
clothes or bench top.

b. The solid formed is the precipitate and in this case, the slightly soluble silver chloride. Allow
the precipitate to settle.
c. Add a few drops of silver nitrate solution. Continue addition until no precipitation is observed.
Divide the mixture into two portions and keep these for procedure 8.

8. SEPARATING A LIQUID FROM A SOLID

A. Filtration

a. Preparation of the filter paper to be used for gravity filtration:


i. Cut out a 5” x 5” piece of filter paper. Fold the filter paper in exact halves and fold it again
crosswise into two.
ii. Make a small tear in one corner. This tear seals the paper against the inflow of air to the
underside of the filter paper.
iii. Open the folded paper so as to form a cone.
iv. Place it in a funnel. Moisten it with a little water and press it against the top wall of the
funnel to form a seal. The filter paper must always be smaller than the funnel.
v. Support the funnel with a clamp or a funnel rack.
b. Transfer the precipitate formed from the previous activity by carefully pouring the mixture, with
the aid of a glass rod, into the filter paper. The liquid that passes through the liquid is called
the filtrate.
c. The tip of the funnel should touch the wall of the receiving beaker to reduce any splashing of
the filtrate.
d. Fill the bowl of the funnel until it is less than two-thirds full.
e. Always keep the funnel stem full with the filtrate; the weight of the filtrate creates a slight
suction on the filter in the funnel, thus this hastens the filtration process.
f. Set aside both precipitate and filtrate for the next two activities.

B. Decantation

a. Transfer the precipitate retained in the filter paper into a beaker by rinsing the filter paper with
jets of water from a wash bottle.
b. Allow the solid to completely settle at the bottom of the vessel for several minutes.
c. Transfer the liquid (called supernatant) into another container with the aid of a clean stirring
rod.
d. Do this slowly so as not to disturb the solid. Is this method applicable for the separation of all
solid-liquid mixtures? Why?

e. Rinse the precipitate with water and decant again.


f. Which of the two separation methods (i.e., decantation or filtration) is better in isolating the
precipitate? Why?
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E. Evaporation

a. Pour the filtrate obtained from 8A into the evaporating dish. Place the evaporating dish on a
wire-gauze supported on an iron ring clamped to an iron stand. Heat the dish over a cool
flame.
b. Continue heating until crystals begin to appear. Cover the dish with a watch glass and allow
the contents to cool. The solid remaining after evaporation is called the residue. What is the
composition of the residue?

9. WEIGHING

a. Weigh 0.5 g of sand. Weighing may be done on platform balance or on an analytical balance.
Rough weighing (to the nearest half gram), can be done on the platform balance. The
analytical balance is used to get more accurate mass measurements.
b. The properties of the substance will often determine the nature of the container where it is to
be weighed. Use a weighing paper, a watch glass, a beaker, or some container to measure
the mass of the chemicals.
c. Do not place the chemicals directly on the balance pan. When in doubt as to what container to
use, ask your instructor.

10. TECHNIQUE IN HANDLING CHEMICALS

a. A reagent is a substance which has a definite composition and a set of specific properties. The
strong solutions are marked “concentrated” and the weak solutions, “dilute”. Some examples
of the reagents are:
Sulfuric acid H2SO4 Ammonia NH3
Hydrochloric Acid HCl Sodium hydroxide NaOH
Acetic acid CH3COOH Calcium hydroxide Ca(OH)2

b. Before getting the desired amount, read the label twice to be sure it is the correct chemical at
the right concentration. Transfer the needed amount into the receiving container. Once
removed, these should never be returned.
c. Do not take out more than what is needed to minimize waste. Do not return excess
chemicals to the reagent bottle. In pouring reagents from bottles, don’t place the stopper on
the table but hold it between your fingers.
d. Never touch, taste or smell chemicals unless specifically directed to do so.

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EXPERIMENT

P R O P E R T I E S O F M AT T E R

This experiment presents several of the properties used to identify a sample of matter. The data
gathered are interpreted by the use of some quantitative method.

For safety and accuracy of results, the experimenter should make sure that all set-ups used should be
properly checked for possible connection leaks and other errors.

Stirring rod should be used to ensure uniform distribution of heat when heating liquids in an open
container. The heat should also be regulated especially when heating closed set-ups.

Laboratory techniques included are: measurement and transferring of liquids, weighing and heating of
liquids and solids.

MATERIALS AND APPARATUS

25 or 50-mL graduated cylinder Thermometer Cork and/or rubber stoppers


50-mL distilling flask Bunsen burner Top loading balance
250-mL beaker Rubber tubings Condenser
25-mL Florence flask Iron stand Oil
Test tube Iron ring Sulfur powder
2-3 iron clamps Wire gauze Isopropyl alcohol
Lead pellets

PROCEDURE

1. BOILING POINT

a) Measure 25 mL of isopropyl alcohol and record the initial temperature.


b) Transfer it into a 50-mL distilling flask. Assemble the distillation set-up (consult the instructor).
c) Warm the set-up gently with a Bunsen burner. Take temperature readings at one-minute time
intervals until the liquid begins to boil, and two more minutes thereafter.
d) Continue distilling until the flask is almost dry. Pour off the liquid still present in the flask.
e) Transfer the distillate into the distilling flask and repeat the distillation process.
f) Make a graph of your data with time on the x-axis and temperature on the y-axis. Compare the
two graphs.
g) Determine the boiling point of the liquid from the graphs. Look for the standard boiling point of
isopropyl alcohol and get the % error of the boiling point obtained experimentally.

2. MELTING POINT

a) Place about 1-gram of sulfur powder into a dry test tube. Clamp the test tube vertically into the oil
bath. See to it that the solid is below the oil level.
b) Hang the thermometer into the test tube such that it is covered by the solid and does not touch the
sides and bottom of the test tube.
c) Heat the oil bath gradually and take temperature readings at one-minute intervals until the solid
has completely liquefied, and two more minutes thereafter.
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d) Make a graph of your data with time on the x-axis and temperature on the y-axis. Determine the
melting point of sulfur from the graph. Look for the standard melting point of sulfur and get the %
error of the melting point obtained in the experiment.

NOTE: Stir the oil bath so that the heat is uniformly distributed.

