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General Chemistry Book

The document is a lab manual for General Chemistry (Chem.1012) at Mekdela Amba University, detailing various experiments and safety protocols for students. It emphasizes the importance of hands-on experimentation to understand chemical theories and outlines objectives for students, including developing skills to obtain reliable results and communicate findings. The manual includes a comprehensive list of experiments, safety rules, and guidelines for lab reports and maintenance.

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0% found this document useful (0 votes)
12 views85 pages

General Chemistry Book

The document is a lab manual for General Chemistry (Chem.1012) at Mekdela Amba University, detailing various experiments and safety protocols for students. It emphasizes the importance of hands-on experimentation to understand chemical theories and outlines objectives for students, including developing skills to obtain reliable results and communicate findings. The manual includes a comprehensive list of experiments, safety rules, and guidelines for lab reports and maintenance.

Uploaded by

adampro212
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
You are on page 1/ 85

            


  

  



  


 
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MEKDELA AMBA UNIVERSITY

COLLEGE OF NATURAL AND COMPUTATIONAL SCIENCES

DEPARTMENT OF CHEMISTRY

GENERAL CHEMISTRY (Chem.1012) LAB MANUAL

PREPARED BY:

(MScin Inorganic Chemistry)


and   (MScin Organic 

EDITTED BY:

Hibstie Tsehay (MSc in Analytical Chemistry)

2022

1
Preface and Acknowledgments

General chemistry is dealing with a number of innovative features, including interactive


exercises and real-world applications, designed to enhance student learning. The
manual covers preparation of solution, diffusion of gas, simple and fractional
distillation, mass and volume measurements, identification of substances by physical
properties, separation of the components of a mixture, chemical reactions, solubility of
salts in water and bomb calorimetry. It’s also concerned with developing the tools used
to examine these properties. Thus, it is important that students of chemistry do
experiments in the lab to more fully understand the theories they study. The manual
helps students understand the timing and situations for the various techniques. Each
experiment is presented with concise objectives, a comprehensive list of techniques,
and detailed lab introduction, step-by-step procedures and discussion questions at the
end of each lab. It is also important that you carefully prepared for each experiment by
reading the related text material before coming to the lab. This way you can maximize
the laboratory experience.

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

Preface and acknowledgments 2


To the student 4
Course policies and information 6
Learning outcomes 6
Format of the lab report 6
Laboratory maintenance 7
Laboratory safety rules 9
Experiment- 1: Preparation of solutions and concentration calculation 16
Experiment- 2: Mass and volume measurements 22
Experiment 3: Bunsen burner 31
Experiment- 4: Physical and chemical properties 35
Experiment- 5: Diffusion of gases 39
Experiment- 6: The acid- base reaction 43
Experiment- 8: Simple distillation 52
Experiment- 9: Fractional distillation 55
Experiment- 10: Extraction 58
Experiment- 11: Recrystallization 62
Experiment- 12: Colorimetric determination of (paracetamol) acetaminophen 67
Experiment -13: Investigating the heat involved in chemical reaction (bomb
calorimetry) 70
Refereces 76

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.

Best wishes for an error-free and accident-free term!

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

At the end of this course students should be able to:

x To become acquainted with safety rule and use appropriate laboratory


equipment
x Identify substance by evaluating physical properties
x Perform solution preparation
x Familiarize the students with the techniques of simple and fractional
distillation.
x To perform separation of mixture

Format of the Lab Report


You should prepare your lab reports by handwriting. They should include tables and
illustrations where necessary. Typically, a lab report should contain the following
sections: title page, introduction, experimental section, results and discussion,
Conclusion and references. Your title page should be a separate page including the
title of the project which might simply be the name of the experiment, your name, name
of the course and the date the report is due.

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.

Emergencies and Fires

1. Laboratory instructors are in-charge of all emergencies. Follow instructions as


directed
2. All laboratory users should learn how to locate the following materials: safety
shower, eyewash, blankets, fire extinguishers, first aid kit, fire alarm
3. Laboratory users should notify the laboratory instructors of any fire.
4. Turn off all gas jets if it is the source of the fire
5. All laboratory users should learn how to use the fire extinguisher

Accidents and Injuries

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

8. Perform in the hood any reactions involving skin-irritating or dangerous chemicals


and/or ill-smelling chemicals. A typical fume exhaust hood is shown below.

