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Laboratory Manual (Inorganic and Organic Chem)
Laboratory Manual (Inorganic and Organic Chem)
Introduction ----------------------------------------------------------------------------------------------2
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Aspirin………………………………………………………..92
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Introduction
Chemistry is a branch of science that deals with the study of matter; its structure, physical and
chemical properties and the energy that is involved during its changes. Using the scientific
methods of solving problems in chemistry through experiments help the student understand how
structures and properties of matter are revealed.
Chemistry lab is a required component of most chemistry courses. Learning about lab
procedures and performing experiments helps you to learn techniques and reinforces textbook
concepts. This laboratory manual in chemistry is designed for students who are taking health
related courses. The objectives of each experiment highlight the basic concepts in chemistry.
Each activity is also followed by post lab questions that would help the students understand the
various concepts of matter.
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Laboratory Safety Guidelines
Any experiment, no matter how often it has been performed in the past, has the potential to fail
with hazardous results. By knowing the hazards, you will develop a healthy respect for what is
happening around you, and with this respect, heightened levels of observation are sure to follow.
This implies that potential accidents can be spotted before they can occur. The following sections
present some general guidelines for your safety while performing General chemistry
experiments.
General Reminders
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16. Never heat a piece of glassware that is chipped or cracked unless otherwise told to do so by
your lab instructor. Heating defective glassware can cause that glassware to break, resulting in a
spill.
17. Light the burner properly..
18. Never take more of a reagent than you need.
19. Never return an unused portion of a reagent to its original container.
20. Never pour a waste chemical in the drain or put it in the garbage, unless otherwise instructed
to do so by your lab instructor. Waste bottles will be provided. Always pour waste in the
appropriate and labeled waste bottle.
21. To insert glass tubes or thermometers through stoppers or adapters, first lubricate both the
glass and the stopper with glycerin or stopcock grease. Then, using a towel, cloth or other hand
protection, and holding the glass tube or thermometer near the end closer to the stopper, insert
the glass tube into the stopper, a few mm at a time, using a rotating motion.
18. When heating in a test tube, hold the test tube at about 45o angle. Be sure the opening of the
test tube is pointing away from anybody else. Never heat the bottom of the test tube instead heat
the middle of the test tube just at the level of the liquid in the test tube, Move the test tube
horizontally back and forth across the flame to prevent the liquid from heating too quickly.
Should the liquid begin to overheat, remove the test tube from the flame and allow the contents
to cool for a minute or so.
22. Never look down the opening of ANY container, including beakers, flasks, and test tubes. 23.
Do not use graduated cylinders for any purpose other than to measure a volume of a liquid 24.
Never put a dropper into a reagent bottle. Instead, put the reagent in a beaker so you can bring it
back to your desk and use a dropper there.
FIRE
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Reacting to Accidents: First Aid
Any serious accident involving poisoning or injury should be treated by a competent physician.
If you witness an accident, you should summon the instructor immediately and leave the first aid
to him or her unless (1) no instructor or assistant is in the laboratory areas; (2) the victim requires
immediate attention, (3) you have had formal training in emergency first-aid procedures.
1. Eye Injuries
If any chemical enters your eyes, they should be immediately be flooded with water from an
eyewash fountain, with the eyelids kept open. If foreign bodies such as glass particles are
propelled into an eye, the injured person should get immediate medical attention. Removal of
such particles is a job for a specialist.
2. Chemical Burns
The affected area should immediately be flushed with water, using a safety shower if the area of
injury is extensive or if it is inaccessible to washing from a tap. Neutralizing solutions,
ointments, or greases should not be used on chemical burns unless specifically called for in a
first-aid procedure. Unless the skin is merely reddened over a small area, a chemical burn should
be examined by a nurse or physician.
3.Thermal Burns
For small thermal burns such as those inflicted by handling hot glass, a sterile gauze pad should
be soaked in a baking soda solution (2 tablespoons of sodium bicarbonate to a quart of lukewarm
water, about 2.4% NaHCO3), placed over the burn, then bandaged loosely in place. If the skin is
not broken, the burned part can be immersed in clean, cold water, or ice can be applied to reduce
the pain. Blisters should not be opened. Unless the skin is merely reddened over a small area, the
burn should be examined by a nurse or physician.
5.Poisoning
If poison is swallowed, a physician or ambulance should be called immediately, and the victim
should be given 2-4 glasses of water or milk to drink. If it is safe to do so, vomiting should be
induced by placing a finger at the back of the victim’s throat or by having the victim drink a
glass of warm water in which 2 teaspoons of table salt have been dissolved (10 g in 200 mL).
Vomiting should not be induced if the patient is unconscious, in convulsions, or has severe pain
and burning sensations in the mouth or throat, or if the poison is a petroleum product or a strong
acid or alkali. When vomiting begins, the victim should be placed face down with head lower
than hips, and vomiting should continue to be induced until the vomitus is clear. When there is
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time, the poison should be identified and an appropriate antidote given. If the poison cannot be
identified and a physician is not present, a heaping table spoon (15 g) of the following universal
antidote can be given in a half glass of warm water; 2 parts activated charcoal, 1 part magnesium
oxide (milk of magnesia) and 1 part tannic acid. A sample of the poison should be saved for the
physician if possible. If the poison is a highly toxic gas such as hydrogen cyanide, hydrogen
sulfide, or phosgene, the persons attempting to rescue the victim should wear gas masks while
they are in contact with the vapors.
6. Chemical Hazards
For your own health and safety, it is essential that you exercise caution while handling chemicals
and minimize your exposure to them. Read the Material Safety Data Sheet for each chemical
reagent that you handle in the lab.
I, the undersigned student have received safety seminar, understood it and agree to abide by the
safety guidelines. I understand the importance of proper eye protection in the laboratory at all
times. I have been warned about the dangers of wearing contact lenses in the laboratory and
understand that I should not wear contacts in the laboratory. I also understand that if I do wear
contacts in the lab or fail to abide by the safety rules, I am doing so at my own risk and will not
hold St. Dominic College of Asia or the professor handling the course liable for any injuries that
result.
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Activity No. 1
Laboratory Techniques
I. Objectives
II. Introduction
Any student performing experiment in Chemistry should be able to acquire the basic
skills of handling hazardous chemicals and the proper technique of using laboratory
glasswares and equipment. Improper usage of equipment and chemicals would not only
lead to accidents but also poor experimental outputs.
III. Materials
IV. Procedures
A. Handling Solutions
Reagent solutions are usually kept in bottles in the laboratory. Unless the chemicals are
alkaline, the bottles are mostly glass-stopper. When pouring the contents from these
bottles, the stopper, if flat-topped is laid with its flat side on the table (Fig. 1).
To pour a liquid into another container, the liquid is guided by a glass rod held against the
lip of the first container, as shown in Fig. 2. This directs the flow of the liquid and
prevents it from spilling down the sides of other container.
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Often it becomes necessary to transfer a certain portion of the content of the bottle by the
use of pipette or a glass tube. In this case, let the tube or pipette fill by gravity or by the
use of a rubber bulb similar to that of a medicine dropper.
Solids or crystalline reagents should always be spooned out of the bottle with a clean dry
spatula, as in Fig. 3. A dirty spatula will not only contaminate the portion taken but also
that which is left in the bottle. Make sure that the covers of bottles of chemicals are not
interchanged. Use watch glass in weighing solid chemicals.
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B. TESTING FOR ODORS
1. Fold a circle of filter paper in half. Fold in half again and tear off one corner of
one folded edge.
2. Fit the opened filter cone in a funnel, placing the torn edge next to the glass.
Wet with distilled water and pressed the top edge of the paper against the
funnel, forming a seal.