3. DENSITY OF A LIQUID

a) Clean and dry the Florence flask. Weigh the dry flask and the rubber stopper on a top loading
balance and record the mass.
b) Fill the flask with distilled water until the liquid level is nearly to the brim. Put the stopper on the
flask in order to drive all the air and excess water. Work the stopper gently into the flask so that it
is firmly seated into position.
c) Wipe any water on the outside of the flask and soak up all excess water from around the top of the
stopper.
d) Again, weigh the flask, which should be completely dry on the outside and full of water, and record
the mass.
e) Calculate for the precise volume of the flask given the standard density of water, the temperature
of the laboratory and the mass of water in the flask.
f) Empty the flask, dry it and fill it with isopropyl alcohol. Stopper and dry the flask as you did when
working with water. Record the weight of the flask filled isopropyl alcohol.
g) Calculate the density of isopropyl alcohol and determine the % error using its standard density.

4. DENSITY OF A SOLID

a) Use the same flask from the previous procedure for this part. Dry the flask completely and add
small chunks of lead metal into the flask until it is about half full.
b) Weigh the flask, with its stopper and the metal, and record the mass. Determine the mass of the
metal in the flask.
c) Fill the flask with water, leaving the metal in the flask, and then replace the stopper. Roll the metal
around the flask to make sure that no air is trapped between the metal pieces.
d) Refill the flask if necessary, and then weigh the dry stoppered flask full of water plus the metal
sample.
e) Compute for the density of the lead using the data obtained in this section and in part 3.
Determine the density of the metal and compute for the % error.

QUESTIONS

1. Interpret the graphs obtained in parts 1 and 2. What changes occur at the different regions of the
graph?
2. What kind of properties are boiling point, melting point and density?
3. Which of these properties may be used to identify a sample of matter? Why?
4. Is one property sufficient to establish the density of the substance?
5. What is the identity of the distillate in Part 1? What is your basis?

12
EXPERIMENT

C H E M I C AL C H A N G E S

This experiment presents different types of chemical change. Some quantitative methods are included
to emphasize proper data handling and interpretation of results. Formula writing and setting up of
simple chemical equations are introduced.

It is to be emphasized that the experimenter should always take note of any physical evidence that a
chemical reaction is taking place. Such physical evidences include the formation of a precipitate,
change in color of the solution or precipitate, evolution of a gas, and absorption or evolution of heat.

 Evolution of gas. This evolution may be quite rapid or it may be a “fizzing” sound.
 Appearance or Disappearance of precipitate. The nature of the precipitate is important; it may
be crystalline, it may have color, it may merely cloud a solution.
 Evolution or Absorption of Heat. The reaction vessel becomes warm if the reaction is
exothermic or cools if the reaction is endothermic.
 Change in color. A substance added to the system may cause a color change.

Also included are the common laboratory operations such as measurement and transferring of liquids,
precipitation, decantation, filtration, washing and transferring of precipitates, drying of solids,
weighing, testing for acidity and basicity, and testing for completeness of a reaction.

This experiment also emphasizes the need for gradual mixing of reactants to make certain the
maximum recovery of the product, and the importance of washing, to ensure the purity of the product.

MATERIALS AND APPARATUS

50-mL graduated cylinder Watch glass Zinc dust


250-mL beaker Evaporating dish 0.100 M Cu(NO3)2
250-mL Erlenmeyer flask Pair of scissors 6.00 M NH3
Funnel Filter paper 6.00 M NaOH
Bunsen burner Litmus paper 6.00M HCl
Stirring rod Medicine Dropper 6.00 M H2SO4

PROCEDURE

1. PRECIPITATION OF COPPER (II) HYDROXIDE

a) Measure 10-mL of 0.100 M Cu(NO3)2 solution in a 250-mL beaker.


b) Add dropwise with constant stirring about 0.5 mL 6.00 M NaOH solution.
c) Place a piece of litmus paper on a dry watch glass and moisten it with the solution using a stirring
rod.
d) If it is not yet alkaline, add more NaOH. Record any change in color of the solution and describe
the precipitate.

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2. FORMATION OF COPPER (II) OXIDE

a) Boil the contents of the beaker in part 1 for about 2 minutes with constant stirring to prevent
“bumping” which may result in loss of material. The precipitate should change in color.
b) Allow the copper (II) oxide precipitate to settle. Take note of the change in color of the precipitate.
c) Test the supernate with a few drops of 6.00M NaOH. If cloudiness is observed, continue the
addition of the base until precipitation is complete.
d) Heat the solution again with constant stirring, until all the precipitate has changed in color. Record
the color changes that occur. What is the evidence of complete precipitation? What is the
composition of the supernate?

3. CONVERSION OF COPPER (II) HYDROXIDE TO COPPER (II) SULFATE

a. Let the precipitate settle until the supernate is clear. Decant the supernate through a filter paper
into the Erlenmeyer flask.
b. Wash the precipitate in the beaker using 10 mL of water. Let the precipitate settle and decant the
wash water through the filter paper into the Erlenmeyer flask containing the filtrate.
c. Repeat the process, so that the precipitate is washed a total of four times.
d. Wash the same filter paper with about 1 mL 6.00 M H2SO4 dropwise, catching the filtrate in the
beaker containing copper (II) oxide precipitate.
e. Rotate or stir the contents of the beaker to dissolve the solid. Add some more H2SO4 to dissolve
the precipitate completely.
f. Wash the filter paper again, this time with 10 mL water, catching the wash water in the same
beaker. Record your observations.

4. REDUCTION OF Cu (II) IONS TO METALLIC COPPER

a. To the solution (from 3), gradually add with constant stirring, about 1.5 g zinc dust in minute
amounts.

