General Chemistry Book
General Chemistry Book
!
!"#$
% " & ' ' ( ($
$ )* +) ,-.+/$ ! #
0 1
0 -.-- % " & '
' ( ($
MEKDELA AMBA UNIVERSITY
DEPARTMENT OF CHEMISTRY
PREPARED BY:
EDITTED BY:
2022
1
Preface and Acknowledgments
This manual was completed with support of chemistry staff members of Mekdela Amba
University. Therefore, I am thankful for their efforts.
2
TABLE OF CONTENT
Content Page
3
To the Student
You are about to engage in what for most of you will be a unique experience. You are
going to collect experimental data on your own and use your reasoning powers to draw
logical conclusions about the meaning of these data. Your laboratory periods are short,
and in most instances, there will not be enough time to come to the laboratory unaware
of what you are to do, collect your experimental data, make conclusions and/or
calculations regarding them, clean up, and hand in your results. Thus, you should read
the experimental procedure in advance so that you can work in the lab most efficiently.
After you’ve read through the experiment, try to answer the review questions we’ve
included at the end of each experiment. These questions will help you to understand the
experiment in advance.
Some of your experiments will also contain an element of danger. For this and other
reasons, your lab instructor is present to assist you. He is your friend. Treat him well
and above all don’t be afraid to ask him questions. Within reason, he will be glad to
help you. Chemistry is an experimental science. The knowledge that has been
accumulated through previous experiments provides the basis for today’s chemistry
courses. The information now being gathered will form the basis of future courses.
There are basically two types of experiments that chemists conduct:
1. Qualitative – to determine the nature of processes, which are often unanticipated and
sometimes unpredictable.
2. Quantitative- to determine the amount of a measurable change in mass, volume, or
temperature, for example, including the time rate of change on processes 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. Invariably there are experimental difficulties encountered in the
laboratory that require care and patience to overcome. There are four objectives for you,
the student, in the laboratory:
1. To develop the skills necessary to obtain and evaluate a reliable original result.
2. To record your results for future use.
4
3. To be able to draw conclusions regarding your results (with the aid of some coaching
and reading in the beginning).
4. To learn to communicate your results critically and knowledgeably.
By attentively reading over the experiments in advance, and by carefully following
directions and working safely in the laboratory, you will be able to accomplish all these
objectives.
5
Course Policies and Information
In this laboratory, you will be working as a team with two or three persons in each
group. During the first lab period your instructor will assign you to a group. You will
then introduce yourself to group members and get to know other members of your
group. Then your instructor will read you important safety rules. In this meeting of the
laboratory, you will also be given your first lab experiment and the rest of this lab period
you will work on a plan of action for the first experiment.
Each student in the group must have a lab Notebook and bring it to the lab every week.
You should keep a good notebook with all the calculations and the results because your
instructor will grade your Lab notebooks at the end of each experiment. Finally, each
member of your group has to write a 5 or 6-page lab report after completing the
experiment. This is going to be an individual report therefore, even if your results are
the same. The reports you write must be your own work. If your instructor finds out
that your report is exactly the same with another member of your group, you will not
receive any credit for that report and he/she may consider it as cheating.
Learning Outcomes
6
Laboratory Maintenance
1. Make sure your Laboratory space(s) is cleaned. Also clean all the equipment’s and
returned them to their assigned positions. Failure to do so will result to a zero grade
for the experiment. NO exceptions please.
2. All glassware must be cleaned before it is put away.
3. Use sponges to clean bench tops and wiping of non-hazardous materials.
4. Laboratory instructors are the ONLY one allowed to clean up corrosive or toxic
materials
5. Sweep up broken glassware with a broom and collect with the dust pan and then
place in the special container provided for glasses.
6. No debris of any type should be left in the sink. Put all debris in allocated containers
7. Make sure all drawers are properly closed and locked when necessary.
General Information
1. Dispense organic solvents, strong acids and bases and other volatile solvents in the
fume hoods.
2. No fee will be collected for broken equipment or glassware. Each broken glassware
and equipment’s will be replaced with two of similar type by the culprit.
Laboratory Techniques
1. Use proper utensils such as crucible tongs to hold or move hot items.
2. Make sure there are no flammable materials near you when lightning a burner
3. Add boiling chips to liquids before heating them up. This will help to prevent
bumping or boil over.
4. Place test tubes in a slanting position away from yourself and others when heating liquids.
Heat liquids at the surface of the liquid.
5. Do not heat up a closed system
6. Heat all substances that emit noxious fumes under the hood
7. Use funnel to transfer liquids into a narrow neck container
8. Use a bulb or pump to pipette a liquid. Never use your mouth
9. Avoid smelling anything unless instructed to do so. While sniffing, gently waffle the
material towards your nose when allowed to do so
10. Do not return excess reagent to its original container
7
11. Do not use your pipette or spatula to remove samples from the stock container. Use
the one provided by the laboratory technologist
12. Correctly label test tubes or other containers indicating their contents
13. Strong acids and bases should be added to water and not vice versa.
1. The chemistry department does not treat injuries or illness. Any injury or illness will
be referred to the University of Mekdela Amba.
2. It is the responsibility of the laboratory instructor(s) on duty to prevent further injury
by taking the appropriate action after the incident. Arrangement should be made to
immediately transport the victim to the Medical Center. If the injury is minor and
the student can walk to the Medical Center, such student should be accompanied by
another person to the Medical Center.
3. An accident report form must be filled at all times even when the victim declines
Medical treatment.
Special Waste
1. The laboratory will provide label containers for hazardous waste. Read the label very
well and dispose the waste appropriately.
2. Organic or toxic wastes such as mercury, lead, chromium should not be dumped
down the drain.
3. Ask when in doubt about proper disposal of waste.
8
Laboratory Safety Rules
The first order of business is to familiarize yourself with the lab room you will be
working in. This safety activity will review rules you are familiar with and introduce
you to new ones rules which are unique to Chemistry. Safety in the laboratory must be
emphasized. The compounds you will work with do have some hazards associated with
them. Therefore, it is important to follow the safety rules outlined in this lab manual.
You should assume that all compounds encountered in the laboratory are toxic and
handle them accordingly. Safety goggles for eye protection are recommended and lab
coats are to be worn by all students at all times when entering the laboratory. Many
chemicals, common in chemical laboratories, will make holes in clothing. Always wash
your hands thoroughly when leaving the laboratory. You should become familiar with
the proper use of the safety 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 intelligent
precautions and a proper understanding of techniques are employed, the laboratory is
no more dangerous than any other classroom. Most of the precautions are just common-
sense practices. These include the following:
1. Wear approved eye protection when required while in the laboratory. Your safety
eye protection may be slightly different from that shown, but it must include
shatterproof lenses and side shields to provide protection from splashes.
9
Typical eyewash Approved eye protections
The laboratory has an eyewash fountain available for your use. In the event that a
chemical splashes near your eyes, you should use the fountain BEFORE THE
MATERIAL RUNS BEHIND YOUR EYEGLASSES AND INTO YOUR EYES. The
eyewash has a "panic bar," which enables its easy activation in an emergency.
2. Eating, drinking, and smoking are strictly prohibited in the laboratory at all times
3. Know where to find and how to use safety and first-aid equipment.
4. Consider all chemicals to be hazardous unless you are instructed otherwise.
Dispose of chemicals as instructed by your instructor. Follow the explicit
instructions given in the experiments.
5. If chemicals come into contact with your skin or eyes, wash immediately with
copious amounts of water and then consult your laboratory instructor.
6. Wear shoes at all times. “Baboosh” shoes are not allowed in the laboratory.
7. Never taste anything. Never directly smell the source of any vapor or gas; instead,
by means of your cupped hand, bring a small sample to your nose (see figure below).
Chemicals are not to be used to obtain a "high" or clear your sinuses.
