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The Art of Teaching Speaking Research and Pedagogy
for the ESL EFL Classroom Keith S. Folse Digital Instant
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Author(s): Keith S. Folse
ISBN(s): 9780472031658, 0472031651
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Language: english
Chemical Principles
in the Laboratory
Eighth Edition

Emil J. Slowinski
Professor of Chemistry
Macalester College
St. Paul, Minnesota

Wayne C. Wolsey
Professor of Chemistry
Macalester College
St. Paul, Minnesota

William L. Masterton
Professor of Chemistry
University of Connecticut
Storrs, Connecticut

Australia • Canada • Mexico • Singapore • Spain

United Kingdom • United States
Preface

A Few Words to the Students

n spite of its many successful theories, chemistry remains, and probably always will remain, an experimen-
I tal science. As the world of the computer has developed, there are those who feel that one can learn chem-
istry by working with software and observing reactions on the computer screen rather than in the laboratory.
We do not agree with this approach. We believe that there is really no substitute for hands-on laboratory expe-
rience if one is to learn what chemistry is all about.
It is not easy to do good experimental work. It requires experience, thought, and care. As beginning stu-
dents, you have not had much opportunity to do experiments. We feel that the effort you put into your labo-
ratory sessions can pay off in many ways. You can gain a better understanding of how the chemical world
works, manual dexterity in manipulating apparatus, an ability to apply mathematics to chemical systems, and,
perhaps most importantly, a way of thinking that allows you to better analyze many problems in and out of
science. Who knows, perhaps you will find you enjoy doing chemistry and go on to a career as a chemist, as
many of our students have.
In writing this manual, we attempted to illustrate many established principles of chemistry with experi-
ments that are as interesting and challenging as possible. These principles are basic to the science, but are usu-
ally not intuitively obvious. With each experiment we introduce the theory involved, state in detail the
procedures that are used, describe how to draw conclusions from your observations, and, in an Advance Study
Assignment, ask you to answer questions similar to those you will encounter in the lab. Before coming to lab,
you should read over the experiment for that week, and do the Advance Study Assignment. If you prepare for
lab as you should, you will get more out of it. To give an experiment a bit of a challenge, we occasionally ask
you to work with chemical unknowns.
Many of you have had considerable experience with computers, using word processors and perhaps sci-
entific software. In the manual there are pages for recording data and making calculations. If you wish, you
can prepare your reports with a word processor. You may find that a graphing program is helpful, and may
make your calculations on a spreadsheet such as Excel. If you do this, you should record your data in a sepa-
rate notebook, and do your report and Advance Study Assignment on your word processor.

A Few More Words, This Time to the Teachers

In this, the eighth Edition of our manual, we have added a few new experiments and modified a few others.
Experiment 5 has been modified to improve clarity; Experiment 8 has a new, simpler procedure that does not
involve a mercury manometer. Experiment 15 is new, and offers a better method for measuring vapor pres-
sure; Experiment 19 is also new, and uses water as the solvent for freezing point depression. The procedures
for Experiments 25 and 42 have been simplified. We have retained the optional microscale procedures for two
experiments and the Appendix describing the chemical properties of the cations in Groups I, II, and III.
The format of the manual is unchanged, and the order of the experiments makes them compatible with
the order of the topics in the text Chemistry: Principles and Reactions, Fifth Edition, by William L. Masterton
and Cecile N. Hurley. We believe, however, that the overall set of experiments should be appropriate for use
with most modern texts in general chemistry.
If this is the first time you are using this manual, we have done what we could to make the transition as
easy as possible. The Instructor’s Manual contains, for each experiment, a list of required equipment and
chemicals, the time it will take to do the experiment, and an approximate cost per student. In the second part
of the manual we offer comments and suggestions for each experiment that may be helpful, along with some
sample data and calculations.
iv Preface

As with any endeavor, there are many people who contribute to the effort. We gratefully acknowledge the
assistance given us by Darlane Kroening of our Department, who arranged for the testing by students in our
laboratories of several of the new experiments. We especially thank Barbara Ekeberg for the many long hours
she put in typing the Instructor’s Manual. Finally, we would like to thank those who responded to our ques-
tionnaire with their opinions and suggestions.
It has been a great experience being involved with this manual over its many editions. We have very much
appreciated the support of our users, some of whom have been with us over nearly all the editions. We hope
that this edition works well for you. We invite any comments, questions and suggestions you may have. Please
send them to: [email protected] or [email protected].
E. J. Slowinski
W. C. Wolsey
W. L. Masterton

September, 2003
Safety in the Laboratory

Read this section before performing

any of the experiments in this manual
A chemistry laboratory can be, and should be, a safe place in which to work. Yet each year in academic and
industrial laboratories accidents occur that in some cases injure seriously, or kill, chemists. Most of these acci-
dents could have been foreseen and prevented, had the chemists involved used the proper judgment and taken
proper precautions.
The experiments you will be performing have been selected at least in part because they can be done safely.
Instructions in the procedures should be followed carefully and in the order given. Sometimes even a change in
concentration of one reagent is sufficient to change the conditions of a chemical reaction so as to make it occur in
a different way, perhaps at a highly accelerated rate. So, do not deviate from the procedure given in the manual
when performing experiments unless specifically told to do so by your instructor.

Eye Protection. One of the simplest, and most important, things you can do in the laboratory to avoid injury
is to protect your eyes by routinely wearing safety glasses. Your instructor will tell you what eye protection to
use, and you should use it. Goggles worn up on the hair may be attractive, but they are not protective. If you
use contact lenses, it is advisable to wear safety glasses as well.

Chemical Reagents. Chemicals in general are toxic materials. This means that they can act as poisons or car-
cinogens (causes of cancer) if they get into your digestive or respiratory system. Never taste a chemical sub-
stance, and avoid getting any chemical on your skin. If that should happen, wash it off promptly with plenty of
water. Also, wash your face and hands when you are through working in the laboratory. Do not pipet by mouth;
when pipetting, use a rubber bulb or other device to suck up the liquid. Avoid breathing vapors given off by
reagents or reactions. If directed to smell a vapor, do so cautiously. Use the hood when the directions call for it.
Some reagents, such as concentrated acids or bases, or bromine, are caustic, which means that they can
cause chemical burns on your skin and eat through your clothing. Where such reagents are being used, we note
the potential danger with a C A U T I O N : sign at that point in the procedure. Be particularly careful when
carrying out that step. Always read the label on a reagent bottle before using it; there is a lot of difference
between the properties of 1 M H2SO4 and those of concentrated (18 M) H2SO4.
A few of the chemicals we use are flammable. These include hexane, ethanol, and acetone. Keep your
Bunsen burner well away from any open beakers containing such chemicals, and be careful not to spill them
on the laboratory bench where they might easily get ignited.
When disposing of the chemical products from an experiment, use good judgment. Some dilute, nontoxic
solutions can be poured down the sink and flushed with water. Insoluble or toxic materials should be put in
the waste crocks provided for that purpose. Your lab instructor may give you instructions for treatment and
disposal of the products from specific experiments.

Safety Equipment. In the laboratory there are various pieces of safety equipment, which may include a
safety shower, an eye wash fountain, a fire extinguisher, and a fire blanket. Learn where these items are, so
that you will not have to look all over if you ever need them in a hurry.

Laboratory Attire. Come to the laboratory in sensible clothing. Long, flowing robes are out, as are bare
feet. Sandals and open-toed shoes offer less protection than regular shoes. Keep long hair tied back, out of the
way of flames and reagents.
vi Safety in the Laboratory

If an Accident Occurs. During the laboratory course a few accidents will probably occur. For the most part
these will not be serious, and might involve a spilled reagent, a beaker of hot water that gets tipped over, a
dropped test tube, or a small fire.
A common response in such a situation is panic. A student may respond to an otherwise minor accident
by doing something irrational, like running from the laboratory when the remedy for the accident is close at
hand. If an accident happens to another student, watch for signs of panic and tell the student what to do; if it
seems necessary, help him or her do it. Call the instructor for assistance.
Chemical spills are best handled by washing the area quickly with water from the nearest sink. Use the
eye wash fountain if you get something in your eye. In case of a severe chemical spill on your clothing or
shoes, use the emergency shower and take off the affected clothing. In case of a fire in a beaker, on a bench,
or on your clothing or that of another student, do not panic and run. Smother the fire with an extinguisher, with
a blanket, or with water, as seems most appropriate at the time. If the fire is in a piece of equipment or on the
lab bench and does not appear to require instant action, have your instructor put the fire out. If you cut your-
self on a piece of broken glass, tell your instructor, who will assist you in treating it.

A Message to Foreign Students. Many students from foreign countries take courses in chemistry before
they are completely fluent in English. If you are such a student, it may be that in some experiments you will
be given directions that you do not completely understand. If that happens, do not try to do that part of the
experiment by simply doing what the student next to you seems to be doing. Ask that student, or the instruc-
tor, what the confusing word or phrase means, and when you understand what you should do, go ahead. You
will soon learn the language well enough, but until you feel comfortable with it, do not hesitate to ask others
to help you with unfamiliar phrases and expressions.

Although we have spent considerable time here describing some of the things you should be concerned
with in the laboratory from a safety point of view, this does not mean you should work in the laboratory in
fear and trepidation. Chemistry is not a dangerous activity when practiced properly. Chemists as a group live
longer than other professionals, in spite of their exposure to potentially dangerous chemicals. In this manual
we have attempted to describe safe procedures and to employ chemicals that are safe when used properly.
Many thousands of students have performed the experiments without having accidents, so you can too.
However, we authors cannot be in the laboratory when you carry out the experiments to be sure that you
observe the necessary precautions. You and your laboratory supervisor must, therefore, see to it that the exper-
iments are done properly and assume responsibility for any accidents or injuries that may occur.
Acquisitions Editor: John Holdcroft Print/Media Buyer: Rebecca Cross
Publisher: David Harris Permissions Editor: Sarah Harkrader
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COPYRIGHT © 2005 Brooks/Cole, a division of Thomson Asia

Learning, Inc. Thomson LearningTM is a trademark used herein Thomson Learning
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Contents

Experiment 1
The Densities of Liquids and Solids 1

Experiment 2
Resolution of Matter into Pure Substances, I. Paper Chromatography 7

Experiment 3
Resolution of Matter into Pure Substances, II. Fractional Crystallization 15

Experiment 4
Determination of a Chemical Formula 23

Experiment 5
Identification of a Compound by Mass Relationships 29

Experiment 6
Properties of Hydrates 35

Experiment 7
Analysis of an Unknown Chloride 41

Experiment 8
Verifying the Absolute Zero of Temperature—Determination of the Barometric Pressure 47

Experiment 9
Molar Mass of a Volatile Liquid 55

Experiment 10
Analysis of an Aluminum-Zinc Alloy 61

Experiment 11
The Atomic Spectrum of Hydrogen 69

Experiment 12
The Alkaline Earths and the Halogens—Two Families in the Periodic Table 79

Experiment 13
The Geometrical Structure of Molecules—An Experiment Using Molecular Models 87
viii Contents

Experiment 14
Heat Effects and Calorimetry 97

Experiment 15
The Vapor Pressure and Heat of Vaporization of a Liquid 105

Experiment 16
The Structure of Crystals—An Experiment Using Models 113

Experiment 17
Classification of Chemical Substances 125

Experiment 18
Some Nonmetals and Their Compounds—Preparations and Properties 133

Experiment 19
Molar Mass Determination by Depression of the Freezing Point 141

Experiment 20
Rates of Chemical Reactions, I. The Iodination of Acetone 149

Experiment 21
Rates of Chemical Reactions, II. A Clock Reaction 159

Experiment 22
Properties of Systems in Chemical Equilibrium—Le Châtelier’s Principle 169

Experiment 23
Determination of the Equilibrium Constant for a Chemical Reaction 181

Experiment 24
The Standardization of a Basic Solution and the Determination of the Molar Mass of an Acid 191