Fig. 5
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Set-ups for filtration (Fig. 6)
Pouring a solution down a stirring rod (Fig. 7). A mixture is slowly poured down the
stirring rod into the funnel.
Note: Be careful not to overfill the paper filter cone.
Fig. 7
D. HEATING LIQUIDS
1. Heating in a Test Tube (Fig. 8). Performed when heating small amount of liquids.
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Fig. 8
2. Heating in a Flask or Beaker (Fig. 9). Performed when heating large amount of
liquids.
Evaporating dish
Fig. 9
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E. USE OF CRUCIBLE
Crucible with its lid (cover) is a porcelain container used to run reactions at rather high
temperature.
a. Place and support the crucible and cover on a clay triangle, and heat it in
the hottest flame possible. Note: The crucible must glow bright orange
to assure adequate heating.
b. Use the tongs to adjust or move the hot crucible and cover.
Place the covered crucible on a clay triangle, adjust the cover so that it is slightly
open, to allow the water vapor to escape and gently heat the crucible for about 5
minutes.
Fig. 10
F. MEASUREMENTS
1. Temperature
The simple act of measuring a temperature with a thermometer can easily involve
errors. When measuring the temperature of a liquid, one can minimize possible
error by observing the following procedures:
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b. Allow sufficient time for the thermometer to reach equilibrium with the
liquid.
c. Be sure the liquid is adequately mixed.
2. Mass or Weight
a. Never place chemicals directly on the weighing pan; first place them on a
weighing paper or in a container.
b. Clean up any materials spilled on or around the balance.
c. Before moving objects on and off the pan, be sure the balance is in the
“arrest” position.
d. When you leave the balance, return the balance to the “arrest” position
and the weights to the zero positions.
e. Never try to make adjustments on a balance.
f. If seems out of order, tell your instructor.
3. Volume
The volume should be read at the bottom of the meniscus and the eye level must
be horizontal to the surface of the liquid.
Fig. 11
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Activity No. 1
Laboratory Techniques
1. Why is it that in heating a liquid using a test tube, the flame should heat the top of the
liquid and not the bottom?
2. In reading a meniscus, why is it that the eye level should be horizontal to the surface of
the liquid, not too high or not too low?
I. Objectives
II. Introduction
Electrons in an atom occupy different energy levels. The electrons in an atom occupy different
energy levels, as you know. When all of the electrons are at the lowest possible energy level they
are said to be in the ground state. Electrons do not always stay in the ground state. Sometimes
they can be promoted to a higher-energy electron shell. This can happen in two ways. First, the
electron can absorb a photon of just the right amount of energy to move it from one quantum
shell to another. Second, when atoms are heated or energized with electricity their electrons can
gain energy. This promotes them to the higher-energy shell. When an electron is in a higher
energy shell it is said to be in an excited state.
Electrons in excited states do not usually stay in them for very long. When electrons lose their
energy they do so by emitting a photon of light. Photons are particles with energy but no mass.
Their energy is directly proportional to the frequency of the light (remember: E = hν). The
photons emitted precisely match the quantum energy difference between the excited state and the
ground state. The light produced by very hot atoms in the gaseous state is a unique spectrum for
each element. To observe the spectrum requires the use of a prism, diffraction grating, or
spectroscope. This ability of metal atoms to produce these colors is put to use by practitioners of
the art of fireworks manufacture. By including different metal salts, or mixtures of metal salts, in
the exploding shell of a firework, these artists can produce beautiful displays in nearly all the
colors of the rainbow.
In this experiment, we are going to observe a unique single color of metals using flame tests. It
is a traditional art of the chemistry laboratory to use these colors to identify specimens of
compounds that contain unknown metals.
III. Materials/Reagents
Safety
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• Wear goggles or risk sitting out the lab
• Treat all chemicals in this lab as toxic. Do
not touch any of them with your bare hands. •
Wash well with water immediately if you touch chemicals accidentally • Use caution with
the burner
o Do not leave burner unattended
o Place burner near middle of lab bench
o Tie back long hair
o Do not wear baggy clothing in the lab
o Hot objects look like cold objects: be cautious!
• CuCl2 (Copper(II) Chloride) is highly toxic by ingestion; avoid contact with eyes, skin
and mucus membranes.
• LiCl (Lithium Chloride) is moderately toxic by ingestion; avoid contact with eyes, skin
and mucus membranes.
• Wash your hands with soap and water after you complete the day’s lab work, even if you
didn’t touch any chemicals directly
IV. Procedure
1. Clean the inoculation loop using distilled water (3 x) and heat each time you change from one
metal salt to another. Failing to do so will result in mixed flame test colors. Again, do not over
heat the loop.
2. Obtain 8 test tubes and label them properly with the name of the salt solutions as indicated in
the laboratory sheet.
3. Place 20 drops of solution and do the flame test.
4. To do a flame test with each metal salt get a film of the solution of a salt inside the loop and
bring it into the hottest part of the flame. If this produces poor color then try the edge of the
burner flame. Repeat the dip into the salt solution as often as necessary to see the flame test
color. Be sure not to over-heat the loop.
5. Carefully note the color of each metal salt when it is put in the flame. Use the chart below to
estimate the approximate wavelength of the color you see.
6. Use the representative wavelength value to determine the energy emitted per mole of electron
that is excited.
7. Clean out the test tube using the method recommended by your instructor (hazardous wastes
must be disposed of properly). Usually, all leftover solutions will be collected in designated
waste containers for hazardous waste disposal.
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Activity No. 2
Flame Tests
Flame Tests
Test Reagent Observation Wavelength (nm) Energy (kJ/mole e-)
CaCl2
LiCl
CuCl2
NaCl
KCl
SrCl2
Unknown 1
Unknown 2
V. Questions
3. Why do the chemicals have to be heated in the flame before the colored light is emitted?
4. Could flame tests be useful in determining identities of metals in a mixture of two or more
salts? Explain your answer.
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Activity No. 3
Chemical Nomenclature
I. Objectives
II. Introduction
In this exercise you will practice naming and writing chemical formulas for many inorganic
compounds, both ionic and molecular. Before beginning the exercise you should carefully read
all the sections of your text (or notes) on the names and formulas of ionic compounds, simple
covalent compounds, and acids. The following is a brief summary of the Nomenclature rules for
each of these types of compounds.
A. Oxidation Number or Oxidation State - the charge that an atom has or appears to have
when certain arbitrary rules are applied; oxidation numbers are useful in identifying atoms that
are oxidized (loss of electrons) or reduced (gain of electrons).
Rules:
Steps to find the oxidation number for an element within a compound: 1. Write the
oxidation number of each known atom below the atom in the formula. 2. Multiply each
oxidation number by the number of atoms of that element in the compound. 3. Write an
equation indicating the sum of all the oxidation numbers in the compound or ion.
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= 0 S = +6
CO2
B. Ionic Compounds Cr2O72-
Step 1 -2 Step 2 2(-2) -2
Na2SO4
Step 3 C + (-4) = 0
+1 -2 2 (Cr) + 7 (O) = -2
C = +4 2 (Cr) + 7 (-2) =
2 (Na) + S + 4 (O) =
0 2 (+1) + S + 4 (-2) -2 Cr = +6
Examples:
Na+ + F- ------> NaF sum of oxidation numbers: +1 + -1=0
Ca2+ + F- --------> CaF sum of oxidation numbers: +2 + -1 = -1, not the correct formula
Ca2+ + 2F- -----> CaF2 sum of oxidation numbers: +2 + -1 x 2= 0
Na+ + SO42- ----> Na2SO4
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a. Metal with Fixed Oxidation State (e.g. IA, IIA, IIIA)- Name the metal and change the
ending of the non-metal to –ide (e.g. NaCl = sodium chloride)
b. Metal with Varying Oxidation State – Determine the oxidation state of cation. Common
Name – Use –ous for lower oxidation state and –ic for higher oxidation state (e.g. Fe2+ = Ferrous;
Fe3+ = Ferric)
FeCl3 is named Ferric chloride
Stock System – Use Roman numeral to indicate oxidation number (e.g. Au +1 = Gold (I); Au 3+ =
Gold (III)
AuCl3 is named Gold (III) chloride
c. Exceptions that Use -ide Endings: Hydroxides (OH-); Cyanide (CN-); Ammonium
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4. Names of Selected Anions
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C. Simple Covalent (Molecular) Compounds
• Composed of non-metal atoms only.