10
Wafting vapors towards one’s nose
11
Fume hood found in the laboratory
Exhaust hoods have fans to exhaust fumes out of the hood and away from the user. The
hood should be used when noxious, hazardous, and flammable materials are being
studied. It also has a shatterproof glass window, which may be used as a shield to protect
you from minor explosions. Reagents that evolve toxic fumes are stored in the hood.
Return these reagents to the hood after their use.
9. Never point a test tube that you are heating at yourself or your neighbour. It may
erupt like a geyser.
12
Beware of spattering
10. Do not perform any unauthorised experiments.
11. Clean up all broken glassware immediately.
12. 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.
13. Avoid rubbing your eyes unless you know that your hands are clean.
14. NOTIFY THE INSTRUCTOR IMMEDIATELY IN CASE OF AN ACCIDENT
15 Many common reagents, for example, alcohols, acetone, and especially ether, are
highly flammable. Do not use them anywhere near open flames.
16. Observe all special precautions mentioned in experiments.
17. Learn the location of fire protection devices. In the unlikely event that a large
chemical fire occurs, a powder extinguisher and a CO2 extinguisher are available in the
lab.
13
Powder and CO2 extinguishers
In order to activate the extinguisher, you must pull the metal safety ring from the handle
and then depress the handle. Direct the output of the extinguisher at the base of the
flames. The carbon dioxide smothers the flames and cools the flammable material
quickly. If you use the fire extinguisher, be sure to return the extinguisher in at the
stockroom so that it can be refilled immediately. If the carbon dioxide extinguisher does
not extinguish the fire, evacuate the laboratory immediately and call the security. One
of the most frightening and potentially most serious accidents is the ignition of one’s
clothing. Therefore, certain types of clothing are hazardous in the laboratory and must
not be worn. Since sleeves are most likely to come closest to flames, ANY CLOTHING
THAT HAS BULKY OR LOOSE SLEEVES SHOULD NOT BE WORN IN THE
LABORATORY. Ideally, students should wear laboratory coats with tightly fitting
sleeves. Long hair also presents a hazard and must be tied back. If a student's clothing
or hair catches fire. his or her neighbours should take prompt action to prevent severe
burns. Most laboratories have a water shower for such emergencies. A typical
laboratory emergency water shower has the following appearance.
14
A safety shower
In case someone's clothing or hair is on fire, immediately lead the person to the shower
and pull the metal ring. Safety showers generally dump 151 to 190 litres of water, which
should extinguish the flames. These showers cannot be shut off once the metal ring has
been pulled. Therefore, the shower cannot be demonstrated. (Showers are checked for
proper operation on a regular basis, however.)
18. Whenever possible use hot plates instead of Bunsen burners
15
EXPERIMENT- 1: Preparation of Solutions and Concentration
Calculation
Theory
Solutions are most commonly used reagents in the laboratory. Making solutions is a very
common activity for lab workers in a chemistry lab. Proper solution making requires
basic math skills, accurate measurement, and the ability to follow instructions. A
solution is a homogeneous mixture of two or more substances. In a solution, the solute
is the substance that is dissolved in the solvent. Most of the time, the solvent will be
H2O, so if it is not otherwise specified, assume that you should dissolve the necessary
amount of solute calculated in H2O. Vinegar is a solution of acetic acid (the solute) in water
(the solvent). Theconcentration ofa solution representstheamount ofsolutedissolvedina unit amount
of solvent or of solution. Concentration is usually expressed in one of the following ways: as
percentage concentration (%), molar concentration(M), as molal concentration (m), or as normal
concentration (N).
Percent by mass (%w/w) is the mass of the solute divided by the mass of the solution (mass of solute
plus mass of solvent), multiplied by 100.
Molarity(M) is probably the most commonly used unit of concentration. Itis the number of moles
of solute per liter of solution. Molality (m) is the number of moles of solute per kilogram of solvent.
Normality (N) is equal to the gram equivalent weight of a solute per liter of solution. A gram
equivalent weight or equivalent is a measure of the reactive capacity of a given molecule.
16
where M is molarity, V is volume, and the subscripts i and f refer to the initial and final values. Another
way of expressing the concentration of solutions is mole fraction. This is the number
of moles of a compound divided by the total number of moles of all chemical species in the solution.
When diluting more concentrated solutions, decide what volume (V2) and molarity (M2)
the final solution. Volume can be expressed in liters or milliliters. Many of the reagents
used in science are in the form of solutions which need to be purchased or prepared. For
many purposes, the exact value of concentration is not critical; in other cases, the
concentration of the solution and its method of preparation must be as accurate as possible.
The Flinn Laboratory Solution Preparation reference section is designed for both the
novice and experienced solution maker. It provides valuable information on the basic
concepts of preparing solutions and instructions for preparing most solutions required in
the high school science laboratory. Professional quality solutions are possible when high
quality and fresh chemicals and solvents are used, and meticulous procedures are followed.
Laboratory SolutionPreparation
• Determine molarity (M1) of starting, more concentrated solution.
• Calculate volume of starting solution (V1) required using equation dilution
Note: V1 must be in the same units as V2.
M1V1 = M2V2
Example: 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
¾ Add 8.26 mL of concentrated HCl to about 50 mL of distilled water, stir, then add water
up to 100 mL.
17
Mass percent solutions are defined based on the grams of solute per 100 grams of
solution.
Example: 20 g of sodium chloride in 100 g of solution is a 20% by mass solution.
Volume percent solutions are defined as milliliters of solute per 100 mL of solution.
Example: 10 mL of ethyl alcohol plus 90 mL of H2O (making approx. 100 mL of solution) is
a 10% by volume solution.
Mass-volume percent solutions are also very common. These solutions are indicated by w/v%
and are defined as the grams of solute per 100 milliliters of solution.
Example: 1 g of phenolphthalein in 100 mL of 95% ethyl alcohol is a 1 w/v% solution.
Conversion Between Percent Solutions፡ You may wish to convert mass percent to volume
percent or vice versa. If so, follow this procedure:
A 10% by mass solution of ethyl alcohol in water contains 10 g of ethyl alcohol and 90 g of
water.
1. The formula for determining the volume of the component (ethyl alcohol in our example) is:
mass of ethyl alcohol
Volume = mass of ethyl alcohol
density of ethyl alcohol
2. Determine the volume of the total solution by dividing the mass of the solution by the density
of the solution.
3. Determine the percent by volume by dividing the volume of the component by the volume
of the solution. Let’s solve 1, 2, and 3 above as follows:
1. Mass of ethyl alcohol = 10 g (given) Density of ethyl alcohol = 0.794 g/mL (from handbook)
mass
Volume = ———
density
10 g
18
3. Volume percent of solution
volume of ethyl alcohol 12.6
Percent = —————————— = ——— = 12.4%
total volume of solution 101.8
To determine the molarity of a mass percent solution, the density of the solution is required.
Use the following procedure:
1. Determine the mass of solution by multiplying the volume of the solution by the density of
the solution.
mass = volume x density
2. Determine concentration in percent by mass of the solute in solution. Change to the decimal
equivalent.
3. Calculate the molar mass of the compound, MM.
4. Multiply mass (step 1) by mass % (step 2) and divide by molecular mass (step 3) to find the
number of moles present in the whole solution.
5. Divide the number of moles (step 4) by the volume in liters of the solution to find the molarity
of the solution.
Example: Determine molarity of 37.2% hydrochloric acid (density 1.19 g/mL).
1. Mass of solution = 1,000 mL x 1.19 g/mL = 1,190 g
2. Mass % = 37.2 % = 0.372
3. Molar mass of hydrochloric acid = 36.4 g/mol
4. mass x mass % 1,190 g x 0.372
———————— = ———————— = 12.1 moles
MMHCl 36.4 g/mol
¾ Beaker
¾ Analytical balance
¾ Measuring cylinder
¾ Test tube
19
Chemical and Reagents
¾ CuSO4
¾ Distilled water
Procedure
1. Label all tubes with the sample name and concentration, and your group’s initials.
2. Review the use of the balance and weigh boats before beginning.
3. Do the calculations necessary to prepare the solutions 5.0 mL of 300 mg/mL, 4.5 mL of 150
mg/mL, 4.0 mL of 75 mg/mL, 3.5 mL of 37.5 mg/mL,3.0 mL of 18.75 mg/mL for tube numbers
1 through 5. Use the Mass/Volume equation to determine the mass of CuSO4 to measure in
order to give the correct concentration at the volume desired for each sample.