Experiment 25
pH Measurements—Buffers and Their Properties 199

Experiment 26
Determination of the Solubility Product of PbI2 209

Experiment 27
Relative Stabilities of Complex Ions and Precipitates Prepared from Solutions of Copper(II) 215

Experiment 28
Determination of the Hardness of Water 223
 Contents ix

Experiment 29
Synthesis and Analysis of a Coordination Compound 229

Experiment 30
Determination of Iron by Reaction with Permanganate—A Redox Titration 239

Experiment 31
Determination of an Equivalent Mass by Electrolysis 245

Experiment 32
Voltaic Cell Measurements 253

Experiment 33
Preparation of Copper(I) Chloride 263

Experiment 34
Development of a Scheme for Qualitative Analysis 269

Experiment 35
Spot Tests for Some Common Anions 275

Experiment 36
Qualitative Analysis of Group I Cations 283

Experiment 37
Qualitative Analysis of Group II Cations 291

Experiment 38
Qualitative Analysis of Group III Cations 299

Experiment 39
Identification of a Pure Ionic Solid 307

Experiment 40
The Ten Test Tube Mystery 315

Experiment 41
Preparation of Aspirin 323

Experiment 42
Rate Studies on the Decomposition of Aspirin 331

Experiment 43
Analysis for Vitamin C 339
x Contents

Appendix I
Vapor Pressure of Water 345

Appendix II
Summary of Solubility Properties of Ions and Solids 347

Appendix IIA
Some Properties of the Cations in Groups I, II, and III 349

Appendix III
Table of Atomic Masses (Based on Carbon-12) 353

Appendix IV
Making Measurements—Laboratory Techniques 355

Appendix V
Mathematical Considerations—Making Graphs 365

Appendix VI
Suggested Locker Equipment 371

Appendix VII
Suggestions for Extension of the Experiments to “Real World Problems” 373
Experiment 1

The Densities of Liquids and Solids

iven a sample of a pure liquid, we can measure many of its characteristics. Its temperature, mass, color,
G and volume are among the many properties we can determine. We find that, if we measure the mass and
volume of different samples of the liquid, the mass and volume of each sample are related in a simple way; if
we divide the mass by the volume, the result we obtain is the same for each sample, independent of its mass.
That is, for samples A, B, and C, of the liquid at constant temperature and pressure,

MassA/VolumeA = MassB/VolumeB = MassC/VolumeC = a constant

That constant, which is clearly independent of the size of the sample, is called its density, and is one of
the fundamental properties of the liquid. The density of water is exactly 1.00000 g/cm3 at 4°C, and is slightly
less than one at room temperature (0.9970 g/cm3 at 25°C). Densities of liquids and solids range from values
that are less than that of water to values that are much greater. Osmium metal has a density of 22.5 g/cm3 and
is probably the densest material known at ordinary pressures.
In any density determination, two quantities must be determined—the mass and the volume of a given
quantity of matter. The mass can easily be determined by weighing a sample of the substance on a balance.
The quantity we usually think of as “weight” is really the mass of a substance. In the process of “weighing”
we find the mass, taken from a standard set of masses, that experiences the same gravitational force as that
experienced by the given quantity of matter we are weighing. The mass of a sample of liquid in a container
can be found by taking the difference between the mass of the container plus the liquid and the mass of the
empty container.
The volume of a liquid can easily be determined by means of a calibrated container. In the laboratory a
graduated cylinder is often used for routine measurements of volume. Accurate measurement of liquid volume
is made by using a pycnometer, which is simply a container having a precisely definable volume. The volume
of a solid can be determined by direct measurement if the solid has a regular geometrical shape. Such is not
usually the case, however, with ordinary solid samples. A convenient way to determine the volume of a solid
is to measure accurately the volume of liquid displaced when an amount of the solid is immersed in the liquid.
The volume of the solid will equal the volume of liquid which it displaces.
In this experiment we will determine the density of a liquid and a solid by the procedure we have out-
lined. First we weigh an empty flask and its stopper. We then fill the flask completely with water, measuring
the mass of the filled stoppered flask. From the difference in these two masses we find the mass of water and
then, from the known density of water, we determine the volume of the flask. We empty and dry the flask, fill
it with an unknown liquid, and weigh again. From the mass of the liquid and the volume of the flask we find
the density of the liquid. To determine the density of an unknown solid metal, we add the metal to the dry
empty flask and weigh. This allows us to find the mass of the metal. We then fill the flask with water, leaving
the metal in the flask, and weigh again. The increase in mass is that of the added water; from that increase,
and the density of water, we calculate the volume of water we added. The volume of the metal must equal the
volume of the flask minus the volume of water. From the mass and volume of the metal we calculate its den-
sity. The calculations involved are outlined in detail in the Advance Study Assignment.
2 Experiment 1 The Densities of Liquids and Solids

Experimental Procedure
A. Mass of a Coin
After you have been shown how to operate the analytical balances in your laboratory, read the section on bal-
ances in Appendix IV. Take a coin and measure its mass to 0.0001 g. Record the mass on the Data page. If
your balance has a TARE bar, use it to re-zero the balance. Take another coin and weigh it, recording its mass.
Remove both coins, zero the balance, and weigh both coins together, recording the total mass. If you have no
TARE bar on your balance, add the second coin and measure and record the mass of the two coins. Then
remove both coins and find the mass of the second one by itself. When you are satisfied that your results are
those you would expect, go to the stockroom and obtain a glass-stoppered flask, which will serve as a pyc-
nometer, and samples of an unknown liquid and an unknown metal.

B. Density of a Liquid
If your flask is not clean and dry, clean it with detergent solution and water, rinse it with a few cubic cen-
timeters of acetone, and dry it by letting it stand for a few minutes in the air or by gently blowing compressed
air into it for a few moments.
Weigh the dry flask with its stopper on the analytical balance, or the toploading balance if so directed, to
the nearest milligram. Fill the flask with distilled water until the liquid level is nearly to the top of the ground
surface in the neck. Put the stopper in the flask in order to drive out all the air and any excess water. Work the
stopper gently into the flask, so that it is firmly seated in position. Wipe any water from the outside of the flask
with a towel and soak up all excess water from around the top of the stopper.
Again weigh the flask, which should be completely dry on the outside and full of water, to the nearest
milligram. Given the density of water at the temperature of the laboratory and the mass of water in the flask,
you should be able to determine the volume of the flask very precisely. Empty the flask, dry it, and fill it with
your unknown liquid. Stopper and dry the flask as you did when working with the water, and then weigh the
stoppered flask full of the unknown liquid, making sure its surface is dry. This measurement, used in conjunc-
tion with those you made previously, will allow you to find accurately the density of your unknown liquid.

C. Density of a Solid
Pour your sample of liquid from the flask into its container. Rinse the flask with a small amount of acetone
and dry it thoroughly. Add small chunks of the metal sample to the flask until the flask is at least half full.
Weigh the flask, with its stopper and the metal, to the nearest milligram. You should have at least 50 g of metal
in the flask.
Leaving the metal in the flask, fill the flask with water and then replace the stopper. Roll the metal around
in the flask to make sure that no air remains between the metal pieces. Refill the flask if necessary, and then
weigh the dry, stoppered flask full of water plus the metal sample. Properly done, the measurements you have
made in this experiment will allow a calculation of the density of your metal sample that will be accurate to
about 0.1%.
DISPOSAL OF REACTION PRODUCTS. Pour the water from the flask. Put the metal in its container.
Dry the flask and return it with its stopper and your metal sample, along with the sample of unknown
liquid, to the stockroom.
Name ____________________________________ Section _________________________________

Experiment 1

Data and Calculations: The Densities of Liquids and Solids

A. Mass of coin 1 ____________ g Mass of coin 2 ____________ g

Mass of coins 1 and 2 weighed together ____________ g

What general law is illustrated by the results of this experiment?

B. Density of unknown liquid

Mass of empty flask plus stopper ____________ g

Mass of stoppered flask plus water ____________ g

Mass of stoppered flask plus liquid ____________ g

Mass of water ____________ g

Temperature in the laboratory ____________ °C

Volume of flask (density of H2O at 25°C, 0.9970 g/cm3; at

20°C, 0.9982 g/cm3) ____________ cm3

Mass of liquid ____________ g

Density of liquid ____________ g/cm3

To how many significant figures can the liquid density be

properly reported? (See Appendix V.) ____________

C. Density of unknown metal

Mass of stoppered flask plus metal ____________ g

Mass of stoppered flask plus metal plus water ____________ g

Mass of metal ____________ g

Mass of water ____________ g

Volume of water ____________ cm3

(continued on following page)

4 Experiment 1 The Densities of Liquids and Solids

Volume of metal ____________ cm3

Density of metal ____________ g/cm3

To how many significant figures can the density of the metal be

properly reported? ____________

Explain why the value obtained for the density of the metal is likely to have a larger percentage error than
that found for the liquid.

Unknown liquid no. ____________ Unknown solid no. ____________

Name ____________________________________ Section _________________________________

Experiment 1

Advance Study Assignment: The Densities of Solids and Liquids

The advance study assignments in this laboratory manual are designed to assist you in making the calculations
required in the experiment you will be doing. We do this by furnishing you with sample data and showing in
some detail how these data can be used to obtain the desired results. In the advance study assignments we will
often include the guiding principles as well as the specific relationships to be employed. If you work through
the steps in each calculation by yourself, you should have no difficulty when you are called upon to make the
necessary calculations on the basis of the data you obtain in the laboratory.

1. Finding the volume of a flask.

A student obtained a clean dry glass-stoppered flask. She weighed the flask and stopper on an analytical
balance and found the total mass to be 31.601 g. She then filled the flask with water and obtained a mass
for the full stoppered flask of 60.735 g. From these data, and the fact that at the temperature of the labo-
ratory the density of water was 0.9973 g/cm3, find the volume of the stoppered flask.

a. First we need to obtain the mass of the water in the flask. This is found by recognizing that the mass
of a sample is equal to the sum of the masses of its parts. For the filled stoppered flask:

Mass of filled stoppered flask = mass of empty stoppered flask + mass of water,
so mass of water = mass of filled flask – mass of empty flask
Mass of water = ____________ g – ____________ g = ____________ g

Many mass and volume measurements in chemistry are made by the method used in 1a. This method
is called measuring by difference, and is a very useful one.

b. The density of a pure substance is equal to its mass divided by its volume:

mass mass
Density = or volume =
volume density

The volume of the flask is equal to the volume of the water it contains. Since we know the mass and
density of the water, we can find its volume and that of the flask. Make the necessary calculation.

Volume of water = volume of flask = ____________ cm3

2. Finding the density of an unknown liquid.

Having obtained the volume of the flask, the student emptied the flask, dried it, and filled it with an
unknown whose density she wished to determine. The mass of the stoppered flask when completely filled
with liquid was 56.796 g. Find the density of the liquid.

a. First we need to find the mass of the liquid by measuring by difference:

Mass of liquid = ____________ g – ____________ g = ____________ g

(continued on following page)

6 Experiment 1 The Densities of Liquids and Solids

b. Since the volume of the liquid equals that of the flask, we know both the mass and volume of the liq-
uid and can easily find its density using the equation in 1b. Make the calculation.

Density of liquid = ____________ g/cm3

3. Finding the density of a solid.

The student then emptied the flask and dried it once again. To the empty flask she added pieces of a metal
until the flask was about half full. She weighed the stoppered flask and its metal contents and found that
the mass was 99.323 g. She then filled the flask with water, stoppered it, and obtained a total mass of
120.827 g for the flask, stopper, metal, and water. Find the density of the metal.

a. To find the density of the metal we need to know its mass and volume. We can easily obtain its mass
by the method of differences:

Mass of metal = ____________ g − ____________ g = ____________ g

b. To determine the volume of metal, we note that the volume of the flask must equal the volume of
the metal plus the volume of water in the filled flask containing both metal and water. If we can find
the volume of water, we can obtain the volume of metal by the method of differences. To obtain the
volume of the water we first calculate its mass:

Mass of water = mass of (flask + stopper + metal + water) − mass of (flask + stopper + metal)
Mass of water = ____________ g − ____________ g = ____________ g

The volume of water is found from its density, as in 1b. Make the calculation.