• The more metallic non-metal is written first.
• Prefixes are used in the name to indicate the number of each atom present. A list of
prefixes is provided below, which must be memorized.
• The prefix “mono” is dropped if there is only one of the first element.
• The name of the second element always ends in __ide.
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D. Naming Acids
E. Naming Hydrates
-Hydrates are solid substances that also contain water molecules in their crystal
structure. -The number of water molecules for each formula unit is fixed.
- The formula is written the same as any other compound, but then we add a dot (.), (Note that
this is NOT a multiplication sign) followed by the number of water molecules per ionic formula
unit and the symbol H2O.
The name is the same as for any other compound, but we add the word “hydrate” at the end with
a Latin prefix to indicate the number of water molecules per ionic formula unit.
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Activity No.3
Chemical Nomenclature
A. Write the formulas of the following compounds presented in the table below.
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B. Name each of the compounds in the following table. Compounds marked with a star (*)
should be named using both the Stock and the “ic/ous” naming systems.
C. Formulas and Names
If the name of the compound is given, write its formula. If the formula is given, write its
name. You may use either the Stock system or “ic/ous” system for naming, if necessary
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Activity No. 4
Lewis Structures and Molecular Modeling
I. Objectives
II. Introduction
Chemists have been using molecular models of one kind or another for more than a century.
Building representations of molecules in three dimensions helps to illuminate both the structure
and function of a compound. With the advent of computers, molecular modeling has become an
even more important tool for both chemists and biochemists. Biological compounds can be
modeled on the computer along with pharmaceutical candidates to study potential interactions
between the molecules. Applications such as these illustrate why this powerful tool has now
become ubiquitous in science.
A Lewis structure is a model used to show the bonding in covalent compounds. In this system,
molecular structures are diagrammed by using a line to represent a bonding pair of electrons, and
a pair of dots to represent lone pairs. The bonding rules can be summarized by the following
basic rules, which have few exceptions:
-Carbon almost always forms 4 bonds
-Hydrogen forms only 1 bond
-Halogens form 1 bond
-Oxygen almost always forms 2 bonds
-Nitrogen almost always forms 3 bonds
In this experiment, you will be trained to construct molecular models using Balls and Sticks and
Hyperchem Software. The software can be downloaded from the internet.
How to Use the Hyperchem
1. Be familiar with the important features of the software.
2. To build a molecule from scratch, begin by double clicking on the draw key. This will open up
a periodic chart for you.
3. Select carbon C and place a carbon somewhere in the black area. Notice that you might have
to click twice to get the carbon to show (it will appear as a small blue circle); this is because
when you click on the periodic chart, that becomes the active window. The first time you click
on the black background, it makes the Hyper Chem window the active screen so the second click
is required to place the carbon.
4. To attach a second carbon to our first, begin by clicking on the carbon already there, and drag
a line a little ways to represent the bond. You will find that the circle disappears, and all that
remains is the line. This is OK; the default rendering (that is , how the program displays
molecules) is a short-hand “stick” form. This line represents the single line between the two
carbons, with a carbon on each end. If the line does not draw the first time, try it again (again, if
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the Hyper Chem window is not the active display, the first time you click on it all it does is
activate the window).
5. If you want to connect another carbon, simply click on one end of the line, and draw another
line.
6. If you want to draw 2-propanone for example, all you have to do is to select Oxygen (O) from
the periodic table (click draw twice) and then point the cursur to the middle carbon and draw a
line to represent oxygen. Notice again that we will only get a line,but this time, the line is blue
on one side (whether the carbon is) and red on the other (to represent oxygen on the other side).
7. If you accidentally clicked on the middle carbon twice, you will notice that it changed from
blue to red. Hyper Chem assumed you wanted to change the identity of that atom (which you did
not). No problem just choose Carbon in the periodic chart and double click the red bend to turn it
back to blue; then click on Oxygen, click and drag the line from the middle carbon to put the
oxygen on just as before.
8. To generate a double bond on oxygen, just click in the middle of the line between the carbon
and the oxygen. You will see it changes from a single line to two lines, to represent a double
bond.
9. To show the number of hydrogens, close the periodic chart and under “Build” choose “Add H
and Model Build”. This feature automatically completes your molecule by adding hydrogen to
any “open valences” (that is location where it is expecting another bond but there is not one) and
selecting the best bond lengths and angles for all of the atoms in the molecule.
10. If you want to change the feature, simply go to “Display” and choose “rendering” and click
on “balls and cylinders” which will make the molecules like balls.
11. To do theoretical calculations for energy, Click on molecular dynamics or MD. Molecular
dynamics simulates the motions of molecules by taking into account attraction and repulsion of
every atom in the system with every other atom. To run MD simulations on 2-propanone begin
by going to “set-up” and choosing “molecular dynamics”. Once in there, select one of the
options, AMBER. There are two basic ways to run MD calculations, “ In Vacuo” or in water. If
you want to add water, under “set-up” choose “periodic box”.
12. To run the calculation, go to “Compute” and “Molecular Dynamics”. Hyper Chem will
remember your choices from the previous step. For example, my MD will run using the AMBER
force field. You will notice there are more choices here such as step size and time of simulation.
Typically, the smaller the step size and the longer the run the more accurate the results, but the
slower it will be. For our purpose, I recommend simply choosing the results. You will see the
2-propanone begins to dance on your screen; this is a simulation of how the molecule can be
expected to actually move if we could see it in reality.
13. To display the results, go to “Compute” and you will see several options that were not
available before (such as properties). Feel free to take a look at what is in this.
III. Materials
Ball and Stick Models Glue Pair of Scissors Pencil Computer BBQ sticks
Ruler
Hyperchem Software Cartolina Protractor
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IV. Procedures
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F. Ball and Stick Model
1. Using the ball and stick model construct the following compounds below. Provide important
information such as hybridization of central atoms, bond angles, and bond lengths.
Compound Central Atom Bond Angle Bond Length Hybridization
of Central
Atom
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Activity No. 4
Lewis Structures and Molecular Modeling
V. Questions
1. Draw the Lewis Structures of the following compounds and provide the following
information:
a. Hybridization of the central atom
b. Bond angle
2. Explain why C-C and C=C bond lengths in Benzene have the same values.
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Activity No. 5
Limiting Reactant and Percentage Yield
I. Objectives
1. To observe the reaction between solutions of sodium carbonate and calcium
chloride.
2. To determine which of the reactants is the limiting reactant and which is the excess
reactant.
3. To determine the theoretical mass of precipitate that should form.
4. To compare the actual mass with the theoretical mass of precipitate and calculate
the percent yield.
