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LABORATORY MANUAL

FOR

CHM 110
(GENERAL CHEMISTRY I)
INSTRUCTOR:

DEPARTMENT OF PHYSICAL SCIENCES


1

College Chemistry I

Laboratory Manual

Glenn Ivett

Trident Technical College

Contents
Page
Introduction

Laboratory Safety Rules


Laboratory Equipment

..

Material Safety Data Sheets

Periodic Chart of the Elements

10

12

13

14

Table of Atomic Weights


Solubility Table

Laboratory Experiment 1

Mass and Volume Determination .

15

Laboratory Experiment 2

Density Determination ..

20

Laboratory Experiment 3

Mixture Separation

28

Laboratory Experiment 4

Determination of a Formula

32

Laboratory Experiment 5

Stoichiometry: Gas Evolution Reaction

37

Laboratory Experiment 6

Stoichiometry: Precipitation Reaction

42

Laboratory Experiment 7

Molecular Structures and Shapes .

47

Page

Laboratory Experiment 8

Molar Mass of a Volatile Liquid ..

56

Laboratory Experiment 9 Freezing-Point Depression .

60

Laboratory Experiment 10 Solution Stoichiometry: Acid-Base Standardization

65

Laboratory Experiment 11 Acid/Base Titration: Solution Analyses

70

Appendix I Laboratory Practical Test Study Guide .

74

INTRODUCTION
This laboratory manual contains appropriate information for all of the experiments in your College
Chemistry I Course, as well as general information on conduct and safety in the laboratory and
guidelines on the format of laboratory reports and notebook entries.
For ease of handling, the handouts for each experiment are ordered in the correct sequence and
are punched and perforated. The final page of the handout for each experiment is a prelaboratory question sheet which must be completed before arrival at the laboratory and handed to
the laboratory instructor upon arrival. Your instructor may also give quizzes about the laboratory
experiment.

LABORATORY REPORTS
For all laboratory experiments, a report must be submitted to your instructor by the next
laboratory session. In the commercial world in many cases a simple outline of data with
accompanying calculations may be all that is required, however in some instances perhaps a
more formal report would be necessary. Therefore during this laboratory course students will be
required to submit both types of reports. The type of report required for each experiment will be
assigned by the instructor.

FORMAL REPORT: A formal report should be typed. A general guideline for this kind of
report is:

1.

Objective ...............................

A BRIEF statement of the aim of the experiment

2.

Materials/Equipment..............

A list of materials and/or equipment which are specific to the


experiment (i.e., non-drawer items)

3.

Procedure ..............................

A BRIEF outline of the conduct of the experiment, avoiding


references to exact amounts if possible

4.

Measurements/Observations

Raw data obtained during the experiment transcribed from lab


notebook onto data sheets provided.

5.

Calculations ...........................

6.

Results ..................................

A SAMPLE of each type of calculation used in the


experiment.
A summary of the results of calculations performed on the
raw data, using the data sheets provided at the end of this
manual.

7.

Discussion .............................

A comparison of experimental results with theoretical, or


handbook values. Answers to post-lab questions should be
attached to the end of the report.

This is only a general guide and it is at your instructor's discretion to decide on the exact required
format.

INFORMAL REPORTS: Using the data sheets provided at the end of this manual, transcribe
data, perform calculations and complete the results section. Write a paragraph in the Discussion
section of the data sheet which discusses the significance of the results. Additionally answer the
post-lab questions. These reports do not have to be typed, but presentation is important and ,
therefore, handwriting MUST be in INK and LEGIBLE.

LABORATORY NOTEBOOKS
All students MUST possess a bound (non-spiral) notebook, such as an English composition book,
into which all measurements and observations taken in the laboratory must be recorded IN INK.
The results of calculations using this raw data must also be recorded in ink in the notebook.
Carbon copies are not required.

LABORATORY PRACTICAL TEST


The laboratory practical test is a written examination conducted on completion of all the laboratory
experiments. It will contain questions on: laboratory techniques and procedures; the theoretical
principles on which the laboratory experiments are based; and examples of the calculations
performed to obtain results from raw data.

LABORATORY GRADES
The laboratory grade constitutes 25% of the overall course grade. The laboratory practical test
counts as 25% of the laboratory grade. The remainder will be assessed on the basis of
performance on pre-laboratory questions and laboratory reports and proper maintenance of a
laboratory notebook .

ABSENCES
Absences from laboratory sessions cannot be made up except by attending a laboratory session
with another section of the course. However, attendance with another section is only possible IF
there is a space available and that instructor agrees to accept another student.
Your instructor may drop your lowest grade if all laboratory reports are submitted, so that it is
possible to be absent for one laboratory session, but this is at your instructor's discretion.
If you are absent for the laboratory practical test, no make-up test is available.

MATERIALS AND EQUIPMENT


During check-in, you and your laboratory partner will check your designated drawer/locker to
ensure that the listed equipment is present. Try to ensure that all of this equipment is maintained
and glassware is clean. Extra equipment should be returned to your laboratory instructor. Note
that your drawer/locker will be used by other students; therefore, you should not keep personal
items, including laboratory aprons and safety glasses, in it.
Extra equipment for particular experiments can be found on the trolleys or the instructor's bench.
There are mass balances in each laboratory. Chemicals which are volatile and/or pungent will be
found, and must remain, in the main fume cupboard. Students are reminded that every
workstation has its own fume hood.

LABORATORY SAFETY RULES


1. Approved eye protection must be worn at all times.
Eyewear can be safety glasses or prescription glasses with side shields. Contact lenses should not be
worn, even with safety goggles. They make it difficult to rinse chemical splashes from the eye. Vapors
in the laboratory (hydrochloric acid, for example) dissolve in the liquids covering the eye and
concentrate behind the lenses. Soft lenses are especially bad as chemicals dissolve in the lenses
themselves and are released over several hours.
2. Appropriate clothing must be worn in the lab.
Because of the danger of chemical splashes/spills, clothing should cover the body. Sandals, canvas
shoes and shorts are not allowed. It is also suggested that a coat or long/large shirt be worn in order to
provide a layer of clothing that can be removed in case of an accident. Material Safety Data Sheets are
available and provide information on each chemical you will be using. Know where they are kept.
3. Bunsen burner use requires caution.
Some experiments will require the use of the bunsen burner and special care must be taken. Long hair
should be tied back and loose clothing secured.
4. Good housekeeping habits promote safety.
A cluttered lab bench invites an accident to occur. Keep all unnecessary books, etc., away from your
work area. Make sure you clean up any mess on your lab bench or at the balance table. Wash your
hands before you leave the lab.
5. Eating, drinking or smoking are not permitted.
Avoid placing objects in your mouth while in the lab. Your fingers or your pencil may have come into
contact with a chemical that should not be ingested.
6. Be familiar with the location of safety equipment.
Each lab is provided with safety showers, eye washes, spill kits, first aid kits, fire extinguishers and
fire blankets. There is a telephone next to the elevator that is a direct connection to the Public Safety
Office.
7. Only authorized experiments are allowed.
8. No one is allowed in lab without instructor or designee being present.
9. No children or animals allowed in the laboratory.
For your safety, if you have a medical condition that results in seizures, blackouts, etc. (e.g., from
epilepsy or diabetes), please inform your instructor. This information will be kept confidential. If you
wish to seek accommodations due to a disability, please contact Services for Students with Disability,
Building 410, Room 210.
I understand that safety MUST come first in the laboratory. My signature below indicates that I have read
the above rules, understand why they are important, and agree to abide by them.
Name (Print): ______________________________ Course: _______________________
Signature: ________________________________ Date: _________________________

LABORATORY EQUIPMENT
TRAY

DRAWER

CABINET

Scoopula

Beakers (5):

Burner

Dropper

30 mL, 50 mL, 100 or 150 mL,

Burner tubing

Watch glass

250 mL, 400 or 600 mL

Iron ring

Marking pencil

Erlenmeyer flasks (2):

Clamp

Crucible

125 mL and 250 mL

Wire gauze

Crucible lid

Graduated cylinders (3):

Clay triangle

Evaporating dish

10mL, 25 or 50 mL, 100 mL

Stirring rod

Funnel
Crucible tongs
Test tube rack
Test tubes (8) 16 x 150 mm

1. At the first laboratory session, wash all glassware.


2. At the end of each lab, clean any glassware and materials used, wipe the benchtop clean
and dry, and clean out the sink. Lab areas which are not cleaned may result in points
being deducted from your lab grade.
3. If materials are broken or disappear during the semester, report this to your instructor
who will provide a replacement.
4. The cabinet is not your own. Other students in other laboratory sessions will be using
your cabinet. DO NOT leave personal items and materials in the cabinets. If you find on
arrival in the laboratory that your cabinet or glassware is in an undesirable condition,
report this to your instructor.
6. At the last lab session of the semester, make sure that all glassware and supplies are
clean, and that all broken or missing materials are replaced. The instructor will inspect
your cabinet before you leave the laboratory for the final time.

MATERIAL SAFETY DATA SHEETS


A.

What are they? A Material Safety Data Sheet or MSDS is an information sheet provided
by the manufacturer of a chemical.

B.

What can they tell me? An MSDS has valuable information on how to use, handle and
store chemicals in your work area. They also provide information on health hazards
associated with the use of the chemical, precautionary measures to follow, and the
emergency procedures for spills, fire and first aid.

C.

Why do we have them? The Federal Right-To-Know laws mandate that any employee
working with a chemical has the right to information about the risks and hazards of
working with that substance. Although you are not employees, Trident Technical college
feels that students working in laboratory settings should have access to information about
the materials they use.

D.

How do I use them? Although MSDS' may vary in appearance and length, most will have
eight to ten sections, usually organized in the following order:
1.

Chemical Identification:
formula.

Includes chemical name, trade name and chemical

2.

Hazardous Ingredients: Lists any hazardous ingredients found within the chemical
or mixture. You may also see the terms TLV (Threshold Limit Value) and PEL
(Permissible Exposure Limit). Both terms are used to express the airborne
concentration levels of a chemical to which most persons can safely be exposed
during a normal workday.

3.

Physical Data: Lists such physical properties as boiling points, appearance, odor,
and vapor density.

4.

Fire and Explosion Data: Provides information on whether this chemical will burn
and if there is a fire, how it is put out. A chemical's flash point (the temperature at
which a chemical will release enough flammable vapor to ignite) is included.
Chemicals that ignite at or above 100 oF are classified as combustible; those that
ignite below 100 oF are classified as flammable.

5.

Health Hazard Data: Describes health effects associated with being exposed to
the chemical through ingestion, inhalation and skin or eye contact. The
information may include: the acute (immediate) and chronic (long-term) effects of
exposure, whether the chemical is a known carcinogen (cancer-causing agent),
and emergency and first aid procedures to follow in case of exposure.

6.

Reactivity Data: Provides information on whether the chemical will react with other
chemicals or conditions. Chemicals that are reactive (unstable) may explode,
burn, or release toxic substances under certain conditions.

7.

Spill or Leak Procedures: Describes the procedures to follow when the chemical is
accidentally released or spilled.

10

E.

8.

Special Protection:
Lists type of special protective equipment that is
recommended to be used when working with the chemical.

9.

Special Precaution: Includes special precautions regarding handling and storage


of the chemical.

Where are they? MSDS' are kept in black and yellow striped binders with "MSDS" printed
on the spine. They are located in the prep room between labs 314 and 310. Since
students are not allowed in the prep room, please ask your instructor to get them for you if
you are interested in more information about a chemical. (MSDS' for chemicals used in lab
307 are maintained on the bookshelf in that room.)

The Chemical Hygiene Officer for this area is the Physical Sciences department Lab Manager.

11

12

13

Solubility Table

1-

1-

2-

1-

2-

C2H3O2

Br

CO3

Cl

CrO4

OH

1+

2+

2+

Co

2+

Cu

2+

1-

1-

2-

NO3

C2O4

2+

3+

2+

2+

3-

2-

2-

SO4

1+

1+

2+

3+

NH4
Ba
Ca

Fe
Fe

Pb

Mg

1+

Ag
Na
Zn

2-

PO4

Al

1-

Key: S = Soluble in water


s = Slightly soluble in water

I = Insoluble in water (less than 1 g/100 g H2O)


d = Decomposes in water

14

EXPERIMENT

Mass and Volume


Determination

OBJECTIVE:
Familiarity with the various instruments used for making physical measurements in the
laboratory is essential to the study of experimental chemistry. In this experiment you will
investigate the uses and limits of the laboratory balances and of the various types of
volumetric glassware.

