GENERAL CHEMISTRY

MANUAL

2009
EXPERIMENT 11-PREPARATION OF SOLUTIONS
1. PURPOSE
The purpose of the experiment is to learn how to prepare a solution with known
concentration.
2. THEORY
A solution is a homogeneous mixture created by dissolving one or more solutes in a solvent.
The chemical present in smaller amount, the solute, is soluble in the solvent (the Chemical
present in larger amount). Solutions with accurately known concentrations can be referred to
as standard (stock) solutions. These solutions are bought directly from the manufacturer or
formed by dissolving the desired amount of solute into a volumetric flask of a specific
volume.
Preparing a Standard Solution from a Solid
A solution of known concentration can be prepared from solids by two similar methods.
Although inherent errors exist with each of the methods, with careful technique either will
suffice for making solutions in General Chemistry Laboratory. In the first method, the solid
solute is weighed out on weighing paper or in a small container and then transferred directly
to a volumetric flask (commonly called a "vol flask"). A funnel might be helpful when
transferring the solid into the slim neck of the vol flask. A small quantity of solvent is then
added to the vol flask and the contents are swirled gently until the substance is completely
dissolved. More solvent is added until the meniscus of the liquid reaches the calibration mark
on the neck of the vol flask (a process called “diluting to volume”). The vol flask is then
capped and inverted several times until the contents are mixed and completely dissolved. The
disadvantage of this method is that some of the weighed solid may adhere to the original
container, weighing paper, or funnel. Also, solid may be spilled when it is transferred into the
slim neck of the vol flask.
In the second method the solid is weighed out first in a small beaker. A small amount of
solvent is added to the beaker and the solution is stirred until the solid is dissolved. The
solution is then transferred to the vol flask. Again, a funnel may need to be inserted into the
slim neck of the vol flask. Before adding additional solvent to the flask, the beaker, stirring
rod, and funnel must be rinsed carefully and the washings added to the vol flask making sure
all remaining traces of the solution have been transferred. Finally, the vol flask is diluted to
volume (additional solvent is added to the flask until the liquid level reaches the calibration
mark).
In general chemistry molarity is the most commonly used concentration unit.
moles of solute
molarity =
liters of solutions
Percent solutions
a) Mass percent means the number of grams of solute per 100 g of solution. For example, 10
g sodium chloride in 90 g water is a 10% by mass solution.
mass percentage = (mass of solute / mass of solution)*100
= 10 g/ (10 g + 90 g) x100%
= 10%
b) Volume percentage means the number of milliliters of solute per 100 mL of solution
Diluting a Solution of Known Concentration
Dilution is the addition of more solvent to produce a solution of reduced concentration. Most
often a diluted solution is created from a small volume of a more concentrated stock solution.
To make such a solution, a volumetric pipet is used to deliver an exact amount of the stock
solution into a clean vol flask, which is then diluted to volume. To prevent extra dilution or
contamination, prerinse the vol pipet with the stock solution to remove any water droplets or
impurities. (The rinsings should be placed in an appropriate collection container.)
The diluted solution’s molarity is less than the stock solution it was created from. The moles
present in the volume of stock solution delivered by the volumetric pipet is equal to the moles
present in the diluted solution created

N1 = N 2
M 1V1 = M 2V2
N: Number of moles of solute in the solutions
M: Molarity of Solution
V: Volume of solutions
3. EXPERIMENTAL PROCEDURE
1. For preparing % 10 weight percent NaOH solution, weight 10 g NaOH and solved it
in 90 g water.
2. For preparing 1 M NaCl solution, calculate the required amount of NaCl then put it
into small beaker and add small amount of distillated water on it. After then put this solution
into
3. Calculate the amount of HCl for preparing 0,5 M 100 ml HCl solution from the
concentrated % 37 HCl solution with a density 1.18 g/ ml. Take required volume with the
help of pipettes then put it into volumetric flask. It is important that initially small amount of
water have to be exist in the flask and fill the volumetric flask to the volume line.
4. REFERENCES
1. Temel ve Genel Kimya Laboratuarı Deney Föyü; Muğla Ünivesitesi FEF Kimya
Bölümü; 2007
2. Manual for Chemistry Laboratory; Department of Chemical Eng. Ege University;
2001
3. http://library.thinkquest.org/3310/nographics/experiments/titrate.html
4. http://en.wikipedia.org/
EXPERIMENT 12-PREPARATION AND STANDARDIZATION OF
ACID-BASE SOLUTIONS

