WOLLEGA UNIVERSITY

COLLEGE OF NATURAL AND COMPUTATIONAL SCIENCE

DEPARTMENT OF CHEMISTRY

LABORATORY MANUAL FOR GENERAL CHEMISTRY

Prepared by Kemal .M (BSc)

Edited by Chala. B (MSc)

August, 2020

Nekemte, Ethiopia
To the Student
To work in the laboratory most efficiently, youshould read the
experimental procedures in advance and understand in detail before you
started the laboratory works.

Afteryou did the experiment; try to answer the review questions at the
end of each experiment. These questions will help you to understandthe
experiment in advance.

Chemistry is an experimental science. Therefore, chemistsperform basic

experimental analysis.Qualitativeanalysis– to determine the nature of
processes, which are oftenunanticipated and sometimes unpredictable

Quantitativeanalysis – to determine the amount of a measurable change

in mass, volume, or temperature etc. For example, including the time
rate of change onprocesses for which the qualitative data are already
known.

It is much easier to appreciate and comprehend the science of

Chemistry, if you actually participate in experimentation. Although there
are many descriptions of the scientific method, the reasoning process
involved is difficult to appreciate without performing
experiments.There are four objectivesfor the students, in the
laboratory:
  To develop the skills necessary to obtain and evaluate a reliable
original result.
 To record your results for future use.
 To be able to draw conclusions regarding your results (with the aid
of somecoaching and reading in the beginning).
 To learn to communicate your results critically and
knowledgeably.

By attentively reading over the experimental procedures in detail, and

carefully followingdirections you cansafely able to accomplishthe
Best wishes for
objectivesin an laboratory.
the error-free and accident-free term!

Laboratory report format

A laboratory report is a written composition of the results of the experiment.Laboratory reports

explain what you did in experiment, what you learned and what the result meant. It should be
written precisely and clearly, using good grammar and punctuation. The laboratory report
formats differ depending up on the type of experiment that you do but the general format
includes the following main points.

1) Cover page

The cover page should contain the following:

 Name of the University

 The name of your college and department
 Experiment number
  Experiment title
 Your name and name of any laboratory partners
 Your instructor’s name
 The date the laboratory was performed
2) The title of the experiment

The title of the experiment reflects the nature (factual content) of the work. The title says what
you did. It should be brief and describe the main point of the experiment or investigation.

3) Purpose or objective of experiments

Objective state the purpose of the experiment and outlines the significant goals intended to be
learned from each experiments. Objective should be specific and has to be written using smart
words. The objective should answer the questions, what will the student know after completing
the experiment and what will student be able to do after completing the experiment?

4) Theory/introduction

Theory explains the background of the experiment briefly. It is usually written in few lines. The
object of theory is to give the reader a sense what you are doing, why you are doing it in the way
you are doing the experiment, and what the results you have determined. It should not directly
copy from the laboratory manual.

5) Apparatus and chemicals

List of all chemicals and apparatus you used for doing the experiment. Sometimes it is necessary
to provide the specification of the chemicals and apparatus used.

6) Procedure

A procedure refers to details of steps followed, in chronological order, while doing the
experiment. A procedure has to be written using passive voice. It is very important that you read
and understand the procedure before you start working.

7) Data and observation

a) Enter data into the notebook as the work is being performed. This means that loose pieces of
paper used for the intermediate recordings are prohibited.
b) Write the chemical reaction that takes place, if available.

c) Show the mathematical formulas utilized for all calculations and also a sample calculation.

d) Construct data tables whenever useful and appropriate. Numerical data obtained from your
procedure usually is presented as a table. Data encompasses what you recorded when you
conducted the experiment. It’s just the facts, not any interpretation of what they mean.

e) Both numerical data and important observation should be recorded.

f) Experimental data should be presented, with the correct units, neatly and succinctly in tabular
and/or graphical form rather than verbally.

g) Data should be presented in chart or graph form. All charts and graphs must have a title.
Columns and rows of charts should be labeled. Axes of graphs should be labeled and units given
in the label. Any data manipulation, such as equations or calculations, should be included and
explained briefly.

8) Results and discussion

Interpretation of data and comparisons with the literature are presented in this section. Describe
in words what the data means. This is where you interpret the data and determine whether or not
a hypothesis was accepted. This is also where you would discuss any mistakes you might have
made while conducting the investigation. You may also wish to describe ways the study might
have been improved. This is the section where the results are explained, and a student can show
the instructor that he or she has a thorough understanding of the concept of the experiment and
the results obtained.

This is probable the most important section of the lab report. It is here that you report your
experimental data, analyze and interpret your results, and draw specific conclusions.Discussion
of results is a concise interpretation of the results.

9) Conclusion

This section summarizes the pertinent concepts discussed in the results and discussion section.
The conclusion should restate the result of the experiment. Conclusion should be brief, as it
refers back to the objectives and considers how and to what degree they have been met. Review
the purpose of the experiment and summarize the implication of the experiments.
Experiment 1: Introduction to Laboratory Safety Rules

General Objective: To become acquainted with the safety rules for working with chemicals and
participating in a safe manner when carrying out laboratory procedures

Theory
The chemistry laboratory may be considered as a place of discovery and learning. However, by
very nature of laboratory work, it can be a place of danger if precautions are not taken. Therefore
it is necessary to take care of your own health and safety and that of others working in the
laboratory. The responsibility for laboratory safety rules with each and every student in the
laboratory. You must use common sense and work carefully to avoid chemical spills, broken
glassware, and fires. This ensures not only your own safety, but that of your laboratory mates.
Knowing the level of hazards of each chemical you are using, make you ready the care you can
do during laboratory session. Doing that, you will not expose to any harmful chemicals during
your laboratory work.

The compounds you are doing with may havehazardous properties associated with them. So it is
important to follow the safety rulesoutlined in the manual such as: safety goggles for eye
protection arerecommended and laboratory coats are to be worn by the students always when
they are working in the chemistrylaboratory. Always don’t forget to wash your hands thoroughly
when you are leaving the laboratory.

The location and use of thesafety equipment in laboratory will be reminded byyour instructor the
first day of your laboratory class and you should become familiar with theproper use of the
safety equipment location and their use. Examples shower, eye-wash fountain, fire blanket and
fire extinguisher.

 Report any accidents which occur immediately to the laboratory supervisor.

Safety rules

The laboratory can be but is not necessarily a dangerous place. When intelligentprecautions and
a proper understanding of techniques are employed, the laboratory isno more dangerous than any
other classroom. Most of the precautions are justcommon-sense practices. These include the
following:
1. Know what you have to do before entering the laboratory. Read the experiment carefully
before starting the laboratory works.
2. Do not engage in games in the laboratory. Failure to follow this rule will result in
immediate dismissal from the laboratory and subsequent conduct action.
3. Eating, drinking, and smoking are strictly prohibited in the laboratory at all times
4. Know where to find and how to use safety and first-aid equipment.
5. Wear approved eye protection when required while in the laboratory. Your safetyeye
protection may be slightly different from that shown, but it must includeshatterproof
lenses and side shields to provide protection from splashes.
6. Consider all chemicals to be hazardous unless you are instructed otherwise.Dispose of
chemicals as instructed by your instructor. Follow the explicitinstructions given in the
experiments.
7. Do not pipet solutions by mouth. Rubber pipet bulbs are provided at each laboratory
station.
8. If chemicals come into contact with your skin or eyes, wash immediately withcopious
amounts of water and then consult your laboratory instructor.
9. Never taste anything. Never directly smell the source of any vapor or gas; instead by
means of your cupped hand, bring a small sample to your nose (see figurebelow).
Chemicals are not to be used to obtain a "high" or clear your sinuses.

Figure 1.1: Wafting vapors towards one’s nose

10. Perform in the hood any reactions involving skin-irritating or dangerous chemicalsand/or
ill-smelling chemicals. A typical fume exhaust hood is shown below.
 Figure 1.2: Fume hood found in the laboratory

Exhaust hoods have fans to exhaust fumes out of the hood and away from theuser. The hood
should be used when noxious, hazardous, and flammablematerials are being studied. It also has a
shatterproof glass window, whichmay be used as a shield to protect you from minor explosions.
Reagents thatevolve toxic fumes are stored in the hood. Return these reagents to the hoodafter
their use.
11. Do not perform any unauthorized experiments.
12. Clean up all broken glassware immediately.
13. Always pour acids into water, not water into acid, because the heat of solution will cause
the water to boil and the acid to spatter.
14. Never point a test tube that you are heating at yourself or your neighbour. It mayerupt
like a geyser.

Figure 1.3: Beware of spattering

15. Avoid rubbing your eyes unless you know that your hands are clean.
16. Notify the instructor immediately in case of an accident.
17. Manycommon reagents, for example, alcohols, acetone, and especially ether, arehighly
flammable. Do not use them anywhere near open flames.
18. Observe all special precautions mentioned inexperiments.
 19. When finished with your Bunsen burner for a given portion of an experiment, turn it off.
20. Exercise good housekeeping practices in the laboratory. Be sure that the laboratory
benches remain free of disorder during the experiment. In the event of a spill, clean the
area immediately and be sure to use a wet sponge to wipe off the work station at the end
of the laboratory session.
21. Learn the location of fire protection devices.In the unlikely event that a large chemical
fire occurs, a powder extinguisher and a CO2extinguisher are available in the laboratory.

Figure 1.4: Powder and CO2extinguisher

In order to activate the extinguisher, youmust pull the metal safety ring from the
handle and then depress the handle. Directthe output of the extinguisher at the base of
the flames. The carbon dioxide smothersthe flames and cools the flammable material
quickly. If you use the fire extinguisher, be sure to return the extinguisher in atthe stockroom so
that it can be refilled immediately. If the carbon dioxideextinguisher does not extinguish the fire,
evacuate the laboratory immediatelyand call the security. One of the most frightening and
potentially most seriousaccidents is the ignition of one’s clothing.

Therefore, certain types of clothing arehazardous in the laboratory and must not be worn. Since
sleeves are most likelyto come closest to flames, any clothing that has bulky or loosesleeves
should not worn in the laboratory. Ideally,students should wear laboratory coats with tightly
fitting sleeves. Long hair alsopresents a hazard and must be tied back. If a student's clothing or
hair catches firehis or her neighbours should take prompt actionto prevent severe burns. Most
laboratories have awater shower for such emergencies. A typicallaboratory emergency water
shower has thefollowing appearance.
 Figure 1.5:A safety shower

In case someone's clothing or hair is on fire,immediately lead the person to the shower andpull
the metal ring. Safety showers generallydump 151 to 190 liters of water, which shouldextinguish
the flames. These showers cannot beshut off once the metal ring has been pulled.Therefore, the
shower cannot be demonstrated.

Table 1:1the following cases must be notified firstly to the laboratory instructor.
Burn: expose the burned area to
the tap water (5-10 min.), apply Cut / Injury: Wash with waterand apply first aid.
first aid.
Fainting: Provide fresh air. Lay Fire: (Notify the assistantimmediately) Put the bunsen
down and put the head lower than burneroff. Use shower in case of hair andclothes caches
the body. fire. Use the fireextinguisher when necessary.
Bleeding: compress on the wound, Chemical Spill:clean in amanner appropriate to the
keep the wound above the heart chemical.Aqueous solutions can be removedwith water.
level and get medical help. Information your assistant.
Acid Burns: Use NaHCO3
Chemicals Spilled in Theeye: The Eye is washed
solution
immediatelywith plenty of water for at least 15
Base Burns: Use Boric acid or
minutes (use the eye-wash showerrooms) Get medical help.
Acetic acid solution

Common Laboratory Equipment

Experiment 2: Basic Laboratory Technique

General Objective: To learn the use of common, simple laboratory equipment.

