General Chemistry Laboratory Manual

CHEM 16
GENERAL CHEMISTRY I
LABORATORY MANUAL
2017 EDITION
INSTITUTE OF CHEMISTRY
University of the Philippines
Diliman, Quezon City 1101
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General Chemistry Group Institute of Chemistry • University of the Philippines • Diliman

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ACKNOWLEDGEMENT
The 2017 edition of the General Chemistry I Laboratory Manual was developed and finalized through the
collective efforts of the General Chemistry academic group of the Institute of Chemistry, University of the
Philippines, Diliman (IC-UPD). The revised experiments in this laboratory manual reflect the group’s
increasing awareness and commitment to improve the management, storage, and disposal of chemical wastes
generated by our teaching laboratories without drastically diminishing the academic content and quality of
experiments. In fact, this awareness furthers the aims of general chemistry as a major endeavor in the life
sciences.
Thus, IC-UPD as a DENR-registered chemical waste generator complies with the current Philippine laws on
Hazardous Waste Management. Aside from proper waste management, waste minimization is also being done
by doing the experiments in microscale amounts.
The IC-UPD acknowledges the efforts of the following instructors and lecturers who contributed in editing and
revising this General Chemistry I Laboratory Manual - Mr. Jose Intano Jr., Ms. Venus Pondevida, Mr. Ralph
John Ugalino, Mr. Kyle Adrianne Benito, Ms. Lizette Mella, Ms. Michelle Ang, Mr. Jacob Noel Inguito, and
Ms. Ma. Ericka Corazon Itang, Mr. Timothy John Talusan, Mr. Moises Jerome Garrero, Ms. Mae Criste
Fajiculay, Mr. Kenee Kaiser Custodio, Dr. Babeh Dimayacyac-Esleta, and Dr. Allan Yago.
Christine Hernandez, Ph.D.

Director, Institute of Chemistry
University of the Philippines – Diliman

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TABLE OF CONTENTS
Experiment No. Page

Acknowledgement iii
List of Figures v
General Policies vi
Laboratory Safety Guidelines viii
Laboratory Techniques xi
Chemical Nomenclature xvi
List of Common Ions xvii
Significant Figures and Rules in Rounding Off Numbers xx
Writing Net Ionic Equations xxii
Some Generalizations Regarding Strong and Weak Electrolytes xxii
Solubility Guidelines for Common Ionic Compounds in Water xxii
1 Purification of Crude Benzoic Acid by Recrystallization and Sublimation 1
2 Oxidation-Reduction Reactions – Activity Series of Metals and Non-Metals 3
3 Chemical Changes – Reactions of Copper 5
4 Titrimetric Analysis – Determination of Acid Content in Soda and Vinegar 7
5 Qualitative Analysis – Determination of Cations and Anions 9
6 Calorimetry – Determination of Heats of Neutralization 12
7 Paper Chromatography – Separation of Food Dyes 14
8 Dynamic Equilibrium and Heats of Solution 16
9 Distillation of Rubbing Alcohol 18
10 Gases – Testing the Ideal Gas Law 20
11 Colligative Properties of Solutions 22
12 Properties of Acids and Bases – pH, Conductivity, and Relative Strengths of 23
Acids and Bases

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LIST OF FIGURES
Figure Title Page

C-1 Regular filtration techniques xii
C-2 Decantation techniques xii
D-1 Burette preparation xiii
D-2 Titration techniques xiii
F Measurement of liquid samples xiv
H-1 Proper addition of reagents using a dropper xv
H-4 Transferring solids xv
J Smelling vapors xv
1.1 Filtration set-up 2
1.2 Sublimation set-up 2
1.3 Melting point determination set-up 2
4 Titration set-up 7
6 Calorimetry set-up 13
7.1 Chromatographic set-up 14
7.2 Chromatogram 15
9 Simple distillation set-up 18
10 Three possible cases for calculation of P trapped air 20
12 Conductivity set-up 24

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GENERAL POLICIES
1. Failure in the laboratory part means an automatic grade of 5.0 for the course.
2. Strictly no labgown, no goggles, no data notebook  NO EXPERIMENT.
3. No visitors during lab hours unless it is an emergency.
4. No make-up experiment.
5. It is your responsibility to:
a. Maintain a clean locker, glassware, and work area.
b. Check that water outlets within the vicinity of your working area are shut off when not in use.
c. Return floating equipment such as iron clamps, hotplates, pipettes, etc. to their proper places.
d. Check that your locker is locked before leaving the room.
e. Finish all assigned task at least 30 minutes before the end of the class period and devote the remaining
time to cleaning your glassware and work area.
f. Follow proper waste disposal.
g. Present the schematic diagram in your lab notebook for the day’s scheduled experiment to your
instructor prior to the actual experiment day.
Duties of Monitors
Each student will be assigned experiment date(s) when (s)he will be the “Monitor of the Day”. The following
are the duties of the monitors:
1. Arrange the reagents for the day’s experiment properly in a designated area.
2. Distribute all floating equipment.
3. Ensure that at the end of the lab period,
a. all electrical equipment are turned off and unplugged (light, fan, fumehood).
b. all reagent bottles are capped.
c. all iron stands are returned to their proper places.
d. all tabletops are clean and dry, and sinks are free of insoluble waste.
e. all lockers are secured.
Laboratory Notebook
1. All information written in this notebook is to be rendered in ink (i.e., pencils are not allowed). Corrections
may be made by enclosing erroneous information in parenthesis and drawing a straight line across it, then
writing the correct information adjacent to the cancelled one. Do not use correction fluid, eraser, or white
tape.
2. Each leaf is to be page numbered on the upper right hand corner of each right hand page. Left hand pages
are neither to be numbered nor written upon.
3. The first three pages of the notebook will serve as the table of contents chronicling the experiment
performed each day. Follow the format given. Fill up the experiment number, title, and date performed
each time you perform an experiment. There should be blank spaces between main entries.

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Table of Contents
Student’s Name Year/Course

Groupmate Subject/Section
Locker No. Instructor
TABLE OF CONTENTS
Expt. Date Instructor’s

Title Score
No. Performed Signature
1 Purification of Crude Benzoic Acid by
Recrystallization and Sublimation
Pre-lab Report
1. The experimental procedure for the first experiment is written on the fourth page according to the format
specified below.
2. Each succeeding experimental procedure must be written on a new page.
3. This is accomplished individually and presented to the instructor for checking before the start of the
designated experiment.
Date Performed: 1
Experiment No. 1
Purification of Crude Benzoic Acid by Recrystallization and Sublimation
I. Objectives:
II. Diagrams/Figures for special set-ups:
III. Outline/Schematic diagram of procedure:
IV. Special Notes (proper waste disposal, safety precautions):

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LABORATORY SAFETY GUIDELINES
Preparing for laboratory work
To carry out safely and efficiently the laboratory experiments for this General Chemistry course, you need to
prepare a work plan before the actual experiment. This work plan will require you to familiarize the objectives,
as well as the instructions and procedures of the experiment to be carried out. You must also know what safety
precautions to take when doing an experiment. Should you have any questions regarding experiment
procedures, consult your laboratory instructor.
Prescribed Personnel Protective Equipment (PPE)
To ensure your personal safety in the laboratory, wear the prescribed personnel protective equipment.
1. Laboratory safety goggles must be worn at all times anywhere in the laboratory whenever experiments are
being performed. DO NOT WEAR CONTACT LENSES! Corrosive fumes and chemicals could get
underneath your contact lenses and into your eyes. Wearing contact lenses would prevent effective
breathing and flushing of the eyes in case of an accident.
2. Closed shoes should always be worn in the laboratory as protection against possible chemical spills and
broken glass.
3. The prescribed laboratory gowns must be worn at all times when experiments are being performed.
4. Protective face mask is recommended when handling chemicals in the form of powder or in the presence of
chemical fumes.
As an additional safety measure, long hair and loose clothing should be properly secured to avoid interference
in your work.
Safety rules in the laboratory
Immediately report to your laboratory instructor:

1. any major spills, breakages, or accidents in the laboratory;
2. all physical injuries sustained in the laboratory (such as burns and cuts) no matter how trivial they may
seem; and
3. all “near-miss” incidents in the laboratory.
To help prevent laboratory accidents, you should observe the following safety rules:
1. WEAR THE PRESCRIBED PPE. No student is allowed to enter the laboratory and carry out
experiments without donning the complete PPE (safety goggles, laboratory gown, closed shoes, face mask,
as needed). Also, avoid wearing jewelry in the laboratory.
2. KEEP FOOD, DRINKS, AND GUM OUT OF THE LABORATORY. Most chemicals in the laboratory
are poisonous. Eating, drinking, and chewing gum in the laboratory are strictly prohibited.
3. NO SMOKING IN THE LABORATORY. Smoking is strictly prohibited, as some of the laboratory
chemicals are flammable. Flammable chemicals like organic solvents must only be used under the fume
hood.
4. NEVER WORK ALONE. Perform experiments only during the scheduled laboratory period and only
under the supervision of your laboratory instructor.

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5. DO NOT PERFORM UNAUTHORIZED EXPERIMENTS. Only scheduled experiments must be

carried out during your laboratory period. Moreover, no additional experiment procedures or deviations
from the experiment procedures described in this manual, is allowed without the permission of the
laboratory instructor.
6. NEVER REMOVE CHEMICALS FROM THE LABORATORY AND STOCKROOM. The
chemicals are properties of the Institute of Chemistry, UP Diliman. Improper handling and misuse of these
chemicals could pose great health and environmental hazard.
7. NO LOITERING IN THE LABORATORY. Do not play games or engage in horseplay in the laboratory.
Concentrate on performing your experiment.
8. DO NOT LEAVE AN ON-GOING EXPERIMENT SET-UP UNATTENDED.
9. READ THE LABELS. Carefully read the labels of chemical reagent containers – check the formula and
the concentration.
10. HANDLE ALL CHEMICALS WITH EXTREME CAUTION. Know the hazards associated with the
chemicals as well as their physical and chemical properties. Examine the Material Safety Data Sheet
(MSDS) and know where to find specific information on the hazards, toxicology, immediate first aid, and
correct disposal of the substance listed on the MSDS.
a. Most chemicals are corrosive. Exercise caution when handling concentrated acids and ammonia.
Concentrated acids must only be used under the fume hood.
b. Treat all chemicals as potentially dangerous. In case of a chemical spillage, immediately take off any
contaminated clothing and wash off spilled chemicals on the skin or eyes with copious running water
for at least 15 minutes. Consult a physician if needed.
c. Take extra care in handling chemicals in the form of fine dust or powder. It is recommended that you
wear a mask to avoid inhalation of these chemicals. If these dusts or powders come into contact with
the eyes, wash with copious running water continuously for at least 15 minutes. Consult a physician if
needed.
11. BE ORDERLY AND DISPOSE LABORATORY WASTES PROPERLY. Observe cleanliness and
orderliness when working in the laboratory. Follow the general guidelines for “Cleanliness in the
Laboratory” and the “Proper Laboratory Waste Disposal” described below. Some specific laboratory
waste disposal procedures are also described at the end of each experiment.
Cleanliness in the laboratory
Cleanliness in the laboratory is a must. Arrange all the materials needed for the experiment on your tabletop so
you can perform the experiment smoothly. During experimentation, the following should be observed:
1. Avoid contaminating the reagents.

2. Practice the habit of rinsing droppers and rods immediately after use.
3. Refrain from accumulating dirty glassware. Use waiting times (e.g. while heating solutions) to clean
glassware.
4. Always wash or wipe off dirt from reagent bottles.
5. Clean up spills immediately even if it is only water.
6. Wash your hands thoroughly before leaving the laboratory and dry them on a clean towel.

