18011

I NORGC?
NI C
CHEMISTRY
LABORATORY
EXPERIMENTS
c- .
WILS BEHGSTHOM, M.S.
and
MCIRLYS HOWELLS, Ph.D.
St. Paul Technical Institute
235 Marshall Avenue
St. Paul, MN 55102
Produced by Independent School District # 625 with the Minnesota

Technical Assistance Program, University o f Minnesota and the
Environmental Protection Agency
PREFACE
In 1966, with the help of local industry, the Chemical Technology

Program at St. Paul Technical Institute was developed to train
qualified technicians to work in industrial chemistry laboratories.
The emphasis of the training became chemistry principle applications
in a laboratory situtation to reinforce chemistry theory.
With a special emphasis on the analytical aspects in the
laboratory, the students are required to perform a wide variety of
experiments and are trained to safely handle many chemicals.
These experiences prepare them for the job related activities they
-- .
will encounter.
The OSHA requirements in the industrial setting made it
imperative that we begin training the students in chemical awareness
and their right to know of the hazards related to materials they
encounter on the job and in their training. Also, the cost of disposal
of waste chemicals and storage requirements make it necessary for
each training facility to evaluate their situation with regard of
maintenance cost their program. This manual was developed to reduce
the amount of hazardous materials and unnecessary exposure of the
students and staff while still allowing for the maximum learning
experience. This was done by microscaling quantities of chemicals
used and by substituting other reagents where possible.
Although it was intended that all of the experiments be tested
and evaluated during the year of writing, this, unfortunately, was
not the case. There are a number of experiments that did not get a
complete appraisal. Also, some of the tested laboratory experiments
did not get a sufficient number of trials to verify their reliabilty
at this time. We will continue to edit and revise over the next year
and will be grateful for any suggestions that will aid in the
producing of a highly useful manual.
We would like to express our appreciation to Cindy McComas for
her help, guidance and support during the past year.
We would like to thank M. Renee Aanson for her help in editing
and formatting of the manual this past year.
c- .
TABLE OF CONTENTS
Laboratory Safety Practices 1
Good Laboratory Work Habits
Analytical Balance Weighing Instructions 6
Basic Laboratory Techniques 8
Locker Check-In, Laboratory Safety, Laboratory Note-
book and Data Recording, Metric, English and SI System
of Measurement, Use of Laboratory Balances, Use of
Bunsen Burner, Requirements for Report
Density Determination 12
Procedure (Solid, Liquid), Requirements for Report
Study Assignment for Symbols, Formulas and Equations 15
Physical Separation of Mixtures 19
Procedure, Requirements for Report
Paper Chromatography 22
r- Charcoal Analysis 25
Procedure (Moisture Content, VCM, Ash & Fixed Carbon)
Requirements for Report
Percentage of Water in a Hydrate 27
Empirical Formula of a Compound 29
Percentage of Potassium Chlorate in a Mixture 32
Inorganic Nomenclature 35
Oxidation Number, Nomenclature for Binary Compounds,
Nomenclature of Compounds Containing Polyatomic Anions,
Nomenclature of Acid Salts, Writing Formulas
Table of Metallic Elements and Polyatomic Ions 42
Table of Nonmetallic Elements and Polyatomic Ions 43
Molecular Geometry 46
Valence-Bond Theory, Valence Shell Electron Pair
Repulsion Theory, Polarity
Table of Likeness of Valence Bond to VSEPR Theory 50
Limiting Reactant 52
Percent of Oxygen in Air 55
Gram Molecular Weight of Carbon Dioxide 57
Equivalent Weight of an Unknown Metal 60
Relationship of Temperature and Pressure to Change in
Physical State 63
viscosity 67
i
TABLE OF CONTENTS
Surface Tension 70
Strengths of Electrolytes 73
Standardization of a Basic Solution 77
Vinegar Analysis 82
Acidity of Fruit Juices 84
c- - Standardization of an Acid Solution 87
Antacid Analysis 91
Analysis of Active Ingredient in Commercial Tablets 94
Iron - Copper Sulfate Reaction 97
Redox Titration with Potassium Permanganate 99
Colloids 103
Colligative Properties 106
Calorimetry 111
Calorimeter Constant, Heat of Neutralization,
Heat of Solution, Procedure, Requirements for Report
Rates of Reaction 117
Factors that affect reaction rates, Procedure,
Requirements for Report.
Determination of a Rate Constant 120
Determination of the Order of a Rate Equation 123
Determination by Spectrophotometric Study the Rate of
Bromination of Acetone 12s
Equilibrium-LeChatelier's Principle 128
Spectrophotometric Determination of an Equilibrium Constant 130
Determination of the Ksp of a Slightly Soluble Salt 133
ii
TABLE OF CONTENTS
Heterogeneous Equilibrium -Determination of the Ksp of a

Slightly Soluble Silver Salt 135
Hydrolysis 137
Dissociation Constants 139
Determination of pKa of an Organic Acid 141
Buffers 142
r-
Electrochemistry - Voltaic Cell -Nernst Equation 144
Electrolytic Cell -
Determination of Avogadro’s Number 14 6
Electrolytic Cell -
Coulometric Production of Cupric Ion 148
Isolation of Caffeine from a Soft Drink 150
Preparation of Aspirin 152
iii
1
LABORATORY SAFETY PRACTICES
The laboratory is a safe working place when precautions and

proper techniques are employed. Your safety practices are as
important to your employer or your school as they are to you they are
to you since your personal safety, the safety of your fellow
workers/students, and the protection of property and equipment are
important to them. Most precautions are just common-sense practices.
These include the following:
1. Wear safety glasses at all times while in the laboratory. It is
the law in this state.
2. Wear shoes at all times.
3. Eating, drinking and smoking are strictly prohibited in the
laboratory at all times.
- * - -4. Know where to find and how to use safety and first aid equipment.
5. Consider all chemicals to be hazardous unless you are instructed
otherwise.
6. If chemicals come in contact with your skin or eyes, wash
immediately with large amounts of water and then report it to
your laboratory instructor.
7. Never taste anything. Never directly smell the source of any
vapor or gas; instead, by means of your cupped hand, bring a
small sample to your nose.
8. Any reactions involving skin irritating or hazardous chemicals,
or unpleasant odors, are to be performed in the fume hood.
9. Never point a test tube that you are heating at yourself or your
neighbor since it may splatter out of the opening.
10. No unauthorized experiments are to be performed in the
laboratory.
11. Clean up all broken glassware immediately.
12. Always pour acid into water, NOT water into acid, because the
heat of solution will cause the water to boil and the acid to
splatter. For the same reason, always pour concentrated reagent
solutions into diluted reagent solutions.
13. Avoid rubbing your eyes unless you are sure your hands are clean.
I
2
14. When inserting glass tubing or thermometers into rubber stoppers,

lubricate the tubing and the hole in the stopper with glycerin.
Wrap the tubing in a towel and grasp the tubing as close to the
end being inserted as possible. Slide the tubing into the rubber
stopper with a twisting motion. DO NOT PUSH. Keep your hands as
close together as possible to reduce the leverage. Finally,
remove excess lubricant by wiping with the towel.
15. Notify your instructor immediately in case of an accident.
16. Many common organic reagents such as alcohols, acetone and ether
are highly flammable. Do not use them any where near an open
flame.
17. Comply with all special precautions mentioned in your experiments
and with all special directions emphasized by your instructor.
18. Never use any chemical found in an unlabelled container.
19. Read the reagent bottle label twice to be certain that it is the
P- - chemical you want. The label of the reagent will list content’s
purity and safety hazards. If there is no indication of safety
hazards of the chemical, treat it as though it is flammable,
volatile, and poisonous until you have check the Material Safety
Data Sheet, MSDS, for the chemical.
20. NEVER WORK ALONE IN THE LABORATORY.
GOOD LABORATORY WORK HABITS

1. Read the assignment before coming to the laboratory.
2. Unless instructed to do otherwise, work independently.
3 . Record your results directly into your notebook. DO NOT recopy
from another piece of paper.
4. Do not clutter your working area with excess chemicals and/or
equipment to avoid accidents.
5 . Excess liquid reagents and solutions should be disposed of by
pouring them in the sink and washing them away with large amounts
of tap water, unless the experiment and instructor outlines a
special disposal method.
6. Place excess solids in designated waste container. Never r e t u r n
excess reagents t o the original b o t t l e .
3
7. Do not place reagent-bottle stoppers and/or caps on the benchtop;

hold them in your hand. Your instructor will demonstrate this
technique. Replace the stopper on the same bottle, never a
different one.
8. Leave the reagent bottles on the shelf where you found them.
9. Use only the amount of reagent recommended in the experiment
10. Always use distilled water in these experiments.
11. Do not borrow apparatus for other lockers. If you need extra
equipment, obtain it from your instructor.
12. When weighing, do not place chemicals directly on the balance
pan.
13. Do not weigh hot or warm objects. Objects should be at room
temperture.
14. DO NOT place hot objects on the benchtop. Place them on a wire
gauze.
15. When finished with your experiment, return all equipment to its
proper storage place and clean all glassware with detergent and
tap water. The glassware should be rinsed several times with
sm-allquantites of distilled water and returned to your locker
or appropriate storage place.
4
DOUBLE BLAM SPATULA
SCOOP SrYLE SPATULA

t
BUCWER FWNEL
-- WATCH G U S S
FORCEPS
5
RING STAH)
W I T H RING
Analytical Balance
Weighing Instructions
0 Woight-contml knob: 0.1 f
@ Woight-contml knob: 1 g
@ Woight-contml knob: 10 g
@ Roadoutpano1
@ T i n knobt
mition8 nf the
I @ Irordjustmontknob
.
0
l fib
= Amrt parition
@
@
Digit8lcountor knob4
~oig~~ingpan
@ hstmenttwor
Plrtiak.(wr mition
*Only on Modrls H20 and H1E.
t A l l &Is except HE.

1 = F u l l - n l r r Position
SOnb on Modrls H10 and H20.
1. lkton mighing, k w n thrt:

I The balance is rmsted. The arrestment kvar
should k in a vertical position (at 0).
A There is nothing on tho pan, thc pan is cban, and
the wbighingchamber doom are closed. FI8.1- nl" EII0.d.
e. The wnightoontrol knobs, digitalcounter knob, A When the n u m b e d rok stops moving, turn the
and t8m knob am st at zero. zem-adjustmrvt lamb until the "00" line of the
n u m b e d sak is p.rfsctly centered in the indi-
II. Setting tho olro point: ator slit (oron Models H8 and H18 until the "00"
The zero point must be rechecked before each wbigh- line of the numbend Kale is perfectly aligned
ing. with the zero line of the vemier Kale).
a. Tum the arrestment lever to the kft to the full- c Amst the balance by tuming the arrestment lever
release position (at I). - to 0.
I
BALANCE READOUTS for
Modo18 Hb, H10, HlO, H2O
111. Waighing tlw mmpk:

a. Place sample on pan with forceps. Use a container
or weighing paper.
b. Close the mighingchamber doom.
c Tum the arrestment b a r to the partialnleasa posi-
tion (see diagram).
d. Tum the l0-g weightcontrol knob clockwise until the
filling guida a m chang, direction. When th.
a m change direction, dial back one step.
c Repeat with th. nmaining mightcontrol knobs.
c- . 1. Turn the arrestment lever to the arrest position and
after a slight pause, tum the lever to the fullnlease
position.
g, If your balance model has a vemier readout (H8and
H18), rwd the result when the numbered scale stops
ming.
If your balance model has a digital readout (H10and
H201, tum the digitalcounter knob counterclockwise
(after the numbered scale stops moving) until th.
next lower scale division line is perfectly centend
in the indicator slit or aligned with t h pointer.
IV. Comploting tha woighing

a. Record the result
b. A m s t the balance.
c R e m sample from pan with forceps.
d. Retum all knobs to zero.
a. Clean the weighing chamber.
M E T T L E R INSTRUMB NT C O R P O R A T I O N
20 Nassau Stmet, Princeton, New Jarsoy OM40
R e i z i n t 2 w i n i s s i o s irznted by i d . 2 5 t l e r in 1985
8
BASIC LABORATORY TECHNIQUES
Locker Check In
A student will be assigned a drawer and locker the first
laboratory period and will be given an inventory list of glassware
and equipment which should be found in the drawer. Refer to the
preceding illustrated pages to identify items which are unfamiliar
to you. If all items are not clean and ready for use, wash with
soap and water, rinse well with tap water, and finally rinse
several times with distilled water before storing them in the
locker. Check with the instructor for replacement of those items
which are not found in the locker.
Laboratory Safety
-* - -
Your laboratory instructor will discuss safety and laboratory
procedures with you. A safety film will be shown on common hazards
and accident situations found in a laboratory. A required reading
assignment in the Chemical Technician's Ready Reference Handbook of
is pages 13 - 36. The instructor will request that you sign a sheet
of standard laboratory and safety procedures signifying that you
understand and will abide by these guidelines. The instructor will
indicate the location of fire and safety equipment in laboratory
and demonstrate their operations. Students will become familiar
with Right To Know Legislation and Material Safety Data Sheets.
Laboratory Notebook and Data Recording
Students will be required to maintain a laboratory notebook of
all laboratory experiences. Required reading assignment in Chemical
Technician's Ready Reference Handbook (CTRRH) is pages 6 - 13. The
organization of the notebook will be left to the individual, however,
the instructor will make initial suggestions.
The notebook should be a bound book, not loose leaf pages. The
first page should show your name, the chemistry course name and
number, and the date on which the course started. This should be
followed on the next page by a "Table of Contents" which will list
each experiment and the page on which it begins. Depending on the
size of the notebook it may be appropriate to leave several pages
before starting the first experiment entry. Each experiment should
be described separately. Use the following form when it applies:
1. Page number
2. Title of experiment
3. Object of experiment
4 . Equations of reactions (if any)
5. Table listing principal reactants and products, their formulas,
and important physical properties and hazardous properties from
the Material Safety Data Sheet available in the laboratory
6. Procedure and sketch of experimental apparatus
74. Data and observations
8. Calculations (if any)
9. Conclusions (and interpretations where they are appropriate).
9
For each experiment items 1 - 6 in the format outline should

be in the notebook before work is started in the laboratory. Data
tables can also be organized prior to starting if you k n o w how the
information is to be collected. Write only on the right hand page
of the notebook. Do not write information on odd Pieces of Paper
to C O P Y into your notebook later. Keep your writing legible,
accurate, neat, and clean. Use ink, preferably black, so that the
record is permanent. Ball point pens are better since they are less
likely to run if liquid is spilled on the notebook. Never erase or
use correction fluids to eliminate mistakes. Instead, draw a line
through unwanted entries. If notebook entries for one experiment are
continued on some page other than adjacent page in the book,
indicate which page to turn to and, at the new page, indicate the
number of the page from which it is continued. Include all the
information necessary for another person to duplicate your
experiment, however, be as brief and concised as possible. Enter data
and observations exactly. The essence of a notebook is accuracy. If
an experiment is ended by an accidental spill or breakage, indicate
this and start it over again. The notebook must be a permanent
c- - record of what you did and what happened.
e
The student will construct a table of metric and SI units and
conversion factors for physical quantities of length, volume, mass,
pressure, temperature, and energy. This information may be obtained
from a textbook or other suitable reference. (In the CTRRH this
information can be found on pages 787 -794.) The student will
construct a second table containing the common metric prefixes, their
abbreviations, and their designated power of ten.
The following is an example problem of how the conversion
information can be used. A 145'1b student, weighs how many kilograms?
Student must recognize that a pound, lb, to kilogram, kg, is necessary
to make the conversion. Since lb is the measured unit the lb must appear
145 l b X 1 ker = 6 5 . 7 5 9 6 kg = 65.8 kg

2 . 2 0 5 lbs
in the denominator of the conversion factor for lb units to cancel.

Another way to preceive the problem is that the unit you wish to
convert to must be in the numerator of the factor. Please note the
answer is rounded off to contain the same number of significant
digits as contained in the original measurement. When just one
conversion factor is not available to make the conversion from the
one system to another, a series of factors are used to make the
conversion. For example, 10 gallons of gasoline are equivalent to
how many milliliters? The gallons are first converted to qts, qts
10 gal X 4.0 ats X 1 liter X 1000 ml = 3 7 , 8 4 2 ml

1 gal 1 . 0 5 7 qts 1 liter 38,000 ml
to liters, liters to ml. Each time the unit which must cancel is
placed in the denominator of the factor. Notice the answer is
rounded off to contain the same number of significant digits as the
measured unit.
10
The following problems are required to be completed

and included in the laboratory report submitted by the student.
1. Convert 175 lbs to kg.
2 . Convert 16 fluid ounces to ml.
3 . Convert 800 m to miles.
4 . Convert 4.00 atm to torr.
5 . Convert 4 5 . 3 kcal to joules.
6 . Convert 4 5 2 ml to kl.
7 . Convert 267 kg to mg
a . Convert 3/8 inch to mm
9 . Convert 65 miles/hour to km/hour
Remember to round off answers to the appropriate number of

significant digits.
The student will use two types of balances when measuring mass
-. in the laboratory. The triple beam balance is capable of measuring
to the nearest hundredth of a gram, 0.01 g, and is normally employed
when approximate weighings are required for a procedure. The analytical
balance is capable of measuring to the nearest milligram or tenth of
a milligram] 0.001 g or 0.0001 g , and is employed when that level of
accuracy is necessary in the procedure. The instructor will demonstrate
a weighing method on both types of balances and the student is
required to read pages 543 - 555 in CTRRH which show the various
models and outlines general procedure of use.
Students will be required to weigh and record weights of the
following items on both types of balances.
1. 50 ml beaker
2. evaporating dish
3 . 125 m l flask
4 . a small test tube
It is recommended that the student weigh these items on the triple

beam balance first to make the weight determination on the analytical
balance more efficiently. When the student is confident about the
operation of the analytical balance, he/she should obtain a
preweighed, numbered metal tag from the instructor and demonstrate
the weighing process. DO NOT handle the tag with your fingers, use
your forceps since fingers will deposit oils and moisture on the
tag and change its weight. Whenever using an analytical balance, it
is recommended that the appropriate tool, tongs or holder, be use to
avoid touching the item. This minimizes the error in the weighing
process. Record the tag’s weight and check your results with the
instructor.
Use of Bunsen Burney
The laboratory burner is one of the most often used pieces of
equipment in your locker. Learning its proper adjustment procedure
is very important. The natural gas used in most laboratories is
composed primarily of methane, C H 4 . If sufficient oxygen is
11
supplied, methane burns with a blue, nonluminous flame producing

carbon dioxide and water. With insufficient oxygen, carbon particles
are produced which, heated to incandescence, produce a yellow,
luminous flame.
Attach the burner’s tubing to the gas outlet on the l a b bench.
Turn off the burner’s gas control valve, located on t h e base of the
burner, by screwing the valve in towards the base. Turn on fully the
gas outlet on the lab bench. Close the air holes located at the base
of the barrel, and open the burner’s gas valve slightly. Bring a
lighted match or striker up the outside of the barrel until the
escaping gas ignites. After it ignites, adjust the gas valve until
the flame is pale blue and has two or more distinct cones. Opening
the air control holes produces a slight buzzing sound characteristic
of a burner’s hottest flame. The addition of too much air may
extinguish the flame. When the best adjustment is reached, three
distinct cones are visible: a bright blue inner, intermediate
luminous and a violet outer area. The intermediate luminous area
represents the hottest part of the flame and this may be demonstrated
c* . by using crucible tongs to hold a wire screen in the flame parallel
.
to the barrel. Refer to CTRRH for illustration of burner diagram.

At the conclusion of each experiment, the student will be
required to summarize the information observed and collected in
report form. A format similar to the notebook outline is required.
The following information must be included:
1. Name of student and date
2. Title of experiment
3 . Object of experiment
4 . Equations of reactions
5 . Data tables and observations
6. Sample calculations and results table
7 . Conclusions
Answer all the questions listed at the end of each experiment.

This information is submitted to the instructor for grading in much
the same way a report would be submitted to a supervisor in an
industrial laboratory. The instructor may request to look at your
laboratory notebook periodically to verify the accuracy of your
records and adherence to the notebook guidelines.
12
DENSITY DETERMINATION
All pure substances have characteristic properties which can be

measured and used to identify them. A common example of this is the
boiling point of water is 1 O O O C . However, many other pure
substances may have the same boiling point as water so other
physical properties must be measured or observed to identify a clear,
colorless liquid as water. One property which is very unique to
pure substances is its density. Density is determined by measuring
the mass of a substance and dividing by the volume that the substance
Density = the mass of the substance
volume of the substance
occupies. Common units for mass are grams or pounds. Common units
for volume are cubic centimeters (cm3), milliliters (ml), or cubic
feet (ft3). The density of water at 40C is 1.000 g/cm3 which is
equal to 1.000 g/ml; therefore] the units milliliters and cubic
centimeters are usually interchangeable. In the US standard system,
-- the density of water at 4 o C is 62.4 lb/fts. Since scientists prefer
easy conversion from metric system to US system, they developed
specific gravity which is a ratio of the substance's density divided by
Specific Gravity = the density of the subst-
the density of water at 40C
density of water at 4oC. The specific gravity is a unitless number,
but in the metric system it has the same numerical value as the
density. Specific gravity is the value reported for a substance]
regardless of which system of measurement is used to determine its
value. The density of iron is 7.86 g/cm3 or its specific gravity is
7.86. Using the specific gravity times the density of water in the US
7.86 X 62.4 lb/ft3 = 793 lb/ftj
system, the density of iron can be calculated. Engineers and
manufacturers generally work with the SI system of measurement. This
is a new version of the metric system adopted by International Union
of Pure and Applied Chemistry] IUPAC, to provide a more logical
mattrix for all basic measurements globally. In this experiment] you
will determine the densities of a solid and a liquid.
The volume of a solid can be measured by two methods:
1) measure with a metric ruler relevant dimensions necessary
for appropriate mathematical volume formula based on the
shape of object;
2 ) measure the volume of the object by water displacement in a
graduated cylinder.
The volume of a liquid can be determined by measuring the volume
of liquid in a graduated cylinder or by using a graduated pipet to
deliver a measured volume to a preweighed flask.
The mass of both solid and liquid must be determined. The
student is required to read pages 193 - 200 in the CTRRH so that he/she
will become familiar with other methods of density determination.
13
Procedure
A. Solid
Obtain a numbered metal cylinder from the instructor and
determine its mass to the nearest 0.01 g. Using a small metric ruler
measure the diameter and length of the cylinder. A cylinder’s volume
formula is 3.14 (pi) x radius ( 1 / 2 of the diameter) squared x length.
Fill a 50 or 100 ml graduated cylinder with water to a convenient
level so that the volume may be determined. Since water adheres
to the glass wall of the cylinder, the water level will not appear
flat. This is a meniscus. To properly read the volume, use a small,
white piece of paper with a wide dark mark. Place the paper behind
the cylinder well below the top of the water and slowly move up the
barrel of the cylinder until the transparent meniscus appears to
darken. At all times read the volume using the meniscus for clear
liquids. Volume readings should always be taken at eye level. This
technique is illustrated on pages 581 - 582 in CTRRH. Record the
volume of water. Carefully add the metal cylinder to the water and
measure the new volume as previously described. Pay close attention
-
c-
to the accuracy with which the volumes can be determined by both
methods and calculate the densities with the appropriate number of
significant digits.
B. Liquid
Obtain unknown liquid from instructor in a 100 ml beaker.
Weigh an empty, clean, 10 ml graduated cylinder to the nearest
0.01 g. From the beaker pour liquid into graduated cylinder with the
aid of your stirring rod just short of the 10 ml mark (page 71 in
CTRRH). This is accomplished by placing the rod over the lip of the
beaker so that it extends 2 inches or more beyond the lip. The rod
is held in place by exerting pressure with index finger while holding
the beaker. To transfer liquid touch the rod to the side of the
graduated cylinder and slowly pour. Use medicine dropper to reach
the 10 ml mark. Carefully weigh the cylinder to the nearest 0.01 g
and record. When measurement has been completed, liquid in the
graduated cylinder may be disposed of in the lab sink with running
tap water. Calculate the density with the appropriate significant
digits.
The remaining liquid in the beaker will be used for a second
trial using a graduated pipet to measure volume and the analytical
balance to measure mass. Weigh a clean, dry stoppered flask to the
nearest 0.001 g. Use the rubber bulb to draw some of the liquid
into a clean, dry pipet. Remove the bulb and use your index finger
to close the opening of the pipet. Hold the pipet horizontally and
slowly roll the liquid in the pipet to wet the inside surface. Allow
liquid to drain from the pipet into the lab sink. Examine the inside
for beads of liquid and if found clean the pipet thoroughly. It is a
necessity that a pipet deliver an exact volume and if small amounts
of liquid adhere to the inside, that is volume which is not measured.
14
Pipets should always drain cleanly. Rinse the inside of the pipet
with another small quantity of liquid and allow it to drain. Draw
the unknown liquid into to the pipet above the 10 ml mark. Using the
pressure of the index finger on the opening slowly bring the meniscus
to the 10 ml mark. Read the volume at eye level. Do not worry if
the meniscus is not exactly at the ten ml mark since the pipet is
graduated it will allow an exact volume reading. Move the pipet to
the preweighed flask and allow the liquid to drain into flask by
lifting your index finger. As the level of draining liquid approaches
the zero line on the pipet, place index finger over opening to control
flow rate and eventually stop it. Remember that flow must be stopped
above the zero line since the area from zero to the tip is not
measureable. Read the volume at eye level and record. Stopper your
flask and measure the mass to the nearest 0.001 g . Calculate the
density of unknown liquid. Dispose of excess unknown liquid in lab
sink with large amounts of tap water.
Follow the guidelines established in Basic Laboratory Techniques
-._ section for writing your report. In the conclusion section, make
comparisons between the two different methods used for density
determinations relative to their accuracy and which measurement
determined the number of significant digits in the calculated density.
Report average density of both solid and liquid with the appropriate
number of significant digits.
1. If you had an irregularly shaped solid, how could you determine

its volume? Explain.
2 . If air bubbles adhere to the surface of the metal cylinder when
submerged for measurement, how does this affect the density
determination? Explain.
3. If several drops of unknown liquid remain on the pipet’s inner
wall, how will this affect the reported density? Explain.
4 . If draw a sketch of a cross section fo a graduated cylinder
illustrating the proper method for reading volume.
5 . Using a suitable reference source, briefly describe two other
methods by which density may be determined.
15
STUDY ASSIGNMENT FOR SYMBOLS, FORMULAS, AND EQUATIONS
The chemist communicates in a technical language that is

specific to the substances with which he/she deals. The language
is a notation abbreviated to save time and space similar to the
shorthand notations used by stenographers. However, if one
becomes familiar with these terms and notations, the language is
readily understandable. A chemist's basic language is symbols
for elements, formulas for compounds, and equations for
reactions.
In this assignment, students will study each of these and
learn to recognize their significance. Students will be supplied
with a periodic table of elements, and will use the CRC Handbook
of Chemistry and Physics or textbook to find necessary information
to complete the exercises.
A symbol represents the name and also one atom of an
c- - element. Since Latin and Greek were the languages used by early
chemists, some of the elements were given Latin names, whereas
the more recently discovered elements have English names. For
example, Au represents aurum (gold), Cu represents cuprum
(copper), Fe represents ferrum (iron), but Co represents cobalt
and Se, selenium. The Periodic Table lists the elements, their
atomic numbers (the whole number), and atomic weights. The
atomic weights are the average masses of all naturally occurring
isotopes of the element and, consequently, many of the elements
do not have whole numbers for their atomic weights. Those
elements having whole number masses have been synthetically
prepared. Elements to the right of the "stepped" line beginning
at boron are nonmetals and to the left are metals.
A formula is a combination of symbols representing the name
and also one molecule or formula unit of a compound, a chemical
combination of elements. Subscripts indicate the number of atoms
of each element in a compound. For example, H2O is the formula
for water, a chemical combination of 2 atoms of hydrogen, H, and
1 atom of oxygen, 0; COz is the formula for carbon dioxide, a
chemical combination of 1 carbon atom and two oxygen atoms
whereas CO is the formula for carbon monoxide, a chemical
combination of 1 carbon atom and 1 oxygen atom. A change in
subscript represents a change in chemical composition of a
compound.
A chemical equation represents a description of a chemical
reaction before and after it takes place. It uses symbols and
formulas to describe chemical substances. The reactants appear
on the left side of the arrow, meaning "to produce", and products
appear on the right side. For example, the reaction between
16
carbon and oxygen to produce carbon dioxide simplifies to

c + 02 ---> c02.
The plus sign, + , means "and", but does not imply a summation.
The chemical equation implys that one carbon atom and one oxygen
molecule react to produce one molecule of carbon dioxide.
A chemical equation not only simplifies a statement, but it
also indicates the number of atoms involved in a reaction and how
they rearrange to form products. In the above equation, note
that 1 C atom and 2 0 atoms are rearranged to form a product
containing 1 C atom, 2 0 atoms. We say that atoms are conserved
in a chemical reaction; they are only rearranged. If each atom
has its own mass, then mass also is conserved.
A correct equation must have the same number of each type
atom appearing on both sides of it. To achieve this mass
balance, coefficients are placed before the symbols or formulas
in the equation. For example, potassium metal and chlorine gas
-. . . react to produce potassium chloride:
K ( s ) + C12 ( 6 ) --- > KC1 ( s ) (unbalanced)
The symbols for potassium and chlorine and the formula for
potassium chloride are correctly written. To indicate 2 atoms
of-chlorine in the product, a coefficient of 2 is placed before
K C 1 , or
K ( s ) + C l 2 (g) ---> 2KC1 (SI (unbalanced)
However, the equation now shows 2 potassium atoms on the right;

a coefficient of 2 in front of the K on the left balances the
equation:
2 K Cs) + C l 2 (g) ---> 2KC1 (s)
The equation is now mass balanced or obeys the Law of Conservation

of Mass.
Section A
Use the Periodic Table (Sargent-Welch) supplied by the instructor
to answer the following questions.
1. Identify the elements'on the Periodic Table which are gases
and liquids. Construct a table containing the symbol of the
element, its name, its state at room temperature and
atmospheric pressure, the smallest particle of the element
that occurs naturally.
2. All naturally occurring gases, except the noble gas, are
are diatomic. All halogens, Group VIIA, are diatomic. Write
the formulas for these elements in their naturally occurring
state.
17
3. Match the following names for the elements with their symbol.
List the standard English name for the element.
Symbol Latin Name English Name Choices
Na aurum
K argentum
Fe cuprum
cu ferrum
Ag hydragyrum
Sn kalium
Sb natrium
W plumbum
Au stannum
stibium
wolf ram
4. Of the 106 known elements, few make a significant contribution
to the composition of the earth’s crust. Using the CRC
Handbook, construct a table of the ten most abundant elements
c- - in the earth’s crust, their percentages, atomic numbers,
symbols, atomic weights, and classify them as metal or nonmetal
Section B
1. Write the formulas for the following compounds which are
encountered commonly in everyday living. Using the CRC
Handbook or chemical dictionary, look up each compound’s
physical state, color, and appearance.
a. table salt 1 Na atom , 1 C1 atom
b. table sugar (sucrose) 12 C atoms, 2 2 H atoms, 1 1 0 atoms
c. ammonia 1 N atom, 3 H atoms
d. water 2 H atoms, 1 0 atom
e. baking soda 1 Na atom, 1 H atom, 1 C atom, and
3 0 atoms
f. limestone 1 Ca atom, 1 C atom, 3 0 atoms
g. Vitamin C 6 C atoms, 8 H atoms, 6 0 atoms
h. vinegar 2 C atoms, 4 H atoms, 2 0 atoms
2. The instructor will make available to you approximately 50

samples of compounds, labelled with name and formula, in large
test tubes. These ionic compounds, normally formed by the
reaction of a metal with a nonmetal, are generally called
salts. Complete the following generalizations based on
your observations.
a. Blue colored salts often contain
b. Green colored salts often contain -
c. Most salts exhibit a --- color.
d. Most cobalt salts are in color.
e. Salts containing MnO4- exhibit a color.
f. Salts containing Crz07-2 exhibit a - color.
g. Salts containing (203-2 exhibit a color
but the exceptions are -- and __-_____--
18
Section C
1. Write a chemical equation for the following statements of
reactions and balance the equation.
a. Methane, C H 4 , and o x y g e n to produce carbon dioxide and
water.
b. Hydrogen and oxygen to produce water.
c. Calcium carbonate, CaC03, and hydrochloric acid, HC1, to
produce calcium chloride, CaC12, water, and carbon
dioxide.
d. Magnesium and nitrogen to produce magnesium nitride,
MgzNa .
e. Potassium and sulfur to produce potassium sulfide, K 2 S .
f . Aluminum and hydrochloric acid to produce aluminum
chloride, A1C13 , and hydrogen.
19
PHYSICAL SEPARATION OF MIXTURES
Matter can be classified into one of two general categories,

pure substances or mixtures. Pure substances are elements or
chemical combinations of elements called compounds. The elements
hydrogen and ‘oxygen can be chemically combined to form the compound
water. Mixtures are physical combinations of two or more pure
substances such that each substance maintains its own chemical
identity. For example, in a salt-water mixture, each component
retains the chemical properties as found in their pure state; the
water is H20 molecules and the salt is sodium ions, Na+, and
chloride ions, C1- .
Mixtures are either homogeneous or heterogeneous. Homogeneous
mixtures consist of two or more substances forming one phase with
uniform properties throughout. The salt-water mixture is an example
and this is referred to as a solution. Air is an example of a
homogeneous mixture of gases. Heterogeneous mixtures consist of two
c- -
or more distinct phases or regions each having its characteristic
properties. Examples of heterogeneous mixtures are concrete, composed
of cement and stone, ice water, composed of solid water and liquid
water, and Italian salad dressing, composed of oil, water and spices.
Most substances found in nature or prepared in the laboratory
are impure, thus representing mixtures. The method chosen to
separate these mixtures depends on the differences in the chemical
and/or physical properties of the mixture’s components. Some of the
common physical methods used to separate components are:
1 . centrifugation - separating solids from liquids or liquids of
different specific gravities by fast rotation
2. chromatography - separating components on the basis of their
individual selective adsorption on a stationary phase as the
mixture passes through or over it
3 crystallization - forming a crystalline solid from solution by
decreasing its solubility
4 . distillation - purifying a liquid by boiling it and condensing and
collecting the vapors
5. extraction - removing a substance from a mixture by adding a
a liquid in which the substance is more soluble
6. filtration - separating a liquid from a solid using a porous
material through which only the liquid will pass
7 . sublimation - heating a solid substance directly to vapor and
recondesing it as a solid ( not all solids sublime)
In this experiment, gravity filtration will be used to separate a
sand-salt mixture. Three techniques are associated with all
filtration processes: decantation, washing, and transfer. When a
solid settles to the container’s bottom in a liquid and does not
appear to be suspended, it can be separated from the liquid by
pouring off the liquid so that no solid is carried along. This
technique is decantation. The solid is then washed with a small
amount of water to remove any remaining soluble material, salt.
20
The solid is allowed to settle and liquid is then decanted. Several

washings are recommended. The transfer of the solid is accomplished
with the aid of a wash bottle and stirring rod with a rubber policeman.
The stirring rod is used in the same manner as liquid transfer
described previously. The beaker and rod are held at inclined
position above the filter with the rod touching the filter. A water
stream from the wash bottle is used to wash the solid into the filter
See pages 266 - 2 7 2 in CTRRH.
Procedure
In a 250 ml beaker, weigh a 2 - 3 g sample of sand-salt mixture
to the nearest 0.01 g. Obtain a ring stand and ring to support the
funnel found in your locker. If funnel is too small to be supported
by the ring, place your clay triangle on the ring and then insert the
funnel in the triangle. Obtain a piece of filter paper and fold it
precisely in half. Fold it in half again but do not make a perfect
right angle(800). You should not have perfect quarters. Take the
edge of the smaller section and tear off the corner. The tear enables
a close seal to be made across the paper’s folded portion when placed
in the funnel. Weigh the filter paper to the nearest 0.01 g .
Place filter paper snugly in the funnel so that the edge with the
tear is in contact with the funnel wall. Moisten the filter with
distilled water and press it against the funnel’s wall to form a
good seal.
Add 20 ml of water to the sand-salt mixture and stir with a glass
rod for several minutes. Incline the beaker so that sand collects
directly below the lip of the beaker. While the sand is settling,
place a 100 ml beaker beneath the funnel so that the tip of the
funnel is just touching the side of the beaker. Decant the liquid
using proper techniques. Add 10 ml of water to the beaker and repeat
the stirring, settling, and decanting processes. Add 10 ml of water
to the beaker and repeat these three manipulations. Transfer the
sand to the filter paper using the wash bottle as previously
described. Allow the liquid to drain from the filter and place it on
a marked watch g l a s s for drying in the drying oven. When the paper is
dry, allow it to cool and weigh it again to determine the mass of the
sand. Calculate the percentage of sand in the mixture by dividing the
mass of sand by original sample mass and multiply by 100.
Remove the funnel from the ring and place a wire gauze on the
ring to support a preweighed evaporating dish. Pour liquid from the
filtering process into the evaporating dish and heat it with a burner.
DO NOT attempt to overfill the evaporating dish. When all the liquid
has been transferred to the dish, rinse 100 ml beaker several times
with wash bottle. Heat the dish until the volume of water has been
reduced to approximately 5 ml. Place in drying oven to complete the
drying of the salt. Allow the dish to cool and weigh to determine
the mass of salt. Calculate the percentage of salt in the mixture in
the same manner used for the percentage of sand. Do the percentages
total loo%? If not, give possible reasons for the discrepancy.
Repeat the entire procedure for a second trial making any
adjustments you think are necessary to improve your results.
21