CAUTION: Stir until no further reaction is observed before adding more zinc to make the solution
colorless.

b. Test for the completeness of the reaction by adding a few drops (1-2 drops) of the solution into a
test tube containing about 1 mL of 6.00 M NH3. If a colored solution is obtained, compare this with
the control solution (prepare by adding a drop of 0.100 M Cu(NO3)2 solution and 2 drops of NH3 to
1 mL water) and add more zinc into the solution with constant stirring. Repeat the process until the
test with ammonia solution gives a colorless solution.
c. Decant and discard the supernate in 4-b. Wash the precipitate in the beaker twice, each time
using 10-mL portions of water. Decant and discard the wash water after each washing, taking care
not to lose any solid.
d. To the precipitate, add 10 mL water and 2 mL 6.00 M HCl slowly and stir the contents until no
more change is observed. Let the precipitate settle, decant and discard the supernate into a waste
acid jar.
e. Wash the precipitate twice, each time using 10-mL portions of water. Decant and discard the wash
water.
f. Transfer the entire solid in the beaker to a previous weighed filter paper. Use as little water as
possible to wash out the solid from the beaker. Discard the filtrate and wash water.
g. Fold the filter paper containing the solid and press this between pieces of dry filter paper to
remove most of the water. Place the partially dried filter paper containing the solid on a watch
glass, and air dry in your locker until the next period. Weigh the solid and the filter paper. Record
all masses obtained.
14
5. OXIDATION OF COPPER

a. Place a pinch of the weighed solid in an evaporating dish and heat the dish directly over a Bunsen
burner. Observe and record your results.
b. Submit the remaining solid, properly packaged and labeled, to your instructor.

QUESTIONS

1. What type of process and/or chemical changes is observed in procedures 1-5?


2. Why must zinc be added very gradually to the solutions in procedure 4.a?
3. What is the purpose of the test using ammonia solution?
4. Why must HCl be added to the solid after the reaction with zinc dust is completed?
5. Why is it not advisable to dry the copper directly over a Bunsen flame?
6. Calculate the percent recovery in the experiment. Does your result refute the law of conservation
of matter? Explain.

15
EXPERIMENT

C L AS S I F I C AT I O N O F M AT T E R

Matter is classified according to its various properties and the type of changes it undergoes. There
are two general types of matter, substances and mixtures. Substances are further subdivided into two
types, elements and compounds. Mixtures are also of two kinds, homogeneous and heterogeneous.

This experiment aims to differentiate several samples of matter. The samples are subjected to
different conditions like temperature and solubility in some solvents. Chemical changes are illustrated
by chemical equations.

MATERIALS AND APPARATUS

Beakers Evaporating dish Sugar crystals


250-mL Erlenmeyer flask Test tubes Sodium chloride
Funnel Thermometer Iodine Crystals
Bunsen burner Mortar and Pestle Sulfur powder
Glass tubing Filter paper Lead (II) nitrate
Watch glass Litmus paper Magnesium ribbon
Medicine dropper Starch solution

PROCEDURE

1. SUBSTANCES, HOMOGENEOUS AND HETEROGENEUOS MIXTURES

a. Measure out one gram of refined sugar in the balance. Dissolve the sample in 50 mL tap water.
Compare the appearance of the solution with that of distilled water. Set up a simple distillation
apparatus using the Erlenmeyer flask, thermometer and glass tubing.
b. Distill the sugar solution and make a boiling point curve on the graphing paper. Collect the sugar
solution and make a boiling point curve of the isopropyl alcohol (from experiment 1). Compare the
boiling point curve of the sugar solution with that of the isopropyl alcohol. Which of the two is a
substance and which is a mixture?
c. Test for the solubility of the powdered sulfur in water. Do the same with sodium chloride. Weigh
out 0.5 g of each chemical on the analytical balance.
d. Grind the two together in a mortar. Note the appearance of the mixture. With a hand lens, observe
the mixture more closely. Can you distinguish the sulfur from the sodium chloride crystals?
e. Transfer half of the mixture into a beaker containing about 15 mL of water. Stir thoroughly then
filter the resulting mixture. Identify the filtrate and the residue on the filter paper.
f. Transfer the filtrate into an evaporating dish. Heat this to boiling. When the crystals begin to form,
cover the dish with watch glass to prevent sputtering. When the crystals are almost dry, stop
heating the dish.
g. Heat the other half of the original mixture in an evaporating dish until melting is observed.
Examine the resulting product closely using a hand lens. Can you now differentiate the two
components? Test its solubility in water. Record all observations.

16
2. ELEMENTS AND COMPOUNDS

a. Take two small crystals of iodine. Place one crystal inside the test tube and heat it gently.
Compare the heated and the unheated crystals with respect to state, color, solubility in water and
their behavior in starch solution.
b. Take a pinch of lead nitrate crystals. Observe carefully and list down its observable physical
properties. Heat it over a burner, gently at first, and then strongly afterwards until no further
change is observed. List down your observations.

3. METALS AND NON-METALS

a. Clamp a medium-sized test tube horizontally. Take a piece of magnesium ribbon and insert one
end into a 10-cm piece of glass tubing.
b. Heat the magnesium ribbon. When it begins to burn, insert the burning magnesium ribbon into the
test tube until the metal has burned completely.
c. Dissolve the residue in 3-mL water. Test the acidity and basicity of the solution with litmus paper.
Repeat using a pinch of sulfur.

QUESTIONS

1. Write all chemical equations involved.


2. Does the appearance of the sugar solution differ from that of distilled water?
3. In part 1, which is an example of a homogeneous and heterogeneous mixture? How are the two
types of mixtures differentiated?
4. What is the composition of the crystals formed after evaporation of the filtrate in 1.b?
5. Based on the results of part 1, how are substances different from mixtures?
6. Is there any evidence that would indicate a change in the identities of each of the substances
heated? What are these evidences?
7. Differentiate the oxides of metals and non-metals.
8. From the results in part 2, define elements, compounds, metals and non-metal.
9. Iodine is liberated from seaweeds by the action of sulfuric acid on the ash of the seaweeds. How
is it collected from the ashes?

17
EXPERIMENT

THE LANGUAGE OF CHEMISTRY: CHEMICAL NOMENCLATURE

Chemical Nomenclature is the system of naming substances. A systematic nomenclature was


established by an organization of chemists called the International Union of Pure and Applied
Chemistry (IUPAC). The standardized rules developed by the IUPAC are summarized below.

1. Binary Compounds

1.1 Binary Compounds Containing Two Nonmetals

If two nonmetals form a compound, the less electronegative is written first, followed by the more
electronegative element. The same pattern is used in naming; the less electronegative is mentioned
first, followed by the stem of the name of the more electronegative ending in –ide. When more than
one compound can be formed from the combination of two elements, Greek prefixes are used to
indicate the number of atoms of each element.