INTRODUCTION:

Mass Determination:
The accurate determination of mass is one of the most fundamental techniques for students
of experimental chemistry. Mass is a direct measure of the amount of matter in a sample of
substance. That is, the mass of a sample is a direct indication of the number of atoms or
molecules the sample contains. Since chemical reactions occur in proportion to the number
of atoms or molecules of reactant present, it is essential that the mass of reactant used in a
process be accurately known.
There are various types of balances available in the typical general chemistry laboratory.
They differ in construction, appearance, operation and in the level of precision they permit in
mass determinations.
No matter what type of balance you use there are some general points to keep in mind when
using any balance:
1. Always make sure that the balance gives a reading of 0.000 grams when nothing is present
on the balance pan.
2. All balances, but especially electrical/electronic balances, are damaged by moisture. Do not
pour liquids in the immediate vicinity of the balance and clean up any spills immediately.
3. No reagent chemical substance should ever be weighed directly on the pan of the balance.
Ideally, reagents should be weighed directly into the beaker or flask in which they are to be
used. Plastic weighing boats or weighing paper may be used if several reagents are
required for an experiment.
4. Procedures in this manual are generally written in such terms as "weigh 0.5 grams of a
substance (to the nearest milligram)." This does not mean that exactly 0.500 grams of
substance is needed. Rather, the statement means to obtain an amount of substance
between 0.450 and 0.550 grams (within 10% of the indicated amount), but to record the
actual amount of substance taken to the nearest .001 g (e.g., 0.496 grams).

15

Unless a procedure states explicitly to weigh out an exact amount (e.g., "weigh out exactly
5.00 grams of NaCl"), you should not waste time trying to obtain an exact amount.
However, always record the amount actually taken to the precision of the balance used.
5. For accurate mass determinations,the object to be weighed must be at room temperature.
If a hot or warm object is placed on the pan of the balance, such an object causes the air
around to it to become heated. Warm air rises, and the motion of such warm air may be
detected by the balance, giving mass determinations that are significantly less than the true
value.
6. For many types of balances, there are likely to be small errors in the absolute masses of
objects determined with the balance, particularly if the balance has not been properly
calibrated or has been abused. For this reason, most weighings in the laboratory should be
performed by a difference method: an empty container is weighed on the balance, and then
the reagent or object whose mass is to be determined is added to the container. The
resulting difference in mass is the mass of the reagent or object.
In today's laboratory exercise you will be weighing various objects by difference on two
separate balances. It should be clear after completion of the lab why it is important to use the
same balance throughout the course of an experiment.

Volume Measurement:
Most of the glassware in your laboratory locker has been marked by the manufacturer to
indicate the volume contained by the glassware when filled to a certain level. The graduations
etched or painted onto the glassware by the manufacturer differ greatly in the precision they
indicate, depending on the type of glassware and its intended use. For example, beakers and
Erlenmeyer flasks are marked with very approximate volumes, which serve merely as a rough
guide to the volume of liquid in the container. Other pieces of glassware, notably burets,
pipets and graduated cylinders are marked much more precisely by the manufacturer to
indicate volumes. It is important to distinguish when a precise volume determination is
necessary and appropriate for an experiment and when only a rough determination of volume
is needed.
The accuracy of a container is determined in part by its diameter. As the diameter is
increased, the volume is increased and thus the margin of error is increased in proportion to
the increase in diameter.
When water (or an aqueous solution) is contained in a narrow glass container such as a
graduated cylinder, the liquid surface is not flat as might be expected. Rather, the liquid
surface is curved downward. This curved surface is called a meniscus and is caused by an
interaction between the water molecules and the surface of the glass container wall. When
reading the volume of a liquid that makes a meniscus, hold the graduated cylinder so that the
meniscus is at eye level, and read the liquid level at the bottom of the curved surface.
In today's lab you will be investigating the accuracy of several types of glassware. In order to
measure the volumetric accuracy it is necessary to introduce the concept of density. (Density
will be discussed in more detail in lab 2.)
Density represents the mass contained in a unit volume of a sample or:

(1) Density =
16

Mass
Volume

Mass is generally measured in grams and volume in milliliters, and therefore the units of
density are g/mL.
The density of water equals approximately 1.000 g/mL. This fact is useful in obtaining an
accurate measurement of a volume of water by weighing it (or any liquid if the density is
assumed to be 1.000 g/mL). As you can see, by rearranging the equation so that

(2) Volume =

Mass
Density

if density equals 1.00 g/mL, then the volume (in milliliters) will be numerically equal to the
mass (in grams).
Example: If a sample of water weighs 32.0 g; then by equation (2)

(3) Volume =

Safety Precautions:

32.0 g
g
1.000
mL

= 32.0 mL

Wear safety glasses at all times while in the laboratory.

PROCEDURE:

Record all data and observations directly into your notebook in ink. Remember to record both
weights and volumes to the precision of the measurement device. (The triple beam balance, for
instance, is capable of weighing to .001 g; therefore, the weights should be recorded to 3 decimal
places.) Generally, volume measurements can be made to the nearest .l mL and weight
measurements to the nearest .001 g.

Mass Determination:
1.

Select three small objects, e.g., keys, watch, ring. Record the name of these objects in
your notebook.

2.

Weigh a beaker that can accommodate the objects whose masses are to be determined.

3.

Transfer the first of your objects to the beaker. Weigh.

4.

Reweigh your first object DIRECTLY on the balance pan.

5.

Weigh your other two objects by difference ONLY, using the known mass of the
beaker from step 2 .

6.

Using a different balance, repeat steps 2 through 4 for your first object ONLY.

17

Volume Determination:

Glassware must be clean and dry before use to ensure accurate weight and volume
measurements.
1. Weigh a beaker capable of containing 25 mL of water.
2. Add distilled water to the pre-weighed beaker to the 25 mL mark. Weigh the beaker
and water.
3. Measure 25.0 mL of distilled water with your 50 or 100 mL graduated cylinder. Pour this liquid
into your pre-weighed beaker and reweigh.
4. Dispense 25.00 mL of distilled water from the buret into your pre-weighed beaker and
reweigh.
5. Dispense 25.00 mL of distilled water from the volumetric pipet into your pre-weighed
beaker and reweigh.

CALCULATE:

Mass Determination

1. The weight, by difference, of each object on the first balance, and of the first object on the
second balance.
2. The difference in the first object's calculated weight between the two balances.
3. The calibration (systematic) error for both balances.

Volume Determination
1. The mass of water dispensed with each piece of glassware.
2. The volume of water dispensed with each piece of glassware using the density formula
(calculated volume).
3. The difference between your observed volume, 25 mL, and the calculated volume.

DISCUSSION:
In a paragraph, comment on how well the objectives of the experiment were met. If a true or
accepted value is known, discuss the accuracy of your results and suggest potential sources of
experimental error.

18

EXPERIMENT

Mass and Volume Determination

Name: _____________________________

Section: __________

Pre-Laboratory Questions:
1. Explain the exact meaning of the following statement: Weigh out approximately 5 grams of
NaCl to the nearest milligram.

2. Why should you never weigh reagents directly on a balance?

3. Why should you never weigh hot objects on a balance?

4. If you have the choice of using a graduated cylinder, a buret, a beaker, or a volumetric pipet to
measure the volume of a liquid, which would you assume to be the most accurate? Why?

19

EXPERIMENT

Density Determination

OBJECTIVE:
Density is an important property of matter, which may be used as a method of identification.
In this experiment, you will determine the densities of regularly and irregularly shaped solids
as well as of pure liquids and solutions.

INTRODUCTION:
The density of a sample of matter represents the mass contained within a unit volume of
space in the sample. For most samples, a unit volume means 1.0 mL. The units of density,
therefore, are quoted in terms of grams per milliliter.
Since we seldom deal with exactly 1.0 mL of substance in the chemistry laboratory, we
usually say that the density of a sample represents the mass of the sample divided by its
volume.

Density =

Mass
Volume

Because the density does in fact represent a ratio, the mass of any size sample, divided by
the volume of the sample, gives the mass that 1.0 mL of the same sample would possess.
Densities are usually determined and reported at 200C (around room temperature) because
the volume of a sample, and hence the density, will often vary with temperature. This is
especially true for gases, with smaller (but still often significant) changes for liquids and
solids. References (such as the various chemical handbooks) always specify the temperature
at which a density was measured. In today's lab you will be comparing a calculated density
with theoretical handbook density and determining a percent error between the two values:

% Error = |

Theoretical Value - Calculated Value


| x 100
Theoretical Value

Density (along with melting point and boiling point) can be used to identify an unknown
substance and can be used to determine the concentration of solutions in certain instances.
When a solute is dissolved in a solvent, the density of the solution will be different from that
of the pure solvent itself. Handbooks list detailed information about the densities of solutions
as a function of their composition. If a sample is known to contain only a single solute, the
density of the solution can be measured experimentally. Then the handbook can be
consulted to determine what concentration of solute gives rise to the measured density.

There are several techniques used for the determination of density. The method will depend
on the type of sample and on the precision desired for the measurement. In general, a

20

density determination will involve the determination of the mass of the sample with a
balance, but the method used to determine the volume of the sample will differ from situation
to situation. Several methods of volume determination are explored in this experiment.
For solid samples, there may be different methods needed for the determination of the
volume, depending on whether or not the solid is regularly shaped. If a solid has a regular
shape (e.g., cubic, rectangular or cylindrical), the volume of the solid may be determined by
geometry:
For a rectangular solid: Volume = (length) (width) (height)
For a cylindrical solid: Volume = (radius) (height)
2

For a cubic solid: Volume = (edge)3


If a solid does not have a regular shape, it may be possible to determine the volume of the
solid from Archimedes' principle, which states that an insoluble, non-reactive solid will
displace a volume of liquid equal to its own volume. Typically, an irregularly shaped solid is
added to a liquid in a volumetric container (such as a graduated cylinder) and the change in
liquid level or volume represents the volume of the object added.
For liquids a convenient method for routine density determinations is to weigh a particular
volume of liquid contained in a graduated cylinder.

Safety Precautions: Wear safety glasses at all times while in the laboratory.

PROCEDURE:
Record all data and observations directly into your notebook in ink.

Density of Solids
1.

Obtain a regularly shaped solid and record its shape. With a ruler, determine the
physical dimensions of the solid to the nearest 0.1 cm (mm).

2.

Weigh the solid to the nearest 0.001 g.

3.

Obtain a quantity of metal pellets. Weigh the sample to the nearest 0.001 g.

4.

Add water to your 100-mL graduated cylinder to approximately the 50-mL mark. Record
the exact volume of water in the cylinder to the nearest 0.1 mL.

5.

Pour the metal sample into the graduated cylinder, making sure that none of the pellets
sticks to the walls of the cylinder above the water level. Stir/shake the cylinder to make
certain that no air bubbles have been trapped among the metal pellets. Read the level of
the water in the graduated cylinder to the nearest 0.1 mL. (Return pellets to instructor
do not discard.)

Density of Water

21

1.

Weigh a clean, dry 10 mL volumetric flask to the nearest 0.001 g.

2.

Add DISTILLED water to the volumetric flask so that the bottom of the meniscus is on
the calibration mark. The volume is exactly 10.00 mL. If the flask is overfilled, use an
eye dropper to remove the excess.

3.

Reweigh the volumetric flask. Ensure the outside of the flask is dry BEFORE weighing.

4.

Place approximately 25 mL of distilled water in a 50 mL beaker. Determine the


temperature of the water using the thermometer provided. From a chemistry handbook
obtain the density of water at this temperature.

Density of Solutions
1.

Weigh a clean, dry 10 mL volumetric flask to the nearest 0.001 g.

2.

Add 10.00 mL of the 5% NaCl solution, filling the volumetric flask to the calibration mark
as in step 2 above.

3.

Reweigh the volumetric flask.

4.

Pour the 5% NaCl solution in the sink. Next, add a small portion (1 mL) of 10% NaCl
to the volumetric flask. Tilt and rotate the flask such that the 10% NaCl solution contacts
all the inner surfaces. Pour this solution out. This procedure is called rinsing. Repeat
the rinse. Fill the volumetric flask to the calibration mark with 10% NaCl and reweigh the
flask to the nearest 0.001 g.