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Proper Waste Disposal
Safety as well as environmental considerations dictates that students should be conscious of proper waste
disposal. Always throw laboratory wastes in their respective waste containers.
1. INORGANIC WASTES. Dispose acids and bases into acid waste container and base waste container,
respectively, to prevent clogging of sinks or premature corrosion of pipes. Excess and waste potassium
permanganate (KMnO4) should also be thrown into inorganic waste containers since this is a powerful
oxidant that may corrode sink pipes.
2. ORGANIC WASTES. Dispose organic wastes into halogenated organic waste containers or non-
halogenated organic waste container.
3. SOLID WASTES. All solids used in experiment procedures (filtration, chromatography, etc.) should be
disposed into contaminated solid waste containers. Other solid wastes should be disposed into the trash bin
available inside the laboratory.
4. BROKEN GLASSWARE. All broken glassware including capillary tubes used in experimental procedures
such as melting point determination, chromatography, etc. should be disposed in broken glassware
container.
Fire safety
Most chemicals used in the General Chemistry laboratory are non-flammable. However, there are solvents such
as ethanol, methanol, and acetone that are flammable. Hence, chemical fire can also occur. There is also a small
risk of electrical fire. If a fire should occur, the first thing to do is to remain calm. Call the attention of your
instructor and leave the laboratory. All laboratory rooms are equipped with a fire extinguisher. Other safety
precautions in case of a fire are given below.
1. Fires in small containers can be extinguished by inverting a small beaker or any other similar equipment
over the burning container. Alternatively, cover the burning container with soaking wet towels. Never use
dry towels.
2. Remove any flammable material such as reagent bottles with flammable chemical from the area of the fire.
3. In case of a person inhaling smoke or toxic fumes, transfer him/her to a well-ventilated area.
4. In case your clothing should catch on fire, use the safety shower.

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LABORATORY TECHNIQUES
One of the aims of a general chemistry course is to teach and train students the proper laboratory working habits
and techniques. These common laboratory techniques are best learned from actual demonstration and constant
reminders. Laboratory work can become more systematic and efficient by following the procedures and safety
guidelines that can lead to successful experimentation. Unnecessary waste of time, effort, and reagents can be
avoided if experimental work is conducted using the following guidelines of laboratory procedures and
techniques.
REMINDER: Always wear prescribed personnel protective equipment (PPE) whenever working in the
laboratory.
A. Filtration
1. Prepare an ordinary filter paper by cutting a square piece of filter paper (adjusted to the size of the
funnel). Fold into half then into quarters. Cut or trim the filter paper for it to have a circular shape.
Make sure that the filter paper is well fitted in the funnel.
2. Open the folded, trimmed filter paper to form a cone, one layer thickness on one side, and three layers
thickness on the other.
3. Cut a small portion from the latter part of the fold. This is to allow continuous flow of air and filtrate.
4. Fit the filter paper into the funnel and moisten its side with water using a glass rod. The edge of the
filter paper must be at least ½ cm lower than the lip of the funnel. At no time must the filter paper
extend above the lip of the funnel.
5. When filtering, guide the liquid from the source beaker with a glass rod, letting the liquid flow by the
thicker side of the filter paper. The tip of the stem of the funnel must touch the sides of the receiving
vessel to avoid spattering and loss of liquid.
B. Precipitation
Precipitation may be used for either separation or identification of mixtures and substances.
1. For separation purposes, precipitation must be complete and the particles of the precipitate sufficiently
large for easy and efficient separation.
a. Add the reagent drop by drop, stirring the mixture thoroughly after each drop. Stop adding the
reagent when formation of the precipitate is no longer observed in the clear supernate.
b. If no precipitate is formed at once, scratch the inside wall of the container using a stirring rod for
about a minute then let the solution stand for a few minutes.
c. To make separation complete, add only a slight excess of the reagent since a large excess may
increase the solubility of the precipitate, or interfere with other tests.
d. Supersaturation, which may cause precipitation to be slow and incomplete, may be avoided by
stirring.
2. For identification purposes, complete precipitation is not necessary.
a. The solution to be tested and the reagent should be absolutely clear.
b. Add the reagent cautiously, and mix well with the solution.
c. Observe the color of the precipitate after it has settled.
C. Separation of the precipitate from the supernate

1. Before filtering, allow the precipitate to settle. Decant the supernate into a prepared filter paper. Add a
small amount of the wash solution to the precipitate and stir.
NOTE: If the precipitate has a tendency to turn colloidal, use a dilute solution of an electrolyte (0.001
M) as wash solution.

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Decant the supernate through the same filter paper. Wash the precipitate again using the same amount
of wash solution, mix thoroughly, and filter. Try to transfer as much precipitate as possible into the
filter paper. Take note that this is a regular filtration process, wherein there is separation of the
supernate from the precipitate and then the precipitate is collected into the filter paper (See figure C-1).
2. However, if the directions indicate that the supernate is to be decanted form the precipitate, this means
that the supernate is to be separated from the precipitate, with the precipitate remaining in the original
vessel. Thus, the supernate is transferred into a new vessel and separated from the precipitate. Wash
the precipitate as many times as possible, taking care not to transfer the precipitate into the filter paper
(See figure C-2).
a. Transfer solid into the filter b. Scrub sides up, down

paper. and around to remove c. Complete the transfer of solid.
residual solid.
Figure C-1. Regular filtration techniques.
a. Decant the supernate. b. Stir the solid to wash. c. Decant the wash liquid.
Figure C-2. Decantation techniques.
D. Titration
1. Preparation of the burettes
The acid burette has a glass stopcock while the base burette has a rubber tubing with a pinchcock. A
burette with a Teflon stopcock may be used for acid or base solutions.
a. Wash the burettes with detergent solution, rinse with tap water, and then rinse with distilled water.
b. Rinse the burette with the solution to be used. (See figure D-1)
c. Fill the burettes with the corresponding solutions.

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2. Titration techniques
Deliver the solution drop by drop while continuously swirling (wrist movement) the solution. (See
figure D-2)
d e
a. A funnel may be used when pouring

solutions into the clean burette;
alternatively, a glass rod may be used. Fill
the burette above the zero mark.
b. Remove the air bubbles at the tip of the
c burette. For the Teflon or glass stopcock,
remove air bubbles by opening it wide for
a few seconds.
c. Refill with the solution to the zero mark
(read lower meniscus).
d. For the rubber tubing stopcock, fold the
tubing and pinch it near the tip.
e. Remove any adhering drops from the
b burette tip.
Figure D-1. Burette preparation.
a. If left-handed, use your right hand to regulate liquid flow

and your left hand to swirl the flask.
b. If right-handed, use your left hand to open and close the
stopcock and your right hand to swirl the flask.
c. Use a white background under the flask to better monitor
any color change in the solution.
Figure D-2. Titration techniques.
E. Test for acidity/basicity

Place a small piece of litmus paper or pH paper on a watch glass. Dip a glass rod in the test solution and
moisten the litmus or pH paper. If the red litmus paper turns blue, the solution is basic. If the blue litmus
paper turns red, the solution is acidic. If a pH paper will be used, compare the color developed against the
scale provided by the instructor.
F. Measurement of liquid and solid samples

In some instances, accuracy in measuring the quantity of the reagents is needed as directed in the
procedure. In many cases, the given volumes of the reagents are only suggestive. The amount of the reagent
to be added depends on the amount of the constituents to be separated or precipitated.
1. One standard drop of a solution is 0.05 mL; thus, 1 mL is equivalent to 20 drops. A “few drops” means
1-2 drops while “several drops” means 3-6 drops.

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2. The quantity of solids is measured with a top-loading balance. Use a watch glass in weighing solids
and not a piece of paper. When measurement does not have to be exact, a spatula may be used. A
heaping spatula-full contains 0.10 to 0.15 g of solid. A “pinch” is about the size of a mongo bean.
3. In filling a series of test tubes with the same volume of test solutions, there is no need to measure the
exact volume of each solution. Fill one test tube with the required volume the fill the other test tubes of
the same diameter to the same level.
There are several types of glassware that can be used for measuring liquids depending on how accurate the
measured volume should be. (See Figure F)
1. Beaker/Erlenmeyer flasks with graduations – measure out volumes accurately up to ± 10 mL.
2. Graduated cylinder – accurate to about ± 0.5 mL.
3. Burettes – accurate to about ± 0.01 mL.
4. Measuring pipettes – one of the most accurate glassware used to measure the desired liquid volume;
accurate to about ± 0.01 mL.
5. Transfer or delivery pipettes – used to transfer an accurately known volume of solution form one
container to another; accurate to ± 0.01 mL.
b
c
a. To avoid parallax error, read lower meniscus at eye level.

b. Proper use of measuring pipette and aspirator; liquid adhering to the tip of the measuring pipette shown be
blown out. In the case of transfer pipettes, the liquid at the tip should not be blown out.
c. Proper measurement of reagents from the reagent bottles into wide-mouthed vessels.
Figure F. Measurement of liquid samples.
G. Heating solutions in a test tube

When heating solutions in test tubes, a hot water bath is recommended. A water bath can be prepared by
filling up a beaker with distilled water to a level that will make the level of the liquid inside the test tube
lower than the level of the liquid outside.
H. Addition of reagents
Keep the reagents pure and preserved against contamination. Any trace of impurity in a reagent may cause
a number of errors in the analysis of your results.
1. In getting reagents from reagent bottles with droppers (Pasteur pipettes), do not allow the tip of the
dropper to come in contact with anything outside the reagent bottle, such as the tabletop. Always hold

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the dropper just above the mouth of the test tube or any other vessel and allow the reagent to fall into
the vessel. Do not let the dropper touch or rest against the inside of the vessel (See figure H-1).
2. Never dip your OWN dropper into the reagent bottle, and do not return any reagent to the bottle.
Figure H-1. Proper addition of reagents using a dropper.
3. If the bottles are equipped with droppers, pour the amount needed into a separate test tube. Never pour
the reagent directly from the bottle to your reaction mixture. This is to avoid contamination of the
reagent with the volatile constituents from the reaction mixture.
4. In getting solid reagents, transfer out the solid from the reagent bottle to a clean dry watch glass and
not on a piece of paper. Add the reagent from the watch glass to your reaction mixture by means of a
clean dry spatula.
Figure H-4. Transferring solids.
I. Mixing
When indicated, mix the reagent mixture thoroughly before drawing any conclusions. To avoid
contaminating the solution, do not cover the test tube with a stopper or finger while shaking.
1. If the solution is less than half of the test tube, it can be mixed by holding the test tube upright between
the palms of your hands and rolling it sufficiently for complete mixing.
2. If the test tube is more than half-full, pour the contents into a small beaker and stir. Stirring is usually
done with a glass rod, using a combination of up and down circulatory motions. Take care not to touch
the sides of the beaker, as you stir the solution.
J. Smelling vapors
Chemical substances should not be inhaled or smelled, unless otherwise instructed. If a substance/solution
is to be smelled, place the container of the substance/solution a few inches away from your face. Using
your other hand, waft the fumes towards you.
Figure J. Smelling vapors

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CHEMICAL NOMENCLATURE
Organic compounds – carbon containing compounds (except carbonates, carbides, oxides of carbon, and
cyanides)
Inorganic compounds – all other compounds
A. Naming cations
1. Cations with one oxidation state – name of element + ion
Example: Na+ is named as sodium ion
2. Cations with two or more oxidation states

a. In the old system of naming, the species with a lower oxidation state uses the suffix –ous while the
species with a higher oxidation state uses the suffix –ic.
Examples: Fe2+ is named as ferrous
Fe3+ is named as ferric
b. The stock system of naming encloses the Roman numeral equivalent of the oxidation state of an
element in parenthesis. Hence, Fe(III) symbolizes the element iron with a +3 oxidation state.
B. Naming anions
1. Anions without oxygen use the suffix –ide
Example: Cl- is named as chloride
2. Oxoanions (oxygen containing anions)

a. An element that forms only one oxoanion uses the suffix –ate
Example: CO32- is named as carbonate
b. An element that forms two oxoanions
 With less number of oxygen atoms makes use of the suffix –ite
Example: NO2- is named as nitrite
 With more number of oxygen atoms makes use of the suffix –ate
Example: NO3- is named as nitrate
c. An element that forms more than two oxoanions makes use of the following prefixes and suffixes:
hypo- -ite is used by the oxoanion with the lowest number of oxygen atoms
-ite
-ate
per- -ate is used by the oxoanion with the highest number of oxygen atoms
Examples: ClO- is named as hypochlorite
ClO2- is named as chlorite
ClO3- is named as chlorate
ClO4- is named as perchlorate
3. Hydrogen containing oxoanions – hydrogen + oxoanion name

Examples: HCO3- is named as hydrogen carbonate (also known as bicarbonate)
HSO4- is named as hydrogen sulfate, also known as bisulfate
C. Naming ionic compounds

Ionic compounds are named by giving the cation name + anion name
Examples: NaCl is named as sodium chloride
FeCl3 is named as ferric chloride or iron(III) chloride

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D. Naming molecular compounds