Volume of water = ____________ cm3

c. From the volume of the water we calculate the volume of metal:

Volume of metal = volume of flask − volume of water

Volume of metal = ____________ cm3 − ____________ cm3 = ____________ cm3

From the mass of and volume of metal we find the density, using the equation in 1b. Make the
calculation.

Density of metal = ____________ g/cm3

Now go back to Question 1 and check to see that you have reported the proper number of significant
figures in each of the results you calculated in this assignment. Use the rules on significant figures as given
in your chemistry text.
Experiment 2

Resolution of Matter into Pure Substances,

I. Paper Chromatography

he fact that different substances have different solubilities in a given solvent can be used in several ways
T to effect a separation of substances from mixtures in which they are present. We will see in an upcoming
experiment how fractional crystallization allows us to obtain pure substances by relatively simple procedures
based on solubility properties. Another widely used resolution technique, which also depends on solubility dif-
ferences, is chromatography.
In the chromatographic experiment a mixture is deposited on some solid adsorbing substance, which
might consist of a strip of filter paper, a thin layer of silica gel on a piece of glass, some finely divided char-
coal packed loosely in a glass tube, or even some microscopic glass beads coated thinly with a suitable adsorb-
ing substance and contained in a piece of copper tubing.
The components of a mixture are adsorbed on the solid to varying degrees, depending on the nature of the
component, the nature of the adsorbent, and the temperature. A solvent is then caused to flow through
the adsorbent solid under applied or gravitational pressure or by the capillary effect. As the solvent passes
the deposited sample, the various components tend, to varying extents, to be dissolved and swept along the
solid. The rate at which a component will move along the solid depends on its relative tendency to be dissolved
in the solvent and adsorbed on the solid. The net effect is that, as the solvent passes slowly through the solid,
the components separate from each other and move along as rather diffuse zones. With the proper choice of
solvent and adsorbent, it is possible to resolve many complex mixtures by this procedure. If necessary, we can
usually recover a given component by identifying the position of the zone containing the component, remov-
ing that part of the solid from the system, and eluting the desired component with a suitable good solvent.
The name given to a particular kind of chromatography depends upon the manner in which the experi-
ment is conducted. Thus, we have column, thin-layer, paper, and gas chromatography, all in very common use
(Fig. 2.1). Chromatography in its many possible variations offers the chemist one of the best methods, if not
the best method, for resolving a mixture into pure substances, regardless of whether that mixture consists of
a gas, a volatile liquid, or a group of nonvolatile, relatively unstable, complex organic compounds.

Figure 2.1 This is a gas chromatogram of a sample of unleaded gasoline. Each peak corresponds to a
different molecule, so gasoline has many many components, at least 50, each of which can be identified.
The molar masses vary from about 50 to about 150, with the largest peak, at about 3 min, that due to
toluene, C6H5CH3. Sample size for the chromatogram was less than 10–6 grams, <0.001 mg! Gas chro-
matography offers the best method for resolution of complex volatile mixtures. Chromatogram courtesy
of Prof. Becky Hoye at Macalester College.
8 Experiment 2 Resolution of Matter into Pure Substances, I. Paper Chromatography

In this experiment we will use paper chromatography to separate a mixture of metallic ions in solution. A
sample containing a few micrograms of ions is applied as a spot near one edge of a piece of filter paper. That
edge is immersed in a solvent, with the paper held vertically. As the solvent rises up the paper by capillary action,
it will carry the metallic ions along with it to a degree that depends upon the relative tendency of each ion to dis-
solve in the solvent and adsorb on the paper. Because the ions differ in their properties, they move at different
rates and become separated on the paper. The position of each ion during the experiment can be recognized if the
ion is colored, as some of them are. At the end of the experiment their positions are established more clearly by
treating the paper with a staining reagent which reacts with each ion to produce a colored product. By observing
the position and color of the spot produced by each ion, and the positions of the spots produced by an unknown
containing some of those ions, you can readily determine the ions present in the unknown.
It is possible to describe the position of spots such as those you will be observing in terms of a quantity
called the Rf value. In the experiment the solvent rises a certain distance, say L centimeters. At the same time
a given component will usually rise a smaller distance, say D centimeters. The ratio of D/L is called the Rf
value for that component:

D distance component moves

Rf = = (1)
L distance solvent moves
The Rf value is a characteristic property of a given component in a chromatography experiment conducted
under particular conditions. It does not depend upon concentration or upon the other components present.
Hence it can be reported in the literature and used by other researchers doing similar analyses. In the experi-
ment you will be doing, you will be asked to calculate the Rf values for each of the cations studied.

Experimental Procedure
From the stockroom obtain an unknown and a piece of filter paper about 19 cm long and 11 cm wide. Along
the 19-cm edge, draw a pencil line about 1 cm from that edge. Starting 1.5 cm from the end of the line, mark
the line at 2-cm intervals. Label the segments of the line as shown in Figure 2.2, with the formulas of the ions
to be studied and the known and unknown mixtures.
Put two or three drops of 0.1 M solutions of the following compounds in small micro test tubes, one solu-
tion to a tube:

AgNO3 Co(NO3)2 Cu(NO3)2 Fe(NO3)3 Hg(NO3)2

In solution these substances exist as ions. The metallic cations are Ag+, Co2+, Cu2+, Fe3+, and Hg2+, respec-
tively. One drop of each solution contains about 50 micrograms of cation. Into a sixth micro test tube put two

Figure 2.2
 Experiment 2 Resolution of Matter into Pure Substances, I. Paper Chromatography 9

drops of each of the five solutions; swirl until the solutions are well mixed. This mixture will be our known,
since we know it contains all of the cations.
Your instructor will furnish you with a fine capillary tube, which will serve as an applicator. Test the appli-
cation procedure by dipping the applicator into one of the colored solutions and touching it momentarily to a
round piece of filter paper. The liquid from the applicator should form a spot no larger than 8 mm in diame-
ter. Practice making spots until you can reproduce the spot size each time.
Clean the applicator by dipping it about 1 cm into distilled water and then touching the round filter paper
to remove the liquid. Continue contact until all the liquid in the tube is gone. Repeat the cleaning procedure one
more time. Dip the applicator into one of the cation solutions and put a spot on the line on the rectangular fil-
ter paper in the region labeled for that cation. Clean the applicator twice, and repeat the procedure with anoth-
er solution. Continue this approach until you have put a spot for each of the five cations and the known and
unknown on the paper, cleaning the applicator between solutions. Dry the paper by moving it in the air or hold-
ing it briefly in front of a hair dryer or heat lamp (low setting). Apply the known and unknown three more times
to the same spots; the known and unknown are less concentrated than the cation solutions, so this procedure
will increase the amount of each ion in the spots. Make sure that you dry the spots between applications, since
otherwise they will get larger. Don’t heat the paper more than necessary, just enough to dry the spots.
Draw about 15 mL of eluting solution from the supply on the reagent shelf. This solution is made by mix-
ing a solution of HCl, hydrochloric acid, with ethanol and butanol, which are organic solvents. Pour the elut-
ing solution into a 600-mL beaker and cover with a watch glass.
Check to make sure that the spots on the filter paper are all dry. Place a 4- to 5-cm length of Scotch tape
along the upper end of the left edge of the paper, as shown in Figure 2.1, so that about half of the tape is on
the paper. Form the paper into a cylinder by attaching the tape to the other edge, in such a way that the edges
are parallel but do not overlap. When you are finished, the pencil line at the bottom of the cylinder should form
a circle, approximately anyway, and the two edges of the paper should not quite touch. Stand the cylinder up
on the lab bench to check that such is the case and readjust the tape if necessary. Do not tape the lower edges
of the paper together.
Place the cylinder in the eluting solution in the 600-mL beaker, with the sample spots down near the liq-
uid surface. The paper should not touch the wall of the beaker. Cover the beaker with the watch glass. The sol-
vent will gradually rise by capillary action up the filter paper, carrying along the cations at different rates. After
the process has gone on for a few minutes, you should be able to see colored spots on the paper, showing the
positions of some of the cations.
While the experiment is proceeding, you can test the effect of the staining reagent on the different cations.
Put an 8-mm spot of each of the cation solutions on a clean piece of round filter paper, labeling each spot and
cleaning the applicator between solutions. Dry the spots as before. Some of them will have a little color; record
those colors on the Data page. Put the filter paper on a paper towel, and, using the spray bottle on the lab
bench, spray the paper evenly with the staining reagent, getting the paper moist but not really wet. The stain-
ing reagent is a solution containing potassium ferrocyanide and potassium iodide. This reagent forms colored
precipitates or reaction products with many cations, including all of those used in this experiment. Note the
colors obtained with each of the cations. Considering that each spot contains less than 50 micrograms of
cation, the tests are quite definitive.
When the eluting solution has risen to within about 2 cm of the top of the filter paper (it will take about
75 minutes), remove the cylinder from the beaker and take off the tape. Draw a pencil line along the solvent
front. Dry the paper with gentle heat until it is quite dry. Note any cations that must be in your unknown by
virtue of your being able to see their colors. Then, with the paper on a paper towel, spray it as before with the
staining reagent. Any cations you identified in your unknown before staining should be observed, as well as
any that require staining for detection.
Measure the distance from the straight line on which you applied the spots to the solvent front, which is
distance L in Equation 1. Then measure the distance from the pencil line to the center of the spot made by each
of the cations, when pure and in the known; this is distance D. Calculate the Rf value for each cation. Then
calculate Rf values for the cations in the unknown. How do the Rf values compare?
DISPOSAL OF REACTION PRODUCTS. When you are finished with the experiment, pour the eluting
solution into the waste crock, not down the sink. Wash your hands before leaving the laboratory.
This page intentionally left blank
Name ____________________________________ Section _________________________________

Experiment 2

Data and Calculations: Resolution of Matter into Pure Substances,

I. Paper Chromatography

Ag+ Co2+ Cu2+ Fe3+ Hg2+

Colors (if observed)

Dry __________ __________ __________ __________ __________

After staining __________ __________ __________ __________ __________

Distance solvent moved (L) __________ __________ __________ __________ __________

Distance cation moved (D) __________ __________ __________ __________ __________

Rf __________ __________ __________ __________ __________

Known Mixture
Distance solvent moved __________ __________ __________ __________ __________

Distance cation moved __________ __________ __________ __________ __________

Rf __________ __________ __________ __________ __________

Unknown Mixture
Cations identified

Dry __________ __________ __________ __________ __________

After staining __________ __________ __________ __________ __________

Distance solvent moved __________ __________ __________ __________ __________

Distance cation moved __________ __________ __________ __________ __________

Rf __________ __________ __________ __________ __________

Composition of unknown __________ __________ __________ __________ __________

Unknown no. __________

This page intentionally left blank
Name ____________________________________ Section ________________________________

Experiment 2

Advance Study Assignment: Resolution of Matter into Pure Substances,

I. Paper Chromatography

1. A student chromatographs a mixture, and after developing the spots with a suitable reagent he observes
the following:

What are the Rf values?

2. Explain, in your own words, why samples can often be separated into their components by chromatography.

3. The solvent moves 4 cm in about 15 minutes. Why shouldn’t the experiment be stopped at that time
instead of waiting 75 minutes for the solvent to move 10 cm?

4. In this experiment it takes about 6 microliters of solution to produce a spot 8 mm in diameter. If the
Cu(NO3)2 solution contains about 6 g Cu2+ per liter, how many micrograms of Cu2+ ion are there in one
spot?

