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VISION
MISSION
EXPERIMENTS:
DATE
EXPERIMENT 1
TITLE
I. OBJECTIVE
II. LAB WORK PRINCIPLE
III. EQUIPMENT AND CHEMICALS
IV. PROCEDURE AND OBSERVATION
1.
2.
B
3.
4.
Laboratories :
Name/NPM : 1. ……….
2. ……….
( )
GROUP
NAME : 1.
2.
NPM : 1.
2.
II.2. CONTENT
DATE
EXPERIMENT 1
TITLE
I. THEORY
II. DATA PROCESSING
III. OBSERVATION RESULT ANALYSIS
IV. ASSIGNMENT AND QUESTION ANSWER
V. REFERENCE
GROUP :
1. ………………….NPM ……………….
2. ………………….NPM ……………….
Signature of Laboratory Assistant
( )
I. Heating
Most of heating process in laboratory are done with gas burner. For some cases, we
will use oven equipment during this process. Bunsen burner (from the figure below) usually
has 2 valves for gas and air arrangement.
To turn on a bunsen burner, please follow these steps:
Air valve is in a closed condition,while the gas valve is in an opened condition
Turn it on with matches. From this step, we will see a not-too-hot red flame
To get a better flame and higher temperature from the bunsen burner, open the air valve
slowly until the blue flame appear.
After combustion, turn off the bunsen burner by closing the gas flow.
If the bunsen burner is used for heating a substance in a beaker glass / test-tube , the
steps can be seen from this figure below:
II. Filtration
Filtration aims to separate a liquid substrate from the solids one by passing the
substrate through a filter paper. The filtration procedure is as follows:
Fold the filter paper like the figure below:
Set it on the funnel, then wet the filter paper with distilled water and avoid any air cavity
behind the filter paper.
Note that the position of the filter paper must 0.5 -1 cm from the top edge of
the funnel and the amount of sediment is 2/3 from the maximum height of the
filter paper.
III. PROCEDURES
III.1. Physical Properties
1. Observe and record the shape, color, and smell of the following substances: Methanol,
CaCO3, sugar, Toluene, Benzene, HCl and NaOH.
2. Dissolve each substance in the water. Shake the solution, observe and record the
changes.
3. Do the step number 2 to ether.
4. Explain how to identify substances that have the same shape and color, based on
the physical properties of these substances.
III.2. Chemical Properties
REPORT SHEET
Physical Properties
Changes Result Explaination About
Sample
Shape Color Smell Substances
Methanol
CaCO3
Sugar
Toluene
Benzene
HCl
NaOH
Chemical Properties
Base Effect Sample
(NaOH) Al Zn Fe CaCO3
Change of
Color
II. INTRODUCTION
Mixtures are not unique to chemistry; we use and consume them on a daily basis. The
beverages we drink each morning, the fuel we use in our automobiles, and the ground we
walk on are mixtures. Very few materials we encounter are pure. Any material made up of
two or more substances that are not chemically combined is a mixture.
The isolation of pure components of a mixture requires the separation of one
component from another. Chemists have developed techniques for doing this. These methods
take advantage of the differences in physical properties of the components. The techniques to
be demonstrated in this laboratory are the following:
1. Sublimation. This involves heating a solid until it passes directly from the solid phase
into the gaseous 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. Extraction. This uses a solvent to selectively dissolve one component of the solid
mixture. With this technique, a soluble solid can be separated from an insoluble solid.
3. Decantation. This separates a liquid from an insoluble solid sediment by carefully
pouring the liquid from the solid without disturbing the solid (Figure 2.1).
4. Filtration. This separates a solid from a liquid through the use of a porous material as a
filter. Paper, charcoal, or sand can serve as a filter. These materials allow the liquid to
pass through but not the solid (see Figure 2.2 in the Procedure section).
5. 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.
IV.2.2.Crystallization
The separation substance based on the solubility and temperature difference from two
or more of substances.
1. Add 10 ml of distillated water into test tube, then adding KNO3 2 M 3 ml into that test
tube with little CuNO3 (1 spatula). Heating that mixture until soluble, then cooling it
and filtering the crystal that form. Rinsing it with distillated water until the color
disappears.