5.

Repeat step 4 with 15%, 20% and 25% NaCl solutions. It is very important to RINSE the
volumetric flask with the solution to be measured before filling the volumetric flask.

Waste Disposal: All solutions used in this experiment may be flushed down the sink.

CALCULATE:
1.

The volume of the solid.

2.

The density of the solid

3.

The density of the metal pellets.

4.

The density of water.

5.

The percent error in your calculated density of water compared to the theoretical density
of water (from the handbook).

6.

The density of each NaCl solution.

DISCUSSION :

22

In a paragraph, comment on how well the objectives of the experiment were met.
If a true or accepted value is known, discuss the accuracy of your results and
suggest potential sources of experimental error.

23

EXPERIMENT

Density Determination

Name: ________________________________

Section: __________

Pre-Laboratory Questions:
1. A metal sphere weighing 23.18 g is added to 15.71 mL of water in a graduated cylinder. The
water level rises to 22.48 mL. Calculate the density of the metal.

2. An empty beaker weighs 47.398 g. A 10.00 mL pipet sample of an unknown liquid is


transferred to the beaker. The beaker weighs 56.182 grams when weighed with the liquid in it.
Calculate the density of the unknown liquid.

27

EXPERIMENT

Mixture Separation

OBJECTIVE:
Separations of the components of mixtures are performed routinely in chemistry. In this
experiment you will use differences in physical properties to separate the components of a
mixture.

INTRODUCTION:
A mixture is defined as material of variable composition that contains two or more
substances. A solution is a homogeneous mixture, whereas wood is a heterogeneous
mixture. Since each component in a mixture retains its own set of physical properties
(boiling point, etc.) differences in these properties can be used to separate the
components.
In today's lab a mixture of ammonium chloride (NH4Cl), sodium chloride (NaCl) and silicon
dioxide (SiO2) will be separated into the several pure substances. The mass of each
substance will be determined and subsequently the percent composition of the original
mixture can be calculated.

% Composition =

weight of component
x 100
weight of mixture

The separation scheme involves first the sublimation of NH4Cl, which is a solid sublimes,
i.e., changes directly from a solid to a gas without forming a liquid at a temperature of 340
o
C. The other two components of the mixture (NaCl and SiO2) do not sublime, but they do
melt (at 801 oC and 1723 oC respectively). Therefore, at the temperature attained with the
burner in the lab both NaCl and SiO2 will remain solids. The NH4Cl, however, will sublime
or go into the gaseous phase (disappearing up the fume hood).
The mixture now contains only NaCl and SiO2 and by comparing the weight of the mixture
now with the original weight, the amount of the NH4Cl originally present can be determined.
The two remaining components can be separated by their differing solubility in water. NaCl
(or table salt) is soluble whereas SiO2 is not. The SiO2 can therefore be separated from
the NaCl and water solution by filtration.
In order to calculate the amount of NaCl in the mixture, it will now be necessary to separate
it from the water solvent. This is done by utilizing the difference in boiling points of NaCl
o
o
and water. Water, of course, boils at 100 C whereas NaCl melts at 801 C and boils at
o
1413 C. Obviously, water (with the lower boiling point) will evaporate first leaving the solid
NaCl behind.

28

Safety Precautions:

Wear safety glasses at all times while in the laboratory.


Burners will be utilized in this laboratory. USE CARE.
Perform experiment under hood to remove toxic NH4Cl fumes that
evolve.

PROCEDURE:
Record all data and observations directly into your notebook in ink. All weights should be
recorded to the nearest 0.001 g (from the triple beam balance).
1.

Obtain a pre-mixed sample of the mixture.

2.

Weigh a clean, dry 100 or 150 mL beaker.

3.

Transfer all the mixture into the beaker. Reweigh.

4.

Place the beaker and its contents on a wire gauze supported by an iron ring. With a
glass stirring rod, break up any chunks.

5.

Heat the beaker and its contents over a gas burner. Begin heating hear the top of the
beaker and slowly move the flame towards the bottom. Heat with the hottest possible
flame for 10 minutes. (NOTE: NH4Cl will sublime from the mixture and deposit on the
cooler upper beaker walls, rather than escaping up the hood, if the walls are not
heated.

6.

Allow the beaker to cool to room temperature (comfortable to the touch). Weigh the
beaker and residue.

7.

Heat the beaker and residue again for about 5 minutes, cool and weigh the beaker
and residue. If the difference in this weight and that obtained in step 6 is greater than
0.01 g, reheat beaker and residue for another 3 minutes. (If there is too great a
difference between the two weights it can be assumed that NH4Cl is still present and
continuing to sublime. When these weights are the same or within 0.01 g, it can be
assumed that all the NH4Cl has been removed.)

8.

Add no more than 10 mL of distilled water to the residue in the beaker to dissolve the
NaCl. Stir gently for 1 minute to loosen all solids.

9. Weigh separately a piece of filter paper and an evaporating dish.


10. Set up a filter funnel using the weighed filter paper.
11. Swirl the NaCl/SiO2 solution in the beaker and quickly pour into the filter funnel,
collecting the filtrate and wash water in the pre-weighed evaporating dish.
12. Use the least amount of water possible from a wash bottle to rinse the beaker and to
flush the SiO2 into the funnel. Let the solution drain from the funnel before continuing.
13. With a minimum amount of water from a wash bottle, wash the filter paper/SiO 2 free of
any NaCl solution.
29

14. Carefully remove the wet filter paper without spilling the SiO2. Spread the filter
paper on a watch glass and place in a drying oven for 30 minutes.
15. Place the evaporating dish and solution on a wire gauze on a wire ring. Heat gently
with a gas burner so that the solution boils gently (simmers) and the volume is
reduced to approximately one-fourth. (NOTE: Be very careful not to lose any sample
by spattering the bubbling liquid out of the dish.)
16. Carefully lift the evaporating dish with tongs and place it over a beaker on the wire
gauze. Heat the bottom of the beaker strongly to evaporate the remaining solution to
dryness.
17. When the NaCl appears dry, carefully remove the beaker and place the evaporating
dish directly on the wire gauze.
18. Carefully wave a small flame of a burner around the outside edges of the evaporating
dish for 5-10 seconds. Always heat cautiously because rapid evolution of steam will
spatter the crystals out of the dish. Then remove the burner to a safe distance. Hold
your ear near the evaporating dish. If any water is present in the crystals, you may
hear the "hiss" of escaping steam.
19. Repeat step 18. Slowly heat until the "hiss" stops. Finally, heat the residue with full
heat for 5 minutes.
20. Allow the dish to cool and then weigh.
21. Take the filter paper/SiO2 on the watch glass out of the oven, allow to cool, and then
weigh. Return to the drying oven for a further 10 minutes, cool, and reweigh.

Waste Disposal:

The dried NaCl may be flushed down the sink.


The filter paper and SiO2 should be put in the trash.

CALCULATE:
1.

The starting mass of your mixture.

2.

The mass of the various components: NH4Cl, NaCl and SiO2.

3.

The sum of the masses of the recovered components.

4.

The percent by mass of each component in the sample.

DISCUSSION:
In a paragraph, comment on how well the objectives of the experiment were met.
If a true or accepted value is known, discuss the accuracy of your results and
suggest potential sources of experimental error.
30

EXPERIMENT

Mixture Separation

Name: ______________________________

Section: __________

Pre-Laboratory Questions:
1. A mixture contains 3.64 g NaCl, 2.87 g NH4Cl, and 4.13 g of SiO2. What is the percent by
mass of each compound in the mixture?

2. When a substance sublimes, it goes from a ____________ to a _____________.

3. If it evaporates, it goes from a _____________ to a _____________.

31

EXPERIMENT

Determination of a Formula

OBJECTIVE:
Stoichiometric measurements are among the most important in chemistry, indicating the
proportions by mass in which various substances react. In this experiment the reaction
between magnesium and oxygen will be used to investigate a stoichiometric relationship.

INTRODUCTION:
Magnesium metal is a moderately reactive elementary substance. At room temperature,
magnesium reacts only very slowly with oxygen and can be kept for long periods of time
without appreciable oxide buildup. At elevated temperatures, however, magnesium will
ignite in an excess of oxygen gas, burning with an intensely white flame and producing
magnesium oxide (MgO). Because of the brightness of its flame, magnesium is used in
flares and in photographic flashbulbs.
In this experiment, however, you will be heating magnesium in a closed container called a
crucible, exposing it only gradually to the oxygen of the air. Under these conditions, the
magnesium will undergo a more controlled oxidation, gradually turning from a shiny metal
to a grayish-white powdered oxide. Because the air also contains a great deal of nitrogen
gas, a portion of the magnesium being heated may be converted to magnesium nitride
(Mg3N2), rather than MgO. Mg3N2 will react with water and, on careful heating, is converted
into MgO
Mg3N2 (s) + 3 H2O (l) 3 MgO (s) + 2 NH3
The ammonia produced by this reaction can be detected by its odor, which is released on
heating the mixture.
Magnesium is a Group IIA metal, and its oxide should have the formula MgO. Based on
this formula, MgO should consist of approximately 60% magnesium by weight.

% by weight =

weight Mg
x 100
weight MgO

By comparing the weight of magnesium used, and the weight of MgO that results from the
reaction, this relationship should be confirmed.

32

Safety Precautions:

Wear safety glasses at all times while in the laboratory.


Magnesium produces an intensely white flame if ignited, which may
be damaging to the eyes. If the magnesium used in this experiment
ignites in the crucible by accident, immediately cover the crucible
and stop heating. Do not look directly at magnesium while it is
burning.
When water is added to the crucible to convert magnesium nitride to
magnesium oxide, the contents of the crucible may spatter when
heated. Use only gentle heating in evaporating the water. Do not
heat the crucible strongly until nearly all the water has been
removed.
Use crucible tongs to handle the hot crucible and cover.
Hydrochloric acid is damaging to skin and clothing. If it is spilled,
wash immediately and inform the instructor.

PROCEDURE:
Record all data and observations directly into your notebook in ink.
1.

Obtain a crucible and cover. They are extremely fragile and expensive. Use caution
in handling them.

2.

If there is any loose dirt in the crucible, moisten and rub it gently with a paper towel to
remove the dirt. If a residue remains in the crucible, add 2-3 mL of 6M HCl (under the
hood) and allow the crucible to stand for 5 . minutes. Discard the HCl and rinse the
crucible with water. The crucible may not be "like new" at this point, but it will be clean
enough for this experiment.

3.

Set up a clay triangle on a ring stand. Transfer the crucible and cover to the triangle.
The crucible should sit firmly in the triangle (the triangle's arms can be bent slightly, if
necessary).

4.

Begin heating the crucible and cover with a small flame to dry them. When the
crucible and cover show no visible droplets of moisture, increase the flame to full
intensity, and heat the crucible and cover for 5 minutes.

5.

Remove the flame and allow the crucible and cover to cool to room temperature.

6.

When the crucible and cover are cool, use tongs to move them to a clean dry watch
glass and carry to balance. Weigh the crucible and cover. (Carrying the crucible and
cover with the watch glass and not in your hands ensures that the weight is not
influenced by the addition of oil from your skin. While not a major concern when
weighing in the milligram range, it can be significant when weights are in the
microgram range.)

7.

Return the crucible and cover to the clay triangle. Reheat in the full heat of the burner
flame for 5 minutes. Allow the crucible/cover to cool completely to room temperature.
33

8.

Reweigh the crucible after it has cooled. If the weight this time differs from the earlier
weight by more than 0.01 g reheat the crucible for an additional 5 minutes and
reweigh when cool. Continue the heating/weighing until the weight of the crucible and
cover is constant to within 0.01 g. This repeated weighing is to ensure that a good dry
weight of the crucible is obtained. There is a certain amount of moisture in porcelain
which should be removed before proceeding with the experiment.

9.

Add approximately 0.5 g of magnesium turnings to the crucible.