CO2 carbon dioxide


PCl3 phosphorous trichloride
Cl2O Dichlorine mon(o)oxide*
HCl Hydrogen chloride
*this is omitted when the more electronegative element begins with a vowel

Greek Prefix Number Greek Prefix Number


Mono- 1 Hexa- 6
Di- 2 Hepta- 7
Tri- 3 Octa- 8
Tetra- 4 Nona- 9
Penta- 5 Deca- 10

1.2 Binary Compounds Containing a Metal and a Nonmetal

The metal is always written first, in both the name and the formula. As with all binary compounds, the
nonmetal takes an –ide ending. There are two types that we must consider: metals with fixed (only
one) oxidation number and those with variable (more than one) oxidation numbers.

1.2.1 Cations

Monatomic ions cations retain their names as elements. The NH4+ ion, ammonium ion is
named as if it were a metal ion because of its saltlike properties.
Li+ lithium ion
Na+ sodium ion
2+
Mg magnesium ion
Al3+ aluminum ion
1.2.2 Monatomic Anions

18
Monatomic anions are named using their names as elements and the suffix –ide.

C4- carbide
N3- nitride
O2- oxide
H- hydride

1.2.3 Metals with Fixed Oxidation Numbers

The metals with fixed oxidation numbers are the IA and IIA, Aluminum and Zinc. All other metals
have variable oxidation numbers. Note that no prefixes are used.

NaCl Sodium chloride


Na2S Sodium sulfide
AgBr silver bromide
Al2O3 aluminum oxide

1.2.4 Metals with Variable Oxidation Numbers

In a binary compound of a metal of this type with a nonmetal, the oxidation number of the metal
must be indicated in the name. There are two methods of doing this, the classical system and the
Stock or Roman numeral system.

1.2.4.1 Classical System

This system can only be used for metals having two oxidation states. An –ic ending is
used for the metal with the highest oxidation state and an –ous ending is used for the
lowest. Also, the Latin name is used for iron (ferric and ferrous), copper (cupric and
cuprous), tin (stannic and stannous) and lead (plumbic or plumbous). The classical
system does not indicate the actual oxidation state.

1.2.4.2 Stock System or Roman Numeral System

The actual oxidation state is designated by a Roman Numeral placed in parenthesis


immediately following the name of the metal. This is useful especially if the metal has more
than two oxidation states.

Formula Classical System Stock System


CuCl Cuprous chloride copper(I) chloride
CuCl2 Cupric chloride copper(II) chloride
FeCl2 ferrous chloride iron(II) chloride
FeCl3 ferric chloride iron(III) chloride

1.3. Compounds Named Like Binary Compounds

Few other compounds take an –ide ending, like binary compounds. These include the following:

OH- hydroxide
O22- peroxide
CN- cyanide
NH2- amide
19
I3- triiodide
N3- azide
1.4. Trivial Names

Some common binary compounds are assigned trivial names that have been assigned arbitrarily.
These are universally used that they are allowed by the IUPAC rules of nomenclature.

H2O water
NH3 ammonia
PH3 phosphine
AsH3 arsine

1.5. Binary Acids

A binary compound composed of hydrogen with a more electronegative element can act as a binary
acid in water solution. For acids of this types, the prefix hydro- is added, and then the –ide ending is
replaced by –ic acid.

HF hydroflouric acid
HCl hydrochloric acid
HBr hydrobromic acid
HI hydroiodic acid

2. Ternary and Higher Compounds

2.1 Oxyacids and Salts

Oxyacids are composed of a nonmetal with more than one oxidation state, along with hydrogen and
oxygen. A salt of oxyacid is formed when one or more of the hydrogen ions of an acid is replaced by a
cation. The prefix hypo-, is used to denote the lowest oxidation state of the nonmetal with the
characteristic ending –ous and the prefix per- is used to denote the highest oxidation state with the
ending –ic. For acids whose names end in –ous, the corresponding salt ends with the suffix –ite, and
those whose names ends in –ic, the name of the salt ends in –ate.

Acid Oxyanion Salt


H2SO3 sulfurous acid SO32- sulfite Na2SO3 sodium sulfite
H2SO4 sulfuric acid SO42- sulfate Fe2SO4 iron(II) sulfate
HClO hypochlorous acid ClO- hypochlorite NaClO sodium hypochlorite
HClO2 chlorous acid ClO2- chlorite KClO2 potassium chlorite
HClO3 chloric acid ClO3- chlorate NaClO3 sodium chlorate
HClO4 perchloric acid ClO4- perchlorate NaClO4 sodium perchlorate

2.2 Salts of Polyprotic Acids

These types of salts are formed when one or more hydrogen ions in polyprotic acids or acids with
more than one replaceable H+ ion (e.g., H2S, H3PO4, H2SO4) is/are replaced by metal ions. In naming,
the word hydrogen is added to the name of the oxyanion.

NaH2PO4 sodium dihydrogenphosphate


Na2HPO4 disodium hydrogenphosphate
Na3PO4 trisodium phosphate
NaHS sodium hydrogensulfide

20
EXERCISES

1. Name the following.


a. FeI2 ___________________________________
b. I2 ___________________________________
c. FeCl3 ___________________________________
d. Fe2(SO4)3 ___________________________________
e. FeS ___________________________________
f. NCl3 ___________________________________
g. H2CO3 ___________________________________
h. CaCO3 ___________________________________
i. Be2C ___________________________________
j. SnSO4 ___________________________________
k. (NH4)2S ___________________________________
l. N2O4 ___________________________________

2. Write the correct chemical formula


a. Barium chloride ___________________
b. Stannous nitrate ___________________
c. Stannic nitrate ___________________
d. Aluminum carbide ___________________
e. Magnesium phosphate ___________________
f. Nitrogen dioxide ___________________
g. Ammonium sulfate ___________________
h. Barium carbonate ___________________
i. Sodium carbonate ___________________
j. Calcium hydrogen phosphate ___________________
k. Disulfur dichloride ___________________

3. Complete the following table

Formula Name as acid Formula of Name of salt


sodium salt
HNO3
HNO2
HBrO
HBrO2
HBrO3 NaBrO3
HBrO4

4. Name the following as binary compounds or as salts from the anions of polyprotic or oxo
acids.
a. NaIO ___________________________________
b. K2HPO4 ___________________________________
c. Na2SO3 ___________________________________
d. KMnO4 ___________________________________
e. BaSO3 ___________________________________
f. FeSO4 ___________________________________
g. HClO3 ___________________________________
h. Na2SO4 ___________________________________
i. Fe(NO3)3 ___________________________________
21
j. Ca(ClO2)2 ___________________________________

5. The spaces below represent portions of some of the main groups and periods of the periodic
table. In the proper squares, write the correct formulas for the chlorides, oxides and sulfates of
the elements of Groups 1, 2 and 3, respectively. Likewise, write the formulas of the
compounds of sodium, calcium and aluminum with the elements of Groups 6 and 7. Two of the
squares have been completed as examples.

