İTÜ

KIM 101EL
GENERAL CHEMISTRY
LABORATORY
BOOKLET

FALL 2020-2021
 EXPERIMENT
Quantitative Preparation of Potassium
Chloride
Objectives
Compare the experimental
mass of a product of a chemical
reaction with the mass predicted
for that product by calculation.
Practice chemical stoichiometry.
1
A known mass of potassium
bicarbonate will be reacted with
excess hydrochloric acid. Knowing
the mass of KHCO3(aq) that reacts,
we can determine from the balanced
equation the mass of KCl that
should be produced. We can compare
this theoretical value with the
actual experimental mass of KCl
produced.

Introduction: Use the following stages in your

calculations:
The study of mass
relationships in chemical 1. Beginning with a balanced
reactions is called stoichiometry. chemical equation, use the number
All problems in stoichiometry of moles of a reactant consumed or
involve mole-mole conversions. product formed to determine the
Such calculations are needed to change in the number of moles of
determine both the quantities of any other reactant or product.
reactants that are required for a 2. Use molar mass to convert
chemical reaction, and the mass of a reactant or product to
theoretical yield of the reaction. moles for use in stoichiometric
calculations or to convert moles
In reactions, one reactant is from stoichiometric calculations
often used in excess in comparison to mass.
to the other. The excess reactant 3. Beginning with a balanced
will not react completely. The chemical equation, the mass of a
reactant that is not used in reactant consumed and the mass of
excess (it gets completely used up product actually produced,
in the reaction) is referred to as determine the percent yield for
the limiting reactant. The amount the reaction.
of product formed is dependent 4. Beginning with a balanced
upon the amount of limiting chemical equation and the initial
reactant present. masses of the reactants, determine
which reactant is limiting and
In this experiment, we will what the theoretical yield is for
investigate the quantitative each product.
relationships in the reaction:
 EXPERIMENT 1
APPARATUS thoroughly dry the bottom of the
dish.
- Evaporating dish
6. The following method of
- heater (hot plate)
drying the product must be
- graduated cylinder
followed to avoid spattering and
- water bath
loss of product. Pay attention
CHEMICALS during this procedure. Do not
- distilled water leave the drying setup unattended.
- potassium bicarbonate Heat the dish and contents for 5-
- 6 M HCl 10 minutes (the KCl should appear
dry).
SAFETY 7. Allow the product to cool at
room temperature in a dessicator,
Wear safety glasses at all and then weight it again. Repeat
times! the procedure up to constant
Wear gloves! weight.
Handle HCl carefully. It can 8. Determine the mass of KCl
cause painful burns if it produced from the data collected.
touches your skin!!!

References
1. M. Hein, J.N. Peisen, L.R.
PROCEDURE Best, R.L. Miner, “Foundations of
Chemistry in the Laboratory” 12th
1. Weigh a clean, dry Edition, 2007, John Wiley & Sons,
evaporating dish. Inc., USA.
2. Add between 2-3 g of
potassium bicarbonate to the
evaporating dish and reweigh.
3. Dissolve the potassium
bicarbonate in 5 mL of distilled
water. If all the potassium
bicarbonate does not completely
dissolve, do not worry about it.
Continue on with the next step.
4. In a graduated cylinder,
obtain 6.0 mL of 6 M HCl and
slowly, with stirring, add it to
the bicarbonate solution. (The
product is formed in this step).
5. Using a beaker of water to
make a water bath, evaporate the
liquid from the solution of
potassium chloride. Replenish the
water in the water bath as needed.
When the water has essentially
evaporated (the residue in the
dish looks dry), allow the system
to cool for a few minutes; remove
the evaporating dish and
 EXPERIMENT 1
Date:

Student’s Name and Surname:

Experiment’s Name:

Instructor’s Name and

Signiture:

REPORT 10. Theoretical moles of KCl ______

mol
I. Write the balanced equation for
the reaction between KHCO3 and
HCl:
11. Theoretical mass of KCl______ g
……………………………………………………………………………………….
12. Percentage error for experiment
al mass of KCl vs. theoretical
II. Experimental Data and
mass of KCl ______ %
Calculations:

1. Mass of empty evaporating dish

______ g

2. Mass of dish and dry KHCO3

______ g

3. Mass of dish and residue (KCl)

after first heating ______ g

4. Mass of dish and residue (KCl)

after second heating ______ g

5. Mass of dish and residue (KCl)

after third heating (if
necessary) ______ g

6. Mass of potassium bicarbonate

______ g

7. Moles of potassium bicarbonate

______ mol

8. Experimental mass of potassium

chloride obtained ______ g

9. Experimental moles of potassium

chloride obtained ______ mol Signature (Student)
 EXPERIMENT 2
Determination of hydration water in a
compound
b) Deliquescent substances:
Objectives They continue to absorb water from
the air and form a wet appearance
You will determine the ratio (a solution, indeed).
of hydration water as a
percentage and as a numerical c) Efflorescent substances:
value to the parent compound. They lose water molecules very
fast when exposed to the
atmosphere.
Here are some examples:
Introduction:
CaSO4 • 2H2O, Calcium sulfate
In this experiment, the percentage dihydrate
of water will be calculated.
CoCl2 • 6H2O, Cobalt (II) chloride
Background: hexahydrate
Hydrates have water molecules Na2CO3 • H2O, Sodium carbonate
embedded into the crystal monohydrate
structure. These water molecules
are bound very strongly and there Heating usually helps a hydrate
is a fixed amount of them being compound to lose water and being
present in a crystal, and commonly an anhydride:
known as water of hydration (or Hydrate  Anhydride + Water
water or crystallization). Crystal
CaSO4 • 2H2O  CaSO4(s) + 2H2O(g)
water are written in the formula
of the compound, and a central dot As there will be a considerable
is used to distinguish them from change between the initial and
the main compound. The number final weighings, the lost amount
designates the molar ratio of will correspond to the water
water per one mole of compound. leaving the compound and by
plugging into the following
Terminology:
formula, you can learn the
There are three different percentage of water:
behaviors of solid substances 𝐌𝐚𝐬𝐬 𝐨𝐟 𝐰𝐚𝐭𝐞𝐫 𝐥𝐨𝐬𝐭
related with the hydration- 𝐏𝐞𝐫𝐜𝐞𝐧𝐭𝐚𝐠𝐞 𝐨𝐟 𝐰𝐚𝐭𝐞𝐫 = × 𝟏𝟎𝟎
𝐌𝐚𝐬𝐬 𝐨𝐟 𝐢𝐧𝐢𝐭𝐢𝐚𝐥 𝐡𝐲𝐝𝐫𝐚𝐭𝐞
dehydration cycle:
Heating to constant mass is an
a) Hygroscopic substances: important technique which enables
These absorb moisture from the air you to be sure about all water has
and they can be used as drying left the compound. When two
agents (dessicants). An example consecutive weights are almost the
includes diphosphorus pentoxide same (limits of uncertainty of the
(P2O5). Almost all anhydrides are balance is generally ±0.02 grams),
hygroscopic. it means that the compound is
 EXPERIMENT 2
sufficiently dry with no water Materials Needed
molecules in the crystal at all.
Equipment Chemicals
Pyrex test tube, holder, iron ring, triangle, tongs, CuSO4 • 5H2O,
Crucible and cover or evaporating dish, cooling pad Unknown hydrate
heat the bottom of the test tube,
observe and make a record of all
the changes.
Wait a couple of minutes for the
test tube to cool down, add a few
drops of water and touch the
bottom of the test tube,
carefully. What have you observed?
Part B: Determination of the
percentage of water in a hydrate
compound
1. Again using copper(II)
sulfate pentahydrate, you
will try to find the
percentage of water this
time.
2. Obtain a clean and dry
crucible and record its
initial weight to 2 decimal
places. Then put about 1.5
grams of copper compound
into the crucible, and weigh
again.
3. Place the crucible on a clay
triangle (or a hotplate) and
heat gently for 5 minutes.
Then continue heating very
gently for 10 minutes.
4. Take the crucible and
preferably put inside a
dessicator, wait for it to
cool, and record the weight.
5. Repeat the procedure 3-4
again to obtain another
Experimental Procedure weight record.
6. If the dehydration step is
Part A: Qualitative test complete, two consecutive
Into a pyrex test tube, put some weight readings should be
copper (II) sulfate pentahydrate. ±0.02 g apart, which means
You don’t need to know the mass of that you don’t need to
hydrate in this part. By referring continue the heating/cooling
to the illustrations above, cycle anymore.
arrange the setup tilted upward 7. By using the above formula,
and its mouth must be away from calculate the percentage of
you and your companions. Gently water in your sample.
 EXPERIMENT 2
8. Calculate the empirical Safety and Waste Disposal
formula of your hydrate.
1. Safety: When using a Bunsen burner, it is imperative that you
obtain a blue-colored flame. Long hair should be tied back. Do not
weigh crucibles when hot; use cooling pads or dessicators to ensure
that they have completely cooled down. Do not handle hot crucibles
without crucible tongs, never touch them with your bare hands. The iron
ring and clay triangle are much hotter than the crucible, and it gets a
long time for them to cool. Wear goggles at all times.
2. Waste Disposal: Used compounds and anhydrides should be discarded
into waste containers.
 EXPERIMENT 2
EXPERIMENT 2: REPORT Name ____________________
Section ______________
DATA AND CALCULATIONS:
Part A: The behavior of a hydrate
Describe the appearance of the copper(II) sulfate pentahydrate, CuSO4 • H2O,
before heating.

Describe the appearance of the anhydride obtained by heating the hydrate.

(The anhydride is the residue.)

Describe the appearance of any other substances seen during heating, other
than the hydrate and anhydride.

Describe all changes observed when a few drops of water were added to the
anhydride.
 EXPERIMENT 2
Part B: Quantitative determination of percentage of water in an unknown
hydrate

Data: Unknown # = _____________

Mass of Crucible and Cover

Mass of Crucible, Cover, and Hydrate

Mass of Crucible, Cover, and Sample

After first heating

Mass of Crucible, Cover and Sample

After second heating

Mass of Crucible, Cover and Sample

After third heating, if necessary

Calculations: Show setups, with numerical values and units. Give answers to
the correct number of significant figures.

Calculate the mass of

the hydrate used.

Calculate the mass of

water lost by heating.
 EXPERIMENT 2
Calculate the
percentage of water in
the unknown hydrate.

Calculation of Empirical Formula.

Background: All ionic substances are represented by formulas which show the
simplest whole number ratio between the elements. The simplest formula is
also called the empirical formula. Given the percent composition of the
compound, an empirical formula can be calculated. In this experiment, we
treat the water molecules as single units rather than breaking them down into
H and O.

Example: Given the percent composition of hydrated zinc sulfate, as follows:

% (per 100 g) can be converted to mole ratios and then to simplest mole
ratio.

ZnSO4 56.15% / 161.45 = 0.3477 mole

0.3477 / 0.3477 = 1
(divide % by molar mass = 161.45)

H2O 43.85% / 18.01 = 2.435 mole

2.435 / 0.3477 = 7
(divide % by molar mass = 18.01)
Thus the formula of the hydrate is ZnSO4.7H2O

Experimental values for unknown # ______ (refer to previous page)

% water __________ % anhydride ___________

Show these to the instructor.
(experimental value ) (100 - % water)

The instructor will now give you the formula of the anhydrous portion of the
salt.

The % water in sample: _______________________ (from instructor)

Percent error for water: _______________________

Formula of anhydride: _______________________ (from instructor)

The complete empirical formula of the hydrated salt can now be calculated
(show set-up below similar to the ZnSO4 example above). Your sample is
probably not zinc sulfate, but some other compound.
 EXPERIMENT 2
Formula of the hydrated substance: _______________________________
Questions and Problems

How do you know that all of the water of hydration has been removed from your
unknown hydrate? Explain.

4.817 grams of an unknown hydrate are heated until all the water is removed.
The anhydride residue weighs 4.301 grams. Calculate the percentage of water
in this hydrate.

3. a) A student records the following data in the laboratory when determining

the percentage water in an unknown hydrate. What is the percentage water in
this student’s unknown?