The number of atoms in molecular compounds is indicated by Greek prefixes (mono, di, tri, etc.). The same
holds true for binary compounds, which are ionic or molecular compounds of two different elements.
Examples: PCl5 is named as phosphorus trichloride
N2O is named as dinitrogen monoxide
HCl(g) is named as hydrogen chloride
NOTE: The prefix mono is never used in the first element of a molecular compound and rarely used in the
second element of a molecular compound. For example, CO is names as carbon monoxide.
E. Naming acids
1. Binary acids are compounds in aqueous solution and make use of the prefix hydro- and the suffix –ic
acid.
Example: HCl(aq) is named as hydrochloric acid
2. Oxyacids are named by giving the name if the element + suffix (depending on the name of the
oxoanion) + acid
 -ite of anion is replaced by –ous acid
 -ate of anion is replaced by –ic acid
Examples: H2SO3 is named as sulfurous acid
H2SO4 is named as sulfuric acid
 This also holds true for acids with elements of more than two oxoanions.
Examples: HClO is named as hypochlorous acid
HClO2 is named as chlorous acid
HClO3 is named as chloric acid
HClO4 is named as perchloric acid
LIST OF COMMON IONS

Monoatomic Cations
Charge Formula Name
H+ Hydrogen
Li+ Lithium
Na+ Sodium
+1 K+ Potassium
Rb+ Rubidium
Cs+ Cesium
Ag+ Silver
Mg2+ Magnesium
Ca2+ Calcium
Sr2+ Strontium
+2
Ba2+ Barium
Zn2+ Zinc
Cd2+ Cadmium
+3 Al3+ Aluminum
Polyatomic Cations
Charge Formula Name
NH4+ Ammonium
+1
H3O+ Hydronium

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Metals with Variable Charges

Element Charge Formula Old Name Stock Name
+3 Sb3+ Antimonous Antimony(III)
Antimony
+5 Sb5+ Antimonic Antimony(V)
+2 Cr2+ Chromous Chromium(II)
Chromium
+3 Cr3+ Chromic Chromium(III)
+2 Co2+ Cobaltous Cobalt(II)
Cobalt
+3 Co3+ Cobaltic Cobalt(III)
+1 Cu+ Cuprous Copper(I)
Copper
+2 Cu2+ Cupric Copper(II)
+2 Fe2+ Ferrous Iron(II)
Iron
+3 Fe3+ Ferric Iron(III)
+1 Au+ Aurous Gold(I)
Gold
+3 Au3+ Auric Gold(III)
+2 Pb2+ Plumbous Lead(II)
Lead
+4 Pb4+ Plumbic Lead(IV)
+2 Mn2+ Manganous Manganese(II)
Manganese
+3 Mn3+ Manganic Manganese(III)
+2 Ni2+ Nickelous Nickel(II)
Nickel
+3 Ni3+ Nickelic Nickel(III)
+1 Hg22+ Mercurous Mercury(I)
Mercury
+2 Hg2+ Mercuric Mercury(II)
+2 Sn2+ Stannous Tin(II)
Tin
+4 Sn4+ Stannic Tin(IV)
Monoatomic Anions
Charge Formula Name
H- Hydride
F- Fluoride
-1 Cl- Chloride
Br- Bromide
I- Iodide
O2- Oxide
S2- Sulfide
-2
Se2- Selenide
Te2- Telluride
N3- Nitride
-3 P3- Phosphide
As3- Arsenide
-4 C4- Carbide

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Polyatomic Anions
Charge Formula Name
CH3COO- Acetate
N3- Azide
OH- Hydroxide
CNO- Cyanate
CN- Cyanide
HCO3- Hydrogen carbonate or Bicarbonate
H2PO3- Dihydrogen phosphite
H2PO4- Dihydrogen phosphate
HS- Hydrogen sulfide
HSO3- Hydrogen sulfite or Bisulfite
HSO4- Hydrogen sulfate or Bisulfate
NO2- Nitrite
NO3- Nitrate
-1 MnO4- Permanganate
SCN- Thiocyanate
ClO- Hypochlorite
ClO2- Chlorite
ClO3- Chlorate
ClO4- Perchlorate
BrO- Hypobromite
BrO2- Bromite
BrO3- Bromate
BrO4- Perbromate
IO- Hypoiodite
IO2- Iodite
IO3- Iodate
IO4- Periodate
CO32- Carbonate
CrO42- Chromate
Cr2O72- Dichromate
HPO32- Hydrogen phosphite or biphosphite
HPO42- Hydrogen phosphate or biphosphate
-2
MnO42- Manganate
C2O42- Oxalate
O22- Peroxide
SO32- Sulfite
SO42- Sulfate
AsO33- Arsenite
AsO43- Arsenate
-3
PO33- Phosphite
PO43- Phosphate

xx
SIGNIFICANT FIGURES AND RULES IN ROUNDING OFF NUMBERS
Significant figures are defined as all of the digits that are “certain” together with the first unknown digit. It
indicates the probable uncertainty in an experimental measurement. It is also important in calculations; hence,
care must be taken to determine the appropriate number of significant figures in the final answer.
Exact numbers, on the other hand, are measurements that are made without the use of any measuring
instrument. It also includes defined numbers. Exact numbers have an infinite number of significant figures and
do not affect accuracy of the calculation or precision of the expression.
The following are the rules used to determine the number of significant figures:
1. Non-zero digits are always significant.
2. Zero is significant when it is between two non-zero digits.
3. Only the final zero or trailing zero in the decimal portion of a number is significant. Zeros between the
decimal point and the non-zero digits serve only as placeholders. They do not involve measurement
decisions; thus they are NOT significant.
Example: 0.0030 has only 2 significant figures
Examples of trailing zeroes in a whole number:

200 has 1 significant figure
2.0 x 102 has 2 significant figures
25,000 has 2 significant figures
200.0 has 4 significant figures
Other examples:
7.09 x 10-5 has 3 significant figures
91,600 has 3 significant figures
In calculations, the following are the rules used to determine the number of significant figures in the final
answer:
1. Addition and Subtraction

The sum or difference can be no more precise than the least precise number involved in the mathematical
operation. Hence, the final answer will contain the same number of decimal places as the one with the least
number of decimal places in the original numbers.
Example: 4.5 - 1.258 = 3.2
2. Multiplication and Division

The number of significant figures is determined after the calculation and is equal to the smallest number of
significant figure.
Example: 4.135 x 2.4 = 9.9

xxi
3. Multiple Operations
The number of significant figures in the final answer is determined by determining the number of
significant figures after each operation.
Example: (2.34 - 1.2) x 0.105 = 0.12
1.1
4. Logarithm Problems
a. For the log of a number, the number of digits to the right of the decimal point in the answer equals the
number of significant digits in the original number.
Examples: log 453.2 = 2.6563
log 3.8 x 1027 = 27.58
b. For the antilog of a number, the number of significant digits in the answer equals the number of digits
to the right of the decimal in the original number.
Examples: antilog 1.709 = 51.2
antilog 38.5 = 3 x 1038
Rules in Rounding Off Numbers
1. Determine what the last reported digit should be, according to the significant figure rules presented above.
2. Consider the digit to the right of the last reported digit.
3. If the digit to the right of the last reported digit is less than 5, then leave the last reported digit unchanged
and discard all digits to the right.
Example: Round off 1.342 to 3 significant figures  1.34
4. If the digit to the right of the last reported digit is greater than 5 then increase the last reported digit by one
and discard all digits to its right.
Example: Round off 1.346 to 3 significant figures  1.35
5. If the digit to the right of the last reported digit is exactly 5 then add one to the reported digit if the reported
digit is an odd number, and leave it unchanged if it is even. However, if it is not exactly 5, then add one to
the reported digit.
Examples: Round off 1.355 to 3 significant figures  1.36
Round off 1.345 to 3 significant figures  1.34
Round off 1.34501 to 3 significant figures  1.35
Other examples:
The following numbers are rounded off to 3 significant figures:
3.521  3.52
3.528  3.53
3.25501  3.26
3.25499  3.25
3.245  3.24
3.255  3.26

xxii
WRITING NET IONIC EQUATIONS
1. Write ionic formula for strongly ionized substances (strong electrolytes) in solution.
Examples: NaOH (aq) is written as Na+(aq) + OH-(aq)
HCl (aq) is written as H+(aq) (or H3O+(aq)) + Cl-(aq)
Na2SO4 (aq) is written as 2 Na+(aq) + SO42-(aq) and NOT as Na22+ + SO42-
2. Write molecular formula for elements, solids, gases, and non-electrolytes.
Examples: I2 (g), Zn (s), CO2 (g), HCl (g), CHCl3 (l) or (g), CCl4 (l) or (g)
3. Write molecular formula for weak electrolytes in solutions.
Examples: H2O(l), NH3(aq), CH3COOH(aq), HCN(aq), HgCl2(aq), H2SO4 (concentrated), Pb(CH3COO)2(aq)
4. Write molecular formula for slightly soluble substances or precipitates.
Examples: MgCO3(s), AgCl(s), BaSO4(s)
5. Omit spectator ions in the net ionic equation.
Example: sodium hydroxide + hydrochloric acid
NaOH (aq) + HCl (aq)  H2O (l) + NaCl (aq)
Na+(aq) + OH-(aq) + H+(aq) + Cl-(aq)  H2O(l) + Na+(aq) + Cl-(aq)
Na+(aq) and Cl-(aq) are spectator ions and hence omitted.
Net ionic equation: H+(aq) + OH-(aq) )  H2O(l)
SOME GENERALIZATIONS REGARDING STRONG AND WEAK

ELECTROLYTES
1. Most salts are strongly ionized.

EXCEPTIONS: HgCl2, CdI2, CdCl2, Hg(CN)2, Pb(CH3COO)2 are weakly ionized.
2. Most acids are weakly ionized.
EXCEPTIONS: The common strong acids: HNO3, H2SO4 (1st ionization), HI, HBr, HCl, HClO3, HClO4.
3. Most bases are weakly ionized.
EXCEPTIONS: The hydroxides of the alkali metals (Group IA) and those of the heavier alkali earth metals
(Group IIA) (i.e. Ca2+, Sr2+, and Ba2+).
SOLUBILITY GUIDELINES FOR COMMON IONIC COMPOUNDS IN WATER*
Soluble Compounds Important Exceptions

Compounds containing NO3-
None
CH3COO-
Cl-, Br-, I- Compounds of Ag+, Hg22+, Pb2+
SO42- Compounds of Sr2+, Ba2+, Hg22+, Pb2+
Insoluble Compounds Important Exceptions

Compounds containing S2- Compounds of NH4+, alkali metal cations, Ca2+, Sr2+,
OH- Ba2+
CO32-
Compounds of NH4+, alkali metal cations
PO43-
*from Chemistry The Central Science. 8th Edition by Brown, Lemay, and Bursten

1
EXPERIMENT 1: PURIFICATION OF CRUDE BENZOIC ACID BY

RECRYSTALLIZATION AND SUBLIMATION
Recrystallization is one of the most important methods used to purify solids. It involves dissolving an
impure sample in a hot solvent and filtering this solution while hot (also called hot filtration). The resulting
filtrate is then cooled to form larger and purer crystals, thus the technique’s name. This purification method
heavily depends on a solvent’s ability to differentiate the compound of interest (solute) from other sample
components (impurities) based on their differing solubilities. Thus, choosing an appropriate solvent is crucial in
recrystallization. An ideal solvent should have the following properties:
1. It should readily dissolve the solute at high temperatures but only sparingly at room temperature.
2. It should dissolve the impurities even at room temperature, such that only the solute recrystallizes upon
cooling.
3. It should be sufficiently volatile to hasten the drying of the purified crystals.
A difficulty often encountered in recrystallization is the failure of the solute to recrystallize. This frequently
happens when the concentration of the solute is too high (supersaturated solution) or when an impurity prevents
recrystallization. In such cases, techniques such as adding a small crystal of the pure substance (also called
seeding) or scratching the inner walls of the container with a glass rod may be used. If the above methods fail
to bring about recrystallization, the solution is probably unsaturated. It is, therefore, heated further to remove
the excess solvent.
In practice, the recrystallization procedure should be repeated until a constant melting point of relatively
narrow range is obtained. The melting point is a physical property that can be used to identify a substance and
to assess its purity. A narrow temperature range of 0.5 to 1.5 ̊C is observed when a solid compound is pure. On
the other hand, when the solid compound is contaminated, the melting point decreases, and the melting point
range widens.
Alternatively, sublimation can be used for the purification of impure solids. It is a reversible physical
process where solid substances are directly converted to the vapor phase when heated without the intermediate
appearance of a liquid state. For sublimation to occur, the solid must have an exceptionally high vapor pressure
at a temperature below its melting point to avoid passing through the liquid state. Though not all solids can be
purified by sublimation and despite its low percent recovery, the method yields crystals of very high purity and
does not require a solvent.
In this experiment, crude benzoic acid samples will be purified using recrystallization and sublimation. For
recrystallization, water will be used as the solvent. Furthermore, the melting point will be determined to
evaluate the purity of the benzoic acid obtained from the two techniques.
MATERIALS AND APPARATUS