____________ micrograms
This page intentionally left blank
Experiment 3

Resolution of Matter into Pure Substances,

II. Fractional Crystallization

ne of the important problems faced by chemists is that of determining the nature and state of purity of
O the substances with which they work. In order to perform meaningful experiments, chemists must ordi-
narily use essentially pure substances, which are often prepared by separation from complex mixtures.
In principle the separation of a mixture into its component substances can be accomplished by carrying the
mixture through one or more physical changes, experimental operations in which the nature of the components
remains unchanged. Because the physical properties of various pure substances are different, physical changes
frequently allow an enrichment of one or more substances in one of the fractions that is obtained during the
change. Many physical changes can be used to accomplish the resolution of a mixture, but in this experiment
we will restrict our attention to one of the simpler ones in common use, namely, fractional crystallization.
The solubilities of solid substances in different kinds of liquid solvents vary widely. Some substances are
essentially insoluble in all known solvents; the materials we classify as macromolecular are typical examples.
Most materials are noticeably soluble in one or more solvents. Those substances that we call salts often have
very appreciable solubility in water but relatively little solubility in any other liquids. Organic compounds,
whose molecules contain carbon and hydrogen atoms as their main constituents, are often soluble in organic
liquids such as benzene or carbon tetrachloride.
We also often find that the solubility of a given substance in a liquid is sharply dependent on temperature.
Most substances are more soluble in a given solvent at high temperatures than at low temperatures, although
there are some materials whose solubility is practically temperature-independent and a few others that become
less soluble as temperature increases.
By taking advantage of the differences in solubility of different substances we often find it possible to
separate the components of a mixture in essentially pure form.
In this experiment you will be given a sample containing silicon carbide, potassium nitrate, and copper
sulfate. Your problem will be to separate two pure components from the mixture, using water as the solvent.
Silicon carbide, SiC, is a black, very hard material; it is the classic abrasive, and completely insoluble in water.
Potassium nitrate, KNO3, and copper sulfate, CuSO4 ⋅ 5 H2O, are water-soluble ionic substances, with differ-
ent solubilities at different temperatures, as indicated in Figure 3.1. The copper sulfate we will use is blue in
its crystalline hydrate and in solution. The solubility of the hydrate increases fairly rapidly with temperature.
Potassium nitrate is a white solid, colorless in solution. Its solubility increases about 20-fold between 0°C and
100°C.
Given a mixture containing roughly equal amounts of SiC and KNO3 and a small amount of CuSO4 ⋅ 5 H2O,
we separate out the silicon carbide first. This is done by simply stirring the mixture with water, which dis-
solves all of the potassium nitrate and copper sulfate in the mixture. The insoluble silicon carbide remains
behind and is filtered off.
The solution obtained after filtration contains KNO3 and CuSO4 in a rather large amount of water. Some
of the water is removed by boiling, and then the solution is cooled to 0°C. At that point the KNO3 is not very
soluble, and most of it crystallizes from solution. Since CuSO4 is not present in large amount, its solubility is
not exceeded and it remains in solution. The solid KNO3 is separated from the solution by filtration. This pro-
cedure, by which a substance can be separated from an impurity, is called fractional crystallization.
The solid potassium nitrate one recovers is contaminated by a small amount of copper sulfate. The purity
of the solid can be markedly increased by stirring it with a small amount of water and then filtering off the
dissolved CuSO4. The purity can be established by the intensity of the color produced by the copper impurity
when treated with ammonia, NH3.
16 Experiment 3 Resolution of Matter into Pure Substances, II. Fractional Crystallization

Figure 3.1

Experimental Procedure
Obtain from the stockroom a Buchner funnel, a suction flask, and a sample (about 20 grams) of your unknown
solid mixture.
Weigh a 150-mL beaker, a 50-mL beaker, and a piece of filter paper, one item at a time, on a top-loading
balance. These, and all other weighings in this experiment, should be made to ±0.1 g. (Do not use an analyt-
ical balance for any weighings.) Use the masses you obtain as needed in your calculations.
Add your sample to the 150-mL beaker and weigh again. Then add about 40 mL of distilled water, which
will be enough to dissolve the soluble solids. Light your Bunsen burner and adjust the flame so it is blue, quiet,
and of moderate size.

Separation of SiC
Support the beaker with its contents on a piece of wire gauze on an iron ring. Warm gently to about 50°C,
while stirring the mixture. When the blue and white solids are all dissolved, pour the contents of the beaker
into a Buchner funnel while gentle suction is being applied (see Fig. 3.2 and Appendix IV). Transfer as much
of the black solid carbide as you can to the funnel, using your rubber policeman. Transfer the blue filtrate to
the (cleaned) 150-mL beaker and add 15 drops of 6 M HNO3, nitric acid, which will help ensure that the
copper sulfate remains in solution in later steps. Re-assemble the funnel, apply suction, and wash the SiC on
the filter paper with distilled water. Continue the suction for a few minutes to dry the SiC. Turn off the suc-
tion, and, using your spatula, lift the filter paper and the SiC crystals from the funnel, and put the paper on the
lab bench so that the crystals may dry in the air. When you are finished with the rest of the experiment, weigh
the dry SiC on its piece of filter paper.

Separation of KNO3
Heat the blue filtrate in the beaker to the boiling point, and then boil gently until the white crystals of KNO3
are visible in the liquid.
 Experiment 3 Resolution of Matter into Pure Substances, II. Fractional Crystallization 17

Figure 3.2 To operate the Buchner funnel, put a piece of circular filter paper in the funnel. Turn on suc-
tion and spray filter paper with distilled water from wash bottle. Keep suction on while filtering sample.

C A U T I O N : The hot liquid may have a tendency to bump, so do not heat it too strongly.
While the filtrate is being heated, prepare some ice-cold distilled water by putting your wash bottle in an ice-
water bath.
When white crystals are clearly apparent in the boiling liquid (the solution may appear cloudy at that
point) stop heating and add 12 mL distilled water to the solution. Stir the mixture with a glass stirring rod to
dissolve the solids, including any on the wall; if necessary, warm the solution but do not boil it.
Cool the solution to room temperature in a water bath, and then to about 0°C in an ice bath. White crys-
tals of KNO3 will come out of solution. Stir the cold slurry of crystals for several minutes. Check the temper-
ature of the slurry with your thermometer. It should be no more than 3°C. Continue stirring until your mixture
gets to that temperature or even a bit lower.

Assemble the Buchner Funnel. Chill it by adding about 100 mL of ice-cold distilled water from
your wash bottle, and, after about a minute, by drawing the water through with suction. Filter the KNO3 slurry
through the cold Buchner funnel. Your rubber policeman will be helpful when you transfer the last of the crys-
tals. Press the crystals dry with a clean piece of filter paper, and continue to apply suction for another 30 sec-
onds. Turn off the suction. Lift the filter paper and the crystals from the funnel, and put the paper and crystals
on the lab bench.

DISPOSAL OF REACTION PRODUCTS. By this procedure you have separated most of the KNO3 in
your sample from the CuSO4, which is present in the solution in the suction flask. This solution may
now be discarded, so dispose of it as directed by your instructor.

Clean and dry your 150-mL beaker and to it add the KNO3 crystals from the filter paper. Weigh the beaker
and its contents.

Analysis of the Purity of the KNO3

The KNO3 crystals you have prepared contain a small amount of CuSO4 as an impurity. To find the amount of
CuSO4 present, weigh out 0.5 g of the crystals into your weighed 50-mL beaker. Dissolve the crystals in 3 mL
distilled water, and then add 3 mL 6 M NH3, ammonia. The copper impurity will form a blue solution in the
NH3. Pour the solution into a small test tube. Compare the intensity of the blue color with that in a series of
standard solutions prepared by your instructor. Estimate the relative concentration of CuSO4 ⋅ 5 H2O in your
product.
18 Experiment 3 Resolution of Matter into Pure Substances, II. Fractional Crystallization

Recrystallization of the KNO3

Given the mass of the KNO3 you recovered (less 0.5 g), use Figure 3.1 to estimate the amount of water needed
to dissolve the solid at 100°C. Add three times that amount of distilled water to the KNO3. Stir the crystals for
a minute or two to ensure that all of the CuSO4 impurity goes into solution.
Cool the mixture in an ice bath. This will recrystallize most of the KNO3 that dissolved. After stirring for
several minutes, check the temperature of the mixture with your thermometer. Continue cooling until the tem-
perature is below 3°C. Then filter the slurry through an ice-cold Buchner funnel, transferring as much of the
solid as possible to the funnel. Press the crystals dry with a piece of filter paper and continue to apply suction
for a minute or so. Lift the filter paper from the funnel and put it with its batch of crystals on the lab bench.
Transfer the purified crystals to a piece of dry filter paper. Weigh the paper and the crystals.
Determine the amount of CuSO4 impurity in your recrystallized sample as you did with the first batch,
and record that value. The recrystallization should have very significantly increased the purity of your KNO3.
Weigh your dry SiC on its piece of filter paper. Show your samples of SiC and KNO3 to your instructor
for evaluation. Then turn the samples in to the stockroom.
Name ____________________________________ Section _________________________________

Experiment 3

Data and Calculations: Resolution of Matter into Pure Substances,

II. Fractional Crystallization

Mass of 150-mL beaker ______________ g Mass of 50-mL beaker ______________ g

Mass of filter paper ______________ g

Separation of SiC
Mass of sample plus 150-mL beaker ______________ g

Mass of sample ______________ g

Mass of SiC plus filter paper ______________ g

Mass of SiC ______________ g

Percentage of SiC in sample ______________ %

Separation of KNO3
Mass of 150-mL beaker plus KNO3 ______________ g

Mass of KNO3 recovered ______________ g

Percentage of sample recovered as KNO3 ______________ %

Analysis of Purity of KNO3

Mass of 50-mL beaker plus KNO3 ______________ g

Mass of KNO3 used in analysis ______________ g

Percentage of CuSO4 ⋅ 5 H2O present in KNO3 ______________ %

(continued on following page)

20 Experiment 3 Resolution of Matter into Pure Substances, II. Fractional Crystallization

Recrystallization of KNO3
Mass of filter paper plus purified KNO3 ______________ g

Mass of purified KNO3 obtained ______________ g

Percentage of sample recovered as pure KNO3 ______________ %

Mass of 50-mL beaker plus purified KNO3 ______________ g

Mass of purified KNO3 used in analysis ______________ g

Percentage of CuSO4 ⋅ 5 H2O in purified KNO3 ______________ %

Name ____________________________________ Section ________________________________

Experiment 3

Advance Study Assignment: Resolution of Matter into Pure Substances,

II. Fractional Crystallization

1. Using Figure 3.1, determine

a. the number of grams of KNO3 that will dissolve in 100 g of H2O at 100°C. If you need to, see
Appendix V for a discussion of how to interpret a graph.

______________ g KNO3

b. the number of grams of water required to dissolve 20 g of KNO3 at 100°C. (Hint: your answer to 1a
gives you the needed conversion factor for g KNO3 to g H2O.)

______________ g H2O

c. the number of grams of water required to dissolve 2.0 g CuSO4 ⋅ 5 H2O at 100°C.

______________ g H2O

d. the number of grams of water required at 100°C to dissolve a mixture containing 20 g KNO3 and 2.0 g
CuSO4 ⋅ 5 H2O, assuming that the solubility of one substance is not affected by the presence of
another.

______________ g H2O

2. To the solution in Problem 1d at 100°C, 15 g of water are added, and the solution is cooled to 0°C.

a. How much KNO3 remains in solution? (See Fig. 3.1.)

______________ g KNO3

b. How much KNO3 crystallizes out?

______________ g KNO3

c. How much CuSO4 ⋅ 5 H2O crystallizes out?

______________ g CuSO4 ⋅ 5 H2O

d. What percent of the KNO3 in the sample is recovered?