10. Using tongs, transfer the crucible/cover and magnesium to the watch glass, carry to
the balance and weigh.
11. Set up the crucible on the clay triangle with the cover very slightly ajar. With a very
small flame, begin heating the crucible gently.
12. If the crucible begins to smoke when heated, immediately cover the magnesium
completely and remove the heat for 2-3 minutes. The smoke consists of the MgO
product and must not be lost from the crucible.
13. Continue to heat gently for 5-10 minutes with the cover of the crucible slightly ajar.
Remove the heat and allow the crucible to cool for 1-2 minutes.
14. Remove the cover and examine the contents of the crucible. If portions of the
magnesium still demonstrate the shiny appearance of the free metal, return the cover
and heat with a small flame for an additional 5 minutes; then re-examine the metal.
Continue heating with a small flame until no shiny metallic pieces are visible.
15. When the shiny magnesium metal appears to have been converted fully to the dull
gray oxide, return the cover to its slightly ajar position, and heat the crucible with the
full heat of the burner flame for 5 minutes. Then slide the cover to about the half-open
position and heat the crucible in the full heat of the burner flame for an additional 5
minutes.
16. Remove the heat and allow the crucible and contents to cool completely to room
temperature. Remove the cooled crucible from the clay triangle and set it on a sheet
of clean paper on the lab bench.
17. With a stirring rod, gently break up any large chunks of solid in the crucible. Rinse any
material that adheres to the stirring rod into the crucible with a few drops of distilled
water. With a dropper, add about 10 drops of distilled water to the crucible, spreading
the water evenly throughout the solid.
18. Return the crucible to the clay triangle, and set the cover in the slightly ajar position.
With a very small flame, begin heating the crucible to drive off the water that has been
added. Beware of spattering during the heating. Remove the flame and close the
cover of the crucible if spattering occurs.
19. Any nitrogen that had reacted with the magnesium is being driven off as ammonia
during this heating and you may detect its odor at this point.
20. When it is certain that all the water has been driven off, slide the cover so that it is in
approximately the half-open position, and increase the size of the flame. Heat the
crucible and contents in the full heat of the burner for 5 minutes.

34

21. Allow the crucible and contents to cool completely to room temperature. When
completely cool, weigh the crucible and contents.
22. Return the crucible to the triangle and heat for another 5 minutes in the full heat of the
burner flame. Allow the crucible to cool completely to room temperature and reweigh. If
this weight differs from the weight above (step 21) by more than 0.01 g, reheat for an
additional 5 minutes and reweigh when cool. Continue heating/weighing crucible and
contents until the weight is constant to within 0.01 g.

Waste Disposal:

HCl and any residue from crucible may be flushed down the sink.
Your product, MgO should be put in the trash.

CALCULATE:
1.

The weight of magnesium taken.

2.

The weight of MgO produced.

3.

The percentage of magnesium in the MgO produced.

4.

The theoretical percentage of magnesium in MgO.

5.

The percent error in your determination.

DISCUSSION:
In a paragraph, comment on how well the objectives of the experiment were met.
If a true or accepted value is known, discuss the accuracy of your results and
suggest potential sources of experimental error.

Environmental Science Notes:


Magnesium, and other metal ions such as zinc, calcium, iron and copper, play important
biological roles as enzymatic cofactors. Many protein enzymes which act as catalysts
(increasing the rate of a reaction) depend on the presence of a cofactor in order to exhibit
optimum catalytic activity, or even any activity at all.
Environmental pollutants can inactivate an enzyme by interfering with these cofactors.
Fluoride, for instance, can effect the action of an enzyme which requires magnesium by
causing the formation of a magnesium fluorophosphate complex, which ties up the metal
ion, making it unavailable as a cofactor..
Pollutants can also inactivate an enzyme by competing with a cofactor for its location on the
enzyme. Beryllium, for instance, can replace magnesium in some enzymes. Beryllium
does not act as a cofactor and, therefore, the enzymes activity is adversely affected.

35

EXPERIMENT

Determination of a Formula
Name: ______________________________

Section:

__________

Pre-Laboratory Questions:

1. Why is it good experimental procedure to use tongs and watch glasses to move the cooled
crucible to the balance for weighing, once it has been heated?

2. Calculate the percentage by mass of chromium in chromium (III) oxide.

3. After initial heating, what solid other than magnesium oxide is present, and what gas is
released after the addition of water.

36

EXPERIMENT

Stoichiometry:
Gas Evolution Reaction

OBJECTIVE:
Stoichiometric measurements are among the most important in chemistry, indicating the
proportions by mass in which various substances react. In this experiment the stoichiometry
of a gas evolution/neutralization reaction will be studied.

INTRODUCTION:
Several common anions, when acidified, evolve gases. The net ionic reactions of the
carbonate, hydrogen carbonate (bicarbonate) and sulfite ions are examples of this:
CO32- (aq) + 2 H1+ (aq) H2CO3 (aq) H2O (l) + CO2 (g)
HCO3 (aq) + H (aq) H2CO3 (aq) H2O (l) + CO2 (g)
1-

1+

SO32- (aq) + 2H1+ (aq) H2SO3 (aq) H2O (l) + SO2 (g)
Now consider the reactions
Na2CO3 (s) + 2HBr (aq) 2NaBr (s) + H2O (l) + CO2 (g)
NaHCO3 (g) + HBr (aq) NaBr (s) + H2O (l) + CO2 (g)
These reactions are basically those given in the first two of the preceding net ionic reactions.
Since one of the products of the reaction is a gas (CO2), and a second of the products can
be conveniently vaporized by heating (H2O), the stoichiometry of the reaction can be studied
by collecting and weighing the solid product of the reaction (NaBr). A similar study could be
made of the reaction of the sulfite ion, but since the product gas SO2 is toxic and noxious, this
will not be done in this experiment.
In this experiment you will treat a weighed sample of sodium carbonate (Na2CO3) with a
calculated amount of 3.0 M hydrobromic acid (HBr). (3.0 M is the molarity, M = molarity, of
the hydrobromic acid being used. Molarity is defined as the concentration of a solution
measured in moles of solute/liter of solution. A 3.0 M solution of HBr is a relatively dilute
solution bearing in mind that concentrated HBr is 12 M). The volume of 3.0 M hydrobromic
acid required can be calculated as:

) g Na2 CO3 (

1 mole Na2 CO3


2 mole HBr
1 L HBr
)(
)(
) = (
105.98g Na2 CO3 1 mole Na2 CO3 3 moles HBr
37

) L HBr

After the reaction is completed you will evaporate the water from the sample and determine
the actual amount of NaBr produced. The theoretical amount of NaBr that should been
produced from the stoichiometric ratios of the balanced equation will be calculated:
(

) g Na2 CO3 (

1 mole Na2 CO3


2 moles NaBr
102.89 g NaBr
)(
)(
) = (
105.98 g Na2 CO3 1 mole Na2 CO3
1 mole NaBr

) g NaBr

Using the actual yield and the theoretical yield a percentage yield can now be calculated:

% yield =

Safety Precautions:

actual yield
x 100%
theoretical yield

Wear safety glasses at all times while in the laboratory.


Hydrobromic acid is damaging to the skin and its vapors are toxic.
Perform the reaction under the bench extraction hood. Considerable
frothing will result as hydrobromic acid is added to the samples. Keep
the casserole covered with a watch glass during addition of the acid.
Beware of spattering.
Evaporation of water from the samples must be done only over a
boiling water bath (double boiler). Dangerous spattering of hot salts
will result if the evaporation is done on an open flame.

PROCEDURE:
Record all data and observations directly into your notebook in ink.
1.

Clean your casserole dish with soap and water. Rinse the casserole with distilled water
and wipe dry with a towel.

2.

On a wire gauze on a ringstand, heat the casserole on a low flame for 5 minutes to dry
it. Move the flame occasionally during the heating so that all portions of the casserole
are heated. Allow the casserole to cool completely to room temperature.

3.

Weigh the casserole. Reheat the casserole on the wire gauze for an additional 5
minutes and reweigh after cooling completely. If the second mass determined for the
casserole differs from the first mass by more than 0.01 g, reheat and reweigh until
constant mass is achieved (within 0.01 g).

4.

Add approximately 1 g of Na2CO3, to the casserole and reweigh.

5.

Add about 150 mL of tap water to a 250 mL beaker on the wire gauze/ring and bring the
water to a boil. This steam bath will not be used until step 8, but in the interest of saving
time (water takes a long time to boil) it is suggested that heating should start as early as
possible.

38

6.

Moisten the Na2CO3 with 2-3 mL of distilled water and add 2 drops of methyl red
indicator (the mixture will be yellow). Cover the casserole with a watch glass to catch
any material that may spatter.

7.

Using an eye dropper, add the volume of HBr calculated from the stoichiometry of the
reaction down the pouring spout of the casserole without removing the watch glass. The
Na2CO3 will froth and fizz as carbon dioxide (CO2) is generated, and the watch glass will
prevent loss of the solid. Retain approximately 1 mL of hydrobromic acid. The indicator
may change to red during this addition; this does not signal completion of the reaction,
however, because some CO2 may remain in solution at this point, thereby affecting the
pH of the mixture.

8.

Transfer the casserole onto the top of the (250 mL beaker) steam bath and heat until the
mixture just begins to boil. This heating is only to drive off CO2; do not attempt to boil off
the water from the mixture at this point. As CO2 is evolved on heating, the mixture
should turn yellow again. Temporarily remove the Bunsen burner from heating the
steam bath.

9.

Add additional HBr dropwise until the mixture in the casserole turns a permanent pale
red. This will ensure that you have added a sufficient amount of HBr to react with all the
Na2CO3 present, i.e., all the Na2CO3 has reacted.

10. Use a stream of distilled water from a wash bottle to rinse any solids that may have
collected on the bottom of the watch glass into the casserole.
11. Now continue heating to evaporate the water in your casserole. Do not attempt to hurry
the evaporation of water by using a direct flame on the casserole. As the mixture in the
casserole becomes more concentrated by evaporation, it will tend to "bump" and spatter
badly if directly heated, leading to loss of product. Spattering of hot solids is also
dangerous.
12. After the solid (NaBr) in the casserole is almost completely dry, remove the casserole
from the steam bath. Begin heating the casserole directly with a very small flame.
13. If the casserole contents begin to spatter, not enough water has been evaporated and
the casserole should be returned to the steam bath for additional slow heating. If no
spattering occurs, continue heating the casserole directly with a small flame for 5
minutes. Increase the size of the flame somewhat, and continue heating the casserole
for an additional 5-minute period to remove all moisture. Let the casserole cool
completely to room temperature.
14. Weigh the casserole once it has cooled completely.

Waste Disposal:

Your product, NaBr, may be washed down the sink.

39

CALCULATE:
1.

The mass of Na2CO3 taken.

2.

The volume of 3.0 M HBr to react with the Na2CO3 taken.

3.

The mass of your product (actual yield).

4.

The theoretical yield of NaBr based on the mass of Na2CO3 taken.

5.

The percent yield for your experiment.

DISCUSSION:
In a paragraph, comment on how well the objectives of the experiment were met.
If a true or accepted value is known, discuss the accuracy of your results and suggest
potential sources of experimental error.

Environmental Science Notes:


In todays experiment a carbonate is reacted with an acid to produce a salt, water and
carbon dioxide. Sodium carbonate is soluble in water; most metal carbonates are not. An
important exception occurs if the water is slightly acidic, as is the case of acid rain. Here
sulfur products released when fossil fuels are burned combine with oxygen in the air and
rain water to form sulfuric acid.
2SO2
SO3

(g)

(g)

+ O2

(g)

-> 2 SO3 (g)

+ H2O (l) -> H2SO4 (aq)

Sulfuric acid dissociates in water to form hydrogen ions (and sulfate ions) which in turn react
with a normally insoluble carbonate - calcium carbonate, CaCO3, or marble, causing its
dissolution.
+

(aq)

2+
(aq)

+ CaCO3 (s) -> Ca

+ HCO3

(aq)

Acid rain, through its effect on metal carbonates, is slowly eroding the finer features of our
statues and other monuments.

40

EXPERIMENT

Stoichiometry: Gas Evolution Reaction

Name: _____________________________

Section: __________

Pre-Laboratory Questions:
1.

What volume of 6 M HBr would be required to react with 2.46 g of Na2CO3?