Crude benzoic acid Ice bath
Charcoal Oil bath
Vials Capillary tubes
Filter papers Hot plate
250 mL Erlenmeyer flasks Watch glass
100 mL graduated cylinder Pasteur pipette
Stirring rod Hot plate
PROCEDURE
A. Recrystallization
Weigh 0.25 g of crude benzoic acid in a 250 mL Erlenmeyer flask. Add 20 ml distilled water, and boil for
1-2 minutes while stirring (Note: Do not let the sample dry up!). Remove the Erlenmeyer flask from the

2
hotplate, and add a pinch (same as the size of a mongo bean) of charcoal. Stir the mixture then gently heat to
boiling.
Filter the hot solution through a fluted filter paper into another 250
mL Erlenmeyer flask containing about 3 mL of hot water. The receiving
flask should be set on a hot plate to sustain the heat (Figure 1.1). Allow
the resulting hot filtrate to cool slowly to room temperature without
disturbance before setting it in an ice bath.
Collect the recrystallized benzoic acid by cold filtration. Wash the
crystals with a minimal amount of cold water to remove adhering mother
liquor. Spread the filter paper on a watch glass, and allow to air dry.
Transfer the crystals to a previously weighed vial. Report its weight and
% recovery.
Figure 1.1. Filtration set-up.
B. Sublimation
Weigh about 0.10 g crude benzoic acid into a 50-mL beaker. Cover the
mouth of the beaker with a filter paper, and secure the cover using a rubber
band. Place the beaker in a water bath such that about 1/3 of the beaker is
immersed and that the filter paper remains dry. Heat the water bath to
100°C (Figure 1.2)
Continue heating for at least an hour until needle-like crystals deposit
on the filter paper and on the sides of the beaker. Carefully remove the
filter paper, and scrape the sublimate into a previously weighed vial.
Report the weight and the % recovery of pure benzoic acid.
C. Melting point determination

Pulverize the sample by placing the dry benzoic acid crystals on a Figure 1.2. Sublimation set-up.
watch glass and crushing them with a spatula or with the end of a test tube.
Mound the pulverized sample and press the open end of the melting point
capillary tube into the sample against the surface of the watch glass.
Lightly tap the sealed end of the tube on the tabletop. Introduce more
samples into the tube until the sample fills about 2-4 mm height (Figure
1.3)
Place 25 ml of oil in a dry 50 ml beaker. Insert a thermometer through
a cork, placing the cork near the top of the thermometer. Attach the
melting point tube containing the sample to the thermometer by means of
a thin strip of rubber tubing.
A second melting point tube with the sample can be attached to the
other side of the thermometer. Heat the oil bath strongly until the
temperature is 10-15°C below the known melting point. Then, heat gently
using a low temperature setting so that the oil bath rises at a rate of about
3°C per minute. As soon as a droplet of liquid forms in the tube (start of
melting), record the temperature. As soon as the last trace of solid has Figure 1.3. Melting point determination
liquefied (end of melting), record the temperature reading. set-up.
WASTE DISPOSAL
1. Any unrecrystallized benzoic acid should be recovered by allowing the mother liquor to air-dry. Place the
crystals in a vial, and submit the vial to the instructor.
2. Used oil may be disposed of in the “Used Oil” container.
3. Dispose used capillary tubes in “Broken Glassware” container.

3
EXPERIMENT 2: OXIDATION-REDUCTION REACTIONS – ACTIVITY SERIES

OF METALS AND NON-METALS
Oxidation-reduction (redox) reactions are simultaneous reactions involving changes in oxidation number
due to loss or gain of electrons. Oxidation corresponds to an increase in the oxidation number and loss of
electrons. Reduction, on the other hand, corresponds to a decrease in the oxidation number and gain of
electrons.
The oxidation state of an atom or ion is defined as the number of electrons gained or lost in a chemical
reaction. For example, in the reaction:
1
Na(s) + Cl2 (g) → NaCl(s)
2
The sodium atom lost an electron to form the sodium cation (Na+) and the chlorine atom gained an electron
to form the chloride ion (Cl-). Hence, in the ionic compound, NaCl, the oxidation number of Na is +1 and the
oxidation number of Cl is -1.
Now, consider the following reaction:
H2 (g) + Cl2 (g) → 2HCl(g)
The covalent molecule, HCl, is formed. Although neither element has completely “gained” or “lost” an
electron, it has oxidation numbers based on differences in their electronegativities. The electrons in the bond are
completely assigned to the more electronegative atom. Since chlorine is more electronegative than hydrogen,
the electron pair in the bond is assigned to chlorine, and is assumed to “gain” an electron, while H “lose” an
electron; the oxidation numbers of H and Cl in the compound are +1 and -1, respectively.
The assignment of oxidation number (O. N.) to atoms in covalently bonded molecules or ions requires
knowledge on the structure and electronegativities of atoms, and is based on a certain set of rules, as follows:
1. The oxidation number of an atom in a free element is zero.
2. In compounds, the following elements will usually show the given common oxidation numbers:
A. Group 1 and H except in hydrides (O.N. is -1) +1
B. Group 2 +2
C. B and Al +3
D. F -1
E. Cl, Br, and I (not bonded to O) -1
F. O except in peroxides (O. N. is -1) and superoxides (O. N. is -1/2) -2
3. Balance O and H as follows:
In acidic medium:
 To the oxygen deficient side, add 1 mole of H2O; add 2 moles of H+ to the other side (for every
mole of H2O added on the oxygen deficient side)
 To the hydrogen deficient side, add 1 mol of H+
In basic medium:
 To the oxygen deficient side, add 2 moles of OH-; add 1 mole of H2O to the other side (for every
2 moles of OH- added on the oxygen deficient side)
 To the hydrogen deficient side, add 1 mole of H2O; add 1 mole of OH- to the other side (for every
one mole of H2O added on the hydrogen deficient side)
4. Balance the net charges of each half reaction by adding electrons to the side deficient in negative
charge.
5. Multiply each half reaction by a multiple that will make both half reactions have the same number of
electrons, when necessary.
6. Add the half reactions and simplify.
7. Check if the reaction is balanced (the number of each kind of atoms, as well as the charge, should be
the same on both sides of the reaction).

4
For example, consider the oxidation of the iodide ion (I-) by acidified permanganate solution.
I(aq) + MnO4(aq) → I2(aq) + Mn2+
- -
(aq)
Steps 1 to 4:
-
Oxidation half reaction 2I(aq) → I2(aq) + 2e-
MnO4(aq) +8H+(aq) +5e- → Mn2+
-
Reduction half reaction (aq) +4H2 O(l)
-
Step 5: 10I(aq) →5I2(aq) +10e-
2MnO-4(aq) +16H+(aq) +10e- → 2Mn2+
(aq) +8H2 O(l)
10I(aq) +2MnO4(aq) +16H+(aq) → 5I2(aq) + 2Mn2+

- -
Step 6: (aq) +8H2 O(l)
Step 7: Check
Right Left
Atoms 10 I, 16 H, 2 Mn, 8 O 10 I, 16 H, 2 Mn, 8 O
Charge +4 +4
The balanced redox equation is 10I(aq) +2MnO4(aq) +16H+(aq) →5I2(aq) +2Mn2+
- -
⸫ (aq) +8H2 O(l) .

Cu metal 0.1 M ZnSO4 0.1 M Na2SO3 toluene
Zn metal 0.1 M H2SO4 0.1 M KMnO4 3 M H2SO4
Iron nails (not galvanized) 0.1 M KCl 6 M NaOH Test tubes
0.1 M FeSO4 0.1 M KBr I2 (saturated solution) Spot plate
0.1 M CuSO4 0.1 M KI Br2 water
PROCEDURE
A. Activity of Metals
Place 5 drops each of 0.1 M CuSO4, 0.1 M FeSO4, and 0.1 M H2SO4 in separate wells on a spot plate. Drop
a small piece of mossy zinc. Record any change in each solution and metal.
Place 5 drops each of 0.1 M ZnSO4, 0.1 M FeSO4, and 0.1 M H2SO4 in separate wells on a spot plate. Drop
a 1 cm long Cu wire. Record any change in each solution and metal.
Place 5 drops each of 0.1 M ZnSO4, 0.1 M CuSO4, and 0.1 M H2SO4 in separate wells on a spot plate. Drop
a small, clean iron nail. Record any change in each solution and metal.
B. Activity of Non-Metals
Place 1 mL each of 0.1 M KCl and 0.1 M KI in separate test tubes. Add 1 mL of toluene. Shake and
observe. Add 1 mL of Br2 water dropwise, shaking the test tube well after each addition. Note the color of the
two layers.
Place 1 mL each of 0.1 M KCl and 0.1 M KBr in separate test tubes. Add 1 mL of toluene. Shake and
observe. Add 1 mL of saturated I2 dropwise, shaking the test tube well after each addition. Note the color of the
two layers.
C. Reaction between SO32- and MnO4- in different media
To 1 mL of 0.1 M Na2SO3, add 2 drops of 0.1 M KMnO4. Describe the result. Do not add excess
permanganate. Excess permanganate has been added if the pink color persists. Record your observations.
Acidify 1 mL of 0.1 M Na2SO3 with 3 M H2SO4; then add a few more drops of acid in excess. Add 2 drops
of 0.1 M KMnO4. Observe the color change. Do not add excess permanganate.
Repeat previous procedure but add 6 M NaOH instead of 3 M H2SO4 until the solution is basic.
WASTE DISPOSAL
1. Dispose solutions containing KMnO4 into the “Inorganic Waste” container.
2. Solutions of Br2 and I2 with toluene must be separated with a separatory funnel before disposing into
“Inorganic Waste” and “Halogenated Organic Waste” containers, respectively.
3. Dispose used copper, zinc, and iron nails into the “Inorganic Waste” container.
4. Dispose H2SO4 solutions into the “Acid Waste” container.

5
EXPERIMENT 3: CHEMICAL CHANGES – REACTIONS OF COPPER
A chemical change involves the change in chemical composition of a substance resulting from a chemical
reaction. It is usually characterized by observable physical evidence including absorption or emission of heat,
formation of precipitate, evolution of gas, or a change in color of the solution or precipitate. Chemical changes
can be classified into four types depending on which kind of chemical reaction is involved in the process:
1. Synthesis or Combination A+B→C
2. Decomposition AB → A + B
3. Single displacement or replacement AB + C → CB + A or AC + B
4. Double displacement or replacement AB + CD → AD + CB
In this experiment, a series of chemical changes involving copper will be observed. Based from the
observations, different compounds of copper can be identified, and chemical changes can be written into their
balanced chemical equations and classified into their type of chemical reaction. In addition, the mass of the final
product will also prove or disprove if the Law of Conservation of Mass applies for this experiment.