2. Dissolve a little crystal into the distillated water and testing ion K with ion specific
test. To another crystal, we do flame test.
IV.1.3. Sublimation
The separation of substances that have a high pressure on temperature basis below the
melting point.
1. Put a mixture of Na2SO4 and NH4Cl (2 grams each) into vaporizer bowl. Heating it
slowly until white steam appears. Put watch glass on bowl, and continuing the heating
until there are no white steam.
2. Collect the white substances that cling on watch glass, then add 10 ml of water. White
substances is divided into 2 parts :
V. POTENTIAL HAZARDS
Potassium Nitrate (KNO3)
- Oxidizing solids may intensify fire; oxidizer. Causes skin irritation. Causes serious
eye irritation. May cause respiratory irritation. Toxic substance.
- Wear safety eyeglasses, protective gloves, and clothing to prevent skin exposure.
Sodium Sulfate (Na2SO4)
- Hygroscopic. May causes eye, skin, and respiratory tract irritation
- Wear protective gloves/protective clothing/eye protection/face protection.
Sodium Cobalt Nitrite
- May intensify fire; oxidizer. Causes skin irritation. May cause an allergic skin
reaction. Causes serious eye irritation.
- Wear safety eyeglasses, protective gloves, and clothing to prevent skin exposure.
Potassium Hydroxide (KOH)
- Corrosive. Water-reactive. Causes severe eye and skin burns. Causes severe
digestive and respiratory tract burns. Harmful if swallowed.
- Wear safety eyeglasses, protective gloves, and clothing to prevent skin exposure.
Kalium Thiocyanate (KCNS)
- Acute toxicity (oral). Harmful if swallowed. Causes skin corrosion/irritation. Causes
serious eye irritation. Harmful to aquatic life.
REPORT SHEET
Observation Result
II. INTRODUCTION
We frequently encounter acids and bases in our daily life. Fruits, such as oranges,
apples, etc., contain acids. Household ammonia, a cleaning agent, and Liquid Plumber are
bases. Acids are compounds that can donate a proton (hydrogen ion). Bases are compounds
that can accept a proton. This classification system was proposed simultaneously by Johannes
Brønsted and Thomas Lowry in 1923, and it is known as the Brønsted-Lowry theory. Thus
any proton donor is an acid, and a proton acceptor is a base.
When HCl reacts with water
HCl + H2 O ⇄ H3 O+ + Cl−
HCl is an acid and H2 O is a base because HCl donated a proton thereby becoming
Cl− , and water accepted a proton thereby becoming H3 O+ . In the reverse reaction (from
right to left) the H3 O+ is an acid and Cl− is a base. As the arrow indicates, the equilibrium in
this reaction lies far to the right. That is, out of every 1000 HCl molecules dissolved in water,
990 are converted to Cl− and only 10 remain in the form of HCl at equilibrium. But H3 O+
(hydronium ion) is also an acid and can donate a proton to the base, Cl− . Why do hydronium
ions not give up protons to Cl− with equal ease and form more HCl? This is because different
acids and bases have different strengths. HCl is a stronger acid than hydronium ion, and
water is a stronger base than Cl− .
In the Brønsted-Lowry theory, every acid–base reaction creates its conjugate acid–
base pair. In the above reaction HCl is an acid which, after giving up a proton,becomes a
conjugate base, Cl− . Similarly, water is a base which, after accepting a proton,becomes a
conjugate acid, the hydronium ion.