Follow guidelines established in Basic Laboratory Techniques
experiment for writing your report. Compare the first and second
trial results and report average percentages of sand and salt.
Quest ions
1. Using a suitable reference source, define the following words:
a) adsorption
b ) phase
c ) soluble
d) solution
e) solvent
f ) suspension
2 . What substance is extracted in this experiment?
3 . Why is the sand washed with 10 ml portions of distilled water?
4 . If the washings in question 2 are not done, how would this affect
-* - the percentage of sand? Explain.
5 . Explain how you would separate a sugar-sand mixture. Would the
procedure in this experiment have to be modified in any way?
22
PAPER CHROMATOGRAPHY
Physical methods used for identification depend upon the

differences in physical properties of substances present in mixtures.
Chromatography is the name applied to a series of processes ir which
the components of a mixture are distributed between a station& y
phase and a mobile phase. Normally, the stationary phase is a solid
such as paper, starch, alumina, or silica and the mobile phase is a
liquid such as water, common organic solvents, or solvent mixtures.
The word chromatography, literally means color writing, and was coined
by a Russian botanist, Twsett, when he separated color pigments into
the individual dyes using this method in 1906. Color is not necessary
to achieve separation by this method. Colorless compounds can be
reacted with other reagents to make them visible.
-. ~
Paper chromatography is the simplest and most efficient

technique available to introduce this unique separation method. The
basis for paper chromatography is the fact that porous paper,
cellulose, has an enormous surface area to which molecules or ions
of substances are attracted (adsorbed) and then released (desorbed)
into the solvent as an aqueous solution passes over the paper.
Separation of components occur, that is, they will travel at
different speeds in a moving solvent because the varying attractions
between these components and the paper. This phenomenon of separation
is known as partitioning.
In paper chromatography, a small line of the mixture to be
separated is placed at one end of a strip of paper, and solvent is
allowed to move up the paper through the line by capillary action.
The solvent and the various components of the mixture travel at
different speeds along the paper. The identity of the components can
be deduced by comparing a chromatogram of the unknown mixture with
chromatograms of mixtures with known composition (standards). An
additional aid in identification of substances is its Rf value, which
is defined as the ratio of the distance traveled by the substance to
R € = distance traveled by component
distance traveled by solvent
the distance traveled by the solvent. The Rf value of a compound is
a characteristic of the compcmnd and solvent used and serves to
identify the constituents of a mixture. Your aim in this experiment
will be to determine the number of substances and their Rt values
present as dyes in commercial ink samples, such as Crayola marking
pens. Any commercial ink sample can be separated into component
colors provided the appropriate solvent is used.
23
Procedure
Fill a 400 ml beaker with water to a height of 1 cm. Obtain
six strips of chromatographic paper. With a pencil, draw a light
line about 1 cm from one end of the strip and parallel to the short
dimension of the strip (Line A ) . Draw a second parallel line, Line B,
1 cm from Line A . Line A will represent the
~- level to which the strip should be submerged into
Sample the solvent, water. Using the marking pen, apply
a thin ink line over Line B on the paper strip.
This may require some practice on filter paper to
ensure a thin straight line. Prepare separate
paper strips for each marking pen color you w.sh
to analyze. Attach a paper clip to the end of the
strip opposite the lines and mark this end, using
a pencil, with the name of the color marking pen.
CAUTION: Do not handle the paper with your fingers
if either they or the paper, or both are wet.
Allow the ink color to air dry after application to
the paper strip. Hang the paper on a stick and
adjust paper clip so that strip will be submerged to
Line A when the stick is placed across the top of
the beaker. Place the strip in the beaker as
described previously and observe what takes place.
Line B When the solvent front has almost reached the top
of the paper strip, remove it from the beaker and
Line A mark the position with a pencil. This should be
done quickly because some solvents evaporate
rapidly. Allow the chromatogram to air dry.
Measure the distance from Line B to each separated
dye in the sample and record in your notebook.
Measure the distance from Line B to the marked
solvent front and record in your notebook. Proceed in the same
manner with the other strips that you prepared using the various
colored marking pens. Save all chromatograms.
Repeat the procedure to separate the same inks into component
colors with a 5 0 : 5 0 methanol-water solvent mixture. Repeat the
procedure with methanol as the solvent. If the student has extra
time remaining in the lab period, samples of other commercial inks
may be done.
Tabulate information found on the individual chromatograms.
The following items should be listed in the table; sample, solvent,
component’s distance traveled, solvent’s distance traveled, and
component’s Rr value. The last entry can be calculated using the
ratio explained in the introduction to the experiment.
Beauiremonts f o r ReDort
Follow established guidelines for the report. Attach to the
report, a representative chromatogram from each solvent system used.
For a sample, discuss the similarities and/or differences of Rf
values with respect to the three solvent systems used. Comment one
components which seem to be the same in the samples.
24
Glues t ions
1. Distinguish between absorption and adsorption.

2. What is an eluting solution and how is it used in
chromatography?
3. Sketch what a chromatogram would l o o k like if it had two
components, one with a Rf = 0.65 and another with a Rf = 0.80.
4 . What factors influence the Rf values? Would it be possible to
compare the Rf values for the dyes in the ink samples to those in
the candy samples?
5. What forces cause the solvent to move along the paper?
25
CHARCOAL ANALYSIS
Fossil fuels represent a large portion of the world’s energy

supply. They also serve as an economical source of raw materials for
the manufacture of products such as plastics. synthetic fabrics, and
medicines. A very important property of a fuel is its heat of
combustion which is the amount of heat (calories, joules, or BTU’s)
released per amount of fuel (barrels, cubic feet, or tons). The
energy rating of a fossil fuel gives us information about its
chemical composition. Although charcoal is not a fossil fuel, but
amorphous carbon from the incomplete combustion of animal or
vegetahie matter, its chemical composition can be analyzed in the
same fashion as fossil fuels. The average person is more familiar
with charcoal as the energy source for cooking on outdoor grills.
In this experiment, the ash, fixed carbon, moisture, and
volatile combustible matter (VCM) for charcoal is determined. The
analysis approximates charcoal’s composition because values vary
c- - between charcoal samples. A student wishing to make a BEST BUY
comparison would be required to do a large number of samples from
different bags of the same brand of charcoal. The collected
information could then be compared to a corresponding number of
samples from other brands.
Procedure
A . Moisture Content
Support a clean, empty crucible and lid on a clay triangle
using a ring stand. Heat the crucible with a hot burner flame for
several minutes to burn off any impurities. Handle the crucible and
lid with crucible tongs for the remainder of the experiment. Move
the crucible and lid to the carrying tray, allow to cool, and weigh
to the nearest 0.001 g. Add approximately 1 g of charcoal to the
crucible and weigh again. The lid may be weighed separately since
its use is not required in the first section of the procedure. Put
the crucible in a 100 ml beaker marked for easy identification and
place in a drying oven for 1 hour. Allow crucible to cool and
reweigh. The weight loss represents the moisture content of the
charcoal.
B. Volatile Combustible Matter, VCM
Now support the crucib.le and dried charcoal in a clay triangle
and cover with the lid leaving a slight opening at one side.
Initially, heat the apparatus gently, gradually increasing to a hot
flame for several minutes. Use tongs to close the lid completely and
allow the sample to cool to room temperature. Before weighing the
crucible, examine the upper portion of the crucible and the lid for
deposits and discolorations. If deposits appear on the lid, heat it
directly in the flame. If deposits appear on the crucible, carefully
heat the upper portion of the crucible without the lid and avoid
heating the charcoal sample. Weigh the crucible, lid and remaining
sample, when cool, to the nearest 0.001 g. The weight loss is the
VCM evolved during the heating process.
26
C. Ash and Fixed Carbon

Support the crucible in the clay triangle and partially cover
it with the lid. Heat the sample intensely and if the sample ignites,
use the tongs to cover the crucible until flame is extinguished.
Continue intense heating until no black residue remains on the lid or
in the crucible. This will require that you periodically use the
tongs to rotate the crucible's position in the flame. The residue in
the crucible should appear to be a light gray-brown color when the
combustion has been completed. Cool the crucible, lid, and contents
and weigh. The residue remaining in the crucible is the ash content.
The weight l o s s after the VCM removal is the fixed carbon content.
Repeat the entire procedure f o r a second trial.
Tabulate the data collected in the experiment and calculate the
percentages of ash, fixed carbon, moisture and VCM from data. Pay
attention to significant digits in the data and reported numbers.
Comment on the consistency or inconsistency of values from the two
trials.
Questions
1. Of the four determinations in the experiment, which is
proportional to the heat content or would be equivalent to an
energy rating?
2. Identify in each section of the procedure whether a physical or
chemical change is being used to analyze the charcoal.
3 . For those physical changes you identified in the previous
question, refer to the Physical Separations experiment to relate
them to a particular separation process.
4 . If the moisture is not removed in the drying oven, how does this
affect the reported VCM (high or low)? Explain.
5 . If the crucible's lid is not used in Section B of the procedure,
what reported values are affected and how? Explain.
27
PERCENTAGE OF WATER IN A HYDRATE
Many pure substances combine with water in a fixed mole ratio to

yield compounds called hydrates. For example, zinc sulfate combines
with water to form crystalline ZnSO4-7HzO which is a stable
compound at normal atmospheric conditions. All pure samples of this
hydrate show the same percentage of water by analysis. Thus, this
hydrated compound obeys the law of constant composition. Upon
heating a sample of such a hydrate, it may lose all its water of
hydration and revert to the anhydrous salt. Substances which have
adsorbed water on the surface do not show constant composition and
therefore are not hydrates. An example of this would be common table
salt, NaC1, which becomes very sticky on humid, summer days. In these
cases, the percentage of water is not constant for all samples of a
particular compound, and the water is not chemically bonded as part
of the crystal structure.
The purpose of this experiment is to determine the percentage of

wate'r in an unknown hydrate. Water is removed from the hydrate by
heating an accurately weighed hydrate sample until the residue has
reached a constant weight. The percentage of water in the sample is
calculated by using the weight of water lost and the initial hydrate
sample weight multiplied by 100.
Procedure
Clean and dry a porcelain crucible and cover. Place the empty,
covered crucible on a clay triangle supported by a ring on a ring
stand. Heat the crucible and cover in the hottest flame of the
Bunsen burner for 5 minutes. A dull red glow should be observed on
the crucible and cover. This will require that you manipulate the
burner to heat uniformly. This will insured that all volatiles and
combustible materials are removed prior to the analysis procedure and
that a constant weight for the crucible and cover may be recorded.
The crucible and cover must be allowed to cool to laboratory
temperature for approximately 15 minutes. Using crucible tongs
transfer the crucible and cover to a carrying tray and weigh them to
the nearest 0.001 g. Add 1 to 1 . 5 g of zinc sulfate heptahydrate
to the crucible and weigh the covered crucible to the nearest 0.001g.
Place the covered crucible on the clay triangle with the cover
slightly opened. Heat the crucible gently for a few minutes to avoid
l o s s of material from spattering during initial heating. Remember
$hat water boils at 1OOoC. Continue to heat the crucible and
contents for approximately 15 minutes gradually increasing the
temperature of the flame. Allow the crucible to cool on the triangle
after removing the flame until it has reached room temperature.
Transfer it to the carrying tray and weigh the covered crucible to
the nearest 0.001 g. Reheat the crucible and contents for about
5 minutes and, after cooling, weigh it again. Repeat this heating,
cooling and weighing sequence until two consecutive weighings are
within 0.005 g. This sequence of heating, cooling and weighing to
obtain consistent results is known as heating to a constant weight.
28
Calculate the actual percentage of water in the zinc sulfate

using the gram formula weight of the hydrate and the weight of water
indicated in the formula multiplied by 100. Calculate the
experimental percentage of water in your hydrate based on water lost
as a result of heating divided by the hydrate sample weight
multiplied by 100. To evaluate your results and determine how well
you did the analysis, you can calculate relative error using the
following formula.
Actual Value - Experimental Value Percent of
Actual Value X 100 = Relative Error
An absolute relative error of 3% or less is excellent. If the
percent of error is greater than 3 % , think about factors that you
observed during the procedure that may have affected your results
Modify your actions accordingly for the unknown hydrate sample.
Ohtain from your instructor an unknown hydrate sample. Repeat
the procedure which you used on the known hydrate. Do a minimum of
two trials and report the average percentage of water in your unknown
hydrate. DO NOT forget to record your sample number and/or letters.
Data tables should be constructed for all hydrate trials so the
information is readily found in the report. One sample calculation
must be demonstrated for a completed trial. Record all observations
and adjustments made to improve your technique.
Questions
anhydrous
deliquescent
desiccant
desiccator
efflorescent
hydrate
hygroscopic
2 . Using the CRC Handbook of Chemistry and Physics find:
a) five hydrates, each with a different number of waters and
record their names and formulas.
b) two crystalline substances with no waters of hydration
c) two substances known to be deliquescent
d) two substances known to be efflorescent
e ) all of the hydrates of.sodium carbonate
3 . If the volatile impurities are not burned off the crucible and
cover, how does this affect the reported percent of water?
Explain.
4 . .If the salt decomposes to yield volatile materials, is the
reported percent of water in the sample too high or too low?
Explain.
5. Anhydrous calcium chloride is used inside dessicators to remove
moisture. Explain how CaC12 removes the water vapor.
29
EMPIRICAL FORMULA OF A COMPOUND

In a given chemical compound, the elements are always combined
in the same proportion by mass. A compound’s empirical formula
specifies the lowest whole number ratio of the atoms in the compound.
Under a specific set of reaction conditions for two elements, only one
compound can be formed. When those conditions are changed, however,
it is sometimes possible for other compounds to be formed. An
example of this is the reaction of hydrogen and oxygen to form two
different compounds, water ( H 2 O ) and hydrogen peroxide ( H 2 0 2 1 .
When water is formed, the ratio is always two hydrogen atoms to one
oxygen atom and in hydrogen peroxide a ratio of two hydrogen atoms to
two oxygen atoms. This illustrates the Law of Multiple Proportions
which state that whenever two elements form more than one compound,
the different masses of one element that combine with the same mass
of the other element are in the ratio of small whole numbers. In
water, 1 gram of hydrogen combines with 8 grams of oxygen. In
hydrogen peroxide, 1 gram of hydrogen combines with 16 grams of
oxygen. Also note that the empirical and molecular formula are the
same formula for water whereas the empirical formula of hydrogen
peroxide is half of its molecular formula because an empirical
formula is always the lowest whole number ratio of atoms in the
compound.
The following information is required to determine the
empirical formula of a compound. First, the composition by weight of
each element is determined. Second, the number of moles of each
element is calculated by using their gram atomic weights. Third, the
empirical formula is expressed as the smallest whole number mole
ratio of the elements. When we determine an empirical formula, the
compound’s weight composition is established by either analysis or
synthesis. In analysis, a known weight of the compound is decomposed
and each elements weight is measured. For instance, water can be
electrolyzed to produce hydrogen and oxygen. Each gas can be
collected separately and measured. In synthesis, the compound’s
weight resulting from the chemical combination of the known weights
of two elements is measured.
This experiment synthesizes a magnesium-oxygen compound and/or
a copper or nickel-sulfur compound. Using the metal’s initial weight
and the compound’s final weight, the weight of the nonmetal (oxygen
or sulfur) is derived. Thus the empirical formula may be determined
by calculating the simplest whole number mole ratio of the elements.
The magnesium-oxygen synthesis may be done at the laboratory bench
but the copperhickel-sulfur synthesis MUST be done in a fume hood
because a side reaction of forming sulfur dioxide, S02, a gas which
is a health hazard as an irritant to eyes, skin and respiratory system.
30
Procedure
Section A
Support a clean crucible and lid on a clay triangle and heat
with a hot, blue, nonluminous flame until it glows red. This will
require that the burner be manipulated to heat all surfaces. While
the crucible and lid are cooling to room temperature, obtain a 0 . 2 to
0.3 g sample of M g ribbon and polish the surface with steel wool.
Cut the ribbon into several small pieces which will conveniently fit
in the crucible and divide the pieces so that two trials may be
completed. When the crucible is cool, using crucible tongs, transfer
it to a carrying tray and weigh it to the nearest 0.001 g. Add
several pieces of Mg to the crucible and reweigh it. The Mg sample
should weigh 0 . l g or more. Place the crucible containing Mg ribbon on
the clay triangle and cover it with the lid leaving a slight opening
on one side. Heat slowly. If too much air reaches the Mg, rapid
oxidation occurs and it burns very brightly. If this happens,
immediately cover the crucible with the lid and then adjust it for
a slight opening again. Continue heating until no change is
apparent in the Mg residue. Remove the lid and heat the open
crucible.
Remove the flame and allow the crucible to cool for several
minutes. Add a few drops of water to the residue in the crucible
to decompose any magnesium nitride formed during combustion. You
may detect a slight odor of ammonia. Dry the residue using a low
flame and allow the crucible to cool. Transfer it to a carrying
tray and weigh to the nearest 0.001g. Repeat the sequence of steps
in this parargraph until the second and third weighings are within
-
+0.008 g.
Section B
Support a clean crucible and lid on a clay triangle and heat
with a hot, blue, luminous flame until it glows red. This will require
burner manipulation to heat all surfaces. While the crucible is
cooling, obtain 0.5 to 1.0 g of copper wire and coil it around a
pencil using forceps. Once it has been coiled, compress the coil so
that it will occupy a minimum of space in the bottom of the crucible.
Using crucible tongs, transfer the crucible and lid to a carrying tray
and weigh it to the nearest 0.001 g. Add the copper sample to the
crucible and reweigh it to the nearest 0.001g. (At the instructor’s
option, nickel may replace copper in this procedure.)
In a FUME ROOD, support the crucible on a clay triangle and add
enough powdered sulfur, approximately 0 . 4 g, to cover the copper wire.
Place the lid on the crucible and adjust it to a very slight opening on
one side. Heat the crucible slowly with a low flame. When the light
blue sulfur flames around the crucible’s edges are no longer visible,
move flame around the crucible and lid to ensure the complete combustion
of the excess sulfur. Cover the crucible completely and heat it with
hot flame for at least 5 minutes. Allow the crucible, lid and contents
to cool to room temperature and weigh it to the nearest 0.001g.
I
31
Return the crucible to clay triangle in the fume hood and add
approximately 0.1 g of powdered sulfur and reheat it as before until
all of the sulfur has burned. The second weighing of the crucible,
lid and contents should be within 2 0 . 0 0 8 g. If it is not, repeat
steps in this paragraph to a constant weight value. A second trial
of the experiment should be run to verify the results of first trial.
Jteauirements for RePort
Data and results tables should be constructed. One sample
calculation must be demonstrated for a completed trial. Record your
observations and adjustments made to improve your results. Using
the CRC Handbook of Chemistry and Physics for the actual formula of
the synthesized compound, calculate the relative error on the average
of your two trials.
Quest ions
a) elemental analysis
b) decomposition
6 ) formula
d) synthesis
e) gram equivalent weight
f) oxidation
2. Using the CRC Handbook of Chemistry and Physics, find the names
and formulas of the compounds prepared in the experiment. In the
case of copper there will be two compounds listed. Search for a
chemical reaction by which the other compound of copper and sulfur
may be prepared. Give your source of information.
3 . If the lid is not used to control the burning of the Mg, what can
happen as a result of the rapid oxidation? How would it affect
the reported empirical formula?
4 . If the copper sulfide compound is heated intensely without the
cover, the surface color changes from blue-black to orange or
orange-red. What chemical reaction is taking place. Justify your
answer with specific chemical facts.
5 . When nitrogen and oxygen combine at various reaction conditions,
the following compounds can be formed: N 2 0 , N O , N O 2 , N 2 0 3 ,
and N 2 0 5 . Calculate the amount of nitrogen that will combine
with 8 g of oxygen for each compound. You will be calculating the
gram equivalent weight of nitrogen in each compound which should
verify the Law of Multiple Proportions.
32
PERCENTAGE OF POTASSIUM CHLORATE IN A MIXTURE
Chemical reactions provide information regarding the

t
relationships between the products and reactants. The stoichiometry
of a reaction is a description of the relative quantities by moles of
reactants and products as indicated by the coefficients in the
balanced equation. In a balanced equation, the sum of the atoms of
each element appearing in the reactants must equal their sum among
the products. A balanced equation is a shorthand notation and
quantitative description of a chemical reaction. For example,
hydrogen reacts with oxygen to form water, but this gives no
information regarding the proportions of reactants and products.
Therefore, it must be translated to an equation form.
H2 + 02 --> H2 0 unbalanced
ZHZ + 02 --> 2Hz 0 balanced
The balanced equation may be read as two molecules of hydrogen react
witb 1 molecule of oxygen to form two molecules of water. The most
common interpretation of the balanced equation is in terms of moles,
that is, 2 moles of hydrogen react with 1 mole of oxygen to form two
moles of water.
This experiment is an example of quantitative analysis, more
specifically, gravimetric quantitative analysis. When potassium
chlorate, KC103, is heated, it decomposes to produce oxygen, 0 2 ,
MnO2
KC103 ------ > KC1 + 02 unbalanced
heat
and potassium chloride, KC1. Manganese dioxide, MnOa, is added to
the potassium chlorate as a catalyst. The role of a catalyst in any
reaction is to initiate the chemical reaction and to reduce the
energy require for the reaction to take place. A mixture of potassium
chlorate and sodium chloride is heated until all of the oxygen has
been released, leaving a residue consisting of K C 1 and unreacted NaC1.
The weight loss of oxygen is calculated by subtracting residue weight
from original mixture weight. The weight of potassium chlorate in the
mixture is calculated from the weight of oxygen lost using the
balanced equation. Thus, the percentage of potassium chlorate in the
original mixture can be computed. To increase the accuracy and
develop good technique for the unknown sample, the student will do
two trials on known, prepared mixtures. By observation and percent
relative error, the student can determine when he/she is ready for an
unknown sample.
33
Procedure
CAUTION: Great care must be taken to avoid introduction of any

organic material or other reducing agents into the potassium chlorate
mixture. A serious explosion is almost certain to result from such
carelessness. Goggles must be worn at all times in the laboratory.
A heat resistant test tube, such as Pyrex or Kimax, must be used for
the experiment.
Wash several heat resistant test tubes, rinsing each very well
with distilled water, and dry in IlOOC drying oven. In a clean,
dry, small beaker, 50 or 100 ml size, obtain approximately 4.0 g of
potassium chlorate and cover with a clean, dry watch glass until you
are ready to start the weighing process. In a clean, dry, small beaker
obtain approximately 2.0 g of sodium chloride and cover with a clean,
dry watch glass. Since both compounds are white crystalline solid,
be sure to mark the beakers to the identify their contents. In small
test tube obtain a very small amount of manganese dioxide, MnOz.
Weigh an empty, clean test tube to the nearest 1 mg. Add half
of*the potassium chlorate in the beaker to the test tube and reweigh.
Add half of the sodium chloride in the beaker to the test tube and
reweigh. Add a tiny amount of the manganese dioxide, which is a
catalyst, to the test tube and reweigh. Be sure to record all
weighings. Shake the test tube to mix the catalyst uniformly
throughout the contents of the test tube.
Support the test tube in a clamp at a 450 angle on a ring
stand. Be sure to choose a clamp whose jaws are not rubber coated to
avoid melting during the heating process. With a hot flame on the
burner, start to heat the upper portion of the sample. The inclined
position of the sample should allow you to control the rate of
decomposition. If rapid decomposition occurs, the sample will
appear to climb the walls of the test tube making good results more
difficult to achieve. After a clear molten liquid has been obtained
in the bottom of the test tube, proceed to heat the upper part of the
tube to ensure complete decomposition. This entire process should
require 10 to 15 minutes. Allow the test tube to cool to room
temperature and weigh to nearest 1 mg. Repeat the heating and
weighing processes until consecutive weighings agree within 0.01 g.
Calculate the actual percent of potassium chlorate in your prepared
sample. Calculate your experimental percentage of potassium
chlorate on the basis of oxygen weight loss from the balanced
equation. Calculate the relative error for your trial. If relative
error is 3% or less, the student has the option of immediately doing
the unknown without a required second trial.
Secure an unknown sample from instructor and weigh to the
nearest 0.001g. Quantitatively transfer the sample to an empty, clean,
weighed test tube and reweigh. Add a small amount of catalyst, MnOz,
and reweigh. Repeat heating and weighing techniques employed on the
known, prepared sample. Calculate and report the percent of potassium
chlorate in unknown sample on the basis of the oxygen weight loss.
34

Data and results tables should be constructed for known and
unknown samples. Sample calculations should be included for known
and unknown samples. Record observations and adjustments made
during procedure to improve results.
Questions
a) catalyst
b ) chemical equation
c) chemical reaction
d ) quantitative
e) stoichiometry
2 . Write the complete balanced equation for the reaction which takes
place when potassium chlorate is heated and gas is evolved.
3. A mixture of 30.0% KC103 and 70.0% NaCl was heated to constant
weight. There was a l o s s of 0 . 7 2 0 g of oxygen. Calculate the
weight of KC103 in the mixture and the original mixture weight.
4 . When MnOz is added to KC103, a characteristic purple color
bften appears during the decomposition. Since MnO2 is black,
use reference sources to explain this observation and cite your
source of information.
5. Potassium chlorate is sometimes used in the manufacture of
matches. Explain the role that potassium chlorate plays in the
chemistry of matches.
I
35
INORGANIC NOMENCLATURE
In order to communicate with chemists internationally, some

standardization of the technical language is needed. In the past
common names for many compounds evolved and are still universally
understood, for example, water, lime, and ammonia. With new
compounds being prepared daily, a random system is no longer
viable. The Committee on Publications of the International Union
of Pure and Applied Chemistry, IUPAC, has generated a system of
rules for naming compounds. The American version of this system
is found in the CRC Handbook of Chemistry and Physics. In this
study assignment, you will learn some rules for naming and writing
formulas for inorganic compounds. You are already familiar with
some symbols for the elements and the names for several common
compounds. For example, NaCl is sodium chloride. Continued
practice and work in writing formulas and naming compounds will
increase your knowledge of the chemist's vocabulary. The
following information is supplied to help you learn the basics of
the language in a systematic manner.
OXIDATION NUMBER
When elements combine to produce a compound, each element is
assigned an "apparent" charge. This apparent charge, the charge
an atom would have if both electrons in each bond were assigned to
the more electronegative element, may be either positive or
negative. It is called the oxidation number or state of the
element in the compound.
Oxidation numbers are very handy bookkeeping devices for
keeping track of what happens to electrons when various elements
combine to form compounds. By remembering a few generalizations
concerning oxidation numbers, the correct chemical formulas for a
large number of compounds can be written and it becomes
unnecessary to memorize disconnected chemical formulas. As in any
system, a consistent s e t of rules must be followed.
Any element in the free state, not combined with another
element, has an oxidation number of zero, regardless of the
complexity of the molecule in which it occurs. Each atom in
Ne, 0 2 , P I , and Se has an oxidation number of zero.
The oxidation number of any monoatomic ion is equal to the
charge on the ion. The ions Ca+2, Fe+3, and Cl- have
oxidation numbers of +2,+3, and -1 respectively.
Oxygen is assigned an oxidation number of - 2 , except in
peroxides when it is -1 such as in H 2 O z and in the
molecule OF2 when it is +2. The oxidation number of
oxygen is - 2 in MgO, Fe203, BaO, and K z O .
36
4. Hydrogen has an oxidation number of +1, except in metal

hydrides such as NaH when it is - 1 . Its oxidation number
is + 1 in H20, NaHSO4 , and H2SO4.
5. Some elements exhibit only one oxidation state in certain

types of compounds:
a. The elements of Group IA (Li, Na, K, Rb, Cs, and Fr)
always have an oxidation number of + 1 in compounds.
b. The elements of Group IIA (Be, Mg, Ca, Sr, Ba, and Ra)
always have an oxidation number of +2 in compounds.
C. Boron and aluminum always possess an oxidation number of
+ 3 in compounds.
a. In binary compounds with metals, the nonmetallic elements
of Group VIA (0,S, Se, and Te) usually exhibit an
oxidation number of -2.
e. In all binary compounds with metals, the elements of
Group VIIA (F, C1, Br, I , and At) have an oxidation number
of -1.
f. In assigning oxidation numbers in compounds, the elements
closest to the most electronegative element, fluorine, in
the periodic table are always given the negative oxidation
number. In the compound N203, oxygen has a - 2 charge.
6. For neutral compounds, the sum of the oxidation numbers of all
the atoms in the compound must equal zero.
Example: Liz Se
2 Li atoms, +1 for each (Rule 5a) = +2
1 Se atom. - 2 for each (Rule 5d) = - 2
Sum of oxidation numbers = o
7. For charged species, ions, the sum of the oxidation numbers of
the elements must equal the charge on that species.
Example: SO4-2
3 0 atoms, -2 for each (Rule 3 ) = -6
1 C atom. must be +4 = +Q
Sum of Oxidation numbers = -2, the ion charge.
a. Some chemical elements show more than one oxidation number
depending on the compound. The rules above may be used to
determine their values. Consider the compounds PbC12 and
PbC14. Since the chlorine atom has an oxidation number of
-1 when combined with a metal (Rule 5e), lead's oxidation
number in PbC12 must be + 2 , whereas it is + 4 in PbC14.
I
37
Consider the compounds H 3 P 0 4 and H 3 P O 3 . According

to Rule 3 , each oxygen atom is - 2 ; but since there is no rule
for the phosphorus atom, it must be determined indirectly.
For H3P04 there are:
3 H atoms, +1 for each = +3
4 0 atoms, -2 for each = -8
1 P atom which, according to Rule 7, must have an
oxidation number equal to + 5 , so that
+3 + ( - 8 ) + ( + 5 ) = 0 ;
and for H3P03, there are:
3 H atoms, + 1 for each = + 3
3 0 atoms, -2 for each = -6
1 P atom which, according to Rule 7, must have an
oxidation number equal to + 3 . so that
+ 3 + (-6) + ( + 3 ) = 0 .
Students will apply these rules to a set of exercises in the

study assignment to become familiar with their usage.
NOMENCLATURE FOR BINARY COMPOUNDS

1 Metal and Nonmetal - Salts. Compounds of two elements are
named directly from the elements involved. In naming a binary
salt, it is customary to list the more metallic or more
electropositive element first. The r o o t of the second element
is then listed with the suffix -ide added to it. NaCl is
called sodium chloride, A1203 is aluminum oxide. The
names of a few exceptions having the -ide ending, but yet
not truly binary compounds, are those that contain the
N H 4 + , O H - , and CN- ions. N h C 1 is ammonium
chloride; NaOH is sodium hydroxide; and KCN is potassium
cyanide.
When a metal cation exhibits more than one oxidation number,
the nomenclature becomes somewhat complicated. Two systems
are used for expressing different oxidation numbers of a
metal. The old system applies a different suffix to the
Latin root name for the metal. The -ous ending designates
the lower oxidation number, whereas the -ic ending indicates
the higher one. The 6econd system, sometimes referred to as
the "Stock" system, uses Roman numerals after the English name
to indicate the metal's oxidation number. Some examples which
illustrate the use of the two systems are iron, copper and
lead salts.
Formula "Old System" Stock System
FeClz ferrous chloride iron(I1) chloride