Theory

Chemistry is an experimental science. It depends upon careful observation and the use
of good laboratory techniques. In this experiment you will become familiar with some
basic operations that will help you throughout this course. Your success as well as
your safety in future experiments will depend upon your mastering these fundamental
operations.
Because every measurement made in the laboratory is really an approximation, it is
important that the numbers you record reflect the accuracy of the device you use to
make the measurement. Our system of weights and measures, the metric system, was
originally based mainly upon fundamental properties of one of the world's most
abundant substances, water. The system is summarized in Table 2.1. Conversions
within the metric system are quite simple once you have committed to memory the
meaning of the pre-fixes given in Table 2.2. Recently, scientists have started to use a
briefer version of the metric system of units in which the basic units for length, mass,
and time are the meter, the kilogram, and the second. This system of units, known as
the International System of Units, is commonly referred to as the SI system and is
preferred in scientific work. A comparison of some common SI, metric, and English
units is presented in Table 2.3. Conversions within the metric system are quite easy if
you remember the definitions for the prefixes and use dimensional analysis in problem
solving.
Table 2.1 Units of Measurement in the Metric System

Measurement Unit and definition

Gram (g) = weight of 1 cubic centimeter (cm3) of water at 4°C and 760mm
Hg
Mass or weight
Mass = quantity of material
Weight = mass x gravitational force
Length Meter (m) =100 cm =1000 millimeters (mm) =39.37 inch.
Volume Liter (L) =volume of 1 kilogram (kg) of H2O at 4° C
°C, measures heat intensity:
5 9
Temperature °C = (°F-32 ) or°F = ( ×°C) + 32
9 5

1 calorie (cal), amount of heat required to raise 1 g of water 1°C

Heat
1 cal = 4.184 joules (J)
d, usually g/ml, for liquids and g/L for gases:
Density
d = mass/unit volume
Sp gr, dimensionless
Specific gravity
Sp gr = density of a substance/density of a reference substance

The quantities presented in Table 2.1are measured with the aid of various pieces of
apparatus. A brief description of some measuring devices follows.

Table 2.2 The Meaning of prefixes in the metric system

Meaning
Prefix Abbreviation
(power of 10)
Femto 10-15 F
Pico 10-12 p
Nano 10-9 N
Micro 10-6 µ
Milli 10-3 M
Centi 10-2 C
Deci 10-1 D
Kilo 103 K
mega 106
M

Giga 109 G
Table 2.3. Comparison of SI, Metric, and English

Some common
Physical quantity SI unit Conversion factors
Metric units
1 m = 102 cm
Meter (m)
Length Meter (m) 1 m = 39,37 in.
Centimeter (cm)
1 inch. = 2.54 cm
Cubic 1 L = 103 cm3
Liter (L)
volume 1L = 10-3 m3
Meter (m ) 3 Milliliter (mL) *
1L = 1.06 qt
1 kg = 103 g
Gram (g)
Mass Kilogram (Kg) 1 kg = 2.205 lb
Milligram (mg)
1 lb = 453.6 g
Energy Joule (J) Calorie (cal) 1 cal = 4.184 J
0 K =- 273.15 °C
Temperature Kelvin (K) Degree Celsius (°C) 5
°C = (°F -32)
9
* A mL is the same volume as a cubic centimeter: 1 mL = 1 cm3

Laboratory Balances

A laboratory balance is used to obtain the mass of various objects. There are several
different varieties of balances, with various limits on their accuracy. Most modern laboratories
possess single-panbalances. These are the most accurate balances; generally, they are also the
simplestto use and are the most delicate and expensive. The amount of material to be weighed
and the accuracy required determine which balance you should use.

Figure 2.1 Digital electronic balances. The balance gives the mass directly when
an object to be weighed is placed on the pan.
Graduated Cylinders

Graduated cylinders are tall, cylindrical vessels with graduationsscribed along the side of the
cylinder. Since volumes aremeasured in these cylinders by measuring the height of a
column of liquid, it is critical that the cylinder has a uniformdiameter along its entire height.
Obviously, a tall cylinder with asmall diameter will be more accurate than a short one with a
large diameter. A liter (L) is divided into milliliters (mL) suchthat 1 mL = 0.001 L and 1 L =
1000 mL.

Figure 2.2: Graduated cylinder

Thermometers
Thermometers are based upon the principle that liquids expand when heated.Most common
thermometers use mercury as the liquid. These thermometers areconstructed so that a uniform-
diameter capillary tube surmounts a mercury reservoir.To calibrate a thermometer, one defines
two reference points, normally the freezingpoint of water (0°C, 32°F) and the boiling point of
water (100°C, 212°F) at 1 atm ofpressure (1 atm = 760 mm Hg). Once these points are marked
on the capillary, itslength is then sub-divided into uniform divisions called degrees. There are
100°between these two points on the Celsius, (°C, or centigrade) scale and 180° between
those two points on the Fahrenheit (°F) scale.

Pipettes
Pipettes are glass vessels that are constructed and calibrated so as to deliver a precisely
known volume of liquid at a given temperature. The markings on the pipettes illustratedin
Figure 2.3signify that this pipette was calibrated to deliver (TD) 10.00 mL ofliquid at 25°C.
Always use a rubber bulb to fill a pipette. It is important that you be awarethat every measuring
device, regardless of what it may be, has limitations in itsaccuracy. Moreover, to take full
advantage of a given measuring instrument youshould be familiar with or evaluate its accuracy.
Careful examination of thesubdivisions on the device will indicate the maximum accuracy you
can expect of thatparticular tool.

Figure 2.3:A typical volumetric pipette, rubber bulbs, and the pipette filling technique.

In this experiment you will determine the accuracy of your 10-mL pipet. Theapproximate
accuracy of some of the equipment you will use in this course is given inTable 2.4.
Not only should you obtain a measurement to the highest degree of accuracy that the
device or instrument permits, but you should also record the reading or measurement
in a manner that reflects the accuracy of the instrument. For example, a mass obtained
from an analytical balance should be observed and recorded to the nearest 0.01 g. This
is illustrated in Table 2.5
Table 2 .4: Equipment Accuracy
Equipment Accuracy
Analytical balance ±0.0001 g (±0.1 mg)
Top-loading balance ±0.001 g (1 mg)
Graduated cylinder ±0.1 mL
Pipet ±0.02 mL
Buret ±0.02 mL
Thermometer ±0.2°C

Table 2.5 Obtaining Significant Figures

Analytical balance Top loader
85.9 g (incorrect)
85.9 g (incorrect)
85.93 g (incorrect)
85.93 g (incorrect)
85.932 g (incorrect)
85.932 g (correct)
85.9322 g (correct)

Apparatus and Chemicals

BalanceIron wireCopper wire

150-mL beakerAluminum wire

50- or 100-mL graduated cylinderClamp

10-mL pipet Distilled water

25-mL Erlenmeyer flaskRubber bulb

125-mL Erlenmeyer flaskThermometer

Iron ring and ring standBunsen burner and hose

Procedure

A. The Bunsen burner

Melting points of metals

The Bunsen burner is a convenient source of heat inthe laboratory. Although there are several
varieties,their principle of operation is the same and is similarto that of the common gas stove.
The Bunsen burner requires gas and air, which it mixes in variousproportions. The amount of air
and gas mixed in thechamber is varied by use of the collar illustrated inFigure 2.4. The relative
proportions of gas and airdetermine the temperature of the flame.

Figure 2.4 Typical Bunsen burner

Examine your burner and locate the gas and airflowadjustments (valves) (see Figure 2.4).
Determine howeach valve operates before connecting the burner tothe gas outlet. Close both
valves; connect a rubberhose to the gas outlet on the burner and the desk; thenopen the desk
valve about two-thirds of the way.Strike a match or use a gas lighter. Hold the lighted
match to the side and just below the top of the barrelof the burner while gradually opening the
gas valve onthe burner to obtain a flame about 7 or 10 cm high. Gradually open and adjust the
airvalve until you obtain a pale blue flame with an inner cone as shown in Figure 2.4.

Flame temperatures can be observed using the melting points of metals.

Adjust the burner to a non-luminous flame to measure the temperatures in the variousregions of
the flame. Use crucible tongs to hold 2-cm strips of iron wire, copper wire,and aluminum wire in
the various regions of the flame. The melting point of iron is1535 °C, which of copper is 1083
°C and that of aluminum is 660 °C. On the Report sheet, record the estimated temperature of the
flame in the regions designated inFigure 2.5.
 Melting point
Metal
(oC)
Iron (Fe) 1535
Copper (Cu) 1083
Aluminium
660
(Al)

Figure 2.5 Regions of the flame for temperature measurement.

B. The Graduated Cylinder

Examine the 100-mL graduated cylinder and notice that it is scribed in milliliters. Fillthe
cylinder approximately half full with water. Notice that the water meniscus(curved surface of the
water) is concave (see Figure 2.6). When water is the liquid,the lowest point on the curve is
always read as the volume, never the upper level.Avoid errors due to parallax; different and
erroneous readings are obtained if the eyeis not perpendicular to the scale. Read the volume of
water to the nearest 0.1 mL.Record this volume. Measure the maximum amount of water that
your 125-mLErlenmeyer flask will hold. Record this volume.

The meniscus reading here is 50.0 mL.

Figure 2.6:Proper eye position for taking volume readings.

C. Using the balance to calibrate your 10-mL pipet

Weighing an object on a single-pan balance is a simple matter. Directions for operation of single-
pan balance vary with make andmodel. Your laboratory instructor will explain how to use the
balance. Proper care required for the balance is thefollowing:
1. Do not drop an object on the pan.
2. Center the object on the pan.
3. Do not place chemicals directly on the pan; use a beaker, watch glass, weighingbottle, or
weighing paper
4. Do not weigh hot or warm objects; objects must be at room temperature.
5. Return all weights to the zero position after weighing.
6. Clean up any chemical spills in the balance area.
7. Inform your instructor if the balance is not operating correctly; do not attempt to
repair it yourself.

The following method is used to calibrate a pipet or other volumetric glassware. Obtain about 10
mL of distilled water in a 150-mL beaker. Allow the water to sit onthe desk while you weigh and
record the weight of an empty, dry 25-mL Erlenmeyerflask (tare) to the nearest 0.1 mg. Measure
and record the temperature of the water.Using your pipet, pipet exactly 10.00 mL of water into
this flask and weigh the flaskwith the water in it (gross) to the nearest 0.1 mg. Obtain the weight
of the water bysubtraction (gross – tare= net). Using the equation below and the data given
inappendix I, obtain the volume of water delivered and therefore the volume of your
pipet.

mass m
Density voume = v

Normally, density is given in units of grams per milliliter (g/mL) for liquids, grams per cubic
centimeter (g/cm3) for solids, and grams per liter (g/L) for gases. Repeat this procedure in
triplicate-that is, deliver and weigh exactly 10.00 mL of water three times.