______________ %
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Experiment 4

Determination of a Chemical Formula

hen atoms of one element combine with those of another, the combining ratio is typically an integer or
W a simple fraction; 1:2, 1:1, 2:1, and 2:3 are ratios one might encounter. The simplest formula of a com-
pound expresses that atom ratio. Some substances with the ratios we listed include CaCl2, KBr, Ag2O, and
Fe2O3. When more than two elements are present in a compound, the formula still indicates the atom ratio.
Thus the substance with the formula Na2SO4 indicates that the sodium, sulfur, and oxygen atoms occur in that
compound in the ratio 2:1:4. Many compounds have more complex formulas than those we have noted, but
the same principles apply.
To find the formula of a compound we need to find the mass of each of the elements in a weighed sample
of that compound. For example, if we resolved a sample of the compound NaOH weighing 40 grams into its
elements, we would find that we obtained just about 23 grams of sodium, 16 grams of oxygen, and 1 gram of
hydrogen. Since the atomic mass scale tells us that sodium atoms have a relative mass of 23, oxygen atoms a
relative mass of 16, and hydrogen atoms a relative mass of just about 1, we would conclude that the sample
of NaOH contained equal numbers of Na, O, and H atoms. Since that is the case, the atom ratio Na:O:H is
1:1:1, and so the simplest formula is NaOH. In terms of moles, we can say that that one mole of NaOH, 40
grams, contains one mole of Na, 23 grams, one mole of O, 16 grams, and one mole of H, 1 gram, where we
define the mole to be that mass in grams equal numerically to the sum of the atomic masses in an element or
a compound. From this kind of argument we can conclude that the atom ratio in a compound is equal to the
mole ratio. We get the mole ratio from chemical analysis, and from that the formula of the compound.
In this experiment we will use these principles to find the formula of the compound with the general for-
mula CuxCly ⋅ zH2O, where the x, y, and z are integers which, when known, establish the formula of the com-
pound. (In expressing the formula of a compound like this one, where water molecules remain intact within
the compound, we retain the formula of H2O in the formula of the compound.)
The compound we will study, which is called copper chloride hydrate, turns out to be ideal for one’s first
venture into formula determination. It is stable, can be obtained in pure form, has a characteristic blue-green
color which changes as the compound is changed chemically, and is relatively easy to decompose into the ele-
ments and water. In the experiment we will first drive out the water, which is called the water of hydration,
from an accurately weighed sample of the compound. This occurs if we gently heat the sample to a little over
100°C. As the water is driven out, the color of the sample changes from blue-green to a tan-brown color sim-
ilar to that of tobacco. The compound formed is anhydrous (no water) copper chloride. If we subtract its mass
from that of the hydrate, we can determine the mass of the water that was driven off, and, using the molar mass
of water, find the number of moles of H2O that were in the sample.
In the next step we need to find either the mass of copper or the mass of chlorine in the anhydrous sample
we have prepared. It turns out to be much easier to determine the mass of the copper, and find the mass of
chlorine by difference. We do this by dissolving the anhydrous sample in water, which gives us a green solu-
tion containing copper and chloride ions. To that solution we add some aluminum metal wire. Aluminum is
what we call an active metal; in contact with a solution containing copper ions, the aluminum metal will react
chemically with those ions, converting them to copper metal. The aluminum is said to reduce the copper ions
to the metal, and is itself oxidized. The copper metal appears on the wire as the reaction proceeds, and has the
typical red-orange color. When the reaction is complete, we remove the excess Al, separate the copper from
the solution, and weigh the dried metal. From its mass we can calculate the number of moles of copper in the
sample. We find the mass of chlorine by subtracting the mass of copper from that of the anhydrous copper
chloride, and from that value determine the number of moles of chlorine. The mole ratio for Cu:Cl:H2O gives
us the formula of the compound.
24 Experiment 4 Determination of a Chemical Formula

Experimental Procedure
Weigh a clean, dry crucible, without a cover, accurately on the analytical balance. Place about 1 gram of the
unknown hydrated copper chloride in the crucible. With your spatula, break up any sizeable crystal particles
by pressing them against the wall of the crucible. Then weigh the crucible and its contents accurately. Enter
your results on the Data page.
Place the uncovered crucible on a clay triangle supported by an iron ring. Light your Bunsen burner away
from the crucible, and adjust the burner so that you have a small flame. Holding the burner in your hand, gently
heat the crucible as you move the burner back and forth. Do not overheat the sample. As the sample warms,
you will see that the green crystals begin to change to brown around the edges. Continue gentle heating, slowly
converting all of the hydrated crystals to the anhydrous brown form. After all of the crystals appear to be
brown, continue heating gently, moving the burner back and forth judiciously, for an additional two minutes.
Remove the burner, cover the crucible to minimize rehydration, and let it cool for about 15 minutes. Remove
the cover, and slowly roll the brown crystals around the crucible. If some green crystals remain, repeat the
heating process. Finally, weigh the cool uncovered crucible and its contents accurately.
Transfer the brown crystals in the crucible to an empty 50-mL beaker. Rinse out the crucible with two 5- to
7-mL portions of distilled water, and add the rinsings to the beaker. Swirl the beaker gently to dissolve the
brown solid. The color will change to green as the copper ions are rehydrated. Measure out about 20 cm of
20-gauge aluminum wire (∼0.25 g) and form the wire into a loose spiral coil. Put the coil into the solution so
that it is completely immersed. Within a few moments you will observe some evolution of H2, hydrogen gas,
and the formation of copper metal on the Al wire. As the copper ions are reduced, the color of the solution
will fade. The Al metal wire will be slowly oxidized and enter the solution as aluminum ions (The hydrogen
gas is formed as the aluminum reduces water in the slightly acidic copper solution.)
When the reaction is complete, which will take about 30 minutes, the solution will be colorless, and most
of the copper metal that was produced will be on the Al wire. Add 5 drops of 6 M HCl to dissolve any insol-
uble aluminum salts and clear up the solution. Use your glass stirring rod to remove the copper from the wire
as completely as you can. Slide the unreacted aluminum wire up the wall of the beaker with your stirring rod,
and, while the wire is hanging from the rod, rinse off any remaining Cu particles with water from your wash
bottle. If necessary, complete the removal of the Cu with a drop or two of 6 M HCl added directly to the wire.
Put the wire aside; it has done its duty.
In the beaker you now have the metallic copper produced in the reaction, in a solution containing an alu-
minum salt. In the next step we will use a Buchner funnel to separate the copper from the solution. Weigh
accurately a dry piece of filter paper that will fit in the Buchner funnel, and record its mass. Put the paper in
the funnel, and apply light suction as you add a few mL of water to ensure a good seal. With suction on, decant
the solution into the funnel. Wash the copper metal thoroughly with distilled water, breaking up any copper
particles with your stirring rod. Transfer the wash and the copper to the filter funnel. Wash any remaining
copper into the funnel with water from your wash bottle. All of the copper must be transferred to the funnel.
Rinse the copper on the paper once again with water. Turn off the suction. Add 10 mL of 95% ethanol to
the funnel, and after a minute or so turn on the suction. Draw air through the funnel for about 5 minutes. With
your spatula, lift the edge of the paper, and carefully lift the paper and the copper from the funnel. Dry the
paper and copper under a heat lamp for 5 minutes. Allow it to cool to room temperature and then weigh it
accurately.

DISPOSAL OF REACTION PRODUCTS. Dispose of the liquid waste and copper produced in the
experiment as directed by your instructor.
Name _____________________________________ Section ________________________________

Experiment 4

Data and Calculations: Determination of a Chemical Formula

Atomic masses: Copper ______________ Cl ______________ H ______________ O ______________

Mass of crucible ______________ g

Mass of crucible and hydrated sample ______________ g

Mass of hydrated sample ______________ g

Mass of crucible and dehydrated sample ______________ g

Mass of dehydrated sample ______________ g

Mass of filter paper ______________ g

Mass of filter paper and copper ______________ g

Mass of copper ______________ g

No. moles of copper ______________ moles

Mass of water evolved ______________ g

No. moles of water ______________ moles

Mass of chlorine in sample (by difference) ______________ g

No. moles of chlorine ______________ moles

Mole ratio, chlorine:copper in sample ______________ :1

Mole ratio, water:copper in hydrated sample ______________ :1

Formula of dehydrated sample (round to nearest integer) ______________

Formula of hydrated sample ______________

This page intentionally left blank
Name _____________________________________ Section ________________________________

Experiment 4

Advance Study Assignment: Determination of a Chemical Formula

1. To find the mass of a mole of an element, one looks up the atomic mass of the element in a table of atomic
masses (see Appendix III or the Periodic Table). The molar mass of an element is simply the mass in
grams of that element that is numerically equal to its atomic mass. For a compound substance, the molar
mass is equal to the mass in grams that is numerically equal to the sum of the atomic masses in the for-
mula of the substance. Find the molar mass of

Cu ___________ g Cl ___________ g H ___________ g O ___________ g H2O ___________ g

2. If one can find the ratio of the number of moles of the elements in a compound to one another, one can
find the formula of the compound. In a certain compound of copper and oxygen, CuxOy, we find that a
sample weighing 0.5424 g contains 0.4831 g Cu.

a. How many moles of Cu are there in the sample?

⎛ No. moles = mass Cu ⎞

⎝ molar mass Cu ⎠

______________ moles

b. How many grams of O are there in the sample? (The mass of the sample equals the mass of Cu plus
the mass of O.)

______________ g

c. How many moles of O are there in the sample?

______________ moles

d. What is the mole ratio (no. moles Cu/no. moles O) in the sample?

______________ : 1

e. What is the formula of the oxide? (The atom ratio equals the mole ratio, and is expressed using the
smallest integers possible.)

______________

f. What is the molar mass of the copper oxide?

______________ g
This page intentionally left blank
Experiment 5

Identification of a Compound by Mass

Relationships

n the previous experiment we showed how we can find the formula of a compound by analysis for the
I elements it contains. When chemical reactions occur, there is a relationship between the masses of the
reactants and products that follows directly from the balanced equation for the reaction and the molar
masses of the species that are involved. In this experiment we will use this relationship to identify an
unknown substance.
Your unknown will be one of the following compounds, all of which are salts:

NaHCO3 Na2CO3 KHCO3 K2CO3

In the first part of the experiment you will be heating a weighed sample of your compound in a crucible. If
your sample is a carbonate, there will be no chemical reaction that occurs, but any small amount of adsorbed
water will be driven off. If your sample is a hydrogen carbonate, it will decompose by the following reaction,
using NaHCO3 as the example:

2 NaHCO3(s) → Na2CO3(s) + H2O(g) + CO2(g) (1)

In this case there will be an appreciable decrease in mass, since some of the products will be driven off as
gases. If such a mass decrease occurs, you can be sure that your sample is a hydrogen carbonate.
In the second part of the experiment, we will treat the solid carbonate in the crucible with HCl, hydrochlo-
ric acid. There will be considerable effervescence as CO2 gas is evolved; the reaction that occurs is, using
Na2CO3 as our example:

Na2CO3(s) + 2 H+(aq) + 2 Cl−(aq) → 2 NaCl(s) + H2O(l) + CO2(g) (2)

(Since HCl in solution exists as ions, we write the equation in terms of ions.) We then heat the crucible strongly
to drive off any excess HCl and any water that is present, obtaining pure, dry, solid NaCl as our product.
To identify your unknown, you will need to find the molar masses of the possible reactants and final prod-
ucts. For each of the possible unknowns there will be a different relationship between the mass of the original
sample and the mass of the chloride salt that is produced in Reaction 2. If you know your sample is a car-
bonate, you need only be concerned with the mass relationships in Reaction 2, and should use as the original
mass of your unknown the mass of the carbonate after it has been heated. If you have a hydrogen carbonate,
the overall reaction your sample undergoes will be the sum of Reactions 1 and 2.
From your experimental data you will be able to calculate the change in mass that occurred when you
formed the chloride from the hydrogen carbonate or the anhydrous carbonate salt you started with. That dif-
ference divided by the mass of the original salt will be different for each of the possible starting compounds.
Let’s call that quantity Q. Your calculation of the theoretical values of Q should allow to determine the iden-
tity of your unknown. Since you already know whether your compound is a carbonate or a hydrogen carbon-
ate, you need only work with the two possible compounds yours might be.
Exploring the Variety of Random
Documents with Different Content
[369] Dis-creˊ
-tion, prudence.
[370] Ac-comˊ
-plish-ments, attainments.
[371] At-tainˊ
-ing, reaching, obtaining.
[372] Mimˊ
-ic, imitator, counterfeit.
[373] Re-moteˊ
, distant.
[374] Ulˊ
-ti-mate, final.
[375] Suˊ
-per-sede, to set aside.
[376] Ac-qui-siˊ
-tion, acquirement, attainment.
 XLVII.—STABILITY OF CHARACTER.

alison.