2. If 5.18 g of pure NaHCO3 is treated with an excess of 3.0 M HBr solution, how many grams of
NaBr will be produced?

41

EXPERIMENT

Stoichiometry:
Precipitation Reaction

OBJECTIVE:
Stoichiometric measurements are among the most important in chemistry, indicating the
proportions by mass in which various substances react. In this experiment, the
stoichiometry of a precipitation reaction will be investigated.
INTRODUCTION:
When aqueous solutions of ionic solutes are mixed, the outcome may be a new combination of
ions that will not be appreciably soluble in water and that will result in the formation of a solid
precipitate. Precipitation reactions find a wealth of uses in chemistry. For example, many
chemical analyses involve quantitative precipitation of the substance under analysis with some
appropriate precipitating agent; the precipitate is then usually filtered, dried, and weighed,
which enables the analyst to calculate the amount of the analyte that was present in the original
sample. In this experiment, the stoichiometric ratio in which the substances calcium chloride
(CaCl2) and sodium phosphate (Na3PO4) react will be determined. When aqueous solutions of
these two salts are mixed, an insoluble precipitate of calcium phosphate (Ca3(PO4)2) forms,
which can easily be collected, dried, and weighed. The approach used in investigating the
stoichiometric ratio of this precipitation reaction is called the method of continuous variations.
To understand how this method works, consider the situation in which a precipitation reaction is
known to take place between aqueous solutions of salts A and B, resulting in the production of
precipitate C, that is:

A(aq) + B(aq) C(s)


Consider that 1.00 M solutions of salts A and B are available, and that a set of experiments is
performed in which different amounts of A and B are mixed, but the total volume after mixing is
kept constant throughout the set of experiments. A table indicating such a set of experiments
follows:
No.

mL 1.00 M Soln. A

mL 1.00 M Soln. B

10.0

90.0

20.0

80.0

30.0

70.0

40.0

60.0

50.0

50.0

60.0

40.0

70.0

30.0

80.0

20.0

90.0

10.0
42

The amount of precipitate C that forms in each experiment in the set will be determined by
the relative amounts of A and B used in the individual experiment and also by the
stoichiometric ratio in which A and B react. For example if A and B react in the ratio of 1:1,
we might expect the amount of C produced to vary in the manner indicated in the following
table:
No.

mL 1.00 M Soln. A

mL 1.00 M Soln. B

g precipitate C

10.0

90.0

0.125

20.0

80.0

0.250

30.0

70.0

0.375

40.0

60.0

0.500

50.0

50.0

0.625 (max.)

60.0

40.0

0.500

70.0

30.0

0.375

80.0

20.0

0.250

90.0

10.0

0.125

Notice that the maximum amount of C produced occurs when equal volumes of solutions A
and B are combined (no. 5); since the solutions of A and B are both 1.00 M in
concentration, the fact that the maximum extent of reaction occurs when equal volumes of
the solutions are mixed confirms the 1:1 stoichiometry. In each of the experiments before
the equal-volume point is reached (nos. 1-4), substance A is the limiting reagent for the
production of C; in the experiments after the equal-volume point (nos. 6-9), it is substance
B that limits the amount of C that can form.
Suppose on the other hand the reaction between A and B were of 1:2 stoichiometry: that is,
suppose the balanced chemical equation for the reaction were really

A(aq) + 2B(aq) C(s)


Because of the different stoichiometry in this situation, it is not expected that the maximum
production of the precipitate would occur at the equal-volume point. Rather with 1:2
stoichiometry, for a total volume of 100.0 mL, the maximum production of C would occur at
volumes between those of experiment 3 and 4 (i.e., at the point where 33.3 mL A would be
mixed with 66.7 mL B). Additional experiments might be performed for intermediate
volumes to confirm this ratio.
The most convenient way of realizing the stoichiometric ratio when studying a reaction by
the method of continuous variations is to make a graph of the data. For the preceding
reactions, such a graph would be a plot of the amount of C produced versus the number of
milliliters of solution A (or solution B) used. A graph of this sort will show a maximum at the
stoichiometric ratio for the reaction.

Safety Precautions:

Wear safety glasses at all times while in the laboratory.


Calcium chloride and sodium phosphate solutions may be irritating
to the skin. Wash after handling.

43

PROCEDURE:
Record all data and observations directly into your notebook in ink.
1.

Your instructor will assign three test tube numbers (see below) to your group.
Test Tube No.

mL 0.500 M CaCl2

mL 0.500 M Na3PO4

2.00

18.00

4.00

16.00

6.00

14.00

8.00

12.00

10

10.00

10.00

12

12.00

8.00

14

14.00

6.00

16

16.00

4.00

18

18.00

2.00

2.

Clean three test tubes and wipe them as dry as possible by using a rolled up paper
towel.

3.

Clean and dry thoroughly a graduated cylinder. Measured assigned amount of CaCl2
with cylinder and transfer to one test tube.

4.

Clean and dry another graduated cylinder and measure assigned amount of Na3PO4
with cylinder and transfer to same test tube used in step 3.

5.

Repeat steps 3 and 4, using the other test tubes and the assigned mixtures.

6.

After the solutions have been dispensed, use a clean stirring rod to agitate each
mixture in its test tube. Use a stream of water from the wash bottle to rinse any solid
adhering to the stirring rod back into the test tube (no precipitate should be lost).

7.

Allow solutions to settle while performing the following steps.

8.

Obtain three pieces of filter paper. Weigh each to the nearest 0.001 g and record the
weight on the filter paper using pencil (do not use pen, it will wash off).

9.

Set up the suction filtration apparatus as follows: Place one weighed filter paper in the
Buchner funnel and insert the funnel into the sidearm flask. Connect tubing from the
flask to the water aspirator at the sink. Turn on the water to start suction and wet the
filter paper with distilled water so that the paper stays in the funnel.

10. Transfer the contents of one test tube to the Buchner funnel. Liquid will be sucked
through the paper, leaving the precipitate behind. Using a wash bottle, rinse the test
tube until all solution and solids have been transferred.

44

11. When all the solution has drained through, squirt the sides of the funnel with water
from a wash bottle to ensure that all the solids are on the paper. Continue applying
suction until all liquid has drained through and then remove the filter paper from the
funnel.
12. Repeat filtering steps with the other test tubes and filter papers.
13. Carefully dry all filter papers/residues in a drying oven at 110-120 oC for 30 minutes.
Allow to cool to room temperature and then weigh.
14. Record the data of all other groups before leaving the laboratory.

Waste Disposal:

All solutions generated in this lab may be flushed down the sink with
excess water.

CALCULATE:
1.

The mass of Ca3(PO4)2 that was produced in the test tubes assigned to you.

2.

For one of your test tubes, calculate the theoretical yield of solid calcium phosphate,
and hence a percent yield.

3.

Graph the amount of precipitate formed (grams) on the y-axis versus volume of
calcium chloride (mL) on the x-axis (from 0 to 20 mL). Use all the data available.
Starting at 0 and 20 mL of calcium chloride, draw ascending best-fit straight lines
through the data points, as described in Pre-Laboratory question 1.
Where these two lines intersect (maximum production of precipitate), construct a line
vertically downwards to the x-axis and determine the volumes of calcium chloride and
sodium phosphate which would generate this maximum amount of precipitate.
Express these volumes in the form of a simplest ratio, e.g. 1:1.

4.

Write out the balanced reaction equation and obtain the theoretical molar ratio of
calcium chloride and sodium phosphate.

DISCUSSION:
Comment on : the percent yield of your reaction, and suggest potential sources of
experimental error ; how well your two lines on the graph fit the data points, and so how
confident you are about the position of their intersection ; the molar ratio indicated by
your graph, and the molar ratio indicated by the balanced reaction equation.
Environmental Science Notes:
The fact that calcium and phosphate ions form an insoluble precipitate is used in the treatment
of wastewater. When phosphate ion is abundant, as in wastewater, it causes excessive
growth of algae which ultimately robs the water of oxygen needed by fish and other aquatic
life. In this case, calcium carbonate (lime) is added to the water. The solid calcium phosphate
which then forms can easily be removed by a settling process.
45

EXPERIMENT

Stoichiometry: Precipitation Reaction

Name: _______________________________

Section: __________

Pre-Laboratory Questions:

1. Construct a graph of the data in the table on p48, plotting grams of C produced on the vertical
axis versus mL of solution A used on the horizontal axis. Draw a straight line through the
ascending data points and a second straight line through the descending points of your graph.
The maximum point in your graph indicates the maximum extent of reaction for the mixture.
At what stoichiometric ratio of A and B does the maximum production of C occur?

2. If you assume that Solution A is CaCl2 and that solution B is Na2CO3 , and the precipitate C
is CaCO3, does the stoichiometric relationship illustrated by the graph mirror the molar
ratio as indicated by the balanced equation of the reaction? Explain your answer.

46

EXPERIMENT

Molecular Structures
and Shapes

OBJECTIVE:
The aim of this experiment is to construct models of molecules in order to illustrate the
predictions of the Valence Shell Electron Pair Repulsion (VSEPR) theory, bond angles, and
molecular geometry.

INTRODUCTION:
The Valence Shell Electron Pair Repulsion (VSEPR) theory considers the arrangement of
valence electron pairs around the central atom of a molecule, such that the mutual repulsion
among the electron pairs is minimized. The general principle is that the electron pairs will be
oriented in three-dimensional space to be as far away from each other as possible.
Some molecules will contain multiple bonds (in other words, not a single bond) between the
central atom and another, outer atom. It has been found that pairs of electrons in multiple
bonds effectively occupy the same space as the pair of electrons in a single bond. Therefore,
a bond, whether single or multiple, can be considered overall as one electron pair "lobe." This
means that the number of electron pair lobes around a central atom is equal to the sum of the
number of outer atoms to which it is bonded, and the number of lone electron pairs on the
central atom. It is this number of lobes which dictates the arrangement of electron pairs in
which the lobes are arranged to produce minimum repulsion, and therefore the bond angle
(the angle between any two bonds).
Possible electron-pair arrangements, and corresponding bond angles, are as follows:

Number of

Electron Pair Arrangement

Bond Angle

Linear

180

Trigonal Planar

120

Tetrahedral

109.5

Trigonal Bipyramid

90, 120

Octahedral

90

Electron Pairs

47

In practice it is found that any lone pairs on a central atom tend to require more space than
bonding pairs, and therefore compress the space available for bonding pairs, which results in
bond angles which are reduced by a few degrees from the normal figure.
The distribution of electron pairs around a central atom is obtained from the consideration of
the Lewis Structure for the particular molecule. In brief outline:
sum all the valence electrons of all the atoms in the molecule. Adjust this figure if the
molecule is an ion, to allow for the ion's overall charge;
draw a simple diagram with the element present as a single atom in the center (often the
least electronegative atom);
assign two (one pair of) electrons to a (single) bond between the central atom and each other
atom;
add electrons in pairs (lone pairs) to each atom of the most electronegative element so that it
obeys the octet rule (add none to hydrogen - it obeys the duet rule);
if any electrons remain after this distribution, place them in lone pairs on the least
electronegative atom.
Finally, check the number of electrons available to the least electronegative atom. If there are
eight or more, then the structure is complete. If there are less than eight, it is still complete if
the central atom is boron or beryllium, but otherwise take a lone pair of electrons from a more
electronegative atom and create a double bond to that atom. Continue this process, using
alternate atoms if available, until the least electronegative atom has access to eight electrons.
This often results in resonance: a double bond could equally be drawn between the least
electronegative atom and any one of several more electronegative atoms. However, as
explained earlier, resonance does not affect the geometric structure of the molecule.
The molecular geometry of a molecule is defined by the geometry of electron pairs involved
in bonding only- ; in effect, it is the shape described by the arrangement of the atoms in the
molecule. This may be more difficult to visualize, when the central atom has lone pair lobes
on it, but conceptually the molecular shape is the shape resulting from removing lone pair
lobes from the electron-pair arrangement. Therefore, the molecular geometry will vary, for
each electron-pair arrangement, according to the number of lone pair lobes that are removed.
A molecule will be polar, and have a dipole moment, if there is at least one lone pair on the
central atom and the molecular geometry is not symmetrical.
A complete summary of electron-pair arrangements and molecular geometries follows:

48

Number of
Electron Pairs

Electron-Pair
Arrangement

Number of
Bonding Pairs

Molecular
Geometry

Linear

Linear

Trigonal Planar

Trigonal Planar

Trigonal Planar

Bent

Tetrahedral

Tetrahedral

Tetrahedral

Trigonal Pyramid

Tetrahedral

Bent

Trigonal Bipyramid

Trigonal Bipyramid

Trigonal Bipyramid

See-Saw

Trigonal Bipyramid

TShape

Trigonal Bipyramid

Linear

Octahedral

Octahedral

Octahedral

Square Pyramid

Octahedral

Square Planar

Octahedral

T-Shape

Octahedral

Linear

It is important, when describing the properties of a molecule, to be able to predict if the molecule
has a dipole moment. Molecules which contain different atoms will naturally exhibit a dipole
moment unless the molecular geometry of the molecule is entirely symmetrical in threedimensional space.
During this experiment, you will: draw Lewis Structures for several molecules; construct the balland-stick model of each molecule's arrangement of electron pairs; predict the bond angle; adjust
the structure to obtain the molecular geometry; and predict if the molecule has a dipole moment.