FeCla ferric chloride iron(II1) chloride
cuI cuprous iodide copper(1) iodide
CUI2 cupric iodide copper(I1) iodide
PbBrz plumbous bromide lead(1I) bromide
PbBr4 plumbic bromide lead(1V) bromide
In naming compounds formed between metals and nonmetals, the
Stock system is the preferred one in chemistry today, however
many chemical manufacturing companies still use old names on
reagent bottles.
2. Two NonmetaI s . Often more than two compounds form from the
chemical combination of two nonmetals. Nitrogen and oxygen,
for example, combine to form NzO, NO, NOz , N203 ,
N z O 4 , and N z 0 5 . It is obvious that these are all
nitrogen oxides, but to identify them individually, Greek
prefixes are used to designate the number of atoms present
in the molecule. Below is a list of common prefixes.
Prefix Heanin4
mono- one
di- two
tri- three
tetra- four
penta- five
hexa- six
hepta- seven
octa- eight
nona- nine
deca- ten
The mono prefix is seldom used, since one is generally
understood unless otherwise specified. The nitrogen oxides
mentioned above are named dinitrogen oxide, nitrogen oxide,
nitrogen dioxide, dinitrogen trioxide, dinitrogen tetroxide and
dinitrogen pentoxide, respectively. Occasionally, part of the
prefix is omitted from the spelling to simplify the
pronunciation. The Stock system is sometimes used in naming
a compound formed between two nonmetals. In this system the
list of nitrogen oxides above would have the names,
nitrogen(1) oxide, nitrogen(I1) oxide, nitrogen(1V) oxide,
nitrogen(II1) oxide, nitrogen(1V) oxide, and nitrogen(V) oxide
respectively. As you can see, the Stock system does not
differentiate between molecular formulas, such as NO2 and
N 2 0 4 , since both are called nitrogen(1V) oxide. It is
suggested that students use prefixes to avoid confusion in
naming and formula writing.
39
3 . Binary Acids. A binary acid is a water solution of a

compound formed between hydrogen and a more electronegative
nonmetal. To name the acid, the prefix hydro- and the
suffix -ic is added to the root name for the nonmetal.
HC1 hydrochloric acid when dissolved in water,
hydrogen chloride as the gas.
HBr hydrobromic acid when dissolved in water.
H2 s hydrosulfuric acid when dissolved in water..
NOHENCLATURE OF COMPOUNDS CONTAINING POLYATOMIC ANIONS
1. Metal Cation and Polvatomic Anion Containina Oxvnen - Salts.
Most polyatomic anions consist of one element which is a
nonmetal and oxygen; the entire group of atoms carries a
negative charge. When a polyatomic anion combines with a
metal to form a salt, the anion is named by using the
element’s root with the suffix -ate. The sulfate ion is
SO4-2, the nitrate ion N03- , and the chromate ion,
CrO4-2. If the element in the polyatomic anion has two
different oxidation numbers the ion having the element with
the higher oxidation number carries the -ate suffix, whereas
the ion containing the element with the lower oxidation number
carries the -ite suffix. For example, SO3-2 in which
sulfur is + 4 is called sulfite and SO4-2 in which
sulfur is +6 is called sulfate. Some examples of typical
salts are properly named in the following list.
Na3 PO4 P is + 5 sodium phosphate
Na3 PO3 P is + 3 sodium phosphite
LiN03 N is +5 lithium nitrate
LiNOz N is + 3 lithium nitrite
K2 Se04 Se is +6 potassium selenate
K2 SeO3 Se is +4 potassium selenite
2. Oxyacids. An oxyacid is a compound consisting of hydrogen
and a polyatomic anion (where one atom is oxygen) dissolved
in water. It is named by adding the suffix -ic to the root
of the element other than oxygen in the polyatomic anion.
Sulfuric acid is H2SO4, nitric acid is HN03, and
chromic acid is HzCrO4. If an element in the polyatomic
anion occurs with two different oxidation numbers in an acid,
the acid having the element with the higher oxidation number
uses the -ic suffix, whereas the acid having the element
with the lower oxidation number uses the -ous suffix. Note
the similarity between the old metal naming system and the
oxyacid naming system. Sulfurous acid is HzSOs and
nitrous acid is HNO2.
40
A comparison of the nomenclature between the salts and acids

containing polyatomic anions shows consistency to the rules
for naming these compounds.
H3As04 arsenic acid K3 As04 potassium arsenate
H3AsOs arsenous acid K3As03 potassium arsenite
HzTeO4 telluric acid Kz TeO4 potassium tellurate
H2 TeO3 tellurous acid K2 TeO3 potassium tellurite
Note that the-ous suffix for the acid becomes the -ite
suffix for the corresponding salt and the -ic suffix for the
acid becomes the -ate suffix in a salt form.
Because of the existence of certain oxyacids in which
oxidation numbers of +7 and + 1 can be assigned to the unique
element in the polyatomic anion, prefixes are added to the
base acid names of the two common oxidation states. A
representative group of acids illustrating this are the
halogen containing oxyacids and their corresponding salts.
HC104 perchloric acid LiClOi lithium perchlorate
HC103 chloric acid LiClOa lithium chlorate
HClO2 chlorous acid LiClOz lithium chlorite
HClO hypochlorous acid LiClO lithium hypochlorite
NOMENCLATURE OF ACID SALTS
Acid salts are salts in which a metal replaces less than the
total number of hydrogens in the parent acid. The presence of
hydrogen is indicated by inserting its name into that of the salt.
KHSOi potassium hydrogen sulfate, one K+ replaces one
H+ in HzSO4
MgHP04 magnesium hydrogen phosphate, Mg+2 replaces
two H+ in H3PO4
NaH2P03 sodium dihydrogen phosphite, Na+ replaces one
H+ in HaPOa
NaHC03 sodium hydrogen carbonate, Na+ replaces one
H+ in HzCO3
The older system of naming acid salts substituted the prefix bi
for the existence of a single hydrogen in the polyatomic anion.
For example, NaHCOs was called sodium bicarbonate and NaHS was
named sodium bisulfide.
WRITING FORMULAS
In writing formulas it is mandatory that the sum of the
elements’ oxidation numbers in the compound always equals zero.
Example - Write the formula for strontium fluoride. From
the Table of Common Names and Oxidation Numbers
you find that strontium exists as Sr+2 and
fluoride as F-. Therefore, in order for the sum
of the oxidation numbers to be zero, the formula
must be SrFz.
41
Example - Write the formula for aluminum sulfide.

Aluminum is A l + 3 and sulfide is S - 2 . The
formula must be A l z S 3 .
Example - Write the formula for potassium dichromate.

Potassium is K+ and dichromate is C r z O r - 2 .
The formul must be KzCrz07.
Example - Write the formula for tin(1V) carbonate.

Tin(1V) is Sn+4 and carbonate is CO3-2.
The formula must be Sn(C0a)z.
42
A. METALLIC ELEMENTS AND POLYATOMIC IONS

Oxidation Number = + 1
NH4+ Ammonium Lit Lithium
Cu+ Copper ( I ) , Cuprous K+ Potassium
H+ Hydrogen Ag+ Silver
Hgz+z Mercury(I),Mercurous Na+ Sodium
Ba+2 Barium Mg+2 Magnesium
Cd+2 Cadmium Mn+2 Manganese(I1)
Cat2 Calcium Hg+2 Mercury(II),Mercuric
Cr+2 Chromium(II),Chromous Ni+ 2 Nickel(I1)
Co+2 Cobalt(II),Cobaltous Pd+2 Palladium(I1)
Cu+2 Copper( 11),Cupric Sr+2 Strontium
Fe+2 Iron(I1) ,Ferrous Sn+2 Tin(II),Stannous
Pb+2 Lead(II),Plumbous Zn+2 Zinc
Al+3 Aluminum co+3 Cobalt(III),Cobaltic
As+3 Arsenic(III),Arsenious Fe+3 Iron(III),Ferric
Cr+3 Chromium(III),Chromic Sc+3 Scandium
idation Number = + 4
c+4 Carbon Si+4 Silicon
Pb+4 Lead(IV),Plumbic Sn+4 Tin(IV),Stannic
Mn+4 Manganese( IV) zr+4 Zirconium
Oxidation Number = + s
As+5 Arsenic(V),Arsenic v5 + Vanadium
I
43
Table I (continued)
B. NONMETALLIC ELEMENTS AND POLYATOMIC IONS

Oxidation Number = - 1
CH3 COO- Acetate or H- Hydril e
c 2 H3 0 2 - Acetate (210- Hypochlorite
Br- Bromide I- Iodide
‘2103- Chlorate NO3 - Nitrate
c1- Chloride NO2 - Nitrite
CN- Cyanide C104 - Perchlorate
F- Fluoride I04 - Periodate
OH- Hydroxide MnO4 - Permanganate
Oxidation Number = - 2
CO3 - 2 Carbonate C204-2 Oxalate
CrO4 - 2 Chromate 02-2 Peroxide
Cr2 07 - 2 Dichromate SO4- 2 Sulfate

s302-2 Dithiosulfate SO3-2 Sulfite
Si03- 2 Silicate s-2 Sulfide
0-2 Oxide Sz 0 3 - 2 Thiosulfate
Oxidation Number - -
BO3 - 3 Borate P-3 Phosphide
As04 - 3 Arsenate PO4 - 3 Phosphate
As033 - Arsenite PO3 - 3 Phosphite
N- 3 Nitride
I
44
ASSIGNMENT
Obtain several sheets of paper from your instructor and

complete the following exercises.
1. Determine the oxidation number of the underlined element in
each of the following compounds or ions.
a. GO m. EC13'
b. GO2 h. QF2 n. SO2
c. LF7 i. NBr3 0. 5Cl2
d. b O 2 p. H2Q2
2. Refer to Table I and locate all cations that have more than
one oxidation number. List them with names according to t h e
"old" system and the Stock system.
3. Name the following compounds.
a. CsF i. Liz S 9. v2 0 5
b. SrBra j. NaCz H3 02 r. NaCN
C. Ca ( BrO3 ) 2 k. ClF3 5 . Cd(0H)z
d. Mg2 N2 1. AgC104 t. Ba(N02 )2
e. SiOz m. Mg2 SO3 U. Na2 0 2
f. P20 5 n. HC 1 V. NH4 C10
8. KMnO4 0. P2 s3 W. NiCz 0 4
h. Na2 CrO4 P. Na3 PO4 X. a1p03
4. Name the following compounds by both "-ous, -ic" and Stock

system.
a. CrS i. Sn(NOa)4 Q. Pb( C204 ) z
b. COP j. CoSiO3 r. FeSOi
C. CrCls k. SnFz S. mn02
d. CuCN 1. Mn(0H)z t. cuc104
e. PbO m. As2S3 U. c0p04
f. Hgz Iz n. HgSz03 V. Hg3 N2
g. cuco3 0. FeB03 W. PbCrO4
h. As2 Os p. Co(N02)z X. As2 (SO3 13
45
5. Name the following as acids.

a. HBr e. H3POa i. H3BOa
b. HClO f. H3AsO4 j. HCN
c. H2S g. HMnO4 k. HNO2
d. H2S04 h. H2CrO4 1. HzCOa
6. Name the following acid salts. Use the older method where
possible.
a. KHSO3 d. KH2AsOa g. NH4H2PO4
b. NaHSO4 e. NaHS h. K2HAs04
c. Ca(HC03)2 f. NaHC03 i. LizHPOa
7. Write formulas for each of the following compounds.
a. Ferrous sulfate 0. Lead(I1) carbonate
b. Potassium permanganate P. Stannous chloride
C. Calcium carbonate 9. Sodium nitrite
d . Iron(II1) oxide r. Barium acetate
e. Cupric hydroxide S. Silver thiosulfate
f. Aluminum sulfide t. Nitrogen triiodide
g. Mercury(I1) chloride U. Potassium iodide
h. Cadmium sulfide V. Sodium silicate
i. Copper(1) chloride W. Calcium hypochlorite
j. Ammonium cyanide X. Potassium chlorate
k. Sodium chromate Y . Cuprous iodate
1. Nickel nitrate 2. Sodium dihydrogen phosphite
m. Manganese(I1) oxide aa. Ammonium oxalate
n. Manganese(1V) oxide bb. Potassium dichromate
8. Write formulas for each of the following compounds.
a. Hydrogen fluoride j. Perchloric acid
b. Sulfuric acid k. Nitrous acid
C. Iodine pentafluoride 1. Silicon dioxide
d. Hydrobromic acid m. Acetic acid
e. Hypobromous acid n. Cobalt(II1) thiosulfate
f. Hydrogen sulfide 0. Nitric acid
g. Sulfur trioxide p. Hydrocyanic acid
h. Phosphorus pentafluoride q. Carbon monoxide
i. Potassium borate r. Chlorous acid
46
MOLECULAR GEOMETRY
A molecule’s structure is necessary to explain its chemical

and physical properties. For example, the fact that water is a
liquid at room temperature, dissolves innumerable salts and
sugars, becomes denser than ice, boils at a relatively high
temperature, and has a low vapor pressure results from its
molecule being bent rather than linear.
Because structure is so important, chemists have developed
theories ‘to explain molecular shapes. In 1916, G . N . Lewis
proposed a theory accounting for the significance of valence
electrons in bonding. He proposed the “Octet Rule” in which
atoms form bonds by losing, gaining, or
sharing enough electrons in order to have
the same number of valence electrons (eight)
a s the nearest noble gas in the Periodic
Table. The bond formed is ionic or covalent
H:O:H m .
depending on whether the electrons are

transferred or shared. The Octet Rule is valid for most compounds
formed between second and third period representative elements.
The Lewis dot structure for HzO shows that by sharing electrons
between the oxygen and hydrogen, all three atoms achieve the same
number of valence electrons as the nearest noble gas. Hydrogen
atoms are isoelectronic with the helium atom and the oxygen atom
is isoelectronic with the neon atom. Lewis dot structures account
only for the valence electrons on each atom and only produce
two-dimensional structures. They do not explain how electrons are
shared, nor do they predict a compound’s actual structure.
VALENCE-BOND THEORY
The basic hypothesis of Valence-Bond Theory is that a
covalent bond forms when adjacent atomic orbitals overlap sharing
pairs of electrons. When these overlapping, adjacent atomic
orbitals point directly at one another, the bond is a sigma-bond.
For example, a sigma-bond forms between a hydrogen atom and a
chlorine atom making the HC1 molecule if the hydrogen atom’s 1 s
atomic orbital overlaps a chlorine atom’s 3p atomic orbital. The
result is a pair of shared valence electrons between two atoms and
sigma-bonding.
47
In 1931, Linus Pauling proposed that the orientation of

orbitals involved in sigma-bonding determines the shape of a
polyatomic molecule or ion. A detailed look at the bonding and
structure of methane, C H 4 , supports this.
The carbon atom’s electronic configuration, Is2 2s2 2p2,
indicates that only two free electrons are available for bonding.
2p- --
2s
11
-
However, for methane all four C-H bonds are equivalent, all H-C-H
bond angles are 109.50, and the structure is tetrahedral in
shape. To account for the CH4 properties, Valence Bond Theory
states that a mixing (hybridization) of the 2s and the three 2p
atomic orbitals (valence orbitals) on the carbon atom provides
four equivalent atomic orbitals, each containing a single electron
that may be used in bond formation with the hydrogen atoms’s
atomic orbitals. See the figure below.
2p- -- Hybridization t -
- f 9-. -
f
41
2s -
I+ 1
Four sp3 orbitals
This hybridization is called sp3, one s and three p atomic

orbitals. Each hydrogen atom 1s is atomic orbital overlaps with
one sp3 hybridized atomic-orbital on the carbon atom forming a
sigma-bond. The four C-H bonds are oriented in space as a
tetrahedron to diminish electrostatic interaction between the
hydrogen nuclei. See the following figure. For some molecules, a
- pair(s) of non-bonding electrons in the central atom’s valence
shell occupies a hybridized orbital(s). Because this hybridized
orbital(s) is the same as the hybridized orbitals which form
sigma-bonds, it also contributes equally to the molecule’s
geometry.
48
Therefore, the orientation of all hybridized valence shell

orbitals (those forming the sigma-bonds and those containing
pairs of non-bonding electrons) determines a molecule’s
gdometric shape. A summary of hybridization models for valence
shell orbitals and corresponding geometries are illustrated in
Table I.
VALENCE SHELL ELECTRON PAIR REPULSION(VSEPR) THEORY
VSEPR Theory proposes that a molecule’s geometry is
determined primarily by the repulsive interaction of electron
pairs in the valence shell of its central atom. The orientation
is such that their separation of the electron pairs is maximized
and the electrostatic interactions minimized.
In methane, C H 4 , the carbon atom, the molecule’s central
atom, has four bonding electron pairs in atom’s valence shell.
Repulsive interactions between these four pairs decrease when
they are arranged in a tetrahedral geometry. One can generalize
that all molecules having four electron pairs in the valence shell
of its central atom have a tetrahedral arrangement of electron
pairs. This arrangement is also true for the oxygen atom in H2O.
The preferred arrangement of bonding electron pairs around
the central atom gives rise to the corresponding geometric shapes
of the molecules. In addition, the number of non-bonding pairs
affects the orientation of these bonding electron pairs. The
various molecular shapes are in Table I, using the following VSEPR
notations:
A - refers to the central stom
X - refers to number of bonding pairs of electrons on A
E - refers to number of nonbonding pairs of electrons on A .
If a molecule has the formula AXmEn, it means there are
m + n electron pairs in the central atom’s valence shell -
m bonding and n non-bonding electron pairs. The general shapes
,possible are linear, trigonal planar, tetrahedral, trigonal
bipyramidal, and octahedral indicating a total of 2, 3 , 4 , 5, and
6 electron pairs on the central atom respectively.
I
49
POLARITY
Once a molecule’s three-dimensional structure is determined,
its degree of polarity can be established. If a bond forms
between two atoms having different electronegativity values, the
bond is polar. The magnitude of this difference in the bonded
atoms measures the degree of the bond’s polarity. A vector, the
dipole moment, represents this difference. For example, HF is
more polar, that is, has a greater dipole moment, than HC1 because
the fluorine atom is more electronegative that the chlorine atom.
If more than one polar bond exists in a molecule, the entire
molecule may be polar or nonpolar, depending on its 3-dimensional
shape. Consider the two molecules, BF3 and H 2 O . The BF3
molecule has the VSEPR formula A X 3 , where each bond is polar.
T a b l e I shows that the BF3 molecule has a trigonal planar
geometric shape. The three fluorine atoms attract the bonding
0 .
electron pairs from the boron atom with equal magnitude. As a

result, the geometric sum of the dipole moments of the molecule’s
three bonds is zero, and the molecule is nonpolar, even though
each B-F bond is polar. The HzO molecule has the VSEPR formula
A X 2 E 2 , and each bond is polar. Table I shows that H2O has
H H
a V-shaped geometry. Since the geometric sum of the bonds’ dipole
moments in the molecule is not equal to zero, the molecule is
polar.
The LikQncss o f Valence Bond ThQorY t o VSEPR ThQorY
VALANCE BOND THEORY VSEPR THEORY
Valance
Shell
Non-bondin6 Electron VSEPR Electron-Pair Geometric
Example
Hybridization Orientation Shapes
thbilats Pairs Formula
,-..--.-.-...
linear
trigonal
planar
3
V-shaped
a-.-..--.-.-.
tet rahedral
t rigonrl
4 AX, E pyramidal NH,, PCI,, H,O+
I
&
V-~haped
2
.------.....-*
trigonal
~
0 by pyramidal
irregular
5 AX4 E tetrahedral ‘SF4, TcCl.
I sp’d
T-shaped ClFs
1
linear la;. XcF,

I
-------- --.-----...-
octahedral
square
I rp’d’ 6 BrF,
pyramidal
2
I
- squire
planar
ICI;. XeFI cn
0
I
51
In this study assignment, a series of molecules and ions

will be given as formulas with the central atom underlined.
Students will write Lewis structure and determine hybridization of
the central atom’s valence shell orbitals, the VSEPR formula, and
the molecule’s geometric shape and polarity.
ASSIGNMENT
With the help of Table I and molecular models, construct the
following molecules or ions and write the Lewis formula.
Determine the hybridization of the central atom’valence shell
orbitals, VSEPR formula, geometric shape and polarity. The
molecule, CF4 is down as an example. On a separate sheet of
paper, construct a table similar to Table I for the following
molecules and/or ions.
EXAMPLE
Molecule Lewis Formula
or Ion ..
Bonding Orbitals or pairs 4
1. CF4 .. .. ..
: F :
t.-nbondingOrbitals or Pairs 0
: F : C : F :
.. .. .. ti;,. ridization: s P3
v’; L L. Formula: AX4
,
..
: F : Geometric Shape: tetrahedral
Polar or Nonpolar: nonpolar
3-D Structure
F
2 . cH3C1 7 . &F2 1 2 . BF4-

3. H3Q+ 8. kF4 13. EF5
4 . BH3 9. E C 1 2 F 3 14. 204-3
5 . uH4+ 10. &F3 15. sF6-2
6. SF4 11. u 0 2 - 1 6 . SF6
Questions
1. Regardless of which theory of covalent bonding is used, the
predicted molecular shape of a given molecule or ion is the
same. Comment on the the rationale for having several
different bonding theories in lieu of one particular accepted
theory.
2 . A pi-bond (VB theory) or a double-bond (VSEPR theory) does
not affect a molecule’s geometric shape.
a. What hybridization of valence shell orbitals on the S and
C atoms in SO2 and C O 3 - 2 are predicted? Draw the
Lewis formula for each.
b. What geometry would you predict for SO2 and C O 3 - 2 ?
I
52
LXMITING REACTANT
Many times an analysis will be based on the fact that you have
a limiting reactant involved in the chemical reaction. The limiting
reactant determines the percent yield of product. Because chemicals
react stoichiometrically, only a limited amount of product forms from
given amounts of reactants. For example, the analysis of a sample
containing soluble sulfate salt such as sodium sulfate can be
performed by dissolving the sample in water and adding a solution
containing barium chloride to form an insoluble barium sulfate salt
NazS04(aq) + BaClz(aq) --> BaS04(s) + 2NaCl(aq)
and sodium chloride which is soluble. Since all of the salts, except
BaS04, are soluble, the net ionic equation for the chemical
reaction is b
Ba+2(aq) + SO4-2(aq) --> BaS04(s).

One mole of barium ion, from BaC12-2H2O (244.2g) in solution,
reaets with 1 mole of sulfate ion, from 1 mole of Na2SO4 (142.lg)
in solution, to produce 1 mole of barium sulfate precipitate (233.4g)
if the reaction takes place completely. The reaction is referred to
as being quantitative since it will allow the determination of the
amount of sodium sulfate in the sample. Sodium sulfate is the
limiting reactant and to ensure that a total, complete reaction takes
place an excess of barium chloride solution is added.
A 1.000 g sample of unknown salt mixture containing sodium
sulfate is weighed to the nearest 1 mg. The number of moles of
sodium sulfate are calculated as if this were a pure sample of the
1 . O O O g NazS04 X 1 mole NazS0 4 = 7.030 x 10-3
142.1 g NazSO4 moles Na2SO4
sodium sulfate, thus representing maximum number of moles of sodium
sulfate which may be present in the sample. Using the balanced
equation
1.00 mole sO4-2 produces 1.00 mole of Bas04
or
7.030 x 10-3 mole Sod-2 produces 7.030 x 10-3 mole Bas01

and
7.030 x 1 0 - 3 mole Bas04 x 233.4 LI R as04 = 1.641 g
1 mole Bas01 Bas04
53
Thus, 1.641 g Bas04 represents the maximum amount of precipitate that

can be formed if the sample is 100% pure. This is referred to as the
theoretical yield of the product. Since the sample is not pure
sodium sulfate, you will obtain less than the theoretical amount
which we will call the experimental value. The percentage of sodium
sulfate in the unknown can be calculated using the percent yield
formula which is defined as:
percent yield = experimw
' tal Yield x 100
theoretical yield
Many industrial products such as food ingredients, deodorants]
mineral waters, and cosmetics would use this procedure for analysis
of sulfate ion.
In this experiment an unknown salt mixture containing NazSO4
is analyzed for the percentage of NazS04 by adding excess BaClz
solution to ensure completeness of reaction. The other ingredient in
the mixture is a nonreactive, soluble substance which will not
interfere with the quantitative reaction. The precipitate, BaSO4,
wi1.l be vacuum filtered, dried, and weighed to obtain experimental
yield of BaSO4. The theoretical yield will be based on 100% activity
of the salt mixture sample weighed.
Procedure
Weigh a clean, empty 400 ml beaker to the nearest 0.001 g. Add
about 1.0 g of the unknown salt mixture to the beaker and reweigh
the beaker to the nearest 0.001 g. Calculate the number of moles of
sodium sulfate that theoretically are contained in this sample
weight. Also calculate the theoretical yield of Bas04 as
demonstrated in the introduction section of this experiment. Add
200 ml of distilled water to the beaker and stir with a stirring rod.
In the hood, measure 1 ml of concentrated HC1 in a small graduated
cylinder and with the aid of a stirring rod add to the solution in
the beaker. (CAUTION: If spilled concentrated HC1, hydrochloric acid,
is a severe skin irritant-flush affected area with large amounts of
water. Check MSDS of hydrochloric acid and include other handling
precautions and spill and disposal procedures in your notebook.)
In graduated cylinder, measure 50 ml of 0 . 5 M BaClz and add to the
solution in the beaker and stir for several minutes with a stirring
rod. Allow the precipitate to settle. Verify that the amount of
barium chloride added to the solution does, in fact, represents an
excess of the reactant.
With the stirring rod in the beaker, cover the beaker with a
watch glass and place the entire apparatus on a hot plate. Heat at
low setting to maintain solution temperature between 80 - 9 O o C for
1 hour. Check the temperature of the solution with your thermometer
oocasionally. Avoid boiling the solution. Heat approximately 100 ml
of distilled water in a beaker to be used as the washing solvent.
Refer to filtration techniques in the Physical Separation of Mixtures
experiment or pages 266 - 268 in Chemical Technician's Ready
Reference Handbook, CTRRH.
54
While the solution is heating, assemble the vacuum filtration

apparatus. Two types of filters will be used: a Buchner funnel with
a paper filter and a fritted glass filtering crucible. Students should
read pages 272 - 276 in the CTRRH. The advantage of vacuum
filtration is the speed of isolation for a solid product from
solution. One trial will be done recovering the precipitate on the
paper and a second trial will recover the solid in the filtering
crucible. It will require the recorded weight of both, paper and
crucible. The order in which these two isolation methods are done
is not a significant factor.
Before the filtration process is started, tip the beaker and
allow the precipitate to settle under the lip of the beaker. While the
solution is still hot, using beaker tongs, decant the supernatant
liquid trying to minimize solid transfer to the filter. Wash the
precipitate several times with warm distilled water, using a rubber
policeman to remove any solid adhering to the sides of the beaker.
Using the wash bottle, transfer the precipitate to the filtering
medium and rinse several times with the warm distilled water. Allow
air. to be drawn through the filtering medium for several minutes
after the last rinse. Break the vacuum seal at the filtering flask
and remove the filtering medium to a clean, dry, preweighed, marked
watch glass. Place the watch glass and filtering medium in drying
oven for several hours or overnight. When the precipitate is dry,
allow it to cool and weigh watch glass and filtering medium.
Calculate the weight of Bas04 isolated. Calculate the percent
yield of the reaction. Report the average percentage yield on two
trials.
Following the established guidelines for the report and in the
conclusion section compare the two vacuum filtering mediums with
respect to their advantages and disadvantages.
Quest ions
a) ionic equation
b) molecular equation
c) net ionic equation
d) spectator ion
e) supernatant liquid
2 . The solublity of the precipitate, BaSO4, is 1.05 x 1 0 - 5 M in water
at 2 5 0 C . Based on a total volume of 250 ml,
a) how many moles of Bas04 are not isolated in the precipitate?
b) how many grams of Bas01 are not isolated in the precipitate?
c) how significant is this weight in relationship to the
measurement you can make?
3 . Since Bas04 is a finely divided precipitate, some may be lost
during the filtration process if coarse filter paper is used. How
. would this affect the reported percent yield? Explain.
4 . What is the purpose of washing the precipitate?
5 . If NaaPO4.is an unknown contaminant of the salt mixture, how would
this affect the yield of Bas04 in the experiment? Baa (PO4 12 is
insoluble also. Write balanced equations as part of your
explanation.
55
PERCENT OF OXYGEN IN AIR
This is a simple experiment which may be used to introduce

students to the need for monitor conditions when measuring gases.
Air is a homogeneous mixture of gases such as nitrogen, oxygen,
argon, and trace amounts of other elemental gases and carbon dioxide.
The amounts of each gas can be measured both by weight and volume to
determine the percent composition. In this experiment, the students
will measure gas volumes using gas measuring burets. A 50 ml sample
of air undergoes a chemical reaction in which only the oxygen is
consumed. Consequently, the measurement of the original volume of
air minus the remaining volume of gas after the reaction results in
the volume of oxygen. To calculate the percent of oxygen, the
volume of oxygen is divided by the air sample volume times 100.
Since gases are very sensitive to changes in temperature and
pressure, the students should carefully note atmospheric pressure,
labaratory and water temperatures. The instructor will demonstrate
the-use of a mercury barometer. The students are required to read
pages 4 7 9 - 4 8 2 in the Chemical Technician Ready Reference Handbook,
CTHRH. The two reagents used in this experiment are a 1M NaOH
solution and pyrogallic acid. Each should have the MSDS precautions
for use listed in the laboratory notebook.
Procedure
To ensure that exactly 50 ml of air will be taken in this
experiment, the volume of the sodium hydroxide solution used, will be
equal to the volume between the 50 ml mark on the gas measuring tube
and the bottom of the rubber stopper used to close the tube. To
determine this volume, fill the tube with water so that the meniscus
is at the 50 ml mark. Insert a rubber stopper and mark, with tape,
the position of the stopper’s bottom. This will allow you to
reproduce the exact volume each time. Invert the tube and read,
using the graduations, the volume of air which was between the
bottom of the stopper and the 50 ml mark. This is the exact volume
of sodium hydroxide solution to use each time. Empty the water out
of the tube. Pour sodium hydroxide solution into the buret and use a
medicine dropper to get to the exact volume measurement required.
Measure 0.58 of pyrogallic acid on a weighing paper and add it to
the tube. Quickly close the tube inserting the stopper to the marked
position. Invert the tube several times to ensure thorough mixing of
the solution and solid. Record your observations. Gently rock the
solution back and forth in the tube for several minutes. Record the
laboratory temperature.
56
Plug a lab sink with an overflow device and fill sink to the top
of the overflow. Record water temperature in the sink. Adjust the
temperature of water in the sink to the laboratory temperature using
a mixture of warm and cold tap water. Submerge the stoppered end of
the tube and remove stopper. Note how water is forced in to replace
the oxygen. .Allow the tube to cool in the water for several minutes,
then raise or lower the tube so that the water levels, inside and
outside the tube, match. It is not necessary to correct the gas
volumes to STP in this method because all operations are done within
a few minutes. However, if there is a significant difference between
laboratory temperature and the water temperature in the sink, use
Charles’ L a w to correct the volume of the gas remaining in the tube.
It is left for the student to calculate what represents a significant
temperature difference. The atmospheric pressure should also be
monitored periodically during the laboratory period to ensure that a
s i g n i f i c a n t pressure change is not taking place due to weather
changes. Student can calculate what would represent a significant
change by using Boyle’s Law. Repeat the procedure a minimum of
three times.
Calculate the average percentage of oxygen in the air. Check the
CRC. Handbook or suitable reference for the actual percentage of oxygen
in air. Calculate the percentage of relative error in your
determination.
Requirement for Report
Use established format for reporting results of the experiment.
Please note all observations and significant temperature and pressure
calculations you are required to make.
Quest ions
1. Why are the water levels inside and outside the tube matched?
2 . Which correction factor, temperature or pressure, would have a
greater effect on your experimental data? Explain.
3 . If 50 ml of air is analyzed according to the above procedure and
the remaining volume of gas is 4 8 . 5 ml;
a) what would be the percent of oxygen and the percent error?
b) what factors could have contributed to this percent error?
c) if laboratory temperature was 200C, what would the water
temperature have to be to totally account for the error?
d) is the temperature calculated in c) a realistic value to
explain the error? Comment.
4 . What is another name for pyrogallic acid? What is its chemical
formula?
I
57
GRAM MOLECULAR WEIGHT OF CARBON DIOXIDE
Carbon dioxide occurs as a variable component in the

atmosphere. It is formed by the decay, fermentation, and
combustion of organic matter. In this experiment, carbon dioxide
will be produced by reacting marble chips, predominantly CaC03,
with hydrochloric acid. To obtain dry carbon dioxide, the gas is
bubbled through a concentrated sulfuric acid which acts as a
dessicant and collected in an Erlenmeyer flask.
The procedure involved in the determination of the molecular
weight of carbon dioxide is called the gas density or vapor
density method. In some texts it will be referred to as the
Dumas method named for the Frenchman who is given credit for
originating the method. It is based on the principle that equal
volumes of gases contain the same number of molecules at the same
temperature and pressure. This principle represents Avogardo’s
Law which has been used to define a standard molar volume of any
gas, 2 2 . 4 liters, at 1 atmosphere pressure ( 7 6 0 torr) and 273 K
(OoC). The ideal gas law, PV = nRT when solved for volume at STP
defines this standard volume. If n, number of moles, in the ideal
gas law is redefined as mass of gas/gram molecular weight (GMW)
the formula can be rearranged to solve for the gram molecular

weight by using measured values obtain in the laboratory for any
PV
gas sample. The variables in the formula are mass (grams), R -
gas law constant (0.0821 liter-atm/mole-K), T - temperature
(degrees Kelvin), P - pressure (atmospheres), and V - volume
(liters). Alternatively, the volume of gas measured at laboratory
conditions could be corrected to the volume which it would occupy
at STP. A simple proportion relationship would then be used to
mass of collected aaS = GMW
volume occupy at STP 2 2 . 4 liters
solve for the GMW.