EXAMPLE 2.1
Using the procedure given above, a weight of 10.0025 g was obtained as the weight ofthe water
delivered by one 10-mL pipet at 22.0°C. What is the volume delivered bythe pipet?

m
Solution: From the density equation given above, we know that v =
d
For mass we substitute our value of 10.0025 g. For the density, consult the table for density of
water at different temperature, Appendix I.At 22.0°C, the density is 0.997770 g/mL.
The calculation is:

10.0025 g
V= = 10.024910.02mL
0.99770 g /mL

The volume must be rounded off to 10.02, because the pipet's precision can bedetermined only to
within ±0.02 mL.

The precision of a measurement is a statement about the internal agreement among repeated
results; it is a measure of the reproducibility of a given set of results. The arithmetic mean
(average) of the results is usually taken as the "best" value. The simplest measure of precision is
the average deviation from the mean. The average deviation is calculated by first determining the
mean of the measurements, then calculating the deviation of each individual measurement from
the mean and, finally, averaging the deviations (treating each as a positive quantity).

Example 2.2: The following values were obtained for the calibration of a 10-mL pipette: 10.10,
9.98,and 10.00 mL. Calculate the mean value and the average deviation from the mean.

Solution:

10.10+9.98+10.00
Mean = 10.03
3

Deviations from the mean: |value – mean|, |10.10 -10.03| = 0.07

|9.98 - 10.03| = 0.05|10.00 - 10.03| = 0.03

0.07+0.05+ 0.03
Average deviation from the mean = =0.05
3
The reported value is therefore 10.030.05mL.
Experiment 2
Basic laboratory techniques
Name(s)________________________ Laboratory Instructor___________________
Section__________________________ date_________________________________
REPORT SHEET
A. Bunsen Burner
Indicate the approximate temperature of the following regions of the flame
(see Figure 2.5)
a. region : Top of the outer cone__________ °C
b. region : Center of the outer cone __________ °C
c. region : Top of the inner cone __________ °C
d. region : Center of the inner cone __________ °C
B. The graduated cylinder
Volume of water in graduated cylinder ___________________________ mL
Volume of water contained in 125-mL Erlenmeyer flask _____________ mL
C. Using the balance to calibrate your 10-mL pipet

Temperature of water ___________°CDensity of water ___________ g/cm3

Trial 1 trial 2 trial 3

Weight of Erlenmeyer (tare wt) ________ _________ ___________ g
Weight of Erlenmeyer plus
~ 10 mL H20 (gross wt)________ _________ __________ g
Weight of ~ 10 mL of H2O (net wt) ________ _________ __________ g
Volume delivered by 10-mL pipet_________ _________ __________ mL
Show calculations overleaf

Mean volume delivered by 10-mL pipet __________ mL

Show calculations overleaf
Trial 1 trial 2 trial 3
Individual deviations from the mean_________ _________ __________ g
Average deviation from the mean______________ mL
Show calculations overleaf
Volume delivered by your 10-mL pipet ____________ mL ± __________mL
Review Questions

You should be able to answer the following questions before beginning this experiment:
1. What are the basic units of length, mass, volume, and temperature in the SI system?
2. A liquid has a volume of 1.35 liters. What is its volume in mL? in cm3?
3. If an object weighs 1.47 g, what is its weight in mg?
4. Why should you never weigh a hot object?
5. What is precision?
6. Define density? Can it be determined from a single measurement?
7. What is the density of an object with a mass of 9.03 g and a volume of 0.1987mL?
8. Weighing an object three times gave the following results: 10.2 g, 10.1 g, and 10.3 g. find the
mean weight and the average deviation from the mean.
9. Normal body temperature is 98.6°F. What is the corresponding Celsiustemperature?
10. What is the weight in kilograms of 950 mL of a substance that has a density of1.274 g/mL?
11. An object weighs exactly five grams on an analytical balance that has an accuracyof 0.1 mg.
To how many significant figures this weight should be recorded?
12. What is the dominant color of a properly adjusted flame from a Bunsen burner?
13. How many distinct cones does a properly adjusted non-luminous flame have on aBunsen
burner (one, two or three)?
Experiment 3: Mass and Volume Measurements

General Objective: To become familiar with measuring, Reading and recording

measurements correctly (significant digits and unit).
Theory

It depends on careful observation and the use of good laboratory techniques. In this experiment
you will become familiar with some basic operations that will help you throughout the course.
Your success in future experiments will depend upon your mastering these fundamental
operations. Because every measurement made in the laboratory is really an approximation, it is
important that the numbers you record reflect the uncertainty of the device you are using to make
the measurement. The assumption is made in this course that an uncertainty of at least one unit
exists in the last digit.

10.01 mL could actually be 10.00 mL or 10.02 mL

Significant Figures and Metric Conversions

Significant figures are important in describing the accuracy of a measurement. The following
rules paraphrased from your textbook will help you determine the number of significant figures
in a measurement.
1. All nonzero digits are significant. 3.467 cm has 4 sig figs
2. Zeros between nonzero digits are significant. 2.07 mL has 3 sig figs
3. Zeros beyond the decimal point at the end of a number are significant. 6.00 mL has 3 sig
figs
4. Zeros preceding the first nonzero digit in a number are not significant. 0.0341 g has 3 sig
figs
5. The number of sig figs is the number of digits shown when the number is written in scientific
notation.
500 g written expressing 3 sig figs would = 5.00 x 102 g
500 g written expressing 2 sig figs would = 5.0 x 102 g
500 g written expressing 1 sig fig would = 5 x 102 g
In science the metric system is used almost exclusively. The basic unit of length is the meter
(m); of mass, the gram (g); of volume, the liter (l). The meter, the gram, and the liter are related
to larger and smaller units by multiples of 10. Prefixes are used for the unit of measure
expressing these multiples of 10.

Prefix Abbreviation Value x basic unit Some Conversion Factors

Kilo- k 1000 1 km = 1000 m

Deci- d 0.1 1 m = 10 dm& 1 km = 10,000 dm

Centi- c 0.01 1 m = 100 cm & 1 dm = 10 cm

Milli- m 0.001 1 m = 1000 mm & 1 cm = 10 mm

How does 1 kilometer compare to the other units in the metric system?

1 km = 1000 meters = 10,000 dm = 100,000 cm = 1,000,000 mm

Exact Numbers and Conversion Factors

Some numbers by their very nature are exact numbers. When you say you are holding five
beakers in your hand, you mean exactly five beakers, not six or four. Thus, if this figure 5 is
used in a calculation, you may regard it as having as many significant figures as desired:
5.0000… (an unlimited number). Another example of an exact number is a number used torelate
quantities (conversion factors) within the same system of units: 1.0000… m = 100.0000… cm.
These are defined values and possess an unlimited number of significant figures.
Sometimes it is necessary to convert from the British system to the metric system or vice versa.
These relationships between units in two different systems are not exact numbers.
These are the most common conversions utilized by students in this course to convert from the
British system to the metric system or vice versa.
1 pound (lb.) = 454 grams (g) 1 inch (in) = 2.54 centimeters (cm)
1 quart (qt) = 946 milliliters (mL)
Mass
The directions in this experiment are written for use with a digital pan balance. These balances
are very accurate, giving a mass measurement to the thousandth place (0.001 g). This is
considered the accuracy of the balance. Even though this is a digital instrument, the balance is
making an estimate at the thousandths place. All measurements recorded in your data sheet
should reflect this degree of precision. When using the analytical balance please be gentle with
these sensitive instruments and use the following procedures:
1. Before placing your item to be massed on the balance check the display to make sure it is
reading zero. If not press the tare bar once to zero out the balance.
2. Carefully place the item on the pan.
3. Allow sufficient time for the mass to be measured.
4. Record the mass, remove the item.
5. Never place chemicals directly on the balance pan; first place them on a weighing boat or in
a container and then place the boat or container on the balance pan.
6. Clean up any materials you spill on or around the balance.
Never make any adjustments to the balance. If it seems out of order tell to your instructor

Volume

The graduated cylinder is the device you will be using in lab.to measure liquid volumes.
Graduated cylinders are tall, cylindrical vessels with graduations scribed along the side of the
cylinder. Since volumes are measured in these cylinders by measuring the height of liquid, it is
crucial that the cylinder have a uniform diameter along its entire height, which is the case with
the glass cylinders you are using in lab.

Beakers and flasks are marked to indicate only approximate volumes and should not be used to
measure volumes during experiments.When measuring a volume in a graduated cylinder, read
the point on the graduated scale that coincides with the bottom of the curved surface, called the
meniscus, of the liquid. Volumes measured in the graduated cylinder should be estimated and
recorded to the correct number of significant figures.

The volume of a solid object can also be measured using the graduated cylinder by water
displacement. Water displacement is filling a graduated cylinder with enough water tocompletely
cover the solid object, when it is placed into the cylinder. Be sure to place a rubber stopper in
the bottom of the graduated cylinder to prevent the solid object from cracking the bottom of the
cylinder. The difference between the measured volume of water before and after adding the
solid object is the volume of that object.

Length – metric ruler

The standard unit of length is the meter (m), which is 39.37 inches in length. The metric rulers
you will be using in lab are 15.2 cm in length, which is 6 inches. Since you can estimate the
measurement to the hundredths place with these rulers, all measurements recorded in your data
sheet should reflect this degree of accuracy (0.01).

Temperature

Most thermometers are based upon the principle that liquid expands when heated. Our
thermometers use alcohol as the liquid and are constructed so that a uniform-diameter capillary
tube surrounds the alcohol reservoir. The thermometer is calibrated by defining two reference
points: (1) the normal freezing point of pure water (0 oC, 32 oF), and (2) the normal boiling point
of pure water (100 oC, 212 oF). There are 100o between these two points on the Celsius
temperature scale and 180o between these two points on the Fahrenheit scale. 100/180 = 5/9 and
this is how the conversion factors were derived for the temperature conversion formula below.
The simple act of taking temperatures with a thermometer can easily involve errors. When
measuring the temperature of a liquid observe the following procedures:

1. Hold the thermometer away from the walls and bottom of the container.
2. Allow sufficient time for the thermometer to reach thermal equilibrium.
3. Be sure the liquid is adequately mixed.
4. Temperature measurements should be estimated and recorded to the nearest 0.1 0C.
This is the accuracy of the thermometer.
When converting from degrees Fahrenheit to Celsius, make use of the following formula:

(0F – 32oF) x 100oC/180oF = oC

Sample problem: Convert the measured temperature of 70.0o F to degrees Celsius.

(70.0oF – 32.0oF) x 100oC/180oF = 21.1oC 3 sig figs

When converting from Celsius to Fahrenheit use the following formula;

(oC x 1800F/100oC) + 32oF = oF

Note that the final answer is 21.1oC because the initial measured temperature (70.0oF) was to the
tenths place and had only 3 significant figures. The 100 oC, 180oF and 32oC are all exact numbers
and do not determine the significant figures. When using conversion factors the number of
significant figures in the answer always comes from the measured quantity in an experiment or
the given quantity in a problem.

Apparatus and Chemicals

Balance Test tube

150 mL beaker 50 mL graduate cylinder

600 mL beaker Metric ruler

125 mL Erlenmeyer flask 400 mL beaker

Rubber stopper sodium chloride

Metal sample

Procedure

Use the format from page 19 to record all data. The data sheet corresponds to the procedure in
letter and number. You will be graded based on accuracy of the values recorded, accuracy
expressed in the correct number of significant figures in your measurement and neatness in
presentation of the lab report.