PROCEDURE:
Obtain a packet of "balls" and "sticks." On the attached sheets, draw a Lewis Structure for each
of the molecules listed by your instructor. Then build a model of the arrangement of electron pairs
and use it to complete the description of the molecule in terms of electron-pair arrangement, bond
angle, molecular geometry, and presence of a dipole moment (yes or no).

49

Environmental Science Note :


It has been assumed that all molecules contain only pairs of valence electrons, so that simple
Lewis Structures can be drawn. There are, however, a few stable molecules which do have an
odd number of valence electrons ; they are often called free radicals because of the presence
of an unpaired electron, and they are generally more reactive than molecules with paired
electrons. A free radical typically reacts with another free radical so that the unpaired electrons
become paired together, or it reacts with another molecule to create new free radicals.
Two well-known molecules which contain unpaired electrons are nitrogen monoxide (nitric
oxide), NO, and nitrogen dioxide, NO2. These free radical molecules promote the development
of atmospheric pollution and are the primary constituents of smog which affects urban areas
when air is relatively stagnant.
Nitrogen monoxide is formed by combination of oxygen and nitrogen in air at the high
temperatures of combustion in an automobile engine, and is exhausted to the atmosphere
where it reacts rapidly with oxygen to form nitrogen dioxide.
Sunlight photochemically splits the nitrogen dioxide molecule back to a nitrogen monoxide
molecule and a free-radical oxygen atom which reacts with oxygen molecules to produce
ozone, O3.
Ozone is an essential component in the upper atmosphere, where it absorbs harmful ultraviolet
(UV) radiation from the sun, but it is an undesirable pollutant at low-level. It is very reactive and
will affect the respiratory system if breathed in at significant concentrations.

50

Name : _______________________________

Section : _____________

MOLECULAR STRUCTURES AND SHAPES

1. Molecule:

Lewis Structure

Pair Arrangement:

Bond Angle:

Molecular Geometry:

Dipole Moment:

2. Molecule:

Lewis Structure

Pair Arrangement:

Bond Angle:

Molecular Geometry:

Dipole Moment:

3. Molecule:

Lewis Structure

Pair Arrangement:

Bond Angle:

Molecular Geometry:

Dipole Moment:

51

MOLECULAR STRUCTURES AND SHAPES (Cont)


4. Molecule:

Lewis Structure

Pair Arrangement:

Bond Angle:

Molecular Geometry:

Dipole Moment:

5. Molecule:

Lewis Structure

Pair Arrangement:

Bond Angle:

Molecular Geometry:

Dipole Moment:

6. Molecule:

Lewis Structure

Pair Arrangement:

Bond Angle:

Molecular Geometry:

Dipole Moment:

52

MOLECULAR STRUCTURES AND SHAPES (Cont)

7. Molecule:

Lewis Structure

Pair Arrangement:

Bond Angle:

Molecular Geometry:

Dipole Moment:

8. Molecule:

Lewis Structure

Pair Arrangement:

Bond Angle:

Molecular Geometry:

Dipole Moment:

9. Molecule:

Lewis Structure

Pair Arrangement:

Bond Angle:

Molecular Geometry:

Dipole Moment:

53

MOLECULAR STRUCTURES AND SHAPES (Cont)

10. Molecule:

Lewis Structure

Pair Arrangement:

Bond Angle:

Molecular Geometry:

Dipole Moment:

11. Molecule:

Lewis Structure

Pair Arrangement:

Bond Angle:

Molecular Geometry:

Dipole Moment:

12. Molecule:

Lewis Structure

Pair Arrangement:

Bond Angle:

Molecular Geometry:

Dipole Moment:

54

EXPERIMENT

Molecular Structures and Shapes

Name: _____________________

Section: ______________
Pre-Laboratory Questions

1. What is the main principle of VSEPR theory?

2. According to VSEPR theory, what effect does the presence of a double or triple bond
between two individual atoms have on the overall geometry of a molecule?

3. How do lone pairs of electrons on a particular atom affect its bond angles?

55

EXPERIMENT

Molar Mass: Volatile Liquid

OBJECTIVE:
The mass of the vapor of a volatile liquid will be measured and, using the ideal gas law, the
molar mass of the liquid will be determined.

INTRODUCTION:
Jacques Charles, Robert Boyle and Amadeo Avogadro investigated separately the
relationship between pressure, volume and temperature of an ideal gas. This relationship
is expressed in terms of the ideal gas equation:

PV = nRT
where P = pressure (atm); V = volume (L); T = temperature (K); n = number of moles and
R = ideal gas constant or 0.0821 L atm/K mole.
The number of moles (n) can be expressed in terms of the mass of the gas sample (m)
and its molar mass (Mm)
m
n =
Mm
This expression can be substituted into the ideal gas equation to give
PV = (

m
) RT
Mm

Solving for the molar mass


Mm

mRT
PV

indicates that there is a useful means of determining the molar mass of a substance from
measurements of mass, temperature, pressure and volume of a gas sample. This directly
yields the molecular weight (MW), since the MW in amu is numerically equal to the molar
mass (M) expressed in grams/mole.
Many substances show ideal gas behavior at low pressures and at temperatures above the
boiling point. In this experiment, a sample of a volatile liquid is vaporized in a flask of
known volume. The air originally present in the flask is swept out by the gas produced
from the liquid sample during the vaporization process. The vaporized sample is assumed
to act as an ideal gas and the number of moles of vaporized sample in the flask is
calculated from the ideal gas law using its pressure and its absolute temperature, the
volume of the flask and the ideal gas constant. The gas pressure is equal to the
atmospheric (barometric) pressure because the flask is not sealed.
56

Upon cooling the vaporized sample remaining in the flask condenses and air re-enters the
flask. The difference between the mass of the flask containing the condensed sample and
the mass of the empty flask is the mass of the volatile liquid that filled the flask in the vapor
form.

Safety Precautions:

Wear safety glasses at all times while in the laboratory.


Assume that the vapors of your as liquid are toxic. Work in a fume
hood.

PROCEDURE:

Record all data and observations directly into your notebook in ink.

1.

Prepare a 125-mL Erlenmeyer flask by cleaning the flask and then drying it
completely. The flask must be completely dry, since any water present will vaporize
under the conditions of the experiment and will adversely affect the results.

2.

Cut a square of thick (freezer) aluminum foil to serve as a cover for the flask. Trim the
edges of the foil so that it neatly covers the mouth of the flask but does not extend far
down the neck.

3.

Prepare a beaker for use as a heating bath for the flask. The beaker must be large
enough for most of the flask to be covered by boiling water when in the beaker. Add
the required quantity of water to the beaker. Set up the beaker on a ring stand over a
Bunsen burner, but do not begin to heat the water bath yet.

4.

Weigh the dry, empty flask with its foil cover.

5.

Add 3-4 mL of a volatile liquid to the dry Erlenmeyer flask. Cover the flask with the foil
cover, making sure that the foil cover is tightly crimped around the rim of the flask.
Punch a single small hole in the foil cover with a needle or pin.

6.

Heat the water in the beaker to boiling. When the water in the beaker begins to boil,
adjust the flame of the burner so that the water remains boiling but does not splash
from the beaker.

7.

Immerse the flask containing the liquid in the boiling water so that most of the flask is
covered with the water of the heating bath. Clamp the neck of the flask to maintain the
flask in the boiling water.

8.

Watch the liquid carefully. The liquid will begin to evaporate rapidly, and its volume
will decrease. The amount of liquid placed in the flask is much more than will be
necessary to fill the flask with vapor at the boiling water temperature. Excess vapor
will be observed escaping through the pinhole made in the foil cover of the flask.

57

9.

When it appears that all the liquid has vaporized, and the flask is filled with vapor,
continue to heat for 1-2 more minutes. Then remove the flask from the boiling water
bath; use the clamp on the neck of the flask to protect your hands from the heat.

10. Set the flask on the lab bench, remove the clamp, and allow the flask to cool to room
temperature. Liquid will reappear in the flask as the vapor in the flask cools. While
the flask is cooling, measure and record the exact temperature of the boiling water in
the beaker, as well as the barometric pressure in the laboratory.
11. When the flask has cooled completely to room temperature, carefully dry the outside
of the flask to remove any droplets of water. Then weigh the flask, foil cover, and
condensed vapor to the nearest 0.001 g.
12. Repeat the experiment with another 3-4 mL sample of the volatile liquid.
13. Fill the flask to the very rim with tap water, cover with the foil cover, and weigh the
flask, cover, and water to the nearest 0.001 g. Determine the temperature of the tap
water in the flask. (Using the density of water at this temperature, the mass of the
water in the flask can be related to the volume of the water in the flask which
represents the volume of the vapor.)

CALCULATE:
1.

The molar mass of the volatile liquid from the separate experiments, and the average.

DISCUSSION:
In a paragraph, comment on how well the objectives of the experiment were met.
If a true or accepted value is known, discuss the accuracy of your results and
suggest potential sources of experimental error.

58

EXPERIMENT

Molar Mass: Volatile Liquid


Name:

_________________________________ Section:

__________

Pre-Laboratory Questions:
1. A student collected the following data using the procedure given in this experiment:
Atmospheric pressure = 30.04 in Hg
0
Temperature of boiling water = 101.4 C
Temperature of water in flask = 21.8 0C
Mass of empty flask = 85.167 g
Mass of flask containing condensed sample = 85.532 g
Mass of flask filled with water = 218.723 g
0
Density of water at 21.8 C = 0.9978 g/ml
a)

Calculate the volume of the flask.

b)

Calculate the mass of the vaporized sample.

c)

Convert the temperature of the boiling water to Kelvin.

d)

Express the pressure in units of atmospheres.

e)

Calculate the molar mass of the volatile liquid.

59

EXPERIMENT

Freezing - Point Depression

OBJECTIVE:
Colligative properties of solutions depend only on the quantity of solute dissolved in the
solvent, but not on the identity of the solute. The aim of this experiment is to determine
the freezing point depression TF, a colligative property, of acetic acid resulting from the
addition of a solute.
INTRODUCTION:
When a solute is dissolved in a solvent, the properties of the solvent are affected by the
presence of the solute, and the relative magnitude of the change in properties is normally
proportional to the amount of solute added. Some properties, such as vapor pressure,
freezing point depression, boiling point elevation, and osmosis, vary normally with the
amount of solute but are independent of its particular molecular size and nature, and
therefore its identity. Such properties are called colligative properties.
In this experiment, the freezing point of glacial (pure) acetic acid will be determined by
cooling a sample, and recording the variation of temperature with time. The physical
processes involved will be: cooling of the liquid; change of state from liquid to solid,
which occurs at constant temperature; and cooling of the solid when no more liquid is
left. Note that it is important to ensure that the temperature of the sample is kept uniform
by stirring, otherwise localized solidification may occur which will distort temperature
readings. The freezing point determination will then be repeated, using a solution of
known concentration of benzoic acid, C6H5COOH, in acetic acid, and finally a solution of
the same concentration of acetamide, CH3CONH2, in acetic acid. In theory the
depression of the freezing point from the normal freezing point of acetic acid should be
the same for both solutions.
The decrease in freezing point, Tf, produced by the addition of a non-volatile,
non-ionizing solute to a solvent is directly proportional to the molal concentration, m, of
solute present in the solvent:
Tf = -Kfm
Note that Tf is defined as the freezing point of the solution minus the freezing point of
the pure solvent, and so will be a negative number. The constant of proportionality, Kf, is
called the molal freezing point depression constant, and represents how many degrees
the freezing point will change when 1 mole of solute is dissolved per kilogram of solvent.
It has a constant value for any particular solvent, and values for common solvents can
be obtained from chemistry handbooks.
The molal concentration, or molality, m, of the solution is defined by:
m =

Moles of Solute
Kilograms of Solvent
60

If the solute ionizes, the effect on the freezing point of the solvent will be larger, because
the ionization of the solute produces more solute particles (ions) than the formal
concentration of the solution indicates.
Finally, rapid cooling may lead to a situation in which the freezing point temperature is
reached before the liquid has achieved the degree of organization necessary to form the
solid state. Therefore, liquid continues to exist below the freezing point, but the correct
ordering then occurs at some point and the solid forms very quickly, which releases heat
that returns the temperature to the freezing point. This phenomenon is called
supercooling.