1. Stability[377] of character is, in all pursuits, the surest

foundation of success. It is a common error of the indolent[378] and
the imprudent to attribute the success of others to some peculiar
talents, or original superiority of mind, which is not to be found in
the generality of men. Of the falseness of this opinion, the slightest
observation of human life may satisfy us. The difference of talents,
indeed, and the varieties of original character, may produce a
difference in the aims and in the designs of men; and superior minds
will naturally form to themselves superior objects of ambition. But
the attainment of these ends, the accomplishment of these designs,
is, in all cases, the consequence of one means alone—that of
steadfastness and perseverance in pursuit.
2. “It is the hand of the diligent,” saith the wise man, “that maketh
rich.” It is the same diligence, when directed to other ends, that
maketh great. Every thing which we see with admiration in the world
around us, or of which we read with delight in the annals of history
—the acquisitions of knowledge, the discoveries of science, the
powers of art, the glories of arms, the dignities of private, or the
splendors of public virtue—all have sprung from the same fountain
of mind, from that steady but unseen perseverance which has been
exerted in their pursuit. The possession of genius alone, is, alas! no
certain herald of success; and how many melancholy instances has
the world afforded to us all, of how little avail mere natural talents
are to the prosperity of their possessors, and of the frequency with
which they have led to ruin and disgrace, when unaccompanied with
firmness and energy of mind!
3. This stability of character is the surest promise of honor. It
supposes, indeed, all the qualities of mind that are regarded by the
world with respect; and which constitute the honorable and dignified
in human character. It supposes that profound[379] sense of duty,
which we every where look for as the foundation of virtue, and for
the want of which no other attainments can ever compensate.[380] It
supposes a chastened and regulated imagination, which looks ever
to “the things that are excellent,” and which is incapable of being
diverted from their pursuit, either by the intoxications[381] of
prosperous, or the depressions of adverse fortune. It supposes, still
more, a firm and intrepid[382] heart, which neither pleasure has
been able to seduce, nor indolence to enervate,[383] nor danger to
intimidate,[384] and which, in many a scene of trial, and under many
severities of discipline, has hardened itself at last into the firmness
and consistency of virtue.
4. A character of this kind can never be looked upon without
admiration; and wherever we meet it, whether amid the splendors of
prosperity, or the severities of adversity, we feel ourselves disposed
to pay it a pure and an unbidden homage.[385] The display of wild
and unregulated talents may sometimes, indeed, excite a temporary
admiration; but it is the admiration we pay to the useless glare of
the meteor, which is extinguished while it is beheld; while the
sentiment we feel for the steady course of principled virtue, is the
admiration with which we regard the majestic path of the sun, as he
slowly pursues his way, to give light and life to nature.
5. This stability of character is, in another view, the surest
foundation of happiness. There are, doubtless, many ways in which
our happiness is dependent upon the conduct and the sentiments of
others; but the great and perennial[386] source of every man’s
happiness is in his own bosom—in that secret fountain of the heart,
from which the “waters of joy or of bitterness” perpetually flow.
6. It is from this source, the man of steadfast and persevering
virtue derives his peculiar happiness; and the slightest recurrence to
our own experience, can tell us both its nature and its degree. It is
pleasing, we all know, to review the day that is past, and to think
that its duties have been done; to think that the purpose with which
we rose, has been accomplished; that in the busy scene which
surrounds us, we have done our part, and that no temptation has
been able to subdue our firmness and our resolution.
7. Such are the sentiments with which, in every year of life, and
still more in that solemn moment when life is drawing to its close,
the man of persevering virtue is able to review the time that is past.
It lies before him, as it were, in order and regularity; and, while he
travels, over again, the various stages of his progress, memory
restores to him many images to soothe and to animate his heart.
The days of trial are past; the hardships he has suffered, the labors
he has undergone, are remembered no more, but his good deeds
remain, and from the grave of time seem to rise up again to bless
him, and to speak to him of peace and hope.
8. Such are, then, the consequences of firmness and stability of
character; and such the rewards which he may look for, who,
solemnly devoting himself to the discharge of the duties of that
station or condition which Providence has assigned him, pursues
them with steady and undeviating labor. It is the character which
unites all that is valuable or noble in human life, the tranquillity of
conscience, the honors of wisdom, and the dignity of virtue.

[377] Sta-bilˊ
-i-ty, firmness.
[378] Inˊ
-do-lent, lazy, slothful.
[379] Pro-foundˊ
, deep, thorough.
[380] Comˊ
-pen-sate, make amends.
[381] In-toxˊ
-i-caˊ
-tion, inclination.
[382] In-trepˊ
-id, fearless, bold.
[383] Enˊ
-er-vate, to weaken, to deprive of nerve or strength.
[384] In-timˊ
-i-date, to inspire with fear.
[385] Homˊ
-age, reverence, respect.
[386] Per-enˊ
-ni-al, perpetual.
 THE YEAR OF SORROW—IRELAND—
1849.

aubrey de vere.

XLVIII.—SPRING.

1. Once more through God’s high will, and grace

Of hours that each its task fulfills,
Heart-healing Spring resumes her place,
The valley throngs and scales the hills

2. In vain. From earth’s deep heart o’ercharged

The exulting life runs o’er in flowers;
The slave unfed is unenlarged:
In darkness sleep a Nation’s powers.

3. Who knows not Spring? Who doubts, when blows

Her breath, that Spring is come indeed?
The swallow doubts not; nor the rose
That stirs, but wakes not; nor the weed.

4. I feel her near, but see her not;

For these with pain-uplifted eyes
Fall back repulsed, and vapors blot
The vision of the earth and skies.

5. I see her not—I feel her near,

As, charioted in mildest airs,
She sails through yon empyreal sphere,
And in her arms and bosom bears

6. That urn of flowers and lustral dews,

Whose sacred balm, o’er all things shed,
 Revives the weak, the old renews,
And crowns with votive wreaths the dead.

7. Once more the cuckoo’s call I hear;

I know, in many a glen profound,
The earliest violets of the year
Rise up like water from the ground.

8. The thorn I know once more is white;

And, far down many a forest dale,
The anemones in dubious light
Are trembling like a bridal veil.

9. By streams released, that singing flow

From craggy shelf through sylvan glades;
The pale narcissus, well I know,
Smiles hour by hour on greener shades.

10. The honeyed cowslip tufts once more

The golden slopes; with gradual ray
The primrose stars the rock, and o’er
The wood-path strews its milky way.

11. From ruined huts and holes come forth

Old men, and look upon the sky!
The Power Divine is on the earth:
Give thanks to God before ye die!

12. And ye, O children worn and weak!

Who care no more with flowers to play,
Lean on the grass your cold, thin cheek,
And those slight hands, and whispering, say,

13. “Stern Mother of a race unblest,

“In promise kindly, cold in deed,—
“Take back, O Earth, into thy breast,
“The children whom thou wilt not feed.”
 XLIX.—SUMMER.

1. Approved by works of love and might,

The Year, consummated and crowned,
Has scaled the zenith’s purple height,
And flings his robe the earth around.

2. Impassioned stillness—fervors calm—

Brood, vast and bright, o’er land and deep:
The warrior sleeps beneath the palm;
The dark-eyed captive guards his sleep.

3. The Iberian laborer rests from toil;

Sicilian virgins twine the dance;
Laugh Tuscan vales in wine and oil;
Fresh laurels flash from brows of France.

4. Far off, in regions of the North,

The hunter drops his winter fur;
Sun-stricken babes their feet stretch forth;
And nested dormice feebly stir.

5. But thou, O land of many woes!

What cheer is thine? Again the breath
Of proved Destruction o’er thee blows,
And sentenced fields grow black in death.

6. In horror of a new despair

His blood-shot eyes the peasant strains,
With hands clenched fast, and lifted hair,
Along the daily-darkening plains.

7. “Why trusted he to them his store?

“Why feared he not the scourge to come?”
Fool! turn the page of History o’er—
 The roll of Statutes—and be dumb!

8. Behold, O People! thou shalt die!

What art thou better than thy sires?
The hunted deer a weeping eye
Turns on his birthplace, and expires.

9. Lo! as the closing of a book,

Or statue from its base o’erthrown,
Or blasted wood, or dried-up brook,
Name, race, and nation, thou art gone.

10. The stranger shall thy hearth possess;

The stranger build upon thy grave.
But know this also—he, not less
His limit and his term shall have.

11. Once more thy volume, open cast,

In thunder forth shall sound thy name;
Thy forest, hot at heart, at last
God’s breath shall kindle into flame.

12. Thy brook dried up, a cloud shall rise,

And stretch an hourly widening hand,
In God’s good vengeance, through the skies
And onward o’er the Invader’s land.

13. Of thine, one day, a remnant left

Shall raise o’er earth a Prophet’s rod,
And teach the coasts of Faith bereft
The names of Ireland, and of God.
 L.—AUTUMN.

1. Then die, thou Year—thy work is done:

The work ill done is done at last.
Far off, beyond that sinking sun
Which sets in blood, I hear the blast

2. That sings thy dirge, and says—“Ascend,

“And answer make amid thy peers,
“(Since all things here must have an end,)
“Thou latest of the famine years!”

3. I join that voice. No joy have I

In all thy purple and thy gold;
Nor in that nine fold harmony
From forest on to forest rolled:

4. Nor in that stormy western fire,

Which burns on ocean’s gloomy bed,
And hurls, as from a funeral pyre,
A glare that strikes the mountain’s head;

5. And writes on low-hung clouds its lines

Of cyphered flame, with hurrying hand;
And flings amid the topmost pines
That crown the steep, a burning brand.

6. Make answer, Year, for all thy dead,

Who found not rest in hallowed earth;
The widowed wife, the father fled,
The babe age-stricken from his birth

7. Make answer, Year, for virtue lost;

For courage proof ’gainst fraud and force
Now waning like a noontide ghost;
 Affections poisoned at their source.

8. The laborer spurned his lying spade,

The yeoman spurned his useless plow;
The pauper spurned the unwholesome aid,
Obtruded once, exhausted now.

9. The roof-trees fall of hut and hall,

I hear them fall, and falling cry,
“One fate for each, one fate for all;
So wills the Law that willed a lie.”

10. Dread power of Man! what spread the waste

In circles hour by hour more wide,
And would not let the past be past?—
The Law that promised much, and lied.

11. Dread power of God! Whom mortal years

Nor touch, nor tempt; Who sitt’st sublime
In night of night—O bid thy spheres
Resound at last a funeral chime!

12. Call up at last the afflicted race,

Whom man, not God, abolished.—Sore,
For centuries, their strife: the place
That knew them once shall know no more!
 LI.—WINTER.

1. Fall, snow, and cease not! Flake by flake

The decent winding-sheet compose.
Thy task is just and pious; make
An end of blasphemies and woes.

2. Fall flake by flake! by thee alone,

Last friend, the sleeping draught is given:
Kind nurse, by thee the couch is strewn,
The couch whose covering is from heaven.

3. Descend and clasp the mountain’s crest;

Inherit plain and valley deep:
This night on thy maternal breast
A vanquished nation dies in sleep.

4. Lo! from the starry Temple Gates

Death rides, and bears the flag of peace:
The combatants he separates;
He bids the wrath of ages cease.