Traditionally a pen is used to record data in the laboratory. If you make an error in recording
your data simply draw a single line through your mistake and rewrite it correctly.

A. Mass
1. Describe the precision of the analytical balance.
2. Be sure to zero out the balance and use the same balance throughout your massing. Place a
clean, dry 150 mL beaker on the pan of the balance, read and record the mass of the beaker.
3. Do the same with the 125 mL Erlenmeyer flask.
4. Do the same with the rubber stopper.
5. Go to your instructor’s lab station and get one of the metal samples and do the same.
6. Do the same with a weighing boat.
7. Carefully add approximately 2.5 grams of NaCl to the weighing boat while it is still on the
pan in the balance. Read and record the mass of the weighing boat with the NaCl. Save this
for part B.
8. Mass the second weighing boat.
9. Leave the second weighing boat on the balance and use the tare bar to zero the balance. Now
add approximately 2.5 grams of NaCl to the boat and read and record the mass of only the
NaCl. Save this for Part B.
B. Volume
1. Fill a small test tube to the brim with water. Transfer the water to a graduated cylinder,
measure, and record the volume of water.
2. Fill a large test tube to the brim with water. Transfer the water to a graduated cylinder,
measure and record the volume of water.
3. Fill a 125 mL Erlenmeyer flask to the brim with water, measure and record the volume of
water.
4. Measure 5.0 mL of water and pour into the small test tube. Use the metric ruler to measure
and record the height in centimeters. In the future you will often find it convenient to
estimate this volume simply by observing the height of the liquid in the test tube.
5. Use the rubber stopper you massed in Part A and determine the volume of this solid object as
described in the introductory reading of this lab.
6. Place the rubber stopper in the bottom of the 50 mL graduated cylinder to prevent breakage.
Take the metal sample you massed in Part A and determine the volume of this solid object.
B. Length
Using a metric ruler, make the following measurements in centimeters.
1. Describe the precision of the metric ruler.
2. Measure the external height of a 400 mL beaker.
3. Measure the total length of a small test tube.
C. Temperature
1. Describe the precision of the thermometer.
2. Fill a 600 mL beaker half full of tap water. Place your thermometer in the beaker and give it
a minute to reach thermal equilibrium. Keeping the thermometer in the water and holding
the tip of the thermometer away from the sides of the beaker, read and record the
temperature.
3. Fill a 250 mL beaker half-full and place on a hot plate. Heat the water to boiling. Read and
record the temperature of the boiling water, being sure to hold the thermometer away from
the bottom of the beaker.
4. Fill a 400 mL beaker one-fourth full of tap water and add a 150 mL beaker full of crushed
ice. Leave this set up for five minutes. Without stirring, place the thermometer in the
beaker, resting on the bottom. Wait at least one minute and then read the temperature.
5. Take the two weighing boats from Part A and add the NaCl from each of them to the ice-
water mixture in step #4 above. Stir the mixture for 1 minute and add more ice if needed.
Read and record the temperature.
Experiment #3
Mass, volume, length and temperature measurements.
Name(s)________________________ Laboratory Instructor___________________

Section__________________________date_____________________________

Report sheet

Read the appropriate section of the lab introduction or procedure before starting each section.

A. Mass

1. Describe the precision of the analytical balance ___________________ g

2. Mass of a clean, dry 150 mL beaker ___________________ g

3. Mass of a 125 mL Erlenmeyer flask___________________ g

4. Mass of the rubber stopper___________________ g

5. Mass of one of the metal sample___________________ g

6. Mass of a weighing boat___________________ g

7. Mass of the weighing boat with the first sample of NaCl___________________ g

8. Mass of the NaCl ___________________ g

9. Mass of only the second sample of NaCl placed in the tared weighing boat
______________ g

B. Volume

1. Volume of a small test tube___________ mL

2. Volume of a large test tube___________ mL

3. Volume of a 125 mL Erlenmeyer flask___________ mL

4. Height in centimeters of 5.0 mL of water in a small test tube ___________ cm

5. Volume of the rubber stopper you massed in part A___________ mL

6. Volume of the metal sample used in part A___________ mL

C. Length

1. Describe the precision of the metric ruler___________ cm

2. Measure the external height of a 400 mL beaker ___________ cm

D. Temperature

1. Describe the precision of the thermometer___________ oC

2. Temperature of the tap water___________ oC

3. Temperature of the boiling water___________ oC

4. Temperature of water with crushed ice___________ oC

5. Temperature of water with approximately 5 grams of NaCl___________ oC

3. Measure thetotal length of a test tube___________ cm

Questions: Show calculation steps and answers for the following problems

1. Convert 23.5 oC to Fahrenheit and Kelvin ___________ oF

___________ K

2. Convert 65.8 oFto Celsius and Kelvin ___________ oC

___________ K

Use dimensional analysis for solving problems 3-5.

3. Convert the mass of the 125 mL flask from grams to kilograms ___________ kg

4. Convert the mass of the weighing boat from grams to centigrams___________ cg

5. Convert the volume of the small test tube from mL to liters.___________ L

How many significant figures are in each of the following?

6. 1.234 cm _____ sf

7. 0.016 g _____ sf

8. 104 L _____ sf

9. 0.05600 ______ sf

Write the following numbers in scientific notation:

10. 1234 m = ________________________ m

11. 0.01234 m = _________________________ m

The definition of density is the mass of an object divided by the volume of the object.
Density = mass / volume
11. Use your data in this experiment to determine the density of the rubber stopper. Check the
number of significant figures in each measurement and follow the rules of calculating with
significant figures given in lecture. _______________ g / mL

Use your data in this experiment to determine the density of the metal sample. Check the
number of significant figures in each measurement and follow the rules of calculating with
significant figures given in lecture. _______________ g / mL
Experiment 4: Identification of Substances by Physical Properties

General Objective: To become acquainted with procedures used in evaluating physical

properties and the use of these properties in identifying substances

Theory:

Propertiesare those characteristics of a substance that enable us to identify it and

to distinguish it from other substances. Direct identification of some substances can
readily be made by simply examining them. For example, we see color, size, shape,
and texture, and we can smell odors and discern a variety of tastes. Thus, copper can
be distinguished from other metals on the basis of its color.

A physicalproperty is a characteristic of matter that is not associated with a change in its

chemicalcomposition. Familiar examples of physical properties include density, color, hardness,
meltingand boiling points, and electrical conductivity. Some physical properties, such as density
and color, may be observed without changing the physical state of the matter. Other physical
properties, such as the melting temperature of iron or the freezing temperature of water, can only
be observed as matter undergoes a physical change. A physical change is a change in the state
orproperties of matter without any accompanying change in the chemical identities of the
substances contained in the matter. Physical changes are observed when wax melts, when sugar
dissolves in coffee, and when steam condenses into liquid water. Other examples of
physical changes include magnetizing and demagnetizing metals (as is done with common
antitheft security tags) and grinding solids into powders (which can sometimes yield noticeable
changes in color). In each of these examples, there is a change in the physical state, form, or
properties of the substance, but no change in its chemical composition.

Figure 4.1: (a) Wax undergoes a physical change when solid wax is heated and forms liquid
wax.
(b) Steam condensing inside a cooking pot is a physical change, as water vapor is changed into
liquid water.
Figure a, is a photograph of butter melting in a pot on a stove. Figure b is a photograph of
something being heated on a stove in a pot. Water droplets are forming on the underside of a
glass cover that has been placed over the pot.
As you probably realize, a specific combination of properties isunique to a given substance, thus
making it possible to identify most substances justby careful determination of several properties.
This is so important that large bookshave been compiled listing characteristic properties of many
known substances.

In this experiment you will use the following properties to identify a substance whose identity is
unknown to you: solubility, density, and boiling point.The solubility of a substance in a solvent
at a specified temperature is the maximumweight of that substance that dissolves in a given
volume (usually 100 or 1000 mL) ofa solvent. It is tabulated in hand-books in terms of grams per
100 mL of solvent; thesolvent is usually water.

A liquid is said to boil when bubbles of vapor from within it, rise rapidly to thesurface, and burst.
Any liquid in contact with the atmosphere will boil when its vaporpressure is equal to
atmospheric pressure-that is, the liquid and gaseous states of asubstance are in equilibrium.
Boiling points of liquids depend upon atmosphericpressure. A liquid will boil at a higher
temperature at a higher pressure or at lowertemperature at a lower pressure. The temperature at
which a liquid boils at 760 mmHgis called the normal boiling point.

Apparatus and Chemicals

BalanceCapillary tubes (5)250 mL beakerSpatula
25 mL Erlenmeyer flaskRing stand and ring
10 mL graduated cylinderUtility clamp
10 mL pipette Thermometer clamp
5 mL pipette Thermometer
50 mL beakers (2)Stirring rod
Burner and hoseApparatus for boiling point determination
Small rubber bandsNaphthalene (1 g)
Boiling chipsEthyl alcohol (15 mL)
Large test tubes (2)Cyclohexane (20 mL)
Small test tubes (6)2 unknowns (liquid and solid)
Test-tube rackSoap solution
Wire gauze
Procedure

A. Solubility

Caution: cyclohexane is highly flammable and must be kept away from open flames.

Qualitatively determine the relative solubility of three solutes: water, cyclohexane, and
ethyl alcohol. Determine the solubility by adding 5 drops of solute to 2 mL of each of
the three solvents in separate, clean, dry test tubes (it is not necessary to measure these
volumes accurately). Place some paraffin in each test tube and shake briefly. Record
your conclusions on the report sheet using the abbreviations s (soluble), sp(sparingly
soluble), and i (insoluble).

The formation of two layers indicates immiscibility (lack of solubility) -i.

Cloudiness indicates partial solubility - sp.

Now repeat these experiments using your liquid unknown as a solute and record your
observations.
B. The density of a liquid

Weigh a clean, dry 25-mL Erlenmeyer flask to the nearest 0.01g. Obtain at least 15 mL of the
unknown liquid in a clean and dry test tube. Using a 10-mL pipet, pipet exactly 10.0 mL of the
unknown liquid into the 25-mL Erlenmeyer flask and quickly weigh the flask containing the 10.0
mL of the unknown to the nearest 0.01 g. Using the weight of this volume of unknown, calculate
its density. Record your results and show how (with units) you performed your calculations.

Save the Liquid for Your Boiling Point Determination

C. Boiling Point of Liquid Unknown

Obtain a 260 °C thermometer. Assemble the boiling point apparatus in Figure 2.3.Complete two
measurements for the boiling point of your unknown.

i. Assemble the Boiling Point Apparatus.Place enough of the liquid unknown (use some of the
samematerial you used to determine the density) into a 75-mm test tube, so that the thermometer
bulb gets completely immersed

Caution: The liquid may be flammable - keep it away from an open Bunsen flame.

Position it beside the thermometer bulb using a rubber band. Invert (open end down) a
10-cm capillary tube in the liquid. Place the apparatus into the water bath.
ii. Measure the Boiling Point.

Place 2-3 boiling chips in the water bath. Slowly heat the water while stirring with the
stirring rod. When a rapid and continuous stream of bubbles escapes the capillary tube,
discontinue heating the water bath, and gently take the test tube out of the bath. The
stream of bubbles slows as the tube cools. When the bubbles cease to escape and
before the liquid re-enters the capillary tube, record the observed boiling point (the
temperature will become constant at the boiling point of the liquid). Estimate the true
(normal b.p. at 1 atm = 760 mmHg) using the pressure correction.

iii. Repeat the Measurement.