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

Objective: To prepare different concentrated solution

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.

Volume percent or volume/volume percent most often is used when preparing


solutions of liquids. Volume percent(%v/v) is defined as volume of solute divided by
the volume of the solution 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.

Dilution is adding solvent to a solution. Adding solvent results in a solution of lower


concentration. You can calculate the concentration of a solution following a dilution by
applying this equation:
MiVi = Mf Vf

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.

Example: Prepare 800 mL of 2 M sodium chloride.


(MM NaCl = 58.45 g/mol)
gNaCl = 58.45 g/mol x 2 mol/L x 0.8 L
gNaCl = 93.52 g NaCl
¾ Dissolve 93.52 g of NaCl in about 400 mL of distilled water, then add more water until
final volume is 800 mL. If starting with a solution or liquid reagent:

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

Volume of ethyl alcohol = ————— = 12.6 mL


0.794 g/mL
2. Mass of solution = 100 g (given)
Density of solution (10% ethyl alcohol) = 0.983 g/mL (from handbook)
100 g
Volume of solution = ————— = 101.8 mL*
0.983 g/mL

18
3. Volume percent of solution
volume of ethyl alcohol 12.6
Percent = —————————— = ——— = 12.4%
total volume of solution 101.8

Calculating Molarity from Percent Solutions

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

5. Molarity = moles/liters = 12.1 moles/1 liter = 12.1 M

Material and Instrument

¾ Beaker
¾ Analytical balance
¾ Measuring cylinder
¾ Test tube

19
Chemical and Reagents

¾ CuSO4
¾ Distilled water

Procedure

Procedure for Making Solutions of Differing Mass/Volume Concentrations

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.

Procedure for Making Dilutions of Concentrated Solutions

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

2. Express the % mass/volume concentrations in g/mL units:


a) 5% CuSO4: ___________________g/mL CuSO4

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)

b) 400 mL of 50 mM glucose solution (The MW of glucose is 180 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

Chemistry is a science that depends on experience and observation for data. An


experiment that yields data requires the appropriate measuring devices in order to get
accurate measurements. Many experiments require some type of measurement, and are
often simple measurements of mass and volume. The validity of an experiment is
dependent on the reliability of these measurements. A measurement’s reliability is
usually considered in terms of its precision. Quantitative measurements are
fundamental to chemistry. One must become familiar with different units of
measurement used to quantify base quantities (such as temperature, length, time, mass,
etc.). You must always keep in mind that every measurement inherently will have an
uncertainty associated with it. This means that a measurement is only as certain as the
instrument used to make the measurement.

Measurement of a Solid: The most common way to measure, a solid is by using a


balance. The first type is the triple beam balance. This balance uses a series of counter
weights to determine the weight of the sample that is placed on a weighing pan. This is
the least accurate of the balances that are available for sample weighing, because a triple
beam balance can only measure to the ones place (no decimal). This can give you a
very rough determination of the weight of your sample.

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

Measuring mass of chemicals is a very common and important step in fulfilling


chemistry labs. Most chemistry labs now use forms of electronic balances - a more time
efficient and user-friendly instrument. The digital readouts are also more precise than
the traditional beam balance. The electronic balance has only one removable part - the
weighing pan. It is a sensitive instrument requiring proper usage, care, and
maintenance. In this activity, you will learn:
9 The proper use of the electronic balance
9 The proper method to weigh out a desired amount of dry chemical
9 Proper set-up and care of the electronic balance
9 Different techniques to measure mass of a chemical

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.

Figure 2. Graduate cylinder

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 most accurate method to measure liquids is by using a micropipette. Micropipettes


are generally used to measure liquids in units smaller than the milliliter, although there
is a micropipette that can measure up to 1 milliliter. These devices generally measure
in the micrometer range and are used in biotechnology labs to measure very small
quantities. Micropipettes require special tips that are placed on the end of the pipette
before liquid dispersal. The tips are usually sterilized prior to use and are disposed of
after one use.

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.