K w , the ion product of water, is still a constant because very few water molecules
reacted to yield hydronium and hydroxide ions; hence the concentration of water essentially
remained constant. At room temperature, the K w has the value of
K w = 1 x 10−14 = [1 x 10−7 ] 𝑥 [1 x 10−7
This value of the ion product of water applies not only to pure water but to any
aqueous (water) solution. This is very convenient because if we know the concentration of
the hydronium ion, we automatically know the concentration of the hydroxide ion and vice
[HA] is the concentration of the acid and [A− ] is the concentration of the conjugate
base. The pK a of the carbonic acid–bicarbonate system is 6.37. When equimolar conditions
exist, then [HA] = [A− ]. In this case, the second term in the Henderson-Hasselbalch equation
[A− ]
is zero. This is so because [HA] = 1, and the log 1=0. Thus at equimolar concentration of the
acid–conjugate base, the pH of the buffer equals the pK a ; in the carbonic acid–bicarbonate
system this is 6.37. If, however, we have ten times more bicarbonate than carbonic acid,
[A− ]
[HA]
= 10, then log 10=1 and the pH of the buffer will be
IV. PROCEDURES
IV.1.The Properties of Acids and Bases
1. Ask your assistant to give you 6 acids and bases. Observe and note the color of the
solutions.
2. Take 5 ml of the solution into the test tube. Sign each solution with name L1 until L6.
3. Take the pH paper, dip the edge into the solution. Be careful not to hit your fingers. Dry
the paper and note the color. Determine the pH of the solution by matching the color of
the pH paper with the instructions in the pH paper’s box.
4. Do the step A3 for all of the solutions given by the assistant. Note all of the solutions’
pH and give sign what solutions are acids and bases. Give basic description of what
you use to distinguish acids and bases.
5. Take one of the acids and bases solution above. Fill into the test tube of each solution 5
ml. Give the sign a0 (acid) and b0 (bases). Perform a ratio of 1:1; 1:10; 1:100; and
1:1000 dilutions. Give the name of each solution a1 until a4 for acids and b1 until b4 for
bases.
6. Measure the pH of each solution as step A2. Record the pH and fill the record into
table accordance with the order of the concentration of the solution.
7. Create a graph of the concentration and pH of the solution. What conclusion that you
get from the experiment?
IV.2. Acids and Bases Reaction
1. Make a solution of 0.1 molar NaOH, HCl and acetic acid as 100 ml each. Write the
calculation and how to make the solutions.
2. By using volumetric pipette, take 5 ml of 0,1 molar solution of HCl and put into
Erlenmeyer. Then give 1-2 drops of phenolphthalein indicator. Observe and record the
color.
V. POTENTIAL HAZARDS
1. What is the indicator of the acid-base titration? Explain how to select an indicator for
titration.
2. What is the difference of acids/bases strong and weak? Mention the ways to identify
whether an acid and base is strong or weak.
REPORT SHEET
REPORT SHEET
Moles
Color
II. INTRODUCTION
II.1. Reactions of acids with metals
Acids react with most metals and a salt is produced. But unlike the reaction between
acids and bases we don't get any water. Instead we get hydrogen gas.
This is the general word equation for the reaction:
metal + acid → salt + hydrogen
II.2. Salts
The salt produced depends upon the metal and the acid. Here are two examples:
zinc + sulphuric acid → zinc sulphate + hydrogen
magnesium + hydrochloric acid → magnesium chloride + hydrogen
It doesn't matter which metal or acid is used, if there is a reaction we always get
hydrogen gas as well as the salt.
II.3.The test for hydrogen
There is a simple laboratory test to see if a gas is hydrogen. A lighted wooden splint
goes pop if it is put into a test tube of hydrogen. This is because the flame ignites the
hydrogen, which burns explosively to make a loud sound.
II.4. Acids and hydrogen
All acids contain hydrogen atoms. Apart from hydrochloric acid, this is not clear from
their names, but you can tell they contain hydrogen from their chemical formulae. Remember
that the chemical symbol for hydrogen is H.
IV. PROCEDURES
IV.1. Qualitative Observation
1. Provide 4 pieces of test tubes, and fill each tube with 6M HCl solution 5ml. Label it
S1 s/d S4.
2. Weigh each 0,1 gr metals Zn, Fe, Cu and Al. Then, insert those metals to the
test tubes Sl s/d S4. Observe and note the changes happened.
3. If the metals reactivity can be seen from the amount of gas formed, order the metals
reactivity based on your observation!
4. Write down the reaction equation from this experiment and suggest an experiment to test
what kind of gas formed on the reaction above.