PROCEDURE:
A.

Determination of the freezing point of acetic acid


Weigh out 10.0 g of glacial acetic acid, pour into a 25 x 200 mm test tube, insert a
thermometer, and record the initial temperature to the nearest 0.2C. Using a
600 mL beaker, prepare an ice bath by placing four to six ice cubes in the beaker
and adding water to a depth of 2 to 3 inches.
Supercooling is encouraged if the ice bath is made too cold and so the rate of
freezing is high. Use a thermometer in the ice bath to monitor its temperature and
aim to keep the temperature in the bath around 6 0C.
Place the test tube into the ice bath and record the temperature to the nearest 0.2C
every 15 seconds, using the thermometer to stir the acetic acid gently and
continuously until the temperature becomes constant.
Record the temperature for at least 8 minutes, after which, if the temperature has
remained constant at any stage for several minutes, stop recording.

Safety note:
This part of the experiment is finished, but any attempt to remove the thermometer
from the solid acetic acid will probably break it. Remove the test tube from the ice
bath and run tap water over the outside or hold it until the acetic acid melts and the
thermometer can be removed.
After the thermometer has been removed safely, dispose of the waste acetic acid in
the waste container provided.

B. Determination of freezing point depression


When all the acetic acid used in part A has melted, place in a beaker and check the
mass again, adding more if necessary, to ensure you have 10.0 g. Calculate how
much benzoic acid (molecular formula C6H5COOH) you need to add to 10.0 g of
solvent in order to prepare a 1.5 molal solution. Check your calculation with your
instructor before proceeding any further. Prepare the 1.5 molal solution by
adding the correct amount of benzoic acid to the 10.0 g of acetic acid, using the
thermometer to stir gently as an aid to the dissolving process.
61

Record the initial temperature when all the benzoic acid has dissolved, place the
solution in the test tube, and use the ice bath to repeat the procedure in part A for
the determination of the freezing point of the solution.
On completion of this temperature-time recording, remember to warm the test tube
before attempting to remove the thermometer.
When all the solution has melted, pour it into the waste container provided.
Now prepare a 1.5 molal solution of acetamide (molecular formula CH3CONH2) in
10.0 g of glacial acetic acid. Again, check your calculation of the mass of
acetamide required with your instructor before proceeding any further. Repeat the
procedure, as outlined above for benzoic acid, and determine the freezing point of
this solution by recording the variation of temperature with time.
On completion, warm the test tube, remove the thermometer and put the melted
solution in the waste container. Rinse all equipment used, and wash your hands
thoroughly before leaving the laboratory.

Waste disposal:
All waste chemicals from this experiment must be placed in the waste
container provided.

CALCULATIONS:
Construct a cooling curve (a graph of temperature versus time, with time as the
horizontal axis) for each cooling process. These three cooling curves can be combined
onto one graph by the use of different symbols, and/or colors, for each set of
measurements.
Estimate the freezing point temperature, TF, for acetic acid and both solutions, to the
nearest 0.2C, from your graphs. Hence, calculate the freezing-point depression, TF,
relative to glacial acetic acid, for each solution.
Write out a detailed calculation of the amount of solute to be added to 10 g of acetic acid
in order to produce a 1.5 molal solution, for one of the solutions.
Calculate the molal freezing-point depression constant, KF, for acetic acid, using the
freezing-point depression (TF) values, for both solutions. Show one such calculation in
detail.
Obtain the accepted value of the molal freezing-point depression constant, KF, for acetic
acid from a handbook.

DISCUSSION:
In a paragraph, comment on how well the objectives of the experiment were met. If a true
or accepted value is known, discuss the accuracy of your results and suggest potential
sources of experimental error.
62

Environmental Science Note:


One of the main practical applications of the concept of freezing-point depression is the practice
of adding antifreeze to the water in automobile radiators. The idea is to mix significant
quantities of a relatively non-volatile substance with the water so that the resultant vapor
pressure of the solution is decreased, compared to that for pure water, and therefore the
freezing point of the solution is lowered.
As the amount by which the freezing-point is lowered is directly proportional to the molality of
the solution, and therefore moles of solute, the ideal solute for use as antifreeze should have:
- a low molecular weight, so that the mole per unit mass ratio is high ;
- a high boiling point (ie, low volatility), so that the solute is not readily lost by
evaporation ;
- high solubility in water.
The solute commonly used as antifreeze is ethylene glycol, C2H6O2, which is a sweet,
somewhat viscous liquid, with a relatively low molecular weight. This molecule contains
0
extensive hydrogen bonding, so it has a high boiling point (198 C), and it is completely miscible
with water. A 60% solution of ethylene glycol in water will not freeze until the temperature
reaches -490C (-560F).
Unfortunately, ethylene glycol is also quite toxic to all animal life. This was highlighted in the
1980s when some Austrian wine producers, after a cold summer did not fully ripen, and
therefore sweeten, the grapes, added ethylene glycol to the wine to create the customary
sweetness. Enzymes in the liver oxidize the ethylene glycol to oxalic acid, which then
precipitates in the kidneys as crystalline calcium oxalate. Drinkers of this Austrian wine were all
treated for severe kidney damage.
Consequently, the use and disposal of antifreeze and solutions of water and ethylene glycol are
controlled by law, and much publicity is given to the dangers of accidentally exposing pet
animals to antifreeze.

63

EXPERIMENT

Freezing - Point Depression

Name : ____________________________

Section : ____________

Pre-Laboratory Questions
1. Define colligative property.

2. List three examples of colligative properties.

3. Which of the following aqueous solutions would have the greatest freezing point depression?
Explain your answer.
0.8 m calcium bromide, CaBr2
1.0 m sodium chloride, NaCl ;
1.5 m benzoic acid, C6H5COOH ;

64

EXPERIMENT

10

Solution Stoichiometry:
Acid-Base Standardization

OBJECTIVE:
A sodium hydroxide (NaOH) solution of unknown concentration will be standardized by the
process of titration using a weighed sample of a known acid salt. In addition, the
concentration of hydrochloric acid (HCl) solution will be determined using this standardized
NaOH solution.

INTRODUCTION:
The technique of titration finds many applications, but is especially useful in the analysis of
acidic and basic substances. Titration is the measuring of the exact volume of a solution of
unknown concentration that is required to react with a measured volume of a solution of
known concentration, or with a weighed sample of a known solid. In this way the solution
is standardized, i.e., its concentration determined. A solution of accurately known
concentration is called a standard solution.
In many cases (especially with solid solutes) it is possible to prepare a standard solution by
accurately weighing the solute, followed by precise dilution to an exact volume in a
volumetric flask. Such a standard is said to have been prepared determinately. One of the
most common standard solutions used in analyses, NaOH, however, cannot be prepared in
this manner.
Solutions of NaOH are commonly used in titration analyses of samples containing an acidic
solute. Although NaOH is a solid, it is not possible to prepare standard NaOH solutions by
weight. Solid NaOH is usually of questionable purity. NaOH reacts with CO2 from the
atmosphere and is also capable of reacting with the glass of the container in which it is
provided. For these reasons, NaOH solutions are generally prepared to be approximately
a given concentration. They are then standardized by titration of a weighed sample of a
primary standard acidic substance. By measuring how many milliliters of the
approximately-prepared NaOH are necessary to react completely with the weighed sample
of the primary standard, the concentration of the NaOH solution can be calculated.
In today's lab a roughly 0.2 M NaOH solution has been prepared and will be standardized
against the primary acid standard, potassium hydrogen phthalate (KHP).

(__) g KHP x

1 mole KHP_ x 1 mole NaOH x


1_____
204.2 g KHP
1 mole KHP
(__) L NaOH

65

= (__) M NaOH

The titration of KHP and NaOH will be done twice and the result averaged. The now
standardized NaOH solution will be used as a secondary standard to determine the
molarity of a HCl solution.

(__) L NaOH x (__) moles NaOH x 1 mole HCl _


1 L NaOH
1 mole NaOH

1____
(__) L HCl

(__) M HCl

In titration analyses, there must be some means of knowing when enough titrant has been
added to react exactly and completely with the sample being titrated. In an acid/base
titration analysis, there should be an abrupt change in pH when the reaction is complete.
For example, if the sample being titrated is an acid, then the titrant to be used will be basic
(probably sodium hydroxide). When one excess drop of titrant is added (beyond that
needed to react with the acidic sample), the solution being titrated will suddenly become
basic. There are various natural and synthetic dyes, called indicators, that exist in different
colored forms at different pH values. A suitable indicator can be chosen that will change
color at a pH value consistent with the point at which the titration reaction is complete.
The indicator to be used in this experiment is phenolphthalein, which is colorless in acidic
solutions, but changes to a pink form at basic pH.

Safety Precautions: Wear safety glasses at all times while in the laboratory.

PROCEDURE:
Record all data and observations directly into your notebook in ink.
For precise quantitative work, volumetric glassware must be scrupulously clean. Water
should run down the inside of burets in sheets and should not bead up anywhere on the
interior of the glassware. Rinse the buret with distilled water to see if they are clean.
If not, partially fill with a few milliliters of soap solution, and rotate the buret so that all
surfaces come in contact with the soap.
Rinse with tap water, followed by several portions of distilled water. If the burets are still
not clean, they should be scrubbed with a buret brush.
Standardization of NaOH solution

1.

Obtain approximately 100 mL of the prepared 0.2 M NaOH. Pour approximately 4-5
mL of the solution into the buret to rinse out any remaining distilled water. Fill buret to
approximately 0 mL mark and open stopcock letting solution flow through tip removing
any air bubble. Note the beginning volume of sodium hydroxide in your buret to the
nearest 0.01 mL.

66

2.

Weigh approximately 1 g of KHP into your Erlenmeyer flask, recording exact weight of
sample to the nearest 0.001 g. Add approximately 50 mL of distilled water to the flask.
Swirl flask until solid KHP is totally dissolved. Add a few drops of phenolphthalein
indicator.

3.

Begin adding the NaOH solution from the buret to the sample in the Erlenmeyer flask,
swirling the flask constantly during the addition. The NaOH solution is approximately
0.2 M. Based on the amount of KHP taken (approximately 1 g) the end point should
be approximately 25 mL:

1 g KHP x

1 mole KHP x 1 mole NaOH x


1 L NaOH____ = 0.025 L NaOH
204.2 g KHP
1 mole KHP
0.2 moles NaOH

As the NaOH solution enters the solution in the Erlenmeyer flask, streaks of red or
pink will be visible. They will fade as the flask is swirled. Eventually the red streaks will
persist for a longer and longer period of time. This indicates the approach of the
endpoint of the titration. Begin adding NaOH one drop at a time, with constant
swirling, until one single drop of NaOH causes a permanent pale pink color that does
not fade away on swirling. Record the reading of the buret to the nearest 0.01 mL.
4.

Repeat the titration with another weighed sample of KHP (see step 2).

Standardization of HCl solution

5.

Refill buret with the now-standardized solution of NaOH, noting the starting volume to
the nearest 0.01 mL.

6.

Weigh an Erlenmeyer flask on a balance. Pour approximately 25 mL of the 0.2 M HCl


into the flask and note the weight to the nearest 0.001 g. It is assumed that the
density of HCl is 1.000 g/mL. Based on this assumption the weight of the solution in
grams is equivalent to the volume of the solution in milliliters.

7.

Add a few drops of phenolphthalein indicator. Begin adding the standardized NaOH
solution from the buret to the flask. Based on 25 mL of the approximately 0.2 M HCl,
and a concentration of the NaOH solution in the 0.2 M range, the endpoint for the
titration should be approximately 25 mL.