1. PURPOSE
The aim of the experiment is to learn how to determine the concentration of a solution also
referred to as standardizing a solution and to practice the technique of titration. Finally we
will determine the molar mass and identity of an unknown acid using titration and your
standardized solution.
2. THEORY
An acid-base reaction is a chemical reaction that occurs between an acid and a base. Several
concepts exist which provide alternative definitions for the reaction mechanisms involved and
their application in solving related problems. Despite several similarities in definitions, their
importance becomes apparent as different methods of analysis when applied to acid-base
reactions for gaseous or liquid species, or when acid or base character may be somewhat less
apparent. There are some definitions for acids and bases.
The Arrhenius definition of acid-base reactions is a more simplified acid-base concept
devised by Svante Arrhenius, which was used to provide a modern definition of bases that
followed from his work with Friedrich Wilhelm Ostwald in establishing the presence of ions
in aqueous solution in 1884, and led to Arrhenius receiving the Nobel prize in chemistry in
1903 for "recognition of the extraordinary services rendered to the advancement of chemistry
by his electrolytic theory of dissociation"
As defined at the time of discovery, acid-base reactions are characterized by Arrhenius acids,
which dissociate in aqueous solution form hydrogen or the later-termed oxonium (H3O+)
ions, and Arrhenius bases which form hydroxide (OH-) ions. More recent IUPAC
recommendations now suggest the newer term "hydronium" be used in favor of the older
accepted term "oxonium" to illustrate reaction mechanisms such as those defined in the
Brønsted-Lowry and solvent system definitions more clearly, with the Arrhenius definition
serving as a simple general outline of acid-base character. More succinctly, the Arrhenius
definition can be surmised as;
“ Arrhenius acids form hydrogen ions in aqueous solution with Arrhenius bases forming
hydroxide ions. ”
The universal aqueous acid-base definition of the Arrhenius concept is described as the
formation of water from hydrogen and hydroxide ions, or hydronium ions and hydroxide ions
produced from the dissociation of an acid and base in aqueous solution
 (2 H2O → OH- + H3O+ ),
which leads to the definition that in Arrhenius acid-base reactions, a salt and water is formed
from the reaction between an acid and a base in more simple scientific definitions, this form
of reaction is called a Neutralization reaction.
acid+ + base- → salt + water
The positive ion from a base can form a salt with the negative ion from an acid. For example,
two moles of the base sodium hydroxide (NaOH) can combine with one mole of sulfuric acid
(H2SO4) to form two moles of water and one mole of sodium sulfate.
2NaOH + H2SO4 → 2 H2O + Na2SO4
The Brønsted-Lowry definition, formulated independently by its two proponents Johannes
Nicolaus Brønsted and Martin Lowry in 1923 is based upon the idea of protonation of bases
through the de-protonation of acids -- more commonly referred to as the ability of acids to
"donate" hydrogen ions (H+) or protons to bases, which "accept" them. In contrast to the
Arrhenius definition, the Brønsted-Lowry definition refers to the products of an acid-base
reaction as conjugate acids and bases to refer to the relation of one proton, and to indicate that
there has been a reaction between the two quantities, rather than a "formation" of salt and
water, as explained in the Arrhenius definition.
It defines that in reactions, there is the donation and reception of a proton, which essentially
refers to the removal of a hydrogen ion bonded within a compound and its reaction with
another compound, and not the removal of a proton from the nucleus of an atom, which would
require inordinate amounts of energy not attainable through the simple dissociation of acids.
In differentiation from the Arrhenius definition, the Brønsted-Lowry definition postulates that
for each acid, there is a conjugate acid and base or "conjugate acid-base pair" that is formed
through a complete reaction, which also includes water, which is amphoteric.
The Lewis definition of acid base reactions, devised by Gilbert N. Lewis in 1923 is an
encompassing theory to the Brønsted-Lowry and solvent-system definitions with regards to
the premise of a donation mechanism, which conversely attributes the donation of electron