Figure 4. Precision and accuracy illustrated by a target

Apparatus and Instrument

¾ Triple beam balance


¾ Digital balance
¾ Measuring cylinder
¾ Burette
¾ Pipette

27
Chemical and Reagent

¾ Water
¾ Sodium chloride

Procedure

Measurement of a Solid Sample using triple beam balance


1. Using the triple beam balance, make sure that when the weighing pan is empty, the
scale is balanced. Remember to push all of the weights to the left at zero.
2. Weigh piece of steel shot. The steel shot may be placed directly on the weighing pan.
Record your data on the data sheet. Remember to record the mass in the correct
number.
3. Repeat the procedure with the lead shot and record your data on the data sheet in the
correct number of significant figures.
Weighing by differences - for solids
1. Set the balance to 0.0 g then place and weigh the emptied weigh boat (filter
paper) on the balance.
2. With a clean spatula, scoop some dry chemical from the bottle and carefully tip the
contents into the container.
3. Weigh and record quantity of the chemical and weigh boat together
4. The difference between the two masses will give the exact mass of the sample
successfully transferred into the beaker.

Weighing by differences - for liquids

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

1. Using a 100 mL beaker, measure out 50 mL of water.


2. Pour that 50 mL of water into the 100 mL graduated cylinder. Is the volume actually
50 mL? If not, what is the actual volume? Record this volume on your data sheet.
3. If there was less than 50 mL of water in the graduated cylinder, add more water until
there is exactly 50 mL. If there was more than 50 mL of water in the graduated cylinder,
pour out the excess water.
4. Pour the 50 mL of water from the graduated cylinder into the 50 mL volumetric flask.
Is the volume of water more or less than 50 mL? Why can’t you record an accurate
volume when there is more or less than 50 mL in the flask?
5. Pour the water back into the 100 mL beaker.
6. With a standard 10 mL pipette, transfer 10 mL of water from the 100 mL beaker to
a 50 mL beaker.
7. With a 10 mL volumetric pipette, remove the water from the 50 mL beaker. Was
there exactly 10 mL of water in the beaker? Was there too much water or not enough?
Why can’t you tell exactly how much water was present?
8. Put the water back into the 100 mL beaker.
9. With the micropipette, transfer 1 mL of water from the 100 mL beaker to the 50 mL
beaker. Use the following procedure:
I. Check the micropipette to make sure that the scale reads 1000. Your instructor will
demonstrate how to adjust the micropipette if it is not set at 1000.
II. Seat the tip firmly on the end of the micropipette. Do not touch the tip with your
hands.
III. Push the plunger down to the first stop. There are actually 3 stops on the
micropipette. The first stop draws up the required amount of fluid. The second stop will
blow out any bubbles that remain in the tip after dispensing the liquid. The third stop
pushes the tip off of the micropipette. Some micropipette's have a separate button for
tip removal.
IV. Once the plunger has been depressed to the first stop, hold the micropipette at the
stop, and put the tip of the micropipette into the water. Slowly let the plunger up until
it is completely back to its original starting point.
V. Remove the micropipette from the water.
VI. Put the micropipette tip into the 50 mL beaker, not touching the sides or bottom of
the beaker.

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.

Note: Before using a bunsen burner in an experiment, it is important to review the


proper techniques of lighting, adjusting, and safely using a bunsen burner.

Apparatus and Instrument

¾ Bunsen burner
¾ Tongs
¾ evaporating dish
¾ lighter

Chemical and Reagent

¾ Copper turnings (metallic Cu)

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

1. Why are chemical reactions often heated in the laboratory?


2. How can the temperature of a bunsen flame be adjusted?
3. Which flame is hotter: a blue flame or a yellow flame?
4.What is the dominant color of a nonluminous flame from a Bunsen burner? Explain.
5. Is the temperature of a luminous flame greater or less than that of a nonluminous
flame? Explain.

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:

Evidence What you might observe

production of a gas bubbles foaming odor


fizzing smoke

Color change (*not all color changes a different color appears


are chemical!!)

Formation of a precipitate cloudiness foggy solid at the


bottom of the container

change in heat or light energy temperature increases or


decreases

sparks explosion glowing

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.