Add some cold water to the bath and determine the boiling point a second time. The
same liquid may be used; however, the capillary tube must be removed, emptied, and
inserted before heating resumes.
Figure 4.2:Apparatus for determining the boiling point of a liquid.

D. Unknown Identification
Your unknown is one of the substances contained in the table of physical properties
enclosed. Compare the properties that you have determined for your unknown with
those in the Appendix II. Identify your unknown and record your results.
Experiment 3
Identification of Substances:
Physical Properties
Name(s)________________________ Laboratory Instructor___________________
Section__________________________ date_________________________________
Unknown n°_______________
REPORT SHEET
A. Solubility s = solublesp= sparingly solublei = insoluble
Solvent (~2mL)
Water Ethanol Cyclohexane

Water
Solute (~5
drops) Ethanol
Cyclohexane
Liquid unknown

B. Density of Liquid Unknown

Volume of liquid 10mL
Weight of 25-mL Erlenmeyer ________g
Weight of 25-mL Erlenmeyer
plus 10.0 mL of unknown _________g
Weight of liquid _________mL
Density __________ g/mL
show calculations overleaf

C. Boiling point of liquid unknown

Observed b.p. 1: ______ °C Observed b.p. 2: _____ °C Average b.p. : ________ °C
D. Unknown Identification
Liquid unknown ___________________

Review Questions

1. List five physical properties?

2. 8.692 mL sample of an unknown weighed 10.02 g. What is the density of the unknown?
3. Could you determine the density of cadmium nitrate using water? Why or why not?
4. Why do we calibrate thermometers and pipets?
5. Is bromoform miscible with water? With cyclohexane?
6. When water and toluene are mixed, two layers form. Is the bottom layer water or toluene? (see
table enclosed)
7. What solvent would you use to determine the density of cadmium nitrate?
8. The density of a solid with melting point of 52 to 54°C was determined to be 1.45 ± 0.02 g/ml.
What is the solid?

Experiment 5: Separation of the Components of a Mixture

Objective:To become familiar with the methods of separating substances from one another
usingdecantation, extraction,and distillationtechniques.

Theory

Materials that are not uniform in composition are said to be impure or heterogeneousand are
called mixtures. Most of the materials we encounter in everyday life, such ascement, wood, and
soil, are mixtures.When two or more substances that do not react chemically are combined a
mixture results. Mixtures are characterized by twofundamental properties: First, each of the
substances in the mixture retains itschemical integrity; second, mixtures are separable into these
components by physicalmeans. If one of the substances in a mixture is preponderant-that is, if its
amount farexceeds the amounts of the other substances in the mixture-then we usually call this
mixture an impure substance and speak of the other substances in the mixture asimpurities.
The preparation of compounds usually involves their separation or isolation fromreactants or
other impurities. Thus the separation of mixtures into their componentsand the purification of
impure substances are frequently encountered problems. Youare probably aware of everyday
problems of this sort. For example, our drinking waterusually begins as a mixture of silt, sand,
dissolved salts, and water. Since water is byfar the largest component in this mixture, we usually
call this impure water. How dowe purify it? The separation of the components of mixtures is
based upon the fact thateach component has different physical properties.

The components of mixtures arealways pure substances, either compounds or elements and each
pure substancepossess a unique set of properties. The properties of every sample of a
puresubstance are identical under the same conditions of temperature and pressure. Thismeans
that once we have determined that a sample of sodium chloride, NaCl, is water soluble and a
sample of silicon dioxide (sand), SiO2, is not, we realize that all samplesof sodium chloride are
water-soluble and all samples of silicon dioxide are not.Likewise, every crystal of a pure
substance melts at a specific temperature, and at agiven pressure, every pure substance boils at a
specific temperature.

Although there are numerous physical properties that can be used to identify aparticular
substance, we will be concernedin this experiment merely with the separation of the components
and not with theiridentification.The methods we will use for the separation depend upon
differences in physical properties, and they include the following:
Decantation: This is the process of separation of a liquid from a solid (sediment) by gently
pouring the liquid from the solid so as not to disturb the solid (see Figure 5.1).

Filtration:This is the process of separating a solid from a liquid by means of a porous substance,
a filter, which allows the liquid to pass through but not the solid (see Figure 5.1). Common filter
materials are papers, layers of charcoal, and sand. Silt and sand can be removed from our
drinking water by this process.

Extraction: This is the separation of a substance from a mixture by preferentially

dissolving that substance in a suitable solvent. This process is used to separate a soluble
compound from an insoluble compound.

Sublimation: This is the process in which a solid passes directly to the gaseous
state without the appearance of the liquid state. Not all substancespossess the ability to be
sublimed. Iodine, naphthalene, andammonium chloride (NH4C1) are common substances that
easilysublime.

Figure 5.1 Description of the processes of decantation and filtration.

The mixture that you will separate contains three components: NaCl, NH 4C1, and
SiO2. Their separation will be accomplished by heating the mixture to sublime the
NH4C1, extracting the NaCl with water, and finally drying the remaining SiO 2, as
illustrated in the scheme shown in Figure 5.2.
 Figure 5.2 Flow diagrams for the separation of the components of the mixture

Apparatus and Chemicals

BalanceUnknown mixture of sodium Chloride

Ring stands (2)ammonium chlorideTongsSilicon dioxide (2-3g)

Watch glassEvaporating dishes (2)50- or 100-mL graduated cylinder
Glass stirring rod

I. Sublimation, decantation, and extraction

Procedure
carefully weighs a clean, dry evaporating dish to the nearest 0.01 g. Then obtain from your
instructor a 2- to 3-g sample of the unknown mixture in the evaporating dish.Weigh the
evaporating dish containing the sample and calculate the sample weight . Place the evaporating dish
containing the mixture on a hot plate under thefumehood. Heat the evaporating dish until white
fumes are no longer formed (a total of about 15 min). Heat carefully to avoid spattering,
especially when liquid is present. After the first 10 min gently stir the mixture with your glass
stirring rod; then apply the heat again. Allow the evaporating dish to cool until it reaches room
temperature and then weigh the evaporating dish with the contained solid.

Never Weigh Hot or Warm Objects!

The loss in weight represents the amount of NH 4Clin your mixture. Calculate this weight.
Add 25 mL of water to the solid in this evaporating dish and stir gently for 5 min. Next, weigh
another clean, dry evaporating dish and watch glass. Decant the liquid carefully into the second
evaporating dish, which you have weighed, being careful not to transfer any of the solids into the
second evaporating dish. Add 10 mL more of water to the solid in the first evaporating dish, stir,
and decant this liquid into the second evaporating dish as before. Repeat with still another 10 mL
of water. This process extracts the soluble NaCl from the sand. You now have two evaporating
dishes; one containing wet sands and the second, a solution of sodium chloride. Place the
evaporating dish containing the sodium chloride solution carefully on the hotplate. Begin gently
heating the solution to evaporate the water. Take care to avoid boiling or spattering, especially
when liquid is present. Near the end, cover the evaporating dish with the watch glass that was
weighed with this evaporating dish, and reduce the heat to prevent spattering. While the water is
evaporating you may proceed to dry the SiO2 in the other evaporating dish as explained in the
next paragraph, if you have another hotplate available. When you have dried the sodium chloride
completely, no more water will condense on the watch glass, and it, too, will be dry. Let the
evaporating dish and watch glass cool to room temperature and weigh them.

The difference between this weight and the weight of the empty evaporating dish and watch
glass is the weight of the NaCl. Calculate this weight.

Place the evaporating dish containing the wet sand on the hotplate and cover the evaporating dish
with a clean, dry watch glass. Heat slowly at first until the lumps break up and the sand appears
dry. Then heat the evaporating dish to dull redness andmaintain this heat for 10 min. Take care
not to overheat, or the evaporating dish will crack. When the sand is dry, remove the heat and let
the dish cool to roomtemperature. Weigh the dish after it has cooled to room temperature. The
difference between this weight and the weight of the empty dish is the weight of the sand.
Calculate this weight.
Calculate the percentage of each substance in the mixture using an approach similar to that
shown in Example 5.1. The accuracy of this experiment is such that thecombined total of your
three components should be in the neighborhood of 99%. If it is less than this, you have been
careless. If it is more than 100%, you have not sufficiently dried the sand and salt.

EXAMPLE 5.1
what is the percentage of SiO2 in a 7.69 g sample mixture if 3.76 g of SiO2 has been
recovered?

wt of compenent ∈grams ×100

% Component =
wt sample ∈grams

Therefore, the percentage of SiO2 in this particular sample mixture is

3.76× 100
% SiO2 = = 48.9%
7.69

II. Simple distillation

Set the simple distillation apparatus by looking at the set up prepared for demonstration (figure
5.3). The distillation is performed not by directly heating the flask but by placing it on the
waterbath. Pour 40 ml of the provided impure (contaminated) ethyl alcohol into the dry distilling
flask by means of funnel. Add 2 or 3 pieces of boiling chips (to avoid several bumping). Place
the thermometer so that its bulb is ca. 0.5 cm below the junction of the side arm of the distilling
flask. Get your set up checked by the instructor before starting the distillation. Collect the
distillate in a measuring cylinder and record the boiling point after every 4 ml .conduct the
distillation slowly but steadily so that the thermometer bulb at all times bears a drop of
condensate and so that 1 or 2 drops of distillate come out of the condenser per second .Turn off
your gas or hotplate and stop the distillation when the volume of the residue is 5-10 ml. Record
the data in your note book by making a table indicating volume collected and temperature. Hand
over the product to your instructor. Plot the results using a graph paper volume (x-axis) vs
temperature (y-axis) and discuss the results in your note book.
Figure 5.3 simple distillation set up.

REPORT SHEET
Separation of the Components of a Mixture
Name(s)________________________ Laboratory Instructor___________________

Section__________________________date_______________________________
Unknown°_____________
A. Weight of evaporating dish ____________ g
Weight of evaporating dish and original sample ______ ______ g
Weight of original sample ______ ______ g
Weight of evaporating dish after subliming NH 4Cl ______ ______ g
Weight of NH4Cl ______ ______ g
Percent of NH4C1 (show calculations) ______ _____ %
B. Weight of evaporating dish and watch glass ____________ g
Weight of evaporating dish, watch glass, and NaCl ____________ g
Weight NaCl ______ ______g
Percent of NaCl (show calculations) _____ ______ %
C. Weight of evaporating dish and SiO2____________ g
Weight of evaporating dish____________g
WeightofSiO2___________g
Percent of SiO2 (show calculations) ___________ %
D .Weight of original samplemass sample= ___________g
Weight of determined [NH4Cl + NaCl + SiO2] total mass= ___________g

Differences in these weights |mass of sample–total mass| ____________g

Percent recovery of matter

Percent recovery of matter

g ma tter recovered mass total

= ×100 = × 100= _________%
g original sample mass sample

If the percent recovery of matter is not exactly 100%, account for your errors below:

Review Questions
1. What distinguishes a mixture from an impure substance?
2. Define the process of sublimation.
3. How do decantation and filtration differ? Which should be faster?
4. Why does one never weigh a hot object?
5. How does this experiment illustrate the principle of conservation of matter?
6. A mixture was found to contain 3.10 g of SiO2, 0.38 g of cellulose, and 6.72 g of calcium
carbonate. What is the percentage of CaCO3 in this mixture?
7. How could you separate a mixture of zinc chloride and cyclohexane? Consult the table for
physical properties, Appendix II.
8. How could you separate zinc chloride from SiO2?
9. Why is SiO2 washed with water three times as opposed to only once?
10 A student found that her mixture was 15 percent NH 4C1, 20 percent NaCl, and 75percent
SiO2. Assuming her calculations are correct, what did she most likely do incorrectly in her
experiment?
Experiment 6: Solution Preparation

General Objective: To practice the preparation of solutions of known concentration from

a solid and by dilution from a stock solution

Theory

Preparation of a solution is an essential skill in the study of chemistry. The solutions which are
prepared are often used in determining quantitative relationships in chemical reactions. Many of
the reactions of qualitative and quantitative chemical analyses take place in solutions. Analytical
chemistry deals with solution measurements and concentrations, from which we calculate mass
and vice- versa. Thus, we prepare solutions of known concentration for calibration of
instruments response or to titrate sample solutions. Laboratory experiments and different types of
research often require preparation of chemical solutions in their procedure.