pairs from bases and the acceptance by acids, rather than protons or other bonded substances
and spans both aqueous and non-aqueous reactions.
Ag+ + 2 : NH3 → [H3N:Ag:NH3]+
A silver cation reacts as an acid with ammonia which acts as an electron-pair donor, forming
an ammonia-silver adduct
In titration, we carefully add a solution of one reactant (the titrant) to a measured amount of
a second reactant. One of these is a standard (known concentration or molar mass) and the
other is unknown (the analyte). A color change (or some other distinctive change) occurs
when enough titrant has been added to consume all the reactant in the analyte. In this acid-
base titration we make use of the general reaction:
OH- + HA _ H2O + A
The equivalence point for this reaction is the state when we have added equal moles of OH
and HA because they react in a 1:1 mole ratio. We can't always determine the equivalence
point accurately, and we often approximate it by the endpoint. Near the equivalence point of
an acid base titration, the pH of the solution changes rapidly with changing relative amounts
of HA and OH-, and this changes the color of an indicator. As we approach the endpoint, the
color change will occur near where the drop of titrant hits the solution, but this color quickly
disappears. We try to reach the point where addition of one drop of titrant causes a permanent
change in color after swirling. (Permanent means lasting more than 10 seconds.) This is the
endpoint. Titration is a very precise technique. Replicate runs should yield values that have a
relative deviation of less than 30 parts per thousand (ppt). The indicator in this titration is
phenolphthalein (pronounced fee-nol-thay-lean). Phenolphthalein is colorless in acid solution,
but turns pink in basic solutions.
Applications of acid/base titrations include: determining the amount of acid or base in a
mixture, determining the molar mass of an acid or base known to be pure, and in acid rain
studies, determining the total amount of acid or base present in natural water.
The titrant concentration is generally determined by standardization. In this experiment you
prepare an analyte solution of sodium hydroxide (NaOH) approximately 0.10 M in
concentration. You then standardize this solution by using it to titrate a weighed amount of a
primary standard acid, HCl, (abbreviated KHP).
Primary Standard A substance of known purity for which we can determine the amount in
moles we have by simply weighing the material. In this experiment, NaOH is a primary
standard; (commercial HCl) is not.
Standardization is the process of determining the concentration of a solution. In this case we
standardize a HCl solution by determining the volume of HCl that reacts with a known
amount in moles of NaOH.
NaOH is a base, HCl is an acid, and they react in a 1:1 mole ratio. The ionic reaction is:
Na+ + OH- + H+ + Cl-
Na+ + Cl+ + H2O
3. EXPERIMENTAL PROCEDURE
1. Preparation of 100 ml 0,2 N HCl solution: For this purpose firstly calculate the
amount of HCl must be taken from the stock solution with 1,19 g/ml density and % 36 wt
percent. After then take enough amount of HCl solution with the help of 10 ml pipette and put
it into volumetric flask then add water to fill it to the volume line.
Important: HCl is very dangerous and corrosive material. It damages the cloths also body
so you have to be careful when you work with it. Dilution of HCl with water is extremely
exothermic so add HCl very slowly onto water.
DON’ T ADD WATER ONTO CONCENTRATED ACIDS
IT MAY CAUSE EXPLOSION
2. Preparation of NaOH solution with known concentration: Calculate the amount of
NaOH for preparing 100 ml 0,1 N NaOH solution. Weight it and put it into a volumetric flask
carefully. Then add little amount of water on it and solve completely. Finally fill it with water
till the volume line.
3. Standardization of HCl solution with NaOH solution: Firstly take 10 ml from the
HCl solution and put it into Erlenmeyer flask. Add one or two drops of phenol phtalane as
indicator. Secondly take enough amount of NaOH solution and fill the burette. And titrate the
HCl solution with the NaOH and calculate the concentration of HCl solution.
4. REFERENCES
1. Temel Ve Genel Kimya Deney Föyü; Muğla 2007
2. Bowdoın College Department Of Chemistry Lab. Manual; SPRING 2002
3. http://en.wikipedia.org/wiki/Acid-base_reaction_theories
EXPERIMENT 13-ACID BASE TITRATION