Procedure
Take two clean, dry, marked Erlenmeyer flasks and obtain
~ rubber stoppers that fit each tightly. Stopper the flasks and
mark the bottom position of the stopper with a piece of tape.
Weigh the flasks to the nearest 1 mg and record the weight.
Record the laboratory temperature and pressure. Using CRC
Handbookof Chemistry and Physics, record the density of air at
laboratory conditions.
58
In the fume hood, set up the apparatus as shown in the

following diagram. This will require that a number of right a n g l e
glass bends must be produced by you. The student should read
glass cutting (830 - 8321, glass polishing (835 -836) and glass
bending (840 - 841) in the Chemical Technician's Ready Reference
Handbook, CTRRH. Remember to lubricate glass with glycerin
before inserting it into the tubing or stoppers. Place 40 g of
marble chips in a generating flask and place approximately 30 ml
of concentrated sulfuric acid, HzSO4 , in the bubbler bottle.
oc
Be sure to check all of the rubber and glass tubing for

constrictions or blockage as the apparatus is assembled. Use a
a paper punch and 3 by 5 index card to make the paper cover for
the collection flask. Making sure that the screw clamp is closed
between the funnel and generator, add approximately 50 ml of
6M HC1 to the funnel. The liquid level in the funnel should never
exceed three-fourths of its total volume capacity nor should it be
allowed to drain completely since air would enter the generator.
Record in your laboratory notebook the handling precautions, and
the spillage and disposal procedures for all chemicals used in
the experiment from MSDS notebook.
Opening the screw clamp slightly, allow the HC1 solution to
pass from the funnel onto t h e marble chips. A moderate rate of gas
generation should be maintained and can be monitored by watching
the bubbler bottle. The generator should be carefully shaken
occasionally to avoid the'use of an unnecessary excess of HC1.
Permit the gas to flow for 5 minutes to ensure the displacement of
air in the apparatus. Touch the bottom of the generator flask and
record the temperature effect. Remove the paper cover and delivery
. tube from the collection flask and quickly insert a rubber stopper
to the marked position. Insert the delivery tube into a second flask
to collect a sample while weighing the first flask to the nearest
0.001 g. Alternate sample collection in this fashion until a
constant weight ( 5 0 . 0 0 5 g) is obtained for both flasks. When
all mass measurements have been completed, fill each of the
59
flasks with water to the marked position and measure the volume of
water using a graduated cylinder. To disassemble, first loosen
stopper on the generator flask to avoid siphoning concentrated
sulfuric acid into the generator. Drain the HC1 from the funnel
into a beaker and use proper disposal procedures for excess acid in
the beaker, generator and bubbler bottle. R e m e m b e r that
concentrated solutions are always poured into more diluted solutions.
To determine the weight of carbon dioxide it is necessary to
calculate the weight of air in the flasks at the initial weighing.
The density of air at laboratory conditions is multiplied times
the volume of the flask to obtain mass of air. The mass of air is
then subtracted from the initial flask weight to obtain weight of
the stopper and flask. This is used to determine the mass of carbon
dioxide collected. Using one of the two methods outlined in the
introduction, calculate the gram molecular weight of carbon dioxide
for each trial and the average value. Calculate the relative error
for your results.
Exchange two clean, dry 250 ml flasks at the stockroom for
two filled with samples of unknown gases. Do not disturb the
'stopper or warm the flask unnecessarily by handling. Mark the
position of the stopper and weigh to nearest 0.001 g. In the hood
remove the stopper and displace the unknown gas with laboratory
air by use of the aspirator. Replace the stopper and weigh the
flask of air accurately. Fill the flask with water to the mark
and measure the volume using a graduated cylinder. Repeat the
calculations that were necessary to determine the gram molecular
weight of carbon dioxide.
Follow the guidelines fo,rexperiment writeup. Be sure to
included unknown sample identification numbers in the report.
Questions
1 . What evidence did you observe during the experiment which would
enable you to decide whether the reaction generating carbon
dioxide is exothermic or endothermic? Explain.
2. If the carbon dioxide were not dried, would this tend to result
in experimental values for the gram molecular weight to be too
large or too small? Explain.
3. State clearly as many practical uses for the gram molecular
weight of a substance as you can.
4. The most common drying'agent used in laboratories is anhydrous
calcium chloride. Would this be a suitable substitute for the
concentrated sulfuric acid used as a dessicant in this
experiment? Explain.
~ 5. Since the laboratory air contains some water vapor, the density
which you obtained from the reference is not the exact density
of the laboratory air. Will this tend to cause your value for
the gram molecular weight of carbon dioxide to be too high or
too low? Outline your reasoning in coming to your conclusion.
60
EQUIVALENT WEIGHT OF AN UNKNOWN METAL
In the early development of the periodic table, the mass of

elements were established by the Law of Combining Weights. It
simply states that the number of grams of any element that will
combine with, or displace 1.008 g of hydrogen or 8.00 g of oxygen.
This mass is also known as the gram equivalent weight (GEW) of the
element. Many of the metals on the periodic table, but not all,
react with acid to form hydrogen gas which may be collected and
measured. The chemical equation for zinc metal reacting with
Zn(s) + 2HCl(aq) --- > ZnClz(aq) + Hz(g)
hydrochloric acid illustrates the type of reaction which takes
place. Analyzing the equation, we observe that 1 mole of zinc
produces 1 mole of hydrogen gas. In terms of mass, o n e gran;
atomic weight (GAW) of zinc, 65.37 g, produces two GAW’s of
hydrogen, 2.016 g. Therefore, the GEW of Zn is equal to one h a l f
the GAW, by definition. We can also relate the volume of the gas
1 GAW of Zn = 2 GAW 8
65.37g 2.018g
1 GEW of Zn - 1 GAW B
32.69g 1.0O8g
collected to the GEW of the metal since 1 mole of any gas at STF
occupies 2 2 . 4 liters. Because hydrogen is a diatomic gas its
standard molar volume actually represents 2 equivalents of
hydrogen or 2GAW’s. Therefore, 1 equivalent of hydrogen will
always be equal to 11.2 liters at STP. Since the number of
equivalents of hydrogen will always be equal to the number of
equivalents of metal, we can determine the GEW of an unknown
metal. Note that the units on the GEW (g/equivalent) are similar
GEW of metal = mass of metal,

number of equivalents
to units on units on GAW (g/mole). Students should a l s o observe
the correlation between the oxidation number of the metal. In the
case of Zn, and one mole of zinc always equals two equivalents of
zinc. Zinc always has a +2 oxidation number, therefore the gram
equivalent weight of a metal can be determined by dividing its
gram atomic weight by the oxidation number.
61
To calculate the volume of hydrogen gas produced from the

reaction, the student may use the Ideal Gas Law relationship, PV =
nRT, or Combined Gas Law relationship, Pi Vi /Ti = PzVz/Tz .
Regardless of which relationship is used, the laboratory pressure,
Ft, must be corrected for the vapor pressure of water since the
Pt = Pgas + Pwattr vapor
hydrogen is collected by displacing water from a collection flask.

The vapor pressure of water at the laboratory temperature can be
determined from a table in the CRC Handbook or other reference
source. Students are encouraged to run through the procedure
using zinc metal as a known until the relative error of their
results are within 3%.
Procedure
Obtain a sample of unknown metal from the instructor. Weigh
it to the nearest 1 mg. Tie a string around the metal sample.
Set up the apparatus shown in the illustration above. The

apparatus consists of a 125 ml Erlenmeyer flask with a one hole
rubber stopper attached by rubber and glass tubing to a 500 ml
Florence flask, filled with water, which is supported in a water
trough. Place 50 m l of 6M HC1 in the Erlenmeyer flask and suspend
the metal sample on the string above the acid solution by using
the rubber stopper to hold it in place. Clamp the flask in an
upright position and attach rubber tubing to the glass tube
extending from the rubber stopper. On the other end of the rubber
tubing attach a short right angle glass tube to act as a delivery
tube to the Florence flask. Submerge the delivery tube in the \
. water trough to eliminate air in the end of the tube and insert
it into the flask. Record the laboratory pressure.
62
When ready to start the reaction between the metal and a c i d ,

tip the flask to about a 4 5 0 angle so that the sample contacts
the acid solution. Allow the reaction to proceed to completion.
Remove the delivery tube from the collection flask. Before
removing the Florence flask to measure the volume of gas
collected, allow the gas to stabilize to the water temperature by
standing for 10 minutes. Record the temperature of the water
trough. Remove clamp from collection flask and tip to the side,
keeping the mouth of the flask submerged. Match the water level
inside the flask to the level in the trough. Slip a glass plate
over the end of the flask and remove it from the trough. Measure
the volume of water remaining in the flask using a graduated
cylinder. Completely fill the Florence flask with water and
measure its total volume capacity.
Repeat the procedure for a second sample and report the
average equivalent weight of the sample. Some educated guesses
can be proposed for the identity of the unknown sample. When two
trials have been completed, consult MSDS information on disposal
of excess HC1 and record it in your laboratory notebook.
The information collected on the known zinc sample must be
included in the report along with the percent error achieved on
the results. Follow the established guidelines for the report.
Questions
1. If the volume of collected hydrogen is mistakenly recorded to
be higher than actual, how does this affect the reported
equivalent weight of the metal? Explain.
2. If all connections in the apparatus are not air-tight and some
hydrogen gas escapes, is the reported equivalent weight larger
or smaller than the actual value? Explain.
3. If several air bubbles are trapped in the collection flask
before the reaction for the sample is started, how would you
correct the problem? If you did not observe these air bubbles
until after the reaction was started, how would this affect the
equivalent weight of the metal? Explain.
4 . A 0.375 g sample of a metallic element is completely dissolved
a 100 ml of 0.500 N sulfuric acid. The liberated hydrogen gas
occupied a volume of 350 ml when collected over water at 25oC,
and the pressure was equalized to the atmospheric pressure of
750 torr.
a) Calculate the equivalent weight of the metal.
b) How many equivalents of acid were used to produce the
hydrogen gas?
c) How many equivalents of acid remain in the solution?
63
RELATIONSHIP OF TEMPERATURE AND PRESSURE TO CHANGE

I N PHYSICAL STATE
A substances may exist in solid, liquid or gaseous state.

The transition of matter from one of these states to another
requires that a quantity of heat be absorbed ( or released) and is
often difficult to measure with equipment available in a general
chemistry laboratory. However, an indication of heat transfer may
be obtained by monitoring the intensity factor, temperature.
The vapor pressure of a liquid is the pressure exerted by the
vapor or gaseous form of the liquid when the vapor and liquid are
in equililbrium with each other at a specified temperature. When
the two states are in equilibrium, there is no change in pressure
if the temperature remains constant; however, if the temperature
is increased,the vapor pressure of the liquid increases.
The normal boiling point of a liquid is the temperature at
which the vapor pressure of the liquid is exactly 1.00 atmosphere.
Since the pressure acting on the surface of the liquid may differ
Irom l . U O atm, the actual temperature at which boiling occurs may
not be the same as the normal boiling point. When liquid boils
in an open container, the pressure acting on the surface of the
liquid is the prevailing barometric pressure. In a closed
container from which air has been removed, the pressure acting on
the liquid is that of the vapor itself. In the process of
evaporation, a liquid vaporizes at the surface only; in boiling,
vapor is formed in bubbles within the liquid as well. The
temperature stays at the boiling point as long as any liquid
remains. The absorbed heat is consumed in overcoming the
attractions between molecules of the liquid and in forcing the
vapr;r sut against the atmospheric pressure. Thiz quantity of
absorbed heat, when expressed in calories per gram of liquid, is
referred to as the specific heat of vaporization. Chemists also
use the term molar heat of vaporization which is the quantity of
heat, in calories, required to convert one mole of liquid to vapor
at the normal boiling point. The quantity of heat energy required
to overcome the cohesive forces of the molecules in the liquid is
different from one liquid to another, but the quantity of heat
used in overcoming atmospheric pressure depends only on the
temperature and on the number of moles of liquid vaporized.
The freezing point of a pure liquid is the same as the
melting point of the corresponding solid when the substance is
pure. ThIs may be defined as the temperature at which pure
liquid is in equilibrium with pure solid at some specified
pressure, usually 1.00 atm. When the two states are in
equilibrium, the solid and liquid coexist with no change in their
. relative amounts with time. For reasons analogous to those
discussed in the preceding paragraph, the temperature remains
constant at the freezing or melting point until the change in
state is complete. The quantity of heat energy required to
.convert a solid to a liquid, when expressed in calories per gram,
64
is referred to as the specific heat of fusion. Similarly, the

molar heat of fusion is the number of calories required to convert
one mole of the pure solid to liquid at a specified pressure.
Procedure
Section A
Wrap a small piece of Kimwipe or Kleenex around the bulb of a
thermometer and fasten securely with a fine copper wire or rubber
band. Record the temperature of the room by simply reading the
thermometer. Then dip the covered bulb of the thermometer in
methanol. Remove the thermometer from the liquid and suspend in
the fume hood. Watch the mercury and record the lowest
temperature. CAUTION: All liquids used in this section of the
experiment are flammable and can constitute a combustion hazard.
Check the MSDS notebook for the precautions, spillage and disposal
procedures of all chemicals used in this experiment and record in
your notebook.
Repeat these steps using the following liquids: propanol,
isopropanol, acetone, diethyl ether, pentane, hexane, and water.
Use a fresh piece of Kimwipe with each liquid. Using the CRC
Handbook or suitable reference source, record the normal boiling
poigts of all the liquids.
Section B (
Before assembling the apparatus shown in the figure below,

make certain that the heat resistant glass test tubes are clean.
65
Remember to lubricate glass tubing and thermometers before

inserting them into rubber stoppers. Do not attempt to change the
position of the thermometer during the course of the experiment.
Heat the water in both tubes to the boiling point with a moving
flame. Continue the boiling until steam venting from the delivery
tube gives a peculiar crackling sound and bubbles of gas no longer
rise through the liquid in the beaker. Observe the change in
the size of the bubbles as this condition is approached. At this
point both thermometers should register nearly l O O o C and should
agree within l o .
Close the screw clamp and immediately remove the flames from
both tubes. Seal the rubber stopper with a ring of water where
the stopper meets the test tube as a means of detecting any
leakage. If leaks occur, the apparatus must be reconstructed and
the experiment repeated. When the temperature has fallen to 9 O o C
in the closed tube, note the temperature in the other tube, and
record both values. Readings of the thermometer m ~ s tnecessarily
be omitted while the mercury in the thermometer is obscured by the
stopper. Below the stopper, visibility may be clouded by
condensed water droplets. To remedy this situation, rock the
assembly stand until the water from the lower part of the tube
washes away the droplets. Record similar observations at
subsequent 100 intervals until no boiling is observed in either
tube. The water will continue to boil in the closed tube down to
at least 6 0 o C and often a much lower temperature. If such results
are not obtained, reconstruct the apparatus and repeat the
experiment. During the course of the experiment, touch the upper
part of both tubes and compare the temperature effects. Record
the lowest point at which boiling occurred. At this point, cool
the upper part of the closed tube with a stream of cold water from
a wash bottle. Observe the rubber tubing connection on the
delivery tube, Release the screw clamp with the delivery tube
under water and record your observations in your notebook.
Section C
Place approximately 10 grams of crystalline sodium
thiosulfate pentahydrate in a dry test tube and immerse the lower
half of the tube in a water bath which has a temperature above
70oC. When all the solid has melted, remove the tube from the
water bath. Stir the melted s a l t continuously with the
thermometer. Record the time and the temperature readings at one
minute intervals until the temperature has fallen to 50oC. At
this time, add a crystal of the salt to prevent undercooling.
Continue to stir and record time and temperature readings for about
ten minutes after solidification begins.
Reheat the thiosulfate in the hot water bath until all solid
-material has melted. All solid particles adhering to the walls of
the tube must be melted or removed. Remove the the test tube from
the bath and cool it under running water until the temperature is
below 40oC. Observe and record the time and temperature.
66
Discontinue the cooling of the tube and drop a small crystal of the
sodium thiosulfate into the melted material. Stir with the
thermometer. Record the temperature and time every 30 seconds until
the temperature of the mixture reaches a maximum. Then continue the
observations at five minute intervals until the temperature has
fallen to about 430C.
Reauirements for Report
For information in Section A , construct a table containing the
names of the compounds, compound’s structure’ compound’s polarity,
compound’s formula weight, compound’s normal boiling point, and
compound’s lowest temperature observed. For the data collected in
Section B, report the lowest temperature at which the water boiled
in the open and closed tube. The data collected in Section C ,
should be presented in a graph using temperature a s the ordinate and
time as the abscissa. Both data groups may be plotted on the same
graph.
Quest ions
1. On the basis of observations recorded in Section A , make a
statement regarding the relationship between the boiling points
of liquids and their effectiveness in cooling by evaporation.
2. What other factors included in the table of information for
Section A appear to have a relationship to effective cooling.
3 . Considering the observations in Section B:
a) Why did the rubber delivery tube collapse during the
experiment?
b) Why did the water rush into the tube when the delivery tube
was opened under water?
c) Why d i d the boiling continue in the closed tube at a much
lower temperature than in the open tube?
d) Why did the upper part of the closed tube cool more slowly
than the upper part of the open tube?
4. Explain why one feels cooler in a wet bathing suit than a dry
one, especially when the wind is blowing.
5. Why is a hot day less disagreeable when the atmosphere is
relatively dry than a day with the same temperature when the
relative humidity is high?
6 . Explain how cooling by evaporation is used in one of the
methods for determining the relative humidity.
7. Explain briefly how a pressure cooker utilizes a principle
studied in this experiment?
a . What is the meaning of supercooling? Was it observed in this
experiment?
67
VISCOSITY
Viscosity is the resistance to flowing of a liquid, and like

other properties of liquids, result from the intermolecular forces
of attraction. As temperature is increased, the liquid’s viscosity
decreases. The viscosity of a liquid can be determined by
measuring the time required for a specified volume of liquid
to empty through a capillary tube in a simple laboratory apparatus
called a viscometer. Liquids with moderate to low viscosities may
be readily measured in this manner. Using the simple viscometer,
a set of simultaneous equations can be derived for determining the
viscosity, n , of any liquid by measuring the flow time in seconds
for the liquid. In equation (l), A is a constant, dependent on the

volume capacity of the viscometer, B is a constant, dependent upon
the length and radius of the capillary, D is the density of the
liquid, and t is the flow time of the liquid in seconds. So that
constants A and B may be conveniently determined for your
viscometer, hexane and water must have their flow times measured.
By obtaining their respective viscosities and densities from the
CRC Handbook of Chemistry and Physics, the following two
simultaneous equations may be solved for A and B by using
determinants or substitution. In equation ( 2 ) , the viscosity
nz = ADztz - BDz/tz (3)
of water, ni , and the density of water, Di , at laboratory

temperature are combined with water’s flow time at the same
i.=?m:.erature resulting in only A and B as unknowns in the e q i i s t i ~ n .
Likewise, in equation ( 3 ) , the viscosity of hexane, n2, and the
density of hexane, Dz, at laboratory temperature are combined
with hexane’s flow time at the same temperature. Since viscosity
is a temperature dependent property, the viscosity value for
hexane may not be found in the CRC Handbook for the specific
laboratory temperature at which the flow times were measured. If
this is the case, use linear interpolation for two viscosity
values closest to the laboratory temperature. Once the constants
have been determined for the viscometer, the viscosity of any
liquid may be determined by measuring the flow times in the
viscometer and the density of the liquid.
For highly viscous materials, such as molasses and motor oils,
a Brookfield viscometer is used to mechanically measure the
viscosity by the drag of the liquid on a moving metal cylinder at
- a fixed speed. Both methods will be used in this experiment.
68
Procedure
Section A
Fill your viscometer with hexane so that the liquid level at
the bottom does not reach the capillary tube in the viscometer.
Using a pipet bulb draw the hexane up to fill the calibrated
volume area, ensuring that the liquid is drawn above the top volume
line. Start the flow time measurement as the liquid passes the
top line and stop timing when the liquid passes the bottom line of
the volume area. All flow times should be measured at a constant
temperature. If the viscometer is submerged in a beaker of room
temperature water, a fairly constant temperature can be
maintained. Measure the flow time of hexane several times. Pour
the used hexane into the appropriate container in the fume h o o d .
Use a pipet bulb to force air through the viscometer’s capillary
to remove all traces of hexane. The viscometer can also be placed
in the drying oven but must be allowed to cool before measuring
the flow time for water. After the flow time for water at room
temperature is measured several times, placed the viscometer in an
ice-water bath for ten minutes. Record the temperature of the
ice-water bath and then measure and record the flow time for water
at this temperature. Calculate the constants A and B.
Measure the flow times for the following compounds: methanol,
propanol, isopropanol, acetone, reagent alcohol and heptane.
Dispose of the liquids each time in the container in the fume hood.
Be sure that the viscometer is free of all traces of residual
liquid before starting the measurement of subsequent flow times.
The density of reagent alcohol will have to be determined since it
is a mixture of alcohols. See the appropriate sections in the
Chemical Technician’s Ready Reference Handbook, CTRRH, for the
pycnometer or hygrometer method.
Section B
The instructor will demonstrate proper use of the Brookfield
viscometer. You will be supplied with a group of commercial
products such as shampoo, creme rinse, olive oil, corn oil, and
glycerin. The accuracy of the Brookfield can be checked by
comparing values for the oils with those found in the CHC
Handbook of Chemistry and Physics.
Rewirements f o r Report
Construct data and results tables containing the following
items: name of compound, compound’s formula weight, compound’s
density, compound’s structure, compound’s polarity, compound’s
flow time average, compound’s calculated viscosity, compound’s
handbook viscosity, relative error for compound’s calculated
viscosity for Section A . Show the calculations for the constants
A and B. For Section B construct a table containing the following
data: sample, spindle number, speed, dial reading, multiplying
factor, viscosity, handbook viscosity if applicable.
69
Questions
1. Analyze the data and results from Section A and answer the
following questions:
a) Why are the viscosities of propanol and isopropanol
different?
b) Why are the viscosities of isopropanol and acetone
different?
c) Does the viscosity of reagent alcohol occur in the sequence
of alcohols where you would expect to find i t s value?
d) Reagent alcohol is a mixture of the alcohols you have
measured and ethanol. Using the percent composition of
reagent alcohol from its label and the handbook values for
the pure alcohcls, calculate an expected viscosity and
compare this to the measured value.
2. H o w do the measured viscosities from the Brookfield viscometer
compare to the handbook values?
3. Use the CTRRH or chemical supplier catalog to describe another
device for measuring viscosity. Take care to describe the
method used and how the device operates. Cite your reference
source.
70
SURFACE TENSION
The surface tension of a liquid can be thought of as that

property which draws liquid molecules together at the surface,
forming a liquid-vapor interface, thereby distinguishing liquids
from gases. The surface tension is a characteristic property of
each liquid and differs greatly in magnitude from one liquid to
another. Of the various methods available to measure surface
tension, such as tensiometer, drop weight, bubble pressure, or
capillary rise, capillary rise is considered the standard method.
The capillary rise method is based on thc fact that most liquids,
when brought in contact with a fine glass capillary tube, will
rise in the tube to a level above the liquid outside the tube. This
will occur only when the liquid "wets" glass, that is, adheres to
it. If a liquid does not "wet" glass, as in the case of mercury,
the level inside the tube will fall below the outside level. A
normal liquid in contact with glass forms a concave surface which i c
referred to as a meniscus. The mercury will exhibit a convex surface
which appears as an inverted meniscus to an observer. To understand
the theory of the capillary rise method, consider a fine capillary
tube of uniform radius, r, immersed in a vessel containing a liquid
that wets g l a s s (Figure 1). By wetting the inner wall of the
capillary, the surface of the liquid is increased. To decrease its
free surface, the liquid must rise within the capillary tube. As
soon as this happens, however, the glass wets again, and the liquid
draws itself upward. This process does not continue indefinitely,
but stops when the force of the surface tension acting upward becomes
equal to the force due to the column of liquid acting downward. If
we assigned T, to be the surface tension in degrees per centimeter of
the inner circumference and consider the force to be acting at an
angle theta, called the contact angle with the vertical dimension,
then the force due to the surface tenaici. I; given by cquation ( 1 ) .
Fr = Z(pi)rTcos(theta) (1)
This force is balanced by that due to the column of liquid of height,

h, with a density, d, and where g is acceleration due to gravity,
980.67 cm/sec2 in equation ( 2 ) . Therefore, at equilibrium

Fr = F2 which results in equation ( 3 ) and may be solved for the
surface tension, T. The resulting equation ( 4 ) can be simplified
Z(pi)rTcos(theta) = (pi)r2hdg (3)
71
by cancelling common terms in the numerator and denominator. For
T = ( p i r2 hda =rhda (4)

Z(pi)rcos(theta) Zcos(theta)
most li'quids which wet g l a s s , theta is essentially zero and thus
cos(theta) = 1. Therefore, the surface tension of a liquid may be
T = rhda (5)
2
calculated if the radius of the capillary, normally 0.035 cm, the
density of the liquid, and the height to which the liquid rises in
the capillary are determined or known values.
Figure 1. Figure 2.
72
Procedure
First the radius of the capillary tube must be verified. The
surface tension of hexane can be obtained from the CRC Handbook of
Chemistry and Physics in conjunction with its density. The capillary
rise of hexane is measured by filling the device in Figure 2 so that
the liquid level is near the zero point on the attached scale.
Record the scale measurement for the liquid level. Using a pipet
bulb, draw the liquid up in the capillary above the point to which it
has risen. Remove the bulb and allow the liquid to drop to its
equilibrium level. Read the height of the liquid column.
Remember to subtract the liquid level value if it is not exactly
zero to obtain the true value for the capillary rise. This
information along with the density and surface tension for hexane
will allow you to solve equation (5) for the radius of the bore.
Dispose of the hexane and all other organic liquids u s e d in
this experiment in the appropriately marked container in the fume
hood. Using a pipet bulb, force air through the capillary to
remave traces of the hexane before measuring the next liquid.
Repeat this step before measuring the capillary rise of each liquid.
Measure the capillary rise f o r the following liquids: methanol,
propanol, isopropanol, acetone, and reagent alcohol. Record the
true value of the rise. Check MSljS notebook for necessary precautions
in handling these chemicals and record in your notebook. If you
have recorded this information for a previous experiment, indicate
on what pages in your notebook the precautions may be found.
Requirements for HeDort
Calculate the surface tension for each liquid using equation
(5). Construct a data table including the following information
for each liquid; compound’s name, compound’s formula weight,
compound’s density, compound’s capillary rise, compound’s
calculated surface tension, compound’s actual surface tension, and
relative error in the calculated surface tension. Include in the
report the data table and a sample calculation for the surface
tension. Discuss the any relationships that you observe from the
calculated surface tension in relationship to formula weight,
structure, and polarity. Discuss possible errors which may have
affected your results.
Questions
1. Which measurement, surface tension or viscosity, appears to
represent a measure of the intermolecular forces? Explain.
2. Using the CTRRH or chemical supplier catalog, cite another
method of measuring surface tension and describe the
operation of the device. Indicate your reference source.
73
STRENGTHS OF ELECTROLYTES
Compounds are frequently divided into two categories:

electrolytes and nonelectrolytes. Electrolytes are compounds that
ionize or dissociate in aqueous solution. As a result of this
behavior, their aqueous solutions conduct an electric current.
Nonelectrolytes are compounds that do not ionize or dissociate in
aqueous solution, and therefore their aqueous solutions do not
conduct an electric current.
Electrolytes are divided into two types. Strona: electrolytes
are compounds that ionize or dissociate completely, or nearly
completely, in dilute aqueous solution. Such solutions conduct an
electric current well. Strong acids, such as HC1, H N O a , and
H 2 S 0 4 , and strong bases, such as NaOH and KOH, are examples of
s t r o n g electrolytes. In addition, most soluble salts, such as
N a C 1 , KzCrz07, and MgSO4 are included in the group of
aqueous solutions which conduct an electric current very well.
- - 1-
1 7
electrolytes are compounds that ionize or dissociate o n l y
slightly in dilute aqueous solutions. Their solutions conduct an
electric current very poorly. Weak acids, such as acetic acid,
citric acid, and ascorbic acid, and weak bases, such as ammonia,
are examples of weak electrolytes. Certain salts which are only
slightly soluble in water are also very poor conductors. Examples
of these salts are AgCl and MgC03.
Whether a salt is a strong or weak electrolyte can be
predicted from the water solubility rules in your textbook.
Whc? inorganic salts dissolve in water they produce ions in
the solution. When aqueous solutions of salts are mixed together,
they can produce a chemical reaction because of the ions.
I'd ;kAis point in the course, we have represented reactants and
products in molecular form for chemical equations. When silver
AgN03(aq) + NaCl(aq) ---- > AgCl(s) + NaNOs(aq)
nitrate is mixed with sodium chloride in aqueous solution, silver
chloride precipitates and sodium nitrate remains in the solution.
An alternate way of representing the chemical equation is to write
all of the soluble salts as ions in solution and all of the
Ag+ (aq) + Nos- (as) + Na+ (as) + C1- (aq) ---- >
AgCl(s) + Na+(aq) + N03-(aq)
insoluble salts in molecular form. This is the i o n i c equation
for a chemical reaction. Note that AgNOs, NaC1, and NaNG3 are
-indicated as ions in solution and AgCl is written in the molecular
form. Only those ionic and molecular species which represent the
74
observed chemical change are used to write the net ionic equation.
The non-participating ions, called spectator ions, are omitted
from the equation. Since Na+ and N O 3 - appear on both reactant and
product side of the ionic equation and they remain in the same
physical state without an observed change, they are considered
spectator ions. Thus, the net ionic equation for the chemical
reaction is as shown below.
Ag+(aq) + Cl-(as) - - - - > AgCl(s)
This type of chemical equation is classified as a metathesis
or double displacement reaction because an exchange of ions takes
place between the reactants. A requirement of this type of
reactions is that a chemical change must be observed by the
formation of a precipitate] a change in color, evolution of a gas,
a change in acidity or basicity] or the release or absorption of
heat energy. If none of these changes are observed, then the
double displacement of ions to produce a molecular species does
not take place. You simply have all the ions reamaining in
solution unchanged.
The procedure requires you to mix pairs of salt solutions
together. First, write a predicted metathesis reaction in
molecular form. Use the solubility rules to help you. Second,
you,will write the ionic equation designating the physical state
of each reactant and product as they exist in solution. Finally,
you will write the net ionic equation based on your experimental
observations.
Procedure
Clean and dry 1 2 test tubes and label them with numbers 1 -
12. Prepare 250 ml of the following solution from the solutes
indicated and store them in appropriately labelled bottles. C h t - k
your calculations for the amount of solute to be weighed with the
instructor. Transfer 2 to 3 ml of each solution to the
correspondingly labelled test tube. Obtain a few crystals of
NHdNOa and place in test tube + I l l . Obtain a few crystals of
CaC03 in test tube $12.
Test tube Number Solution or Reagent
1 0 . 1 M FeCls from FeC13-6HzO
2 0.1M Na2COs from NazCO3
3 0 . 1 M BaClz from BaClz-2HzO
4 0 . 1 M NasPO4 from NasPO4. 1 2 H z O
5 0.1M NiClz from NiClz. 6HzO
6 0.1M CuSO4 from CuSO4-5 H z O
7 0 . 1 M CoCl2 from CoClz-6H20
8 0 . 1 M AgN03 from AgN03
9 1.OM HC1 from concentrated HC1
10 1.OM NaOH from NaOH
11 Crystals of NH4 NO3
12 Crystals of CaC03
75
For each pair of solutions that will be mixed:
a) write a predicted metathesis equation in molecular form

b ) observe and note any properties of the reactants
c) mix he recommended amounts of the two reactants and note
any chemical reactions that occur (refer to the
introduction section for chemical change information)
d) write the net ionic equation that describes the chemical
reaction.
CAUTION: I f a gas is evolved, do not attempt to detect odor unless
spezifically told to do so and then only in the appropriate
manner.
Combine the following solutions and/or reagents in the
amounts specified:
a) Combine 1/2 of #l with 1/3 of # l o
b ) Combine 1/3 of #2 with 1/3 of # 6
c ) Combine 1/2 of # 5 with 1/3 of # 2
d) Combine 1/2 of #3 with 1/3 of #6
e) Add 1/2 of # 4 to the remainder of 86
f) Add 1/2 of #7 to the remainder of # l
g ) Add 1/3 of #lo to # l l ; heat over cool flame and cautiously
detect odor
h) Add 1/2 of #9 to #12
i) Add the remainder of #9 to the remainder of # l o ; insert
a thermometer in #lo before addition and note any
temperature change.
j) Add the remainder of # 4 to the remainder of #t5
k ) Combine 1/2 of #8 to the remainder of tt7
1) Add the remainder of #8 to the remainder of #2
Reauiremnents for Report
As procedure requires, show all equations and evidence of
chemical reactions from experimental observations.
Questi ong
1. List five ways of identifying a chemical change.
2. What is the difference between an ionic and a net ionic
equation?
3. In general, what can you conclude about most salts containing
C1- and S O I - ?
4. In general, what can you conclude about most salts containing
C03-2?
76
5. If equal volumes of 1 . O M N H 4 O H and 0 . 1 M CuSOs are mixed an

intensely blue colored solution results. This blue color is
significantly different than the original CuSO4 solution
color.
a) Predict a metathesis equation.
b) Check you textbook or reference source to verify or
disprove your prediction.
c) Write the net ionic equation for the chemical reaction.
d) How is this reaction different than the typical metathesis
reaction.
77
STANDARDIZATION OF A BASIC SOLUTION
When a solution of strong acid is mixed with a solution of a

strong base, a chemical reaction occurs that can be represented
by the following net ionic equation:
H+ + OH- ---- > H2O
This is called a neutralization reaction and chemists use it

extensively to change the acid-base properties of solutions. The
equilibrium constant for the reaction is 1 0 1 4 at room temperature,
so that the reaction can be considered to proceed completely
to the right, using up whichever of the ions is present in the
lesser amount and leaving the solution acidic or basic, depending
on whether H+ or OH- ion was in excess.
Since the reaction is essentially quantitative, it can be
used to determine the concentrations of acidic and/or basic
Solutions. A frequently used procedure involves the titration of
an acid with a base. In the titration, a basic solution is added
from a buret to a measured amount of acid until the moles of OH-
ion added is just equal to the number of moles of H+ ion present
in the acid. At that point, the volume of base that has been added
is measured.
The equivalence point or end point in the titration is
determined by using a chemical, called an indicator, that changes
color at the proper point. The indicators used in acid-base
titrations are weak organic acids or bases that change color when
neutralized. One of the most common indicators is
phenolphthalein, which is colorless in acid solutions but becomes
red or pink when the pH of the solution becomes 9 or higher. The
point at which the phenolphthalein changes color is the endpoint
of the titration. Indicators are selected so that the reaction’s
equivalence point and the indicator’s endpoint occur at
essentially the same pH in the titration.
In Section A of the procedure, dry potassium hydrogen
phthalate, KHCeH404, is used as the primary standard acid for
determining the normality of the sodium hydroxide solution. This
standard is used because of its high purity and because it is not
hygroscopic. The accurately weighed acid sample is dissolved in
distilled or deionized water. The equivalents of KHCsH404, KHP,
used for the titration is calculated from the acid’s measured mass
and its equivalent weight:
mass ( E ) = eq KHP
equivalent weight (g/eq)
The equivalent weight of K H P is 2 0 4 . 2 g/eq. Recall that an
equivalent is that amount of pure substance necessary to generate
one mole of H+ ion or one mole of OH- ion. The NaOH solution is
then added from the buret to the KHP solution until the
equivalence point is reached, signaled by the phenolphthalein
indicator changing from colorless to pink. At this point the
volume of NaOH solution added to the K H P solution is determined
and recorded. Because one equivalent of KHP reacts with one
equivalent of NaOH, the normality of the NaOH solution is
calculated using the following equations:
eq KHP = eq NaOH (2)
Normality (N) NaOH = ~ C INaOH
L solution (3)
In Section E of the procedure the equivalent weight of an
unknown acid is determined. The standardized NaOH solution f r o m
Section A is used to titrate an accurately measured amount of
unknown acid to the equivalence point. By knowing the volume and
the normality of the NaOH, the equivalents of acid in the unknown
are determined using the following equations:
Volume ( L ) X Normality (N) = eq NaOH (4)
eq acid = eq NaOH (5)