Solution isa uniform homogeneous mixture of two or more substances. The individual
substancesmay be present in varying amounts.The relative amount of a given solution
component is known as its concentration. Often, thoughnot always, a solution contains one
component with a concentration that is significantly greaterthan that of all other components.
This component is called the solvent and may be viewed as themedium in which the other
components are dispersed, or dissolved. It is a substance which does the dissolving (typically a
liquid, such as water or alcohol). Solutions in which water isthe solvent are, of course, very
common on our planet. A solution in which water is the solvent iscalled an aqueous solution.

A solute is other component of a solution that is typically present at a much lower concentration
thanthe solvent.Solute is a substance which is dissolved, or has gone into solution (typically a
solid).Its concentrations are often described with qualitative terms such as dilute (ofrelatively
low concentration) and concentrated (of relatively high concentration).Concentrations may be
quantitatively assessed using a wide variety of measurement units, eachconvenient for particular
applications.

Preparing a solution of known concentration is perhaps the most common activityin any
analytical lab. The method for measuring out the solute and solvent dependon the desired
concentration units, and how exact the solution’s concentrationneeds to be known. Pipets and
volumetric flasks are used when a solution’s concentration must be exact; graduated cylinders,
beakers, and reagent bottles suffice whenconcentrations need only be approximate. Two methods
for preparing solutions aredescribed in this section.

a. Preparing stock solutions

Stock solution isa solution of known concentration from which other solutions are prepared. Itis
prepared by weighing out an appropriate portion of a pure solid or by measuring out an
appropriate volume of a pure liquid and diluting to a known volume. Exactly how this is done
depends on the required concentration units. For example, to prepare a solution with a
desiredmolarity you would weigh out an appropriate mass of the reagent, dissolve it in a portion
of solvent, and bring to the desired volume. To prepare a solution where the solute’s
concentration is given as a volume percent, you would measure out an appropriate volume of
solute and add sufficient solvent to obtain the desired total volume.

b.Preparing solutions by dilution

Dilution is the process whereby the concentration of a solution is lessened by the addition of
solvent. A known volume of the stock solution is transferred to a newcontainer and brought to
anew volume.Solutions with small concentrations are often prepared by diluting a more
concentrated stock solution. Since the total amount of solute is thesame before and
afterdilution,C1× V1 = C2 × V2

WhereC1 is the concentration of the stock solution, V1is the volume of the stocksolution being
diluted, C2 is the concentration of the dilute solution, and V2 is thevolume of the dilute solution.
Again, the type of glassware used to measure V1 andV2 depends on how exact the solution’s
concentration must be known.
Apparatus and Chemicals
Volumetric flask sodium chloride (NaCl)
Stirrer glacial acetic acid (CH3COOH)
Beaker sulphuric acid (H2SO4)
Measuring cylinder Distilled WaterAnalytical balance
Procedure
I. If starting with a solid,
Use the following procedure:
 Determine the mass in grams of one mole of solute, the molar mass, MMs.
  Decide volume of solution required, in liters, V.
 Decide molarities of solution required, M.
 Calculate grams of solute (gs) required using equation 1eq. 1gs = MMs x M x V
Sample calculation

Example 6.1
Prepare 250 mL of 0.1 M sodium hydroxide.
(MMNaOH= 40 g/mol) gNaOH= 40 g/molx 0.1mol/L x 0.25 L= 1 g NaCl
Dissolve 1g of NaCl in about 100 mL of distilled water,and then add more water until final
volume is 250 ml.
1) Preparation of 0.5M of NaCl from solid NaCl
i) Weigh 7.3 g of NaCl and add to the beaker.
ii) Add 50 mL of water to the beaker containing NaCl and dissolve it by shaking.
iii) Using a funnel transfer the solution to 250 mL volumetric flask.
iv) Slowly add the more water to the volumetric flask up to the mark.

II.If starting with a solution or liquid reagent

Use the following procedure:
 When diluting more concentrated solutions, decide what volume (V 2) and molarity (M2)
the final solution should be.Volume can be expressed in liters or milliliters
 Determine molarity (M1) of starting, more concentrated solution.
 Calculate volume of starting solution (V1) required using equation
Note: V1must be in the same units as V2. Using dilution lawM1V1= M2V2
Example 6.2
Prepare 100 mL of 1.0 M hydrochloric acid from Concentrated (12.1 M) hydrochloric acid.
M1V1= M2V2
(12.1 M)(V1) = (1.0 M)(100 mL)
V1= 8.26 mL conc. HCl
Add 8.26 mL of concentrated HCl to about 50 mL of distilled water, stir, and then add water up
to 100ml
2) Preparation of 1L of 2% (v/v) acetic acid using concentrated glacial acetic acid
i) Transfer 20 mL of glacial acetic acid to 1 L volumetric flask.
ii) Shake it very well to get homogeneous solution; turn it upside down three or more times.
iii) Add sufficient water to bring the solute to the desired volume (1 L).
Questions
1) Describe how you would prepare the following three solutions:
(a) 500 mL ofapproximately 0.20 M NaOH using solid NaOH
(b) 1 L of 150.0 ppm Cu2+using Cu metal
(c) 2 L of 4% v/v acetic acid using concentrated glacial acetic acid
2) A laboratory procedure calls for 250 mL of an approximately 0.10 M solution of NH 3.
Describe how to prepare this solution using a stock solution of concentrated NH3(14.8 M).
3) A sample of an ore was analyzed for Cu 2+ as follows. A 1.25-g sample of the ore was
dissolved in acid and diluted to volume in a 250 mL volumetric flask. A 20 mL portion of the
resulting solution was transferred by pipet to a 50 mL volumetric flask and diluted to volume. An
analysis showed that the concentration of Cu2+ in the final solution was 4.62 ppm. What is the
weight percent of Cu in the original ore?
Experiment 7: Chemical Reaction

General Objective: To observe some typical chemical reactions, identify some of the
products, and summarize the chemical changes in terms of balanced chemical equations.

Theory
Chemical equations represent what transpires in a chemical reaction. For example, the equation
below means that potassium chlorate, KClO3, decomposes on heating (is the symbol used for
heat) to yield potassium chloride, KCl, and oxygen, O2.

2KClO3 (s) + heat→2 KCl (s) + 3O2 (g)

Before an equation can be written for a reaction, someone must establish what the products are.
How does one decide what these products are? Products are identified by their chemical and
physical properties as well as by analyses. That oxygen and not chlorine gas is produced in the
above reaction can be established by the fact that oxygen is a colorless, odorless gas. Chlorine,
on the other hand, is a pale, yellow-green gas with an irritating odor.

In this experiment you will observe that in some cases gases are produced, precipitates are
formed, or color changes occur during the reactions. These are all indications that a chemical
reaction has occurred.
Table 7.1 Properties of reaction products
Water soluble solids Manganese oxyanions

white (colorless
KCl MnO4- Purple
solution)
white(colorless
NH4Cl MnO42- dark green
solution)
KMnO4 purple MnO43- dark blue
MnCl2 pink, (very pale) Gases
Cu(NO3)2 blue H2 colorless, odorless
brown, pungent odor
Water-insoluble solids NO2
(TOXIC)
very dark blue or colorless, slight pleasant
CuS NO
black odor
Cu2S black CO2 colorless, odorless
BaCrO4 yellow Cl2 pale yellow-green
BaCO3 white SO2 colorless, choking
colorless, rotten- egg odor
PbCl2 white H2S
(TOXIC)
MnO2 black or brown
APPARATUS AND CHEMICALS
Crucible and cover6M NH3Mossy zinc0.01 M CuSO4
Copper wire (2-in. length) 6M H2SO4Copper sulfideConc. HNO3
0.1 M sodium oxalate 3M (NH4)2CO3Na2C2O4KMnO4 (solid)0.1 M
KMnO4Na2CO3 (solid)10 M NaOHNa2SO3 (solid)0.1 M Pb(NO3)26-in. test tube
0.1 M BaCl26 M HCl1 M K2CrO40.1 M NaHSO3 (freshly prepared)
Procedure
A. Reaction between the elements Copper and Sulfur

Samples of copper (I) sulfide and copper (II) sulfide will be provided to you.Copper (II) sulfide,
CuS, is insoluble in aqueous ammonia, NH3 (that is, it does not react withNH3), while copper (I)
sulfide, Cu2S, dissolves (that is, reacts) to give a blue solution withNH3.
Place a small portion of your sample in a test tube and add2 mL of 6 M NH3in the hood. Heat
gently with a hot plate
1. Does your product react with NH3?
2. Suggest a possible formula for the product.
3.Write a reaction showing the formation of your proposed product:
Cu (s) + S8 (s)→?
B. Oxidation-Reduction Reactions

Many metals react with acids to liberate hydrogen and form the metal salt of the acid. The
noble metals do not react with acids to produce hydrogen. Some of the “unreactive” metals
doreact though with nitric acid, HNO3 (see Table 7.2); however, in these cases gases that
areoxides of nitrogen are formed rather than hydrogen.