Period Group 1 Group 2 Group 3 Group 6 Group 7


2 LiCl (Omit sulfate)
Li2O
Li2SO4
3 Na2S
CaS
Al2S3
4

EXPERIMENT

22
WATER OF HYDRATION

Most solid chemical compounds will contain some water if they have been exposed to the atmosphere
for any length of time. In most cases the water is present in very small amounts, and is mere
adsorbed on the surface of the crystals. Other solid compounds contain larger amounts of water that
is chemically bound in the crystal. These compounds are usually ionic salts. The water that is present
in these salts is called the water of hydration and is usually bound to the cations in the salt.

In this experiment you will study some of the properties of hydrates. You will identify the hydrates in a
group of compounds, observe the reversibility of the hydration reaction, and test some substances for
efflorescence or deliquescence. Finally you will be asked to determine the amount of water lost by a
sample of unknown hydrate on heating. From this amount, if given the formula or the molar mass of
the anhydrous sample, you will be able to calculate the formula of the hydrate itself.

MATERIALS AND APPARATUS

watch glass iron ring crucible tongs


test tubes iron stand triangular clay
Bunsen burner crucible desiccators

PROCEDURE

1. Identification of Hydrates. Place about 0.5 g of the compounds listed below in small, dry test
tubes, one compound to a tube. Observe carefully the behavior of each compound when you heat
it gently with a burner flame. If droplets of water condense on the cool upper walls of the test tube,
this is evidence that the compound may be a hydrate. Note the nature and the color of the residue.
Let the tube cool and try to dissolve the residue in a few cm3 of water, warming very gently if
necessary. A true hydrate will tend to dissolve in water, producing a solution with a color very
similar to that of the original hydrate. If the compound is a carbohydrate, it will give off water on
heating and will tend to char. The solution of the residue in water will often be caramel colored.

Nickel chloride
Potassium chloride
Sodium tetraborate (borax)
Sucrose
Potassium dichromate
Barium chloride

2. Reversibility of Hydration. Gently heat a few crystals ~0.3 g, of hydrated cobalt (II) chloride,
CoCl2 6H2O, in an evaporating dish until the color change appears to be complete. Dissolve the
residue in the evaporating dish in a few cm3 of water from your wash bottle. Heat the resulting
solution to boiling (CAUTION!), and carefully boil it to dryness. Note any color changes. Put the
evaporating dish on the lab bench and let it cool.

3. Deliquescence and Efflorescence. Place a few crystals of each of the compounds listed below
on separate watch glasses and put them next to the dish of CoCl2 prepared in Part B. Depending
upon their composition and the relative humidity (amount of moistures in air), the samples may
gradually either lose water of hydration to, or pick up water from, the air. They may also remain
unaffected. Any changes in crystal structure, color, or appearance of wetness should be noted.
23
Observe the samples occasionally during the rest of the laboratory period. Since the changes tend
to occur slowly, your instructor may have you compare your samples with some that were set out
in the laboratory a day or two earlier.

Na2CO3 10H2O (washing soda)


CaCl2
KAl(SO4)2 12H2O (alum)
CuSO4 5H2O
4. Percent Water in a Hydrate. Clean a porcelain crucible and its cover with 6 M HNO3. Any stains
that are not removed by this treatment will not interfere with this experiment. Rinse the crucible
and cover with distilled water. Put the crucible with its cover slightly ajar on a clay triangle and
heat with a burner flame, gently at first and then to redness for about 2 minutes. Allow the crucible
and cover to cool, and then weigh them to 0.001 g on an analytical balance. Handle the crucible
with clean crucible tongs.

Obtain a sample of unknown hydrate from the stockroom and place about a gram of sample in the
crucible. Weigh the crucible, cover, and sample on the balance. Put the crucible on the clay
triangle, with the cover in an off-center position to allow the escape of water vapor. Heat again
gently at first and then strongly, keeping the bottom of the crucible at red heat for about 10
minutes. Center the cover on the crucible and let it cool to room temperature. Weigh the cooled
crucible along with its cover and contents.
Examine the solid residue. Add water until the crucible is two thirds full and stir. Warm gently if the
residue does not dissolve readily. Does the residue appear to be soluble in water?

DATA AND OBSERVATIONS

A. Identification of Hydrates

Water appears Color of residue Water soluble Hydrate


Nickel chloride
Potassium chloride
Sodium tetraborate
Sucrose
Potassium dichromate
Barium chloride

B. Reversibility of Hydration

Summarize your observations on CoCl2 6H2O. Is the dehydration and hydration of CoCl2 reversible?

C. Deliquescence and Efflorescence

Observation Conclusion
Na2CO3 10H2O
CaCl2
KAl(SO4)2 12H2O (alum)
CuSO4 5H2O

D. Percent water in a Hydrate

24
Mass of crucible and cover
Mass of crucible, cover, and solid hydrate
Mass of crucible, cover, and residue

Mass of solid hydrate


Mass of residue
Mass of water lost
Percentage of water in the unknown hydrate
Formula mass of anhydrous salt (if furnished)
Number of moles of water per mole of unknown hydrate

25
EXPERIMENT

G AS E S

This experiment illustrates three of the common gas laws: Boyle’s law, Charles and
Gay-Lussac’s law and Graham’s law. Boyle’s law states that the volume, V, of a certain quantity of an
ideal gas is inversely proportional to its pressure, P, at a given temperature and amount of gas.
Charles’ and Gay-Lussac’s law states that the volume of a gas is directly proportional to the absolute
temperature, at a certain pressure and amount of gas. Graham’s law describes that the velocity of an
ideal gas is inversely proportional to the square root of its molar mass.

The first two gas laws will be validated using plots of the properties involved. Graham’s law will be
determined by comparing the velocities of two sample gases.