II. Introduction
In this experiment, you will react a known amount of sodium carbonate solution
with a known amount of calcium chloride solution. The skeletal (unbalanced) equation
for the resulting double replacement reaction is:
Note that three of the chemicals have their states or phases designated as (aq) and
one is designated as (s). The (aq) represents the term aqueous which means that the
substance is soluble and dissolved in water. The (s) means that the substance is a solid (in
this case, it is a precipitate). Precipitate formation is easily observed as the mixed
solutions turn cloudy and, if desired, the precipitate can be easily separated from the
solution by filtering. Since your precipitate will be separated and weighed, you will need
to dry the precipitate in a drying oven before measuring its mass. Stoichiometry will then
be used to determine the amount of precipitate that should be formed in the reaction.
It is often difficult as well as impractical to combine just the right amount of each
reactant that is required for a particular reactant that is required for a particular reaction to
occur. Given this fact, this experiment is designed so that only one of the reactants will be
completely used up. This is called the limiting reactant because it limits the amount of
products formed. Since the other reactant will have a quantity remaining, it is called the
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excess reactant. One of your tasks will be to determine which of your reactants is limiting
and which is in excess.
III. Materials
Balance Drying Oven
(2) 25-mL graduated cylinders (3) 250-mL beakers
wash bottle Filtering apparatus (ring with stand, funnel)
Filter paper 0.70 M sodium carbonate solution, Na2CO3
0.50 M calcium chloride solution, CaCl2
IV. Procedures
1. Obtain two clean, dry 25mL graduated cylinders and two clean, dry 250mL
beakers. 2. In one of the graduated cylinders, measure 25mL of the Na 2CO3 solution.
3. In the other graduated cylinder, measure 25mL of the CaCl 2 solution.
4. Record these volumes.
5. Pour the contents of both graduated cylinders into one of the 250mL beakers and observe the results.
6. Record these qualitative observations.
7. Allow the contents of the beaker to sit undisturbed for 5 min. to see what happens to the suspended
solid particles. Meanwhile, proceed to step 8.
8. Obtain a piece of filter paper. Weigh and record the mass of the filter paper, then use it to set up a
filtering apparatus.
9. Use the wash bottle to lightly wet the filter paper in the funnel to keep the filter paper in place. 10.
Swirl the beaker and its contents to suspend the precipitate in the solution, and then pour it carefully
and slowly into the filter funnel. Use the wash bottle to rinse the remaining precipitate from the beaker.
11. Use the wash bottle one last time to rinse the precipitate in the filter paper. This will remove any
residual NaCl(aq) that remains with the precipitate.
12. After the filtering is complete, remove the wet filter paper containing CaCO 3 precipitate and suspend
it carefully in the third 250mL beaker.
13. Put your labeled beaker with filter paper + precipitate in the drying oven for 30-45 min. 14.
Remove the beaker with filter paper + precipitate from the drying oven and allow cooling for a few
minutes.
15. Weigh and record the mass of the dry filter paper containing the CaCO3 precipitate. 16. Using the
data collected, calculate the moles of each of the chemicals that are added together to react. 17.
Determine which chemical is the limiting reactant.
18. Calculate the percent yield of that particular chemical by using this formula:
Moles of Na2CO3
Moles of CaCl2
Limiting Reactant
Percent Yield
Computation:
V. Questions:
1. If you were to evaporate the filtered solution to dryness, would you be left with only solid
NaCl? Explain.
2. What theoretical volume of the Na2CO3 solution used in this experiment would result in no
excess reactant?
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Activity No. 6
Solutions and Colloids
I. Objectives
1. To examine the influence of solvent and solute on solution formation
2. To prepare a solution for use in a later experiment
3. To make a colloid and demonstrate its properties
II. Introduction
Two liquids that are completely soluble in each other are called miscible. When a
liquid solute doesn't dissolve in a liquid solvent, but instead forms a separate layer,
the liquids are said to be immiscible.
In Part I of this experiment, you will test the solubility of a series of compounds
in two solvents, one polar and one nonpolar.
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Molarity = M = moles of solute
liter of solution
In order to make a solution of a given molarity, you can weigh out a calculated
amount of solute and dissolve it in enough solvent to make the desired volume of
solution.
In Part III, you will compare a solution and a colloid, using the Tyndall effect to
test for the presence of the colloid.
III. Materials/Reagents
Chemicals
methanol NaCl table sugar oil
MgSO4 solid NaOH distilled water Na2S2O3
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IV. Procedures
Part I. Influence of solute and solvent on solubility
A. Polar solvent
1. Place 8-10 drops of water in each of 9 test tubes
2. Add the following solutes and test for solubility: methanol, NaCl, table
sugar, oil, MgSO4. (For solids, add a few crystals. For liquids, add 8-10
drops)
3. Shake to mix and record your observations.
B. Non-polar solvent
1. Repeat the experiment, using 8-10 drops of oil in each test tube instead of
water.
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Activity No. 6
Solutions and Colloids
Methanol
NaCl
table sugar
Oil
MgSO4
Part II
V. Questions:
2. Define the following concentration terms, and give their units: percent by mass, mole fraction,
molarity, and molality.
3.Why is there no colloid in which both the dispersed phase and the dispersing medium is gas?
41
Activity No.7
Acids, Bases, and Salts
I. Objectives
II. Introduction
In this experiment, we are going to assess the conductivity of different substances. Substances
that are capable of conducting an electric current iin solution are known as electrolytes; those
that do not are known non electrolytes. Among electrolytes, the ability to conduct varies greatly.
Some substances are excellent conductors, while others conduct only slightly.
III. Materials/Reagents
IV. Procedure
42
B.1. Conductivity Test
1. Prepare nine (10) 50- mL beakers and label them with the following reagents: NaCl,
CH3COOH, NaOH, Urea, NH4Cl, HCl, NH4OH, Sucrose, Water, and Ethanol 2. Place 20 mL of
the solution and determine the conductity using the conductivity apparatus. 3. Note the relative
intensity of light and record your observation, as nonconductor, weak conductor, moderate
conductor, and strong conductor.
NaCl
CH3COOH
NaOH
NH4OH
HCl
NH4Cl
B.1.Conductivity Test
Reagents Conductivity Classification(strong/we
ak electrolytes
Water
Urea
Ethanol
NaCl
NH4Cl
NaOH
HCl
NH4OH
Sucrose
CH3COOH
0.0001 M CH3COOH
0.001 M CH3COOH
0.01 M CH3COOH
0.1 M CH3COOH
44
V. Questions.
What conclusion can you draw from the results in B.2. Conductivity Test?
45
Activity No. 8
Classifications of Chemical Reactions
I. Objectives
Matter undergoes three kinds of change: physical, chemical, and nuclear. While the composition
of a chemical substance is not altered by physical changes (such as freezing and evaporation),
chemical changes, or reactions, result in the formation of new substances when bonds are formed
and/or broken. Indicators of chemical reactions include change in color,
evolution of gas, change in temperature and formation of precipitate. Some relatively simple but
common types of chemical reactions are illustrated in this experiment. Examples and
descriptions of each reaction type appear in the following section.
Chemical reactions can be classified as Combination reaction, Decomposition reaction, Single
displacement reaction and Double decomposition reaction. Combination reaction occurs when
two or more substances, elements or compounds, combine to form one new substance.
Decomposition reaction occurs when a compound breaks apart to yield two or more new
substances. In single displacement reaction, one element in a compound is displaced by another
element. This process will only occur if the element that is being displaced is less reactive than
the other element. Double Displacement or Metathesis Reactions occur when two compounds
that form ions in solution react by switching ion partners. One of three conditions must be met
for these reactions to occur: (1) the formation of an insoluble ionic compound, observed as a
precipitate,(2) the formation of a gas, or (3) the production of water from hydroxide and
hydrogen ions (an example of an acid-base neutralization). In each case one of the products
results by combining two ions that are removed from the solution by the reaction.