From the measured mass of the unknown acid titrated, the
equivalent weight of the acid is calculated using:
Gram Equivalent Weight (acid) = mass of acid ( E )
eq acid (6)
Procedure
Section A
Obtain a clean 1500 mL flask from the stockroom, add boiling
chips and more than one liter of distilled water. Heat the water
to a rolling boil for 10 minutes. Cool the water in an ice bath.
Weigh approximately 4 to 4 . 5 g of NaOH pellets. Obtain a one
liter plastic bottle from the stockroom and clean it well with
soap and water being careful to rinse it thoroughly with distilled
water. Transfer some of the cooled water to the plastic bottle
and add the previously weighed sodium hydroxide pellets. Shake
and swirl the mixture until the pellets have dissolved. Add the
remaining water to fill the container completely. Cap the
container and shake it to ensure a homogeneous solution. Label
the container as approximately 0.1N NaOH with your initials and
‘the date on which the solution was prepared. Be sure to shake
the solution well before you use it.
79
Prepare three clean Erlenmeyer flasks and weigh three samples

of KHP while at the balance. Weigh the weighing bottle containing
the KHP to the nearest 0.001 g . Into each clean Erlenmeyer
flask, weigh 0.4 to 0.5 g of KHP to the nearest 0.001 g . Pour the
KHP samples from the weighing bottles and reweigh the weighing
bottle to obtain sample weight. Be sure to mark the flasks with
numbers for identification purposes. Add 50 ml of distilled water
to each flask and 2 drops of phenolphthalein indicator.
Wash a 50 ml buret thoroughly with soap and water using a
long buret brush. Also thoroughly clean a funnel. Flush the
buret and funnel with tap water and rinse several times with
small quantities of distilled water. Fill the buret with distilled
water and allow it to drain. A clean buret shows no water droplets
clinging to its inner walls. If the buret is glass, care must be
taken to properly grease the stopcock to avoid leaks during the
titration. Rinse the buret with three 5 ml portions of the NaOH
solution, making certain that the NaOH wets the entire inner
surface of the buret. Drain the NaOH through the buret tip.
Using the funnel, fill the buret with the NaOH solution and
kecord its initial volume to the nearest 0.01 ml. Do this by
holding a white card with a black line in back of the buret and
reading the bottom of the meniscus. Be certain that all air
bubbles are removed from the buret and buret tip. Place white
paper beneath the Erlenmeyer flask. Slowly add drops of NaOH
solution to the acid, swirling the flask after each drop. Note
that the pink color of phenolphthalein appears and disappears as
the drops hit the acid solution and are mixed with it. When the
the pink color begins to persist, slow down the rate of NaOH
addition. Rinse the inner wall of the flask with a wash bottle
periodically during the titration. In the final stages of trie
titration add NaOH drop by drop until the entire solutiori just
t r i r r l q a pale pink color that persists for 30 seconds. Many times
a full drop of NaOH solution added to the acid solution may be too
much near the endpoint. If this is the case, then a partial drop
is formed on the buret tip and washed into the flask with a wash
bottle. Again the wall of the flask should be thoroughly rinsed
and the solution swirled. Continue the titration until an
endpoint is reached. Read the volume of NaOH solution in the
buret and record.
Refill your buret and repeat the titration at least two more
times with varying but accurately known amounts of KHP. Calculate
the normality of the NaOH solution based on each sample of KHP.
The values should agree within one percent. If there are any
discrepancies, additional samples of KHP should be weighed and
titrated. Calculate the average normality for the NaOH solution
clith its standard deviation. Record the normality on the label of
~ the bottle of NaOH solution. When not in use, the NaOH solution
should be tightly sealed as it absorbs CO2 from the atmosphere
to form an acid solution, thereby weakening the concentration of
the solution. When you have completed the titration process for
8C
the day, drain the buret into the sink and rinse several times
with distilled water. Fill the buret with distilled water and
place in the buret stand with a small beaker below the tip. This
is the proper storage procedure for a glass buret and will allow
you to know when it will be necessary to regrease the stopcock due
to leakage. If teflon stopcocks are used, the empty buret should
be inverted with tip up and stopcock loosened slightly.
Section B
Two unknown acid samples are to be titrated. Three trials of
each unknown must be performed. Weigh each unknown sample by
difference as described for weighing the KHP. The sample size
may vary greatly due to the wide range of gram equivalent weights
found in the unknown samples. It is suggested that the student
start with 0 . 3 g (to 0.001 g ) sample size. If after the first
titration has been completed, this sample size required more than
50 ml of NaOH, reduce the sample size accordingly.
Add 50 m l of distilled water and two drops of phenolphthalein

to each unknown acid sample. Fill the buret or refill the buret
as the case may be and record the initial volume of standardized
NaOH solution. Titrate to the phenolphthalein endpoint. Head the
final level of NaOH solution in the buret and record. Repeat the
titration at least twice using varying amounts of unknown acid.
For each acid, calculate the average gram equivalent weight and
standard deviation. Again, discard any NaOH solution remaining in
the buret and clean and store the buret as previously described.
Save the remaining NaOH solution in the plastic bottle for future
experiments.
Requirements f o r Report
Construct a data table for each section. Section A’s table
should contain the following information: weight of KHP sample,
equivalents of KHP, equivalents of NaOH, total volume of NaOH
solution used, normality of NaOH for each sample, the average
normality of NaOH solution with the standard deviation. For
Section B, each unknown acid sample must have the following
information included in the data table: unknown number, sample
weight, total volume of NaOH used, equivalents of NaOH,
equivalents of acid, gram equivalent weight for each trial, and
average gram equivalent weight of each unknown with standard
deviation.
stions
1. Explain the difference between an equivalence point and an
endpoint.
. 2. Is it quantitatively acceptable to titrate all KHP samples
with the NaOH solution to the same dark red endpoint?
Explain.
81
3. If the endpoint in the titration is mistakenly exceeded ( t o o

pink), what effect does this have on the calculated normality
of the NaOH solution? Explain.
4. ”If 2 drops are good, then 20 drops are better.” Explain why
this reasoning is not acceptable when adding phenolphthalein
indicator for endpoint determination.
5. A 0.325 g sample of potassium hydrogen phthalate, KHP, is
dissolved in a 100 m l of diqtilled water. If 2 1 . 6 4 ml of the
sodium hydroxide solution are required to reach the
equivalence point, what is the normality of the NaOH solution?
6. A 0.394 g sample of an unknown acid requires 23.75 ml of
0.123 N NaOH to reach a phenolphthalein endpoint. What is the
unknown acid’s equivalent weight?
7. If KHP were hygroscopic, how would this property tend to
affect the normality values of NaOH? Explain the reasons for
predicting values too high or too low for normality.
F
82
VINEGAR ANALYSIS
Many commercial products contain or are low percent acid

solutions. Vinegar is a water solution that is 4 to 5 percent by
weight acetic acid, CHaCOOH. The minimum federal standard for all
vinegars is 4 % . Many manufacturers add flavorings and color to
make the product sell better. The purpose of this experiment is
to compare the acetic acid concentrations in various commercial
vinegars and determine a best buy for the purchase price.
The percent by weight of acetic acid in vinegar can be
determined by titrating a measured weight of vinegar to a
phenolphthalein endpoint with a measured volume of standardized
base. The number of equivalents of acetic acid can be calculated
using:
Volume (L) X N ( equivalents ) = eq base

L solution
A t the equivalence point, the number of equivalents of
standardized base is equal to the number of equivalents of acetic
acid.
The number of grams of acetic acid titrated can be determined
by multiplying the number of equivalents of acetic acid by its
equivalent weight, which is the same as its molecular weight since
there is only one active hydrogen in CH3COOH.
eq acetic acid X ( 60.05 gram acetic acid.) = grams acetic
one eq acetic acid acid (2)
The percent acetic acid in the vinegar cnn be ~ : ~ l c u l z t e ! das
grams acetic acid X 100 = % acetic acid by weight
grams of vinegar (3)
Procedure
Select a brand of vinegar from the samples available and
record the brand name and purchase price. Pipet 5 ml of vinegar
into a clean, dry Erlenmeyer flask, previously weighed to 0.001 g .
Reweigh the flask and contents. Add 2 drops of phenolphthalein to
the vinegar and dilute with 50 ml of distilled water.
Rinse a clean buret with the previously prepared standardized
NaOH solution, making certain no droplets of liquid cling to the
inside walls of the buret. Fill the b i i r e t ~ I t h
tkAe stadardized
. NaOH solution. Eliminate all air bubbles from the buret and tip
and record the level of NaOH solution to the nearest 0.01 ml.
83
Titrate the vinegar to a phenolphthalein endpoint. Record the

level of the buret at the endpoint to the nearest 0.01 ml. Repeat
the procedure on a duplicate sample.
Select another brand of vinegar and perform duplicate
analyses to determine the acetic acid content.
Construct a data table containing the following information:
brand name, purchase price, vinegar sample weight, total volume of
standardized base, normality of standardized base, equivalents of
acetic acid, weight of acetic acid, percent acetic acid in
vinegar, average percent acetic acid in vinegar. From the this
information determine which vinegar is the "best buy".
Questions
1. A total of 3 4 . 2 ml of 0.105N NaOH was required to reach a
phenolphthalein endpoint in titrating 6.15 g of vinegar.
a) Calculate the number of equivalents of acetic acid in the
vinegar .
b ) Calculate the number of grams of acetic acid present in the
sample.
c) Calculate the percent by weight of acetic acid in the
vinegar.
2. A drop of standardized NaOH solution adheres to the side of
the Erlenmeyer flask and is not washed into the vinegar with
the wash bottle; how does this affect the reported percent
acetic acid in vinegar? Explain.
3. In determining the percent acetic acid in vinegar, the samples
are weighed rather than measured volumetrically. Explain.
4. If the vinegar were measured volumetrically, what additional
piece of data would you need to complete the calculations in
this experiment?
5. Phenolphthalein changes color in the pH range 8 . 2 to 10.0;
methyl red changes from 4 . 2 to 6.0. Comment on the
advisability of using methyl red indicator in this experiment
and the consequences if indsed the substitution is made.
84
ACIDITY OF FRUIT JUICES
Some citrus fruits taste more sour, and therefore are more
acidic,'than others. The purpose of this experiment is to
determine the total acidity of apple, orange, lemon, grapefruit
and/or lime juice. Citric acid is the acid responsible for the
sour taste in citrus fruit. Citric acid is a polyprotic acid in
which three ionizable hydrogens may be neutralized by a strong
H O H O
I ti I II
H - C - C -OH H - C - C -0-Na+
H - C - C -OH + 3NaOH ----> H - C - C -0-Na+ + 3HzU
H H
base. It is not the only water soluble acid found in citrus

fruits, since ascorbic acid, Vitamin C, is also contained in fruit
juices. Ascorbic acid is a monoprotic acid with only one titratable
HCsH706 + NaOH ---- > NatCsH706- + H2O

hydrogen per molecule. Consequently, only total acidity can be
determined on the basis of equivalents of acid per.volume of juice
solution. This will allow the pH of the fruit juice to calculated
total eq of acid = moles of hydrogen ion in juice (1)
by taking the moles of H+ and dividing by the volume in liters of

pH = - log ( mole of H+) = - log (H+ molarity) (2)
liters of juice
the juice sample titrated with the standardized NaOH solution.
The pH values for the individual fruit juices should be found
in the CRC Handbook of Chemistry and,Physics (p. D151) prior to
starting the experiment.
85
E rocedure
Section A
Apple cider will be used as the representative sample of
apple juice. Cut the citrus fruit in half and use the juicer
apparatus to obtain juice from the fruit.. Filter the juice using
a Buchner funnel to remove the pulp. Be sure to use a trap bottle
between the filtering flask and aspirator to avoid contaminating
the juice with tap water. Into a 250 ml Erlenmeyer flask, pipet
5.00 m l of juice. If the juice is highly colored, a lesser
quantity, 1.00 or 2.00 ml, may be used instead. Dilute the juice
to approximately 100 ml total volume with distilled water and
add two drops of phenolphthalein indicator.
Rinse and fill your buret with standardized NaOH solution
from a previous experiment. Record the initial volume level of
NaOH solution. Titrate the juice solution to the phenolphthalein
endpoint and record the final volume level in the buret. Repeat
the titration on a duplicate sample to check for reproducibility.
C-lciilate the pH of the fruit juice using equations ( 1 ) and ( 2 j .
kompare your results with the CRC Handbook value for the
corresponding fruit juice. Choose another citrus fruit or apple
juice and repeat the above procedure on duplicate samples.
Section B
Using a pH meter which has been calibrated, measure the pH of
each fruit juice. Take care to rinse the electrode with
distilled water between individual measurements. Record the pH
values in your notebook.
Keauirements for Report
Construct a data and results table containing the following
items: name of the juice, volume of the juice, normality of the
NaOH, total volume of the base used in the titration, equivalents
of the acid, moles of H+, molarity of H+, the calculated pH of
the juice sample, measured pH value and pH range from the CRC
Handbook. Comment on the consistency of the sour taste to the
actual pH range found in the CRC Handbook and whether your
experimental results parallel the actual values. Discuss the two
methods of determining pH used in the experiment and state reasons
why one method may be preferable. (Hint: Check your textbook for
the buffering capacity of salts of weak acids.) Show a set of
sample calculations for the experiment.
I
86
Q u e s ti on s
1. Is it acceptable to report the total acidity of a juice sample

as equivalents of citric acid? Explain your reasoning.
2. Why are pH ranges for various fruit juices reported rather
than exact values?
3. If a 5.00 ml sample of lemon juice require 37.78 ml of 0.125 N
NaOH solution to reach a phenolphthalein endpoint;
a) calculate the equivalents of acid.
b ) calculate the moles of H+ ion.
c) calculate the molarity of H+ in the juice sample.
d ) calculate the pH of the juice sample.
a7
STANDARDIZATION OF AN ACID SOLUTION
Neutralization titrations are widely used for determining the

concentration of substances that react directly or indirectly with
a solvent to form hydrogen or hydroxide ions. For most
applications, water is chosen as the solvent because of its
availability] low cost and low toxicity. In most neutralization
reactions between strong acids and bases, a pronounced pH change
takes place at the equivalence point. It is for this reason that
standard solutions for such titrations are always prepared from
strong acids or strong bases. Hydrochloric acid is the most
commonly used standard acid solution for the titration of bases.
Dildte solutions of the reagent are stable indefinitely. A
standard acid solution is ordinarily prepared by diluting an
approximate volume of the concentrated reagent and subsequently
standardizing the diluted solution against a primary standard b a s e .
In this experiment] you will determine the concentration of a
0.1 M HC1 by standardizing it directly against the weak base called
?'RAM or TRIS, which means tris(hydroxymethy1)aminomethane. THAM is
a primary standard base whereas KHP is a primary standard acid.
The results for the HC1 molarity] from the direct standardization
against THAM, will be compared to the results obtained indirectly
by titration against the previously standardized NaOH solution.
The equation for the reaction of THAM with HC1 is similar to

H H t
HN: + HC1 ---- > HN:H + c1-
H H
that for the reaction of ammonia, NH3, with HC1. Sometimes this
reaction is written in the chemically equivalent way where NH4OH
NH4OH + H+C1- ---- > NH4tCl- + HOH
is 1 ammonia molecule associated with 1 un-ionized water molecule.
Note the formation of a covalent bond between the hydrogen ion and
the ammonia molecule, using the lone pair of electrons on the
nitrogen atom.
THAM is a derivative of NHa and a covalent bond between the
hydrogen ion and a lone pair of electrons also forms during its
neutralization by HC1. It is clear that there is a one to one
H H +
(HOCH2)aC-N: + H+C1- -e-- > (HOCH2)sC-N:H + c1-
H H
88
mole relationship in the reaction of THAM and HC1. Knowing this,

we can write the equation for the calculation of HC1 molarity f r o m
Molarity (HC1) = ( Qrams THAM) ( 1000 1
(GMW of THAM) (ml of HC1)
the titration results as indicated above. The gram molecualr

weight of THAM is 121.4 g/mole.
To obtain results for the comparison value against the
standardized NaOH solution, a fixed volume of acid will be
pipetted into a clean Erlenmeyer flask with phenolphthalein
indicator added and titrated to the normbl endpoint. Since the
reaction of HC1 with NaOH is a one to one mole relationship, the
HC1 + NaOH ---- > HOH + NaCl
equation for the calculation of the molarity of the HC1 can be
Molarity (HC1) = (ml of NaOH) (molarity of NaOHl
(ml of HC1) (2)
written from the titration results

Procedure
Section A
Weigh four samples of THAM contained in the labelled weighing
bottles, by difference, into 250 ml Erlenmeyer flasks. The THAM
has been dried in an oven at 1000C for one hour to remove
adsorbed moisture. The samples should weigh between 0.5 and 0.6 g
to the nearest 1 mg. Dissolve each samyic in 7 5 1111of distilled
water. Add water to the flask from a wash bcttle to ensure that
any powder adhering to the neck and walls of the flask is washed
into the solution. Add 3 drops of Methyl Red Indicator ( 0.2%
methyl red in ethanol) to each flask. The acid color of this
indicator is light red or pink while the basic color is yellow. At
the endpoint the solution will be orange.
Rinse a clean buret with three 5 nl portions of the HC1
solution to be standardized. Fill the buret with the HC1 solution
taking care to remove air bubbles from t h e buret and tip. Record
the initial volume of HC1 solution. Titrate the THAM solution
with the acid solution to an orange colored endpoint. Using a
hot plate, heat the resulting solution gently for 3 minutes to
remove COz dissolved in the solution. If the solution is not
boiled, you may obtain a premature endpoint due to the buffering
effect of the dissolved C O z . T h i s will be pxriderlt because the
'indicator color will revert to the yellow color when the solution
is heated. Heat until small bubbles appear on the bottom of the
flask. Do NOT boil too long or too hard, otherwise the HC1 will
be lost and the indicator will be destroyed. After cooling the
flask
. - under the tap or in an ice bath, add an extra drop or two of
:r t,c, the sc.Jllution. If t)i? e n j i l t ; 1 - , 2 = t r r r n G J tf- ;
-1m i
' yellow color, continue the titration until the orange endpoint is
reached.
I
89
Finish each of the four titrations completely befclre

proceeding to the next titration; this avoids errors in the buret
readings for the volume of HC1 solution. Read and record the
final volume of HC1 solution. If the endpoint is exceeded, a back
titration with your standardized NaOH solution is possible. You
must remember to adjust the equivalents of acid accordingly before
calculating your acid normality.
Section B
Drain the remaining HC1 solution from the buret into a
beaker and save this solution for later use. Clean the buret and
fill with standardized base from a previous experiment. Add more
H C 1 solution to the beaker and pipet three 2 5 ml aliquots into
separate 250 ml flasks. Add two drops of phenolphthalein
indicator to each flask. Record initial level of NaOH solution in
the buret and titrate to the normal light pink endpoint. Record
t h e final level of NaOH solution in the buret. Refill b u r e t w i t h
NaOH solution and titrate the remaining samples completing each
sample before starting the next. Record all volumes and the
qormality of the NaOH solution.
Construct a data table for information obtained in the
experiment and also for results from the necessary calculations in
the experiment. Show one set of sample calculations for each
section of the procedure. Report the average molarity of the HC1
solution with the standard deviation for both sections. Compare
the molarity of the acid as determined by THAM titration to the
molarity of the acid as determined by NaOH titration. Express the
difference in molarities as percent difference.
Gluestions
1. Why is it proper to use phenolphthalein indicator for the KHP
titrations with NaOH while a methyl red indicator is reqilired
in the THAM titrations with HCl? Explain.
2. If 2 3 . 5 6 ml of the hydrochl3ric acid solution is required in
the titration of 0.536 g of THAM by the procedure in the
experiment, what is the molarity of the acid?
3. Using the results from problem 2:
a) calculate the percent error in the molarity of the acid
solution which would result from an error of 0.02 ml in
the titration volume.
b ) calculate the percent error in the molarity of the acid
solution which would result from an error of 5 mg in the
weight of THAM.
90
4. Compare the percent errors in a) and b) of problem 3 . Using

this information, state which error would have a more
significant effect on your results. What measurements should
you take great care when making?
5 . Why might the values of the molarity of the HC1 solution,
determined by THAM, be slightly different from the values
determined by NaOH? Which should be more accurate?
6. The reaction between a strong acid, HC1, and a strong base,
NaOH, is quantitative; between HC1 and a weak base, THAM, is
quantitative; between NaOH and a weak base, KHP, is
quantitative. Why is the reaction between THAM and KHP not
quantitative?
7. Borax, Na2E407. lOHzO, may be used as a standard in
place of THAM. In this case, the reaction is
NazB.107 + 2 HC1 t 5 H2O - - - - > 2 NaCl + 4 H3BO3
Compute the equivalent weight of borax and compsre it to

THAM. Does this suggest an advantage that borax may have
over THAM?
91
ANTACID ANALY S I S
Various commercial products claim to give the "best relief"
for acid indigestion. Pharmaceutical companies issue quantitative
results from their laboratories that verify their advertisements.
Rolaids, for example, claims to "consume 4 7 times its own weight
in excess stomach acid. This information was published in an
article in Chemistry, Volume 4 4 , page 28 in 1971. The normal pH
of the stomach ranges from 1.0 to 2.0. Acid indigestion and
heartburn normally occur at a lower pH. The purpose of an antacid,
regardless of its claims of effectiveness, is to neutralize or to
buffer the excess hydrogen ion in the stomach and, therefore,
relieve acid indigestion. Milk of magnesia, an aqueous suspension
of magnesium hydroxide, Mg(OH)2, is a simple antacid that
Mg(0H)z + 2H+ ----> Mg+z + 2H2O (1)
neutralizes H+. The "fast relief" antacids that buffer the

excess acid in the stomach are those that contain calcium
rqrhonate, CaC03, or sodium bicarbonate, NaHC03. A HC03-,
C O 3 - 2 buffer system is established in the stomach with these
antacids as shown in the following equations. Rolaids, which
contains dihydroxylaluminum sodium carbonate, is a combination

antacid, that is, it both neutralizes and buffers. It reacts with
a c i d according to the following equation:
NaAl(OH)2COa + 3H+ ---- > Na+ + Al+3 + 2HzO + HC03- (4)
This experiment determines the total effectiveness of several

antacids by means of a strong acid-strong base titration. TG
avoid the possibility of a buffer system being established during
the titration, an excess of hydrochloric acid will be added to the
dissolved antacid forcing the equilibrium to the right (Refer to
equations 3 and 4 above). The solution will be heated to drive off
the carbon dioxide as a gas. The excess hydrochloric acid will be
titrated with standard NaOH solution.
The number of equivalents of antacid in the commercial sample
plus the number of equivalents of NaOH used in the titration
equivalents of base = equivalents of acid (5)
eqantacid + eqNaOH = eqHCl (6)
92
equals the number of equivalents of H C 1 added.Therefore, the

equivalents of antacid can be obtained by solving equation ( 6 ) .
The number of equivalents of antacid per gram allows the
comparison of effectiveness of the various brands.
Procedure
Weigh one tablet of antacid and record the weight and brand
name. Grind the tablet using a mortar and pestle. Record the
cost and number of tablets per bottle for each brand which you
analyze. Weigh two clean, dry 250 ml flasks and mark each for
identification purposes. Transfer one half of the pulverized
antacid tablet, approximately 0.7 g, to each flask and reweigh the
flasks to the nearest 1 mg. Pipet 60.0 ml of 0.1N HC1, previously
standardized, into each flask and s w i r l to dissolve. The solution
may appear cloudy due to the insoluble binder, an inert ingredient,
used to prepare the tablet. Record the normality of the HC1.
Heat the solution to a gentle boil for 3 minute to remove any
dissolved C02. Add 4 - 8 drops of bromophenol blue indicator.
Bromophenol blue indicator is yellow in acidic solution and blue
in basic solution. If the solution is blue, pipet an additicnal
10.0 ml of the 0.1N HC1 solution into the sample flask and boil
again. Cover the flask with a watch glass or Parafilm and place
in an ice bath to cool to room temperature. Rinse a clean buret
several times with small quantities of the standardized NaOH
solution before filling. Record the normality of the NaOH
solution and the initial volume of the NaOH to the nearest
0.01 ml. Be sure there are no air bubbles in the buret tip.
Titrate the acidic solution with the standardized NaOH solution
to a blue endpoint. Record the final volume of NaOH in the buret
to the nearest 0.01 ml. Repeat the titration with s second
sample of the same brand.
Choose a second brand of tablet and repeat the procedure
described above. Compare the strengths of antacid tablets on the
equivalents per gram basis. Calculate the cost of antacid
tablets per gram so that the "best buy" can be determined.
Requirements for Report,
Construct a data table containing the following pieces of
information: brand name, weight of sample, normality of HC1
solution Used, volume of H C 1 added, equivalents of acid added,
normality of NaOH solution used, total volume of NaOH,
equivalents of NaOH added, equivalents of acid in excess,
equivalents of antacid in the tablet, equivalents of antacid per
gram, cost of antacid per gram, and equivalents per cent. Show
one complete set of calculations for a'sample. On the basis of
information collected, compare the brands, and rate the best buy
for effectiveness.
93
Questi ons
1. Write the balanced equation for the reaction of 1 mole of the
active ingredient in Rolaids with excess H+ ion.
2. If the pH of the stomach is 1.0 and the volume of the stomach
is one liter, how many grams of milk of magnesia will be
required to raise the pH of the stomach to 3.0?
3. Salts of weak acids can also produce a neutralizing effect in
the stomach by reacting with water, this is called hydrolysis.
Write a balanced equation for sodium citrate, Na3CsH507,
whose parent acid is citric acid, H 3 C s H s 0 7 .
4. If the C 0 2 is not removed from the solution by boiling after
the 0 . 1 N H C 1 is added, how will this affect the amount of
NaOH required to reach the bromophenol blue endpoint?
5. If results from trials on the same sample differ by a
substantial amount, more than 5%, what should you do before
presenting your results?
94
ANALYSIS OF ACTIVE INGREDIENT IN COMMERCIAL TABLETS
Many of the commercial pharmaceutical products have weak.

acids as active ingredients which are titrable using a
standardized base solution and an appropriate indicator such as
phenolphthalein. In this experiment, two products, Vitamin C and
aspirin, will be investigated for activity. Each tablet will
contain a specified amount of active ingredient as indicated by
the label on the bottle. After titration with the standardized
base solution, the experimental value can be calculated and compared
% activity = E active ingredient ( e x periment) X 100
g active ingredient (reported) (1)
to the reported value on the bottle to verify the manufacturers’
claims. Both acids are monoprotic so calculations can be done
using molarity or normality.
Aspirin, acetylsalicylic acid, is both an organic ester and
an organic acid. It is used extensively in medicine as a pain
killer and fever reducing drug. When ingested, the
acetylsalicylic acid remains intact in the acidic stomach, but in
the basic medium of the upper intestinal tract, it hydrolyzes
forming the salicylate and the acetate ions. Aspirin’s analgesic
action is probably due to the salicylate ion, however, its
additional and physiological effects are still not totally
understood. It is known that when salicylic acid is ingested,
the same therapeutic effects are observed, however, it causes an
upset stomach whereas aspirin is less l i k e l y tc do so. The
quantitative reaction of acetylsalicylic acid with a standardized
O-C-CH3
C-OH
It
0
II
+ OH- ----> allrcH’ II
0
ii
+ HzO
0
sodium hydroxide solution occurs according to the following
reaction. The volume of base times the normality yields
equivalents of base which are equal t-o equivalents of acid. The
grams of acetylsalicylic acid may be calculated using the
following relationship.
eq acetylsalicylic acid X 180.2a = g acetylsalicylic
eq acid (2)
95
Vitamins are a group of organic substances required in the

diet of man and animals. Vitamin C , ascorbic acid, can be
obtained from citrus fruits, tomatoes, potatoes, and fresh
vegetables. All animals, except man, are capable of synthesizing
their own ascorbic acid; man must obtain it from food sources.
The long established use of citrus fruits, particularly limes,
to prevent the occurrence of scurvy was readily justified when it
was established that the condition was a result of a Vitamin C
deficiency. A well-balanced diet provides adequate amounts of the
vitamin as measured by the Recommended Daily Allowance (RDA) of
75 mg per day.
Ascorbic acid is a cheap, water soluble, organic compound
which has a molecular formula, C s H 8 O 6 . It is a weak monoprotic
acid and may be titrated with standard NaOH solution to a
phenolphthalein endpoint. Ascorbic acid oxidizes readily in air,

particularly at high temperatures, and therefore the vitamin is
easily destroyed in cooking and long storage. Similar to the
calculations for aspirin, when the equivalents of ascorbic acid
are known, the grams of ascorbic acid may be calculated from the
following relationship.
eq ascorbic acid X 176.2~ = grams ascorbic acid
eq (3)
Procedure
Obtain three tablets of each type from the instructor and
grind each tablet using a mortar and pestle. Transfer this
powder to a 250 ml Erlenmeyer flask and be sure to wash the
residue of each tablet into the flask with a wash bottle. Check
the bottle of both the aspirin and vitamin C and record the
potency of each tablet as rated by the manufacturer. Add 50 ml of
distilled water to each sample and swirl to dissolve the tablet.
The solution may have a cloudy appearance which is the result of
the binder, an inert ingredient, used to produce the tablet. Add
two drops of phenolphthalein to each flask. Rinse a clean buret
with several small quantities of the standardized NaOH solution.
Fill the buret with the NaOH solution and record the inital volume
to the nearest 0.01 ml. Titrate to a light pink endpoint and
record the final volume of the NaOH solution.. Repeat the last
two steps on each sample. Record the normality of the NaOH
solution used in the titration process.
I
96

Construct a data table for information collected on each
sample and the results of each tablet should include equivalents
of acid, grams of acid, and percent activity. Show a sample set
of calculations necessary to reach the final result.
Questions
1. I f 6 fluid ounces of a well known.vegetable juice contains 35%
of the RDA of vitamin C, how many milliliters are necessary
to provide the recommended daily allowance of 7 5 mg?
2. Explain why cooked vegetables have lower vitamin C content
than fresh vegetables.
3. What reaction occurs when aspirin enters the intestinal tract?
4. What is the active ingredient in aspirin and why it is not
ingested directly?
5. A 325 mg tablet of aspirin was titrated to a phenolphthalein
endpoint with 16.3 ml of 0.107N NaOH. What is its percent
activity?
97
IRON - COPPER SULFATE REACTION

Most chemical reactions are classified as being either acid-
base or oxidation-reduction, redox. Acid-base reactions p r o d u c e
water as a reaction product. In redox reactions, electrons are
transferred from one substance to another, resulting in a change
in oxidation number. The substance achieving a higher oxidation
number by losing electrons is oxidized. The substance achieving a
lower oxidation number by gaining electrons is reduced. Electrons
are never considered as reactants or products. The total number
of electrons gained must equal the total number lost. For
example, magnesium metal reacts with oxygen gas to form magnesium
Mg(s) + 02(g) - - - - > MgO( s ) (unbalanced)
oxide. Magnesium increases its oxidation number from 0 to +2 by
l o s i n g 2 electrons per mole of Mg, that is, it is oxidized.
Mg - - - - > Mg+z + 2e- (an oxidation half-reaction)