4. Prepare the solutions in labeled 15 mL plastic tubes, using deionized water as the solvent.
Use the vortex on your bench to help dissolve the CuSO4. You may need to let the more
concentrated samples sit in the warm water bath for several minutes in order for the CuSO4
to dissolve fully.
5. Is the difference in concentration of the tubes obvious in one tube versus another? Compare
your tubes’ colors and volumes to the standard “key” solutions prepared by the instructor. If
any of the volumes or colors are obviously wrong, try to identify where you may have made
an error. Then dump them out, and remake them.
6. Keep tube #1 for use in dilution process.
1. You should still have a tube of 5 mL of 300 mg/mL CuSO4 solution (tube #1 from the above
activity). If not, make this solution. This solution will now serve as your 300X stock solution.
2. Label 5 tubes with the concentrations of (150X, 30X, 15X, 3X, and 1X) M and a volume of
5, 7, 5, 5 and 6 mL respectively in your group’s initials. Then, do the calculations in your lab
notebook and prepare the solutions.
3. Prepare a 1:10 serial dilution of the concentrated (300 mg/mL) stock according to 30 mg/mL
with 3 mL, 3mg/mL with 3 mL and 0.3 mg/mL with 3 mL. Do the calculations in your lab
notebook and prepare the solutions in 15 mL plastic tubes. Feel free to check your calculations
with the instructor before beginning to prepare the dilutions.
20
4. When you are done, review your calculations and consider why this is a 1:10 serial dilution.
Does this make sense? Compare the colors and volumes of your samples to others in the class
and to the “key” tubes made by the instructor. If any of the volumes or colors are obviously
wrong, try to identify where you may have made an error. Then dump them out, and remake
them.
Post-Lab Question
1. For mass/volume solutions, show the calculation (equation with all units) for the preparation
of each solution. Then, describe how you would make the solution in an appropriate container.
a) 10 mL of 50 mg/mL CuSO4 solution
3. For each of the following molar solutions, show the calculation (equation with all units) for
the preparation of each solution. Then, describe how you would make the solution in an
appropriate container.
a) 3 L of 0.5 M CuSO4 solution (The MW of CuSO4 is 250 g/mol)
4. For each of the following dilutions, show the calculation (equation with all units) for the
preparation of each solution. Then, describe how you would make the solution in an appropriate
container.
a) 50 mL of 15 mg/mL NaOH solution from 100 mg/mL NaOH
b) 10 mL of 0.5 M CuSO4•5H2O solution from 10 M CuSO4•5H2O solution
21
EXPERIMENT- 2: Mass and Volume Measurements
Objective: To become familiar with measuring, Reading and recording
measurements correctly (significant digits and unit).
Theory
The second type of balance is the digital top loading balance. These are more accurate
than the triple beam balance because they can usually measure to several decimal
places. Top loading balances are useful for measuring chemicals for large quantity
solutions. Top loading balances can usually measure to 400-600 grams, but anything
heavier would max out the balance and you would not be able to get a measurement.
22
Figure 1. Different forms of Balances
23
A) Set-up: Ensure the balance has a stable, level surface to rest on. Plug in the balance
and turn it on by holding in the on/off button for a few seconds. Wait until the digital
reading stays at a constant number and press TARE. This will set the balance to zero.
B) Weighing vessels: In this class, you will use filter paper as the carrying vessel of
the chemical to be weighed. Occasionally, we will need to weigh the chemicals in a
transfer beaker or the actual beaker you are using to carry out your experiment.
C) "TARE"ing the weighing vessel: This is the most common technique to determine
the weight of a dry chemical. It is important to make sure the weigh boat is wiped clean
to prevent contamination and false readings.
Measurement of a Liquid: There are many different ways to measure a liquid also.
Here to, the degree of accuracy varies based on what method you use. The least accurate
measurement is achieved by using the marked gradations on a beaker or flask. These
marks are approximate and usually have a 5% error margin. Next, there is the graduated
cylinder. Graduated cylinders are accurate for large whole number measurements.
They are not useful for decimal measurements, as most graduated cylinders are divided
in whole number gradations. When measuring with a sample with a graduated cylinder,
you should choose a cylinder that is no larger than 10 times the volume you want to
measure. For example, if you need to measure 1 mL of liquid, you should use a 10 mL
graduated cylinder instead of a 1 liter graduated cylinder. Look at your graduated
cylinder. At the top of most graduated cylinders, there is a small TC 20 0 stamped on
the glass. This tells you that the graduated cylinder is manufactured to measure a liquid
accurately at 20 0C. If you are measuring a liquid that is hotter or colder than this
temperature, your measurement may not be completely accurate.
24
The another type of liquid measuring device is the volumetric flask. This type of flask
comes in varying sizes, but they only have one gradation. They are specifically designed
to make solutions of a particular quantity. For example, if you wanted to make one liter
of a 0.9 % salt solution, you would add 9 grams of sodium chloride to enough water to
fill the one-liter volumetric flask to the gradation. This would give you an accurate
measure of the solution you just made. However, you can only use these flasks to make
solutions in the amounts that the flasks are manufactured for usually 1 L, 500 mL, 250
mL, 100 mL, 50 mL, and 25 mL.
Pipettes can also be used to accurately measure liquids. There are two types of pipettes
that can be used to accurately measure a liquid. The first is the standard pipette or a
Mohr pipette. They generally come is varying sizes from 1 mL to 50 mL with different
size gradations marked on them. They are stamped at the top with their accuracy
(usually +/- so many milliliters) and TD 200, which means total delivery at 200 Celsius.
When using a pipette, some type of additional device is necessary to draw the liquid up
into the chamber.
The other type of pipette is the volumetric pipette. It is made the same way the
volumetric flask is made there is only one gradation marked on the pipette. This type
of pipette is used to measure a specific amount of liquid only. They usually come in
varying sizes from 1 mL to 50 mL. As long as you measure accurately to the line, you
will have the marked amount of liquid. Other pipettes are used to transfer liquids, but
cannot be used to accurately measure how much liquid you are transferring unless you
just need to count drops.
25
Figure 3. A typical volumetric pipet, rubber bulbs, and the pipet filling technique.
The measuring device usually contains a scale. The scale, with its subdivisions or
graduations, tells the limits of the device’s accuracy. You cannot expect to obtain a
measurement better than your instrument is capable of reading. Finally, how do
precision and accuracy compare? Precision is a determination of the reproducibility of
a measurement. It tells you how closely several measurements agree with one another.
Several measurements of the same quantity showing high precision will cluster together
with little or no variation in value; however, if the measurements show a wide variation,
the precision is low. Random errors are errors which lead to differences in successive
values of a measurement and affect precision; some values will be off in one direction
26
or another. Accuracy is a measure of how closely the value determined agrees with a
known or accepted value. Accuracy is subject to systematic errors. These errors cause
measurements to vary from the known value and will be off in the same direction, either
too high or too low. A consistent error in a measuring device will affect the accuracy,
but always in the same direction. It is important to use properly calibrated measuring
devices. If a measuring device is not properly calibrated, it may give high precision, but
with none of the measurements being accurate. However, a properly calibrated
measuring device will be both precise and accurate. (See Figure 4) A systematic error
is expressed as the difference between the known value and the average of the values
obtained by measurement in a number of trials.
27
Chemical and Reagent
¾ Water
¾ Sodium chloride
Procedure
Find the mass of the empty beaker and cap empty, add the liquid and find the mass of
the beaker, cap, and liquid together. The difference of the two weights is the weight of
the liquid.