5. Descend, benignant Power! But O,

Ye torrents, shake no more the vale:
Dark streams, in silence seaward flow:
Thou rising storm, remit thy wail.

6. Shake not, to-night, the cliffs of Moher,

Nor Brandon’s base, rough sea! Thou Isle,
The Rite proceeds! From shore to shore,
Hold in thy gathered breath the while.

7. Fall, snow! in stillness fall, like dew,

On church’s roof and cedar’s fan;
And mold thyself on pine and yew;
 And on the awful face of man.

8. Without a sound, without a stir,

In streets and wolds, on rock and mound,
O, omnipresent Comforter,
By Thee, this night, the lost are found!

9. On quaking moor, and mountain moss,

With eyes upstaring at the sky,
And arms extended like a cross,
The long-expectant sufferers lie.

10. Bend o’er them, white-robed Acolyte!

Put forth thine hand from cloud and mist;
And minister the last sad Rite,
Where altar there is none, nor priest.

11. Touch thou the gates of soul and sense;

Touch darkening eyes and dying ears;
Touch stiffening hands and feet, and thence
Remove the trace of sin and tears.

12. And ere thou seal those filmed eyes,

Into God’s urn thy fingers dip,
And lay, ’mid eucharistic sighs,
The sacred wafer on the lip.

13. This night the Absolver issues forth:

This night the Eternal Victim bleeds:
O winds and woods—O heaven and earth!
Be still this night. The Rite proceeds!
 LII.—DEATH OF LITTLE NELL.

dickens.

1. By little and little, the old man had drawn back towards the
inner chamber. He pointed there, as he replied, with trembling lips,
“You plot among you to wean my heart from her. You will never do
that—never while I have life. I have no relative or friend but her—I
never had—I never will have. She is all in all to me. It is too late to
part us now.”
2. Waving them off with his hand, and calling softly to her as he
went, he stole into the room. They who were left behind drew close
together, and after a few whispered words, not unbroken by
emotion, or easily uttered, followed him. They moved so gently that
their footsteps made no noise; but there were sobs from among the
group, and sounds of grief and mourning. For she was dead.
3. There, upon her little bed, she lay at rest. The solemn stillness
was no marvel now. She was dead. No sleep so beautiful and calm,
so free from trace of pain, so fair to look upon. She seemed a
creature fresh from the hand of God, and waiting for the breath of
life; not one who had lived and suffered death.
4. Her couch was dressed with, here and there, some winter
berries and green leaves, gathered in a spot she had been used to
favor. “When I die, put near me something that has loved the light,
and had the sky above it always.” These were her words.
5. She was dead! Dear, gentle, patient, noble Nell was dead. Her
little bird—a poor slight thing the pressure of a finger would have
crushed—was stirring nimbly in its cage; and the strong heart of its
child-mistress was mute and motionless for ever!
6. Where were the traces of her early cares, her sufferings and
fatigues? All gone. His was the true death before their weeping eyes.
Sorrow was dead indeed in her, but peace and perfect happiness
were born; imaged in her tranquil beauty and profound repose.
7. And still her former self lay there, unaltered in this change. Yes.
The old fireside had smiled on that same sweet face; it had passed
like a dream through haunts of misery and care; at the door of the
poor schoolmaster on the summer evening, before the furnace fire,
upon the cold, wet night, at the still bed-side of the dying boy, there
had been the same mild, lovely look. So shall we know the angels in
their majesty, after death.
8. The old man held one languid arm in his, and kept the small
hand tightly folded to his breast, for warmth. It was the hand she
had stretched out to him with her last smile—the hand that had led
him on through all their wanderings. Ever and anon he pressed it to
his lips; then hugged it to his breast again, murmuring that it was
warmer now; and as he said it, he looked, in agony, to those who
stood around, as if imploring them to help her.
9. She was dead, and past all help, or need of it. The ancient
rooms she had seemed to fill with life, even while her own was
ebbing fast—the garden she had tended—the eyes she had
gladdened—the noiseless haunts of many a thoughtless hour—the
paths she had trodden as it were but yesterday—could know her no
more.
10. “It is not,” said the schoolmaster, as he bent down to kiss her
on the cheek, and gave his tears free vent, “it is not in this world
that Heaven’s justice ends. Think what it is compared with the world
to which her young spirit has winged its early flight, and say, if one
deliberate wish, expressed in solemn terms above this bed, could call
her back to life, which of us would utter it!”
11. When morning came, and they could speak more calmly on
the subject of their grief, they heard how her life had closed. They
were all about her at the time, knowing that the end was drawing
on. She died soon after daybreak. They had read and talked to her
in the earlier portion of the night; but as the hours crept on, she
sank to sleep. They could tell, by what she faintly uttered in her
dreams, that they were of her journeyings with the old man; they
were of no painful scenes, but of those who had helped and used
them kindly, for she often said “God bless you!” with great fervor.
Waking, she never wandered in her mind but once, and that was at
beautiful music which she said was in the air. It may have been.
12. Opening her eyes at last, from a very quiet sleep she begged
that they would kiss her once again. That done, she turned to the
old man with a lovely smile upon her face—such, they said, as they
had never seen, and never could forget—and clung with both her
arms about his neck. They did not know that she was dead at first.
For the rest, she had never murmured or complained; but with a
quiet mind, and manner quite unaltered—save that she every day
became more earnest and more grateful to them—faded like the
light upon the summer’s evening.
13. And now the bell—the bell she had so often heard by night
and day, and listened to with solemn pleasure, almost as a living
voice—rung its remorseless tone for her, so young, so beautiful, so
good. Decrepit age, and vigorous life, and blooming youth, and
helpless infancy poured forth—on crutches, in the pride of strength
and health, in the full blush of promise, in the mere dawn of life; to
gather round her with angels; and when they called to mind how
she had looked, and spoken, and her early death, some thought it
might be so indeed. Thus coming to the grave in little knots, and
glancing down, and giving place to others, and falling off in
whispering groups of three or four, the church was cleared in time of
all but the sexton and the mourning friends.
14. They saw the vault covered and the stone fixed down. Then,
when the dusk of evening had come on, and not a sound disturbed
the sacred stillness of the place—when the bright moon poured in
her light on tomb and monument, on pillar, wall, and arch, and most
of all (it seems to them) upon her quiet grave—in that calm time,
when all outward things and inward thoughts teem with assurances
of immortality, and worldly hopes and fears are humbled in the dust
before them, then, with tranquil and submissive hearts, they turned
away, and left the child with God.
 LIII.—SORROW FOR THE DEAD.

washington irving.

1. The sorrow for the dead is the only sorrow from which we
refuse to be divorced.[387] Every other wound we seek to heal, every
other affliction to forget; but this wound we consider it a duty to
keep open; this affliction we cherish and brood over in solitude.
Where is the mother who would willingly forget the infant that
perished like a blossom from her arms, though every recollection is a
pang? Where is the child that would willingly forget the most tender
of parents, though to remember be but to lament?
2. Who, even in the hour of agony, would forget the friend over
whom he mourns? Who, even when the tomb is closing upon her he
most loved—when he feels his heart, as it were, crushed in the
closing of its portals—would accept of consolation that must be
bought by forgetfulness?
3. No, the love which survives the tomb is one of the noblest
attributes of the soul. If it has its woes, it has likewise its delights;
and when the overwhelming burst of grief is calmed into the gentle
tear of recollection, when the sudden anguish and the convulsive
agony over the present ruins of all that we most loved, is softened
away into pensive meditation on all that it was in the days of its
loveliness, who could root out such a sorrow? Though it may
sometimes throw a passing cloud over the bright hour of gayety, or
spread a deeper sadness over the hour of gloom, yet who would
exchange it, even for the song of pleasure, or the burst of revelry?
4. No, there is a voice from the tomb sweeter than song. There is
a remembrance of the dead to which we turn even from the charms
of the living. Oh! the grave! It buries every error, covers every
defect, extinguishes every resentment! From its peaceful bosom
spring none but fond regrets and tender recollections. Who can look
down even upon the grave of an enemy, and not feel a
compunctious[388] throb, that he should ever have warred with the
poor handful of earth that lies moldering before him!
5. But the grave of those we loved, what a place of meditation!
There it is that we call up in long review the whole history of virtue
and gentleness, and the thousand endearments lavished upon us,
almost unheeded in the daily intercourse of intimacy; there it is that
we dwell upon the tenderness, the solemn, awful tenderness of the
parting scene; the bed of death, with all its stifled griefs, its
noiseless attendance, its mute watchful assiduities.
6. The last testimonies of expiring love! the feeble, fluttering,
thrilling, oh! how thrilling! pressure of hand! The faint, faltering
accents, struggling in death to give one more assurance of affection!
The last fond look of the glazing eye, turning upon us even from the
threshold of existence! Ay, go to the grave of buried love, and
meditate. There settle the account with thy conscience for every
past benefit unrequited[389], every past endearment unregarded, of
that departed being, who can never, never, never return to be
soothed by thy contrition.
7. If thou art a child, and hast ever added a sorrow to the soul, or
a furrow to the silvered brow of an affectionate parent; if thou art a
husband, and hast ever caused the fond bosom that ventured its
whole happiness in thy arms, to doubt one moment of thy kindness
or thy truth; if thou art a friend, and hast ever wronged in thought,
or word, or deed, the spirit that generously confided in thee; if thou
art a lover, and hast ever given one unmerited pang to that true
heart which now lies cold and still beneath thy feet;—then be sure
that every unkind look, every ungracious word, every ungentle
action, will come thronging back to thy memory, and knock dolefully
at thy soul; then be sure that thou wilt lie down sorrowing and
repentant in the grave, and utter the unheard groan, and pour the
unavailing tear, more deep, more bitter, because unheard and
unavailing.
 8. Then weave thy chaplet of flowers, and strew the beauties of
Nature about the grave, console thy broken spirit, if thou canst, with
these tender, yet futile[390] tributes of regret; but take warning by
the bitterness of this thy contrite[391] affliction over the dead, and
henceforth be more faithful and affectionate in the discharge of thy
duties to the living.

[387] Di-vorcedˊ
, disunited or separated.
[388] Com-punc-tious, repentant; sorrowful.
[389] Unˊ
-re-quited, not repaid; not done or given in return.
[390] Fuˊ
-tile, trifling; worthless.
[391] Conˊ
-trite, sorrowful; bowed down with grief.
 LIV.—ISABELLA THE CATHOLIC,
QUEEN OF SPAIN.

prescott.
William H. Prescott was born in Salem, Mass., May 4th, 1796,
and died in Boston, January 28 1859. His historical and
biographical works, published in fifteen octavo volumes, have
enjoyed a wide and deserved popularity; although in many
instances marred by views and statements, which seem to betray
a mind warped by religious prejudice. In his edition of Robertson’s
“History of the Emperor Charles V.” he has permitted some of the
most glaring errors of that writer to pass uncorrected, although
Maitland, in his admirable work entitled “The Dark Ages,” had very
clearly and conclusively exposed them.