MATERIALS AND APPARATUS

Glass syringe 250 or 400-mL beaker Black cardboard


Syringe holder Iron stand Ruler
Thermometer Iron ring Graphing paper
Glycerol Wire gauze Concentrated HCl
Modeling clay Glass tubing Concentrated ammonia
Standard weights Cotton balls Cooking oil
Bunsen burner Medicine droppers

PROCEDURE

1. BOYLE’S LAW

a. Remove the plunger from the barrel of the syringe, weigh and determine its diameter. Apply a thin
film of glycerol to the lower side of the plunger, and with a screw-like motion, insert it back into the
barrel.
b. Inspect the syringe carefully to make sure that the lubricant is evenly distributed over the inner
wall of the syringe (there should be no translucent spots). Add more lubricant if necessary but
avoid any excess.
c. Withdraw the plunger so that there are 20 mL of air inside the syringe. Carefully plug the tip of the
syringe with modeling clay and insert the tip as far as it would go into a one-hole rubber stopper.
Fill-up the hole of the stopper with more modeling clay.
d. Record the initial volume, temperature and pressure acting on the gas. The pressure is computed
as:
e. Number and weigh each weight. Carefully balance one weight immediately on the plunger. If there
is no leakage, the plunger should rise to its original level once the weight is removed.
f. If it does not, check the set-up for leaks and repeat the previous procedure.
CAUTION: Do not allow the weight to remain too long on the plunger to avoid the loss of gas
between the barrel and the plunger.
g. Record the volume and pressure readings. Repeat using two weights, three weights, etc. Tabulate
the results.
h. Make a graph using the data with the pressure on the x-axis and volume on the y-axis. Express in
word and in mathematical symbols the effect of pressure on the volume of gases. Determine the
proportionality constant from the graph.

26
2. CHARLES’ AND GAY-LUSSAC’S LAW

a. Pour the oil into the beaker. Make sure that the level of the oil is above the highest mark of the
syringe.
b. Hang a thermometer in the beaker. The thermometer should not touch the sides or bottom of the
beaker.
c. Heat the oil to around 120 C. Place the syringe very slowly into the beaker of hot oil with its
plunger at the highest mark. Clamp the syringe.
d. Notice what happens to the air in the syringe. Clamp the plunger to keep it from moving. Remove
the burner as long as the desired temperature is reached.
e. When bubbles stop coming out of the tip of the syringe, read the volume and temperature in
tabulated form.
f. Stir the oil occasionally to keep the temperature uniform. Observe what happens to the volume of
the air inside the syringe as the oil cools.
g. At regular volume reading intervals, such as 0.5 mL, read and record the temperature reading until
the temperature drops to 30 C.
h. Plot the data of volume and temperature readings. State the relationship between the volume and
the temperature of the gas as shown in the graph. Determine the proportionality constant from the
graph.

3. GRAHAM’S LAW

a. Place about 6 drops of hydrochloric acid on one cotton plug and 6 drops of ammonia on the other.
CAUTION: Concentrated acids and bases are toxic upon skin contact. Avoid touching the cotton
plugs with your bare hands.
b. Hold the tube horizontally against the black sheet of paper or cardboard and place the plugs
simultaneously on the opposite ends of the tube.
c. Record the time when the ring is observed. Measure the distance of the ring from both ends of the
tube with a ruler.
d. Determine the rate of diffusion of the gases. Calculate the molar masses of the gasses and
determine the relationship between the two properties.

QUESTIONS

1. What factors were kept constant in parts 1 and 2? Why is it necessary to do so?
2. What will be the effect of using different pressure units in your results?
3. What will be the effect of using different temperature in the volume vs. temperature plot? Will the
relationship stay the same?
4. Which gas travels faster in part 3?
5. Do the results verify the gas laws? Account for the discrepancy if there are any.

27
EXPERIMENT

OXYGEN

This experiment aims to determine the different sources of oxygen. Moreover, its properties, both
physical and chemical, will also be investigated.

MATERIALS AND APPARATUS

Mortar and pestle Cork stoppers Test tubes


Bunsen burner Beaker Glass funnel
Delivery glass tube Glass tubing Plastic water bath (ice cream container)
Iron clamp

PROCEDURE

1. PREPARATION OF OXYGEN

a. Mix in a dry mortar about 0.5 g of potassium chlorate and about 0.2 g of manganese dioxide.
b. Transfer into a dry Pyrex test tube, clamp horizontally, and tap gently to distribute the mixture
along the lower side of the test tube.
c. Fit the test tube with the delivery glass tube, being careful to leave a clear opening for the
passage of the gas through the delivery tube, otherwise, an explosion may occur.
d. Half-fill the plastic container with water and float in it 3 cork stoppers for the test tube.
e. Fill four test tubes with water. Cover the mouths with your thumb in such a way that no air
bubbles are left in the test tubes and then invert the test tubes in the water bath.
f. Remove your thumb from the mouth while they are held under water.
g. Heat the mixture slowly by moving the flame slowly along the tube. Collect the gas produced
by water displacement.
h. Discard the first test tube of the gas collected. Cover tightly the mouth of the other test tube
with a cork stopper before removing from water.
i. The test tube should be set on the test tube rack with their mouths upward.
j. After filling up the last test tube, remove the delivery tube from water before removing the
flame under the test tube. Save the residue for part 3.

2. PROPERTIES OF OXYGEN

a. Based on your observation during its preparation, determine the following properties of
oxygen: color, odor, taste and solubility in water
b. Place a small amount of sulfur at the inner tip of the glass tubing and then heat it using a
Bunsen flame until it ignites. Note the resulting flame in the air.
c. Lower the tubing into a test tube of oxygen being careful not to touch the walls of the test tube.
d. Keep the mouth of the test tube covered by means of a glass plate in order to retain the
combustion products. Do not remove the glass tubing until the reaction ceases.
e. Compare the appearance of the flame in oxygen and in air. After removing the glass tubing
from the test tube, add about 5 mL of distilled water. Cover with cork and shake thoroughly.
f. Test the acidity and alkalinity of the solution using litmus paper.

28
g. Clean and dry the glass tubing. Repeat the entire process using red phosphorous instead of
sulfur. Notice the changes taking place.

3. ANALYSIS OF THE RESIDUE

a. Transfer the residue of the test tube in part A to a beaker and dissolve in 30 mL of distilled
water.
b. Warm if necessary to effect dissolution. Filter.
c. To 5 mL of the filtrate above, add several drops of silver nitrate (2% solution) and a drop of
nitric acid (10% solution).
d. Treat 5 mL of potassium chlorate (10% solution) in the same way and compare the results
obtained in the two tests.