0.100 M Cu(NO3)2 250 mL Erlenmeyer flask Test tubes
6.00 M NaOH 100 mL graduated cylinder Evaporating dish
3.00 M H2SO4 100 mL beaker Vial
Zn dust 5 mL volumetric pipette Filter paper
6.00 M NH3 Pasteur pipettes Iron ring
0.100 M Zn(NO3)2 Stirring rod Iron stand
6.00 M HCl Watch glass Hot plate
Litmus paper Funnel Top loading balance
PROCEDURE
A. Precipitation of copper(II) hydroxide
Pipette 5.00 mL 0.100 M Cu(NO3)2 into a 100-mL beaker containing 25 mL distilled water. Add
approximately 1.00 mL 6.00 M NaOH dropwise while constantly stirring the solution.
Allow the precipitate to settle, and then test if the solution is alkaline by placing a piece of red litmus paper
on a dry watch glass and moistening it with the solution using a stirring rod. If it is not yet alkaline, add 10
drops NaOH to the solution. Record any change in color of the precipitate and supernate.
B. Formation of copper(II) oxide

Using a hot plate, heat the mixture (from A) for about 2 minutes while stirring constantly to prevent
bumping (formation of a large bubble in a locally overheated area of the liquid in the beaker), which may result
to loss of sample. Take note of the change in the color of the precipitate.
C. Conversion of copper(II) oxide to copper(II) sulfate

Allow the precipitate (from B) to settle until the supernate is clear. Decant the supernate through a filter
paper into an Erlenmeyer flask. Wash the precipitate in the beaker with 10 mL distilled water. Let the
precipitate settle and decant the wash water through the same filter paper into the same Erlenmeyer flask.
Repeat the process until the precipitate is washed four times. (NOTE: Avoid putting all the precipitate into the
filter paper)
Wash the same filter paper by adding 1.00 mL 3.00 M H2SO4 dropwise, catching the filtrate into the beaker
containing the copper (II) oxide precipitate. Dissolve the precipitate by swirling or stirring the mixture. Wash

6
the filter paper with 5 mL distilled water, catching the wash water into the same beaker. Record your
observations.
D. Reduction of copper(II) ions to metallic copper

CAUTION:
 Wear FACE MASK when handling zinc dust to prevent inhalation of the particles.
 Be careful not to let zinc dust into your eyes. If it comes into contact with your eyes, wash with copious
running water continuously for at least 15 minutes. Consult a physician if needed.
With constant stirring, gradually add zinc dust in small amounts until the solution turns colorless (NOTE:
Stir until evolution of gas is no longer observed before adding more zinc.). Record your observations.
To test the completeness of the reaction (reduction of copper(II) ions to metallic copper), add few drops of
solution (from previous process) into a test tube containing about 5 drops 6.00 M NH 3. If a colored solution is
obtained, gradually add more zinc dust into the beaker with constant stirring. Repeat this process until the test
with NH3 gives a colorless solution. Record your observations.
A control solution, for comparison, may be prepared by adding a drop of 0.100 M Cu(NO 3)2 to 2 drops 6.00
M NH3 and 1 mL distilled water in a test tube. This indicates the presence of copper(II) ions. In another test
tube, add a drop of 0.100 M Zn(NO3)2 to 2 drops of 6.00 M NH3 and 1 mL distilled water. This shows the color
of a solution with zinc(II) ions. Record your observations
After the reaction is complete, decant the supernate. Wash the precipitate in the beaker twice with 10-mL
portions of distilled water. Decant the wash water after each washing. (NOTE: Be careful not to lose any of the
solids) To the precipitate, add 20 mL distilled water. Slowly add 1.00 mL 6.00M HCl and stir the contents.
Record your observations.
When no more change is observed, allow the precipitate to settle. Decant the acidic supernate. Wash the
precipitate twice with 20-mL portions of distilled water. Decant the wash water after each washing.
Transfer the metallic copper to a previously weighed filter paper by washing it out from the beaker using
distilled water. Discard the filtrate and wash water.
Place the filter paper in between pieces of dry filter paper and press it to remove most of the water. Unfold
the filter paper and place it on a watch glass and air dry in your locker until the next laboratory period.
5. Oxidation of copper
If the product from the previous process is not yet black, place the filter paper with solid on an evaporating
dish and heat it on a hot plate. Observe what happens to the solid and record your result.
Weigh the solid and filter paper on a top-loading balance and record the mass obtained. After weighing,
transfer the product into a labeled vial and submit to your instructor.
WASTE DISPOSAL
1. Dispose used litmus paper and filter papers into the “Contaminated Solid Waste” container.
2. Dispose all combined filtrate and washings into the “Inorganic Waste” Container.
3. Dispose excess zinc dust into the “Inorganic Waste” Container.
4. Dispose all acidic supernates into the “Acid Waste” Container

7
EXPERIMENT 4: TITRIMETRIC ANALYSIS – DETERMINATION OF ACID

CONTENT IN SODA AND VINEGAR
Titrimetric analysis is a technique in which a solution of known concentration (titrant) is made to react with
a known quantity of the substance being analyzed (analyte). The titrant is added in small increments to the
analyte solution using a burette until an indicator, which is added to the solution at the start of titration, gives a
sharp color change. This change in color indicates the endpoint of the titration. The endpoint is a close
approximation of the equivalence point, which is the point when all of the analyte has completely reacted with
the titrant. An example of an indicator is phenolphthalein, which changes in color depending on whether the
solution is acidic (colorless) or basic (pink). The titration setup is shown in the figure below.
The exact concentration of the titrant is determined through a process called standardization. During
standardization, a primary standard is weighed with high accuracy, dissolved and titrated with the solution until
endpoint is reached. A primary standard is a stable solid of high purity and high molecular weight, whose
reaction with the substance to be standardized is known. An example of a primary standard is potassium
hydrogen phthalate (KHP) which is used for the standardization of NaOH.
For a titrimetric analysis to be feasible, (1) the reaction between the standard and analyte must be known,
(2) the reaction between the reactants must be reasonably fast, (3) the reaction must proceed quantitatively to
completion and, (4) there must be some method or substance available to detect the endpoint.
In this experiment, the amount of acidic component of a soda and vinegar sample will be determined using
titrimetric analysis involving acid-base neutralization reactions.

potassium hydrogen phthalate (KHP) 1 mL volumetric pipette
0.1 M NaOH 20 mL volumetric pipette
1% phenolphthalein 250 mL Erlenmeyer flasks
white vinegar 50 mL base burette
colorless soda sample burette clamp
iron stand
PROCEDURE
A. Preparation of burette
Rinse a previously cleaned base burette with approximately 4 mL
of titrant solution (0.10 M NaOH), allowing some of the liquid to run
through the tip of the burette. Repeat the rinsing process two or more
times, discarding the NaOH used each time.
Fill the burette with 0.10 M NaOH, taking care that no air bubble
is trapped in the space below the pinchcock. Clamp the burette onto
the iron stand. Adjust the volume reading to or below the zero mark.
Touch the tip of the burette onto an iron stand. Adjust the volume
reading to or below the zero mark.
Touch the tip of the burette to the side of the beaker to remove
any hanging drop. Allow the solution to stand for a few minutes and
observe for any leakage. Look at the lower meniscus of the solution
in the burette at eye level, then read and record the initial volume of
the solution (Figure 1.4).
Figure 4. Titration set-up.

8
B. Standardization of NaOH solution (Class Experiment)

Note the weight and % purity of the pre-weighed KHP standard provided by the instructor. Add about 50
mL of distilled water and swirl to mix and dissolve the solid. Add 2-3 drops of phenolphthalein indicator.
Titrate with the NaOH solution until it gives a permanent faint pink color. This is the endpoint of the titration.
Record the final volume of the solution in the burette.
Perform two additional trials. Remember to record the initial and final volumes of the solution in the
burette.
Solve for the average molarity of the NaOH solution; express this in four significant figures.
C. Analysis of acetic acid (CH3COOH) in a vinegar sample

Pipette 1.00 mL of white vinegar into a clean Erlenmeyer flask. Dilute with approximately 50 mL of
distilled water and add 2-3 drops of phenolphthalein indicator. Swirl to mix. Titrate with the standard NaOH
solution until endpoint is reached. Remember to record the initial and final volumes of the solution in the
burette. Perform another trial.
Use the average molarity of NaOH obtained in the standardization step to calculate the average molarity of
acetic acid in the vinegar sample. Express the answer in three significant figures.
D. Analysis of carbonic acid (H2CO3) in a soda sample

Pipette 20.00 mL of soda into a clean Erlenmeyer flask. Dilute with approximately 50 mL of distilled water
and add 2-3 drops of phenolphthalein indicator. Swirl to mix. Titrate with the standard NaOH solution until
endpoint is reached. Remember to record the initial and final volumes of the solution in the burette. Perform
another trial.
Use the average molarity of NaOH obtained in the standardization step to calculate the average molarity of
carbonic acid in the soda sample. Express the answer in three significant figures.
WASTE DISPOSAL
1. Collect the NaOH rinsings into a beaker, dilute with plenty of water and flush directly down the sink with
copious running water.
2. Dilute all titrated solutions with plenty of water and flush directly down the sink with copious running
water.

9
EXPERIMENT 5: QUALITATIVE ANALYSIS – DETERMINATION OF CATIONS

AND ANIONS
Analytical chemistry is divided into two main facets: quantitative analysis and qualitative analysis.
Quantitative analysis deals with the determination of the amount of a substance found in a given sample, while
qualitative analysis involves finding out the identity of a substance or substances composing a particular
sample. The identification of these substances can only be accomplished if the experimenter has prior
knowledge of their properties, both physical and chemical.
This experiment aims to perform tests that help determine the presence or absence of ions in aqueous
solutions, and it will be done in two phases. First, the properties and reactivity of each of the five cations (Cu 2+,
Fe3+, Ca2+, Zn2+, and NH4+) and seven anions (CO32-, PO43-, SO42-, Cl-,Br-, I-, and NO3-) in various qualitative
tests found in the Procedure section will be observed. Formation and dissolution of precipitates, stratification or
layering of mixtures, evolution of gases and color changes will be observed. These results will then be used to
correctly identify unknown ions present in a solution.

0.1 M Cu(NO3)2 1.0 M Na2CO3 0.1 M MgCl2
0.1 M FeCl3 18.0 M H2SO4 1 M HNO3
0.1 M CaCl2 6.0 M H2SO4 1 M NaOH
0.1 M Zn(NO3)2 0.01 M KMnO4 1 M NH3
0.1 M NH4NO3 FeSO4 (freshly prepared) 1 M CH3COOH
0.1 M NaI Toluene Pasteur pipettes
0.1 M NaBr 0.1 M KSCN Test tubes
0.1 M NaSCN 0.1 M K3Fe(CN)6 Evaporating dish
0.1 M NaNO3 0.1 M K4Fe(CN)6 Watch glass
0.1 M Na3PO4 0.1 M (NH4)2C2O4 Litmus paper (red and blue)
0.1 M Na2SO4 0.1 M Ba(NO3)2
PROCEDURE
I. QUALITATIVE ANALYSIS OF KNOWN IONS
Prepare five clean and dry test tubes for the qualitative test for anions (Part A) and seven test tubes for the
qualitative test for anions (Part C).
TEST FOR CATIONS

A. Elimination Tests
Place five drops each of the Cu2+, Fe3+, Ca2+, Zn2+, and NH4+ cation test solutions separately into five test
tubes. Use fresh cation solutions for tests A-1 to A-2 and B-1 to B-5. Take note of all color changes (whether in
the precipitate or supernatant) as well as formation and dissolution of precipitates.
A-1. Add a drop of 1.0 M NaOH into each of the test solutions. If a precipitate forms, continue adding
NaOH dropwise until precipitation is complete. If not, stop adding NaOH. Complete precipitation is
reached if addition of more NaOH does not produce any more precipitates. Note the color and type of
precipitate formed. Continue adding excess base to the precipitates (about five to ten drops more).
A-2. Repeat A-1 using 1.0 M NH3 (instead of 1.0 M NaOH).

10
B. Confirmatory Tests
These tests are performed to verify the identity of the ions obtained in the elimination tests. There are
visible results already obtained in A which may be used to confirm an ion’s identity. Only one confirmatory test
needs to be done for each cation.
B-1. Copper(II) ion, Cu2+: The deep blue complex obtained by mixing Cu2+ solution in A-2 with excess NH3
is enough confirmation of the presence of the Cu 2+.
B-2. Iron(III) ion, Fe3+: Add two drops of 0.1 M KSCN to five drops of the fresh Fe 3+ test solution. A blood
red FeSCN2+ complex will be formed. Another test for Fe3+ is the formation of a dark blue precipitate,
KFeIIIFeII(CN)6, when two drops of 0.1 M K4Fe(CN)6 is added to five drops of the fresh test solution.
B-3. Calcium(II) ion, Ca2+: To five drops of the Ca2+ test solution, add two drops of 0.1 M (NH4)2C2O4. A
white precipitate will be obtained.
B-4. Zinc(II) ion, Zn2+: To five (5) drops of the Zn2+ test solution, add two drops of 0.1 M K 3Fe(CN)6. A
yellow precipitate, KZnFe(CN)6, will be obtained. A white precipitate, K2Zn3[Fe(CN)6]2, will be
formed upon addition of 0.1 M K4Fe(CN)6.
B-5. Ammonium ion, NH4+: Moisten two small pieces of litmus paper (one red, one blue) with distilled
water and allow these to stick to the underside of a watch glass. Place 10 drops of the NH 4+ test
solution in an evaporating dish. To the NH4+ test solution, add five drops of 1.0 M NaOH. Immediately
cover the evaporating dish with the watch glass, with the side on which the litmus papers are attached
facing the solution. Observe as the red litmus paper turns blue. Do not allow the solution to touch the
litmus paper.
TEST FOR ANIONS

C. Elimination Tests
Place five drops each of the CO32-, SO42-, PO43-, I-, SCN-, Br-, and NO3- anion test solutions separately into
seven test tubes. Use fresh anion solutions for tests C-1 to C-3 and D-1 to D-7, unless stated otherwise. Take
note of all color changes (whether in the precipitate or supernatant) as well as formation and dissolution of
precipitates. In addition, take note of color changes in the toluene and aqueous layers.
C-1. Add two drops of 0.1 M Ba(NO3)2 into each test solution. If a precipitate is formed, continue the
addition of Ba(NO3)2 dropwise until precipitation is complete. Decant as much supernatant as possible
after the precipitate has settled. Set the precipitates aside for the confirmatory tests in Part D.
Note: Perform C-2 and C-3 using only the anion test solutions that did not form precipitates with Ba(NO 3)2.
Handle toluene with utmost care!
C-2. Add two drops of 1.0 M HNO3 into each test tube containing the fresh anion test solution. To this
mixture, add three drops of 0.1 M Fe(NO3)3 and five drops of toluene. Shake well and allow the
immiscible layers to stratify. Record the color of each layer. Add a few more drops of toluene if the
color of the top layer is difficult to see.
C-3. To the fresh anion test solution, add one drop of 0.01 M acidified KMnO 4 and five drops of toluene.
Shake well and allow the mixture to stratify. Record the color of each layer. If the KMnO 4 solution is
not yet acidified, first add two drops of 1.0 M HNO 3 before adding one drop of 0.01 M KMnO4 into
the test solution.
D. Confirmatory Tests
Like in the confirmatory tests for cations, these tests are performed to verify the identity of the anions
determined through the elimination tests. There are also visible results already obtained in C which may be used
to confirm an ion’s identity. Only one confirmatory test needs to be done for each anion.