Add a small piece of zinc to a test tube containing 2 mL of 6M HCl and note what happens.
4. Record your observations.
5. Suggest possible products for the observed reaction: Zn (s) + HCl (aq)→ ?
Place a 1-in. piece of copper wire in a clean test tube; add 2 mL of 6M HCl and note if
areaction occurs.
6. Record your observations.
7. Is Cu an active or an inactive metal?
While Holding a Clean Test Tube in the Hood, place a 1-in. piece of copperwire in it and add
1 mL of concentrated nitric acid, HNO3.
8. Record your observations.
9. Is the gas colored?
10. Suggest a formula for the gas.
11. After the reaction has proceeded for 5 min, carefully add 5 mL of water. Based upon thecolor
of the solution what substance is present in solution?
Potassium permanganate, KMnO4, is an excellent oxidizing agent in acidic media. The
permanganate ion is purple and is reduced to the manganous ion, Mn , which has a very
2+

faint,pink color.
While Holding a Test Tube in the Fume Hood, add one or two drops of
potassium permanganate, KMnO4, solution to 1 mL of 6 M HCl.
12. Record your observations.
13. Note the color of the gas evolved.
14. Based on the color and familiar odor of the gas, what is the gas?
C. Metathesis Reactions
Additional observations are needed before equations can be written for the reaction above, but
we see that we can identify some of the products. The remaining reactions are simple, and
youwill be able, from available information, not only to identify products but also to write
equations. A number of reactions may be represented by equations of the following type:
AB + CD→AD + CB
These are called double-decomposition, or metathesis, reactions. This type of reaction involves
the exchange of atoms or groups of atoms between interacting substances. The following is a
specific example:
NaCl (aq) + AgNO3 (aq)→ AgCl (s) + NaNO3 (aq)
Place a small sample of sodium carbonate, Na2CO3, in a test tube and add several drops of 6 M
HCl.
15. Record your observations.
16. Note the odor and color of the gas that forms.
17. What is the evolved gas?
18. Write an equation for the observed reaction: HCl (aq) + Na2CO3 (aq)→
(NOTE: In this reaction the products must have H, Cl, Na, and O atoms in some
newcombinations, but no other elements can be present)
Note that H2CO3 (carbonic acid) and H2SO3 (sulfurous acid) readily decompose as follows:
H2CO3 (aq)→ H2O (l) + CO2 (g)
H2SO3 (aq)→ H2O (l) + SO2 (g)
To 1 mL of 0.1 M lead nitrate, Pb(NO3)2, solution in a clean test tube, add a few drops of 6
MHCl.
19. Record your observations.
20. What is the precipitate?
21. Write an equation for the reaction HCl (aq) + Pb(NO3)2 (aq)→ ?
To 1 mL of 0.1 M barium chloride (BaCl2) solution, add 2 drops of 1 M potassium chromate
(K2CrO4) solution.
22. Record your observations.
23. What is the precipitate?
24.Write an equation for the reaction BaCl2 (aq) + K2CrO4 (aq)→ ?
To 1 mL of 0.1 M barium chloride, BaCl2, solution add several drops of 3 M ammonium
carbonate, (NH4)2CO3, solution in a test tube.
25. What is the precipitate?
26. Write an equation for the reaction (NH4)2CO3 (aq) + BaCl2 (aq)→ ?
Use a centrifuge to separate quickly the precipitate from the liquid phase and decant (that is,pour
off) the excess liquid. Add 1 mL of water to the test tube, shake it, and isolate the solidagain by
using the centrifuge. Pour off the excess liquid. Finally, to the remaining solid, addseveral drops
of 6 M HCl.
27. Record your observations.
28. Note the odor.
29. What is the evolved gas? (Recall the reaction in step 26 of this experiment)
30. Write the equation of this reaction.

Experiment 7
Chemical Reactions
Name(s)________________________ Laboratory Instructor___________________
Section__________________________ date_________________________________
REPORT SHEET
A. Reaction between the elements Copper and Sulfur
1.______________________________________________
2.______________________________________________
3.Cu (s) + S8 (s)→
B. Oxidation-Reduction Reactions
4. _________________________________________
5. Zn (s) + HCl (aq)→
6._____________________________________________
7._____________________________________________
8._____________________________________________
9._____________________________________________
10._____________________________________________
11._____________________________________________
12._____________________________________________
13._____________________________________________
14._____________________________________________
C. Metathesis Reactions
15______________________________________________
16._____________________________________________
17._____________________________________________
18.HCl (aq) + Na2CO3 (aq)→
19._____________________________________________
20._____________________________________________
21.HCl (aq) + Pb(NO3)2 (aq)→
22._____________________________________________
23._____________________________________________
24.BaCl2 (aq) + K2CrO4 (aq)→
25._____________________________________________
26.(NH4)2CO3 (aq) + BaCl2 (aq)→
27._____________________________________________
28._____________________________________________
29._____________________________________________
30. _____________________________________________
Review Questions
1. Before a chemical equation can be written, what must you know?
2. What observations might you make that suggest a chemical reaction has occurred?
3. How could you distinguish between NO2and NO? (Hint: use appendix III)
4. Define metathesis reactions. Give an example.
5. What is a precipitate?
6. Balance these equations:
KBrO3 (s)→ KBr (s) + O2 (g)
MnBr2 (aq) + AgNO3 (aq)→Mn(NO3)2 (aq) + AgBr (s)
7. How could you distinguish between the gases H2and H2S?
8. Using water, how could you distinguish between the white solids KCl and PbCl2?
9. Write equations for the decomposition of H2CO3(aq) and H2SO3(aq).

Experiment 8: Solubility of Salts in Water

General Objectives: To predict the solubility of common inorganic compounds by using

solubility rules.
Theory

The solubility of a solute is the amount of solute dissolved in a given amount of a solvent at
equilibrium at specified conditions. The usual units used to express solubility are gram of solute
per 100 grams of solvent at a specified temperature. Solubility of different substances usually
varies with temperature. A solution is said to be saturatedif there is undissolved solute in
equilibrium with the solution. If a solution contains more solute that can dissolve at a given
condition it is called a supersaturatedsolution, and if less solute dissolves in the solution than it
can dissolve at a given temperature it is said to be unsaturated.

Table 8.1 Solubility of some salts at different temperature in grams of anhydrous salt per 100 g
of water are given in the following table.
Temp. o C CuSO4NaCl CaCrO4KNO3
0 14.3 35.7 13.0 13.3
10 17.4 35.9 12.0 21.0
20 20.7 36.0 10.4 31.6
30 25.0 36.3 9.4 45.8
40 28.5 36.6 8.5 63.9
50 33.3 37.0 7.3 85.5
60 40.0 37.2 6.0 111.0
70 - 37.9 5.3 139.0
80 55.0 38.4 4.4 -
90 - 39.0 3.8 202.0
100 75.4 39.8 3.0 246.0

Note from the above table that the solubility of CaCrO4decreases with increasing temperature
while the others show increase in solubility with temperature.

General Solubility Rules for Inorganic Compounds

Nitrates (NO3–): All nitrates are soluble.
Acetates (C2H3O2–): All acetates are soluble; silver acetate is moderately soluble.
Bromides (Br–) Chlorides (Cl–) and Iodides (I–): Most are soluble except for salts containing
silver, lead, and mercury.
Sulfates (SO42–): All sulfates are soluble except barium and lead. Silver, mercury (I) and calcium
are slightly soluble.
Hydrogen sulfates (HSO4–): The hydrogen sulfates (aka bisulfates) are more soluble than the
sulfates.
Carbonates (CO32–), phosphates (PO43–), chromates (CrO42–), silicates (SiO42–): All carbonates,
phosphates, chromates, and silicates are insoluble, except those of sodium, potassium,
andammonium. An exception is MgCrO4, which is soluble.
Hydroxides (OH–): All hydroxides (except lithium, sodium, potassium, cesium, rubidium, and
ammonium) are insoluble; Ba(OH)2, Ca(OH)2and Sr(OH)2are slightly soluble.
Sulfides (S2–): All sulfides (except sodium, potassium, ammonium, magnesium, calcium and
barium) are insoluble. Aluminum and chromium sulfides are hydrolyzed and precipitate
as hydroxides.
Sodium (Na+), potassium (K+), ammonium (NH4+): All sodium, potassium, and ammonium
salts are soluble. (Except some transition metal compounds)
Silver (Ag+): All silver salts are insoluble. Exceptions: AgNO 3and AgClO4; AgC2H3O2and
Ag2SO4are moderately soluble.
Apparatus and chemicals
Evaporating dish Bunsen burner
Balance wire gauze
Thermometer glass rod
Beaker crucible tongs
Metal ring saturated solution of potassium nitrate
Metal stand
Procedure
1. Take a dry evaporating dish and weigh accurately.
2. Record the temperature of a saturated solution of potassium nitrate.

3. Add about 10 to15 mL of the saturated potassium nitrate solution into the evaporating dish and
take the mass of the solution and the evaporating dish accurately.
4. Take a beaker nearly filled with water and boil the water with a burner flame.
5. With crucible tongs carefully put the evaporating dish with solution on the beaker. Do not heat
the evaporating dish directly on the flame.
6. Continuously stir the solution in the evaporating dish till a fine powder of potassium nitrate
salt remains.
Make sure that there is an opening between the mouth of the beaker and the bottom of the
evaporating dish. Never heat the beaker to dryness. If you have a small volume of water
remaining in the beaker carefully add more water.
7. Cool the evaporating dish; dry the moisture on its outer bottom with a piece of paper.
8. Weigh the evaporating dish with the salt accurately and put the salt in a container prepared for
this purpose.

Experiment 8

Solubility of salts in the water

Name(s)________________________ Laboratory Instructor___________________

Section__________________________ date_________________________________

Format sheet

Mass of empty evaporating dish (X) ______________________g

Temperature of the saturated solution of potassium nitrate (T) ________ oC

Mass evaporating dish + solution (y) _____________g

Mass evaporating dish + residue (n) _____________g

Mass of solution alone (y-x)____________________g

Mass of solute alone (n-x)______________________g

Mass of water lost by evaporating (y-x) –(n-x) = (y-n) __________________g

Solubility of the salt in 100grams of water at T oC

mass of solute ×100

=______________g
mass of water lost by evaporation

Error calculation

(In standard tables look for the solubility of potassium nitrate at above given temperature (T),
and compare with your result above)

practical−theoretical
% error = × 100
theoretical

Possible sources of error _________________

Experiment 9: Vinegar Analysis

General Objective:To determine the percentage by mass of acetic acid via titrimetricanalysis,
making use of the reaction of acetic acid with a strong base, sodium hydroxide.

Theory

Vinegar is an acidic liquid, which is made both naturally and synthetically, from theOxidation of
ethanol, CH3CH2OH, in an alcohol-containing liquid such as wine,fermentedfruit juice (e.g.
cider) or beer. It has been used since ancient times as an important cookingingredient, e.g. in
salad dressings and on fish and chips. The key chemical component ofvinegar is acetic acid,
CH3COOH (systematic name: ethanoic acid). The trivial name,acetic acid, is derived directly
from the word for vinegar, which, for example, in Italian iscalled aceto. The word vinegar itself
derives originally from the Latin vinumaegrum,meaning “feeble wine”. In fact, when a wine has
“gone off” and has acquired a sour taste,this is due to the oxidation of the ethanol in the wine to
acetic acid. (The “corking” ofwine, i.e. tainting of the wine by compounds transferred from or
through the cork, is due toa totally different chemical process.) Vinegar derived from red or
white wine is the mostcommonly used form of vinegar in Mediterranean countries and central
Europe. The aceticacid content of vinegar can vary widely, but for table vinegar it typically
rangesfrom 4 to8 % v/v. When used for pickling, the acetic acid content can be as high as 12 %.

Thepurpose of this experiment is to determine the acetic acid content of commercial vinegar by
titrimetricanalysis.It is used to determine the percent by mass of acetic acid in vinegar. A
measured mass of vinegar is titrated to the phenolphthalein end point with a measured volume of
a standardized sodium hydroxide solution.In any reaction between two or more species; the
reaction equation shows the stoichiometric ratio of reactingspecies. Hence, if the concentration
of one of the solutions is known, the concentrations ofthe others can be determined from the
volumes used.Take,for example, the reaction being investigated today, that between solutions of
aceticacid and sodium hydroxide, NaOH. The reaction equation is:

CH3COOH (aq) + OH–(aq) → H2O(l) + CH3CO2–(aq)

The OH– (from sodium hydroxide) is present at a known molar concentration. A fixed
volume of CH3COOH solution is taken and the OH– solution progressively added until thepoint
at which complete reaction of the substances is reached. This is called the
equivalence point, i.e., the point at which the moles of OH– added equals the numberof moles of
CH3COOH present in the original solution. The incremental process of adding theOH – solution is
called titration. It enables the concentration of the CH3COOH to bedetermined from the
stoichiometric equation and the volume of the CH3COOH solutionneeded to reach the
equivalence point.