1. Set the balance to 0.0 g then weigh and record the mass of the empty beaker.
2. Measure the amount of liquid and then pour the liquid in the beaker
3. Return to the balance and insure the reading is at 0.0 g
4. Weigh and record the mass of the beaker and liquid
5. The difference between the two masses is the mass of the liquid.
28
Measurement of a Liquid Sample
29
VII. Depress the plunger to the second stop, removing all the liquid from the tip.
VIII. Remove the micropipette from the beaker and remove the tip by pushing the
plunger to the third stop. Throw the tip in the trash.
10. With a plastic transfer pipette, pick up the 1 mL of water from the 50 mL beaker.
Can you tell if you have all of the 1 mL? Why isn’t this type of pipette good for
volumetric measurements?
11. Put a blue rubber bulb on the end of a Pasteur pipette. Draw up into the pipette water
from the 100 mL beaker. Can you tell how much liquid you have just collected?
Post-Lab Questions
1. What are the basic units of length, mass, volume, and temperature in the SI system?
2. What is precision?
3. Define density? Can it be determined from a single measurement?
4. What is the density of an object with a mass of 9.03 g and a volume of 0.1987 mL?
5. What is the weight in kilograms of 950 mL of a substance that has a density of 1.274
g/mL?
6. An object weighs exactly five grams on an analytical balance that has an accuracy of
0.1 mg. To how many significant figures should this weight be recorded?
30
EXPERIMENT 3: Bunsen Burner
Objective: To learn handling the Bunsen burner and study properties of its flame
Theory
Tirrill or Bunsen burners provide a ready source of heat in the chemistry laboratory. In
general, since chemical reactions proceed faster at elevated temperatures, the use of heat
enables the experimenter to accomplish many experiments more quickly than would be
possible at room temperature. Burners come in verity of designs but most operate on the
principle of mixing gas with air to produce a hot flame. Bunsen burners are used to provide
a safe heat source during many laboratory experiments. It serves as the primary heat source
(thermal energy). The principle of work of a bunsen burner is the combustion of a gas
composed of lower hydrocarbons. That may be natural gas (which consists of mainly
methane, CH4) or butane, C4H10, the one used in laboratory and also sold locally in metal
cylinders for domestic needs.
The complete combustion of hydrocarbons produces carbon dioxide and water with a
considerable release of heat energy. Butane for example is completely burnt in
sufficient supply of oxygen according to the equation.
C4H10 + 13O2 → 8CO2 + 10H2O + heat
The complete combustion of butane gas produces a blue nonluminous flame. If the
supply of oxygen is limited, the hydrocarbon would not be completely combusted,
one of the products being carbon.
2C4H10 + 8O2 → 3CO2 + 10H2O + 5C + heat
The incomplete combustion of butane gas produces a yellow luminous flame whose
colour is due to the hot particles of carbon. These move to the air and settle on surfaces
of surrounding objects forming a layer of carbon (commonly known as soot). The
modern bunsen burner has consists of a base, a gas inlet, the gas jet, the air control
vent with a collar for adjusting the air flow, the barrel, and the mouth of the tube
(Figure 5).
31
Figure 5. Diagram of Bunsen burner
The gas flow can be controlled either at the main gas valve or at the gas control valve
at the base of the burner. Manipulation of the air vents at the bottom of the barrel
allows air to enter and mix with the gas. The hottest flame has a violet outer cone, a
pale-blue middle cone, and a dark-blue inner cone; the air vents, in this case, are
opened sufficiently to assure complete combustion of the gas. Lack of air produces a
cooler, luminous yellow flame. This flame lacks the inner cone and most likely is
smoky, and often deposits soot on objects it contacts. Too much air blows out the
flame.
Increasing the air flow to the burner produces more complete combustion and a hotter
flame. The air is increased by opening up the air vent (turning the metal collar). The
air is drawn into the barrel of the burner by the gas coming out of the gas jet. The gas-
air mixture is then ignited above the barrel. The result is a noisy, bluish-colored, three-
cone flame. This blue flame provides the highest possible temperature from the
burner.
32
The flame can also be adjusted by adjusting the gas flow. Major adjustments in gas
flow are made by turning the handle on the natural gas valve. The height and intensity
of the bunsen burner flame depend on both the gas flow and the amount of air available
for combustion. If either of these two gases is too high, the flame will continually
“blow out.” If this happens, turn off the gas and close the air vents, allow the burner
to cool for 30 seconds, and relight the burner with less gas and air pressure.
¾ Bunsen burner
¾ Tongs
¾ evaporating dish
¾ lighter
Procedure
1. Clear off the lab bench. Remove all flammable and combustible materials from the
work area.
2. Connect rubber tubing to the lab burner gas inlet and gas valve. Check for holes or
cracks in the tubing.
3. Close or partially close the air vents on the burner to make it easier to light.
4. Obtain matches, a piezo lighter, or striker (also called a flint lighter). If using
matches or a lighter, light it now.
5. Turn on the gas.
6. Bring the lit match (or lighter) alongside the barrel of the burner and raise it slowly
over the edge of the barrel from the side. If using a flint lighter, hold it slightly off
center of the barrel of the burner and a few inches above the tip. Strike the flint lighter
to create a spark over the gas coming out of the burner.
7. After the burner is lit, thoroughly extinguish the match with water.
33
8. A lit Bunsen burner with closed or partially closed air vents gives a yellow safety
flame. Closing the air vents makes it easier to light the Bunsen burner and to observe
the flame. The soft yellow flame should never be used to heat anything
9. Adjust the air supply by turning the metal collar to get a tight, bright blue, cone-
shaped flame. This is a very hot flame.
10. Never leave a lit burner unattended.
11. Turn off the gas at the gas source when finished using the bunsen burner
POST-LAB QUESTIONS
34
EXPERIMENT- 4: Physical and Chemical Properties
Objective: To distinguish between physical & chemical changes, and the use of
these properties in identifying substances.
Theory
Matter undergoes changes all of the time. There are two types of changes, physical and
chemical. Physical Changes: PHYSICAL PROPERTIES are those properties that can
be observed without altering the composition of the substance. Whereas it is difficult
to assign definitive values to such properties as taste, color, and odor, other physical
properties, such as melting point, boiling point, solubility, density, viscosity, and
refractive index, can be expressed quantitatively. For example, the melting point of
copper is 1087 °C, and its density is 8.96 g/cm3. As you probably realize, a specific
combination of properties is unique to a given substance, thus making it possible to
identify most substances just by careful determination of several properties.
Physical changes occur when the appearance of a substance changes, but chemically
the substance is the same or a physical change occurs when the substance changes state
but does not change its chemical composition. Examples of physical changes are
melting, freezing, or changing size or shape. A physical change also occurs when
substances are mixed and something dissolves, like when making salt water. The water,
salt, and sugar still keep their original properties and the substances can be separated
again. For example, water freezing into ice, cutting a piece of wood into smaller pieces,
etc. The form or appearance has changed, but the properties of that substance are the
same (i.e. it has the same melting point, boiling point, chemical composition, etc.)
Chemical Changes: A chemical change occurs when the atoms making up matter
rearrange to form a new substance with new properties. This usually occurs during a
chemical reaction.
35
Evidence of a chemical change:
A chemical change occurs when a substance changes into something new. This occurs
due to heating, chemical reaction, etc. You can tell a chemical change has occurred if
the density, melting point or freezing point of the original substance changes. These are
only clues… a chemical change has not actually taken place unless matter has changed
into a new substance. Some common examples of chemical changes include rusting,
tarnishing, burning, cooking, and digesting. If you have the chemical equation, you can
tell if a chemical change has taken place by looking to see if the products in the equation
are different from the reactants. The process of dissolving itself may be either a physical
or a chemical one depending on the nature of a solute and a solvent. In this experiment,
you will observe examples of these.
36
Chemical and Reagent
¾ Distilled Water
¾ NaCl
¾ Dilute HCl
¾ AgNO3
¾ Marble or limestone
Procedure
37
residue may splash out of the dish. This is avoided by decreasing the flame. Do not stay
unnecessarily close to the dish.