11
D-1. Carbonate ion, CO32-: Add 1.0 M CH3COOH dropwise until the precipitate from C-1 is completely
immersed. Observe as the precipitates dissolve with effervescence or bubbling. The formation of
bubbles indicates the reaction of CO32- in solution with CH3COOH and its subsequent conversion to
CO2 gas.
D-2. Phosphate ion, PO43-: Add 1.0 M CH3COOH dropwise until the precipitate from C-1 is completely
immersed. Observe as the precipitates dissolve without effervescence or bubbling. Another
confirmatory test for PO43- is through the addition of one drop of 0.1 M MgCl 2 to five drops of the
PO43- test solution. The reaction produces a white precipitate, Mg3(PO4)2.
D-3. Sulfate ion, SO42-: Add five drops of 1.0 M CH3COOH to the precipitate from C-1. Notice that the
sulfate precipitate of barium remains undissolved after the addition of acetic acid.
D-4. Iodide ion, I-: A pink or pinkish-red color of the toluene layer in C-2 confirms the presence of I- in the
test solution. I2 in toluene is pink.
D-5. Thiocyanate ion, SCN-: The deep red aqueous solution obtained in test C-2 is the complex FeSCN2+.
D-6. Bromide ion, Br-: A yellow or orange toluene layer obtained in C-3 verifies the presence of Br- in the
test solution. This color indicates dissolved Br2 in the toluene layer.
D-7. Nitrate ion, NO3-: Acidify five drops of the test solution by adding six drops of 6.0 M H 2SO4. Add
eight drops of the freshly prepared FeSO4 solution. Tilt the test tube to 60o and allow two drops of 18.0
M H2SO4 to slowly slide down the side of the test tube and into the solution. DO NOT SHAKE THE
CONTENTS OF THE TEST TUBE. Very slowly, bring the test tube into an upright position. Note the
formation of the brown ring at the interface of the concentrated acid and the solution. It may take a few
minutes for the brown ring to become visible. The addition of the H 2SO4 solutions must be done under
the fume hood. (The presence of iodide, bromide, or thiocyanate ions interferes in this test.)
II. ANALYSIS OF UNKNOWN IONS IN SOLUTION

Record all available pertinent information regarding the unknown solution. Dilute this solution with
distilled water, at your discretion. Dilution increases the volume of available unknown solution for analysis, but
this decreases the number of moles of component ions per drop of the diluted test solution. Lesser number of
moles of the component ions may hinder in the proper observation of the positive results for the elimination or
confirmatory tests. Ideally, five drops of the test solution is used for every qualitative test (elimination or
confirmatory).
WASTE DISPOSAL
1. Dispose all solutions of inorganic salts by diluting them with plenty of water and flushing them directly
down the sink with copious running water. Dilute acidified and basic solutions with water when needed,
before flushing them down the sink.
2. Dispose excess concentrated acids into the acid waste container.
3. Dispose solutions containing KMnO4 into the inorganic waste container, or to the KMnO 4 waste container,
if available.
4. Dispose all undissolved solids into the solid waste container. Place and wrap these precipitates in a filter
paper or tissue before throwing them into the solid waste jar.
5. Pour all mixtures with layering into a separatory funnel. Separate the toluene layer from the aqueous layer.
Dispose the toluene layer into the halogenated organic waste jar. Dispose the aqueous layer into the
inorganic waste jar.

12
EXPERIMENT 6: CALORIMETRY – DETERMINATION OF HEATS OF

NEUTRALIZATION
The calorimeter is a device used to measure heat changes that accompany a physical or a chemical process.
It usually consists of a container that is surrounded by an insulating vessel. A thermometer is inserted into the
container to monitor the changes in temperature inside the calorimeter.
The heat that is released or absorbed by a process is used to heat or cool any substance that is in contact
with the reaction, such as the solvent, the thermometer, the air, and the calorimeter. Being an adiabatic system,
the Law of Conservation of Energy applies to a calorimeter:
heat lost/gained by the process = heat gained/lost by the calorimeter
or
qreaction = -qcalorimeter
That is, when a process is carried out inside a calorimeter, the heat lost or gained by the process (q reaction) is
equal to but opposite in sign to the heat gained or lost by the calorimeter (q calorimeter). The magnitude of q is the
same on both sides of the equation because of the Law of Conservation of Energy. However, the sign is
opposite because the heat lost by the process is gained by the calorimeter, and vice versa.
The heat measured from a process conducted under constant pressure is referred to as enthalpy, ΔH. The
enthalpy of a reaction with n mole(s) of limiting reagent (LR) is equal to
q𝑟𝑒𝑎𝑐𝑡𝑖𝑜𝑛
∆Hrxn =
nLR
A process or reaction may be classified as either exothermic or endothermic, depending on the sign of
qreaction or ΔH. Exothermic processes release heat and thus have negative values for q reaction and ΔH. Endothermic
processes, on the other hand, absorb heat and thus have positive values for q reaction and ΔH.
In this experiment, an improvised constant pressure calorimeter is constructed using a test tube surrounded
by Styrofoam. The calorimeter and everything external to the process has a certain heat capacity, denoted as
Ccal. Using the known enthalpy for the following reaction:
H+ (aq) + OH- (aq)  H2O (l) ΔHrxn = -55.85 kJ/mol
and the observed changes in temperature (ΔT), the heat capacity of the calorimeter, C cal, may be determined.
qcalorimeter −q𝑟𝑒𝑎𝑐𝑡𝑖𝑜𝑛 −∆Hrxn × nLR
Ccal = = =
∆T ∆T ∆T
This Ccal may then be used for the subsequent calorimetric determination of ΔH for the neutralization
reaction of a different acid-base system.

1.00 M HCl 6” test tube
1.00 M NaOH 10 mL volumetric pipette
1.00 M HNO3 5 mL measuring pipette
Styrofoam cube/ball rubber stopper
thermometer
PROCEDURE
A. Construction of Improvised Calorimeter
Carve a hole at the center portion of the Styrofoam cube/ball so that a 6” test tube could fit inside
completely. Do the same to the rubber stopper and insert the thermometer. Afterwards, seal the 6” test tube with
the rubber stopper. The thermometer must be positioned halfway inside the test tube.
Insert the sealed 6” test tube into the carved hole of the Styrofoam cube/ball. Only the rubber stopper with
the inserted thermometer should be visible on the surface of the Styrofoam cube/ball (Figure 6).

13
B. Calibration of the Calorimeter

Pour 10.0 mL of 1.00 M HCl into the test tube of the
constructed calorimeter. Wait until the temperature reading in
the thermometer becomes stable. Record the temperature of the
1.00 M HCl solution. This is your T initial. Remove the top of the
calorimeter (which consists of the rubber stopper and the
thermometer). Add 5.00 mL of 1.00 M NaOH into the test tube.
Immediately cover the calorimeter and swirl the contents
gently.
Record the temperature every after 30 seconds while
swirling occasionally. Continue taking the temperature-time
data until the temperature is constant or decreasing at a constant
rate. This temperature is your T final.
Make a graph of temperature (in °C) vs. time (in sec). Figure 6. Calorimetry set-up.
Compute for the heat capacity of the calorimeter, Ccal.
C. Determination of the Enthalpy of Reaction of Nitric Acid and Sodium Hydroxide

Pour 10.0 mL of 1.00 M HNO3 into the test tube of the constructed calorimeter. Wait until the temperature
reading in the thermometer becomes stable. Record the temperature of the 1.00 M HNO 3 solution. This is your
Tinitial. Remove the top of the calorimeter (which consists of the rubber stopper and the thermometer). Add 5.00
mL of 1.00 M NaOH into the test tube. Immediately cover the calorimeter and swirl the contents gently.
Record the temperature every after 30 seconds while swirling occasionally. Continue taking the
temperature-time data until the temperature is constant or decreasing at a constant rate. This temperature is your
Tfinal.
Make a graph of temperature (in °C) vs. time (in sec). Compute for the ΔH rxn of nitric acid and sodium
hydroxide using the calorimeter’s heat capacity computed in part B.
WASTE DISPOSAL
Dilute all solutions with tap water and flush directly down the sink with copious running water.

14
EXPERIMENT 7: PAPER CHROMATOGRAPHY – SEPARATION OF FOOD DYES
Chromatography is technique used to separate components of a mixture based on differences in

intermolecular forces of attraction. It makes use of a mobile phase which is used to carry the components of the
mixture and the stationary phase, the structure in which the components of the mixture is carried to. Depending
on the polarity, the components are carried by the mobile phase at different rates through the stationary phase.
Paper chromatography is a chromatographic technique where the stationary phase is the water bound to the
cellulose of the paper while the mobile phase is the solvent which can either be polar or nonpolar. In this
technique, the chromatogram, which is the visual output, is shown in the stationary phase itself.
Given a specific stationary and mobile phase, a component will always have the same retention factor (Rf).
The retention factor is defined as the fraction of a component which is retained in the mobile phase. It can be
expressed as follows:
𝑑𝑖𝑠𝑡𝑎𝑛𝑐𝑒 𝑡𝑟𝑎𝑣𝑒𝑙𝑙𝑒𝑑 𝑏𝑦 𝑠𝑜𝑙𝑢𝑡𝑒 𝐴
RfA =
𝑑𝑖𝑠𝑡𝑎𝑛𝑐𝑒 𝑡𝑟𝑎𝑣𝑒𝑙𝑙𝑒𝑑 𝑏𝑦 𝑠𝑜𝑙𝑣𝑒𝑛𝑡
In the experiment, the separation of food dyes in M&M’s samples using 1% NaCl as solvent will be
investigated. The retention factors will be calculated and will be used to qualitatively describe the components
of the samples.

M&M’s samples 250 mL beaker
filter paper watch glass
spot plate pencil
Pasteur pipette ruler
capillary tubes
PROCEDURE:
Place each candy (green, red, blue, orange, and
brown M&M’s) on a spot plate and put a drop of distilled
water on each and let the samples sit for about 30-60
seconds.
While waiting for the M&M’s extract to concentrate,
prepare the chromatographic chamber in a 250-mL
beaker. Add the mobile phase (1% NaCl) to the beaker to
a depth of about 0.5 cm. Place a strip of filter paper (7 x
8 cm) inside the beaker. Cover the beaker with a watch
glass and wait until the developing solvent (mobile
phase) saturates the filter paper (Figure 7.1).
Cut a sheet of filter paper (14 x 8 cm). Draw a light
pencil line across the paper about 0.8 cm from the top
and bottom of the sheet. Using a capillary tube, apply a
small spot of the M&M’s extract on the pencil line near Figure 7.1. Chromatographic set-up.
the bottom of the paper (allow about 2.0 cm distance
between each spot) as shown in figure 7.2.