Apparatus and Instrument

¾ Bunsen burner ¾ Test tubes


¾ Beakers ¾ Measuring cylinder
¾ Evaporating dishes ¾ Funnels
¾ Nichrome wire ¾ Spatula
¾ Tripod ¾ Filter paper and litmus paper

36
Chemical and Reagent

¾ Distilled Water
¾ NaCl
¾ Dilute HCl
¾ AgNO3
¾ Marble or limestone

Procedure

Dissolving sodium chloride in water


1. In a beaker dissolve one spatula full of NaCl in 10 mL of distilled water. Steps 2-4
are tests of NaCl. Carefully observe any changes that occur.
2. Test the solution with red and blue litmus paper.
3. Pours about 1 mL of the solution to the test tube and add a drop of AgNO3 solution.
(This is a test for a Cl- anion) Ag is a precious metal and its compounds can't be wasted.
Put the substances from the test tube to the special container provided by the instructor.
Silver can be recovered.
4. Heat a piece of nichrome wire in a non-luminous flame, cool it and after immersing
in the NaCl solution, introduce to the flame again. The color of the flame confirms the
presence of Na+
5. Transfer the solution to the evaporating dish, and heat it on a water bath until a
complete evaporation of water takes place.
6. Examine the residue by appearance.
7. After cooling the evaporating dish add 10 mL of water to dissolve the residue. Test
the solution obtained as in steps 2-4.

Dissolving marble (limestone) in dilute HCl

1. Take spatula full of limestone or a piece of marble and try to dissolve it in 10 mL of


distilled water. Label the sample in the vessel 'A'.
2. Take spatula full of limestone or a piece of marble and try to dissolve it in 10 mL of
dilute HCl. Label the sample in the vessel 'B'. Note your observations. Avoid dropping
hydrochloric acid to your clothes and skin.
3. Separately filter mixtures obtained in 1 and 2, collect filtrates in two evaporating
dishes and evaporate to dryness on a water bath. By the end of the evaporation, the

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):

    
 =
 

Figure 6. Gas Diffusion Apparatus

40
Material and Instrument

¾ Glass tube
¾ cotton
¾ stand
¾ lamps
¾ ruler
¾ cork or stopper
¾ beaker

Chemical and Reagent

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:

HIn (aq) ⇌ H+ (aq) + In‾ (aq) [6]

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.

Table 1. Some Common Acid-Base Indicators

Color

Indicator in acid in base pH range

thymol blue red yellow 1.2−2.8

bromophenol blue yellow bluish purple 3.0−4.6

methyl orange orange yellow 3.1−4.4

methyl red red yellow 4.2−6.3

chlorophenol blue yellow red 4.8−6.4

bromothymol blue yellow blue 6.0−7.6

cresol red yellow red 7.2−8.8

phenolphthalein colorless reddish pink 8.3−10.0

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.

Expression of titratable acidity:


1) Soxhlet Henkel degree (°SH): – the volume (mL) of 0.25 N NaOH used per 100 mL
of sample
2) Thorner degree (°Th): – the volume (mL) of 0.1N NaOH used per 100 mL of sample
3) Domic degree (°D): – the volume (mL) of 0.1N NaOH used per 100 mL of the sample

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.

Material and Instrument

¾ Burette
¾ Volumetric pipette
¾ Volumetric flasks
¾ Conical Erlenmeyer flasks
¾ Beakers
¾ Graduated cylinder
¾ Stand
¾ Funnel
¾ Balance

Chemical and Reagent

¾ Sodium hydroxide
¾ Phenolphthalein indicator
¾ Deionized water

46
PROCEDURE

1. Mix the milk sample thoroughly by avoiding incorporation of air.


2. Transfer 10 mL milk to the 150 mL conical flask or beaker.
3. Add 20 mL of distilled water (ambient water that has been just boiled).
4. Add 3-4 drops of phenolphthalein indicator and stir.
5. Rapidly titrate the contents with 0.1 M NaOH solution, continue to add alkali drop
by the drop and stirring the content till first definite change to faint pink color, which
lasts for 5 sec.
6. Note down the final burette reading: VNaOH = __________________
NNaOH = _______________________
7. Calculate Total Acidity using formula: TA = VNaOH * 10 (T0)

8. Calculate percentage of lactic acid:

 . . 
  %= ! "%


47
EXPERIMENT- 7: Determination of Solubility of Salts

Objective: To measure the solubility of a salt in water over a range of


temperatures and to construct a graph representing the salt solubility.