4. In one of the dishes there will be a residue. Divide it into two portions.
5. To the first portion add 5 mL of distilled water and try to dissolve.
6. To the second portion add 5 mL of dilute HCl and try to dissolve. Note your
observations.
38
EXPERIMENT- 5: Diffusion of Gases
Objective: To verify Grahams law by measuring the relative diffusion rate of two
gas and to observe the motion of gas molecule
Theory
On the account of molecular motion and the great distance between molecules of the
gas one will mix or diffuse with another even against the force of gravity. When
characteristic odour of gas is released in to a room the odour will move through the
room. This proves that the gas molecules have sufficient energy to move through the
air. We call this process diffusion. From a quantitative point of view the kinetic theory
of gases demands the average kinetic energy of molecules of two gases (A and B) to be
equal at the same temperature. Rates of diffusion yield information that can lead to
calculation of the molecular weights of gases. Gases consist of particles that are in
constant rapid motion. This motion causes gases to travel across space (diffuse) and
completely mix with each other.
½ MAV2A= 1/2MBVB2
Where MA and MB are the molecular masses of gas A and B. VA and VB are average
speed of gas molecules A and B respectively. Rearranging and cancellation of the above
equation gives
MB/MA= (VA/VB)2
Heavier gases diffuse at a lower rate than light gases at a given temperature. Rate of
diffusion of gas A/rate of diffusion gas B= (MB/MA)1/2. This mathematical relationship
between the rate of motion and the densities (or molecular motion) of the gases is
expressed in Grahams law. This law states that the rate of diffusion of gases vary
inversely as the square root of their densities (molecular masses). Diffusion of hydrogen
is four times that of oxygen. In this experiment, the rates of diffusion of two gases,
ammonia (NH3) and hydrogen chloride (HCl), will be investigated. These gases are
convenient to use for such an experiment because, when they meet and react, they form
a white smoke consisting of ammonium chloride (NH4Cl):
NH3(g) + HCl(g) → NH4Cl(s)
Therefore, if ammonia gas and hydrogen chloride gas are released simultaneously at
opposite ends of a glass tube, a white ring of smoke will form at the location where they
39
meet. This experiment will demonstrate rates of diffusion, a property of gases
investigated by Thomas Graham. In 1829, he proposed his law of diffusion which states
that the rate of diffusion of a gas is inversely proportional to the square root of its
density:
R =
√
However, since the ideal gas law indicates that the density of a gas and its molecular
weight are proportional, we can write:
R = 1/(√MW)
If the rates of diffusion of two gases are compared, this yields the following equations
1
= √1
1
√2
Thus, if the rates of diffusion of two gases are known and the molecular weight of one
of them is known, the molecular weight of the other gas can be calculated:
( )
=
In this experiment, the distance each gas travels will be measured as well as the time it
takes for them to meet and react (D = distance, t = time):
=
40
Material and Instrument
¾ Glass tube
¾ cotton
¾ stand
¾ lamps
¾ ruler
¾ cork or stopper
¾ beaker
¾ Conc. ammonia
¾ HCl
Procedures
1. Clamp a glass tube horizontally and insert a piece of cotton wool at each end of the
tube using a tong.
2. Using a medicine dropper place 5 drops Conc. HCl on one plug of cotton wool at the
same time as another student in adding five drops of Conc. aqueous ammonia to the
other plug.
3. As quickly possible to record the time of start and gently cork/close both end of the
tube.
4. Record the time immediately when a white ring is formed and indicate the point at
which the ring occurs with a marker and measure the distance from this mark to the
inner edge of each pieces of cotton wool.
5. Clean the tube by pushing cotton pad with glass rod and repeat the above again.
POST-LAB QUESTIONS
1. Which one diffuses faster? Show by calculating their rate: NH3/HCl, H2/N2, N2/O2
2. In the laboratory experiment gas X was found to diffuse at the rate three times that
of the gas Y. Calculate the molar mass of Y interms of gas X.
3. How did an increase temperature affect each diffusion distance? Explain?
41
4. Arrange the following in their increasing rate of diffusion under the same conditions. H2,
CO, CO2 N2, He, O2, SO2
5. How many times faster will CH4 gas diffuse compared to C4H8 gas?
6. If CH4 gas and C4H8 gas are released simultaneously at the left and right ends respectively
of a 50.0 cm long glass tube, at what distance from the left end of the tube will they meet?
7. Methane gas, CH4, diffuses 2.3 times faster than an unknown gas at the same temperature
and pressure. What is the molecular weight of the unknown gas?
8. Does the first appearance of the white smoke indicate the first contact of the NH3 and HCl
molecules? Explain your answer. If the answer is “no”, how will this affect the calculated value
of the molecular weight of HCl?
42
EXPERIMENT- 6: The Acid- Base Reaction
Objective: To determine total acidity of milk via acid-base titration, making use of the
reaction of weak acid with a strong base
Theory
Titrimetry is a chemical method for determining the concentration of the solution using another
solution of known concentration, called standard solution or titrant. Titration is the slow
addition of one solution of a known concentration to a known volume of another solution of
unknown concentration until the reaction reaches completion. Acid-Base titration involves
neutralization reaction between an acid and a base. Its basis is the equivalence point, wherein
the amount of the titrant added is stoichiometrically equivalent to the amount of analyte, thus,
the concentration of the unknown can be calculated. The type of acid-base titration where
titrant is strong base solution is called Alkalimetry. Sodium hydroxide is the titrant wide used
in titrating various foods and drinks to determine its acidity. Food acids are usually organic
acids, with citric, malic, lactic, tartaric, and acetic acids being the most common. The organic
acids present in foods influence the: flavor (i.e., tartness), color (though their impact on
anthocyanin and other pH-influenced pigments), microbial stability (via inherent pH-sensitive
characteristics of organisms), keeping quality (arising from varying chemical sensitivities of
food components to pH).
Organic acids may present:
• Naturally,
• By Fermentation,
• Added as part of a specific food formulation.
The importance of determining food acidity:
1) To determine the degree of maturity of fruits and vegetables and crop (The titratable acidity
of fruits is used, along with sugar content, as an indicator of maturity, generally the higher the
maturity, the lower the acid content. e.g. in the ripening process).
2) To determine the freshness of foods (for example in milk, the more the lactic acid levels,
means that milk is rotten.
3) Acidity indicators reflect the quality of food (the amount of organic acids in food directly
affects the food flavor, color, stability, and the level of quality.
4) Determination of acid on the microbial fermentation process (such as: fermentation products
in soy sauce, vinegar and other acids is an important indicator of quality).
43
There are two ways to express food acidity: Total Acidity or Titratable Acidity (TA) refers to
the total concentration of free protons [H+] and undissociated acids in a solution that can react
with a strong base and be neutralized. Active Acidity (AA) is the concentration only of free
the H+ protons that are present in the solution. The measure of the active acidity is the pH of
the solution. AA is only part of the total acidity and can not be greater than it. A Titratable
Acidity titration will generally use the strong base, NaOH, and either a chemical indicator or
pH meter to signal when equivalent amounts of base have been metered into the sample. The
concentration of sodium hydroxide used is typically 0.1 N.
Principle is alkalimetry i.e. neutralization with sodium hydroxide solution of known normality
using a suitable indicator, such as methyl orange, phenolphthalein indicator, etc. The choice of
the indicator depends on the pH when the colour changes and which acid is titrated. For the
titration of weak acids by strong base we choose indicator with colour rearrangement at higher
pH (6, 8 to 10) i.e. phenolphthalein indicator.
ACID-BASE INDICATORS
The equivalence point, as we have seen, is the point at which the number of moles of
OH‾ ions added to a solution is equal to the number of moles of H+ ions originally
present. To determine the equivalence point in a titration, then, we must know exactly
how much volume of a base to add from a burette to an acid in a flask. One way to
achieve this goal is to add a few drops of an acid-base indicator to the acid solution at
the start of the titration. An indicator is usually a weak organic acid or a base that has
distinctly different colors in its nonionized and ionized forms. These two forms are
related to the pH of the solution in which the indicator is dissolved. The end point of a
titration occurs when the indicator changes color. However, not all indicators change
color at the same pH. Therefore, the choice of indicator for a particular titration depends
on the nature of the acid and base used in the titration (that is, whether they are strong
or weak). By choosing the proper indicator for a titration, we can use the end point to
determine the equivalence point.