Ehch oxygen atom in the0 2 molecule decreases its oxidation number
from 0 to -2. Each mole of 0 2 must gain 4 moles of electrons to
02 + 4e- ---- > 20-2 (a reduction half-reaction)
to be reduced to two moles of 0-2. The half-reactions show what
is taking place with each element in the chemical reaction. To
yield the balanced equation, the number of electrons lost in the
oxidation half reaction must equal the number of electrons gained
in the reduction half-reaction. Balancing f o r electrons gained and
2 ( M g ---- > Mg+2 + 2e-)
1 ( 0 2 + 4e- ---- > 3.0-21
4e- + 2Mg + 0 2 ---- > 2Mg+2 + 20-2 + 4e-
2Mg + 02 ---- > 2Mg0
lost and adding the two half-reaction together produces the
balanced redox reaction. In this reaction, Mg, in causing 0 2 to
accept its electrons, is the reducing agent and 02, causing Mg to
release its electrons, is the oxidizing agent. A reducing agent
causes reduction or is oxidized itself and an oxidizing agent
causes oxidation or is reduced itself.
In this experiment, you will perform a simple redox reaction
by allowing iron filings to react with a copper sulfate solution.
An excess of copper sulfate will be used to ensure that all of the
iron will react. By weighing the amount of iron used and the
amount of new substance formed, you will be able to determine the
quantitative relationship between reactants and products for this
reaction. It is a redox reaction, therefore, you can verify your
results by half-reactions for the reactants to produce a balanced
. redox reaction.
98
Procedure
On a weighing paper or boat, measure approximately 1 gram of
iron filings to the nearest .001 g . In a clean 100 ml beaker,
weigh approximately 5 grams of copper sulfate to the nearest . 1 g.
Add 25 ml of distilled water to the salt in the beaker. Heat the
solution until it just starts to boil. DO NOT let the solution
boil over. Remove the heat source when the solution is hot.
While stirring the hot copper sulfate solution with a glass rod,
add iron filings in small amounts until all has been added to the
solution. Reweigh paper or boat after addition to obtain an
accurate mass of iron added. Record the weight and any
observations made during the reaction.
Weigh a filter paper and record its weight to the nearest
0.001 g. Filter the solution by gravity, carefully decanting the
solution and transfer the solid with the aid of a wash bottle and
rubber policeman. Wash solid several times with 10 ml portions of
distilled water. Allow the solid and paper to dry until the next
laboratory period and weigh it to obtain the weight of the product.
Construct a data table for the information collected during
the experiment. The table should include the following items:
moles of iron used, moles of copper produced based on product
weight, mole ratio of Fe/Cu using the appropriate number of
significant digits.
Questions
1. Write a balanced redox equation using half-reactions for the
chemical reaction which took place.
2. What evidence did you observe to indicate that some of the
copper solution remained unchanged?
3. What evidence other than product formation would indicate
that a chemical reaction is taking place?
4. Starting with 0.500 g of iron fillings, how many moles of
copper can be formed? H o w many grams of copper are formed?
5. If 1.545 grams of copper are produced from the reaction, how
many grams of iron fillings were needed to start with?
1
99
REDOX TITFWTION WITH POTASSIUM PERMANGANATE
Reactions in which substances undergo changes in oxidation

number are referred to as oxidation-reduction reactions or redox
reactions. Oxidation is defined as an algebriac increase in
oxidation number, or a process in which electrons are lost.
Reduction is defined as an algebraic decrease in oxidation number]
or a process in which electrons are gained. Oxidation-reduction
processes must occur simultaneously.
The species that gains electrons is called the oxidizing
agent, therefore] it is reduced. The species that loses
electrons is called the reducing agent, therefore, it is oxidized.
One gram equivalent weight, GEW, of oxidizing agent is the weight
that gains 6.02 x 1023 electrons and one gram equivalent weight of
the reducing agent is the weight that loses 6.02 X 1 0 2 3 electrons.
Note that the term gram equivalent weight is defined so that one
GEW of oxidizing agent reacts with one GEW of reducing agent.
c-
GEWox = GEWred
Consider the reaction of potassium permanganate with oxalic
acid in the presence of excess sulfuric acid. The balanced
molecular and net ionic equation are:
2KMnO4 + 5HzC204 + 3H2SO4 ---- > lOC02 + 2MnS04 + K2SO4 + 8H2O
2Mn04- + 5HzC204 + 6H+ ---- > 10C02 + 2Mn+2 + 8 H z O
In W n O 4 (or in the Mn04-) the oxidation state of Mn is +7,

while in MnSO4 (or in the Mn+2 ion) it is + 2 . Therefore, each Mn
undergoes a change in oxidation number of five. Since each formula
unit of W n O 4 contains one Mn, and each Mn gains five electrons,
one mole of W n O 4 is five gram equivalent weights in this
reaction. Consequently, W n O 4 produces 5 moles of electrons per
mole of W n O 4 or has five equivalents per mole of KMnO4.
GEW of W n O 4 = 158.0 R X 1 mole = 31.60 R

mole 5 eq eq
Therefore] the gram equivalent weight of W n O 4 in this reaction is

31.60 grams.
100
In H2C204 the oxidation state of carbon is + 3 while in COz it

is + 4 . Each carbon undergoes a change in oxidation number of one.
Since each formula unit of H2C204 contains two carbons, and each
carbon loses one electron, one mole of oxalic acid is two gram
equivalent weights in this reaction. Consequently, H2C204
produces 2 moles of electrons per mole of oxalic acid or has 2
GEW of HzC204 = 90.0 g X 1 mole = 45.0 4
1 mole 2 eq eq
equivalents per mole of oxalic acid. The gram equivalent weight
A 2 C a C 4 is 45.0 grams. The simple rule for for obtaining the
grax equivalent weight of an oxidizing or reducing agent is divide
the weight of one mole of the substance by the change in oxidation
number per mole of substance.
In this experiment, you will prepare an approximately 0.1N
KMn04 solution and standardize this solution by titrating against
a standard solution of H2C204 solution. You will then use the
C. - standardized KMnO4 solution to determine the concentration of an
unknown oxalic acid solution. Just as in acid-base titrations
where the number of equivalents of acid must be equal to the
number of equivalents of base, in redox titrations the number of
eq of oxidizing agent = eq of reducing agent
equivalents of oxidizing agent must be equal to the number of
equivalents of reducing agent. For this reaction of KMnO4 with
eq of W n 0 4 = eq H2C204
HzC204. Alternatively, we can express this relationship as
litersoxid X N o x i d = litersted X Nr,d
At the end of a titration, three of the four variables will be

known and the unknown variable can be calculated. In the
standardization process for potassium permanganate, the normality
will be the unknown variable. After the standardization process
has been completed, the oxalic acid normality will be the unknown
variable.
Procedure
The preparation of a stable solution of KMnO4 can be time
consuming process. Traces of MnO2 and many other substances, as
well as exposure to light, catalyze the decomposition of KMnO4
solutions. It is possible to make a W n O 4 solution by diluting a
concentrated W n O 4 solution which has been p r t p u a d well in
advance. The diluted solution should be standardized and used for
analysis within a re1ativelv short per iod of time in order to
obtain good results. Alternatively, calculate the weight of
101
KMn04 required to prepare 250 ml of a 0.1N WnO4 solution.

Check your calculations with your instructor. Weigh the required
amount KMn04 and transfer it to a dark brown bottle. Using
your graduated cylinder add distilled water to give an approximate
total volume of 250 ml. Mix the solution thoroughly by vigorous
swirling and shaking. This solution must be used the day it is
preuared.
Assemble a clean buret and rinse it three times with 5 ml
portions of your KMn04 solution, allowing the rinse solution to
drain through the tip of the buret each time. Discard the rinse
solutions. Fill the buret with KMnO4 solution and allow it to
drain through the buret tip until no air bubbles remain in the
tip. Record the buret reading before beginning the
standardization. Because the KMn04 solution is opaque, the buret
is read at the top of the meniscus.
Standardize your W n 0 4 solution by titrating it against the

standard k c 2 0 4 of known concentration indicated on the bottle
label. Pipet separate 10.00 ml samples of the standard oxalic acid
c- - solution into three 2 5 0 ml Erlenmeyer flasks. Add approximately
25 ml of distilled water to each flask. In the fume hood,
cautiously add 10 ml of 1 2 M H2SO4 solution to each sample using
a stirring rod. CAUTION: &SO4 is very corrosive and should be
handled with great care. Check MSDS notebook for the precautions
and spill cleanup method and record in your notebook. Using a hot
plats, heat the samples to 80 - 9OoC and titrate the hot
solutions with the W n O 4 solution. The W n O 4 solution must be
added very slowly initially. If it is added rapidly, brown MnOa
often precipitates and the titration must be discarded. The
reaction of W n O 4 and HzC204 is apparently catalyzed by
the presence of Mn+2 ions. After a few milliliters of W n O 4
solution has been added, the rate of addition can be increased.
As the endpoint is approached, the W n 0 4 solution should again
be added slowly as in any titration. Since KMn04 is so intensely
colored, it serves as its own indicator. The endpoint is the point
at which a faint pink coloration persists throughout the stirred
solution for at least thirty seconds. When you think you have
reached the endpoint, read the buret and record the volume. Then
add one more drop of m 0 4 . If an intense pink color is
obtained, this indicates that the endpoint was reached before the
last drop was added. Calculate the normality of the KMnO4
solution and repeat the titration until you obtain at least three
values which agree within 2 2 in the third significant digit.
Determine the average normality with the standard deviation. Use
the average normality for the remainder of calculations in the
experiment.
Pipet 10.00 ml samples of the unknown H2C204 solution into
clean 250 ml flasks and treat these samples in the same manner as
the oxalic acid solutions used in the standardization process.
Follow the directions precisely. When you have finished the
titrations, calculate the normality of the unknown oxalic acid
sample, determine the average and the standard deviation.
102
When you have finished, discard the W n 0 4 solution in the

lab sink with large amounts of tap water. Add 10 ml of 3% HzOz
arid 2 ml of 12M HzSO4 to a beaker that contains 50 ml of
distilled water. Use this solution to rinse all of your
equipment that the W n O 4 solution has touched because it leaves
a thin film of MnO2 on glass. The acidic hydrogen peroxide
solution will remove this residue. Then clean all glassware
with soap and water using distilled water for the final rinse.
Construct a data table for the information collected during
the experiment. A results table should include the following
items: normality of standardized KMn04 for each sample, its
average and standard deviation, normality of unknown oxalic acid
solution for each sample, its average and standard deviation, and
a sample calculation for each result.
Quest i ons
C. - 1. What weight of KMn04 would be required to prepare 300 ml of
0.150N KMnOs to be used in this experiment? What would be the
molarity of this solution?
2. A standard oxalic acid solution is 0.300N. What weight of
HZC204. 2 H z O would be required to prepare 1.50 liters
of the standard oxalic acid solution?
3. Tetraarsenic hexoxide, AS406, is frequently used as a primary
standard for W n 0 4 solutions. However, since As406 is
insoluble in H20, it is usually dissolved in NaOH solution,
4NaOH + AS406 ----> 4NaAsOz + 2HzO
and the resulting solution is acidified with hydrochloric acid
NaAsOz + HC1 ----> HAsOz + NaCl
and then titrated with W n O 4 solution. The above reactions do
not involve oxidation-reduction and serve only to prepare the
solution for titration with KMnO4 solution.
a. Balance the following equation.
KMnO4 + HAsOz + HzO + HC1 - - - - > KC1 + MnC12 + H3As04
b. A 0.04852 g sample of As406 was dissolved in NaOH solution,
acidified with HC1 solution, and required 2 4 . 7 5 ml of KMnO4
solution for complete oxidation. Calculate the normality
of the W n O 4 solution.
4. Great care must be exercised in the standardization process to
avoid formation of MnO2 in the early stages of the titration.
Explain why the sample must be discarded if this occurs. Use
balanced equations to aid your explanation.
103
COLLOIDS
A colloid is a very fine dispersion of one substance in

another, in which the substance is not soluble. For example,
a starch-water mixture forms a colloidal dispersion in which
solid starch is dispersed in water. A colloidal dispersion is
like a true solution since the dispersed particles can not be
removed by filtering, however, unlike a true solution all the
particles carry the same electric charge. The principal
distinction between true solutions, colloids and suspensions is
particle size. The particle size in true solutions is less than
10 nanometers (nm) while colloid particles range from 10 to
1000 nm. Neither solutes or colloid particles are visible with an
ordinary microscope, as are the larger particles found in
suspensions. Colloidal solutions do scatter light at right angles
to the light beam and, in addition, the size, shape and g e n e r a l
behavior of these particles determine the intensity and color of
the scattered light. The rapid, irregular movement of colloidal
particles through the dispersion is called Brownian motion.
There are many kinds of colloidal systems, two common types
being liquid dispersed in liquid called emulsions and solid
dispersed in liquid called a s o l . The sols are divided into two
large classes; lyophilic sols in which there is an attraction
between the colloidal particles and the solvent and lyophobic sols
in which there is little or no attraction for the solvent.
Lyophilic s o l s tend to form gels or semirigid liquids, while
lyophobic sols are usually quite fluid.
Colloidal systems may be prepared by condensation w h i c h
“’-ol
LA,*
_.
,-=es building up molecules or ions to colloidil size o r b y
dispersion which involves breaking down larger particles into
clolloidal size. Colloids may be separated from ions or molecules
in true solution by a process known as dialysis.
In a given colloid the particles usually have a charge,
either positive or negative, due to ions adsorbed on the surface
of the particles. Since the particles all adsorb the same charge,
the colloidal dispersion is more stable because like charges
repel. If the charge on the particles is removed or neutralized,
they may form larger aggregrates and separate from the solution.
The colloidal particles can be precipitated from solution, by
adding an oppositely charged ion that has an affinity for the
adsorbed ion, by adding an ion of different charge, or by mixing
colloids of opposite charge.
In this experiment, the student will form a variety of
colloidal systems and investigate their individual properties
1
104
Procedure
Colloidal Fe(OH13
Heat 50 ml of distilled water to boiling and while boiling
add slowly, drop by drop, a solution of 0.5M FeCla until a highly
colored liquid is obtained. This will require approximately 5 ml
of the iron solution. Note the color of the liquid. Assuming
complete hydrolysis of the FeC13, write the equation. Set this
preparation aside f o r later use.
Carbon Black S o l
Put the amount of carbon black that can be held on the tip of
a spatula into a mortar, add 2 ml of water and some tannin. Grind
until the substances are finely mixed. Add 50 ml of distilled
water and set aside for later use. What is the purpose of the
tannin?
Gal
Place 10 m l of saturated calcium acetate solution in a beaker
and ad3 50 ml of reagent alcohol, mixing the solution thoroughly.
c- - Describe what happens. After 5 minutes elapses, invert the
beaker. Cut a piece of this material, place it in an evaporating
dish. In the fume hood try igniting this material with a match
and record the results.
Foam
Dissolve about 5 g of Alz(S04)3. 18Hz0 in 40 ml of hot water.
Add about 0.5 g of detergent. In another beaker dissolve about 5
g of NaHC03 in 50 ml of water. Mix 5 ml of each solution in a 50
ml graduated cylinder and record the results. Explain the results
observed. In a laboratory sink, mix the remaining portions of the
solutions in a large beaker.
Emulsion
Fill two test tubes with 2 ml of kerosene and 10 ml of water.
To one of the test tubes add 4ml of soap solution. Shake both
test tubes vigorously and record the separation times. E x p l a i n
results.
Fi1t ration
Take some of the colloidal Fe(OH)3 and try to filter it. Dc
the same f o r the carbon black sol and the emulsion. Record your
results.
Dialysis
Fill a test tube halfway with the colloidal Fe(OH)3 and in a
second test place a corresponding amount of 0 . 1 M CuC12. Cover the
top of each test tube with a piece of plastic wrap or other
semipermeable membrane which should be held in place by a strong
rubber band. Invert the test tubes, placing each in a separate
beaker of water and allow to stand for 30 minutes. Have either of
the two substances diffused out? Explain the difference.
105
Tyndall Effect
Take some of the Fe(OH)3 solution and hold it in a sharp
narrow beam of strong light. Do likewise for some of the CuClz
solution. Explain the results. Place the Fe(OH)3 solution
against a black background and view the reflected light
perpendicular to the light beam.
Coagulation
Divide the remaining Fe(OH)3 solution into five equal parts
in test tubes or small beakers and label them 1 to 5. Into the
first tube, from a dropper, add 0 . 1 M KC1 counting the drops and
stirring until the colloid precipitates. Into the second tube add
in the same manner 0.1M KzSOs counting drops. To the third tube
add in the same manner as before drops of 0 . 1 M K 3 P 0 4 . To the
fourth tube add in the same manner drops of 0.1M B a C 1 2 . To the
fifth tube add some 0 . 1 M sugar solution.
Colloids, such as Fe(OH)a, are stabilized by electrical
charges. Higher charged ions of opposite sign are more effective
c- -
in neutralizing the charge and causing the colloid to coagulate.
Tn view of these facts, explain why different amounts of the
various solutions were needed to.coagulate the colloid. On the
basis of your results, what is the charge on the Fe(OH)3 colloidal
solution? Why was the BaClz solution not as effective as the
K z S 0 4 solution since each contain bivalent ions? Why was the
sugar solution not effective?
Requirements f o r Report
Write a brief summary of the observations recorded in the
procedure. Be sure to include explanations where required and
answer all questions asked in the procedure.
Chi e 3t ‘Lons
1. How is a colloidal dispersion like a true solution?

2. How is a colloidal dispersion different than a true solution?
3. HOW does a colloidal dispersion acquire an electrical charge?
4. How does a suspension differ from a colloidal dispersion?
106
COLLIGATIVE PROPERTIES
The addition of a nonvolatile solute to a solvent produces

characteristic changes in the physical properties of the solvent.
For example, when salt is used to freeze ice cream, the salt-ice-
water mixture's temperature drops below the temperature observed
for an ice-water mixture itself. Also we know that when
antifreeze, ethylene glycol, added to an automobile's cooling
system prevents freezing in the winter and boiling during the
summer because the antifreeze solution has a lower freezing point
a n d a higher boiling point than pure water.
The figure below is a plot of the vapor pressure of pure

water, solid line, and the vapor pressure of a water solution
containing a dissolved nonvolatile solute, dashed line. Pure
water boils at 1 O U o C when its
vapor pressure is 760 torr. When a
C. "
nonvolatile solute is added forming
a solution, solute molecules or
ions occupy part of its surface
area. This inhibits the water
molecule's movement into the vapor
state causing a vapor pressure
c lowering of water, a , under the 760
torr value. Since the solution's
vapor pressure is less than 760
torr, it does not boil at 1 O O O C .
For the aqueous solution to boil,
its vapor pressure must be
t' T m r t u r e I-Cl 1W
0 t raised to 769 torr by increasing
the solution's temperature above
100cC. "hi: is t h e boiling point
elevation, b, of the water due to the solute. The freezing point
depression, c , results from the solute molecules inhibiting the
formation of the crystal lattice necessary for water to solidify.
Water's normal freezing point is OoC, however, the freezing poir?t
of an aqueous solution containing a nonvolatile solute is lowered.
Vapor pressure lowering, boiling point elevation, and
freezing point depression are colligative properties of
solutions. These properties are determined by the number, rather
than the type, of solute particles dissolved in the solvent. For
example, an equal number of moles of glucose or urea lower the
freezing point of a fixed amount of water to the same temperature.
One mole of NaCl and 2 moles of glucose in the same amount of
water produce the same effect on the colligative properties of the
solution because one mole of NaCl prodaces L w t ; m ? e s of solute
particles, Na+ and C1-, whereas the 2 moles of glucose remain
unionized.
107
The change in the colligative proerties of an aqueous

solution is directly proportional to the amount of solute
dissolved in the solvent. For water, one mole of a nonvolatile,
nonelectrolyte dissolved in 1 kilogram of water, a 1 molal solution,
produces a solution with a boiling point elevation of 0.51oC and a
freezing point depression of 1,860C. The freezing point
depression, A T f , and the boiling point elevation, A T b , are
proportional to the molality, m , of the solute in the solution.
ATi = Kfm
ATb = Kbm
m = moles of solute = jtz/ GFW) solute
kg solvent kg solvent
Kf and Kb are molal freezing point and boiling point constants for
the solvent.
c-
In this experiment you will determine the gram formula weight
of a nonvolatile solute in tertiary butanol by measuring the
freezing point for pure t-butanol and for the solution containing
a mass of solute, The mass of the solvent and solute must be
determined by weighing. The molal freezing point constant] Kf ,
is S.loC-kg/molal and pure t-butanol's freezing point is 2 5 . 5 0 C .
Using the above equations you will calculate the moles of solute
and also the solute's gram formula weight.
The freezing point of t-butanol and that for the solution will be
obtained from a cooling curve, a graph of decreasing temperature
as a function of time. The figure below illustrates that
1
108
t-butanol’s cooling curve achieves a plateau at its freezing point.

Extrapolation of the plateau to the temperature axis determines
its freezing point. The student should be aware that supercooling
may occur and consequently, the temperature should be monitored
for at least ten minutes after it appears that a plateau has been
reached. The solution’s cooling curve does not achieve a plateau,
but continues to decrease slowly as the t-butanol freezes. Its
freezing point is determined at the intersection of two lines
drawn tangent to the curves above and below the freezing point.
Procedure
Assemble the apparatus shown in the figure at the left.
Weigh a clean, dry 200 mm test tube
in a 250 ml beaker to the nearest
0.01 g. Add approximately 10 -
1 5 g of t-butanol to the test tube
and reweigh the tube and contents
to the nearest 0.01 g. Record both
measurements. Prepare about 300 ml
of an ice-water mixture in a 400 ml
beaker. A 600 ml insulating beaker
which may be filled with cold water,
near OoC, to minimize heat
absorption for the surroundings by the
ice-water mixture in the 400 ml beaker.
“OY Insert a 1100C thermometer in a two
hole rubber stopper using glycerin as
a lubricant. Carefully remove all
traces of glycerin from the thermometer. Insert the wire
stirrer in the other hole before stoppering the test tube.
Heat the test tube and contents to 450C by inserting it in a
beaker of warm water. Place the test tube and contents in the
ice-water bath and while stirring with the wire, record
temperatures to the nearest 0.loC at 1 minute intervals. The
temperature remains constant at the freezing point until
solidification is almost complete. Continue recording until the
temperature begins to drop again. The freezing point
determination may be repeated by simply immersing the test tube
and its contents in the warm water beaker again and repeating the
temperature-time measurements. On graph paper, plot the
temperature, vertical axis, versus time, horizontal axis, to
obtain t-butanol’s cooling curve.
Melt the t-butanol in the warm water bath to remove any of the
solvent from the thermometer and wire stirrer. Remove the stopper
from the test tube and dry the outside of the test tube and
reweigh the test tube and contents in the 250 ml beaker to the
nearest 0.01 g . Obtain an unknown from the instructor in a
/
109
weighing boat. Quantitati rely transfer the 1 nknc Jn to the test

tube and reweigh the tube to the nearest 0.01 g . Record the
weight measurements. If the unknown adheres to the sides of the
test tube roll the solvent in the test tube until the solute
dissolves. The wire stirrer may be used to aid in forming an
uniform solution. Replace the stopper in the test tube and warm
the solution to 4 5 o C hy placing it in a beaker of warm water.
Place the test tube in the ice-water bath and while
stirring with the wire, record temperatures to the nearest 0 . l o C
at one minute intervals. A break will occur when the solution
nears its freezing point and the time interval should be shortened
to 30 seconds. This break may not be as pronounced as the plateau
was for the pure solvent. Plot the temperature versus time on the
same graph as the cooling curve for pure t-butanol. Draw the
t.angent lines to the curve above and below the freezing point.
The intersection of the tangent lines is the solution’s freezing
point.
Warm the test tube and its contents in the warm water beaker.
Remove the stopper and wire stirrer. Dry the outside of the test
tube and reweigh in the 250 ml beaker. Obtain from your
instructor an additional amount of the same unknown sample and
quantitatively transfer to the test tube. Reweigh the tube and
contents. Record these measurements. Repeat the freezing point
determination and plot the data on the same graph. After all
experimental data has been completed, dispose of the contents in
the test tube by adding a warm soap water solution to the tube and
discard in the laboratory sink with large amounts of tap water.
The graph of experimental data must be clearly l z k c l l c d LZCI
freezing points of the solutions and t-butanol indicated on the
temperature axis. All weight measurements and results should be
tabulated. A sample calculation for the gram formula weight of
the solute should be demonstrated.
110
Questions
1. A 0.578 g sample of a nonvolatile solute dissolves in 15.0 g
of t-butanol. The solution freezes at 2 3 . 0 o C . What is the
gram formula weight of the solute?
2. If ten grams of t-butanol and the same mass of solute were
used in the above problem, would you expect the freezing point
depression to be larger or smaller than that observed for the
solution in the above problem. Explain.
3. If the solution’s freezing point is mistakenly read 0 . 2 0 C
lower than it should be, wiil the gram formula weight be too
high or too low? Explain.
4. If the t-butanol is initially contaminated with a nonvolatile,
nonreactive nonelectrolyte, how does this affect the reported
gram formula weight?
5. If the thermometer is miscalibrated 0 . 5 0 C higher than the
actual temperature over its entire scale, how will it affect
t h e reported gram formula weight of t h e solute? E x p l a i n .
111
CALORIMETRY
In nearly all chemical and physical changes, a transfer of
heat energy is observed. This heat flow for a chemical reaction,
measured in a calorimeter, is quantitatively expressed as the heat
of reactions or enthalpy of reaction, AH, at constant pressure and
temperature. Reactions evolving heat are exothermic reactions and
their A H values are negative. Reactions absorbing heat are
endothermic reactions and their A H values are positive.
In this experiment three calorimetric determinations will be
conducted. First, a calorimeter constant will be determined for
the calorimeter used in subsequent measurements of enthalpy of
reaztions. Second, a heat of neutralization, A h , for a strong
acid/strong base reaction will be determined. Third, the heat of
solution, A H s , will be measured for a salt dissolving in water.
Calorimeter Constant
c- When a chemical process is carried out in a calorimeter,
some of the heat transferred during the reaction is absorbed by
the environment. For example, hot coffee in a Styrofoam cup loses
heat to the cup and surrounding air. In other cases, some heat is
released by the calorimeter to the chemical system. An example of
this would be ice melting in a styrofoain cup since it would
absorb heat from the cup and immediate environment. Heat energy
always flows from a hot system to a cold system. The calorimeter
constant will be measured by adding warm water to cold water
contained in the calorimeter. Since the heat energy which is lost
by the hot system must equal the heat energy which is gained by the
Qhot = Qcold + Qcal
cold system the calorimeter and surroundings must be considered a s

part of the cold system. If the heat transferred to the calorimeter
and surroundings is divided by the experimental temperature change,
the calories transferred to the calorimeter and surroundings per
degree of temperature change is referred to as the calorimeter
constant. The number of calories per degree will be essentially
the constant for any similar reaction run in that particular
calorimeter if the temperature change and the volume of the final
solution is approximately the same as that used in the
determination of the calorimeter constant.
The calorimeter constant can be calculated using the data
from the mixing of hot and cold water in the calorimeter.
where Q c a l is the quantity of heat transferred to the calorimeter

and surroundings, Q h o t is the quantity of heat transferred from
the hot water, and Q c o l d is the quantity of heat transferred to
I
112
the cold water. Equation 3 allows the calculation of heat
Q = m (g) X Cp (cal/g-oC) X AT (0C) (3)

transferred by the water where m is the mass of water, C p is the
heat capacity of water, and AT is the temperature change of
water. By substitution into Equation 2 , the following Equation 4
results. Rearrangement of Equation 4 allows the calculation of
the calorimeter constant where A T c a l is the temperature change of

t h e calorimeter.
Heat of Neutralization
C.
The reaction of a strong acid with a strong base produces
H+ + OH- ---> Hz0 + heat
water and heat. The heat evolved during a reaction taking place
Qrxn = Qiq + Qcal (6)
in a calorimeter must be the sum of heat absorbed by the liquid
reaction mixture and the heat absorbed by the calorimeter. The
density and heat capacity of combined acid-base solution is
assumed to be equal to those of water. The temperature change is
measured for the reaction mixture and the same temperazure change
Is assumed for the calorimeter. When th;= :31c:r'-es p r ~ d u c e dfor
Qrxn = (mCpAT)liq + (Ccal A T c a l ) (7)
this reaction have been calculated from Equation 7, it can be

converted to the enthalpy of neutralization by dividing by the
number of moles of water produced. The acid will be the limiting
AHneut = Qrxn
moles of HzO
reactant for the neutralization reaction. The enthalpy of
reaction can then be compared to the expected A H for the reaction
of HC1 with NaOH.
Heat approximately 200 ml of distilled water to 4 0 0 C on a
hot plate. Support the calorimeter, the two cup assembly, in a
250 ml beaker. Place 50 ml of room temperature distilled water
in the calorimeter. Suspend a thermometer, using a clamp and
ring stand, so that the bulb of the thermometer is immersed in the
water in the calorimeter. The thermometer should not touch the
sides or the bottom of the calorimeter and should be capable of
being read easily. Weigh a 100 ml beaker to the nearest 0.01 g.
Place approximately 50 ml of the warm distilled water in a 100 ml
beaker and reweigh. Record the weight of warm water. Suspend a
thermometer in the warm water in similar fashion as described
above. F o r a 5 minute period, measure and record the temperatures
at 30 second intervals.
While stirring the sample of water in the calorimeter,
rapidly p o u r the hot water in the beaker into the cold water. To
e n s u r e total transfer of the hot water reweigh the 100 ml beaker
st the erla of trial. Record time of mixing and continue to
measure and record temperature-time data for a 15 minute period
c-
at one minute intervals. Construct a graph where the temperature
is the vertical axis and time is the horizontal axis. Plot the
temperature-time data on the graph. Draw a vertical line on the
graph to represent the time of mixing. The best straight line
curve is drawn through the plotted points prior to the time of
mixing. These curves are extrapolated so that they intersect the
line representing the time of mixing. The best straight lina
curve is drawn through the plotted points after the time of
mixing. This line is extrapolated so that it intersects the line
of mixing. The point of intersection represents the maximum
temperature achieved by the mixture in the calorimeter. The
difference between the initial temperature of the cold water and
38
37
36
u
28
28
26
1
114
Heat of Solution
The lattice energy of a s a l t , A H ~ and
~ , the hydration energy,
A H h , of its composite ions govern the quantity of heat evolved
or absorbed when it dissolves in water. Lattice energy, an
endothermic quantity, is the energy required to vaporize 1 mole of
the salt into gaseous ions. Hydration energy, an exothermic
quantity, is the energy released when gaseous ions are attracted
and surrounded by water molecules as a solution forms. The heat
of solution, H s , is the difference between these two energy
AHLE = A h + AHs
values and may be either an exothermic or endothermic process

depending on the magnitude of the lattice energy and hydration
energy for a particular salt.
In t h i s experiment the heat transferred by the dissolution of

N H 4 C 1 can be calculated by using equation 9 . The heat transfer
for the calorimeter, Q c a l , is dependent on the temperature change

observed in the solution. The heat transfer of solution, C a s o l , is
determined by total mass of solution, combined salt and water,
Qsol = (mass of solution)(heat capacity of solution)(AT)
times the heat capacity of the solution times the temperature
change observed. To find the enthalpy of solution, A H s , the
AHe = QS
moles of N H 4 C 1
heat transferred, Q s , is divided by the number of moles of N H 4 C 1
dissolved in the water. This value can be compared with a
literature value.
Procedure
Calorimeter Constant
Obtain two 6 ounce Styrofoam cups and lid from instructor.
Place one cup inside the other. Before starting measurements of
the calorimeter constant, 150 ml of hot distilled water should be
placed in the inner cup and allowed to stand for several minutes.
This process should be repeated several times to remove any
residual chemicals remaining after the manufacturing process for
the cup. If this is not done, difficulty may be encountered in
obtaining a consistent calorimeter constant.
115
the maximum temperature of the mixture is the temperature change

for the cold water. In similar fashion, the temperature change
for the hot water can be found. Calculate the calorimeter
constant as described in the introduction.
Repeat the entire procedure and determine the second
calorimeter constant. If values agree within 5%, proceed to the
next section and if they do not, repeat the procedure until
agreement is obtained.
Heat of Neutralization
Measure 50 ml of 1.00 M HC1 at room temperature into a clean,
dry calorimeter. Suspend a thermometer in the solution in the
same manner as described in the first section of the procedure.
Weigh a clean, dry 109 ml beaker. Measure 50 ml of 1 . 0 5 M NaOH
at room temperature into the 100 ml beaker and reweigh. Record
b o t h weight measuremeiits. Suspend a thermometer in the N a U i i
solution. Adjust the temperature of the NaOH solution by heating
or cooling until the temperature is the same a s the HC1 solution.
--. F a r a 5 minute period, measure and record temperature-time data
f o r the t w o solutions at 1 minute intervals.
While stirring the HC1 solution in the calorimeter with a

g l a s s stirring rod, pour rapidly the NaOH solution into the HC1
solution. Record the time of mixing and continue to measure and
record temperature-time data for 15 minutes at one minute
intervals. Construct a graph similar to that described in the
previous section of the procedure. Plot the temperature-time
data and draw the best straight line for piotted points before
mixing and the best straight line for the plotted points after
mlxirig. Extrapolate both lines to intersect the vertical line
representing the time of mixing. From the graph deLerrriiiie t i l e
-axi-miirri temperature at mixing and calculate the temperature chs.nge
for the solution. Reweigh the 100 ml beaker which contained the
NaOH solution. Determine the heat transferred and the
enthalpy of neutralization using the equations found in the
introduction section. Repeat the entire procedure for a second
determination. Compare average enthalpy value to literature
value.
Heat of Solution
Measure 2 . 5 to 2 . 8 g of ammonium chloride in a weighing boat.
Record mass of boat and ammonium chloride. Place 100 ml of room
temperature distilled water in a clean, dry calorimeter. Suspend
a thermometer in the calorimeter as previously described. For a
5 minute period, record temperature of the distilled water at 30
a e ~ o n dintervals. While stirring with a glass stirring rod,
rapidly add the ammonium chloride and save boat to reweigh later.
Note the time of mixing and continue to measure and record
temperature-time data for a 15 minute period at 30 second
intervals. Construct a graph of the data with temperature on the
I
116
ordinate and time on the abscissa. The same procedure should be

followed to obtain the maximum temperature change by
extrapolation. The heat capacity for the ammonium chloride
solution is 0.966 cal/(g-oC). Remember the mass of the solution
is the mass of water plus the mass of salt used. Reweigh the
weighing boat to determine the mass of ammonium chloride added to
the water. Refer to the equations in the introductory section to
calculate heat transferred, and the enthalpy of solution. Repeat
for a second determination and compare the average value to the
literature value found for N H 4 C 1 .
Report must include all graphs and calculations for heat
transfer, experimental enthalpy values, literature enthalpy
values, and relative error percent on the comparison.
c-
3
117
RATES OF REACTION
A . Factors that affect reaction rates.
The study of chemical reaction rates, mechanisms