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.

Material and Instrument


¾ Goggles balance ¾ Stirring rod
¾ Aprons beaker ¾ Test tubes
¾ Graduated cylinder ¾ Marking pencil,
¾ Thermometer ¾ Test tube
¾ Micro spatula

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

Objective: To purify a contaminated liquid sample by 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).

Simple Distillation: A simple distillation apparatus is shown in Figure 7. This consists


of a round-bottomed flask connected by means of a distillation adapter to a water-
cooled condenser. A thermometer is held in place in the vertical arm of the distillation
adapter by a special rubber connector at a height adjusted so that the top of the
thermometer bulb is 5-10 mm below the opening of the side-arm. A (vacuum) adapter
is connected to the lower end of the condenser. The distilled liquid is collected in a
clean, dry receiver, commonly an Erlenmeyer flaks or small-mouthed bottle. To reduce
vapor losses and minimize fire hazards, it is desirable to insert the lower end of the
adapter well into the mouth of the receiver. A distilling assembly must have an opening
to the atmosphere to avoid developing a dangerously high pressure within the system
when heat is applied.

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

1: Heating mantle 2: Still pot 3: Still head 4: Thermometer 5: Condenser 6: Cooling


water in 7: Cooling water out 8: Vacuum adaptor 9: Receiving flask 10: Anti-bump
granules 11: Expansion place for inserting a fractionating column

Apparatus and Instrument

¾ Water bath
¾ Still pot
¾ Thermometer
¾ Condenser
¾ Receiving flask
¾ Vacuum adaptor

Chemical and Reagent

¾ Contaminated Ethyl alcohol

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.

POST LAB QUESTIONS

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

Objective: To Separate a mixture of two liquids by fractional distillation

Theory

Fractional distillation: Mixture of volatile liquids can be separated in to their


component parts by a technique known as fractional distillation. In this process volatile
liquids which boil within 25 oC of each other are separated in to components which are
called fractions. The separation is made possible by a fractionated column which is
attached to a distilling flask. The fractionating column may be packed with glass beads
or helices or even other solid pieces like ceramic, metal chips etc. The presence of these
materials in the column causes several tiny distillations to occur on the surface of
column packing.

In order to understand the principles underlying fractional distillation, we will briefly


review the relationship between vapor pressure and boiling point. If the solution of two
miscible components A and B obeys Raoult’s Law, the contribution that each
component makes at a given temperature to the total vapor pressure can be calculated:
Psolution = Xsolvent + Po solvent Where X is the mole fraction
When a mixture of two liquids is boiled the vapor normally contains a higher proportion
of the more volatile (lower boiling component) and the residue contains a higher
proportion of the less volatile component. The amount of each substance in the vapor
depends on the contribution each liquid is making to the total vapor pressure at the
boiling point of mixture. The vapour moves up wards, comes in contact with the
packing material in the fractionated column and partially condenses. The condensate is
richer in the more in less volatile as the vapour that continues to rise is richer in more
volatile liquid. A number of such equilibrations take place in the fractionation column,
resulting in the rise of vapour of the more volatile component while the liquid of the
less volatile component runs down the column.

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.

Apparatus and Instrument

¾ Water bath
¾ Still pot
¾ Thermometer
¾ Condenser
¾ Receiving flask
¾ Vacuum adaptor

Chemical and Reagent


¾ Contaminated ethanol

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

Objective: To introduce about way of isolating a substance from reaction mixture or


natural resources by extraction techniques

Theory

Extraction, as the term is used pharmaceutically, involves the separation of medicinally


active portions of plant or animal tissues from the inactive or inert components by using
selective solvents in standard extraction procedures. The products so obtained from
plants are relatively impure liquids, semisolids or powders intended only for oral or
external use. The isolation of pure compounds of a mixture requires the separation of
one component from another. Chemists have developed techniques for doing this. This
method takes advantages of the difference in physical properties of the components.
Some of the techniques are the following:
1. Sublimation: This involves heating a solid until it passes directly from the solid phase
into the gase phase. The reverse process, when the vapor goes back to the solid phase
without a liquid state in between, is called condensation or deposition. Some solids
which sublime are iodine caffeine, and paradichlorobenzene (mothballs)
2. Decantation: This separates a liquid from insoluble solid sediment by carefully
pouring the liquid from the solid without disturbing the solid.
3. Filtration: This separates a solid from liquid through the use of a porous material as
a filter. Paper, charcoal, or sand can serve as filter. This material allows the liquid to
pass through but not the solid or residue.
4. Evaporation: This is the process of heating a mixture in order to drive off, in the
form of vapor, a volatile liquid, so as to make the remaining component dry.