Let us consider a weak monoprotic acid that we will call HIn. To obtain an effective
indicator, HIn and its conjugate base, In‾, must have distinctly different colors. In
solution, the acid ionizes to a small extent:
44
If an indicator is in a sufficiently acidic medium, the equilibrium, according to Le
Châtelier’s principle, shifts to the left and the predominant color of the indicator is that
of the nonionized form (HIn). On the other hand, in a basic medium the equilibrium
shifts to the right and the color of the solution will be due mainly to that of the conjugate
base (In‾). The end point of an indicator does not occur at a specific pH; rather, there is
a range of pH within which the end point will occur. In practice, we choose an indicator
whose end point lies on the steep part of the titration curve. Because the equivalence
point also lies on the steep part of the curve, this choice ensures that the pH at the
equivalence point will fall within the range over which the indicator changes color.
Table 5.1 lists a number of indicators commonly used in acid-base titrations. The choice
of a particular indicator depends on the strength of the acid and base to be titrated.
Color
As the acidity has a major influence on the taste of the product, this parameter is used
to test the quality of milk. As the acidity of milk increases with the storage time, this
parameter is also a means of checking storage conditions. The acidity of milk is of two
kinds. Natural acidity which is due to citrates and phosphates present in the milk and
45
dissolved CO2 during the process of milking and thereafter. Developed acidity which is
due to lactic acid produced by the action of bacteria on lactose in milk.
Usually, acidity of milk is expressed as percentage of lactic acid. In this case the acidity
of cow milk ranges from 0.10 to 0.26 %. Generally, the acidity of milk means the total
acidity (Natural + developed) or titrable acidity. Fresh, freshly baked milk has the total
acidity of 16 – 18°T, but after two hours (if the milk has not cooled) the acidity rises.
Milk allowed for sale has an acidity of less than 21°T.
¾ Burette
¾ Volumetric pipette
¾ Volumetric flasks
¾ Conical Erlenmeyer flasks
¾ Beakers
¾ Graduated cylinder
¾ Stand
¾ Funnel
¾ Balance
¾ Sodium hydroxide
¾ Phenolphthalein indicator
¾ Deionized water
46
PROCEDURE
. .
%= ! "%
47
EXPERIMENT- 7: Determination of Solubility of Salts
Theory
The solubility of solute is the amount of solute dissolved in a given amount of a solution
at equilibrium of specified condition. The usual units used to express solubility are gram
of solute per 100 grams of solvent at a specified temperature. Solubility of different
substance usually vary with temperature. A solution said to be saturated if there is un
dissolved solute in equilibrium with the solution. If a solution contains more solute that
it can dissolve at a given condition it is called a supersaturated solution, and if less
solute dissolves in the solution than it can dissolve at a given temperature it is said to
be unsaturated. The one component of a solution, which is usually present in the
greatest proportion, is called the solvent. The other components, present on a smaller
scale, called solutes, are considered to be dissolved in the solvent. There are a number
of different kinds of solutions: gases in gases (example: air), liquid in liquids (example:
gasoline), gases in liquids (example: carbonated soft drinks), solids in solids (example:
alloys such as brass), and solids in liquids (example: salt water). This experiment will
involve a solution formed with a solid solute (a chemical salt) and a liquid solvent
(water).
If the properties of a solution remain constant, the system of solute and solvent is
considered to be at equilibrium. Obviously, if the solid is disappearing into the solvent,
the system is not at equilibrium. Solubility of a solid in a liquid is dependent on
temperature, thus, at a given temperature, only a certain maximum amount of solute
will dissolve in a given amount of solvent. Beyond that amount of solute, no more will
dissolve and excess solute will remain in the solid form, settling to the bottom of the
solution container. This maximum amount of dissolved solute, expressed
quantitatively, is given in units of grams of solute/100 g of solvent. Such a solution is
termed a saturated solution, since it is holding all the solute it can hold at that
temperature. Experiments show that when excess solute is in contact with a saturated
solution, equilibrium is established in which solute is continually dissolving in amounts
just equal to the solute separating from solution (crystallization).
48
When saturated solutions of solid solutes are prepared at elevated temperatures and then
permitted to cool, the excess solute usually separates from the solution by crystallizing.
However, if a saturated solution is prepared at an elevated temperature and any excess,
undissolved solute is removed, crystallization often does not take place when the
solution is allowed to cool undisturbed. The solution can contain more of the solute
than normally is held in equilibrium with the solid state. Such solutions are said to be
supersaturated. A supersaturated solution is a system in unstable condition. Agitation
of the solution or the addition of a seed crystal of the solute may start crystallization of
the excess solute. After crystallization, a saturated solution remains. In general, when a
solution, which is nearly saturated with a solid solute is cooled, a temperature is reached
at which the solution becomes saturated. On further cooling, the excess solute will
crystallize, and will appear as particles separated from the solution. For solutions of
various salts in water it has been found that temperature effects on solubility vary from
salt to salt. Salts are usually more soluble at elevated temperatures than at lower
temperatures. In addition, the change in solubility for a given salt, say between 20° and
30°C, may not be the same as the change in its solubility between 50° and 60°C.
In this experiment, you will study the solubility of potassium nitrate (KNO3) in water.
You will dissolve different quantities of this salt in a given amount of water at a
temperature close to the water’s boiling point. Each solution will be observed as it
cools, and the temperature at which crystallization of the salt occurs will be noted and
recorded. The start of crystallization indicates that the solution has become saturated.
At this temperature, the solution contains the maximum quantity of solute that can be
dissolved in that amount of solvent. After solubility data for several different quantities
of solute have been collected, the data will be plotted on a graph. A solubility curve
for KNO3 will be constructed by connecting the plotted points.
49
Chemicals and Reagent
¾ Potassium nitrate (KNO3) and Distilled water
Procedure
1. Your instructor has set up four numbered test tubes at your station. Place the
numbered test tubes in a test tube rack.
2. Using the electronic balance and a weighing boat, measure out exactly 2.0 g of
potassium nitrate (KNO3). Pour the salt into test tube #1.
3. Repeat step 2 for the following masses of KNO3. Add each quantity to the test
tube indicated:
4.0 g to test tube #2
6.0 g to test tube #3
8.0 g to test tube #4
4. Add exactly 5.0 mL distilled water to each test tube.
5. Fill a 500 mL beaker about three-fourths (3/4) full of tap water. This will be used as
a water bath for all test tubes. Using a hot Plate, heat the water bath to about 90 0C,
maintain the water at this temperature.
6. Using a glass stirring rod carefully stir the KNO3 water mixture until the KNO3 is
completely dissolved. Remove the stirring rod and rinse it off.
7. Once dissolving is complete, remove the test tube from the hot water bath. Place a
warmed thermometer into the test tube, raise the test tube to the light and begin to
observe at what temperature crystallization occurs.
8. Procedural steps 6 & 7 should be followed for all four test tubes. Record all
temperatures in your data table.
9. If any doubtful results are obtained, the procedure can be repeated by re-dissolving
the KNO3 in the hot-water bath and allowing it to once again re-crystallize.
10. While running water, dispose of KNO3 down the drain. Rinse all test tubes.
50
Observation and Data
Crystallization
Test Tube # grams of KNO3/5.0 mL H2O temperature (oC)
1 2.0 g/5.0 mL ______________
2 4.0 g/5.0 mL ______________
3 6.0 g/5.0 mL ______________
4 8.0 g/5.0 mL ______________
51
EXPERIMENT- 8: Simple Distillation
Theory
Distillation is a separation process that involves heating a liquid to its boiling point,
transferring the vapour to a different portion of the apparatus, then condensing the
vapour and collecting the condensate in another container. This technique is one of the
most useful for separating a mixture of liquids when the components have different
boiling points. Industrially, distillation is the basis for the separation of crude oil into
the various, more useful hydrocarbon fractions. Chemically, distillation is the principal
method for purifying liquids (e.g. samples, or solvents for performing reactions).