~7f reaction and control is called chemical kinetics.
The rate of a chemical reaction is defined as the change in
reactants (or products) concentration divided by the time required
for this change. The unit of time may be seconds, minutes, hours,
days or years. Rates are also, affected by five factors which are
listed as follows: (1) Nature of the reactants, i.e., once metal
may react vigorously with acid while another does not react. (2)
The particle size of the reactants, i.e., a lump of coal b u r n s
slowly but powdered coal may explode. ( 3 ) Temperature increases in
general increase the rate of reaction, i.e., a 1 O o C rise in
-__
.temperature doubles the reaction rate. ( 4 ) Catalysts affect the
rate by using or allowing a different pathway for the reaction to
follow. There still is a great deal of things to learn in this
topic. (5) Concentration affects the rate of reaction, i.e.,
if the concentration of one of the reactants is doubled and is an
integral part of the reaction the rate increases appropriately.
To study the factors that affect the rate of a
chemical reaction they must be isolated one from another.
Procedure
[l] Nature of the reactants:
(a) Into 4 separate 150 mm testtubes place 1 ml each of 3M s u l f u l i ,
acid, 6M hydrochloric acid, 6M nitric and 6M phosporic acid.
[Review the handling procedures for acids.]
Next place a small piece of polished magnesium strip into each
testtube and record your observations.
(b) Into 3 separate 150 mm testtubes place 2 m l of 6M hydrochloric
acid. To one tube add a piece of zinc metal, to the next add a
piece of lead and to the third add a piece of copper. Record your
observations.
[2] Size of the reactants:
(a) Prepare a 250 ml side arm flask with a thistle tube and a one
hole stopper. Connect to the side arm a rubber tube with a piece of
bent glass tube in the other end.
Arrange a beaker of water with an inverted 250 mm test tube filled
with water so as to collect evolved gas.(See page 131 in CTRRH)
Next place about 3 g of marble chips into the flask and 50 ml of
water. Insert the stopper with the thistle tube into the neck of
the flask and make sure the end of the thistle tube extends below
the water level in the flask. Now slowly add 10 ml of 6M HC1
through the thistle tube. Record your observations.
(b) Clean the generator flask and set it up again as before, but
replace the marble chips with 3 g of ground up chips or with
powdered calcium carhnnPte Repeat the p r c , c + d l l r + a q h e f nre s n d
compare the results with the first trial.
1
118
[3]Temperature:
(a) Some reactions lend themselves to rate determinations. The
reaction of HCl and thiosulfate is such a reaction:
HC1 + NazS203 = S + SO2 + NaCl + H2O
the formation of the sulfur is time related. In three testtubes
place 5.0 ml of 0 . 1 M thiosulfate and in a second set of three
test tubes place 5.0 ml of 0.1M H C 1 . Now taking one set of the tubes
each; place them in (1) an ice water bath, (2) a hot water bath at
7 0 O C , ( 3 ) a room temperature setting. Starting with the room
temperature pair, pour the acid into the thiosulfate solution and
stopper and mix thoroughly far a few seconds. Record the mixing
time and measure the time until the first cloudiness appears.
Next repeat the process with the tubes in the icebath. Again
record the time elapsed from mixing to the appearance of the sulfur.
Last mix the heated solutions and replace them into the warm water
and record the time. When all the data has been collected plot the
C. - temperature on the y-axis and the time on the x-axis. Discuss the graph.
(b)Another reaction theat exhibits the affects of temperature is
the reaction of oxalic acid with permanganate.
5HzCz04 + 2KMnO4 + 3HzSO4 = 1OCOz + 2MnSO4
+ 8 H z O + KzSOs
Place 10 ml fo 0.3M oxalic acid in a 10 ml Graduated cylinder and
2.0 m l of 0.01M permanganate solution in a 250" testtube with 8.0
ml of 3M sulfuric acid. When one student mixes the solutions the
other should record the time and ther temperature. When the purple
color disappears the time is recorded. Repeat the experiment at
40oC allowing some time for the solutions to reach the temperature
of the water. Again pour the oxalic acid into the permanganate and
record the temperature and time. Do the same thing at 800C and
record the data. Plot the temperature versus time as before and
discuss the graph.
[ 4 ] Presence of a catalyst: The affect of a catalyst on peroxide
decomposition exhibits the property of this factor.
Procedure: In a 250" testtube place 5 ml of peroxide solution
provided for the reaction, In a second tube place another 5 ml of
the peroxide solution and a pinch of manganese dioxide.
Observe and compare the two solutions. Try warming the tubes in a
water bath.
[5] The affects of concentration on reaction rate: A reaction
called the time clock or iodine clock reaction gives a good answer
to the affect of concentration on rate.
2HI03 + 5HzSO3 = I2 + 5H2SO4 + H2O
I2 + starch = 12-starch (complex) blue
Procedure
Into a 150 ml beaker labeled ( A ) place the following,
3.0 ml of 0 . 1 M iodate, 5 ml starch and 92.0 ml of distilled water.
T - i t C a n o t h e r 1 5 0 m l beaker labeled (E] place 10.0 m l of 0 . 1 M
,bisulfite ion plus 90.0 ml of distilled water.
3
119
Next place a sheet of white paper on the desktop and on top of that
p u t a clean dry 250 ml beaker. Now while one student holds the
flasks labeled A and B, another will mark the time of mixing and
the running time of the reaction. The first student on the
signal of the student doing the timing will pour the two beakers
contents together into the 250 m l beaker. When the b l u e complex just
shows the time is complete. Repeat the experiment, but this time adjust
the concentration of the (A) beaker to 6.0 ml of iodate, 5 ml of
starch and 89.0 ml of water. The solution in (B) is held constant.
With a clean dry 250 ml beaker repeat the above procedure.
Thirdly, adjust the solution ( A ) to 10.0 ml of 0.1M iodate, 5 m l
of starch and 58.0 m l of water. Again repeat the prior procedure.
When the three trials are complete plot the concentration of the
iodate versus time in seconds. Remember the solutions were diluted.
Requirements for report
Follow the established guidelines for the writng of the
report.
c- - 0 1 e s t,i ons
1 . What factors effect the rate most markedly? Why?

2. In the time clock experiment would the acid concentration be
imp0rtant?
[Reference:Fundementals of Chemistry by Brady and Holum, published

by John Wiley and Sons]
1
120
B. DETERMINATION OF A RATE CONSTANT
To study the properties of hydrolysis of an organic

molecule and use these properties to gain knowledge of the rate of
a chemical reaction.
The rate of a homogeneous reaction is dependant
on the factors that affect the rate, i.e., nature of the reactants,
temperature, concentration of the reactants, catalysts and physical
state and size. For reactions in solvents the nature of the solvent
interaction must also be included as a factor that may affect the
rate of hydrolysis of the organic molecule in its conversion to the
product that will be studied.
We will be utilizing a molecule called an organic halide and will
be reacting this material with a mixed solvent to moderate the
--- speed of the reaction. The following is a representative example of
the reaction equation.
RX + H2O = ROH + H+ + X-
‘The term RX represents the organic molecule and some examples for
this are t-amyl chloride, t-butyl chloride or t-butyl bromide. ROH
the reaction product formed after the hydrolysis of the halide. The
important part of the products side of the reaction is the
generation of the hydrogen ion which will allow monitoring of the
reaction progress.
The rate of the reaction is dependant on the first step of the
reaction; HC1 == R+ + C1- which is slow in comparison
to the rest of the reaction steps. This step is designated as the
rate determining step because the sequential steps occur quickly
once the carbon cation(carb0nium ion) is formed. The resulting
reactions may take one of the following paths;
( 1 ) R+ + H2O = ROH + H+
(2) R+ + HOR = ROR + H+
( 3 ) R+ = R’C=CH2 + H+
In each case a mole of hydrogen ion is produced per mole of
reactant so our monitoring of the reaction is independant of the
pathway after the cation formation.
Since in equation(2) a reaction with the alcohol solvent is noted
and in equation(1) with water the solvent properties must be
considered in all portions of the reaction or we lose overall
knowledge of which factors are affecting our rate.
This reaction, the hydrolysis of the organic halide is a first
order reaction, i.e., the rate is proportional to the concentration
of the organic halide to the first power.
121
This basically is true unless there is competition with the solvent
in the first step of the reaction. The hydrolysis is therefore
adjusted by maintaining a constant composition of a mix of water
and an alcohol such as isopropyl alcohol.
When a substance is being consumed by means of a reaction of first
order rate its concentration decreased at an exponential rate thus
if No is the initial concentration then at some later time (t)
Nt is the concentration. It can be shown then that
Nt = No e-kt
where k is the specific rate constant and equals the k in the rate
equation. The above equation can be rearranged to the following;
2.303log(No/Nt ) = kt
If we know the initial concentration of the reactant No and

measure the reactant Nt at measured time intervals we can graph the
log(No/Nt) versus time and for a first order reaction the slope
of the line will equal k/2.303. Since it can be shown that the
units of concentration cancel in the ratio No/Nt it is not
c_ necessary to use concentration but only the total amounts of
reaLLdrit(vO1umes) at time zero and at time t or Ao and At.
A measureable rate of hydrolysis for t-butyl chloride is obtained
with a solvent mixture of 60% isopropyl alcohol and 40% water
by volume. A solution of 50:50 IPA and water is about a factor of
4 times faster than the 60:40 mix. The method is fairly easy fot
the determination. A measured volume of the halide is added to a
volume of the specified solvent. Then 10 to 15 drops of
phenolphthalein is added and finally a starting volume sodium
hydroxide made up in the same solvent mixture is added. The amount
of NaOH may be from 1 to 5 ml. The flask is stoppered and shaken
a i d dhen the indicator color fades the time is taken. Another
Fgrtion of base is added, shaken and the time to fading is noted.
This process continues throughout the lab period and then the mix
is set aside until the following lab period. At that time the final
titration is done to determine the value of A o .
The calculations for the plot then are simply the value Ao(tota1
volume of titrant) in the numerator and Ao minus the volume at time
(t) in the denominator. The logio of the ratio is taken and
plotted against the time for that particular titrations fade time.
Procedure
Prepare enough of the solvent mixture(60:40,50:50)
to allow for t w o trials of 100 ml each and 100 ml for the
preparation of the titrating base.
Next weigh about 0.40 g of NaOH and dissolve it in 100 m l of the
solvent mixture and set it aside for filling your buret when you
begin the experiment.
Now using a clean, dry Erlenmeyer 250 ml flask pour in 100 ml of
the solvent and add 10 drops of the indicator. Place the flask into a
prepared water bath at the temperature you will use for the
experiment. Most will start with a room temperature trial. Allow
ten minutes for equilibration and then the flask to the HOOD
,-, ~-
A b - qrganic halides are to be dispensed. Pipet 1 ml of the
r
u e the flask and mix well and mark this as the starting
~ ~ i \ i ~ir11;o
time.
122
Now using the base solution that has been placed in the buret add
on to two milliliters to the flask and measure the time until the
indicator turns colorless. Mark this time for that base addition.
Add another portion of base and continue the process until the
time of the lab period has expired. Then place the stoppered flask
in your locker until the next lab period where the final titration
will be performed.
The experiment will also be done at a different temperature
setting. The directions are the same except that the flask will
be kept in a temperature bath during all the tiration activities.
DATA: When all the data has been collected for all trials you
will begin the calculations to generate your plotting points for
the graph.
The value called Ao will be defined as the total volume used
f o r the titrations through the final titration done the following
l a b period. The time at the final titration is called infinite.
The values for the concentration A t are determined by taking
the difference between A0 and the total titration volume at
time (t). For example if AO is 6 9 . 7 0 ml and the volume after
125 sec is 3 . 6 7 ml then A t = 6 9 . 7 0 - 3 . 6 7 or 6 6 . 0 3 ml. This is
then divided into Ao and the loglo is taken and plotted against
the value for time in seconds or minutes.
Reauirements for report
Follow the guidelines established to write your report and in
the conclusion discuss the effects of temperature on your results
Questions
1. What other rate affecting properties could be studied with this
reaction?
2. Does the volume of water versus alcohol raally effect the rate?
3. What other solvent system could be s t u d i e d ?
[Reference:Laboratory Studies and Problems in General Chemistry by
Stone and McCullough published by McGraw-Hill]
1
123
C. DETERMINATION OF THE ORDER OF A RATE EQUATION

The utilization of our knowledge of the rate law for a chemical
reaction can be used to determine the order of reaction.
In a reaction the rate equation;
rate = k[A]a [B]b
is a function of the concentrations of the participating species
raised to a power relating the order to which that reactant affects the
rate. For example, if the concentration of A is doubled with everything
else held constant and the rate is increased by a factor of four, the
value for a is two( a=2). Likewise, if the concentration of B is changed
and the other factors are held constant and there is a one to one change
t h e n b is one ( b = 1) and is first order. The specific rate constant k
o n l y varies with temperature and is unaffected by concentration changes.
In this experiment we will determine from the reaction kinetics of
[S2O8-2] and [KI] the rate law and the order with respect to each
reactant.
rate = k[S208-2]x [KI]Y
c- "We will accomplish this investigation by a variation of concentration
of each of the two reactants versus time. The results are then plotted
as a function of the l o g rate versus log [ 3 . This method allows us to
take the rate equation:
rate = k[A]aC(constant)
and holding one reactant constant and taking the log,
log(rate) = log k + a log[A] + log C
where log k and log C are constants for this reaction and the equation
becomes
where m is the lope of the plotted line and the value for th order of
the reaction. Treating both reactants this way we can then substitute
the values into the rate equation and solve for k.
The experiment requires an intermediate to help measure the rate of
formation of I2 with time, so we will use a constant volume of sodium
thiosulfate to give a time interval before the formation of the free
Iz. The reaction equations are as follows:
S208-2 + 21- = 2S01-2 + I2
I2 + starch = 1 2 - starch( complex)
Procedure
To summarize the experiment a table will give the
composition of the five test solutions we will use to calculate the
values for the order of the reaction for the two reactants.
124
1 ! 148 ml ! 10 ml ! 2 ml 1 10 ml I 1
30 ml I 1
2 ! 133 m l ! 20 ml ! 2 ml ! 10 ml I I
30 ml d
3 ! 128 m l ! 30 ml ! 2 ml ! 10 ml 1 1
30 ml , I
4 1 108 ml ! 30.1
ml ! ml ! 1 1
50 m
5 1 88 ml ! 30 ml ! 2 ml ! 10 ml I t
7 0 ml 1 ,
-Prepare solution A for trial 1 in a clean 250 ml beaker. Mix the

solution and record the temperature.
-Next measure 30 ml of 0.1 M persulfate into a clean 100 ml beaker and
record the temperature.
-Now add solution B to A and start timing the reaction with a
stopwatch. The appearance of the blue end point is sudden so place the
250 ml beaker on a white background for easier observance of the end
point.
-
c- -Repeat the above procedure for the next four test solutions recording
bcth time and temperature.
Calculations The data from the above experiment must now be adjusted
to give us the needed information for our rate law determination.
-First the concentration of the thiosulfate is used to determine the
amount of iodine(1z) that is formed in each trial. The moles of iodine
is exactly one half of the moles of thiosulfate. This value is then
divided by the time interval for the specific trial and the l o g of this
value is taken. This is the first half of the information needed to
plot the graph of l o g rate versus l o g [ 3 .
The concentration of the iodide ion is next determined. The total
volume of the mixture of the two solutions is 200 ml. If for trial one
we use the concentration of the 10 ml of 0.3 M KI diluted to 20U ml, we
then get the value of 0.015M KI. Now we take the l o g of this value and
plot it with the first value.
This is continued for the first three trials.
Another graph of the trials 3 through 5 is done the same except the
concentration of the persulfate is substituted for the iodide.
When the order of the reaction is determined for each of the
participants, then the value for k is found by simply substituting the
concentrations of iodide and persulfate raised to their respective
powers and the value for the rate at that trial and just calculate.
7
0 0
Follow the established guidelines outlined for report writing.
1. What is the effect on the experiment when the starch solution is

old?
2. Would more starch increase the rate of the reaction?
[Reference:Fundementals of Chemistry by Brady and Holum published by
John Wiley and Sons]
125
D. DETERMINATION BY SPECTROPHOTOMETRIC STUDY THE RATE OF

BROMINATION OF ACETONE
We will utilize our knowledge of the rate law and the factors
of the visible spectrum to study the kinetics of the bromination of
acetone in the presence of an acid media.
In the rate equation; rate = k[Alx[B]~ the values of
A and B are concentration dependant factors. The values of x and y are
dependant on their affect on the rate of the reaction and likewise the
value for k is dependant on the rate law and temperature. With careful
planning each of the nonconcentration dependant variables can be deter-
mined by varying the concentration of the reactants while holding other
parameters in the reaction constant. This reaction is a case in point.
We will be doing a study of the affect of three reacting species by
varying the concentration of one while we hold the other two constant at
constant temperature. Our reaction is
H3CCOCH3 + Brz + H+ = H3CCOCH2Br + HBr
c- .
With three variables, the logistics become rather formidable but we are
aware of the fact that the order of the reaction with respect to bromine
is zero; and, therefore, its concentration has no affect on the rate of the
reaction. We will test this fact but needless to say it reduces the work,
needed to complete the study of this reaction. Another factor we can study
in this reaction is the value called the activation energy (Ea). This
is found by the following equation:
log k = -Ea/(2.303RT) + const.
k at two different temperatures an;! plot
if we take the value for log
LL Vthe
S Cvalue 1/T, the slope of the line is equal tc - E a / / 2 . 2 2 2 E .
~ ~ U
One other factor we need to discuss is the method of following the

FrDgress of the reaction. Since neither acetone nor hydrogen ion is
colored, they don’t absorb light, but bromine absorbs light until it
is converted to the bromide ion. We can monitor the progress by the slow
disappearance of the bromine color. To do this, we must use an instrument
called a spectrophotometer which has the ability to distinguish between
small concentrations in the material being analyzed. For a given analyte,
the instrument at a specified wavelength will respond according to
the following equation:
Absorbance(A) = a [Brz]
At 390 nm of wavelength bromine absorbs strongly and therefore we will
use this as our selected wavelength. We will run a series of different
concentration of the bromine to determine the value of (a) a constant
of absorbance for bromine. Once this value is known, we can compute the
concenterationsof the bromine from the absorbance data and use this in
our plots of conc changes versus time to determine the rate of the
experiment. By varying one concentration, we can determine the order
due to that species. When this is determined the value for k can be
determined; and, thus, the value for the activation energy of the
reaction is found.
126
Procedure
Prepare the following solutions in volumes of lOOml for
the experimental procedures: 4M acetone solution is made by diluting 2 9 . 5
ml of acetone with water to a volume of 100 ml total volume, 1M HC1
solution, and from the instructor get 100 ml of 0.02M bromine-water
solution.(This must be handled very carefully and protective gloves and
eyewear is mandatory.)
Determination of the absorbance constant is done by testing various
concentration of bromine solutions made by pipeting 10 ml of bromine stock
into a fifty ml volumetric flask and then adding 10 ml of HC1 stock and
diluting to the mark. Next pipet 5 ml of bromine and follow the above
directions, repeat with 2 ml of bromine stock. The instructions for
the use of the spectrophotometer will be given separately by the instructor.
Determination of the rate and rate law constants. We will use the
values from the following table:
Trial Number Volume of Volume of Volume of Volume of
acetone HC1 bromine water
(4M) (1M) (0.02M) (ml>
c- - (ml) (ml) (ml)
1 10.0 10.0 10.0 20.0
2 10.0 10.0 10.0 20.0
3 5.0 10.0 10.0 25.0
4 10.0 5.0 10.0 25.0
5 - 10.0 10.0 20.0 10.0
Step 1: Pipet 10.0 ml of the acetone into a clean 125 Erlenmeyer flask;
and, to this, add 10.0 ml of acid and 20.0 ml of distilled water.
In a similar flask, pipet 10.0 ml of the bromine solution. Measure
the temperatures of the two solutions being sure that they are
within 0 . 5 degrees of one another.
Make sure your machine has been setup for the measurements and
then carefully mix the two flasks by pouring the solutions back and forth
a few times. This is the starting time for the reaction. Carefully plac=c
some of the solution into the cuvette for the instrument and begin
monitoring the experiment by taking readings periodically on one minute
intervals. If the solution is being tested at a temperature other than
room temperature, it will be necessary to remove the cuvette from the
machine and replace it in the temperature bath being used between
measurements. Make between five and ten readings and then start Trial 2
and repeat for the rest of the trials. You will be required to run the
above experiment at another temperature to obtain necessary information
for the activation energy determination. When all data has been collected
you may proceed with the calculations in the next section.
Calculations: -The spectrophotometer constant (a) is determined by
using the concentration [Brz] for each of the trials in the first step
of the experiment. This value is then divided into the absorbance reading
for that concentration and the three values are then averaged.
Rate measurement and rate law calculations. In each trial determine L h 6
concentration of the bromine[Brz] as a function of time.
[Brz 3 = Absorbance/a
127
k41~lwg#il:lt t h e c u n l z u n t r a t i a n versus time. tiring the S i o p U ; $ram t h i s piiZlt.
and equating it to -rate you can evaluate the order of the reaction with
respect to each of the participating reactants. The following sequence
will allow for calcualtions of each of the species.
rate for trial 1 {Iacetonel}x
rate for trial 3 = { acetone]}^
rate for trial 5 r B r z y
rate for trial 1 = [Br2]Y
rate for trial 1 = rH+lz
rate for trial 4 [H+lz
O n c e the exponents for each participant is determined the value for k
at the temperature of the reaction is found by the following equation;
k = - slope/[Alx[H+l~
Use the concentrations for trial 1 for each temperature determination.

When the values for k at the two temperatures are found, then the log
--k- is--plotted
lAAG
versus 1/T and the slope of the line is equal to -Ea/2.303R.
uLcs:ptable value to use for R is 1.99cal/mole-oK.
Follow the established guidelines for report writing as presented in
the l a b discussion.
Que st ions
1. What is the acceptable value in the literature for Ea?
2. Write out the chemical equations and suggest the mechanisn? for the
reaction.(How does it work?)
rR+ference:Modern Laboratory Programs i n Chemistry by W . Roy Mason
published by Willard Grant Press]
b 128
EQUILIBRIUM-LeCHATELIER'S PRINCIPLE
To study equilibrium and the effects of changes on that
equilibrium. We will look at liquid and solid systems of equilibrium
and the things that influence these systems.
Our studies, to this time, assume the completion of a reaction
when we place the ingrediants in contact with one another. This
assumption is true only in a relatively small number of reactions.
Therefore, the fact that most reactions do not go to completion implies
that we have a system where reactants are mixed with products. When a
reaction system reaches the point where no further reaction is
apparent, we have a state of "dynamic equilibrium". This is a property
of a reversible reaction and at a given temperature can be equated to a
constant value called the equilibrium constant(Keq).
If our system is in equilibrium and we change the concentration of one
of the reactants or products, we should find some evidence of a change
in the system. i.e. 2NO + 0 2 = 2H02 and if we add NO to the system
there should be a shift to the right in the equation indicated by an
intensifying of the brown color of the N O z . This effect was first
proposed by Henri LeChatelier in 1888 and is now called the LeChatelier
- P r i n c i p l e . The principle states that if a system in dynamic equilibrium
is effected by an external stress, the system will shift the equilibrium
in the direction that minimizes the effect of that stress.
Procedure
In this experiment we will look at a series of equili-
brium situations and the effect of a stress(temp, conc., etc.) applied to
the equilibrium. From our observations we will gain understanding crf the
reaction equation and learn to predict the outcome of stresses applied
to other equilibria.
A . To 5 ml of a 0.1M aqueous solution of Cu+2, we will add dropwise
a 1.U1-l NH3 solution. Add NH3 until a defiriite coior change occurs in
f 5 e test tube. Note the results. Write the equ?+,icn of the reaction.
Repeat the experiment with 0.1M Ni+z solution. Note these results and
write the equation.
N u w to the tube containing the copper-ammonia add dropwise 1.0 M
sulfuric acid, shake the tube and observe the results. Write an
equation to explain what you see. Repeat the procedure with the nickel-
ammonia solution but use 1.OM HC1. Again write the equations to explain
the results.
B. To a 5 m l quantity of 0.01M silver nitrate in a test tube add 5 ml
of 0.1M sodium carbonate. Note the reaction. Write an equation to
explain what you see.
Now add 5 ml of 0.1M HC1 and describe what happens. Allow the solution
to settle and carefully pour off all but about 4 to 5 m l of the clear
liquid. To the test tube, add concentrated NH3(use the EOOD) with an
eyedropper until the solution just disscllvqs. Ncw rarefully a d d 6M
HN03. What happens? Write an equation. Add an excess of NH3 dropwise,
what happens?
129
Now add 5 ml of 0 . 1 M KI to the test tube- what happens? Write a

sequence of equations to explain the results.
C. To 5 ml of 0 . 1 M acetic acid add a few drops of universal indicator.
Note the color and then add 0.1 g of solid sodium acetate. When it
dissolves compare the color of the indicator.
Separate the solution into two equal quantities in test tubes and add a
few m l of water to each. Add several drops more of the indicator and add
the same amount of indicator to two other tubes with distilled water.
To one of the first tubes and one of the water tubes add 1.0 ml of 0.1M
NaOH. Note the colors for the specific tubes. To the other t w o tubes,
add 1.0 ml of 0.1M HC1 and again note the colors for the specific
t u b e s . Explain the differences. Look up the definition of the word
buffer.
Follow extablished guidelines for report writing as presented in
lab discussion and include all pertinant equations to exnlain what is
observed in the laboratory experiments.
&a s t i ons
1. Define hydrolysis on the basis of your experience in this
laboratory.
2. Find and write out the Henderson-Hasselbach equation.
[Reference:Laboratory Manual for General Chemistry by Bcran and Brady

published by John Wiley and Sons]
130
SPECTROPHOTOMETRIC DETERMINATION OF AN EQUILIBRIUM CONSTANT

To use the knowledge of the spectrophotometer to study and
to determine the equilibrium constant of a complex-ion reaction.
Many metal ions interact with nonmetallic ions or
molecules to form a relatively stable complex as we found in our study
of Cu+2 + 4NH3 = Cu(NHs)4+2 complex in the previous experiment.
This property is also found with ferric ion (Fe+3) and thiocyanate
ion (SCN-). Both the ferric ion and the thiocyanate ion are colorless,
but the complex forms an intense red-brown color which will allow us to use
the spectrophotometer. The reaction follows:
Fe+3 + SCN- = [Fe(SCN)+21
(colorless) (colorless) (red-brown)
The spectrophotometer will allow us to determine the concentration of
the complex for the given reaction mixtures. With the concentration
v a l u e of the complex, the equation Keq=[Fe(SCN)+21/[Fe+3 ICSCN-1
and the beginning concentration of the ferric ions and thiocyanzte
ions, it is possible to determine each concentration and then
- - c a l c u l a t e the L q value for a variety of the concentration conditions.
For example if we define the starting quantities:
[Fe+3]init = known initial conc Fe+3
[SCN-]init = known initial conc SCN-
[Fe(SCN)+z]final= measured final conc of complex
then
[Fe+3]final = [Fe+a]init - [Fe(SCN)+2]final
[SCN-]final = [SCN-]init - [Fe(SCN)+z]final
and our calculations reduce to
We will make our measurements for a series of five different

concentration mixtures and evaluate each and average the results to
obtain a statistical value representing our work. Since we are
presuming that Keq is a constant, our values should fall within a
set of parameters consistent with experimental error.
To effectively analyze each mixture for the complex ion concentration,
we will determine the absorbance of a set of standards prepared from
our stock solution and use this to prepare a calibration curve. This
can then be used to determine the final concentration of the complex at
any point in our series of measurements.
Procedure
The wavelength we will use for the spectrophotometer
readings is 4 4 7 nm. This wavelength is sensitive to the complex ion
color and will give good response to small changes in concentration.
The stock solutions for the ferric ion must be made in a 0.05M nitric
iicid solvent to keep the ferric ion from any hydrolysis reactions with
water that will interfere with our desired reaction. The concentration
- '- i i r stock ferric ion will be 0.2M and the thiocyanate will be
u .d02M.
I
131
MaLerials Needed:
2 5 ml flasks
I-.
.,urct
pipets
0 . u 5 M nitric acid (HNO3)
0.2M ferric ion stock (Fe(N03 )3 )
0.002M thiocyanate ion stock (KSCN)
spe.2trophotometer
cuvette
Using the following chart, prepare the standard solutions
f o r the calibration curve which will be used for the rest of the
experiment. Proceed to make the standards by measuring the quantites using
a buret and a pipet. The total volume of solution is 25 ml so use an
apprjpriate flask.
Solution 0.00200M KSCN 0.200M Fe(NCh 13

1 5 . 0 ml 5 . 0 ml
2 4.0 ml 5.0 ml
3 3.0 ml 5.0 ml
--- 4
5
2.0 ml
1.0 ml
5.0 ml
5.0 ml
Now set the wavelength on the spectrophotometer as suggested in the
beginning of this section and prepare to measure the absorbance of each
of the solutions. Use the 0.050M nitric acid solution as the blank or
reference and starting with solution # 5 , rinse the cuvette three times
with the solution and then wipe the surface carefully after filling
with the solution and take the reading. Repeat with solution # 4 and
the rest up the line until you finish with #l. Now plot the absorbanc2
for each solution versus concentration of the complex [Fe(SCN)+Z] which
in essence is equal to the concentration of the thiocyanate ion since
we ndve greatly over matched the ferric ion concentration to t i l e
t L : r r ~ : . - ~ ~ . i t Remember
e . these solutions were diluted to 25 ml for t,kAE final
': 1urn5 .
%,'-
Next we will prepare the equilibrium solutions from our stock KSCN and
a diluted Fe(N0313 according to the following chart:
Solution 0.00200M Fe(N0a 13 0.00200M KSCN 0.05M HNO3

1 5.0 ml 1.0 ml 4.0
2 5.0 2.0 3.0
3 5.0 3.0 2.0
4 5.0 4.0 1.0
5 5.0 5.0 0.0
Measure the absorbance of each of these solutions as we did with the

standards and record the values of the concentrations from the working
c3libretion curve. From the discussion section, use the formulas to
determine the concentrations of the Fe+3 i o n and the SCN- ion in each
solution. Then substitute these values in the equilibrium equation and
caliilate the Keq for each solution and average the results.
I
132
Requirements for r e m r t
Follow the guidelines established for report writing and include
a l l graphs and tables as they apply with the proper labels and t i t l e s
Questions
1. If the blank used to set the spectrophotometer parameters was
distilled water would this effect y o u r answer?
2. Why is nitric acid used in the ferric ion solution?
[Reference:Laboratory Manual for General Chemistry by Beran and Frady
p u b l i s h e d by J o h n Wiley and Sons.]
C.
133
DETERMINATION OF TH6 Ksp OF A SLIGHTLY SOLUBLE SALT
We will use the knowledge of equilibrium and solutions to

determine the approximate solubility product of a slightly soluble
salt.
In this experiment we will be comparing the formation of
a precipitate of two unknown ions versus the concentration of these ions
after succesive dilutions. The equation for the equilibrium will be
given, but the material being tested will not be known. We, therefore,
must rely on our knowledge of the equilibrium process for slightly
soluble species in solution. We know, for instance, that when the
product of the concentrations of the ions in solution becomes greater
than a given value, the excess material will precipitate out from the
solution as a solid. If the concentrations of the ions is such that
their product is l e s s than the given value, we will have no precipitate.
Eor example:
Ba+2 + SO4-2 = BaS04( s )
Ksp = [Ba+z][SO4-2] = 1 X 10-10
C. -
It tne concentration of the barium ion is one millionth of a mole per
liter and the sulfate ion is the same their product is 1 X 1 0 - 1 2 which
is below the ion product for the Ksp and there will be no precipitate
formed. If the concentrations of the ions is l O - 4 M then their product
is 1 0 - 8 and this is greater than the Ksp and the excess will form a
solid.
In this experiment we will use a method of serial dilutions to estimate
the order of magnitude of the equilibrium constant for the unknown
species. By using careful dilution and then combining the solutions and
viewing any evidence of a precipitate, we should be able to estimate
raLrry accurately to the power of ten for the equilibrium constant. A
it.:Jle dettl:;d s t i i d y woKld allow for the deterininaticn of the mcltislier
associated with the power of Ksp value, but for our purposes this
zpgroach will suffice.
Procedure
This experiment will attempt to calculate an approximate value
for the Ksp of an unknown salt generically called MA. You will,
therefore, be given 'a solution that contains 0.200M M(NO3)z and 0.20OM
K z A . Also, another trial of a different ratio of anion to cation will
be determined and it is called XY2 where starting solutions are 0.200M
X(NO3 ) 2 plus 0.200M KYz.
a. The procedure for the determination of the Ksp for MA begins with
the procurement of 10 to 20 ml of M(N03)z and 10 to 20 ml of KzA.
In a clean, dry test tube careful-ly place 10 drops of the M solution
and 10 drops of the A solution, stir vigorously and wait. If a
precipitate forms within 20 minutes proceed to the next step.
134
b. Place 30 drops of the solution M and 30 drops of water into a
different clean dry test tube. In another clean dry test tube place 30
drops of A solution and 30 drops of water and calculate the
concentrations of these solutions. Now place 10 drops of the new M
solution in a clean, dry test tube and add 10 drops of the new A
solution. Mix thoroughly - does a precipitate form? Continue the
experiment by placing 30 drops of the new M solution in a new clean,
dry test tube and add 30 drops of water and repeat this with the A
solution. Again calculate the concentrations of M and A. Again add 10
drops of the newest M solution to 10 drops of the newest A solution. If
a precipitate forms continue the precedure until no more precipitate
is noted. Calculate the Ksp by multiplying the concentration calculated
for the M solution times the concentration for the A solution.
c. The procedure for the XYZ unknown is the same, but the
X ( N 0 3 ) 2 and the KY solutions are used. The calculations proceed by
multiplying the concentration of the X solution times the square of the
ccncentration of the Y solution.
Follow the established guidelines for report writing.
-- "
w u~ 5 t i ons
1. From your data and the knowledge that the generic formula is MA can
you determine a set of possible compounds that might fit your data?
2. What effect would a high concentration of one ion of the pairs have
on the precipitate formed?
[Reference: Experiments in General Chemistry by Whitten and Gailey
published by Saunders College Publishing.]
135
tJETEROGENEOUS EQUILIBRIUM
DETERMINATION OF TJB Ksp OF A SLIGHTLY SOLUBLE SILVER SALT
The principle of equilibrium is used to determine the Ksp a
slightly soluble silver salt.
The basis for gravimetric quantities analysis rests in the
equilibrium between solid ionic materials and solutions of their ions.
In general, this is a simple concept where the solution is
saturated with the counter ion to force precipitation of the desired
ion and then the product is washed, filtered and dried for weighing.
Our experiment could follow this method and we probably would obtain
satisfactory results, but by careful selection of our ions we can use
alternate methods.
In this experiment we will use silver ion and oxalate ion and
experimently determine determine the Ksp by mixing varying
concentrations of each solution, allowing equilibrium to be
established, then titrating the excess amount of one of the reactants.
Since the starting concentrations are known it easy to relate the final
concentrations of the ions and using the equation for the salt
qa.lculate the Ksp. i.e.
AgzC204 = 2Ag+ + c204-2
KSP = [Ag+]2[Cz04-2] = #
We will determine the oxalate ion concentration at equilibrium by
titrating it against potassium permanganate in acid solution. The
equat i on ;
2KMn04 + 5 K z C z O 4 + 8 H z S O 4 = 2MnS04 + l O C 0 2
8 H z O + 6K2SO4
The presence of the oxalate ion is determined by the permanganate
titration and, also, the concentration of the silver ion, since it will
be a stoichimetric relationship with the oxalate ion in solution.
Procedure
Prepare 200 ml of 0.250 M A g N 0 3 and 200 ml of 0.250M
NazCzO4 solutions by accurately weighing reagent grade
chemicals and dissolving them volumetrically using a 200 ml volumetric
flask.
Next obtain three 1 2 5 ml Erlenmeyer flasks that have been cleaned
and dried. Number them in order and to flask number one, add by pipet
50 ml of 0.250M A g N 0 3 and 2 5 ml of 0.250M NaaC204 to the flask and
stopper it. To flask number 2 add 7 5 ml of the silver nitrate solution
and 2 5 ml of the oxalate solution, stopper and set aside. To the last
flask add 50 ml of the silver nitrate and 50 ml of the sodium oxalate
and stopper and set aside.
Allow the flasks to sit for 30 minutes, but periodically shake
them to prevent supersaturation from occuring.
Next prepare and standaridize 250 ml of 0.1000 M mnO4 with
primary standard grade sodium oxalate.
136
When the flasks have set for thirty minutes, then filter the flask
contents through a dry retentive fliter paper and a dry funnel into a
dry beaker. Then transfer by pipet 50 ml of the filtrate(fi1tered
liquid) into a clean dry 250 ml Erlenmeyer flask. To the flask add 3 ml
of concentrated H2SO4 and heat the flask gently to 800C. Titrate
carefully with the permanganate until a persistent pink color remains
for thirty seconds. If the titration takes to long a time you may have
to reheat the solution.
Repeat the procedure for each of the flasks and record all the
titration volumes.
Now using the equation:
2Mn04- + 5 C Z O 4 - 2 + 16H+ = Mn+2 + lOCO2 + 8H2O
we can calculate the amount of oxalate not precipitated as the salt.
From this calculation and the fact that silver ion must react in two to
one ratio calcualte the amount silver ion left in solution. N o w using
the equation for Ksp and the concentrations determined calculate the
Ksp for each trial.