IV.2. Quantitative Observation
1. Provide 5 pieces of clean erlenmeyer flask 100 ml. Label it S1 s/d S5.
2. Fill each erlenmeyer with 6M HCl 10 ml (use volumetric pipette 10ml, measure it
correctly), then close it with watch glass. Calculate the mole of HCl, and write down
the answer.
3. Insert Zn, Fe, Cu and Al metals 0,2 gr each into erlenmeyer S1 s/d S4. Solution in
erlenmeyer S5 will be reacted with nothing.
4. Note when the metals reacted, and let the reaction happened for 30 -40 minutes.
(determined by the assistant).
V. POTENTIAL HAZARDS
Zinc (Zn)
- Self-heating: may catch fire. In contact with water releases flammable gases. Very
toxic to aquatic life: Very toxic to aquatic life with long lasting effects.
- Wear protective gloves/protective clothing/eye protection/face protection.
Copper (Cu)
- Flammable solid. Causes respiratory tract irritation. May cause lung damage. May
cause liver and kidney damage. Causes eye and skin irritation. Can be explosive
when exposed to heat or flames.
- As in any fire, wear a self-contained breathing apparatus in pressure-demand,
MSHA/NIOSH (approved or equivalent), and full protective gear.
Iron (Fe)
- Flammable solid. May cause mechanical eye and skin irritation. May cause blood
abnormalities. May cause lung damage. Inhalation of fumes may cause metal-fume
fever. May cause cardiac disturbances. May cause liver damage.
- Wear protective gloves/protective clothing/eye protection/face protection.
1. Is there any effect from the location of these metals in periodic table and their
reactivity to react with acid? Explain!
2. What factor affect the rate of reaction in general as long as you know?
REPORT SHEET
Qualitative Observation
Metals Reaction Time Changes
(0,1 gr) S1 S2 S3 S4 Result
Zn
Fe
Cu
Al
Note: S1-S4 reacted with 5 mL 6M HCl.
REPORT SHEET
%-HCl Conversion
Type of %-HCl
Metals Conversion
Zn
Fe
Cu
Al
III. PROCEDURES
III.1. Qualitative Observation
1. Ask a assistant 3 kinds of solid materials containing crystalline water. Observe and
write down the name of the substance and their colors.
2. Insert those substance into a pyrex test tube each. Label it.
3. Use a wood clamp to hold the test tube, then heat the substance in the tube on the
bunsen burner. Observe and write down the changes happened.
4. Then, drop a water into the test tube. Observe and write down the changes
happened.
5. Write down the reaction equation, all of the heating and watter addition activity.
Explain those equation and the difference between those substance based on your
observation.
V. POTENTIAL HAZARDS
CuSO4.XH2O
- Toxic if swallowed. Very toxic to aquatic life with long lasting effects.
- Wear safety eyeglasses, protective gloves, and clothing to prevent skin exposure.
MgSO4.XH2O
- Not classified.
- Wear safety eyeglasses, protective gloves, and clothing to prevent skin exposure.
CaCl2.XH2O
- Serious eye damage/eye irritation.
- Wear safety eyeglasses, protective gloves, and clothing to prevent skin exposure.
REPORT SHEET
Qualitative Observation
Cystalline Changes Result Reaction Addition Activity
Water Heating Water Equation Heating Water
CuSO4.XH2O
FeCl3.XH2O
MgSO4.XH2O
Quantitative Observation
Changes Result Material Mass
Cystalline Reaction
Heating Color Before After
Water Equation
Heating Heating
CuSO4.XH2O
FeCl3.XH2O
MgSO4.XH2O
Unsaturated hydrocarbon has less number of hydrogen which can make bond from its
maximum number. This compound must have double bond so that the total number of
covalent bond is four. Ethylene and acetylene are examples for this compound.
But, both of them represent a different molecule. Structure (c), using circle inside the
hexagon, can be accepted. The circle represents the six electrons which are distributed evenly
at the aromatic π bond at six carbon atoms. The bonds which are represented by the
hexagonal side are σ bond. Structure (c) can be used to represent all kind of carbon bonds
inside the benzene correctly.