III. Materials/Reagents
Solids: Al, CuSO 4•5H2O, Ca, Cu, Zn, NaHCO3, CaO, (NH4)2CO3
Solutions: 6M HCl, 3 M HCl, 3 M NaOH, 6M NaOH, and 0.1M solutions of CuSO4, ZnSO4,
AgNO3, NaCl, Ni(NO3)2, Pb(NO3)2 and K2CrO4, 0.1 M CuCl2, 0.1 M Fe(NO3)3, 0.1 M Ni(NO3)2,
0.1 M Pb(NO3)2
Crucible tongs 5 mL test tubes (10)
Test tube holder test tube rack
100 mL beaker (3) Litmus paper
Bunsen burner Stirring rod
stirring rod
46
IV. Procedures
Safety
1 Be especially cautious with the 6 M and 3 M acid solutions as they can burn your
skin. 2 Do not stare directly at the magnesium when it burns as the light can hurt your
eyes. 3 Skin discoloration will result from contact with silver nitrate.
4 Do not touch metals with your hands.
Perform each of the following reactions except those that are to be demonstrated by your
instructor. Use 12-15 drops of the solution in many of the reactions. Record your observations on
the data page as you complete each reaction. Make sure that you observe the results of every
reaction even if you didn’t actually mix the chemicals yourself. Then write a balanced equation
for each reaction. Be sure to include the states of all compounds in your equations (solid, liquid,
aqueous, or gas). If no reaction occurs write the words "no reaction" (or NR) instead of the
products in your balanced equation. Do not put metal strips in the sink.
A. Combination Reaction
A.1. Instructor Demonstration. Pour about 35 mL of a clear saturated solution containing
calcium oxide into a 100 mL beaker. Allow the solution to stand for about 15 minutes.
Observe. Use a straw to blow bubbles into the solution for a few seconds. Observe the solution
again.
B. Decomposition Reaction
B.1 Decomposition of Ammonium Carbonate
1. Place 0.5 g ammonium carbonate into a clean, dry test tube (100 x 13
mm). 2. Gently heat the test tube in the flame of a Bunsen burner.
3. As you heat, hold a piece of wet red litmus paper at the mouth of the test tube. What happens
to the solid? Are there gases produced? What happens to the color of the litmus paper? Record
your observation and complete a balanced equation if you see that a reaction has occurred.
1. Place a small amount (an amount that will fit on the end of a spatula) of solid copper(II)
sulfate pentahydrate in a medium test tube.
47
2. Use a test tube holder to hold the tube at about a 45º angle and heat in a burner flame for a
few minutes, remembering not to point the tube at anyone in the room.
3. Note any changes in the appearance of the solid and anything else that appears in the test
tube.
4. Allow the solid to cool and add a few drops of water. Observe. Dispose of the copper
compound in the waste container.
1. Place 8 clean test tubes (10 mL size) in a test tube rack and number or position-code them. 2.
Place 1 ml (approximately 20 drops) of the following solution and add the following small pieces
of metals as outlined in the table below.
Test Tube No. Solution Metal
1 H2O Ca
2 H2O Zn
3 6 M HCl Cu
4 6 M HCl Zn
5 0.1 M CuSO4 Zn
6 0.1 M ZnSO4 Cu
7 0.1 M AgNO 3 Cu
8 0.1 M CuCl2 Al
48
D. Double Displacement Reaction
1. Each part of this experiment consists of mixing equal volumes of 2 solutions in a test
tube. 2. Use about 10 drops of each solution as outlined in the table below.
Test Tube No. Solution no. 1 Solution no. 2
4 3 M NaOH 3 M HCl
A. Combination Reaction
Reactants Observation Reaction Equation
Aluminum and O2
B. Decomposition Reaction
Reactants Observation Reaction Equation
Ammonium carbonate
Arrange copper, silver, calcium, zinc, and hydrogen in an activity series from most active to least
active on the basis of the results from the displacement reactions that you performed. Recall that
a more active metal displaces a less active metal, a more active metal to is needed to displace
50
hydrogen from water than to displace it from an acid, and that a metal that displaces hydrogen
from acid is ranked as more active than hydrogen.
Most active (most easily oxidized): _____>______>______>_______>______ Least Active
NaCl + KNO3
NaCl + AgNO 3
Na2CO3 + HCl
NaOH + HCl
Fe(NO3)3 + NaOH
Ni(NO3)2 + NaOH
Pb(NO3)2 + K2CrO4
V. Questions
1. Why must a chemical equation be balanced? What law is applied in the balanced chemical
equation?
2. The following reactions are performed , and the results are shown below. Use these results to
determine the relative activities of the two elements involved in each reaction next to that
reaction. Then place the elements gold, hydrogen, zinc and tin in an activity series in order of
decreasing activity.
51
Activity No. 9
Chemical Equilibrium
I. Objectives
II. Introduction
Chemical reactions are processes in which one of more substances change into new
substances. When all of the reactants and products of a given chemical reaction system are
present in some amount and in contact with each other at the same time, and the reaction is not
producing or using up any of them, the reaction is said to be in equilibrium.
The equation for a reaction that reaches equilibrium instead of going to completion is written
using two arrows instead of one, with one arrow representing the forward direction and the
other the reverse direction:
When the reactants are first mixed together, they begin producing products right away and
with a particular reaction rate. The rate of the reaction, or amount of product produced per
second, generally depends on a number of factors including the concentrations of the reactants
Once a reaction reaches equilibrium, the system will remain at equilibrium unless something
from the outside influences it. This addition of outside influences is called a stress, because it
exerts a kind of “force” on the equilibrium.
Another factor that affects the position of equilibrium for a chemical reaction system is the
energy (most commonly heat) produced or absorbed by a reaction. If a reaction is exothermic,
it produces heat in the forward direction, so if the temperature of the equilibrium system goes
up, the stress put on the equilibrium will push it back toward the reactants. If a reaction is
endothermic, it absorbs heat in the forward direction, so raising the temperature of the system
will push the position of equilibrium toward the products.
In this experiment you will prepare a number of chemical reaction systems, observe them at
equilibrium, subject the system to a stress, and observe the shift of the system in response to
that stress.
52
II. Materials
III. Procedure
Part I. The Effect of Temperature on Equilibrium
1. Set up a hot plate with a 250mL beaker on it.
2. Add about 150mL of water to the beaker.
3. Allow the water to boil.
4. Use a 400mL beaker to obtain about 300mL of ice.
5. Add enough water to this ice just to bring the water level up to the top of the ice, but
without making the ice float.
6. Label three small test tubes as follows:
a. Aqueous cobalt(II) + chloride at room temperature
b. Aqueous cobalt(II) + chloride at 0.0 °C
c. Aqueous cobalt(II) + chloride at 100.0 °C
7. Put about 2mL of Cobalt (II) chloride solution to each test tube.
8. Add 25 drops of 12M HCl to each of the three test tubes.
9. Observe the color of the solutions and record these observations.
10. Keep test tube A in the test tube rack. Place test tube B in the ice water, and place test
tube C in the boiling water.
11. Observe and record any changes.
53
Activity No. 9
Chemical Equilibrium
V. Questions:
2. List four factors that can shift the position of equilibrium. Only one of these factors can
alter the value of the equilibrium constant. Which one is it?
54
Activity No. 10
Acid –Base Titration
I. Objectives
II. Introduction
Acid-base titrations can provide valuable information about the nature and properties of an acid
or a base. These titrations can be useful not only in determining the molecular mass and pKa
values, but also whether the substance is polyfunctional. Polyfunctional acids and bases have two
or more acidic or basic functional groups; i.e., they may donate or accept more than one proton.