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.

Organic chemistry employs the following method for isolation or extraction of a


substance from a mixture: solid-liquid, liquid-liquid, and acid base extraction.
Separatory funnel liquid-liquid extraction continues liquid-liquid extraction, solid
phase extraction, soxhlet extraction, ultrasonic extraction and supercritical fluid
extraction.

Liquid-liquid extraction, also known as solvent extraction and partitioning, is a method


to separate compounds based on their relative solubility’s in two in different immiscible
liquids usually water and an organic solvent. It is an extraction of a substance from one
liquid phase in to another liquid phase. Liquid- liquid extraction is a basic technique in
chemical laboratories, where it is performed using a separatory funnel. This type of
process is commonly performed after a chemical reaction as part of the up. The organic
product will be soluble in an organic solvent (organic layer) while the inorganic
substance will be soluble in water (aqueous layer). The organic solvent used for
extraction must meet a few criteria:
1. Should readily dissolve substance to be extracted
2. Should not react with the substance to be extracted
3. Should not react with or miscible with water (the usual second solvent)
4. Should have a low boiling point so it can be removed from the product

59
Note: common extraction solvents are petroleum ether, diethyl ether, and methylene
chloride

Apparatus and Instrument

¾ Filtration set up
¾ Test tube
¾ Separatory funnel
¾ Beakers

Chemical and Reagent

¾ Benzoic acid
¾ Water
¾ Diethylether
¾ Drying agent

Procedures

1. Add 50 mg of benzoic acid following by addition of 10 mL of water and 10 mL of


diethyl ether to a test tube.
2. This is a sample solution for extraction. Place the solution to be extracted in
separatory funnel. Shake it well.
3. You should be able to see the two layers (organic and aqueous) clearly. You should
also have two beakers ready.
4. One labeled “organic layer” and the other labeled “aqueous layer”.
5. To remove all in organic substance from organic layer, shake the separatory funnel
again to increase the contact between these substances and the water.
6. At this point the two layers can be separated in to their respective beakers.
7. To be safe never throw out any removed layer until the desired product has been
isolated.
8. Once the extraction process is completed, add magnesium sulphated or other the
organic phase as drying agent and the product can be isolated from the organic
solvent by filtration.

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

Objective: To purify contaminated solid compound by recrystallization

Theory

Recrystallization of solids is a valuable technique to master because it is one of the


methods used most often for purification of solids. Other techniques for purifying solids
include sublimation, extraction and chromatography. Nevertheless, even when one of
these alternative methods of purification has been used, the solid material thus isolated
may still be recrystallized to achieve the highest possible state of purity. The process of
recrystallization involves dissolution of the solid in an appropriate solvent at an
elevated temperature and the subsequent re-formation of the crystals upon cooling, so
that any impurities remain in solution. This technique, called solution re crystallization,
is discussed here. An alternative approach involves melting the solid in the absence of
solvent and then allowing the crystals to re-form so that impurities are left in the melt.
This method is seldom used in the organic laboratory because the crystals often form
out of viscous oil that contains the impurities and from which it is difficult to separate
the desired pure solid. It is interesting to note, however, that this is the technique used
to prepare the high-purity single crystals of silicon used in computer chips.