1.THEORY
Titration is a common laboratory method of quantitative/chemical analysis that can be used to
determine the concentration of a known reactant. Because volume measurements play a key
role in titration, it is also known as volumetric analysis. A reagent, called the titrant, of known
concentration (a standard solution) and volume is used to react with a solution of the analyte,
whose concentration is not known in advance. Using a calibrated burette to add the titrant, it
is possible to determine the exact amount that has been consumed when the endpoint is
reached. The endpoint is the point at which the titration is complete, as determined by an
indicator. This is ideally the same volume as the equivalence point - the volume of added
titrant at which the number of moles of titrant is equal to the number of moles of analyte, or
some multiple thereof (as in polyprotic acids). In the classic strong acid-strong base titration,
the endpoint of a titration is the point at which the pH of the reactant is just about equal to 7,
and often when the solution permanently changes color due to an indicator. There are
however many different types of titrations.

Figure 1. Titration apparatus[2]

Before starting the titration a suitable pH indicator must be chosen. The endpoint of the
reaction, when all the products have reacted, will have a pH dependent on the relative
strengths of the acids and bases. The pH of the endpoint can be roughly determined using the
following rules:
• A strong acid reacts with a strong base to form a neutral (pH=7) solution.
• A strong acid reacts with a weak base to form an acidic (pH<7) solution.
• A weak acid reacts with a strong base to form a basic (pH>7) solution.
When a weak acid reacts with a weak base, the endpoint solution will be basic if the base is
stronger and acidic if the acid is stronger. If both are of equal strength, then the endpoint pH
will be neutral.
A suitable indicator should be chosen, that will experience a change in color close to the end
point of the reaction.
2. EXPERIMENTAL PROCEDURE
1. Clean and dry the burettes and beaker, and clamp the two burettes to the ring stand. Fill
one of the two burettes with 1M HCl solution, and the other with the NaOH solution.
2. Use the buret to measure out 20 mL of HCl into an empty beaker. Add 2-3 drops of the
indicator solution.
3. Titrate slowly with the NaOH solution, with constant swirling, until one single drop of
NaOH causes a permanent pink color that does not fade on swirling. Record the volume of
NaOH used.
4. Use the formula M1V1=M2V2 to determine the concentration of the NaOH solution. This
solution may now be used to titrate the unknown acid sample.
5. Replace the burette containing the 1M HCl with the burette containing the HCl solution of
unknown concentration. Refill the NaOH burette, and wash out the beaker.
6. Repeat the titration from steps 2-4 using 20 mL of the unknown acid solution to determine
the concentration of the HCl solution.
3. REFERENCES
1. Temel ve Genel Kimya Laboratuarı Deney Föyü; Muğla Ünivesitesi FEF Kimya
Bölümü; 2007
2. Manual for Chemistry Laboratory; Department of Chemical Eng. Ege University;
2001
3. http://library.thinkquest.org/3310/nographics/experiments/titrate.html
4. http://en.wikipedia.org/wiki/Titration
EXPERIMENT 14-pH and INDICATOR

1. THEORY
A pH indicator is a halochromic chemical compound that is added in small amounts to a
solution so that the pH (acidity or alkalinity) of the solution can be determined easily. Hence
a pH indicator is a chemical detector for hydronium ions (H3O+) (or Hydrogen ions (H+) in
the Arrhenius model). Normally, the indicator causes the colour of the solution to change
depending on the pH. pH values above 7.0 are basic, and pH values below 7.0 are acidic.
Solutions with a pH value of 7.0 are neutral.
pH indicator themselves are frequently weak acids or bases. When introduced into a solution,
they may bind to H+ (Hydrogen ion) or OH- (hydroxide) ions. The different electron
configurations of the bound indicator causes the indicator's color to change
pH indicator are frequently employed in titrations in analytic chemistry and biology
experiments to determine the extent of a chemical reaction. Because of the subjective
determination of color, pH indicator are susceptible to imprecise readings. For applications
requiring precise measurement of pH, a pH meter is frequently used.

Figure1. The color characteristics of some common indicators[2]

2. EXPERIMENTAL PROCEDURE
1. Add 9 ml of water to 1 ml of 0.1 M HCl solution. Measure the pH of this solution. Prepare
a solution that has a Ph OF 4.
2. Prepare 0.01 M 100 ml CH3COOH solution by using 1 M CH3COOH solution.
3. Take 4 test tubes and mark them as 1,2,3,4. Then put 2-2.5 ml 0.1 M HCl at each of them.
Repeat the steps by taking four other test tubes and by putting same amount of 0.1 M NaOH
instead of HCl
4. Add 1 drop of methyl orange to test tubes number 1 of acid and base
5. Add 1 drop of bromotymol blue to test tubes number 2 of acid and base
6. Add 1 drop of phenolphthalein to test tubes number 3 of acid and base
7. Add 1 litmus paper to test tubes number 4 of acid and base
3. REFERENCES
1. Temel ve Genel Kimya Laboratuarı Deney Föyü; Muğla Ünivesitesi FEF Kimya
Bölümü; 2007
2. Manual for Chemistry Laboratory; Department of Chemical Eng. Ege University;
2001
3. http://en.wikipedia.org/
EXPERIMENT 15-BUFFER SOLUTIONS