II.2. Reactivity of Hydrocarbon
The σ bond from saturated bond (alkane) is very stable so it is not reactive. At high
temperature, saturated hydrocarbon can react with oxygen (combustion). From this reaction,
carbon bonds are broken and the products are carbon dioxide and water. If the combustion is
not efficient, then carbon monoxide or even single carbon (soot) can be produced. But,
generally, saturated hydrocarbon is combusted more efficiently than other types of
hydrocarbon.
The hydrogen-carbon bond from alkane can be replaced by halogen. General reaction
for bromine is:
Look at the equation, HBr is a product from the reaction. To react with halogen, we
need heat or light energy.
The π bond from unsaturated hydrocarbon (alkene and alkyne) is reactive and it is
easier for additional reaction to happen. In this reaction, a molecule like bromine forms two
single bonds of carbon-bromine which is in one π bond energy level. Ethylene reacts with
bromine to form 1,2-dibromothane.
The π bond from aromatic compound is hold out in the reaction. Even for saturated
group which make bond with benzene ring can be attacked by oxidizing agents with a very
large energy. The product which is produced when single group alkyl bonded with benzene
ring is benzoic acid.
Hydrogen atom from benzene can be substituted by bromine, but it needs catalyst Fe.
Look that the following reaction is a substitution reaction and HBr is produced.
IV. PROCEDURES
Caution: all organic waste must be thrown at the right place.
Note:
1. Do all the following experiments below.
2. Experiment A until D use three types of hydrocarbon: heptane, 1-octene, and toluene.
Use clean and dry test tubes for all reactions. The structure for the three compounds
are :
V. POTENTIAL HAZARDS
Flame risk from heating chemical. Use gloves when heating the chemicals with
Bunsen or with water bath.
Heptane
- Breathing vapors may cause drowsiness and dizziness. Causes eye, skin, and
respiratory tract irritation. Aspiration hazard if swallowed. Can enter lungs and
cause damage. Dangerous for the environment.
REPORT SHEET
Solubility of Hydrocarbon
Solubility
Sample
Water 1-butanol Ligroin
heptane
1-octene
toluene
Flammability of Hydrocarbon
Flammability
Sample
Type Color Carbon Total Residue
heptane
1-octene
toluene
REPORT SHEET
II. INTRODUCTION
Alcohol can be said as organic solvent which is analog to water. In alcohol, hydroxyl
group (-OH) is attached to saturated carbon not at the hydrogen atom as in water. The
hydroxyl group makes physical and chemical properties very different with hydrocarbon.
Structure from hydroxyl group which is strongly affected character of alcohol is a polar bond
between hydrogen-oxygen and a pair of electrons from the oxygen.
Some chemical differences from alcohol depends on the alkyl group structure. One
important thing is how many carbon atom which is bonded with the –C-OH group. Primer,
secondary, and tertiary alcohol have 1,2, and 3 carbon group consecutively, which is attached
at the carbon atom bonded to oxygen atom.
Hydroxyl group from alcohol can make hydrogen bond with water. That is why,
alcohol is soluble in water than in hydrocarbon. All alcohol with low molecular weight is
completely soluble in water, and the solubility of high molecular weight is more likely to
alkane’s solubility. As the size of alkyl group increase, the polar hydroxyl group will give
less contribution to physical properties.
Proton from water molecule is more acidic than proton from hydroxyl group. That is
why proton from hydroxyl group can only be neutralized by strong alkaline.
Proton from hydroxyl group from water can be reduces by active metal and produces
hydrogen gas. This reaction is between active metal and water.
For tertiary alcohol, the reaction is very fast in room temperature. Secondary alcohol
reacts in 5-10 minutes. Primary alcohol can react after hours in room temperature. Because
alkyl chloride is not soluble in Lucas reagent, then the turbidity means that the reaction has
occurred. Time needed to start the reaction indicates the type of structure in alcohol.
Primary, secondary, and tertiary alcohols give different reaction to oxidizing agents.
Type of oxidizing agent which is typically used is sodium dichromate (Na2Cr2O7) in dilute
sulphate acid solution.