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

Class of substance Efficient solvents

Hydrocarbons Pentane, hexane,


petroleum ether

Ethers Diethyl ether, chloroform

Amines, Esters, Ketones, Acetone, ethyl acetate


Aldehydes
Phenols, alcohols Acetone, ethyl acetate

Carboxylic acids, Sulphonic acids, ethanol, methanol, water


Organic salts

Apparatus and Instrument

¾ Erlenmayer flask
¾ Bunsun burner
¾ Measuring cylinder
¾ Spatula
¾ Filter paper
¾ Buchner funnel

Chemical and Reagent

¾ Acetanilide
¾ Benzoic acid

Procedures

1. Place 20 g of the impure sample in an Erlenmeyer flask.


2. Add about 20 mL of water and heat flask gently over wire gauze with Bunsen burner.
Allow the water to boil gently.

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.

#$& '* +#,-'  '+,# *#/ /#/03-',


% Recovered = ! "
#$& '* +#,-'  +#*'/# /#/03-',

65
POST- LAB QUESTIONS

1. Under what circumstances should one mixed solvents for recrystallization?


2. What is the advantage of using fluted filter paper?
3. Why is solution in the above experiment filtered while still hot?
4. After collecting the solid from suction filtration, why does one always break the
suction before turning off the water?
5. A solid (x) is soluble in water to the extent of 1 g per100 mL of water at the boiling
point. How would you purify x from the mixture of 10 g of x with 0.1 g of impurity
y, completely in soluble in water, and 1 g of impurity z, having the same solubility
characteristics in water as x? How much pure x could be obtained one
recrystallization from water?
6. What are the disadvantages of having excess solvent during recrystallization?
7. Why is minimum amount of cold solvent used for washing precipitates already
collected on a filter paper?

66
EXPERIMENT- 12: Colorimetric Determination of (Paracetamol)
Acetaminophen

Objective: To determine the amount of Acetaminophen in Plasma

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.

Paracetamol (acetaminophen) is one of the most widely used analgesics/antipyretics


worldwide. In patients presenting with paracetamol overdose, the current standard of
care is to undertake a risk assessment based on measurement of the plasma paracetamol
concentration and to compare this with a nomogram to establish the need for antidote
treatment with N-acetylcysteine (NAC). In some circumstances, such as the absence of
an assay service, risk assessment can be made on the history of the ingested dose;
however, this generally leads to overtreatment of many patients who are at low risk of
hepatotoxicity as there is a poor correlation between patients stated ingested dose of
paracetamol and paracetamol concentration. The incidence of paracetamol poisoning
gradually increased over 5 years (2004–2008) from 2.8 to 6.4% (95% CI = 2.3–4.9; p
< 0.001). Although pesticide poisoning remains more common, paracetamol is now the
most common drug in patients presenting with self-poisoning. Laboratory facilities to
determine plasma paracetamol concentrations are only available in a few private
laboratories. As paracetamol assays are not widely available, risk assessment in patients
presenting with paracetamol poisoning is based on the history of the dose ingested and
this results in a significant proportion of individuals having unnecessary treatment with
the antidote.

The plasma paracetamol concentration is also important in patients admitted with


paracetamol poisoning with an uncertain history and/or in individuals who have
congested agents that cause drowsiness. Recently a quick colorimetric method has been
described, based on a procedure for estimating the drug concentration. This involves

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.

Material and Instrument


¾ Pipette
¾ Beaker
¾ Uv-visible spectroscopy

Chemical and Reagent

¾ Trichloroacetic acid
¾ Sodium nitrite
¾ Sodium hydroxide
¾ Sulfamic acid
¾ Hydrochloric acid
¾ Paracetamol tablet
¾ Blood

Procedure

The colorimetric assay

1. 0.5 mL of plasma is pipetted into a 15 mL centrifuge tube containing 1.0 mL of 15%


trichloroacetic acid.
2. After vortex mixing, it is centrifuged briefly for 3 min and the clear supernatant is
decanted into a 10 mL test tube containing 0.5 mL 6 N hydrochloric acid.
3. Nitrous acid is generated by adding 0.4 mL of sodium nitrite to the resulted solution.
4. After allowing the contents to stand for 2 min, 1.0 mL of 15% sulfamic acid is added
carefully to neutralize excess nitrous acid.
5. Finally, 2.5 mL of 15% sodium hydroxide is added and the absorbance of each
sample is measured at 430 nm, against a reagent blank of water.
6. Use the calibration graph to determine the concentration of paracetamol in the
solution and use this to work out the mass of paracetamol in the tablet.