1. PURPOSE:
The purpose of this experiment is to prepare buffer solutions and to determine their buffer
capacity.
2. THEORY
Its more difficult to prevent a known pH solution than to prepare it. If the solution is open to
air then it will be more acidic because of the carbondioxide absorption. If the solution is kept
on in glass bottle, the basic impurities from the glass may change the pH of it.
A buffer solution is one that is resistant to change in pH when small amounts of strong acid or
base are added. For example, when 0.01 mole of strong acid or base are added to distilled
water, the pH drops to 2 with the acid and rises to 12 with the base. If the same amount of
acid or base is added to an acetic acid – sodium acetate buffer, the pH may only change a
fraction of a unit.
Buffers are important in many areas of chemistry. When the pH must be controlled during the
course of a reaction, the solutions are often buffered. This is often the case in biochemistry
when enzymes or proteins are being studied. Our blood is buffered to a pH of 7.4. Variations
of a few tenths of a pH unit can cause illness or death. Acidosis is the condition when pH
drops too low. Alkalosis results when the pH is higher than normal.
Two species are required in a buffer solution. One is capable of reacting with OH- and the
other will react with H3O+. The two species must not react with each other. Many buffers
are prepared by combining a weak acid and its conjugate (acetic acid and sodium acetate) or a
weak base and its conjugate (ammonia and ammonium chloride). In general, the pH range in
which a buffer solution is effective is +/- one pH unit on either side of the pKa. The
Henderson–Hasselbalch provides the information needed to prepare a buffer.
The pH of the acidic or basic solutions are calculated by following formulas:
Ca
pH = pK a − log Ca = Concentration of weak acid
Cs Cs = Concentration of salt
Cb = Concentration of weak base
Cb
pOH = pK b − log
Cs
There is a limit to the amount of acid or base that can be added to a buffer solution before one
of the components is used up. This limit is called the buffer capacity and is defined as the
moles of acid or base necessary to change the pH of one liter of solution by one unit.
Buffer Capacity = (number of moles of OH- or H3O+ added)
 (pH change)(volume of buffer in L)
3. EXPERIMENTAL PROCEDURE
1. Take three erlenmayer of 100 ml and pour 2 ml of 30 % acetic acid solution, 25 ml of
distilled water, 5 drops of 0.1 % Congo red. The solutions have to be turn into dark
blue color.
2. Pour 5 ml of concentrated sodium acetate (CH3COONa) in to first and second erlen.
The color of the solutions changes from dark blue to pink (pH changes from 2.7 to
5.2). So, a buffer solution is prepared.
3. Pour 5 ml of 0.1 N HCl into first, 5 ml of 0.1 N NaOH into second erlenmayers. The
colors of both solutions stay constant.
4. When 5 ml of 0.1 N NaOH solution is poured into third erlenmayer, you will see the
change in color.

4. REFERENCES
1. Temel ve Genel Kimya Laboratuarı Deney Föyü; Muğla Ünivesitesi FEF Kimya
Bölümü; 2007
2. Manual for Chemistry Laboratory; Department of Chemical Eng. Ege University;
2001
3. http://library.thinkquest.org/3310/nographics/experiments/titrate.html
4. http://en.wikipedia.org/
EXPERIMENT 16-QUALITATIVE ANALYSIS OF GROUP-I CATIONS
AND GROUP-I ANIONS

1. THEORY
Classical qualitative inorganic analysis is a method of analytical chemistry which seeks to
find elemental composition of inorganic compounds. It is mainly focused on detecting ions in
an aqueous solution, so that materials in other forms may need to be brought into this state
before using standard methods. The solution is then treated with various reagents to test for
reactions characteristic of certain ions, which may cause color change, solid forming and
other obviously visible changes.
According to their properties, cations are usually classified into five groups. Each group has a
common reagent which can be used to separate them from the solution. The separation must
be done in the sequence specified below; otherwise, for example, some ions of 1st group can
also react with 2nd group reagent, so that the solution must not have any ions left from
previous groups to obtain meaningful results. The division and precise details of separating
into groups vary slightly from one source to another; given below is one of the commonly
used schemes.
2. 1ST ANALYTICAL GROUP OF CATIONS
1st analytical group of cations consists of ions that form insoluble chlorides. As such, the
group reagent to separate them is hydrochloric acid, usually used at concentration of 1–2 M.
Concentrated HCl must not be used, because it forms a soluble complex ion - [PbCl4]2- with
Pb2+. Consequently the Pb2+ ion would go undetected
The most important cations in 1st group are Ag+, Hg22+, and Pb2+. The chlorides of these
elements cannot be distinguished from each other by their colour - they are all white solid
compounds. PbCl2 is soluble in hot water, and can therefore be differentiated easily. To
distinguish between the other two, ammonia is used as a reagent. While AgCl dissolves in
ammonia (due to the formation of the complex ion [Ag(NH3)2]+ion), Hg2Cl2 gives a black
precipitate consisting of a mixture of chloro-mercuric amide and elemental mercury.
Furthermore, AgCl is reduced to silver under light, which gives samples a violet colour.
PbCl2 is far more soluble than the chlorides of the other two ions, especially in hot water.
Therefore, HCl in concentrations which completely sedimentize Hg22+ and Ag+, may not be
sufficient to do the same to Pb2+ and higher concentrations ca not be used for the
aforementioned reasons. Thus, a filtrate obtained after first group analysis of Pb2+ contains an
appreciable concentration of this cation, enough to give the test of the second group, viz.
formation of an insoluble sulfide. For this reason, Pb2+ is usually also included in the 2nd
analytical group.
2.1. EXPERIMENTAL PROCEDURE:
Route for analysis of silver group is given below.