IV. PROCEDURES
IV.1. The Solubility of Alcohol in Water
1. Put 1 ml of water in small test tube.
2. Add some drops of ethanol while shaking until it does not soluble anymore or until
the volume is twice from initial volume of water.
3. Repeat the test with another alcohol (1-butanol, 2-butanol, 2-methyl-2-propanol, 1-
pentanol, and 1–octanol).
4. Characterize each alcohol: soluble, a litte soluble, or totally soluble. Write down on
your report.
V. POTENTIAL HAZARDS
Methanol
- Toxic by ingestion and inhalation. Can be toxic by skin absorption. Affects central
a.
b.
c.
d.
e.
g.
REPORT SHEET
Lucas Test
Lucas Test
Sample
5 minute 10 minute Chemical Equation
1-butanol
2- butanol
2-methyl-2-
propanol
REPORT SHEET
Oxidizing Alcohol
Color Change
Sample
1 drop Shake
methanol
ethanol
1-propanol
2- propanol
1-butanol
2-butanol
2-methyl-2-
propanol
1-pentanol
1–octanol
Iodoform Reaction
Color Change
Sample Amount I2-KI
2 minutes 5 minutes
Methanol
1-propanol
2- propanol
2-butanol
2-methyl-2-propanol
II. INTRODUCTION
Triglyceride, one kind of lipid, is ester from alcohol glycerol and long chain
carboxylic acid.
Triglyceride consists of acid with 8 to 12 carbon atom and mix of different types of
acid. If most of the acid is not saturated, then glycerides will be liquid and classified as oil.
Glycerides which have more saturated acid will have higher melting point and classified as
lipid/fat.
Hydrolysis of lipid or oil with base will produce glycerol and salt from the acid, it is
known as saponification. Soap is salts from long chained carboxylic acid. Sodium and
potassium salts are water soluble, while salts from magnesium, calcium, and iron are not
water soluble.
Since calcium salts from aryl sulfonate and alkyl sulfate are water soluble, detergent
is usually used in hard water, while soap will produce not soluble precipitate.
Every year, Americans use millions kilogram of detergent to wash clothes or other
things. Nearly every gram from detergent flows to lake or river. Most of laundry products
contain phosphate which will make algae fertile in the water. Phosphate act as fertilizer to
algae in the same form as phosphate when it make plants or grass fertile in garden. Algae
consume dissolved oxygen in water in a large number. Concentration of dissolved oxygen
will reduce so it be difficult for the life of fishes or other sea animal, hence, it will disturb
ecosystem equilibrium.
In this experiment, commercial detergent will be tested to know the existence of
phosphate in it. The basic of this reaction is chemical reaction between phosphate anion and
molybdate anion in acid solution.
V. POTENTIAL HAZARDS
Cotton seed oil
- May cause irritation. This is expected to be a low hazard for usual industrial
handling.
- Wear appropriate protective eyeglasses, protective gloves, and protective clothing
to prevent skin exposure.
Hexane
- Extremely flammable liquid and vapor. Vapor may cause flash fire. Possible risk
of impaired fertility. Breathing vapors may cause drowsiness and dizziness.
Dangerous for the environment. May cause nervous system effects.
- Wear appropriate protective eyeglasses, protective gloves, and protective clothing
to prevent skin exposure
REPORT SHEET
Unsaturated Triglyceride
No Sample Amount of Drops Need
1 Cottonseed Oil
2 Crisco
Soap
Alkaline Characteristic
No Sample Color of Litmus Paper
1 Soap
2 Commercial soap
3 Detergent
Emulsion Characteristic
No Sample Characteristic
1 Mineral Oil
2 Soap
3 Commercial Soap
The Effect of Metal Salt
Solution
No. Sample
Calcium chloride Magnesium chloride Iron (III) chloride
1 Soap
2 Commercial soap
3 Detergent
II. INTRODUCTION
Fats are esters of glycerol and fatty acids. Liquid fats are often called oils. Whether a
fat is solid or liquid depends on the nature of the fatty acids. Solid animal fats contain mostly
saturated fatty acids, while vegetable oils contain high amounts of unsaturated fatty acids. To
avoid arteriosclerosis, hardening of the arteries, diets which are low in saturated fatty acids as
well as in cholesterol are recommended.