Vinegar is a substance whose acidity varies quite a bit because it can have from 4 to 6 % of
acetic acid. The manufacturers of vinegar, and also of other substances, often need to precisely
determine the acidity of their products. To titrate a vinegar means to determine its acetic acid
content.
In water, the sodium hydroxide dissociates as follows: NaOH Na+ + OH-. The OH- ions
combine with as many H+ ions if they are available. Essentially, to titrate vinegar you have to
add a solution of sodium hydroxide having a concentration known with precision to the
sample to be titrated, until you neutralize all the excess H+ ions produced by the acetic acid. To
know when the sample is neutralized, some drops of a suitable indicator are added to it. In this
way, when the sample is neutralized suddenly it will change color. At this point, the number of
moles of NaOH present in the titrant solution you have used will correspond exactly to the
number of moles of the acetic acid present in the sample of vinegar to be titrated.
III. Materials
Erlenmeyer flask. 2. Dilute with
Dropping pipette about 50mL of distilled water. 3.
Burette Add 3 drops of phenolphthalein.
Erlenmeyer flask Chemicals
Iron stand Vinegar
Iron clamp 0.1M NaOH Phenolphthalein
IV. Procedure
Computation:
V. Question:
2. What is the difference between the term equivalent point and end point?
57
Activitity No. 11
Boiling Point and Melting Point Determination
I. Objectives
1. To be familiar with the principles of melting point and boiling point determinations. 2. To
master the method of determination of melting point and boiling point using capillary tube. 3. To
determine the melting point and boiling point of organic solids and liquids.
II. Introduction
The determination of physical properties of organic compounds such as boiling points, melting
points, density, solubility, refractive index, etc. is important for characterizing and identifying
organic compounds. In this experiment you will be learning the techniques for measuring the
melting point of a solid and the boiling point of a liquid.
Boiling point is formally defined as the temperature at which the vapor pressure of the liquid
becomes equal to the pressure at the surface of the liquid. The boiling point of a liquid can
change if the pressure at the liquid's surface changes. Since pure substances have a distinct
boiling point, boiling points are sometimes used to determine the purity of substances.
A solid is said to melt sharply if the melting point range is 0.5 - 1.0 oC (narrow melting point
range). A pure solid will generally melt sharply because the forces of attraction between its
particles are the same. However, the presence of a foreign particle in a crystal lattice interrupts its
uniform structure and the forces of attraction are weakened. An impure solid melts at a lower
temperature and over a wider range. Thus, a solid's melting point is useful not only as an aid in
identification but also as an indication of purity.
(1) Iron Ring, Iron Stand, Wire Gauze 0.5 mL Acetic Acid
Put one end of a prepared capillary tube to the edge of a small hot flame and rotate the capillary
tube slowly so that the end is sealed. To ensure the capillary tube sealed compactly and smoothly,
you should operate it carefully and not make it bended or into a small ball.
Place a small sample of the solid pulverized finely on a clean watch glass, then collect the solid
into a small mound and push the open end of the capillary tube down into the sample. The solid
may be forced down by dropping the tube (sealed end downward) through a long length of
ordinary glass tubing onto the desktop. Further increments of the sample are introduced in the
same way until the material forms a compact column 3-5 mm high at the bottom of the tube after
repeated dropping. It is essential that the material be packed firmly and densely into the end of
the tube.
Follow the method above; fill three tubes with benzoic acid, urea, and mixtures of unknown
sample.
3. Arranging assembly.
Introduce oil bath liquid into a 50-mL beaker and keep the bath level at the position of the two
third of the beaker. The capillary tube containing the sample is attached to a thermometer by
means of a small rubber band. The rubber band must be kept well above the level of the hot oil,
or the oil could melt the rubber and break the band. For accurate reading, the sample compound
in the capillary tube is kept close to and at the level of the thermometer bulb, which is fully
submerged and centered in the oil bath, as shown in Figures 1-2.
When the apparatus has been arranged, properly heat the bottom portion of the side arm with
burner. Convection currents carry the heated oil up through the side arm and down the main shaft
of the apparatus for uniform heating. Apply heat at a moderately rapid rate until the bath liquid is
within 15-20 oC of the melting point. Continue the heating with a very small flame adjusted so
that the temperature rises slowly and at a uniform rate (about 1 oC per minute). If necessary, hold
the burner by its base and move it back and forth under the bath. Observe carefully the samples
in the melting point tube and the thermometer reading. Record as the observed melting point the
range between the thermometer reading when sample starts to liquefy and that when the melt is
clear. After the samples have melted, extinguish the flame and allow the bath to cool.
59
illustration.
Dispose of the used capillary tubes by putting them in your trash can. If any isopropyl alcohol is
left in your test tube, you may pour it down the drain with water.
61
Activity No. 11
Boiling Point and Melting Point Determination
Course:______________________ Professor:__________________
Benzoic Acid
Urea
(Expt’l) (Theoretical)
Isopropyl Alcohol
Acetone
Acetic Acid
V. Questions.
1. Which of the following solid samples has the largest melting point range?
Explain. 2. Which of the three liquids has the highest boiling point? Explain.
62
Activity No. 12
Recrystallization of Impure Benzoic Acid
I. Objectives
II. Introduction
A suitable recrystallization solvent should also be partially volatile in order to be easily removed
from the purified crystals. The solvent should not react with the compound being purified and it
should have the boiling point below the melting point of the compound being purified. In
selecting a good recrystallization solvent one should also consider flammability, toxicity, and
expense.
In this experiment, we are going to purify Benzoic acid that is contaminated with a small
amount of Copper (II) sulfate.
III. Materials/Reagents
(1) Hot Plate (3) 5 mL Test tubes
IV. Procedure
1. Place a pinch of pure benzoic acid sample in three separate test tubes.
2. In the first test tube, add 10 drops of Hexane; second test tube, 10 drops of Ethyl alcohol; and
third test tube, 10 drops of Water.
3. Swirl and compare the relative amount of Benzoic acid that is dissolved in the three solvents.
4. Place the three test tubes in a water bath and heat to 70 oC. Observe which solvent has
dissolved the Benzoic acid in greatest amount. This will be your best extracting solvent.
1. Obtain a sample of Benzoic acid that is contaminated with Copper(II) sulfate. 2. Add
approximately 0.5 g (record the actual mass) of the contaminated Benzoic acid and 5 mL of
water to a 25-mL Erlenmeyer flask.
3.Warm the flask and its contents on a hot plate and slowly add near-boiling water to
dissolve the solids.
4. Continue to warm the flask and add near-boiling water until all of the solids have Dissolved.
Do not add too much water or the solution will not be saturated and the yield of purified Benzoic
acid will be reduced. Keep adding water in small amounts (several drops at a time from a Pasteur
pipette) until all of the Benzoic acid is dissolved while the solution is boiling.
5. Remove the flask from the hot plate and add a scoop of activated carbon (Note: Add the
carbon gradually, effervescence might occur). Heat it for 5 minutes and filter right away.
6. Allow the beaker containing the filtrate to cool slowly on the bench top. After approximately
twenty minutes, crystals will have formed. Cool the suspension further using an ice bath.
7. Transfer the crystals to a filter funnel, and filter the Benzoic acid–water suspension.
8. Wash the Benzoic acid crystals with ice-cold water by pouring ice-cold water over the
crystals.
9. Dry the crystals for a week and determine the mass of pure Benzoic
acid. 10. Determine the melting point of Benzoic acid.
11. Determine the percent purity of the impure Benzoic acid using the
formula: % Benzoic Acid = mass of pure benzoic acid/mass of mixture X100
64
Activity No. 12
Recrystallization of Impure Benzoic Acid
Course:__________________ Professor:_________________
Hexane
Ethyl Alcohol
Water
Questions
2. Impure Benzoic acid was dissolved in hot water. The container of solution was placed in an
ice-water bath instead of being allowed to cool slowly. What will be the result of cooling the
solution in this manner?