General procedure for

analysis of Group 1 cations
3. DETERMINATION OF SOME ANIONS
The principles that are employed in the identification of cations can also be applied to the
analysis of anions. The qualitative detection of anions in a sample depends on the distinctive
solubility properties of particular salts of the ions and specific chemical reactions that are
(ideally) unique to a particular ion. In this experiment, we will explore ways to detect the
presence of , SO4-2, Cl-,and I-. You will be testing both known and unknown solutions.
3.1. EXPERIMENTAL PROCEDURE:
Test for the Sulfate Ion
To 1 mL of the test solution, add 6 M HNO3 drop by drop until the solution is acidic. Then
add 1 mL of 0.1 M BaCl2 solution in order to produce a white precipitate of BaSO4.
SO4-2(aq) + Ba+2(aq) → BaSO4(s) (1)
Test for the Chloride Ion
To 1 mL of a new test solution, add a couple drops of 6 M HNO3 as needed to make the
solution slightly acidic. Add 10 drops of 0.1 M AgNO3. No precipitate proves the absence of
Cl-, Br-, or I-. Centrifuge the mixture.
Test the clear filtrate with 1 drop of 0.1 M AgNO3 for complete precipitation. If necessary,
centrifuge again. Discard the filtrate. To this precipitate, add 1 mL of D.I. water, 2 drops of 6
M NH3, and 6 drops of 0.1 M AgNO3. The proportions are important, since we want to
dissolve ONLY AgCl.
AgCl(s) + 2 NH3(aq) → Ag(NH3)2 +(aq) + Cl-(aq)
Shake the mixture well and centrifuge. Transfer the clear solution to a clean test tube, and
acidify once again with 6 M HNO3. A white precipitate of AgCl confirms the presence of Cl-.
Ag(NH3)2 +(aq) + Cl-(aq) + 2H+ → AgCl(s) + 2NH4+(aq)
Test for the Iodide Ion
Acidify a 2 mL sample of a new test solution by adding 6 M HCl. Add 1 mL of 0,1 M FeCl3
to oxidize any I- to I2. (Br- is not oxidized by Fe+3.) Add 1 mL of CCl4 and agitate the
mixture. A purple color of I2 in the CCl4 layer indicate I- was present in the original sample.

2I-(aq) + 2Fe+3(aq) → I2(aq) + 2Fe+2(aq)

Test for the NO3 - Ion
Place 10 drops of the solution to be tested in a clean, well-rinsed test tube. Make the solution
acidic by adding 3 M H2SO4 as needed. Next, add 5 drops of a freshly prepared, saturated
solution of iron (II) sulfate (FeSO4) and mix gently. Incline the test tube at a 45o angle, and, as
shown in the sketch, carefully add 5 drops of concentrated H2SO4 so the drops roll down the
side of the test tube and slide gently onto the top of the solution. DO NOT MIX the solutions!
Two separate liquid layers will be observed in the test tube. If NO3 - is present, a very faint
brown ring will be observed near the bottom of the test tube, thereby confirming the presence
of nitrate ion.
4. REFERENCES
1. Temel ve Genel Kimya Lab. Föyü, Muğla Üniv., 2007

2. A New Approach to General Chemistry Laboratory; G.A.Öktem, M. Acımış; Abant

Đzzet Baysal Üniv. Yayınları No:9; 1998

3. Genereal Chemistry Laboratory Manual; Ege Üniv.; 2001

4. General Chemistry; 8th Edition; R.H.Petrucci et al; Prentice Hall; 2002

EXPERIMENT 17-CHEMICAL EQUILIBRIUM

1.THEORY
In a chemical process, chemical equilibrium is the state in which the chemical activities or
concentrations of the reactants and products have no net change over time. Usually, this
would be the state that results when the forward chemical process proceeds at the same rate as
their reverse reaction. The reaction rates of the forward and reverse reactions are generally not
zero but, being equal, there are no net changes in any of the reactant or product
concentrations. This process is called as dynamic equilibrium.
In a chemical reaction, when reactants are mixed together in a reaction vessel (and heated if
needed), the whole of reactants do not get converted into the products. After some time
(which may be shorter than millionths of a second or longer than the age of the universe),
there will come a point when a fixed amount of reactants will exist in harmony with a fixed
amount of products, the amounts of neither changing anymore. This is called chemical
equilibrium.
For any reaction such as:
aA + bB cC + dD
to be at equilibrium the rates of the forward and backward (reverse) reactions have to be
equal. In this chemical equation, A and B are reactant chemical species, C and D are product
species, and a,b,c and d are the stoichiometric coefficients of the respective reactants and
products.
Forward reaction rate: k + A a B b