Note that even solid fats contain some unsaturated fatty acids, and oils contain
saturated fatty acids as well. Besides the degree of unsaturation, the length of the fatty acid
chain also influences whether a fat is solid or liquid. Short chain fatty acids, such as found in
coconut oil, convey liquid consistency in spite of the low unsaturated fatty acid content. Two
of the unsaturated fatty acids, linoleic and linolenic acids, are essential fatty acids because the
body cannot synthesize them from precursors; they must be included in the diet.
The four unsaturated fatty acids most frequently found in vegetable oils are:
All the C=C double bonds in the unsaturated fatty acids are cis double bonds, which interrupt
the regular packing of the aliphatic chains, and thereby convey a liquid consistency at room
temperature. This physical property of the unsaturated fatty acid is carried over to the
physical properties of triglycerides (oils).
In order to separate the potassium salts of fatty acids from glycerol, the products of
the saponification mixture must be acidified. Subsequently, the fatty acids can be extracted
by petroleum ether. To identify the fatty acids that were isolated, they must be converted to
their respective methyl ester by a perchloric acid catalyzed reaction:
The methyl esters of fatty acids can be separated by thin-layer chromatography (TLC).
They can be identified by comparison of their rate of migration (Rf values) to the Rf values of
authentic samples of methyl esters of different fatty acids (Fig. 4.1).
IV. PROCEDURES
IV.1. Extraction of Fatty Acids
1. Weigh a 50-mL Erlenmeyer flask and record the weight on your Report Sheet (1).
2. Add 2 mL of corn oil and weigh it again. Record the weight on your Report Sheet (2).
3. Add 5 mL of 0.5 M KOH in ethanol to the Erlenmeyer flask. Stopper it. Place the
flask in a water bath at 55 OC for 20 min.
4. When the saponification is completed, add 2.5 mL of the concentrated HCl. Mix it by
swirling the Erlenmeyer flask. Transfer the contents into a 50-mL separatory funnel.
Add 5 mL of petroleum ether. Mix it thoroughly. Drain the lower aqueous layer into a
Figure 1. Spotting
5. When the solvent front has risen to about 1–2 cm from the top edge, remove the plate
from the beaker. Mark the advance of the solvent front with a pencil. Dry the plate
with a heat lamp under the hood. Place the dried plate in a beaker containing a few
iodine crystals. Cover the beaker tightly with aluminum foil. Place the beaker in a 110
O
C oven for 3–4 min. Remove the beaker and let it cool to room temperature. This
part is essential to avoid inhaling iodine vapors. Remove the TLC plate from the
beaker and mark the spots with a pencil.
6. Record the distance the solvent front advanced on your Report Sheet (4). Record on
your Report Sheet (5–9) the distance of each iodine-stained spot from its origin.
Calculate the Rf values of your samples on Report Sheet (10–14).
V. POTENTIAL HAZARDS
Corn oil
- May cause irritation. This is expected to be a low hazard for usual industrial
handling.
Na2SO4
- May cause eye, skin, and respiratory tract irritation. Hygroscopic (absorbs
REPORT SHEET
1. Weight of beaker ______________ g
2. Weight of beaker and oil ______________ g
3. Weight of oil ______________ g
Calculated Rf values
10. For spot no.1 [(5)/(4)] a______ b______ c______ d______ e______
11. For spot no. 2 [(6)/(4)] ______________
12. For spot no. 3 [(7)/(4)] ______________
13. For spot no. 4 [(8)/(4)] ______________
14. For spot no. 5 [(9)/(4)] a______ b______ c______ d______ e______
15. How many fatty acids were present in your corn oil?
16. How many fatty acids could you identify? Name the identifiable fatty acids in the
corn oil.
The reaction typically gives 60% to 70% of the maximum yield. The reaction is a reversible
process. An ester reacting with water, giving the carboxylic acid and alcohol, is called
hydrolysis; it is acid catalyzed. The base-promoted decomposition of esters yields an alcohol
and a salt of the carboxylic acid; this process is called saponification. Saponification means
“soap making,” and the sodium salt of a fatty acid (e.g., sodium stearate) is a soap.