When the difference in boiling points of the components is large (>40-60 °C), a fairly
good separation often can be made with a simple distillation. When the difference in
boiling points of the components is small, then a simple distillation cannot achieve a
good separation. If a better separation is desired when the components have similar
boiling points, then a fractional distillation can be done. The fractionating column can
be thought of as a place where the vapors condense and then boil again. Each time a
very small sample condenses and then boils again, the vapor is even more enriched in
the more volatile (lower boiling) component. Thus, fractional distillation can produce
samples that are much purer. This increase in purity comes with a cost of more complex
equipment and more distillation time.
52
Figure 7. Laboratory display of distillation
¾ Water bath
¾ Still pot
¾ Thermometer
¾ Condenser
¾ Receiving flask
¾ Vacuum adaptor
53
Procedures
1. The distillation is performed directly heating the flask but by placing it on water
bath.
2. Pour 25 mL of the provided contaminated ethyl alcohol (by a dye or glycerin or
ethylene glycol) in to the dry distilling flask by means of funnel.
3. Add 2 or 3 pieces of boiling chips. Place the thermometer so that its bulb is about
0.5 cm below the junction of the side arm of the distilling flask.
4. Get you set up checked by the instructor before starting the distillation.
5. Collect the distillate in a measuring cylinder and record the boiling point after 2
mL.
6. 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.
7. Turn off your gas and stop the distillation when no more drops will come out.
8. Record the data. Check the boiling point of organic liquid in a hand book or in a
text book and record this as well. Discuss the results by plotting the graph.
1. Why does not all the liquid vaporize at once when the boiling point is reached?
2. If the liquid to be distillated had a boiling point higher than 90 0C, what kind of
bath would you use?
3. Why are boiling chips added to the liquid before heating is begun?
4. How do you know when distillation is complete?
54
EXPERIMENT- 9: Fractional Distillation
Theory
55
The composition of the liquid remaining in the flask changes gradually by becoming
richer in the higher boiling component. The boiling point of the mixture therefore rises
as the distillation proceeds. If the distillate s collected infractions, and the fractions
redistilled almost complete separation is achieved. Separation is, of course, easiest if
there is a large boiling point between the two liquids. This is the essence of fractional
distillation column repeated distillation is carried out in a simple way with the help of
the fractionated column which in effect causes several tiny distillation.
¾ Water bath
¾ Still pot
¾ Thermometer
¾ Condenser
¾ Receiving flask
¾ Vacuum adaptor
Procedures
1. Arrange a set up of for fractional distillation following the one prepared for
demonstration.
2. This set up differs from that of simple distillation by introduction of a fractionated
column.
3. Pour the provided 50 mL of ethanol- water mixture (1:1) into distillate flask. Place
the distilling flask over a water bath, introduce two or three boiling chips, get the set up
checked by the instructor and then start the fractional distillation.
4. Collect the distillate directly into a measuring cylinder and record the temperature
after every 12 mL.
5. Change the receiver and record the temperature after every 12 mL.
6. After collecting of two fractions the temperature begins to fall down so that remove
the water bath and heat the flask with a gentle flame.
7. Hand over the distillate separately to your instructor and report the volume of the
each and the boiling point ranging during collection.
56
8. Estimate the percent composition of the starting ethanol-mixture.
9. If possible, calculate the specific gravity of the two fractions by determining the
weight of empty 10 mL measuring cylinder and then add 10 mL of fraction 1 to it and
weight again.
10. Find the specific gravity of each fraction this way. Note that the specific gravity of
pure ethanol is 0.8. Tabulate your data and a graph showing the relationship of (y-axis)
and volume (x-axis).
57
EXPERIMENT- 10: Extraction
Theory
Generally organic compounds are obtained from different sources including plant
materials (wood, bark, seeds, leaves, flowers, herbs, and marine source), animal, and
petroleum. The organic compounds can be separated and purified by one of the
following methods:
a) Solid organic compounds can be isolated and purified by extraction, sublimation or
recrystallization
b) Liquid organic compounds can be isolated and purified by simple distillation,
fractional distillation, distillation under reduced pressure, steam distillation, etc
58
Extraction is a very common laboratory procedures used when isolating or purifying a
reaction product from reaction mixtures or natural products of large number of organic
compounds. If the impurities present are solids then a solvent is so chosen as would
dissolve only the compound to be purified and not the impurities. A heterogeneous
mixture of impurities as solid and compounds in liquid phase is obtained. The liquid
solution is obtained from solid by filtration. The filtrate containing is collected and the
organic compound obtained in pure form after evaporation of solvent. If the organic to
be purified to be present in aqueous solution then it is a separating funnel. Now a solvent
in which the compound to be purified is more soluble than water and which is miscible
with water is added. The contents are mixed by shaking for some time and then the
solution allowed to stand when separate layers are obtained in separating funnel. The
layers are separated by decanting the lower layer to the receiving. After repeated
extraction solvent solution of the compound is dried by drying agent and distilled to
remove solvent, leaving behind the pure organic compound.
59
Note: common extraction solvents are petroleum ether, diethyl ether, and methylene
chloride
¾ Filtration set up
¾ Test tube
¾ Separatory funnel
¾ Beakers
¾ Benzoic acid
¾ Water
¾ Diethylether
¾ Drying agent
Procedures
60
POST- LAB QUESTIONS
1. Calculate the percent recovery of each component in a mixture. (Assume that each
component was present in equal amount in your sample.
2. During an extraction, if you became uncertain about which layer is the organic layer,
how can you determine it experimentally?
3. From the result of this experiment, what can you conclude about the solubility’s of
each component in your mixture?
61
EXPERIMENT- 11: Recrystallization
Theory
Almost all solids are more soluble in a hot than in a cold solvent, and solution
crystallization takes advantage of this fact. Thus, if a solid is first dissolved in an
amount of hot solvent insufficient to dissolve it when cold, crystals should form when
the hot solution is allowed to cool. The extent of precipitation of the solid depends on
the difference in its solubility in the particular solvent at temperatures between the
extremes used. The upper extreme is determined by the boiling point of the solvent,
whereas the lower limit is usually dictated by experimental convenience. For example,
an ice-water bath is often used to cool the solution to 0 0C, whereas ice-salt and dry ice-
acetone baths are commonly used to cool solutions to -20 0C and -78 0C, respectively.
The solid should be recovered with greater efficiency at these temperatures, provided
the solvent itself does not freeze.
If the impurities present in the original solid mixture have dissolved and remain
dissolved after the solution is cooled, isolation of the crystals that have formed should
62
ideally provide pure material. Alternatively, the impurities may not dissolve at all in
the hot solution and may be removed by filtration before the solution is cooled. The
crystals that subsequently form should be purer than the original solid mixture. Solution
recrystallization is seldom quite so simple in practice, but these two idealized
generalizations do outline the basic principles of the technique. Even after a solid has
been recrystallized, it may still not be pure. Thus, it is important to determine the purity
of the sample, and one of the easiest methods to do this is by determining the melting
point of the solid. The technique of solution recrystallization involves the following
steps:
l. Selection of an appropriate solvent.
2. Dissolution of the solid to be purified in the solvent near or at its boiling point.
3. Decolouration with an activated form of carbon, if necessary, to remove colored
impurities and filtration of the hot solution to remove insoluble impurities and the
decolorizing carbon.