68
The validation experiment

A calibration curve is calculated using this method to measure standard paracetamol


concentrations (25, 50, 100, 150, 200, 250, 300, and 400 mg/L) using a UV-visible
spectrophotometer. The stability of the final colored solution is also assessed up to 10
min by measuring the absorbance (this was an end-point measurement rather than a
kinetic one).

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

Any chemical or physical change involves a


change in energy. Heat is a form of energy that
can be observed as a flow of energy. Heat can
pass spontaneously from an object at a high
temperature to an object at a lower temperature.
Two objects in contact at different temperatures,
given enough time, will eventually reach the
same temperature. The flow of heat energy can
also be either into or out of a system under study.

Heat released in a chemical reaction can be


determined experimentally by using an adiabatic
calorimeter. The reaction must proceed without
any side reactions and sufficiently fast that the
heat exchange with the surroundings is
negligible. In an oxygen bomb calorimeter, the
combustion reaction occurs in a closed container
under constant volume (“bomb”). The bomb is Figure 8. Adiabatic bomb
immersed in a weighed quantity of water and calorimeter
surrounded by an adiabatic shield that serves as a
heat insulator (see Figure 8).
The bomb and the water bath, which are in direct
thermal contact, constitute an adiabatic bomb
calorimeter. Continuous stirring ensures that heat
is distributed evenly in the system. In this
experiment an oil sample is combusted and its
heat of combustion is determined.

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.

Figure 9. Parts of the Parr 1341 oxygen bomb calorimeter

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

= -26.434 KJ/g / 4.184

= -6.318 Kcal/g

Knowing that J6EF = D6EF G ∆H6EF , then we can calculate the heat of combustion of
the assigned material.

Apparatus and Instrument

¾ Parr 1341 oxygen bomb calorimeter ¾ Firing mechanism


¾ Oxygen bomb ¾ Amperemeter/Ohmmeter
¾ Digital thermometer ¾ Balance
¾ Nickel-chromium fuse wire ¾ Iron ring and stand
¾ Oxygen cylinder

Chemical and Reagent

¾ Benzoic acid pellets


Procedure

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.

Determination of ∆ '+ of an oil sample:

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

Mass of benzoic acid = 1.00 g


Tinitial = _______0C
Tfinal = ________0C
∆T = ________0C
∆56789 (:;<>?@A BA@C) = -26.434 KJ/g
_________KJ/0C
D6EF = _________Kcal/0C

74
2. Determination of ∆Hcomb oil sample

Mass of oil sample = 1.00 g


MW of oil sample = 872.3 g/mol
N mol of oil sample = _____ mol
Tinitial = _______0C
Tfinal = ________0C
∆T = ________0C
Ccal = _________KJ/0C
∆Hcomb (oil sample) = - _________KJ/mol
- _________Kcal/mol

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

Bettelhim and Landsberg. Laboratory_experiments_for_General_Organic chemistry, 4th


edition.
Chemistry 2A Lab Manual Standard Operating Procedures. 2019. Department of
Chemistry, University of California.
Classic chemistry experiments. The effect of temperature on reaction rate.
David A. K. The solubility of a salt in water at various temperatures, 1995.
Fathima Shihana, Dhammika Dissanayake, Paul Dargan, and Andrew Dawson. 2010. A
modified low-cost colorimetric method for paracetamol (acetaminophen)
measurement in plasma. Clinical Toxicology, 48: 42–46
Laverman.L.E. Chemistry 116 Lab Manual Experiments in Analytical, Physical and
Inorganic Chemistry – 3rd Edition
Linne & Ringsrud, Clinical Laboratory Science. The Basics and Routine Techniques, 4th
ed., 1999.
Marina C. K. Indirect Gravimetric Determination of Waters of Hydration. Chem. Educator,
2009.
Mukhanbetova Nazira. 2019. Experimental laboratory manual on discipline analytical
chemistry chemical methods of analysis: Titrimetry and gravimetry.
Seinko, j., Robert, A., Plane, Stanley, T. Marcus Experimental chemistry, 6th edition.
Stephen, C. Simple and Fractional Distillation. 5th edition.
William B. J. The Origin of the Bunsen burner. Chem. Educ., 2005
Wollo University laboratory manual, 2016.

76
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