65
3. What are the reasons of adding the following materials in recrystallization of
solids? a. boiling stones
b. activated carbon
c. seed crystals
I. Objectives
II. Introduction
Caffeine is a heterocyclic (i.e., has atoms other than carbon in a ring) amine found in
many plant materials including tea leaves, coffee beans, kola nuts, and cocoa beans. Compounds
found in nature are referred to as “natural products” and amine natural products are called
alkaloids. Hence, Caffeine is an alkaloid. Many alkaloids, including Caffeine, have
pharmacological effects. Some other examples are Morphine, Codeine, Cocaine, and Nicotine.
Caffeine-containing beverages, mainly tea and coffee, have been used for their stimulant effect
for over a thousand years. Caffeine is also a diuretic and a vassoconstrictor (constricts blood
vessels). Recognition of the vassoconstriction effect suggests Caffeine’s use as a treatment for
headaches especially migraines. In fact, it is often added to headache remedies, including
Excedrin and other OTC analgesics and is also a key ingredient in the new prescription drug,
Fioret. Caffeine’s side effects and addictive nature lead many people to use decaffeinated coffee,
cola, etc. The Caffeine can be removed from coffee beans by extracting the beans with an organic
solvent (the old method) or with supercritical carbon dioxide.
Spots with identical Rf values in two different samples can reasonably be concluded to indicate
the presence of the same compound in both samples.
67
III. Materials/Reagents
8 x 6 cm TLC plate (5) 10-mL test tubes
2 Capillary micropipettes Spatula
TLC Tank and Lid (2) Pasteur Pipette
Ruler Caffeine
UV Lamp Ethanol
Dichloromethane TLC solvent (5% acetic acid in ethyl acetate) Diet Cola, Instant
Coffee, and Analgesic Pill
Dragendorff Reagent
IV. Procedure
Extraction of Caffeine
1. Solid samples – instant beverages and analgesic pills. Use 500 mg of the sample. Make sure to
record the actual mass used. If a solid sample is not a fine powder to begin with, then you
will need to grind it to a powder, preferably by using a mortar and pestle. Put each powder
into a small, labeled test tube. Add 2.0 mL Ethanol to each test tube and shake to mix
thoroughly. Heat the tubes gently on a hot water bath for 2-3 minutes and then allow the
contents to cool and settle. Not all of the powder will dissolve; the inorganic buffering agent
(if present) and binder are insoluble in ethanol. However, any organic compounds present
will dissolve. Remove the ethanol solution from undissolved solids using a pipet. Use this
solution to spot the TLC plate.
2. Liquid samples. Measure 4 mL of the liquid into a large test tube. Wear gloves during the rest
of this step. Add 5 mL of CH2Cl2 to the tube. Cap the tube with a tight fitting rubber sleeve
stopper or cork and shake gently at first, frequently removing the stopper to allow venting of
any pressure build up. Shake well then allow the layers to separate. Caffeine is much more
soluble in CH2Cl2 than in H2O so any caffeine present goes into the CH2Cl2 layer. Use a
Pasteur pipet to transfer most of the lower dichloromethane layer to a small test tube. Add a
few CaCl2 pellets to this tube and let stand for 5-10 minutes- the solution should clear up as
the CaCl2 absorbs any remaining water . Use this solution to spot the TLC plate.
TLC Procedure
1. Put approximately 25 mg of Caffeine in a small, labeled test tube. Add 4.0 mL of Ethanol mix,
and heat gently to dissolve the caffeine.
2. Obtain a TLC plate. The plate should be handled using forceps so as to avoid contamination.
A light pencil line should be drawn using a straight edge about 1 cm from one end of the
plate.
3. The instructor will demonstrate the spotting technique. Use a capillary micropipette to make a
small spot of the pure Caffeine solution (made in step 3) on the plate. Place the spot 1 cm
from the left edge along the pencil line you drew. Also spot the TLC plate with each of the
solutions prepared in steps 1 and 2. Make these three spots at 1-cm intervals to the right of
68
the Caffeine spot. In order to avoid confusion make sure to label the spots lightly in pencil
bellow the line.
4. Develop the TLC plate by placing it in a beaker that has been filled with developing solvent
(5% acetic acid in Ethyl acetate) to a level of less than 1 cm high (the spot on the TLC plate
should be above the level of the solvent). Cover the beaker with aluminum foil immediately
after the TLC plate is immersed. Allow the solvent to migrate up the TLC plate until it is
about one centimeter from the top. Do not allow the solvent line to reach the top of the plate.
5. Remove the TLC plate and mark the level to which the solvent rose with a pencil. Allow the
solvent to evaporate off of the plate in the hood and then visualize the plate under UV light or
spray the plate with Dragendorff reagent. Outline all spots with a pencil.
6. Measure the distance the solvent moved as well as the distances of all spots. Carefully sketch
the TLC plate in the space provided on the report sheet.
69
Activity No. 13
Diet Cola
Instant Coffee
Analgesic
V. Questions
2. Give the structures of the other organic compounds being used as solvents in this experiment:
Acetic Acid, Ethyl acetate, Ethanol, and Dichloromethane. Identify the functional group family to
which each of these belongs.
70
Activity No. 14
Simple and Fractional Distillation
I. Objectives
II. Introduction
Distillation is the most common method used to separate and purify liquids. The process
consists of heating a liquid to its boiling point and conducting the vapors to a cooling device
where they are condensed. The condensate is then collected. The vapor pressure of a liquid is
defined as the pressure that is exerted by a liquid at a given temperature. This force is due to the
molecules escaping from the liquid’s surface into the gas phase. The vapor pressure of a liquid
increases with increasing temperature. The boiling point of a liquid is that temperature at which
the vapor pressure is equal to the pressure of the surroundings. There are three common
distillation processes that are commonly used in separating components of mixtures,
Simple distillation is used in separating liquid components with boiling point difference greater
than 25 oC. However, for liquid components having boiling points less than 25 oC, fractional
distillation is preferred. In this process, a fractionating column is employed.
In steam distillation, which is commonly used to separate essential oil from plants, the
component (oil) is extracted using steam. In this process, the component boils below its normal
boiling point because of the presence of water which contributes to the total pressure of the
whole mixture in the sample.
In this experiment, you are going to perform the first two methods (simple distillation and
fractional distillation). Steam distillation is reserved for the next activity.
III. Materials/Reagents
(1) Hot Plate Chloroform
(1) boiling flask Isopropyl alcohol
(1) Distillation apparatus Boiling chip
(1) 25-mL graduated cylinder100 (1)- 100-mL thermometer
(4) 10-mL test tubes (3)-Universal clamp
(1) separatory funnel (1) Test tube rack
Mixture of Methanol and 1-Butanol (1:1)
71
IV. Procedure
For setting up the apparatus for simple and fractional distillations refer to the figures
below.
1. Take 40 mL of the Methanol-Butanol mixture into the 100-mL round bottom distilling flask.
Add two or three boiling chips to promote even boiling. Make sure all connections in the
apparatus are tight.
2. Turn the setting of the hot plate so that temperature reading is between 60-80oC.
3. Adjust the heat until the distillate drops at a rate of one drop per second. 4.
Record the temperature and volume of the distillate at 1 mL intervals.
5. After 25 mL of distillate has been collected, quickly replace the 25 mL graduated cylinder
with a 10 mL graduated cylinder. Continue to take volume and temperature readings until
another 10 mL of distillate has been collected.