Mass of container = 78.311 g

Mass of container and hydrate = 81.055 g
Mass of container and contents after:
First heating = 80.899 g
Second heating = 80.137 g
Third heating = 79.999 g

b) Based on the values obtained in the three heatings above, do you

think the student should have confidence in his results? Why? What do you
think the student should do to be more confident in his result?
 EXPERIMENT
Determination of Sodium Hypochlorite
Levels in Bleach
Objectives
Determination of amount of sodium
hypochlorite (OCl-) in bleach by
redox titration.
Redox reactions, or oxidation-
reduction reactions, primarily
involve the transfer of electrons
between two chemical species. The
compound that loses an electron is
said to be oxidized, the one that
gains an electron is said to be
reduced. There are also specific
terms that describe the specific
chemical species. A compound that
is oxidized is referred to as a
reducing agent, while a compound
that is reduced is referred to as
the oxidizing agent.
Household bleach is a solution of
sodium hypochlorite (NaOCl) and
water. It is widely used as a
disinfectant and in the bleaching
of textiles and paper.
In order to determine the amount
of bleach in each bottle, a redox
titration will be performed. This
redox titration is similar to an
acid-base titration a reagent of
known concentration is added to
the unknown until a color change
occurs. In this redox equation,
the color change is from brown-
yellow (I2) to colorless (I-).
The buret in the titration will be
filled with Na2S2O3 and will act as
a reducing agent.
3
When the S2O32- ion reacts with the
I2 in the flask, I- is formed. When
all of the I2 reacts, the solution
becomes clear.
I2(brown) + 2S2O32- ------> S4O62- + 2I-
(clear) (1)
Reacting the bleach directly
with the S2O3 -2 solution would
result in reduction of the OCl-
to Cl- according to equation 2.
As you can see, both
OCl-(faint yellow) + 2S2O32-colorless) -
--->
Cl-(colorless) + S4O62-(colorless)
(2)
solutions are mostly colorless. It
would be difficult to see the
transition from faint yellow to
colorless. For this reason, the
bleach solution is added to an I -
solution (equation 3)
OCl- + 2I-(clear) ----> I2(brown) + Cl-
(3)
1.00 mole of bleach results in
the formation of 1.00 moles of
I2. According to equation 1,
0.500 moles of I2 then reacts
with 2.00 mole of S2O32-. The
result is that for 1.00 mole of
OCl- in the flask, 2.00 moles of
S2O32- are required to reach the
endpoint.
 EXPERIMENT 3
APPARATUS REPORT
- Erlenmayer
- Pipette
- Graduated cylinder (1) Record the volume of the
- Burette buret at the endpoint.
(2) Subtract the initial volume
CHEMICALS from the final volume to
Two types of bleach (one normal determine the volume of Na2S2O3
and one ‘concentrated”) used
•An acidic I- solution prepared (3) Using the concentration of
from 6.3 g of NaI (or 7.0 g of KI) the Na2S2O3 (given by your
and 20 mL glacial acetic acid instructor), determine the
diluted to 1L with water number of moles of S2O3 used.
2-

•A 0.100 M solution of Na2S2O3 (4) Determine the number of

SAFETY
 Wear your safety googles.
 Be cautions when working
with concentrated acid!
 Wear gloves!
PROCEDURE
To begin the titration, fill
the clean buret with the Na2S2O3
solution. Add 50 mL of the
acid/I- solution to a 125 mL
Erlenmeyer flask or 250 mL
beaker. Add 1.0 mL of your
bleach to flask as well. When
the bleach is added, the
solution should turn brown.
Record the initial volume of
the S2O32- in the buret. Slowly
add the S2O32- solution to the
bleach in the flask or beaker.
Do not add the solution too
quickly. The color of the
iodine will get lighter and
lighter. You will need to add
the solution dropwise as the
solution becomes very light.
You should see the color
completely disappear in one
drop.
moles of NaOCl that were in the
flask or beaker
(5) Using the volume of bleach
you added to the flask or
beaker, determine the
concentration of the NaOCl in
the bleach.
Calculation.
The volume of S2O32- solution
(spent in the reaction) is:
V(as liter)
Molarity of S2O32- is: M
Moles of OCl- : (V x M) /2
1 mL NaOCl solution was
initially added
Concentration of the NaOCl
solution as molarity:
[(V x M) / 2] / 0.001
Signature (Student)
 EXPERIMENT
Lewis Structures and VSEPR Theory
Objectives
In this experiment you will
investigate the Lewis structures
of some assigned molecules and
construct their molecular shapes
using Valence Shell Electron Pair
Repulsion (VSEPR) Theory with the
molecular model kits.
Lewis Structures and Formal
Charge:
Although it has recently become
possible to image molecules and
even atoms using a high-
resolution microscope, most of our
information about molecular
structure comes from often this
information enables us to piece
together a 3-dimensional picture
of the molecule. Sketching on
paper, one of the best methods we
have of representing this model is
by drawing a Lewis Dot Structure
of the molecule or ion.
In 1916, L.G.N. Lewis, at the
University of California at
Berkeley, devised a simple way to
understand the nature of the
chemical bond in both ionic and
molecular compounds. His method
rests upon focusing on the valence
electrons, i.e. on the electrons
in the outermost energy level of
an atom or ion. He represents
these valence electrons as "dots"
around the four sides of the
elemental symbol as shown in the
figure below.
4
Lewis structures of molecules or
ionic species are representations
showing all electrons (bonding and
nonbonding) of the each element of
the compound. The bonding or
shared electron pairs are shown
either as lines or pair of dots
between two atoms. The nonbonding
or lone pairs are shown as pair of
dots on individual atoms. Atoms,
other than hydrogen, tend to gain
or lose, or share electrons until
it is surrounded by eight valence
electrons satisfying the rule
called OCTET RULE. This is the
electron arrangement corresponding
to the configuration of a noble
gas (ns2np6). Here are the rules to
write the Lewis structures
For ionic or molecular compounds:
1. Draw skeletal structure of
compound showing what atoms are
bonded to each other.
2. Put the least electronegative
element in the center (H and F are
usually in terminal positions).
3. Count total number of valence
e- and add 1 e- for each negative
charge or subtract 1 e- for each
positive charge.
4. Draw single covalent bonds (2
electrons) between all the atoms
and complete an octet for all
atoms except for the central atom.
 EXPERIMENT 4
5. Complete an octet for the For example:
central atom and, if the octet
rule is not satisfied, add
multiple bonds on central atom as
needed (see below for some
examples).