4. SLOW OXIDATION OF METALS

a. Place about 1 gram of iron fillings in a test tube and add just enough water to wet and make
them cling to the bottom of the tube.
b. Invert the tube in a beaker of water and clamp it with the mouth of the tube about 1 cm below
the surface of the water. Leave it in this position until the next laboratory period.

QUESTIONS

1. In the preparation of oxygen, why is the first test tube of the gas discarded? Why should the
stoppered test tube of oxygen be set upwards?
2. What is the role of manganese dioxide in the reaction?
3. Which of the reactants used in part 1 decomposed to produce oxygen gas? What was the other
product?
4. Compare the appearance of the ignited sulfur and red phosphorous outside and inside the test
tube containing oxygen. State the reason for the observed differences.
5. What is the significance of the precipitate formed in part 3?
6. In part 4, explain why water rises into the tube after sometime?
7. Does iron rust more rapidly when dry or wet?
8. How would you protect your metal utensils from oxidation?

EXPERIMENT
29
HEAT AND VOLUME EFFECTS

Liquids maybe completely miscible, partially miscible or immiscible with each other. Miscible liquids on
mixing may release heat, absorb heat or show no heat absorbed or evolved. Volume changes may
accompany these heat changes.

The magnitude of such heat and volume changes is related to the type of strength of the
intermolecular forces of attraction (IMF), making the solution process possible. These intermolecular
forces in turn depend on the structure of the molecules concerned. From previous lessons on Lewis
structures and molecular geometry, these molecular structures could already be drawn. Hence, the
polarity of each molecule could then be predicted.

There are six basic types of IMF. Such types are enumerated according to decreasing IMF (assuming
all other variable affecting IMF are equal).
1. ion-ion interaction
2. ion-dipole interaction
3. ion-induced dipole interaction
4. dipole-dipole interaction
5. dipole-induced interaction
6. induced dipole-induced dipole interaction

The presence of hydrogen bonding enhances the overall interaction.

In this experiment, different two-component systems are prepared. Observed heat and volume effects
are rationalized, on the basis of the molecular structures of the components and predicted
intermolecular forces of attraction among similar molecules and among dissimilar forces.

MATERIALS AND APPARATUS

6 pcs 10 mL test tubes corks ethanol


burette or transfer pipettes distilled water methanol
aspirator acetone

PROCEDURE

1. Measure out from the burette or using pipettes 8 mL portions of distilled water into each of the 6-
10mL test tubes, which has been previously cleaned and dried.
2. Mark the level of water in each of the test tubes. Pour off the water and allow them to dry
thoroughly. The test tubes are now calibrated to the 8 mL volume mark.
3. Prepare each of the mixtures listed, by mixing 4 mL each of the two solutions in a calibrated test
tube. Stopper the tube immediately, (see NOTE 1), shaking to mix well.
4. Feel the test tube for any temperature change (see NOTE 2). Set aside the test tubes containing
the solutions (10-20 minutes) to allow the temperature of the system to return to room temperature
(see NOTE 3).
5. Note any change in the volume of the solution relative to the calibrated 8 mL mark. Record the
volume as > than , < than or = to 8 mL.
6. Predict the effect on the vapor pressure of the resulting solution based on your data. Tabulate the
data.

30
Soln. A + Soln. B Vsoln vs. 8 mL Tsoln vs. TA + TB
1. methanol + water
2. ethanol + water
3. acetone + water
4. methanol + ethanol
5. methanol + acetone
6. ethanol + acetone

NOTES
1. Prevent loss of solvent by keeping the
test tube tightly stoppered.
2. Use your palm to determine the
temperature changes immediately after
mixing.
3. Volume readings must be made when
the liquids are at room temperature.

QUESTIONS

1. Determine the type of intermolecular


force of attraction among the same
molecules and among the molecules of
the liquids in the mixture.
2. Correlate intermolecular H-bonding with
heat and volume effects.

31
EXPERIMENT

SPECTRA OF DIFFERENT
ELEMENTS: FLAME TEST

Atoms, ions and molecules can be excited to


higher energy levels through many processes,
including treatment in a flame. The excited
species has a short lifetime (usually 10-6 to 10-9
sec), and relaxation to a lower energy level or
to the ground state takes place with the
release of energy with frequencies
corresponding to wavelengths in the visible
spectrum.

Objects are seen by means of either


transmitted or reflected light. Since only the
transmitted waves reach the eye, the particular
wavelengths correspond to a particular color.
This color is complementary to the color that
would be perceived, if the absorbed light could
be inspected. As in the visible spectrum,
(commonly viewed as rainbows), violet has the
shortest wavelength, hence violet bears the
highest energy, whereas red has the lowest
energy.

MATERIALS AND APPARATUS

Platinum or nichrome wire


Bunsen burner
Dilute HCl
Chloride salts of Cu, K, Li, Ba, Sr, Ca, and Na

PROCEDURE

1. Thoroughly clean a platinum wire by


alternately dipping it into dilute HCl and
holding it in a Bunsen burner flame.
The wire should be cleaned until it does
not color the flame when heated to
redness.
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2. Prepare dilute solutions of chloride
salts listed above and label each
solution.
3. Dip the platinum wire into one of the
solutions and place it at the junction of
the yellow and blue flame. Record the
color imparted to the flame by the
substance.
4. Clean the platinum wire before dipping
it in another solution.
5. Repeat steps 3 and 4 for the rest of the
solutions.

QUESTIONS

1. Why is the wire placed at the junction of


the yellow and blue flame?
2. Why are chloride salts used instead of
any soluble salt?

EXPERIMENT

THE ELECTROMOTIVE SERIES

Metals react to various ionic compounds


differently. One metal may react to an ionic
compound while another may remain
undissolved to the same compound. Their
dissolution is usually due to chemical
reactions. Most metals dissolve with acids to
produce hydrogen gas as a by-product.

The reactivity of metals to different ionic


compounds depends on the nature of the
metals themselves. Some metals can displace
another metal in solution. This is due to the
reduction potential of the metal.

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The electromotive series is a list of metals
arranged according to decreasing reactivity. In
this experiment, the reactivity of some metals
will be compared and the series will be listed
based on the results of the experiment.