IV. PROCEDURES
IV.1. Carboxylic Acids and Their Salts
IV.1.1. Characteristics of acetic acid
1. Place into a clean, dry test tube (100 x 13 mm) 2 mL of water and 10 drops of glacial
acetic acid. Note its odor by wafting (moving your hand quickly over the open end of
the test tube) the vapors toward your nose. Of what does it remind you?
2. Take a glass rod and dip it into the solution. Using wide-range indicator paper (pH 1–
12), test the pH of the solution by touching the paper with the wet glass rod.
IV.3. Saponification
This part of the experiment can be done while the esterification reactions are being heated.
1. Place into a test tube (150 x 18 mm) 10 drops of methyl salicylate and 5 mL of 6 M
NaOH. Heat the contents in a boiling water bath for 30 min. Record on the Report
Sheet what has happened to the ester layer (1).
2. Cool the test tube to room temperature by placing it in an ice water bath. Determine
the odor of the solution and record your observation on the Report Sheet (2).
3. Carefully add 6 M HCl to the solution, 1 mL at a time, until the solution is acidic.
After each addition, mix the contents and test the solution with litmus. When the
solution is acidic, what do you observe? What is the name of the compound formed?
Answer these questions on the Report Sheet (3).
V. POTENTIAL HAZARDS
H2SO4
- Very hazardous in case of skin contact (corrosive, irritant, permeator), of eye
contact (irritant, corrosive), of ingestion, of inhalation. Liquid or spray mist may
produce tissue damage particularly on mucous membranes of eyes, mouth and
respiratory tract.
- Wear chemical safety goggles, protective gloves, and clothing to prevent exposure.
REPORT SHEET
Carboxylic acids and their salts
Characteristics of Acetic Acid
HCl
Property Water Solution NaOH Solution
Solution
Odor
Solubility
pH
Odor
Solubility
pH
Esterification
Test Tube Acid Odor Alcohol Odor Ester Odor
1
2
3
4
5
6
REPORT SHEET
Saponification
1. What has happened to the ester layer?
II. INTRODUCTION
Carbohydrates are polyhydroxy aldehydes, ketones, or compounds that yield
polyhydroxy aldehydes or ketones upon hydrolysis. Rice, potatoes, bread, corn, candy, and
fruits are rich in carbohydrates. A carbohydrate can be classified as a monosaccharide
(glucose or fructose); a disaccharide (sucrose or lactose), which consists of two joined
monosaccharides; or a polysaccharide (starch or cellulose), which consists of thousands of
monosaccharide units linked together. Monosaccharides exist mostly as cyclic structures
containing hemiacetal (or hemiketal) groups. These structures in solutions are in equilibrium
with the corresponding open chain structures bearing aldehyde or ketone groups. Glucose,
blood sugar, is an example of a polyhydroxy aldehyde (Fig.11.1).
b. Ketoses (polyhydroxy ketones). All ketoses are reducing sugars because they have
a ketone functional group next to an alcohol functional group. The reactivity of
this specific ketone (also called α-hydroxyketone) is attributed to its ability to
form an α-hydroxyaldehyde in basic media according to the following equilibrium
equations:
V. POTENTIAL HAZARDS
NaOH
- Mucous membrane irritant. Skin: severe irritation, sensitization, dermatitis &
burns. Eyes: irritation, conjunctivitis & burns. Ingestion: damage to mucous
membranes or tissues.
- Wear protective gloves, and clothing to prevent exposure.
c. Lactose
2. Sucrose is a nonreducing sugar. After complete acid hydrolysis, will there be reducing
groups? How many per sucrose molecule?
3. When a reducing sugar reacts with Fehling’s reagent, what will be the product besides
Cu2O?
REPORT SHEET
Hydrolysis of Carbohydrates
Hydrolysis of sucrose (acid versus base catalysis)
Condition of Fehling’s reagent(positive or
Sample
hydrolysis negative)
1 Acidic (H2SO4)
2 Basic (NaOH)