6. Set aside the distillates and proceed to fractional distillation.
B. Fractional Distillation
1. Return all the distillates back to the boiling flasks and set up Figure 2 for fractional
distillation. Add 3 new chips of boiling chips.
2. Heat the mixture and observe the formation of condensate which gradually rises up in the
fractionating column.
3. Once condensation of the vapors occurs, it should continue steadily at a rate
not greater than one drop per second.
4. Collect the distillate in the graduated cylinders and record the temperature and volume of the
distillate at 1 mL intervals until the temperature starts to rise.
5. When you see the temperature increases, record the temperature and volume of distillate at
intervals of 0.5 mL until the temperature no longer continues to increase.
At this point, record the temperature and volume of the distillate at 1 mL intervals until about 35
mL of total distillate has been collected. Do not distill to dryness.
6. Plot Temperature vs. Volume of Distillate. Compare your result with that of simple distillation.
72
Activity No. 14
Simple and Fractional Distillation
1. Plot the distillation temperature as a function of the volume of distillate. Use the Excel
plotting program to accomplish this task. Superimpose the plot for fractional distillation over
the plot for simple distillation. Based on the plots of simple versus fractional distillation,
what conclusions can you draw regarding the efficiency of separation of the liquids for each
method? Account for the difference in shape of the curve.
I. Objectives
II. Introduction
The term “capsaicinoids” describes a group of pungent chemical analogues found in hot peppers
(Capsicum annum and C. frutescens). There are five naturally occurring capsaicinoids: capsaicin,
dihydrocapsaicin, nordihydrocapsaicin, homocapsaicin, and homodihydrocapsaicin . The most
abundant and potent analogues in peppers (and consequently pepper extracts) are capsaicin and
dihydrocapsaicin. Nordihydrocapsaicin, homocapsaicin, and homodihydrocapsaicin are also
present, but generally contribute little to the total capsaicinoid concentration and pungency of the
pepper.
For centuries, people have used concentrated extracts of peppers (oleoresin capsicum) or the
dried fruits to prepare spicy foods. Other historical and current uses of pepper products include
neurobiological research, weight loss, local anesthesia, anti-microbial defense, anti-inflammation
preparations, and recently for the production of self-defense and less than-lethal (LTL) weaponry.
The extensive use of peppers and pepper extracts for such diverse purposes emanates from the
presence of capsaicinoids in the pepper.
III. Materials/Reagents
(1) 400-mL beaker Soxhlet Extractor
Knife 95% Ethanol
20 pieces unripe Hot peppers (5) 10-mL Test tubes
Warnings
• Pure capsaicin powder in milligram amounts can cause severe skin blistering, burns, and
reported nerve damage.
• Use full personal protection equipment (lab coat, goggles, gloves) and have an eye wash
ready
• Use a dust mask when handling dried peppers
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IV. Procedure
1. Weigh and cut the peppers, separate the seeds from the flesh manually.
2. Dry the seeds and flesh in the oven at 100 oC for 1h.
3. Grind the seeds and flesh separately in a mortar and pestle.
4. Set up 250 mL round bottom flask in heating mantle or water bath, add clean, new boiling
chips, and 50 mL 95% ethanol.
5. Place soxhlet extractor onto flask, fluff 1 or 2 cotton balls and place at the bottom of the
extractor (pack with a glass rod).
6. Add dried seeds to extractor, and level out. Add pepper flesh until full and level out. Place
another 1-2 cotton balls ontop and pack gently with a glass stir rod.
7. Fit adapter and condenser to the extractor. Begin heating to boiling.
8. Maintain heating and replenishing water bath as necessary for 2 hours (typically until ethanol
coming off the extractor is clear).
9. As the ethanol boils, it travels at the side arm, filling up the thimble with ethanol. Once the
side arm is filled with ethanol, the liquid from the thimble is siphoned off, and the whole process
repeats again, with the new alcohol extracting the sample but using the same 50 mL Ethanol. Do
not leave unattended and see to it that the container will not run dry. The solution turns dark.
Concentration Procedure
1. If available, use a rotary evaporator with a bump-trap to remove solvent. 2. Set up a distillation
apparatus, evaporate solvent under reduced pressure carefully to prevent bumping
3. Allow concentrate to stand overnight in a sealed vial once cool. Oil will form separate
layer. 4. Use pasteur pipette to remove bottom oil layer (red-brown).
5. Weigh the isolated capsaicinoids oil.
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Qualitative test for Phenolic Group
1. FeCl3 Test
Br2/CCl4 test
V. Questions.
capsaicinoid.
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Activity No. 16
Solubility of Organic Compounds
I. Objectives
II. Introduction
The solubility of a solute (a dissolved substance) in a solvent (the dissolving medium) is the
most important chemical principle underlying three major techniques you will study in the
organic chemistry laboratory: crystallization, extraction, and chromatography. In this experiment
on solubility you will gain an understanding of the structural features of a substance that
determine its solubility in various solvents. This understanding will help you predict solubility
behavior and understand the techniques that are based on this property.
Five common reagents are used for solubility tests: (1) water, (2) 5% NaOH, (3) 5% NaHCO3,
(4) 5% HCl, and (5) concentrated (96%) H2SO4. Except in the case of water, solubility
experiments probe the acid-base properties of organic compounds. If a compound is an acid, you
can obtain a relative measure of its acid strength by testing it against the weak base sodium
bicarbonate and the stronger base sodium hydroxide. Naturally, any organic compound that is
soluble in water is also likely to be soluble in 0.6 M NaHCO3, 1.5 M HCl, and 2.5 M NaOH
solutions because these solutions are composed largely of water.
III. Materials/Reagents
IV. Procedure
General Procedure
Place approximately 1 mL of the test solvent into a small test tube. Add 3 drops of the liquid (or
a few crystals of the solid) test substance to the solvent. Stir by gently tapping the test tube with
your finger. Determine if the small amount of compound immediately dissolves (if not you may
need to stir some more, wait a few minutes or use very gentle heating. If the small amount of
sample does not dissolve, the compound is insoluble in that solvent. If the small sample does
dissolve, add several more drops of liquid (or crystals of solid) to determine whether the
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compound is very soluble or slightly soluble. Record your observations and determination of
solubility (I – insoluble, SS – slightly soluble, VS – very soluble) in the data table.
Properly dispose of the solution. Dispose of all aqueous solution in the Aqueous Waste
Container. Leftover organic compounds should be disposed of in either Halogenated or Non
Halogenated Organic Waste container.
A. Solubility of Alcohols
1.Take 1 mL of distilled water and add 3 drops of Methanol. Note the result. 2. Repeat the
experiment using other alcohols, Ethanol, Propanol, 1-Butanol, and tert-Butyl Alcohol
3. In another test tube, add 1mL of Hexane and add 3 drops of Methanol. Note the result. 4.
Repeat the experiment using other alcohols: Ethanol, Propanol, 1-Butanol, and tert-Butyl
Alcohol
3. Solubility of Phenol
a. Take 1 mL of distilled water and add a pinch of Phenol. Note the result b. Repeat the
experiment using other solvents: 5% M NaOH, 5% M NaHCO3, 5% M HCl, Concentrated
H2SO4. Note the results.
5. Solubility of Hexane
a. Take 1 mL of distilled water and add 3 drops of Hexane. Note the result b. Repeat the
experiments using other solvents: 5% M NaOH, 5% M NaHCO3, 5% M HCl, Concentrated
H2SO4. Note the results.
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6. Solubility of Benzaldehyde
a. Take 1 mL of distilled water and add 3 drops of Benzaldehyde. Note the result b. Repeat the
experiments using other solvents: 5% M NaOH, 5% M NaHCO3, 5% M HCl, Concentrated
H2SO4. Note the results.
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