4. Formation of crystalline solid from the solution as it cools.
5. Isolation of the purified solid by filtration.
6. Drying the crystals.
A most suitable solvent for recrystallization should:
a) Dissolve the substance to be purified at elevated temperature but not at room
temperature
b) Dissolve the impurities to be readily or only a very small extent
c) Yield well-formed crystal of the purified compound
d) Not react with the substance that is to be recrystallized
e) Be removed readily from the purified compound. Some of the common solvents
used for recrystallization in clued hexane, benzene, chloroform, ethyl acetate,
acetone, methanol, ethanol, water, and acetic acid
63
Table 2. Some class of substance
¾ Erlenmayer flask
¾ Bunsun burner
¾ Measuring cylinder
¾ Spatula
¾ Filter paper
¾ Buchner funnel
¾ Acetanilide
¾ Benzoic acid
Procedures
64
3. Place 50 mL of water in measuring cylinder and from this add to the boiling mixture
5 mL at a time until all the compound has dissolved. (there may still be small particles
of dirt present).
4. Keep a record of the total amount of water added up to this point.
5. Place the fluted filter paper on stem a stem less funnel and use a flask to collect the
filtrate.
6. Filter the hot solution by pouring it in small portions, keeping the apparatus as hot as
possible.
7. It may help to warm the funnel by placing it in the mouth of the flask or by heating
the entire sep-up.
8. Any precipitate which forms may be redissolved by adding small portions of boiling
water.
9. Do not add more water at this stage because addition of more water will prevent the
formation of crystals.
10. Cool the filtrate to room temperature. If crystals do not form at this, cool this further
by placing it in an ice bath.
11. Scratch the flask with a glass rod if necessary. Collect the crystals by filtering the
solution with the aid of suction flask attached to a water aspirator and a Buchner funnel.
12. A filter paper is on the Buchner funnel; it is washed the aspirator is then turned on
by opening the water tap and after ensuring that there is proper suction the mixture is
poured on it as fat as possible.
13. Make an open paper box, write your name and section (group) on it and keep the
isolated in the paper box till the next laboratory session.
14. You will determine the weight and the melting point of this substance NEXT
WEEK.
Calculate the percent recovered using the following written formula and determine the
melting point of your recrystallized benzoic acid.
65
POST- LAB QUESTIONS
66
EXPERIMENT- 12: Colorimetric Determination of (Paracetamol)
Acetaminophen
Theory
4-hydroxy-acetanilide, often denoted as acetaminophen (Ac), is a non-narcotic
analgesic belonging to the class of nonsteroidal anti-inflammatory drugs (NSAIDs).
However, its clinical use goes back when it was recognized as the main active
metabolite of both acetanilide and phenacetin (4-ethoxy-acetanilide). Up to now it has
been used as a substitute for acetanilide as antipyretic and analgesic because of the
serious collateral effects of the latter.
67
removal of the plasma proteins by precipitation with trichloroacetic acid, followed by
nitration of the paracetamol to give a yellow product, which is converted to a more
intense orange colour by addition of alkali. In view of the apparent advantages of speed
and simplicity inherent in this method it was decided to assess its suitability as a
replacement for the differential absorbance method in this laboratory.
¾ Trichloroacetic acid
¾ Sodium nitrite
¾ Sodium hydroxide
¾ Sulfamic acid
¾ Hydrochloric acid
¾ Paracetamol tablet
¾ Blood
Procedure
68
The validation experiment
69
Experiment -13: Investigating the heat involved in chemical reaction
(Bomb calorimetry)
Objectives: To determine the heat capacity of the metal and enthalpy of combustion
of an oil sample
Theory
70
The Parr bomb calorimeter (see Figure 9) is a self-contained instrument used in
determination of heats of combustion of certain fuels and pure organic substances. The
results obtained are sufficiently precise to make them of extreme importance in most
commercial and laboratory procedures concerned with heats of combustion.
The combustion bomb, made of corrosion-resistant metal, holds the sample whose heat of
combustion is to be measured. The sample is held in a cup and an ignition wire, used to
start the combustion reaction, is attached to the electrodes (see Figure 10).
71
Figure 10 (a) Interior of the bomb vessel.
(b) Schematic of the sample support stand.
(c) Attachment of the nickel-chrome ignition wire.
After the sample and the wire have been properly placed in the bomb, it is charged with
oxygen gas from a commercial cylinder to the pressure of about 25 atm. The assembled
bomb is then placed in a bucket containing a specified quantity of water (2000.00g). The
temperature rise accompanying the combustion is read from a digital thermometer. A stirrer
insures an even distribution of the heat in water. The bucket in turn is surrounded by an
insulating air space, which prevents, as far as possible, heat leakage to the surroundings.
First, it is necessary to obtain the heat capacity of the calorimeter system (Ccal). This is the
number of calories necessary to raise the temperature of the entire calorimeter system by 1
°C. This is found by burning a sample material of known heat of combustion. Benzoic acid
of high purity is usually employed. The temperature rise due to the sample is noted, and
the number of joules of heat released in the combustion is calculated. These two values
enable one to calculate the heat capacity of the calorimeter system Ccal, in kJ/°C or
kcal/°C.
72
−D6EF G ∆H
∆56789 (:;<>?@A BA@C) =
I
I
D6EF = −∆56789 (:;<>?@A BA@C)G
∆H
= -6.318 Kcal/g
Knowing that J6EF = D6EF G ∆H6EF , then we can calculate the heat of combustion of
the assigned material.
Determination of Ccal:
1. You will find an oxygen bomb calorimeter charged with 1.00 g benzoic acid pellet under
an oxygen atmosphere (P ≈ 25 atm).
2. When ready, stand back and let your instructor fire the bomb; start recording the
temperature at 30s intervals by reading the digital thermometer.
3. The bomb is fired by plugging the 19 V battery for 5 seconds.
4. A typical temperature increase during the experiment will be in the range of 4 °C.
73
5. Record the difference between the highest and lowest temperatures reached, ΔT.
6. Compute the heat capacity of the calorimeter Ccal.
1. Then, the oxygen bomb calorimeter is emptied and charged with 1.00 g of oil sample
(Moil = 872.3 g/mol) under an oxygen atmosphere (P ≈ 25atm).
2. When ready, stand back and fire the bomb under the supervision of your lab instructor;
start recording the temperature at 30s intervals by reading the digital thermometer.
3. A typical temperature increase during the experiment will be in the range of 4°C.
4. Record the difference between the highest and lowest temperatures reached, ΔT.
5. Compute comb H of this oil by using the value of Ccal previously determined in above.
Note:
In this experiment, several approximations are made to simplify the calculations of Ccal and
∆H comb. In a more rigorous procedure, several corrections would have to be applied:
- correction of the temperature rise ΔT
- correction for the heat of formation of HNO3 and H2SO4
- correction for the heat of combustion of the Nickel-chrome fuse wire
Moreover, it is recommended to perform 7 trials to get a representative mean value.
Data sheet
1. Determination of Ccal
74
2. Determination of ∆Hcomb oil sample
PRE-LAB QUESTIONS
1. What is a calorimeter?
2. A student has a hot iron rod and thrusts it into a container of cold water. Explain what
will happen in terms of heat flow.
3. Does this experiment violate the Principle of Conservation of Energy? Explain.
4. In an experiment, 1.50 g of sucrose (C12H22O11) is burned and causes the temperature of
the bomb calorimeter to rise from 25.00 °C to 27.88 °C. If the heat capacity of the bomb
calorimeter Ccal is 8.57 kJ/°C, calculate the enthalpy of combustion, expressed in kJ/mol
comb ∆H.
75
REFERECES
76
Buy your books fast and straightforward online - at one of world’s
fastest growing online book stores! Environmentally sound due to
Print-on-Demand technologies.
Buy your books online at
www.morebooks.shop
Kaufen Sie Ihre Bücher schnell und unkompliziert online – auf einer
der am schnellsten wachsenden Buchhandelsplattformen weltweit!
Dank Print-On-Demand umwelt- und ressourcenschonend produzi
ert.
Bücher schneller online kaufen
www.morebooks.shop
KS OmniScriptum Publishing
Brivibas gatve 197
LV-1039 Riga, Latvia info@omniscriptum.com
Telefax: +371 686 204 55 www.omniscriptum.com