MATERIALS AND APPARATUS

Test tube Zn metal 2 M HgCl2


Test tube Cu metal 2 M NaCl
rack
Medicine 2 M H2SO4 2 M CuSO4
dropper
Steel wool 2 M ZnSO4 2 M FeSO4
Mg metal

PROCEDURE

1. Obtain 1-cm strips of Mg, Cu, Zn and


Al. Thoroughly polish each metal to
remove any oxide coating.
2. Place about 2 mL of the following
solutions into separate test tubes:
H2SO4, HgCl2, CuSO4, NaCl, and
FeSO4. Let the tubes stand for 20
minutes.
3. Place a strip of zinc into each test tube.
Record your observations.
4. Repeat the procedure replacing CuSO4
with ZnSO4 and the Zn metal with Cu
metal.
5. Repeat the procedure again, replacing
Zn metal with Mg metal and adding a
test tube containing CuSO4. Tabulate
all results.

QUESTIONS

1. Write out the displacement reactions


involved.
2. On the basis of reactions, list down the
metals, in descending order of their
reactivity.

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EXPERIMENT

SOME ASPECTS OF CORROSION

Corrosion is a chemical or electrochemical


attack on the surface of the metal. The most
common example of corrosion is the rusting of
iron. In a redox reaction, the site where
reduction occurs is referred to as the cathode
and the site where oxidation occurs is referred
to as the anode.

In this experiment, the corrosion of iron will be


observed. The incorporation of a more
oxidizable metal in combination with iron is
done and seen as a way by which the
corrosion of iron is prevented. Incorporation of
a less oxidizable metal on the other hand,
enhances the rate of corrosion of iron.

MATERIALS AND APPARATUS

Colorless gelatin bars 0.1 M K3Fe(CN)6


250-mL beakers 1% phenolphthalein
Zn metal 2 petri dishes
Cu wire Pliers
4 clean 1 ½” (ungalvanized) clean iron nails Sandpaper

PROCEDURE

A. Preparation of Gelatin

1. Boil about 250-mL distilled water. Stir


into the boiling water ½ bar of colorless
gelatin. Heat the mixture with
continuous stirring until the gelatin is
well dispersed. Set aside until the
temperature of the solution reaches
60oC.
2. Add 20 drops of K3Fe(CN)6 into the
solution. Stir thoroughly. Add 1.0 mL of
1% phenolphthalein into the cooled
unsolidified solution before pouring into
the prepared jars.

B. Preparation of Iron Nails


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1. While the gelatin solution is being
prepared, sand the nails to remove the
surface coating. Then prepare the two
petri dishes according to the following
set-up:
a. Petri dish A nail 1: straight
nail 2: bent to a 45o
angle using a pair of
pliers
b. Petri dish B nail 3: with a clean
piece of bare copper wire twisted
around it
nail 4: with a piece of
mossy zinc forced
through the nail

2. Place the nails side by side at the


bottom of the petri dish, making sure
that the nails do not touch each other.
3. Pour the gelatin solution into the
prepared jars taking care that the nails
and metals are covered to a depth of at
least 1.0 cm.
4. Observe the nails in the jar towards the
end of the lab period. Make a properly
labeled diagram of your set-up. Indicate
the colors develop around each nail.
Bring the jars home to make further
observation.

WASTE DISPOSAL

1. Carefully remove the mossy zinc and


copper wire from the nails. Rinse these
well with running water and return to
the instructor.
2. Dispose all nails used in the experiment
into the “Used Nails” container provided
by your instructor.
3. Dispose used gelatin in the “Solid
Waste” container.

QUESTIONS

1. What do the blue ends in the straight


nails represent?
2. What does the pink coloration in the
gelatin solution indicate?
3. Compare the results of the nails in petri
dish A to those in petri dish B.

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a. How does the copper wire affect the
corrosion of the iron nail?
b. Explain the effect of the zinc metal
on the corrosion of the iron nail.

EXPERIMENT

COLLIGATIVE PROPERTIES

A. Freezing Point Depression

A saturated aqueous solution has a freezing


point lower than 0oC at a pressure of 1 atm.
The addition of salt to ice causes the ice to
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melt at a temperature lower that\n its melting
temperature. A cold slushy salt and water
solution, with enough salt to bring the
temperature down to about -14 oC, is
sufficiently cold to freeze an ice cream mixture.

Because it lowers the freezing point of water,


salt is also useful in thawing the ice on roads.
With the advent of home refrigerators and
freezer, it was no longer necessary to use salt
to make homemade ice cream. And for
freezing commercial ice cream, liquid ammonia
is used to lower the temperature.

B. Boiling Point Elevation

The normal boiling point of water is 100oC.


With the addition of salt, the boiling point is
elevated by a few degrees depending on the
amount of salt added.

In this experiment, these two important


colligative properties will be demonstrated.
Practical application of the freezing point
depression will be shown in the making of ice
cream.

MATERIALS AND APPARATUS

(3) 250-mL all purpose cream rock salt


¼ cup condensed milk or sugar plastic cups
1 tsp vanilla extract plastic spoons
tube ice mixing bowl and spoon
flavorings: cocoa, strawberry, etc. 1-2 tsp gelatin powder
toppings: mallows, nuts, etc. thermometer (w/ <0 and >100 oC marks)
distilled water ice cream cans

PROCEDURE

A. Freezing point depression

1. Mix the all-purpose cream, milk or


sugar, vanilla extract and gelatin
extract. When the mixture is well
dispersed, add the desired flavorings.
2. Pour into each cup. Place the cup into
the ice contained in metal cans. Make
sure that the cup is well submerged in
the ice taking care not to contaminate
the ice cream mixture.

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3. Place several spoonfuls of salt into the
ice, taking care not to put some in the
ice cream mixture. To appreciate the
freezing point lowering, monitor the
temperature of the ice slurry from time
to time.

B. Boiling Point Elevation

1. Place 100 mL of distilled water in the


beaker. Place around 28.56 g of salt
into the water until the water is
saturated.
4. Heat the solution and monitor the
temperature from time to time. Notice
the increase in the normal boiling point
of 100oC.

QUESTIONS

Based on the observed temperature


changes, compute the weight of the salt
added to the solution to cause the freezing
point depression and boiling point
elevation. Compare with the actual value.

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