-- Follow the established guidelines for report writing and include
your data for the standardization of the permanganate solution.
Questions
1. Would the reaction be effected with a cold solution? Write the
equation.
2. Could you suggest a different method to analyze this experiment to
get the needed results?
[Reference: Experiments in General Chemistry by Drago and Brown
published by Allyn and Bacon, Inc. pg 153-581
137
HYDROLYSIS
, We will use the knowledge of equilibrium and an understanding of

pH to determine the interactions of ionic substances and water.
When a strong acid (or base) is placed in water the
result is a definite acidic (basic) solution. The total ionization of
this acid (or base) increases the hydrogen ion concentration (or
decreaes) well above the normal or neutral level of water. This
phenomenon is expected when dealing with strongly ionized acids and
bases.
When the salts of strong acids and bases are dissolved in water there
is no apparent effect on the concentration of the hydrogen ion
concentration.
On the other hand when a weak acid (or base) is dissolved in water
t I l e r e is an increase in the concentration of the hydrogen ion or(0H-)
but rlot to the extent of the strong acid or base. When a salt of the
weak acid (or base) is placed in water the effect is to balance the
equilibrium equation, i.e.;
C. ~
HA + HzO = H30+ + A-
A- + H z O = OH- HA +
where the anion reacts with water to generate the undissociated acid
(or base).
The experiment will acquaint the student with the effect of variuos
ionic: salts on the hydrogen or hydroxide ion concentrations with
respect to their interaction with water.
Procedure
In this experiment the use of the pH meter will be
rlecessary
-
to evaluate the hydrogen ion concentration of the solutions.
ine instructor will provide detailed precedures in tila use arid ~ ‘ a ‘11
~ e
t L I - F‘! Toter and the associated electrodes.
Frepare 0.1 M concentrations of the following salts:
NaCl
NaCz H3 Oz
NaHCO3
NaHSOs
NaHz PO4
NH4 C1
( NH4 ) 2 SO4
NH4 Cz H3 0 2
When sufficient solution is prepared for each of the students to obtain
about 100 ml of each one then proceed to test each solution according
to the directions outlined by your instructor. Record the pH reading of
each Yoltltion and what ions it contained. For each determination write
an equation that explains the observation that was made.
1
138

Follow the established guidelines for report writing and include
the equation for each of the hydrolysis reactions.
Quest ions
1. What would you expect when a salt such as NazHPO4 is placed in
water? Write the equation.
2. How is t h e concept of hydrolysis used in chemistry?
[Reference: Laboratory Manual for General Chemistry b y Beran and Brady
published by ; o h Wiley & Sons]
139
DISSOCIATION CONSTANTS
We will use the knowledge of equilibrium and pH to determine the

dissociation constants of a weakly dissociating acidic or basic
campound.
Usually an equilibrium reaction takes a little time to
establish the equilibrium when the participants are joined together. In
the case of the weak acid or base with water the equilibrium is in
place almost immediately. Therefore their study is used in this
experiment.
The equation for the reversible reaction can be represented in a
generic sense by the following; HA = H+ + A - , where the
corresponding equilibrium equation becomes;
Ka = [H+][A-l/[HAl
and the equilibrium constant Ka (called dissociation constant) is the
constant for that acid. If we used acetic acid as our representative
acid the value would be about 1.8 X 10-5 when the concentrations are in
moles per liter and the temperature is 25oC.
-A The expression can be written for a weak base much the same way and the
C o I l c i u s i o n s amount to much the same except we are working with a base
instead of an acid.
If we are aware of the K value for our particular reaction we can
determine the concentration of the various species with relative ease,
but if the acid is unknown it becomes a little more difficult to
determine the concentrations af the various species unless we take
advantage of the fact that the equilibrium equation is totally
reversible and we can then evaluate the information obtained in our
titration data to determine the K value.
There are two methods that allow for the calculation of the K value fclr
our uniLrLownmaterial. The first method is based on the fact that when
...-
- 1?1szc thc acid or base in solution the concentratian of the hydrzgen
j o n or the hydroxide ion and the corresponding counter ion will have
th? same value, If we know the total concentration of the acid or base
then at any given pQint in the equilibrium [HA] = F - [H+], where F is
the formal concentration of the acid, and [H+] = [A-I
Using the above information we can substitute into the equilibrium
equation a s follows:
Ka = [H+]2/ F - [H+]
From this arrangement we can calculate Ka. The error of this technique
is potentially high due to the fact that the value used to determine
[H+] is then squared and divided by a difference using the value of
[H+]. The second method reduces the potentially large error because the
measurements are not magnified so extremely. In this technique the
reaction of the acid with the base produces the following;
HA + OH- = A- + HzO
and we see there is a quantity of anion produced in relation to the
undissociated acid. When one fourth of the original HA has been
titrated then one fourth of the anion has been generated. Then using
the equation;
Ka = CH+l{CA-I/[HAl)
the values for Ka can be calculated at various ratios of anion to
undissociated acid and the values can be averaged.
I
140
Requirements f o r report
Follow the established guidelines for report writing and show a
calculation set up for each result.
Questions
1. Calculate the result using both methods decribed in the discussion.
Is there any difference?
2. What would you do to improve the results?
[Reference:Laboratory Studies and Problems in General Chemistry by
Stone and McCullough published by McGraw-Hill, Inc.]
14 1
DETERMINATION OF pKa OF AN ORGANIC ACID

We will utilize the knowledge of the pH plot and the equation of
the equilibrium constant to determine the pKa of an unknown weak
organic acid.
Most organic acids are less soluble in water solution as
a result of the intramolecular hydrogen bonding of the carboxyl group
on the molecule. This leads to a lowering of the ionization of the
molecule and thus a lower solubility. The equilibrium constant (Ka) is
a function of the strength of the acid. If the organic acid has an
attached group that reduces the ability of the hydrogen ion to separate
from the molecule the acid is said to be weak. If the group attached to
the carboxyl group is an electro-negative group such as a nitrogen
containing group then we may see a strengthening of the acid and it may
become closer to the ionizing capability of a mineral acid such as
phosphoric acid.
By using a slightly less polar solvent such as alcohol and water
con-ihination we can more easily dissolve an organic acid such as benzoic
acid and then study the dissociation constant of these acid types.
If we titrate the acid with a known concentration of a weak base and
carefully plot the pH versus volume relationship it is possible tc,
estimate the pKa of the unknown acid. At the point on the graph where
one half of the acid has been neutralized the ratio of undissociated
acid to anion concentration is 1 : l . At this point the pH then is equal
to the pKa. (See the Henderson-Hasselbach equation).
Procedure
Weigh out an approximate 0 . 0 2 g quantity of the assigned acid
and dissolve them with 25 ml of denatured (reagent) alcohol in a 100 to
150 ml beaker and then add 25 ml of distilled water.
Prepare to titrate with a 0.10 N NaOH solution using a pH meter and a
stirring apparatus. Be sure to insulate the beaker from the heat of the
ztirring motor or use a A T C ( A u t o T e m p C o m p e m s a t o r ) attachment with the
meter.
Add your titrant slowly inb 1.0 ml increments recording both volume and
pH readings. Reduce the increment size when you approach the endpoint.
continue the titration well beyond the endpoint to get a good plot.
Plot your pH versus volume data and determine graphically the
equivalence point and the pKa at the point where the volume is equal to
1 / 2 oh the neutralization volume.

Follow the establishied guidelines for report writing and include
your graph of the titration properly titled and labeled.
Questions
1. Would it be more advantageous to use higher weights and
concentrations to do this lab? Why?
2 . Would it be necessary to Know the molarity of the base?
[Reference: Experimental Methods in Organic Chemistry by Moore,

Palrymple, and Rodig published by Saunders College Publishing pg 1 8 9 -
911
142
BUFFERS
The use of the knowledga of hydrolysis and acid-base
equilibria can be used to study the properties of buffer solutions.
When a weak acid or base is placed in water there is dissociation of
the acid or base to a small degree and the properties used to define an
acid or base are present in the solution.
A l s o , when the soluble salt of one of those weak acids or bases is
placed in water the dissociation is basically complete and the conjugate
species interacts with water to exhibit the opposite properties of the
weak acid or base and as such could be analyzed as the opposite species.
When a weak acid and its salt are present in the solution a situation
exists a s if the solution were in equilibrium at a set state of conditions
and neither additional acid or base added can greatly effect this stable
state. This situaltion is described as a buffer solution.
There ios e n o u g h of the undissociated acid molecules present to
neutralize a finite quantity of base when added. Also, there is enough of
the dissociated conjugate base(anion) present to react with any acid that
maybe added. The overall equilibrium remains status quo.
Depending on the particular species there are a large variety of pH
buffers that can utilized.
Henderson-Hasselbach equation allowsfor the calcualtion of a variety
of possible buffer solutions and the determination of the ratio of the
buffering species in solution.
pH = pKa + log [A-]/[HA] for a weak acid
pH = pKb + log [B-]/[BOH] for a weak base
Bilffers are generallly obtained commercially but in some instances it
is advantageous to know how they might be prepared. Our experiment is to
generate a few buffers.
Procedure
( 1 ) The first step is to prepare a buffer that is easily
done arid test the solutions.
Prepare a 100 ml solution of 0.10 M N a C z H 3 0 2 and 100 ml of 0.10 M
HCz H3 0 2 .
Place 20 ml of each in a 100 ml beaker and test the pH of the solution
with a pH meter. It should read 4 . 7 - 8 according to the Henderson-
Hasselbach equation. If it does not check the calibration of the pH meter.
Next add to the solution 5 m l of 0.05 M HC1 and recheck the pH meter.
Does it remain the same?
N o w add 0.5 M HC1 carefully recording the volume added until there is
a one unit change in the pH meter reading( i.e. 4 . 7 -3.7.) How many ml’s
does it take?
Again place 20 ml of each of the starting solutions in a 100 ml beaker
and repeat the above procedure but using 0.05M NaOH and 0 . 5 M NaOH.
reiterate the questions and determine the answers.
143
(2) Now using the Chemical Rubber Company Handbook prepare and test a
buffer that will give you a pH of 7 and not change with the addition of
acid or base over a range of 5 ml of 0.02M concentration.
Follow the established guidelines f o r report writing and submit your
prepared buffer to the instructor for test.
Questions
1. What is meant by the capacity of a buffer?
2. Choose another buffer system then the one you prepared and calculate
the ratio of the salt to acid or base needed.
144
ELECTROCmMISTRY
VOLTAIC CELL - "ST EQUATION
We will utilize the knowledge of a spontaneoous oxidtion-
reduction reaction and the electromotive series to study the voltaic
electrochemical cell.
When an oxidizing agent is placed in the presence of a
reducing agent there is a reaction and the electrons are transferred
from the reducing agent to the oxidizing agent. If the reaction species
are separated by a semipermeable membrane then the electrons must pass
from the reducing agent through an outside conductor to the oxidizing
agent for the reaction to proceed. This is accomplished by connecting a
wire(conductor) from the electrode in contact with the reducing agent
to the electrode in contact with the oxidizer. The electrolytes in the
solution will act as elctron carriers within the cell to complete the
ccircuit and allow the reaction to take place.
The reducing agent, generally in the form of a metal strip, is defined
as the anode for a spontaneous reaction and is the negative terminal of
the voltaic cell. The oxidizing agent,(may be ions in solution with an
inert electrode), is the cathode and is positive. The two electrodes
'are is contact with a solution of their ions, or other electrolytes,
but are separated form one another by means of a porous cup, salt
bridge, or gravity dddue to density of the two solutions.
When an electrode pair is set up with an external conductor there will
be a current generated and a voltage. The voltage may be determined by
cornparin-g the location of the electrode pair onb the Electromotive
Force Table, or a table of Standard Reduction Potentials. For example,
zinc is located below hydrogen on the Standard Reduction Potential(SRP)
table and has a value of -0.763 Volts as an oxidizing agent, or its
ability to be reduced. While copper has a SRP value of + 0 . 3 3 7 Volts. If
we place Cu(I1) i o n in the presence of zinc metal the copper will be
displaced in solution by the zinc. The potential voltage of the cougie
would be +0.337V - (-0.763V) = 1 . 1 O O V . This reaction woald taka p1a.z.s
a5 a spontaneous reaction as shown in the equation GO = -nFEo, since
EO is positive, GO would be negative and by definition this denctes a
spontaneous reaction.
The reaction equation is as follows:
where the zinc is oxidized and the copper is reduced.

Now with G = - RTln Kc, then EO = RT/nF(lnkc) and if l o g l o is
used then EO = 0.059l/n(log kc), or the potential of the cell is a
function of the concentration of the ionic species in solution and the
E c e l l is equal to EO - 0.0591/n (log Q), where Q equates to the
mass-action quotient. If our cell has a change in concentration from the
values expressed in the SRP tables this equation allows for calculation
of the change in potential.
I
145
Procedure
In this experiment we will compare a series metal-metal ion
redox couples and determine the cell potentials and compare them to the
literature values from various sources.
The metal-metal ion couples we will consider are; Zn-ZnSO4(1M), Mg-
MgSO4(1M), Cu-CuS04(1M), Ni-NiS04(1M) and Sn-SnClz(1M).
The cells will be arranged by placing in a 250 ml beaker, the first of
the metal-metal ion and then in a porous cup place the second of the
metal-metal ion pairs. Before starting any of the reactions be sure the
surface of the electrodes(meta1 strip) is polished clean.
To the first metal strip(e1ectrode) attach an alligator clip and a high
resistance and to the second terminal of the resistance connect another
conductor which will be connected to the second electrode. Across the
two terminals of the resistance connect a voltmeter (watch your
terminals). Now connect the second electrode with the alligator clip
and quickly read the voltage and record this value.
Remove the porous cup and disconnect the leads. Wash the cup with
A 1
C.”.
-
distilled water and place the next metal-metal ion pair to be tested in
- - .- -.r?connect as before but check to see if the terminals of the
voltmeter are in the right places. Each cell is different.
Repeat the procedure until each of the ion pairs has been tested with
all the other pairs and you have values for all.
Now arrange the metal-metal ion pairs in order of potentials determined
in the experiment.
Nernst equation: Now take the ZnSO4 solution and reduce it to a U . O l M
concentration by dilution of 1 ml to 100 ml. Set up the Zn-ZnS04(0.01M)
cell along with the Cu-CuSO4(1M) half cell and determine the voltage.
Use the equation from the discussion to calculate the anticipated
v a i i i e - are they the same? If not, why not?

Fallcx the established guidelines for report writing and include a
drawing of your cell arrangement.
Quest ions
1. If the zinc electrode was used as the reference value on the SRI?
table, what would your voltage determinations be?
2. Why is it necessary to isolate the two solutions?
[Reference: Fundementals of Chemistry by Brady and Holum, John Wiley
publisher]
14 6
ELECTROLYTIC CELL
DETERMINATION OF AVOGADRO’S NUMBER
We will use the knowledge of an electolytic cell and the Laws of

Faraday to verify Avogadro’s Number.
The electroyltic cell is nonspontaneous and the redox reactions
performed in this cell must be forced by an external source (i.e. a
battery or power supply.) This type of a cell has is uses such as
electroplating or refining of metals like aluminum, ets. They, also,
a r e useful in studying the various phenomnon of oxidation-reduction
reactioris or analyzing theory that has been studied in various
scientific presentations.
We will apply the properties of this ccell to a study of Avogadro’s
Number. Avogadro suggested the value 6.022045 X 1 0 2 3 particles in his
study of the properties of gases although the actual number was
determined a w h i l e later.
By using the electrolytic cell we will experimentally determine the
value called Avogadro’s Number by depositing a measureable quantity of
--
an element such as silver or copper onto a preweighed electrode and
using the electrochemical law (Faraday’s)that the amount of mass of
an element deposited by an electrical source is directly proportional
to the amount of electricity used. The electrical quantity Q in
coulombs is equal to the amperes (I) times time (t) in seconds.
The electrical charge carried by an electron is 1.6 X 10-19 coulomb
as measured by a scientist named Millikan. Therefore;
Q X 1 electron/l.6 x 10-19 coulomb = # electrons
and by knowing the number of electrons needed to deposit the mass of
the element we worked with, we can determine the number that would
equate to the number of atoms in one gram-atomic weight(mo1e) of that
e l 2 = a : e n t . This should equal Avogadro’s Number.
__-__-
Procedure
.
Prepare 200 ml of 0.5 M CuSO4 in a 250 ml beaker. To the

heaker suspend 2 polished and preweighed copper strips to be used as
electrodes. To the copper strips attach two leads with alligator clips.
Using a D.C. power supply, a milliammeter, a 90 ohm rheostat connect
the leads and complete the circuit. Adjust the amperage to about 50
milliamps by varying the voltage or the resistance and allow the
current to flow about one hour. Monitor the flow rate of electrons
periodically(every 10 minutes) and record the value.
At the end of the time disconnect the leads and carefully remove the
anode(+) and the cathode(-) from the cell. Rinse them carefully withe
distilled water and then with a little acetone to dry. Weigh each of
them separately and record the weight gain and loss for each.
Determine the average mass transferred and use this value to calculate
the value for Avogadro’s Number.
Compute the value for Q (multiply I X t(sec)) then diviae Q by the
charge per electron (1.6 X 1 0 - 1 9 ) to get the number of electrons.
Now arrange a proportion to determine the number of electrons
transferred per gram-atomic weight. Then determine the number of
electrons transferred on the basis of an equivalent weight.
I
147
F o l l o w the established guidelines for report writing.
Questions
1’. What is the precision of this experiment? Why?
2. State Avogadro’s theory.
3. How does your experimental value compare to Avogadro’s?
4 . What is the % error?
5. What caused the difference?
[Reference: Laboratory Experiments for Foundations of Chemistry by Toon
and Ellis, published by Holt, Rinehart and Winston, pg 1611
148
ELECTROLYTIC CELL
COULOMETRIC PRODUCTION OF CUPRIC ION
We will use the knowledge of Faraday’s laws to study the
electrolytic cell and to compare techniques in measurement of various
quantitatively produced elements.
Faraday stated two truths as follows:
( a ) the weight of an element generated at an electrode is directly
proportional to the quantity of electrons transferred through the cell,
(b) that the weights of different elements that are produced by
equivalent amounts of electron are proportional to their respective
equivalent weights.
In studying the above statements it becomes clear that electrons relate
to quantitative measurements as do mass quantities or volume or gases.
With understanding and the fact tthat amperes times time in seconds
equals coulombs, which when divided by the value 96,500 equals
equivalents we can study the various parts of an electrolytic
cell(nonspontaneous).
In this experiment we will arrange a copper anode(+) and a Chromel
cathode(-) in an electrolyte solution such as dilute H 2 S O 4 . With the
~ t of e an inverted buret or a eudiometer tube we can collect the
C.
hydrogen gas evolved at the cathode. During the reaction there will be
copper (11) ions evolved at the anode and a measure of the time and
amperage will give us a record of the coulombs of electricity utilized
in the cell to compare with the amount of each of the other two species
produced.
The reactions for each of the electrodes is as follows:
Cu(e) = Cu+2(aq) + 2e-
2H+(aq) + 2e- = H2c tz)
Using the simple loss of weight at the anode as a measure of the
copper(I1) put into solution and the time in seconds times the average
amperage we have two measurements of the equivalents utilized. When we
finally compare these to the equivalents of hydrogen at the cathode
there should be good agreement in the results.
In addition, if desired, an iodometric determination of the copper ion
in the sulfuric acid solution may be carried out as a fourth
measurement technique.
Prepare a solution of 0.25M H 2 S O 4 sufficient

to fill a 50 ml buret and have about 75 ml in a 150
ml beaker. Next clean a piece of #12 copper wire, of
which the last 6 inches of a 12 inch piece have been
twisted around a pencil and bent at right angles to
the straight stem, using 50 ml of warmed 0.5 M nitric
acid solution. Rinse the wire with distilled water and
then a little acetone to dry it. Weigh the wire to thc
nearest 0.1 mg and attach it as the anode. Next a piece
of 12 inch Chromel is prepared as the copper wire but
the bend is in a U-shape and the wire not inside the
inverted buret must be sealed form the solution using
..., either glass tubing and an epoxy sealant or shrink
A*-44. insulation used for electrical junctions.
cr-
-
149
With the electrodes prepared place them in the beaker with enough of
the H2S04 solution to fill the buret. Invert the buret and insert the
Chromel electrode into the open end of the buret and with a suction
b u l b draw the solution into the buret above the last calibration mark.
Seal the buret with the stopcock and watch for any leakage. If there is
none lower the meniscus to the calibration mark(50 m l or 2 5 ml for what
ever size buret used.) Add the rest of the liquid and prepare thm
circuit for the reaction.
A 6-12 volt D.C. source is needed or a higher voltage source with a
sufficient resistance in the circuit can be used. A milliammeter is
also necessary in the circuit. Connect the positive terminal of the
power supply to the copper wire and the negative lead to the Chromel
wire. Begin timing the reaction as soon as the leads are connected and
a current is flowing. A current of 30 to 50 milliamperes is suggested
to give enough data to evaluate the consistency of the current. Take
readings of the amperage and the hydrogen gas production on a periodic
basis and record these values. At the end of the experiment average the
the ampere readings and the hydrogen gas production and this will
verify the consistency. Continue the experiment until 2 5 to 40 ml of
the hydrogen has been collected and then disconnect the leads.
Remove the copper wire, rinse with a little distilled water and then
c\ iAttle acetone to dry it and weigh it.Do not place it i n a
C.
n A r l A
drying oven. Why? Record the volume of hydrogen and measure the liquid
volune in ml in the buret that is above the liquid level in the beaker.
iiecord this value.
Repeat the experiment once more and collect the data in the same
manner .
Now compute the number of equivalents of copper generated by dividing
the weight loss on the electrode by the weght per equivalent according
t o the equation inthe discussion section. Next compute the number cf
equivalents of electrons by multiplying the average amperage by the
. . - : x k - r 2f sFconds the reaction was run and dividing by the factcr
QP '11, -niJl@mhs/equivalent. Finally, compute the number of equvalents
I
of hydrogen generated using the ideal gas law and the laboratory
temperature and pressure and the change in the pressure due to the
suspended column of liquid remaining in the buret. The volume in ml
measured times the density of the liquid (about 1.014g/ml) and then
divided by the density of mercury (13.6g/ml) will give the amount of
pressure drop in the buret. This is then subtracted from the pressure
reading plus the vapor pressure due to water at the lab temperature to
obtain the proper values to substitute into the gas law equation.
Compare the values obtained for each determination and compute the
percent relative error in the methods.
&wirenents for report
Follow the established guidelines for report writing including
tables for your data.
Questiong
1. Which one deviates the most? Can you'explain why?
2 . Nhat would improve the method?
[Reference: Laboratory Studies and Problem in General Chemistry by

StorLe and McCullough published by McGraw-Hill]
150
ISOLATION OF CAFFEINE FROM A SOFT DRINK
The purpose of this experiment is to extract or isolate

caffeine from Pop. Although pop is mainly a solution of flavored
sugar in water there are other interferring materials. Some soft
drinks contain ingrediants such as caffeine to enhance the flavor
of the drink. Some of the impurities are the flavoring agents which
may include some complicated organic structures and preservatives
such as potassium benzoate.
The other water soluble products are eliminated when the
caffeine is extracted with the organic solvent such as dichloro-
methane.
Procedure
In a 250ml Erlenmeyer flask place 100.0ml of pop then
attach a hose to an aspirator and evacuate until the solution
ceases to evolve carbon dioxide bubbles. At this time add 2.ug of
-- calcium carbonate and warm gently. Filter using a qualitative
filter paper, filter the solutionby gravity into a 125ml Erlenmeyer
flask. Rinse the residue left in the flask with two 10 ml washings
of hcjt water and add to the filtered material. Discard the residue
after extracting the remaining liquid by carefully pressing the
residue and filter paper.
Cool to room temperature and extract with 4.0ml of dichloromethane.
Be careful to avoid an emulsion by to vigorous agitation of the
solution.
Allow the layers to separate and withdraw the bottom layer
with a Pasteur pipet and transfer to a small filtering flask
by means of a funnel with a small layer of anhydrous sodium
sulfate.(about 2.0g) Repeat the extraction procedure with four
additional 2.0ml portions of dichloromethane and add these to the
filtering flask.
The organic solvent is now evaporated to dryness using a steam
bath or sand bath in the HOOD.
The product is now ready for purification and characterization
which requires sublimation of the crude caffeine.
Using an aspirator, a filtering flask and a cold finger the
sublimation canbe accomplished. First clamp the flask on a ring
stand and connect to the aspirator. Next seal the cold finger in
the flask about 1/2cm above the crude caffeine. Then with a micro-
burner begin the heating process. Be sure not cause the crude
caffeine to begin melting for it will then decompose. Continue this
process until the sublimation is complete, no more caffeine forms
on the cold finger. Remove the heat and allow the system to cool to
room temperature under reduced pressure.
When the cooling is completed carefully remove the vacuum and
the cold water connections. Then remove the cold finger from the
flask and scrape the crystals of caffeine onto a weighing paper or
other preweighed collecting container. A melting point and an IR
spectrum should be included with this experiment.
151
Reqirements for r e p o r t
Follow the established guidelines for report writing and
include the satructural formula of caffeine and its properties.
Questions
1. What.is the term alkaloid defined as?
2 . What is the LDora1 for a rat?
[Reference: Microscale Organic Laboratory b y Mayo, Pike and Butcher

published by John Wiley & S o n s ]
152
PREPARATION OF ASPIRIN
Aspirin has been used for years as a fever reducer, anti-
inflamation drug, and pain reliever. Its effect on the body is still
not fully understood, but its chemistry is not to difficult.
The molecule is actually an ester of salicylic acid and the acetate
ion. Most esters are the condensation of an organic acid and an
alcohol, but aspirin is actually the condensation of anorganic acid and
an organic acid.
This is actually not the case, since salicylic acid is composed of
an acid molecule with a hydroxy group also attached.
CsH5(0H)(COOH) + H3C202H = CsHs(H3C20z)(COOH) + H2O
The reaction equation decribed above is an abreviated form of the
reaction. The complete reaction must also include a catalyst to enhance
the reaction kinetics. If hydrogen ion is used it will help to
facilitate t h e speed of the reaction and push it towards completion.
Erocedure
In a 18 X 150 mm test tube place 1 g of pure salcylic acid and
a b o u t two ml of acetic anhydride. To this add two drops of concentrated
sulfuric acid and heat the tube gently in a hot water bath to about 8 5 -
9 0 0 C . Heat for ahout five minutes and then remove the tube from the
heating bath and add two ml of distilled water to decompose the
anhydride.
The material is then crystallized by adding an additional 10 ml of
water and chill thoroughly in an ice bath.
Collect the crude product by vacuum filtration and draw air thru
t h e product until it is dry.
Tc purify the crystals, dissolve them in 10 m l of ether (ether is
extremely flammable and must be handled carefully) and theii add d r i
c-qx--l c\zQur,t of petroleum ether(bp 30-600) and then cool in an ice
Lac:-. Again collect by vacuum filtration and determine the melting
point of the dry crystal.
Requirement for report
Follow the established guidelines for report writing and include
your melting point data and yield amounts.
Qu es tion s
1. How is the commercial aspirin prepared?
2 . Are there any other salicylic acid derivatives used in medicine?
[Reference: Laboratory experiments in Organic Chemistry by Adams and

Johnson published by Macmillan Company]

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I NORGC?

WILS BEHGSTHOM, M.S.

MCIRLYS HOWELLS, Ph.D.

St. Paul Technical Institute

235 Marshall Avenue

St. Paul, MN 55102

Produced by Independent School District # 625 with the Minnesota

In 1966, with the help of local industry, the Chemical Technology

Heterogeneous Equilibrium -Determination of the Ksp of a

LABORATORY SAFETY PRACTICES

The laboratory is a safe working place when precautions and

14. When inserting glass tubing or thermometers into rubber stoppers,

GOOD LABORATORY WORK HABITS

7. Do not place reagent-bottle stoppers and/or caps on the benchtop;

DOUBLE BLAM SPATULA

SCOOP SrYLE SPATULA

*Only on Modrls H20 and H1E.

t A l l &Is except HE.

1. lkton mighing, k w n thrt:

111. Waighing tlw mmpk:

IV. Comploting tha woighing

BASIC LABORATORY TECHNIQUES

For each experiment items 1 - 6 in the format outline should

145 l b X 1 ker = 6 5 . 7 5 9 6 kg = 65.8 kg

in the denominator of the conversion factor for lb units to cancel.

10 gal X 4.0 ats X 1 liter X 1000 ml = 3 7 , 8 4 2 ml

The following problems are required to be completed

Remember to round off answers to the appropriate number of

It is recommended that the student weigh these items on the triple

supplied, methane burns with a blue, nonluminous flame producing

to the barrel. Refer to CTRRH for illustration of burner diagram.

Answer all the questions listed at the end of each experiment.

All pure substances have characteristic properties which can be

1. If you had an irregularly shaped solid, how could you determine

STUDY ASSIGNMENT FOR SYMBOLS, FORMULAS, AND EQUATIONS

The chemist communicates in a technical language that is

carbon and oxygen to produce carbon dioxide simplifies to

However, the equation now shows 2 potassium atoms on the right;

The equation is now mass balanced or obeys the Law of Conservation

2. The instructor will make available to you approximately 50

PHYSICAL SEPARATION OF MIXTURES

Matter can be classified into one of two general categories,

The solid is allowed to settle and liquid is then decanted. Several

Requirements for Report

Physical methods used for identification depend upon the

Paper chromatography is the simplest and most efficient

1. Distinguish between absorption and adsorption.

Fossil fuels represent a large portion of the world’s energy

C. Ash and Fixed Carbon

PERCENTAGE OF WATER IN A HYDRATE

Many pure substances combine with water in a fixed mole ratio to

The purpose of this experiment is to determine the percentage of

Calculate the actual percentage of water in the zinc sulfate

EMPIRICAL FORMULA OF A COMPOUND

PERCENTAGE OF POTASSIUM CHLORATE IN A MIXTURE

Chemical reactions provide information regarding the

CAUTION: Great care must be taken to avoid introduction of any

Requirements for Report

In order to communicate with chemists internationally, some