Sometimes we can write more than
one Lewis structure for certain
molecules or polyatomic ions. It
is possible to determine the
correct Lewis structures using the
concept of formal charge. The
formal charge of an atom is the
charge that an atom (in a less than eight electrons (BF 3) or
molecule) would have if all of the
atoms had the same
electronegativity and is
calculated using the following
equation:
Formal Charge = (# of valence e -)–
(# of non bonding e-)–½(# of
bonding e-)
So the best Lewis structure is the
one with the fewest formal charges
and that puts a negative charge on
the most electronegative atom.
Exceptions to Octet Rule and Lewis
Dot Structure
There are compounds that cannot be
represented by these rules (octet
rules) for Lewis dot structures.
The central atom may have either
more than eight electrons (PCl 5,
SF6, XeF4, etc). For most of these
compounds, the central atom and
each outer atom are bonded by
single bonds consisting of one
pair of electron. If there are any
extra electrons on the central
atom, they are grouped as shared
pairs on the central atom. For
example:
 EXPERIMENT 4
BF3= 1(3e-) + 3(7 e-) = 24 e-= 12 Thus all hetero-nuclear diatomic
pair e- molecules are polar. The greater
the electronegativity differences
of the atoms, the greater the
distortion of the electron
density, thus, the more polar is
the molecule.

The direction and magnitude of the

PCl5= 1(5 e-)+5( 7 e-)= 40 e-= 20
pair e-
polarity are represented by a
vector, drawn in the direction of
the greater electron density; the
δ+ center of the molecule is
indicated by a plus sign on the
tail of the vector. For example,
the HF molecule is more polar than
the HCl molecule because the
fluorine atom is more
electronegative than the chlorine;
both are more electronegative than
the hydrogen atom. Therefore, the
δ+ is on the hydrogen; the vector
is drawn in the direction of the
fluorine and chlorine.

Polarity of Molecules or Ions If more than one polar bond exists

in a molecule, the entire molecule
Once the three-dimensional shape may be polar or nonpolar,
of a molecule is determined, its depending on the geometry of the
polarity can be qualitatively molecule since the polarity from
understood. A molecule is polar one bond may be cancelled by the
if an unsymmetrical distribution polarity of another. Consider BF 3
of electrons exists in the and OF2. The BF3 molecule has a
molecule resulting in a partial VSEPR formula of AX3, where each
separation of charges. An B-F bond is polar.
unsymmetrical distribution of
charge occurs when bonded atoms Table 1 shows that the BF3
have different molecule has a trigonal planar
electronegativities; the atoms geometry. The three more
having a higher electronegativity electronegative fluorine atoms
(electronegativity increases as attract the bonding electron pairs
you move up and to the right in from the boron atom with equal
the periodic table) more strongly magnitude, which is all dipoles
attract bonding electrons, are cancelled.
acquiring a greater electron
density and a partial negative
charge, δ-, relative to another
portion of the molecule, δ +.
 EXPERIMENT 4
Polarity of bonds in BF3 The OF2 molecule has the VSEPR
formula AX2E2 and each O-F bond is
polar. Table 1 shows that OF 2 has
a V-shaped geometry. The
geometric sum of the magnitude
(all the same) and direction of
the two vectors produces a
resultant vector that is not equal
A geometric sum of the magnitude
to zero. A resultant vector can
(all the same) and direction of
be drawn indicating a δ+ and δ-
the three vectors equals zero.
electron density in the molecule.
Because in the BF3 molecule there
In such cases the molecule is
is no resultant vector that can be
polar; therefore, OF2 is a polar
drawn to indicate a resultant δ +
molecule.
or δ- electron density in the
molecule, it is said to be a
nonpolar molecule, even though Experimentally, polar molecules
each B-F bond is polar. are attracted to an electric
field; nonpolar molecules are not.
 EXPERIMENT
In an experiment using an
electrostatically charged rod, a
polar liquid, such as water,
flowing near an electrically
charged rod, is deflected slightly
whereas a nonpolar liquid, such as
benzene, is unaffected by the
electric charge.
Although the conclusions we have
drawn regarding molecular geometry
and polarity can be obtained from
Lewis structures, it is much
easier to draw such conclusions
from models of molecules and ions.
The rules we have cited for octet
rule structures transfer readily
to models. In many ways the
models are easier to construct
than are the drawings of Lewis
structures on paper. In addition,
the models are three-dimensional
and hence much more representative
of the actual species.
Using the models, it is relatively
easy to see both geometry and
polarity, as well as to deduce
Lewis structures.
VSEPR and Hybridization Theory
Lewis structure provides only the
position of the atoms within the
molecule, the number or bonding
and nonbonding electrons and the
type of bonds. Valence Shell
Electron Pair Repulsion model
(VSEPR) provides a method to
predict the shape of most
compounds. The theory works on the
principle that electron pairs in
the valence shell repel each other
and thus will remain as far from
each other as possible.
The rules of this model are laid
out in Table 2 above, with E
representing a central atom and X
representing bonded atoms. Notice
4
that the bonded atoms will attempt
to fill the empty 3D space around
a central atom evenly. As lone
pairs of electrons are introduced,
the electron pairs will repel the
atoms. If more than one lone pair
is present the lone pairs will
repel each other first, and the
overall shape of the molecule is
governed by the number of lone
pairs. The bonded atoms will
evenly fill up the molecule
wherever they may reach an
equilibrium of repulsion between
the lone pairs.
Let’s finally discuss how the the
bonds between the atoms are formed
so that the molecules can assume
the shape described in the VSEPR
theory. Hybridization is a process
in which atomic orbitals are mixed
to form new identical orbitals and
is useful in the explanation of
the shape of both ionic species
and molecules. The concept of
hybridization is an integral part
of valence bond theory. In the
valence bond theory the bonds are
assumed to be formed by overlap of
atomic orbitals and the shared
region in space between orbitals
is the orbital overlap. There are
two e- (one from each atom) with
opposite spin in the orbital
overlap. Linus Pauling first
developed the hybridization theory
in order to explain the structure
of molecules such as methane
(CH4). The hybrids are named based
on the atomic orbitals that are
involved in the hybridization, and
the geometries of the hybrids are
also reflective of those of the
atomic-orbital contributors. For
example, in the methane (CH4) a
set of sp3 orbitals are formed by
mixing one s and three p orbitals
on the carbon atom, and are
directed towards the four hydrogen
 EXPERIMENT 4
atoms which are located at the represents the central atom and B
vertices of a regular tetrahedron the electron domains surrounding
as shown in the scheme below: the central atom:

Here are listed the steps

necessary to predict the Class Hybrid. Electron Domain Geometry
hybridization of the central atom; AB2 sp linear
2
a. Draw a Lewis structure AB3 sp trigonal planar
AB4 sp3 tetrahedral
b. Count the number of bonding AB5 sp3 d trigonal bipyramidal
pairs and the number of nonbonding sp3 d2
AB6 octahedral
pairs

c. Assign the electron-domain During the lab period, you will

geometry using VSEPR theory determine the VSEPR geometry of
each species, the hybridization of
d. Specify the hybridization the central atom, and the overall
required to accommodate the dipole moment and when possible,
bonding and nonbonding electron its orientation within the
pairs based on their geometric molecule or ion listed in the
arrangement according to the worksheet. Visualizing these
following table (Where A shapes is not always easy, and 3D
models can help in this aspect. In
the lab, you will be provided with
 EXPERIMENT 4
molecular modeling sets to build 3.Dakota State University General
the molecules. Chemistry Laboratory Manual.
PROCEDURE 4.College of Alameda General
Chemistry Laboratory Manual.
You will be asked to determine the
Lewis structures of any ten
molecular particles from the list
of molecular species (see below),
the molecular shapes around each
central atom of the molecular
structure, and construct 3-
dimensional models of the
structures using the molecular
model kit, Table of molecular
shapes, and Fig 1 with 3-D
drawings of all possible molecular
shapes. You will also be asked to
draw 3-D schemes of these
molecular structures. All this
work has to be done in the
worksheets provided below. The lab
report is due at the end of the
laboratory period.

References

1.General Chemistry, Principles

and Modern Applications, Ralph H.
Petrucci [et al.] 10th ed., 2011
Pearson Canada Inc., Toronto,
Ontario.

2.Inorganic Chemistry, D.F.

Shiver, P.W. Atkins, 3th ed., 1999,
Oxford University Press, Oxford.
 EXPERIMENT 4
Date:

Student’s Name and Surname:

Experiment’s Name:

Instructor’s Name and

Signiture:

You will be asked to determine the Lewis structures of any ten molecular
particles from the list of molecular species (see below), the molecular
shapes around each central atom of the molecular structure, and construct 3-
dimensional models of the structures using the molecular model kit
 EXPERIMENT 4
Molecule Lewis Structure Data Sketch of the 3-D
Bonding orbitals or pairs 4
Non-bonding orbitals or pairs 0
1) CF4 Hybridization sp3
VSEPR formula AX4
Geometry Tetrahedral
Polar or nonpolar Non-polar
Bonding orbitals or pairs
Non-bonding orbitals or pairs
2) CF3Cl Hybridization
VSEPR formula
Geometry
Polar or nonpolar
Bonding orbitals or pairs
Non-bonding orbitals or pairs
3) H2O Hybridization
VSEPR formula
Geometry
Polar or nonpolar
Bonding orbitals or pairs

Non-bonding orbitals or pairs

4) HNO3 Hybridization
VSEPR formula
Geometry
Polar or nonpolar

Bonding orbitals or pairs

Non-bonding orbitals or pairs
5) NH3 Hybridization
VSEPR formula
Geometry
Polar or nonpolar
 EXPERIMENT 4
Bonding orbitals or pairs
Non-bonding orbitals or pairs
6) C2H6 Hybridization
VSEPR formula
Geometry
Polar or nonpolar
Bonding orbitals or pairs
Non-bonding orbitals or pairs
7) XeF4 Hybridization
VSEPR formula
Geometry
Polar or nonpolar
Bonding orbitals or pairs

Non-bonding orbitals or pairs

8) NO2- Hybridization
VSEPR formula
Geometry
Polar or nonpolar

Bonding orbitals or pairs

Non-bonding orbitals or pairs
9) PCl5 Hybridization
VSEPR formula
Geometry
Polar or nonpolar
Bonding orbitals or pairs
Non-bonding orbitals or pairs
10) SF2 Hybridization
VSEPR formula
Geometry
Polar or nonpolar
Signature (Student)
 EXPERIMENT
Synthesis of Soap
Objectives
To observe the process of
saponification.
Today in lab, you will make soap
using vegetable oil. Vegatable
oils are tri-esters of glycerol.
Soaps are carboxylate salts with
very long hydrocarbon chains.
Soaps can be made from the base
hydrolysis of a fat or vegatable
oil. Fat molecules are made up of
fatty acids and glycerol, held
together by ester linkage. A
saponification reaction occurs
when a base is used to catalyze
the breaking or hydrolysis of
ester link.
5
surround an oil droplet so that
their non-polar tails are embedded
in the oil and their charged
“polar tail” groups are on the
exterior of the droplets, facing
the water. If the oil droplets are
small enough and if there are
enough soap molecules to surround
them, the oil droplets become
dispersed in the water and can
then easily be washed away.
Soaps are less effective in hard
water, which is water that
contains a significant
concentration of Mg2+, and Ca2+
ions. These ions form precipitates
with soap molecules, and this
precipitate is often seen as a
gray line on a sink.
Detergents are similar to soaps in
that they have a charged head
group and a long non-polar tail
group, but they are not prepared
from fats or oils.
APPARATUS FOR SAPONIFICATION
- 600 mL beaker
- 50 mL test tube
- magnet

Chemicals for Saponification

-Olive oil
-95% Ethanol
-6M NaOH solution
-NaCl solution

SAFETY
Wear your safety googles.
NaOH can cause permanent
eye damage!!!
Soap can emulsify fats and oils by
forming miscelles around oil Wear gloves!
droplets. The soap molecules
 EXPERIMENT 5
Watch your reaction mixture References
at all times as it is 1. M. Koscho,
heating. Do not turn back http://greenchem.uoregon.edu/PDFs/Reso
urceID51.pdf
to system!!
2.www.chem.latech.edu/~deddy/chem122m/
The soap mix is highly L06U00Soap122.htm
alkaline (basic) and will 3.
www.laney.edu/wp/chelifossum/files/201
burn your skin if you touch 2/01/13-Saponification.pdf
it before the
saponification reaction is
complete.