Backward reaction rate: k − C c D d

where A, B, C and D are active masses and k+ and k− are rate constants. Since forward and
backward rates are equal:
k+ Aa B b = k − C c D d
k+ Aa B b
Kd = = c d
k− C D
and the ratio of the rate constants is also a constant, now known as an equilibrium constant.
c d
Pc Pd
Kp = a b
P: Partial pressure
Pa Pb
The following equilibrium can be written for Kd and Kp:
∆n
K p = K d (RT ) R: Gas Constant; T: Temperature; n: (nproducts - nreactants)
2. EXPERIMENTAL PROCEDURE
Take and wash six glass tubes by distilled water carefully. Pour 5 ml of 0.002 M KSCN into
each. Add 5 ml of 0.2 M Fe(NO3)3 into first tube. This (first) tube will be your standard. Pour
10 ml of 0.2 M Fe(NO3)3 into a graduated cylinder. Add distilled water by stirring up to 25
ml. Pour 5 ml of this diluted (concentration is 0.08 Fe+3) solution into second tube. Throw the
solution out from graduated cylinder to the lavatory until it contains 10 ml. Fill the graduated
cylinder again by distilled water up to 25 ml. Strongly stir the solution. And pour 5 ml of this
solution into the third glass tube. Repeat this dilution procedure for 4th, 5th and 6th glass tubes.
The concentration of FeSCN2+ in the tubes will be found by comparing with the first glass
tube. Compare the darkness of the color of 1st tube with other tubes. For this procedure you
can take two tubes in hand and cover them with a white paper. If you look them from top you
can easily compare the colors. If their darkness of color are same then measure the heights of
the solutions. If they are not same, take a few of the solution from 1st glass tube into a clean
dry beaker (it can be used later) and compare them again. Repeat the procedures until the
darkness are same. Measure the heights of the solutions. Repeat the procedure for all glass
tubes.
Table 1. Data Table For Chemical Equilibrium Experiment
Height of the solution Height of the Standard
nd
2 tube
3rd tube
4th tube
5th tube
6th tube

3. REFERENCES
1. Temel ve Genel Kimya Lab. Föyü, Muğla Üniv., 2007

2. A New Approach to General Chemistry Laboratory; G.A.Öktem, M. Acımış; Abant

Đzzet Baysal Üniv. Yayınları No:9; 1998

3. Genereal Chemistry Laboratory Manual; Ege Üniv.; 2001

4. General Chemistry; 8th Edition; R.H.Petrucci et al; Prentice Hall; 2002

EXPERIMENT 18-EFFECT OF TEMPERATURE ON REACTION RATE

1.THEORY
The rate of a chemical reaction is the time required for a given quantity of reactant(s) to be
changed to product(s). Reaction rate usually is expressed in terms of moles per unit time.
This rate is affected by several factors, including the nature of the reactants, concentration of
the reactants, temperature, pressure, and the presence of catalysts. In this experiment, you
will study the effects of temperature and concentration.
A chemical reaction is the result of effective collisions between particles of reactants.
Increasing the temperature of a system raises the average kinetic energy of the particles of the
system. This results in more collisions and, of greater importance, more effective collisions
per unit time. This affects the rate of the reaction.
At constant temperature, increasing the concentration of one or more of the reactants
increases the number of particles present and, hence, the number of collisions. This affects
the rate of the reaction.

Figure 1. Reaction progress with respect to potential energy [ref. 5]

The rate of reaction increases by increasing temperature, generally. The Arrhenius equation
is a simple, but remarkably accurate, formula for the temperature dependence of the rate
constant, and therefore rate, of a chemical reaction. In short, the Arrhenius equation gives "the
dependence of the rate constant k of chemical reactions on the temperature T (in Kelvin) and
activation energy Ea", as shown below.
− Ea

k = Ae RT
where A is the pre-exponential factor or simply the prefactor and R is the gas constant.
2. EXPERIMENTAL PROCEDURE
Pour 5 ml of 0.0005 M KMnO4 solution and 1 ml of 0.25 M H2SO4 solution into five glass
tube. Take five more glass tube and pour 9 ml of 0.0025 M oxalic acid (C2H2O4) in to them
with the help of a pipette. Put one of the tube containing KMnO4 and one containing C2H2O4
into the water bath at 25 oC. Wait for three minutes at this temperature. Then, pour the oxalic
acid solution into the permanganate solution carefully. Record the time passed when the color
of the solution changes from pink to colorless. Be sure the temperature of the final solution
kept at 25 oC.
Repeat the same procedure for different temperatures (35, 45, 55, 65 oC) and record the time
passed for the color change.
3. RESULTS
1.Draw the graph for time versus temperature.
2.Calculate the reaction rate for each temperature.
4. REFERENCES
1. Temel ve Genel Kimya Lab. Föyü, Muğla Üniv., 2007