0.025 L HCl x 0.2 moles HCl x 1 mole NaOH x


1 L NaOH____ = 0.025 L NaOH
1 L HCl
1 mole HCl
0.2 moles NaOH

8.

Repeat this titration with another weighed sample of HCl. Again record both initial and
final readings of the buret to the nearest 0.01 mL.

67

Waste Disposal:

All of the solutions in this lab may be flushed down the sink with an
excess of water.

CALCULATE:
1.

The molarity of the NaOH solution from the two separate titrations, to three significant
figures.

2.

An average molarity for the NaOH solution.

3.

Repeat steps 1 and 2 for the HCl solution.

DISCUSSION:
In a paragraph, comment on how well the objectives of the experiment were met.
If a true or accepted value is known, discuss the accuracy of your results and
suggest potential sources of experimental error.

68

EXPERIMENT

10

Solution Stoichiometry: Acid-Base Standardization

Name: ___________________________________

Section: __________

Pre-Laboratory Questions:
1. Suppose a sodium hydroxide solution were to be standardized against pure solid primary
standard grade KHP. If 0.843 g of KHP requires 18.3 mL of the sodium hydroxide solution to
reach a phenolphthalein endpoint, what is the molarity of the NaOH solution?

2. If a solution of unknown concentration of HCl weighs 22.64g and takes 19.5 mL of


0.221 M KOH to be neutralized, what is the molarity of the acid?

69

EXPERIMENT

11

Acid/Base Titration:
Solution Analyses

OBJECTIVE
Using titration techniques the percent acetic acid in vinegar and the percent ammonia in
household ammonia will be calculated.
INTRODUCTION
The technique of titration finds many applications, but is especially useful in the analysis of
acidic and basic substances. Titration is the measuring of the exact volume of a solution of
known concentration that is required to react with a measured volume of a solution of
unknown concentration, or with a weighed sample of an unknown solid. In this way the
solution is standardized, i.e., its concentration is determined. A solution of accurately
known concentration is called a standard solution.
The goal of every titration is the careful addition of standard solution until an equivalent
molar amount of reactants is present. This is called the equivalence point. For example,
the equivalence point in titration of sodium hydroxide with hydrochloric acid is attained when
exactly one mole equivalent of sodium hydroxide has been added for every mole equivalent
of hydrochloric acid in the sample. The equivalence point is a theoretical concept and in
actual practice can only be estimated by observing physical changes in the solution. The
point in the titration where such changes occur is called the end point. In a well-designed
titration experiment, the volume differences between the end point (observed) and the
equivalence point (theoretical) will be small.
In titration analyses, there must be some means of knowing when enough titrant has been
added to react exactly and completely with the sample being titrated. In an acid/base
titration analysis, there is an abrupt change in pH when the reaction is complete. For
example, if the sample being titrated is an acid, then the titrant will be basic (probably
sodium hydroxide). When one excess drop of titrant is added (beyond that needed to react
with the acidic sample), the solution being titrated will suddenly become basic.
There are various natural and synthetic dyes, called indicators, that exist in different colored
forms at different pH values. A suitable indicator can be chosen that will change color at a
pH value consistent with the point at which the titration reaction is complete. A common
indicator used in titrations is phenolphthalein, which is colorless in acidic solutions, but
changes to a pink form at basic pH. The text book describes other common indicators and
the pH range of their color transition.
In todays laboratory exercise, titration techniques will be employed to analyze vinegar and
household ammonia. Vinegar contains a certain percentage of acetic acid (HC2H3O2) which
gives vinegar its distinctive bite. Household ammonia contains only a small percentage of
ammonia (NH3), the rest being water. These percentages will be calculated in todays lab
experiment.
70

PROCEDURE

For precise quantitative work, volumetric glassware must be scrupulously clean. Water
should run down the inside of burets in sheets and should not bead up anywhere on the
interior of the glassware.
Rinse the buret with distilled water to see if it is clean. If it is not, partially fill the buret with a
few milliliters of soap solution and rotate it so that all surfaces come in contact with the
soap. Rinse with tap water, followed by several portions of distilled water. If the buret is still
not clean, it should be scrubbed with a buret brush.

Percent acetic acid in vinegar


1. Obtain approximately 60 mL of the prepared standard solution (0.200 M sodium
hydroxide). Pour approximately 4-5 mL of the solution into the buret to rinse out any
remaining distilled water. Fill buret to approximately the 0 mL mark and open the
stockcock letting the solution flow through the tip removing any air bubbles. Note the
beginning volume of sodium hydroxide in your buret to the nearest 0.1 mL.
2. It is assumed that the vinegar contains 5% acetic acid. Calculate how much vinegar
must be weighed out so that the endpoint requires 25 mL of the standard sodium
hydroxide solution for the phenolphthalein endpoint. (Remember, if density is
assumed to be 1.00 g/mL, then the volume of your solution in mL will equal the mass in
grams.) Weigh your vinegar in an Erlenmeyer flask and add a few drops of
phenolphthalein indicator. Add a stir bar and place the flask on a magnetic swirler.
3. Begin adding the NaOH solution from the buret to the sample of vinegar in the
Erlenmeyer flask, swirling the flask constantly during the addition. As the sodium
hydroxide solution enters the standard solution in the flask, streaks of red or pink will be
visible. They will fade as the flask is swirled. Eventually the red streaks will persist for a
longer and longer period of time. This indicates the approach of the end point of the
titration. At this point, begin adding NaOH one drop at a time, until one single drop of
NaOH causes a permanent pale pink color that does not fade on swirling. Record the
reading of the buret to the nearest 0.1 mL.
4. Repeat the titration with another sample of vinegar.

Percent ammonia in household ammonia.

1. Dispose of the rest of the solution in the buret in the sink. Wash the buret with distilled
water. Obtain approximately 60 mL of the standard solution of 0.200 M hydrochloric
acid. Pour approximately 4-5 mL of the solution into the buret to rinse out any remaining
distilled water. Fill the buret to approximately the 0 mL mark and open the stopcock
letting the solution flow through the tip removing any air bubbles. Note the beginning
volume of HCl in your buret to the nearest 0.1 mL.

71

2. It is assumed that household ammonia contains 3% ammonia. Calculate how much


ammonia must be weighed out so that the end point requires 25 mL of your
hydrochloric acid solution for the methyl red end point. Weigh the household ammonia
in an Erlenmeyer flask and add a few drops of methyl red indicator.
3. Titrate the household ammonia sample with HCl.
4. Repeat the titration with another sample of household ammonia.

CALCULATE

1. Percent acetic acid in vinegar from the two titrations.


2. Average percent acetic acid in vinegar.
3. Percent ammonia in household ammonia from the two titrations.
4. Average percent ammonia in household ammonia.

DISCUSSION

In a paragraph, comment on how well the objectives of the experiment were met. If a true or
accepted value is known, discuss the accuracy of your results and suggest potential sources
of experimental error.

72

EXPERIMENT

11

Acid/Base Titrations : Solution Analyses

Name: ____________________________________

Section: ________________________

Pre-Laboratory Questions
1. If a sample of household ammonia weighing 27.5 g took 19.8 mL of a 0.221 M HCl solution to
be neutralized, what percentage of ammonia was there in the household ammonia?

2. If you assume that there is 5% acetic acid in vinegar, how much vinegar should you weigh out
so that the endpoint requires 25.0 mL of 0.186 M NaOH?

73

APPENDIX

Laboratory Practical
Test Study Guide

1. LABORATORY EQUIPMENT AND TECHNIQUES


A. What do you use in the laboratory to measure most accurately?
Mass?
Volume?
Temperature?
End-point of a titration?
pH?
B.

What are the techniques involved in:


measuring mass by difference?
measuring volume by difference?
reading the level of a liquid meniscus?
using the Buchner funnel for suction filtration?
titration?

C.

Can you recognize a/an:


evaporating dish?
scoopula?
crucible?
watch glass?
erlenmeyer flask?
test tube clamp?
clay triangle?

74

D.

What is the problem with:


weighing a hot beaker?
using tap water?
weighing chemicals directly onto a balance?
using wet equipment?
using the same indicator for all titrations?
preparing a standard solution of NaOH?

2. EXPERIMENTAL CONCEPTS
A.

Give the meaning of the following.


Density
Homogeneous mixture
Heterogeneous mixture
Percent composition by mass
Sublimation
Filtration
Solubility
Solute
Solvent
Solution
Molarity
Dilute
Concentrated
Saturated
Concentration
Precipitate
Percent yield

B.

Acid
Base
Limiting reagent
Standard solution
Indicator
Freezing Point Depression
Cooling Curves
pH
Saturated Vapor Pressure
Salt
Ion
Colligative Property
Resonance
Dipole Moment
Octet Rule
Molecular Geometry
Bond Angle

How can you change the:


volume of a gas?
concentration of a solution?
purity of a mixture?
yield of a reaction?
color of an indicator?
pH of a solution?

75

3. FORMULAS, EQUATIONS, CALCULATIONS

A. The mass of a beaker is measured to be 24.614 g on a centigram balance. When a


steel object is placed in the beaker, the mass is measured to be 61.582 g. What is the
mass of the steel object?
If the steel object on its own is measured at 37.148 g on the same balance, which
measurement is more accurate? What correction could you apply when using that
same balance again?

B. What is the approximate volume of 27.5 g of water?

C. When a rubber stopper of mass 4.22 g was immersed in a graduated cylinder containing
17.8 mL of water, the water level rose to 20.4 mL. Calculate the density of the rubber
stopper. If air bubbles had remained attached to the rubber stopper when immersed,
would your calculated density be too high or too low?

D. After separating a mixture into its component compound parts, you found that you had
4.07 g NaCl, 4.32 g SiO2, and 3.23 g NH4Cl. Calculate the percentage composition by
mass of the mixture for each component.

E. The balanced equation for the reaction between sodium carbonate and hydrochloric acid is:
Na2CO3 (s)

2HCl (aq)

2NaCl (aq)

H2O (l) +

CO2 (g)

If 2.45 g of pure sodium carbonate is treated with excess hydrochloric acid, how many
grams of sodium chloride will theoretically be produced?
If your actual yield is 1.54 g of sodium chloride, what is the percent yield of this reaction?

F. Calculate the percentage by mass of magnesium in magnesium oxide, MgO.

G. The balanced equation for the reaction between calcium chloride and sodium phosphate
in aqueous solution is:
3CaCl2 (aq) +

2Na3PO4 (aq) 6NaCl (aq)

Ca3(PO4)2 (s)

Calculate the mass of calcium phosphate that can theoretically be produced from the
reaction between 8.00 mL of 0.500 M CaCl2 and 12.00 mL of 0.500 M Na3PO4 solutions.

76

H. You performed an experiment in which you boiled a volatile liquid in a flask, using a hot
water bath, until the liquid had all evaporated. A small hole in the lid of the flask allowed
the pressure to remain constant throughout. When the flask was cooled to room
temperature, the gas condensed. Various measurements were taken:
Atmospheric pressure
Temperature of boiling water
Room temperature
Mass of empty flask
Mass of flask + condensed sample
Mass of flask filled with water
Density of water at 24.8 0C

=
=
=
=
=
=
=

761.6 torr
99.6C
24.8C
155.263 g
156.074 g
398.518 g
0.997 g/mL

Calculate the volume of the flask.

Calculate the molar mass of the volatile liquid.

I. Describe the following molecules by drawing a Lewis Structure diagram and predicting
the electron-pair arrangement, bond angle, molecular geometry, and presence of a
dipole moment :
SF2 , ICl41- , CS2 , BCl3 .
J.

Sodium hydroxide solution and KHP (M.W. = 204.2 g/mol) react in a 1:1 mole ratio. If
0.454 g of KHP requires 23.2 mL of a sodium hydroxide solution to reach an endpoint,
calculate the molarity of the sodium hydroxide solution.

K.

Calculate the molal freezing-point depression constant for benzene, C6H6, if its normal
freezing-point temperature is 5.45 0C but a solution prepared by dissolving 1.37 grams of
acetamide, CH3CONH2 , in 25.0 grams of benzene freezes at 0.75 0C.

L.

Calculate the percentage by mass of acetic acid, HC2H3O2 , in vinegar if it takes


21.5 mL of 0.210 M KOH to neutralize 7.04 g of vinegar.

77

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