-SAPONIFICATION REACTION
1. Fill a 600 mL beaker with water
and heat to boiling on a hot plate
2. While your water bath is
heating, clean a large test tube
and rinse with deionized water.
3. To your test tube add 5 g of
olive oil and 10 mL of 95%
ethanol.
4. Place your test tube in your
boiling water bath.
5. Slowly add 8 mL of 6M NaOH to
your solution.
6. Stir and keep hot for 15
minutes.
7. During the boiling, add 95%
ethanol peridiocally to replace
the ethanol that has boiled off.
8. Remove test tube and allow the
solution to cool at room
temperature.
9. Add 25 mL of saturated NaCl
solution.
10. Thoroughly mix the contents of
your test tube and cool in an ice-
bath for 10 minutes. Your soap
should now precipitated out of
solution.
11. Vacuum filter your solution to
isolate the solid soap.
 EXPERIMENT 5
Date:

Student’s Name and Surname:

Experiment’s Name:

Instructor’s Name and

Signiture:

REPORT b) Mix 20 drops of pink liquid lab

soap with 50 mL of deionized
1. Describe your crude product. Do
water. Swir this solution to mix
you expect it to be pure soap? Why
it well.
or why not?
pH TEST
Label 3 separate test tube. In the
first tube, place 10 mL of the
soap solution you made it. In the
second tube, place 10 mL of
commercial soap solution. In the
2. Why are sufficient base, heat third tube, place 10 mL of
and time important in the deionized water.
saponification reaction?
One by one, stir each solution
with glass rod and then touch the
pH paper to the solution.
1.tube pH =
2.tube pH =
3.tube pH =

3. Why is only a catalytic amount Foam Test

of NaOH used in the biodiesel
reaction? What would happen if a
full equivalent of NaOH were
added?
Stopper each of tubes from pH test
and shake each one continously for
10 seconds. Observe tubes.
1.tube

2.tube

3.tube

4. Properties of Soap
a) Mix 1 g of soap you prepared
with 50 mL of warm deionized Signature(Student)
water. Swirl solution to mix it
well. (but try not to shake it)
 EXPERIMENT 6
Determination and Removal of Hardness
of Water
necessary for cleaning. Soap used
Objectives in hard water combines with the
minerals to form a sticky soap
The concentration of certain curd. Some synthetic detergents
dissolved ions such as calcium, are less effective in hard water
magnesium ions that make water hard because the active ingredient
will be determined by using EDTA is partially inactivated by
titration and soap solution. hardness, even though it stays
The removal of hardness of dissolved. Bathing with soap
water by boiling and chemical in hard water leaves a film
method will be compared to get the of sticky soap curd on the
idea of removal efficiency. skin. The film may prevent removal
of dirt and bacteria. Soap curd
interferes with the return of skin
The water containing one or more to its normal, slightly acid
soluble salts of earth alkaly condition, and may lead to
metals (Mg2+, Ca2+, Ba2+, Sr2+), irritation. Soap curd on hair may
earth metals (Al3+, Ga3+), some make it dull, lifeless and
transition metals (Fe3+, Mn2+) or difficult to manage.
some anions (SO42-, CO32-, PO43-,
SiO32-, NO3-, NO2- , HCO3-, Cl-) is However, hard water is not a
called as hard water. health hazard. People regularly
take calcium supplements. Drinking
Why Be Concerned About Hard Water? hard water contributes a small
The determination of water amount of calcium and magnesium
hardness is a useful test that toward the total human dietary
provides a measure of quality of needs of calcium and magnesium.
water for households and Type of Hardness
industrial uses. When hard water
is heated, CaCO3 precipitates out; There are two types of hardness,
this then clogs pipes and temporary and permanent.
industrial boilers. This leads to 1. Temporary Hardness
malfunction or damage and is
expensive to remove. Temporary Hardness is due to the
bicarbonate ion, HCO3-, being
On the other hand, hard water present in the water. This type of
interferes with almost every hardness can be removed by boiling
cleaning task from laundering and the water to expel the CO2, as
dishwashing to bathing and indicated by the following
personal grooming. Clothes equation:
laundered in hard water may look
dingy and feel harsh and scratchy.
Dealing with hard water problems
in the home can be a nuisance. In
addition, hard water affects the
amount of soap and detergent
 EXPERIMENT
2. Permanent hardness
2+ 2+
Water soluble salts of Mg , Ca ,
Ba2+, Fe3+, Al3+, Mn2+ cations and
sulphate (SO42-),carbonate (CO32-),
phosphate (PO43-), SiO32-,nitrate
- -
(NO3 ), nitrite (NO2 ), chloride
(Cl-) anions cause temporary
hardness which cannot be removed
despite prolonged boiling.
Total hardness is the sum of the
temporary and permanent hardness.
Degree of the Hardness
French degree of hardness is equal
to 10 mg CaCO3 dissolved in 1
liter of water, or the amount of
hardness causing compunds which is
equivalent to the amount of gram
of CaCO3 dissolved in 100 liter of
water is called as French degree
of hardness (Fr0).
How hard is the water?
The hardness of the water is
classified in terms of French
degrees (Fr0) as follows:
6
b) Using a soap solution of
potassium palmitate (C16H31-COOH).
c) Titrating with the EDTA
(Ethylenediaminetetraaceticacid)
solution. In this titration, a
buffer (NH4Cl-NH4OH) is added to
change the water to the
appropriate pH, then EDTA is
slowly added to the sample water.
EDTA reacts with Ca2+ and Mg2+ in
the water, removing them from
solution. When all of the Ca2+ and
Mg2+ have been used up, the
indicator changes color and you
can calculate the amount of
hardness that was present in the
sample water.
EDTA has a greater affinity for
Ca2+ and Mg2+ when it is in the form
of the dihydrogen anion H 2EDTA2-.
This is the ionic form of EDTA at
pH 10. H2EDTA2- binds to a Ca2+ ion
by forming four special covalent
bonds called coordinate covalent
bonds.