2. A New Approach to General Chemistry Laboratory; G.A.Öktem, M. Acımış; Abant

Đzzet Baysal Üniv. Yayınları No:9; 1998

3. Genereal Chemistry Laboratory Manual; Ege Üniv.; 2001

4. General Chemistry; 8th Edition; R.H.Petrucci et al; Prentice Hall; 2002

5. http://en.wikipedia.org/
EXPERIMENT 19-SAPONIFICATION AND THE MAKING OF SOAP

1. THEORY

In today's experiment, we will perform a reaction that has been used for millennia: the making
of soap. Animal fat and vegetable oils are composed principally of esters of the long chain
fatty acids and glycerol (glycerin; 1,2,3-propantriol). Hydrolysis of these triglycerides
(triacylglycerides; TAG) in base (e.g., NaOH) yields glycerol (a carbohydrate) and the sodium
salts of the fatty acids. Because the fatty acids are ions, they are soluble in low concentrations
in water (actually they are soluble because they form micelles), but in high concentration form
insoluble aggregates called soap. You will start with a vegetable oil and will use NaOH to
hydrolyze these triglycerides. Basic hydrolysis of esters is called saponification. The reaction
for this experiment is shown:

The triglycerides most commonly used to make soap commercially are from animal sources,
such as tallow, although plant fats from coconut, palm and other vegetable oils can be used.
Pure coconut oil yields soap that is very soluble in water because it contains predominately
myristic and lauric acids (14- and 12-carbon fatty acids, respectively). Soaps made from
animal and other vegetable sources contain more 16- and 18-carbon fatty acids and are
generally harder and easy to form into shapes. To soften these harder soaps, coconut oil is
often included in the saponification reaction to make the soap softer.

The function of soaps and detergents is to remove grease and dirt by emulsifying the grease
(bringing it into suspension). Dirt adheres to clothing and to skin primarily by being “glued”
to these surfaces with a thin film of oil or grease; the oil (lipid) on the skin is generally
secreted during perspiration. The soap or detergent removes the oil film and the dirt can be
washed away. How do soaps and detergents “dissolve” non-polar substances such as fats, oils,
and greases? Molecules of soaps and detergents contain a non-polar (hydrophobic)
hydrocarbon end, and a polar (hydrophilic) end that is usually ionic. The non-polar ends of the
molecule surround the tiny oil droplets and are partially dissolved in them (like dissolves
like). The polar ends of the molecules, which are extremely soluble in water, solubilize or
emulsify the entire droplet.

2.EXPERIMENTAL PROCEDURE

Prepare a mixture of 15 mL of 20% (5 M) sodium hydroxide and 10 mL of vegetable oil in a

150-mL flask. Add a stirring bar to the flask, to prevent explosive boiling of the NaOH-oil
mixture. Turn the stirring hot plate on at any setting to get it boiling, and then switch to the
lowest setting when boiling begins. Turn on the stirrer to let the stirring bar rotate. Boil the
mixture, observing the precautions listed above. Carefully control the heating, but you should
heat the mixture high enough to maintain a constantly boiling mixture. The saponification is
complete if a wax-like solid begins to form that on further cooling becomes hard and
somewhat brittle. On the other hand, if the mixture cools to a syrupy liquid, saponification is
not complete, and heating and stirring must be resumed. It might be advisable to add more (5
mL) 20% NaOH and boil the mixture until its water is expelled. Saponification should be
complete by 30-45 min (but it may take only 15-20 min).

While the mixture is heating, prepare a concentrated salt solution by dissolving 50 g of NaCl
in 150 mL of distilled water in a 400-mL beaker. (Prepare this solution immediately so that it
is ready when your soap is ready.) When the saponification reaction is complete, remove the
flask from the heat source using HotHandsTM to hold the hot flask. Pour the reaction mixture
quickly into the saturated salt solution (you may have to scrape the solid into the NaCl
solution using a scoopula). Stir the mixture thoroughly for several minutes; then, collect the
precipitated soap on a Büchner funnel. Wash the soap twice with 10 mL of ice-cold distilled
water (cool the water with ice, but don't add the ice to the distilled water). After you have
collected and washed the soap, continue to draw air through the soap for several minutes to
help dry it. Save the soap for use in the evaluation section.