15
Let each spot dry and reapply the color

concentrate (do this for 2 more times).
Note: Avoid overloading! Put a label below each

spot indicating the color of the candy.
Roll the paper to form a cylinder and use a

stapler to join the edges of the cylinder. Place the
rolled chromatographic paper into the chamber
and ensure that the spots are not below the
solvent level and the paper is not touching the
sides of the beaker. Cover the chamber with a
Figure 7.2. Chromatogram.
watch glass.
Do not disturb the beaker for 5-10 minutes. Monitor the solvent level from time to time. When the
developing solvent rises up to a height approx. 5 mm below the pencil line at the top of the cylinder, remove the
chromatogram from the chamber and open it flat. Allow the chromatogram to dry for 2-5 minutes.
Mark the spots and note their colors. Measure the distance travelled by the solvent. Measure the distances
travelled by each color. Calculate the retention factor, Rf, of each of the spots, and compare their retention
factor values.
WASTE DISPOSAL
1. Dispose the developing solvent (mobile phase) directly down the sink with copious running water.
2. Dispose used capillary tubes in the “Broken Glassware” container.

16
EXPERIMENT 8: DYNAMIC EQUILIBRIUM AND HEATS OF SOLUTION
For the chemical reaction:

aA + bB ⇌ cC + dD
where the small letters represent the coefficient and the capital letters represent the chemical species in a
balanced chemical reaction, the system is said to be at dynamic equilibrium when the rates of the forward and
backward reactions are equal. When stress is applied to this system at equilibrium, the system responds in such
a way to reduce the stress. This is Le Chatelier’s principle.
A. Acid-Base Equilibria
In this experiment, pH is seen as a factor that can affect equilibrium. Anthocyanins encompass the range of
red, violet, and blue pigments in plants. This experiment demonstrates the change in color of anthocyanins as a
function of pH.
This ability of anthocyanins to change color at different pH levels is related to the concept of visual
indicators such as phenolphthalein, which changes color with varying pH. With phenolphthalein, the solution
changes color from colorless to pink as an acid solution is made more basic and back to colorless as a basic
solution is made more acidic.
B. Solubility Equilibria
Physical changes can also involve heat changes. As an example, the dissolution of a solute in a solvent will
typically involve measurable heat changes. This heat change is known as the heat of solution, ΔH soln.
The dissolution process involves at least three energy changes:

1. Solute particles are separated from the solid mass or move apart to make space for solvent
particles (energy is absorbed, ΔH1)
2. Solvent particles move apart to make space for dissolved solute (energy is absorbed, ΔH2)
3. Solute and solvent particles are attracted to one another (energy is released, ΔH 3)
The total heat of the solution, ΔHsoln will be the sum of all three energy changes and will either be
endothermic (ΔHsoln = +), exothermic (ΔHsoln = -) or athermic (ΔHsoln = 0). This value will be dependent on the
relative strengths of the interparticle forces of attraction between like and unlike particles.
For most solids dissolving in water, the sum of the first two terms is greater than the third and thus
dissolving is usually endothermic and solubility generally increases with increasing temperature. When ΔH soln
becomes highly positive, it is often because the solute and solvent are dissimilar (i. e., they have “unlike”
interparticle forces of attraction). In this extreme case, the solute becomes immiscible or insoluble in the
solvent. The general rule therefore “like dissolves like” is a good basis for predicting the solubility of solutes in
solvents.
Volume changes may also accompany heat changes. Stronger forces of attraction between unlike particles
result in an overall contraction in the volume of solution; otherwise an overall expansion in the volume of
solution is observed.
This experiment will explore the solubility of several solutes in different solvents. Heat and volume
changes that accompany the mixing process will also be observed, as well as the effect of temperature on
solubility.

17

NaCl acetone 5 mL measuring pipettes
naphthalene methanol 10 mL measuring pipettes
glycerol 1 M HCl 10 mL volumetric flasks
iodine crystals 1 M NaOH hot plate
1.0 M KI NH4Cl crystals test tubes
ethanol Pasteur pipette ice bath
toluene graduated cylinder pH paper
PROCEDURE
A. Acid-Base Equilibria
Cut into small pieces 15 g well-washed camote tops, red gumamela flowers, boat of Moses, or red
bougainvillea flowers. Add approximately 100 mL water and boil for 15 minutes to extract the pigment. Filter
the extract using a filter paper.
Note the color of the extract and then determine its pH. To 20 ml of the extract, add 3 drops of 1 M HCl.
Record any color changes and determine the pH. Repeat the last step but this time add 1 M NaOH instead of
HCl.
B. Solubility Equilibria
B-1. Effect of the nature of solute and solvent
Pipet 0.50 mL each of distilled water, ethyl alcohol, and toluene in three separate test tubes. To each of the
solution, add a pinch of NaCl. Shake the test tube and let it stand. Observe and record results as soluble of
insoluble. Repeat the procedure using pulverized naphthalene instead of NaCl.
Pipet 0.50 mL each of distilled water, ethyl alcohol, and toluene in three separate test tubes. To each of the
solution, add a drop of glycerol. Shake the test tube and let it stand. Observe and record results as miscible or
immiscible.
Pipet 0.50 mL distilled water into two separate test tubes. To each test tube, add a small iodine crystal then
shake. To one solution, add a drop of 1.0 M KI and shake. Compare the colors of the solutions and record your
observation.
B-2. Effect of Temperature

Place 1 mL distilled water into a test tube. Add NH4Cl into each test tube until no more salt dissolves. Note
any changes in the temperature. Heat the mixture gently and observe what happens. Repeat the same steps for
Ca(OH)2 but instead of heating the mixture, put it in an ice bath.
B-3. Heat and Volume Changes

Prepare three clean and dry 10-mL volumetric flasks and label them with (1), (2), and (3). Pipette 5 mL of
water into (1), 5 mL of ethanol into (2), and 5 mL of methanol into flask (3). Fill up the rest of the flask to mark
with methanol (1), acetone (2), and ethanol (3). Cover and shake to mix the two liquids. Note the changes in
temperature and the final volume of the solution.
WASTE DISPOSAL
1. Dispose organic solvents, including glycerol and naphthalene into the “Non-halogenated Organic Waste”
container.
2. Dispose other solutions by flushing directly down the sink with copious running water. Dilute solutions
before flushing when needed.

18
EXPERIMENT 9: DISTILLATION OF RUBBING ALCOHOL
The separation of components of a mixture is usually based on differences in the physical properties of its
components. Examples of separation methods include filtration (based on differences in physical state),
centrifugation (based on differences in density), chromatography (based on differences in solubility and ability
to be adsorbed), and distillation (based on differences in volatility or boiling point of the mixture components).
Distillation is usually used to separate two miscible compounds in a mixture so that one component can be
isolated from the mixture. The mixture is heated until the more volatile component evaporates, while the less
volatile component remains in the mixture. The vaporized component is then condensed separately in order to
isolate this component as a liquid.
Several distillation techniques have been devised, but the most basic type is called simple distillation,
which is typically used for two miscible liquids with boiling points that are below 150 °C and far from each
other.
In this experiment, simple distillation is performed on a sample of rubbing alcohol in order to isolate the
alcohol from its mixture with water.

Boiling chips or sticks Two (2) rubber tubings
Simple distillation apparatus ice bath
Rubber stopper (with hole) graduated cylinder
PROCEDURE
Prepare the simple distillation setup as shown in Figure 9. Your instructor will assist you in constructing it.
Figure 9. Simple distillation set-up.
Obtain a round bottom flask that will serve as the distilling flask. Fill this flask with 20 mL of the rubbing
alcohol sample, and then add 2 to 3 pieces of boiling chips or boiling sticks. Boiling chips (small porcelain
chips) or boiling sticks (tiny glass capillaries) are added to prevent bumping. They should never be added to a
hot liquid.
Iron clamps may be used to secure the round bottom flasks, and a rubber stopper with a hole should be
inserted to the top opening of the three-way adapter. Use a rubber tubing for each of the water outlet and inlet,

19
making sure that the water flows into the bottom of the condenser’s cooling jacket and out from the top. Insert
the thermometer into the rubber stopper hole such that its bulb is placed just below the side arm of the three-
way adapter.
Turn the water supply on and check the water flow through the condenser. Check that all ground glass
joints fit well.
Place the distilling flask into a hot water bath and slowly heat the flask until its contents are gently boiling.
Obtain the experimental boiling point of the alcohol. Maintain the temperature at about 82 to 84 °C (for
isopropyl alcohol) or about 78 to 80 °C (for ethyl alcohol). The vapors and condensate will pass through the
side arm of the three-way adapter and into the condenser, where most of the vapor will condense into liquid and
will finally drip from the adapter into the receiving flask.
Once the distillate starts to accumulate in the receiving flask, wait until about 1 mL of distillate is collected.
Discard this distillate, and then collect the remaining fraction that distills at the boiling point of the alcohol.
Measure the volume of the distillate (not including the first 1 mL), and then calculate for its percent recovery. In
calculating the percent recovery, take into account the original percentage of alcohol in the rubbing alcohol
sample. Allow the entire setup to cool before dismantling it.
WASTE DISPOSAL
Dispose of the rubbing alcohol distillate into the non-halogenated organic waste container

20
EXPERIMENT 10: GASES – TESTING THE IDEAL GAS LAW
Gas is a state of matter where molecules are separated by large distances and in random movement. It fills
up its container, adopting both the shape and volume of the container.
The behaviors of gases are based on relationships among measurable parameters: pressure (P), temperature
(T), volume (V) and amount of gas (n). Gas laws illustrate the relationships among these parameters, which are
summarized in the table below.
Gas Law Statement Equations

Boyle’s Law For a fixed amount of gas at a constant temperature, pressure is 1
inversely proportional to volume. 𝑃 = 𝑘( )
𝑉
𝑃1 𝑉1 = 𝑃2 𝑉2
Charles’ Law For a fixed amount of gas at a constant pressure, volume is 𝑉 = 𝑘𝑇
directly proportional to the absolute temperature. 𝑉1 𝑉2
=
𝑇1 𝑇2
Avogadro’s Law For a fixed temperature and pressure, volume is directly 𝑉 = 𝑘𝑛
proportional to the amount of gas. 𝑉1 𝑉2
=
𝑛1 𝑛2
Ideal Gas Law Combination of above simple gas laws using universal gas
𝑃𝑉 = 𝑛𝑅𝑇
constant, R
The experiment illustrates the use of Ideal Gas Law in the analysis of magnesium ribbon. The number of
moles of the gas produced can be calculated from the experimental data of pressure, volume and temperature.
The volume reading of trapped air may exhibit any one of the three cases shown below.
Figure 10. Three possible cases for calculation of Ptrapped air.
Calculations of Ptrapped air depend on which one of these three cases is observed,
ℎ
Case A 𝑃𝑡𝑟𝑎𝑝𝑝𝑒𝑑 𝑎𝑖𝑟 = 𝑃𝑏𝑎𝑟 − (1)
13.6
Case B 𝑃𝑡𝑟𝑎𝑝𝑝𝑒𝑑 𝑎𝑖𝑟 = 𝑃𝑏𝑎𝑟 (2)
ℎ
Case C 𝑃𝑡𝑟𝑎𝑝𝑝𝑒𝑑 𝑎𝑖𝑟 = 𝑃𝑏𝑎𝑟 + (3)
13.6
where Ptrapped air is the pressure of gas trapped in the eudiometer, P bar is the barometric pressure and h is the
height difference (mm) between the water levels inside and outside the eudiometer.
For all cases, the pressure of gas produced in dry conditions can be calculated as
𝑃𝑑𝑟𝑦 𝑎𝑖𝑟 = 𝑃𝑡𝑟𝑎𝑝𝑝𝑒𝑑 𝑎𝑖𝑟 − 𝑃𝑤𝑎𝑡𝑒𝑟 𝑣𝑎𝑝𝑜𝑟 (4)
where Pdry air is the pressure of gas produced in dry conditions and P water vapor is the pressure of water vapor at
specified temperature.

21

6.00 M HCl Mg ribbon measuring pipette
eudiometer thermometer 400 mL beaker
PROCEDURE
Place 10.0 mL of 6.0 M HCl into a eudiometer partially filled with distilled water. Add water to fill the
eudiometer to the brim. Cover the mouth of the eudiometer with your finger and invert into a glass jar that is
two-thirds filled with water. Quickly insert the folded Mg ribbon, approximately 0.02-0.03 g, into the
eudiometer, taking care that it does not stick to the sides of the tube.
When the reaction has stopped, allow five minutes for the system to attain the same temperature as
surroundings before reading the volume of enclosed gas. Record the volume of enclosed gas, the height
difference between the water levels inside and outside the eudiometer, and the temperature of the water outside
the eudiometer. Take note of the case observed.
From the data obtained, calculate the number of moles of gas evolved and the mass of the Mg ribbon
sample. Assuming 100% purity of the ribbon, compare the calculated mass of Mg with pre-weighed Mg (%
error).
WASTE DISPOSAL
Dilute HCl with plenty of water and flush directly down the sink with copious running water.