Table 1. Classification of
hardness of water*
Hardness French degrees
rating (Fr0) + + 2H+
Very soft 0 to <7 Ca2+

Soft 7 to <14 Ca2+ ion

H2EDTA2-
Medium hard 14 to <22 chelated
by EDTA
Moderately hard 22 to <32
Fig.1 The formation of Ca2+ complex
Hard 32 to <42 with EDTA.
Very hard 42 and greater
*According to the Turkish Food Codex. APPARATUS
Hardness determined by -Burette
-Erlenmayer
a) The analysis of the ions -Beaker
causing hardness is done to -Hydrometer bottle
determine their amounts in -Glass-rod
solution.
 EXPERIMENT 6
CHEMICALS
-%5 NaOH solution 1 2
-%5 Na2CO3 solution
-NH4Cl-NH4OH buffer solution
-EDTA solution
-A sample of hard water
-Eriochrome Black T indicator
3 4
SAFETY

The pH 10 buffer is toxic

and gives off toxic vapors!
Handle it carefully and
always keep it in the hood.
Fig.2 EDTA endpoint color change.
Eriochrome Black T will
stain skin and clothes!
Record the volume of EDTA solution
and calculate the amount of
PROCEDURE
hardness (as ppm CaCO3) in the
water using the following
Determination of hardness of water
equations:
1. Titration with EDTA solution
Take 50-100 mL of hard water
sample and add 5 mL of (pH=10)
buffer solution and 5 drops of
liquid indicator or 20 mg of solid
indicator. Stir and titrate the
solution with EDTA from your
buret. As you near the endpoint,
the solution will turn purple.
Continue to slowly add EDTA until
the solution turns blue, with no
trace of red.
The color change from 1 to 4 (Fig. Fr0 = French degree of hardness
2) is due to the compact nature of ppm = parts per million
the complex. The statement "the
compact nature of the complex" 2. Using a soap solution
means when the indicator is added
to the hard water, the indicator Pour 40 mL of sample of hard water
Erio-T forms a complex with the into the hydrometer bottle and
Ca+2 ions that is pink in color. As shake it. Add soap solution until
EDTA is added to the solution, the suds persist for 5 minutes in
EDTA forms a complex with the thickness of 1 cm. Consumption in
Ca+2 leaving the indicator Erio-T the hydrometer burette gives
uncomplexed, which is blue in French degree of hardness.
color.
 EXPERIMENT 6
Removal of hardness of water

1. By chemical method

Take 100 mL of hard water anda a

10 mL of %5 NaOH and 10 mL of %5
Na2CO3. Stir it. Wait about 10-15
minutes until it precipitates.
Filter it. Take 10 mL from the
solution put into the hydrometer
bottle and dilute with distilled
water up to 40 mL. Repeat the same
procedure.
2. By boiling

Take 100 mL of hard water and put

into the erlenmayer. Boil the
water for about 10-15 minutes
until 1/3 of it evaporates. Then
filter and cool it. The volume of
the filtered solution is brought
up to 100 mL by adding distilled
water. Take 10 mL of it and dilute
to 40 mL. Determine its hardness.
The hardness of this type is
permanent hardness.

References
1. Water Hardness: Determination
with EDTA, General Chemistry
Laboratory Manual, University of North
Carolina at Wilmington.
2. D. Spurlock, Determination of
Water Hardness by Complexometric
Titration Class Notes, Indiana
University Southeast.
3. D. Dey, A. Herzog, V.
Srinivasan, Chemical Precipitation:
Water Softening, Michigan State
University, 2007.
 EXPERIMENT 6
Date:

Student’s Name and Surname:

Experiment’s Name:

Instructor’s Name and

Signiture:

REPORT 3. Write the chemical reactions to

explain how hardness is removed by
1. Which ions are responsible from
chemical method and boiling.
the total hardness? Write the
chemical formulas. State which
ones are causing temporary
hardness.
Total hardness:

Temporary hardness:

2. Calculate the hardness of

4. Report the degree of hardness
sample water in terms of French
(Fr0) of water after boiling and
degrees.
chemical method.

mol CaCO3 =.......................

After boiling = ...............Fr0

MCaCO3 =.......................... After chemical method =........Fr0

ppm CaCO3 =.......................