1. Her person was of the middle height, and well proportioned.

She had a clear, fresh complexion, with light blue eyes and auburn
hair, a style of beauty exceedingly rare in Spain. Her features were
regular, and universally allowed to be uncommonly handsome.
2. The illusion which attaches to rank, more especially when
united with engaging manners, might lead us to suspect some
exaggeration in the encomiums[392] so liberally lavished on her. But
they would seem to be in a great measure justified by the portraits
that remain of her, which combine a faultless symmetry[393] of
features, with singular sweetness and intelligence of expression.
3. Her manners were most gracious and pleasing. They were
marked by natural dignity and modest reserve, tempered by an
affability[394] which flowed from the kindliness of her disposition.
She was the last person to be approached with undue familiarity; yet
the respect which she imposed was mingled with the strongest
feelings of devotion and love.
 4. She showed great tact in accommodating herself to the peculiar
situation and character of those around her. She appeared in arms at
the head of her troops, and shrunk from none of the hardships of
war. During the reforms introduced into the religious houses, she
visited the nunneries[395] in person, taking her needle-work with her,
and passing the day in the society of the inmates. When traveling in
Galicia,[396] she attired herself in the costume of the country,
borrowing for that purpose the jewels and other ornaments of the
ladies there, and returning them with liberal additions. By this
condescending and captivating deportment, as well as by her higher
qualities, she gained an ascendency[397] over her turbulent[398]
subjects, which no king of Spain could ever boast.
5. She spoke the Castilian[399] with much elegance and
correctness. She had an easy fluency of discourse, which, though
generally of a serious complexion, was occasionally seasoned with
agreeable sallies, some of which have passed into proverbs. She was
temperate, even to abstemiousness,[400] in her diet, seldom or
never tasting wine: and so frugal in her table, that the daily
expenses of herself and family did not exceed the moderate sum of
forty ducats.[401]
6. She was equally simple and economical in her apparel. On all
public occasions, indeed, she displayed a royal magnificence;[402]
but she had no relish for it in private, and she freely gave away her
clothes and jewels, as presents to her friends.
7. Naturally of a sedate, though cheerful temper, she had little
taste for the frivolous amusements which make up so much of a
court life; and, if she encouraged the presence of minstrels and
musicians in her palace, it was to wean her young nobility from the
coarser and less intellectual pleasures to which they were addicted.
8. Among her moral qualities, the most conspicuous, perhaps, was
her magnanimity.[403] She betrayed nothing little or selfish, in
thought or action. Her schemes were vast, and executed in the same
noble spirit in which they were conceived. She never employed
doubtful agents, or sinister measures, but the most direct and open
policy. She scorned to avail herself of advantages offered by the
perfidy[404] of others.
9. Where she had once given her confidence, she gave her hearty
and steady support: and she was scrupulous to redeem any pledge
she had made to those who ventured in her cause, however
unpopular. She sustained Ximenes[405] in all his obnoxious[406] but
salutary reforms. She seconded Columbus in the prosecution of his
arduous enterprise, and shielded him from the calumny[407] of his
enemies. She did the same good service to her favorite, Gonsalvo de
Cordova;[408] and the day of her death was felt, and, as it proved,
truly felt, by both, as the last of their good fortune.
10. Artifice[409] and duplicity[410] were so abhorrent to her
character, and so averse from her domestic policy, that when they
appear in the foreign relations of Spain, it is certainly not imputable
to her. She was incapable of harboring any petty distrust, or latent
malice; and, although stern in the execution and exaction of public
justice, she made the most generous allowance, and even,
sometimes, advances, to those who had personally injured her.
11. But the principle which gave a peculiar coloring to every
feature of Isabella’s mind, was piety. It shone forth from the very
depths of her soul with a heavenly radiance, which illuminated her
whole character. Fortunately, her earliest years had been passed in
the rugged school of adversity, under the eye of a mother who
implanted in her serious mind such strong principles of religion, as
nothing in after life had power to shake.
12. At an early age, in the flower of youth and beauty, she was
introduced to her brother’s court; but its blandishments,[411] so
dazzling to a young imagination, had no power over hers; for she
was surrounded by a moral atmosphere of purity, “driving far off
each thing of sin and guilt.” Such was the decorum of her manners,
that, though encompassed by false friends and open enemies, not
the slightest reproach was breathed on her fair name in this corrupt
and calumnious[412] court.

[392] En-coˊ
-mi-um, a high commendation; praise.
[393] Sym ˊ-me-try, a due proportion of the parts of a body to
each other.
[394] Af-fa-bil ˊ-i-ty, easiness of approach; readiness to
converse.
[395] Nun ˊ-ne-ry, a religious house for females who have
forsaken the world.
[396] Gal-iˊ
-cia, an old province of Spain.
[397] As-cendˊ
-en-cy, superior or controlling influence.
[398] Turˊ
-bu-lent, riotous; violent; mutinous.
[399] Cas-til ˊ-ian, the language spoke in Castile, considered the
most elegant dialect of Spain.
[400] Ab-steˊ
-mi-ous-ness, a sparing use of food, or strong drink.
[401] Duc ˊ-at, a coin of several countries in Europe, struck in
territory governed by a duke. A silver ducat is generally of nearly
the value of an American dollar, and a gold ducat of twice the
value.
[402] Mag-nif ˊ-i-cence, grandeur of appearance; splendor of
show or state.
[403] Mag-na-nimˊ
-i-ty, greatness of mind; dignity or elevation of
soul, which meets danger with calmness and firmness, which
raises the possessor above revenge, which makes him hate
injustice and meanness, and moves him to act and suffer for
noble objects.
[404] Perˊ
-fi-dy, treachery; falsehood.
[405] Cardinal Xi-me ˊ-nes, born 1437, died 1517. He was a
distinguished ecclesiastic, and a great statesman.
[406] Ob-noxˊ
-ious, odious; unpopular.
[407] Calˊ
-um-ny, the uttering of a false charge, proceeding from
hatred against another.
[408] Gonsalvo de Cordova, called also “the Great Captain,” was
a Spanish warrior, distinguished by his victories over the Moors in
Spain, and the French in Naples. Born 1443, died 1515.
[409] Arˊ
-ti-fice, an artful or skillful contrivance; a fraud or trick.
[410] Du-plicˊ
-i-ty, double-dealing; deceitfulness.
[411] Blandˊ
-ish-ment, words or actions expressive of affection or
kindness, and tending to win the heart, or to flatter.
[412] Ca-lumˊ
-ni-ous, slanderous.
 LV.—PALESTINE.

altered from whittier.

John Greenleaf Whittier is a well-known and popular writer in
prose and verse.

1. Blest land of Judea! thrice hallowed of song,

Where the holiest of memories, pilgrim-like, throng
In the shade of thy palms, by the shores of thy sea,
On the hills of thy beauty—my heart is with thee.
With the eye of a spirit I look on that shore,
Where pilgrim and prophet have lingered before;
With the guide of a spirit I traverse the sod
Made bright by the steps of the angels of God.

2. Blue sea of the hills! in my spirit I hear

Thy waters, Gennesaret[413], chime on my ear;
Where the Lowly and Just with the people sat down,
And thy spray on the dust of His sandals was thrown.
Beyond are Bethulia’s[414] mountains of green,
And the desolate hills of the wild Gadarene[415];
And I pause on the goat-crags of Tabor[416] to see
The gleam of thy waters, O dark Galilee!

3. There sleep the still rocks and the caverns which rang
To the song which the beautiful prophetess sang,
When the princes of Issachar[417] stood by her side,
And the shout of a host in its triumph replied.
Lo! Bethlehem’s[418] hill-site before me is seen,
With the mountains around and the valleys between;
There rested the shepherds of Judah[419], and there,
The song of the angels rose sweet on the air.
4. And Bethany’s[420] palm trees in beauty still throw
Their shadows at noon on the ruins below;
But where are the sisters who hastened to greet
The lowly Redeemer, and sit at his feet?
I tread where the Twelve in their wayfaring trod;
I stand where they stood with the Incarnate God;
Where his blessing was heard, and his lessons were taught;
Where the blind were restored, and the healing was wrought.

[413] Gen-nes ˊ-a-ret, a sea or lake in Palestine, the borders of

which, in the time of Christ, were covered with numerous towns
and villages; called also, Sea of Galilee.
[414] Beth-u-li ˊ-a, a city which appears to have overlooked the
plain of Esdraelon, and to have guarded one of the passes to
Jerusalem.
[415] Gad-a-rene ˊ, an inhabitant of Gadara, a city in a
mountainous region near the Sea of Galilee.
[416] Ta ˊ-bor, an isolated mountain, of a conical form, a few
miles southwest of the Sea of Galilee.
[417] Is ˊ-sa-char, a son of Jacob and Leah; also, the tribe
named after him.
[418] Bethˊ
-le-hem, the city where Our Lord was born.
[419] Juˊ-dah, the name of one of the tribes of Israel, afterwards
applied to the whole nation.
[420] Bethˊ
-a-ny, a town near Jerusalem the residence of Martha
and Mary.
 LVI.—LOVE OF COUNTRY AND OF
HOME.

montgomery.

1. There is a land, of every land the pride,

Beloved by heaven o’er all the world beside;
Where brighter suns dispense[421] serener[422] light,
And milder moons imparadise[423] the night:
A land of beauty, virtue, valor, truth,
Time-tutored age, and love-exalted youth.

2. The wandering mariner, whose eye explores

The wealthiest isles, the most enchanting shores,
Views not a realm so bountiful and fair,
Nor breathes the spirit of a purer air;
In every clime, the magnet[424] of his soul,
Touched by remembrance, trembles to that pole:

3. For in this land of heaven’s peculiar grace,

The heritage[425] of nature’s noblest race,
There is a spot of earth supremely[426] blest,
A dearer, sweeter pot than all the rest,
Where man, creation’s tyrant, casts aside
His sword and scepter, pageantry and pride,
While, in his softened looks, benignly[427] blend
The sire, the son, the husband, father, friend.

4. Here woman reigns; the mother, daughter, wife,

Strews with fresh flowers the narrow way of life;
In the clear heaven of her delightful eye,
An angel guard of loves and graces lie;
Around her knees domestic duties meet,
And fireside pleasures gambol[428] at her feet.
Where shall that land, that spot of earth be found?
Art thou a man? a patriot?[429] look around;
Oh! thou shalt find, howe’er thy footsteps roam,
That land thy country, and that spot thy home.

[421] Dis-pense ˊ, deal or divide out in portions or parts;

distribute.
[422] Se-renˊ
-er, clearer; more soothing.
[423] Im-parˊ
-a-dise, make very happy; render like Paradise.
[424] Magˊ
-net, the loadstone; that which attracts.
[425] Her ˊ-it-age, inheritance; portion; an estate devolved by
succession.
[426] Su-premeˊ
-ly, in the highest degree.
[427] Beˊ
-nignˊ
-ly, graciously; kindly.
[428] Gam ˊ
-bol, dance and skip about in sport; play in frolic, like
boys and lambs.
[429] Pa ˊ-tri-ot, a person who loves his country, and zealously
supports and defends it and its interests.
 LVII.—THE HEAVENLY REST.

anon.

1. There is an hour of peaceful rest

To mourning wanderers given,
There is a tear for souls distrest,
A balm for every wounded breast—
’Tis found above—in heaven!

2. There is a soft, a downy bed,

’Tis sweet as breath of even;
A couch for weary mortals spread,
Where they may rest the aching head,
And find repose in heaven!

3. There is a home for weary souls,

By sin and sorrow driven,
When tossed on life’s tempestuous shoals
Where storms arise, and ocean rolls,
And all is drear—but heaven!

4. There faith lifts up the tearful eye,

The heart with anguish riven;
And views the tempest passing by,
The evening shadows quickly fly,
And all serene in heaven!

5. The fragrant flowers immortal bloom.

And joys supreme are given;
There rays divine disperse the gloom:
Beyond the confines of the tomb
Appears the dawn of heaven!
 LVIII.—LOVE OF COUNTRY.

scott.

1. Breathes there the man, with soul so dead

Who never to himself hath said,
“This is my own, my native land!”
Whose heart has ne’er within him burned,
As home his footsteps he hath turned,
From wandering on a foreign strand?
If such there breathe, go, mark him well;
For him no minstrel raptures swell.

2. High though his titles, proud his name,

Boundless his wealth as wish can claim;
Despite those titles, power, and pelf,
The wretch, concentrated all in self,
Living, shall forfeit fair renown;
And, doubly dying, shall go down
To the vile dust from which he sprung,
Unwept, unhonored, and unsung.

3. O Caledonia! stern and wild,

Meet nurse for a poetic child,
Land of brown heath and shaggy wood,
Land of the mountain and the flood.
Land of my sires; what mortal hand
Can e’er untie the filial band
That knits me to thy rugged strand!
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