22
EXPERIMENT 11: COLLIGATIVE PROPERTIES OF SOLUTION
Colligative properties are properties of solutions which depend on the concentration of the non-volatile
solutes. These properties refer to physical property changes of solutions such as freezing point depression
(FPD), boiling point elevation (BPE), vapor pressure lowering (VPL) and osmotic pressure (Π).
FPD and BPE are expressed, respectively, as follows: ∆𝑇𝑓 = −𝑖𝐾𝑓 𝑚 and ∆𝑇𝑏 = 𝑖𝐾𝑏 𝑚, where ∆𝑇𝑓 and ∆𝑇𝑏
are the changes in freezing point and boiling point, respectively; 𝐾 and 𝐾𝑏 are the freezing point and boiling
point constants for particular solvents; and 𝑚 is the molality of the solution.
The van’t Hoff factor, i, is the ratio of the actual concentration of particles in the solution and the calculated
concentration based on the amount of solute. For non-electrolytes, the value i is 1. For strong electrolytes in
dilute concentrations, the value of i is equal to the number of ions present in a single electrolyte particle (e.g.
NaCl has i = 2). For weak electrolytes, value of i varies on the initial concentrations of the solute as well as the
identity of the solute.
The experimental van’t Hoff factor can be calculated by dividing the experimental ∆𝑇𝑓 or ∆𝑇𝑏 by the
expected ∆𝑇𝑓 or ∆𝑇𝑏 when the value of i = 1 (non-electrolyte):
∆𝑇𝑓,𝑒𝑥𝑝𝑒𝑟𝑖𝑚𝑒𝑛𝑡𝑎𝑙
𝑖=
∆𝑇𝑓,𝑛𝑜𝑛−𝑒𝑙𝑒𝑐𝑡𝑟𝑜𝑙𝑦𝑡𝑒

rock salt test tubes
ice tubes or cubes 250 mL beakers
110 ˚C thermometers 400 mL beakers
hot plate
PROCEDURE
A. Freezing Point Depression
Prepare an ice-salt water bath by filling a 400 mL beaker with crushed ice, rock salt and a small amount of
tap water. Fill one-third of a 6-inch test tube with distilled water and insert a thermometer. Cool the test tube in
ice-salt water bath and record the temperature-time data at 30-second intervals. Stir the contents of the test tube
using the thermometer. Continue taking the temperature until the water has frozen. Record the freezing
temperature. NOTE: If the temperature drops below -2.0°C, supercooling has occurred. Add a small fragment of
ice into the test tube. The temperature should rise abruptly and then level off. Record the resulting temperature
as the freezing point.
Prepare a 0.65 molal NaCl solution by dissolving the appropriate mass of NaCl (FW=58.44 g/mol) in 10.0
mL distilled water (d= 1.00 g/mL).
Using the same method described above, determine the freezing point of the NaCl solution and obtain ΔT I
for the NaCl solution. Calculate the van’t Hoff factor for the NaCl solution (K f, water= 1.86°C/m).
Repeat the entire procedure using 1.10 molal NaCl solution.
B. Boiling Point Elevation

Determine the boiling point of distilled water. Prepare 1.50 m rock salt solution in a 250 mL beaker by
dissolving the appropriate amount of NaCl in 50 mL distilled water. Heat the solution and monitor the
temperature of the solution. Record the constant temperature at which the solution boils. Calculate the van’t
Hoff factor for the NaCl solution (Kb, water= 0.512°C/m).
Repeat the entire procedure using 2.50 m rock salt solution.
WASTE DISPOSAL
Dispose all salt solutions in the sink with copious running water.

23
EXPERIMENT 12: PROPERTIES OF ACIDS AND BASES — pH, CONDUCTIVITY,

AND RELATIVE STRENGTHS OF ACIDS AND BASES
Electrolyte solutions can conduct electricity because they contain charged species called ions. These ions
come from the dissociation of ionic salts into positively charged cations and negatively charged anions when
they are dissolved in water. The conductivity of a solution depends on the number and kind of ions between
electrodes. Some ions are better conductors than others. Also, the greater the number of ions, that is, the greater
the electrolyte concentrations, the larger the conductivity. Strong electrolytes are salts that are completely
dissociated/ionized in solution. Weak electrolytes are incompletely dissociated/ionized in solution.
Nonelectrolytes do not ionize in solution.
Acid and base solutions are particularly important classes of electrolyte solutions. They ionize in solution,
usually forming H+ and OH−. According to Arrhenius, acids are substances bearing H+ while bases are those
substances bearing OH−. Brønsted-Lowry, on the other hand, described acids as proton donors whereas bases as
proton acceptors. In another way, Lewis defined acids as electron acceptors where bases as electron donors.
pH and pOH are measures of the acidity or basicity of a solution and is mathematically defined as being
equal to –log [H+] and –log [OH-], respectively. An acid is any substance that increases the hydrogen ion
concentration ([H+]) in aqueous solution while a base is one that increases the hydroxide ion concentration
([OH-]) in aqueous solution. Hence, the following conditions can be observed:
[H+] > [OH-] acidic solution
[H+] < [OH-] basic solution
[H+] = [OH-] neutral solution
One of the general properties of acids and bases is their ability to displace weaker acids and weaker
bases, respectively, from their corresponding salts. For instance, if the following reaction proceeds to a greater
extent towards the formation of the product,
HA(aq) + B−(aq) ⇌ HB(aq) + A−(aq)
then, HA is a stronger acid than HB and B- is a stronger base than A-.
In this experiment, the conductivity of various solutions will be observed; the pH of various solutions
will be determined; and the reactivities and strengths of certain acids and bases will be compared.

0.1 M HCl 6 M HCl light-colored softdrink
0.1 M NaOH 1 M Na2CO3 light-colored fruit juice
0.1 M NaCl 6 M CH3COOH detergent
0.1 M CH3COOH 6 M NaOH watch glass
0.1 M NH3 1 M NH4Cl hot plate
0.1 M NaHCO3 pH paper litmus paper
1 M NaCH3COO conductivity setup
PROCEDURE
A. Conductivity of test solutions
Each group will be assigned a solution to test in the conductivity setup.
Test solutions
1.00 M HCl 1.00 M NaCH3COO mix equal volumes of 2.00 M NH3 and 2.00 M HCl
1.00 M CH3COOH 1.00 M sucrose mix equal volumes of 2.00 M NH3 and 2.00 M CH3COOH
1.00 M NaOH 1.00 M NH3 glacial acetic acid

24
1.00 M NaCl
Prior to each test, wash the electrodes with distilled water
prior to each test. Wipe the electrodes with a piece of tissue
paper after washing. Prepare ~20 mL of the test solution in 50
mL beakers. Immerse the electrodes 1 cm apart into the test
solution (A to J). Note the intensity of the glow (bright, dim, or
none) of the light bulb. After each test, wash and wipe the
electrodes again. The conductivity setup is shown in figure 12.
Take test solution J from part 1. Add 10 mL of distilled
water to the solution. Then, test for its conductivity. Repeat
steps for second dilution. Compare the
intensities of the glows.
B. pH determination
Using a stirring rod, moisten a piece of pH paper placed on
a watch glass with the assigned test solution. A different piece
of pH paper is used for each solution.
Using the color wheel of pH values, determine and record
the pH values in your data sheet. Classify the solutions as Figure 12. Conductivity set-up.
strong acid, strong base, weak acid, weak base, or neutral, and
calculate [H+] of the solutions.
C. pH as a function of concentration
Using a 10-mL pipette, measure out 1 mL of 0.1 M HCl into a small beaker. Determine its pH and calculate
the [H+]. Also, calculate the pOH and the [OH-].
Using another 10-mL pipette, add 9 mL of distilled water to the acid in the same beaker. Stir the mixture.
Calculate the new concentration of the solution and determine its pH, [H+], pOH and [OH-].
Measure out 1 mL of the previously-prepared HCl solution into a new beaker and add 9 mL of distilled
water into it. Stir the mixture. Calculate the new concentration of the solution and determine its pH, [H+], pOH
and [OH-].
Repeat the entire procedure using 0.1 M NaOH instead.
D. Relative strengths of acids and bases

To 2 mL of 1 M NaCH3COO in a test tube, add 8 drops of 6 M HCl. Heat the solution very gently and smell
the vapor by wafting the gas towards your nose. Describe the smell and record your observation. Also, write the
net ionic equation for the reaction.
To 2 mL of 1 M Na2CO3 in a test tube, add 8 drops of 6 M CH3COOH. Observe for effervescence. Write the
net ionic equation for the reaction.
To 1 mL of NH4Cl in an evaporating dish, add 5 drops of 6 M NaOH. Attach a small piece of red litmus
paper to the underside of a watch glass and place this over the evaporating dish. Boil the mixture. Record any
change in the color of the litmus paper. Write the net ionic equation for the reaction.
WASTE DISPOSAL
1. Flush the solutions down the sink with copious amounts of running water.
2. Dispose used litmus and pH paper into the contaminated solid waste container.

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CHEM 16

General Chemistry Group Institute of Chemistry • University of the Philippines • Diliman

Christine Hernandez, Ph.D.

General Chemistry Group Institute of Chemistry • University of the Philippines • Diliman

Experiment No. Page

General Chemistry Group Institute of Chemistry • University of the Philippines • Diliman

Figure Title Page

General Chemistry Group Institute of Chemistry • University of the Philippines • Diliman

General Chemistry Group Institute of Chemistry • University of the Philippines • Diliman

Student’s Name Year/Course

Expt. Date Instructor’s

II. Diagrams/Figures for special set-ups:

III. Outline/Schematic diagram of procedure:

IV. Special Notes (proper waste disposal, safety precautions):

General Chemistry Group Institute of Chemistry • University of the Philippines • Diliman

LABORATORY SAFETY GUIDELINES

Preparing for laboratory work

Prescribed Personnel Protective Equipment (PPE)

Safety rules in the laboratory

Immediately report to your laboratory instructor:

General Chemistry Group Institute of Chemistry • University of the Philippines • Diliman

5. DO NOT PERFORM UNAUTHORIZED EXPERIMENTS. Only scheduled experiments must be

Cleanliness in the laboratory

1. Avoid contaminating the reagents.

General Chemistry Group Institute of Chemistry • University of the Philippines • Diliman

Proper Waste Disposal

General Chemistry Group Institute of Chemistry • University of the Philippines • Diliman

C. Separation of the precipitate from the supernate

General Chemistry Group Institute of Chemistry • University of the Philippines • Diliman

a. Transfer solid into the filter b. Scrub sides up, down

Figure C-1. Regular filtration techniques.

Figure C-2. Decantation techniques.

General Chemistry Group Institute of Chemistry • University of the Philippines • Diliman

a. A funnel may be used when pouring

Figure D-1. Burette preparation.

a. If left-handed, use your right hand to regulate liquid flow

Figure D-2. Titration techniques.

E. Test for acidity/basicity

F. Measurement of liquid and solid samples

General Chemistry Group Institute of Chemistry • University of the Philippines • Diliman

a. To avoid parallax error, read lower meniscus at eye level.

Figure F. Measurement of liquid samples.

G. Heating solutions in a test tube

General Chemistry Group Institute of Chemistry • University of the Philippines • Diliman

Figure H-1. Proper addition of reagents using a dropper.

Figure H-4. Transferring solids.

Figure J. Smelling vapors

General Chemistry Group Institute of Chemistry • University of the Philippines • Diliman

2. Cations with two or more oxidation states

2. Oxoanions (oxygen containing anions)

3. Hydrogen containing oxoanions – hydrogen + oxoanion name

C. Naming ionic compounds

General Chemistry Group Institute of Chemistry • University of the Philippines • Diliman

D. Naming molecular compounds

LIST OF COMMON IONS

General Chemistry Group Institute of Chemistry • University of the Philippines • Diliman

Metals with Variable Charges

General Chemistry Group Institute of Chemistry • University of the Philippines • Diliman

General Chemistry Group Institute of Chemistry • University of the Philippines • Diliman

SIGNIFICANT FIGURES AND RULES IN ROUNDING OFF NUMBERS

Example: 0.0030 has only 2 significant figures

Examples of trailing zeroes in a whole number:

1. Addition and Subtraction