Signature (Student)
=..............................Fr0
 EXPERIMENT
Determination of Acetic Acid Content
of Vinegar: An Acid-Base Titration
Objectives
To determine the molarity
and percent by mass of acetic acid
in a commercial vinegar by
volumetric analysis.
The method used to measure the
total acidity of the vinegar being
studied is an analytical chemistry
technique called an acid-base
titration. A titration mixes two
solutions which contain reactants
for a known chemical reaction
under conditions such that:
a) the point at which both
reactants have been completely
consumed by the known reaction can
be detected (end point),
b) the amount of one reactant can
be calculated from the known
concentration of reactant in a
standard solution, the volume of
standard solution used, and the
balanced known chemical equation.
For an acid-base titration, the
known chemical reaction in general
is:
acid+basewater+salt (1)
and for the titration of the
vinegar in this experiment the
following specific reaction will
be used to calculate the acetic
acid content of the vinegar
sample:
CH3COOH(aq) + NaOH(aq)  H2O(l) +
CH3COONa(aq) (2)
Sodium hydroxide will be the
standard reactant solution for
7
this titration, and acetic acid
the calculated unknown reactant.
The end point in this experiment
will be detected with an acid/base
indicator. An acid/base indicator
is a colored substance with two or
more different colors depending on
the value of the pH of the
solution. Indicators are also very
weak acids or bases and react with
added acid or base if no other
base or acid is present in a
solution. Phenolphthalein is the
indicator used in this experiment,
and phenolphthalein is colorless
in acid and neutral solutions but
is red in basic solutions. The
phenolphthalein will change color
with the addition of a single drop
of sodium hydroxide if no other
acid (acetic acid for this
experiment) is present in the
phenolphthalein - sodium hydroxide
solution.
Concentration refers to the
composition of a solution and can
be expressed as the ratio of
solute / solution.
Molarity (M) = moles of solute /
liters of solution (3)
% by mass = (mass of solute / mass
of solution) 100% (4)
Molarity is a convenient
laboratory unit (Eq. (3)) that
delivers for a measured the volume
of solution a known number of
solute molecules (i.e. moles of
solute). Percent is a familiar
concept to most people and for
this reason percent by mass (Eq.
(4)) is used on many labels. Both
 EXPERIMENT 7
of these units will be used in PROCEDURE
this experiment.
APPARATUS 1. Pipette 5 mL of the
concentrated vinegar sample and
-50 mL burette
the dilute to 250 mL in a
-5 mL volumetric pipet
volumetric flask.
-Pipette bulb
-Erlenmeyer flask (250 or 125 mL) 2. Pipette 50 mL of the diluted
-Wash bottle with distilled water sample solution into 250 mL
erlenmeyer flask.
CHEMICALS
3. Dilute with distilled water
-Standard solution of NaOH(~0.1 M)
to about 50 mL.
-Phenolphthalein indicator
-Vinegar 4. Add 2-3 drops of
phenolphthalein.
5. Titrate with 0.1 M NaOH
solution till the first color
Initial Reading change.
Burette clamp 6. Reading of the burette is
Burette
taken before and at the end of the
titration volume. Record value in
the following data table.

Final reading
Trial Trial Trial
NaOH (aq) 1 2 3
known
concentration
Final buret
Stand 5.00 mL vinegar reading
50 mL H2O (mL)
2-3 drops
phenolphthatelin Initial
buret
reading
(mL)
Volume of
NaOH needed
Fig. 1 Experimental set-up. to reach
end point
(mL)

SAFETY References
1. W. Scharf, C. Malerich,
Be especially careful when Determination of Acetic Acid Content
handling the sodium of Vinegar, Natural Sciences, Baruch
hydroxide base (NaOH), as it College, New York, NY 10010.
is corrosive!!! and can
cause chemical burns to the
skin. If any NaOH spills on
you, rinse immediately under
running water.
 EXPERIMENT 7
Date:

Student’s Name and Surname:

Experiment’s Name:

Instructor’s Name and

Signature:

REPORT
4. Convert the moles of CH3COOH
in the vinegar sample (previously
1. First, using the known molarity calculated) to a mass of CH 3COOH,
of the NaOH(aq) and the volume of via its molar mass.
NaOH(aq) required to reach the
equivalence point, calculate the
moles of NaOH used in the
titration. ………………………………………………………………………………………
Note: Ma(CH3COOH) : 60 g/mol
Dilution factor:(250 mL/50 mL = 5 for this
titration).

5. Then determine the total

……………………………………………………………………………………….
mass of the vinegar sample from
the vinegar volume and the vinegar
2. From this mole value (of
density. Assume that the vinegar
NaOH), obtain the moles of CH 3COOH
density is 1.000 g/mL (= to the
in the vinegar sample, using the
density of water).
mole-to-mole ratio in the balanced
according to the Eq. (2).

…………………………………………………………………………………….

6. Finally, calculate the mass

………………………………………………………………………………………. percent of acetic acid in vinegar
from the mass of CH3COOH and the
3. Finally, calculate the mass of vinegar.
molarity of acetic acid in vinegar
from the moles of CH3COOH and the
volume of the vinegar sample used.

……………………………………………………………………………………….
Hint: Molarity = Moles of Acetic Acid /
Volume of Vinegar (in L)
………………………………………………………………………………….
Hint: Mass % = [Mass of Acetic Acid / Mass
of Vinegar] x 100
Signature (Student)
 EXPERIMENT 8
Thermochemistry: Determination of the
Heat Reaction
Objectives concerned with changes in state or
To determine the energy changes solvation of molecules or ions.
accompanying neutralization 4. The enthalpy of
reaction by using a calorimeter. neutralization is the heat evolved
when 1 mole of water is produced
by the reaction of an acid and
base.
Thermochemistry concerns the
energy changes that are manifested
as the enthalpy change APPARATUS
of reaction, ∆H that is the heat -polystyrene cup
given off or absorbed by the -rubber stopper
reaction at constant pressure. A -thermometer
reaction in which heat is lost by -beaker
the reactants to the surroundings -graduated cylinder
has a negative ∆H and is said to
be exothermic; one in which heat
CHEMICALS
is absorbed has a positive ∆H and
is said to be endothermic.
-1.0 M NaOH
The general term, enthalpy of -1.0 M HCl
reaction, may be classified into
more specific categories:
1. The enthalpy of formation
is the quantity of heat involved
in the formation of 1 mole of the
substance in its standard state
directly from its constituent
elements in their standard states.
2. The enthalpy of
combustion is the quantity of heat
evolved per mole of a combustible
substance, such as carbon or
methane, undergoing a reaction
with excess oxygen.
3. The enthalpies of
solution, vaporization, fusion,
and sublimation are
 EXPERIMENT 8

Calculation
PROCEDURE
Mass of solution:
Place 50.0 mL of 1.0 M HCl in m = 100 mL x 1.02 g/mL = 102 g
one calorimeter. With the lids and
thermometers in place, read the Heat gained by solution, q soln = m C
temperature. Then, quickly mix ∆T
50.0 mL of 1.0 M NaOH thoroughly
into the HCl solution, and 100 g x 4.00 J g–1 °C–1 x ∆T o
C =
continue the readings for 2 min at ….J
15 sec intervals. Calculate the
enthalpy of neutralization per Heat of reaction:
mole of water produced. (The qrxn = - qsoln
density of the 0.5 M NaCl produced
is 1.02 g/mL, and its specific Moles of HCl = moles of NaOH =
heat is 4.00 J g–1 °C–1.) moles of H2O = 0.05 L x 1.0 M =
0.05 moles

NaOH + HCl → NaCl + H 2O Change in enthalpy,

∆H = (- qsoln ) / (0.05 moles )