Thus the mass of CH3COOH in the vinegar is calculated from the measured moles of CH 3COOH
and its molar mass, 60.05 g /mol:
MassCH3COOHnCH3COOHMCH3COOH
Finally, the percent by mass of CH3COOH in vinegar is calculated:

mas s CH 3 COOH (g)

%bymassCH3COOH = × 100
mass vinegar ( g)

pH Indicators

Up to the equivalence point the reacting solution contains an excess of one reactant (here
CH3COOH); after the equivalence point the solution contains an excess of the other reactant
(hereOH–). We need some means of observing this switch-over. In acid/base titrations(to which
the acetic acid/hydroxide titration belongs), the change in the color of a pHindicator is often used
to identify the switch-over. The point at which this observed changeoccurs is called the end point
of the reaction. An appropriate indicator is one in which theend point and the equivalence point
are as close together as possible.

pH indicators themselves are generally both weak acids and strongly colored dyes, whichrespond
with a dramatic change in color when they react with base, i.e. OH–. Becausethey react with
base, in principle they compete with the acid whose concentration you aretrying to measure (i.e.
CH3COOH). However, because the indicators are so highlycolored, very low concentrations are
required, and you can generally ignore perturbationof the titration by the indicator in your
calculations. However, it is important to keep theindicator concentration low. In this experiment
you will use the indicator phenolphthalein, which undergoes a sudden change in color from
colorless in acidic solution to pink in basic solution. The midpointof the color change occurs at a
pH of 9.5, i.e. already slightly basic. This is a perfectchoice as an indicator for the titration of
acetic acid with hydroxide ion, becausethesolution at the equivalence point of this titration is
slightly basic.
APPARATUS AND CHEMICALS
50 mL beaker0.1M NaOH
100 mL beakerPhenolphthalein
2 Erlenmeyer flasks Potassium hydrogenphthalate
FunnelVinegar sample
25 mL graduated cylinder
Ring stand and burette clamp

Procedures
Standardization

Solutions of sodium hydroxide react slowly with carbon dioxide gas present in the
atmosphere. Consequently, the solution of sodium hydroxide which you will use in
today'sexperiment needs to be standardized (i.e. its concentration accurately determined)
beforeuse. This is done by titrating with a solution of a stable acidic compound of high
puritywhich can be very accurately prepared to a known concentration. This is known as
theprimary standard. In this experiment you will use potassium hydrogen phthalate, KC8H5O4,for
this purpose. The equation for its reaction with hydroxide ion is:

C8H5O4–(aq) + OH–(aq) → H2O(l) + C8H4O42–(aq)

In this experiment, you will perform a series of acid/base titrations. In the course of these
titrations you will become familiar with the technique of titration and the calculations
associated with volumetric analysis.

Safety

Chemical Hazard Identification

 1 M sodium hydroxide-hazardous. Corrosive,irritant. Avoid eye or skin contact.

 Potassium hydrogenphthalate-non-hazardous. Low toxicity,irritant.
 Phenolphthalein-moderate toxicity, irritant. Avoid eye and skin contact.

Risk Assessment and Control

Moderate risk
Pipettes are easily broken, resulting in dangerous jagged glass edges, especially if the
pipette filler is used incorrectly. Ask your lab instructorfor its correct use techniquesbefore
proceeding.Waste Disposalall of the solutions used today can be washed down the sink with
water. Solid wasteshould be thrown in the bin.

Experimental Procedures
NOTE: Failure to follow the correct procedures will result in wildly inaccurate results.
Part AStandardization of 0.1 M sodium hydroxide with the primary
Standard potassium hydrogen phthalate
1)In a clean, dry 100 mL beaker take about 40 mL of the approximately 1 M solutionof NaOH.
Dilute the solution by a factor of ten by pipetting 25.00 mL of it into a 250 mLvolumetric flask
and making the volume up to 250.0 mL with deionized water.Swirl/shake/invert for about 2
minutes to mix the solution thoroughly.

2) Transfer this solution to a 250 mL conical flask and label the solution as 0.1 M NaOH. Retain
this as your stock of 0.1 M sodium hydroxide for standardization.

3) Use an analytical balance in the balance room at the back of the lab to weigh out accurately
about 4 g (anywhere in the range 3.9 – 4.1 g will do) of potassium hydrogen phthalate from the
sample tubes provided into a clean, dry 100 mL beaker . You need to know the mass accurately
to ±0.0002 g for your subsequent calculations.Record the exact mass in your notebook.

4) Add about 80 mL of deionized water to the potassium hydrogen phthalate solid and stir to
dissolve it. Transfer the solution to a 250 mL volumetric flask with the aid of the stirring rod and
a plastic funnel. Add some more deionized water to the flask until just below the mark, mix to
homogenize the solution andthen make the solution up to the mark with deionized water, adding
the water with adropper. (Note: Never add water directly from a wash bottle. You can easily go
past themark and you’d have to throw the solution away and start again). Mix. Transfer
thesolution to a 250 mL conical flask and label it as KC8H5O4.

For your notebook:Calculate the molar concentration of the potassium hydrogen phthalate,
KC8H5O4, solution.

5) Use a pipette to transfer 25.00 mL of your 0.1 M NaOH solution to a conical flask. Add 2
drops of phenolphthalein indicator and swirl to mix. Carry out arapid titration with your
KC8H5O4solution in the burette, gently swirling the conical flaskas you titrate. In yournotebook
record the rough volume required to reach theendpoint (i.e. the volume required to just observe a
persistent colorchange).

6) Pipette another 25.00 mL of your 0.1 M NaOH into a clean conical flask. Add the
indicator. Fill the burette again with the KC8H5O4 solution and record the initial volumein the
burette (in mL to two decimal places) in your logbook. Then titrate the KC8H5O4solution from
the burette into the NaOH solution, slowing down to drop by drop and thensplit drops about 2
mL before the rough titration volume from your last titration. Recordthe final volume of
KC8H5O4 in the burette at the endpoint and hence calculate thetotal volume of KC 8H5O4 solution
added (the titre value) in your logbook.

7) Repeat accurate titrations (as described in (A6)) until you have 3 concordant titre values that
are within 0.10 mL of one another.For your notebook:

Calculate the exact concentration of your roughly 0.1 M solution of NaOH. Check your
concentration with your demonstrator before proceeding to Part B.

Part B Titration of vinegar with standard sodium hydroxide

Sample of vinegar is analyzed for the amount of acetic acid inthe sample. A titration set up is
used for the analysis, using standardized NaOH solution as thetitrant and phenolphthalein as the
indicator. Stoichiometry calculations determine the percent ofacetic acid in the vinegars.

Use the standardizedNaOH solution from part A as your titrant. Record the exact molar
concentration of theNaOH solution. Your instructor will advise you.Be sure to record all data
in the table on your results sheet.

Clean at least two 125- or 250-mL Erlenmeyer flasks. When dry, label each flask and measure
its mass (±0.01 g).

1. Carefully measure and pour 10.00 mL of vinegar into a clean 125 mL Erlenmeyer flask with a
previously measured mass (±0.01 g). Measure the combined mass of the flask and sample.

Add 3-5 drops of phenolphthalein to the solution and rinse the wall of the flask with 20 mL of
deionized water.
2. To properly clean your burette, first rinse the burette with distilled water. Then rinse the
burette with 3 x 5 mL sample of the titrant (NaOH). Allow this solution to drain from the bottom
by opening the stopcock. Make sure the whole interior of the burette has been sufficiently
rinsedwith distilled water and the titrant solution. Discard the titrant used to rinse the burette and
close the stopcock. Fill the burette with titrant as close as you can to the top of the burette. Now
open the stopcock and allow some of the titrant to be released. (This eliminates any bubbles at
the tip which can cause error in your data.) Try to start your titration with the titrant level near
the 0.00 mL mark. However, it does not have to be exactly 0.00 mL, so please do not waste time.
Always record this initial volume. The technique for reading the values from a burette are the
same as those for the graduated cylinder, read the bottom of the meniscus.

3.After properly cleaning your burette, fill the burette with sodium hydroxide solution and record
the initial volume.

4. Titrate your vinegar sample with the sodium hydroxide solution, making sure to gently swirl
your flask as you are adding the sodium hydroxide. Add the sodium hydroxide until you have a
very slight pink color that remains for more than thirty seconds. You will see a pink color as you
add the sodium hydroxide to the flask but will notice when you swirl the flask it disappears. This
means that you have not reached the equivalence point yet and need to add more base. Once the
color remains for more than thirty seconds, you can be confident thatyou have reached the
equivalence point for your titration.

On your first attempt at performing the titration, you may find you have passed the equivalence
point and now have a deep pink color instead of slightly pink. This is okay since you will not
count this trial run when you work on calculations with your data. This trial run is to give you a
good idea as to the number of milliliters of base that need to be added to reach the equivalence
point. Since you are measuring the same amount of vinegar each time, you now will know when
you are getting relatively close to the equivalence point and then you can add more carefully as
you get closer to the volume of base that you need.
5. Repeat steps 1-4 two more times.
6. using the data from step 4, calculate the average percentage of acetic acid in vinegar.
Provide a sample calculation for each calculation you perform in the space provided under
calculations.

Disposal: All test solutions and the NaOH solution in the buret can be discarded in
the sink, followed by a generous flow of water.
Experiment 9
Vinegar analysis
Name(s)________________________ Laboratory Instructor___________________

Section__________________________ date_________________________________
REPORT SHEET
Molar concentration of NaOH: __________mol/
Trial 1 trial 2 trial 3
Titration

1. Mass of flask (g) ________ _________ __________

2. Mass of flask and vinegar (g) _________ ________ __________
3. Mass of vinegar (g)_________ ________ __________
4. Burette reading of NaOH initial (mL) _________ _________ __________
5. Burette reading of NaOH final (mL) __________ _________ __________
6. Volume of NaOH used (mL)_________ __________ __________
Calculation
1. Amount of NaOH added (mol) __________ ___________ ________
2. Amount of CH3COOH in vinegar (mol). __________ ___________ __________
(Same as NaOH)
3. Mass of CH3COOH in vinegar (g)__________ ___________ __________
4. Percent by mass of CH3COOH in vinegar _____________________ ___________
5. Average percent by mass ofCH3COOH in vinegar _____________

References

Skoog, D.A.; West, D.M.;Holler,F.J Fundamental of Analytical chemistry 8 th ed.; Saunders

College Publishing, New York.;2004.
Ebbing, D.D. General Chemistry,5thed.,Houghton Mifflin company, 2001.
Zumdahl,S.S.Chemical Principle 5thed.Houghton Mifflin company, Boston, 2005.
Harvey,D.Modern Analytical Chemistry,McGraw-Hill companies,Inc.,Boston,2000.

Appendix I
Density of pure water (g/cm3) at temperatures ranging from 10.0°Cto 30.9°C by 0.1°C
increments (example: density at 20.6oC = 0.998078 g/cm3).
 Appendix II

Physical Properties of Some Common Laboratory Chemicals

Appendix III
Activity Series