1

GENERAL CHEMISTRY-I
LABORATORY MANUAL

Instructor: Şenel TEKE TUNCEL, Assoc. Prof.

Lab Assistant: Volkan YALMAN, MSc.
Betül SUBAŞI, MSc.

T.C. İstanbul Arel University

Department of Molecular Biology and Genetics
2023

2
Table of Contents

Experiment I : Properties of Pure Substances ................................................. 5

Experiment II : Identification of Substances by Their Reactions ................ 11
Experiment III : Preparation of Solutions ...................................................... 19
Experiment IV : Stochiometry of a Chemical Reaction ................................ 22
Experiment V : Preparing Solutions Through Serial Dilutions ................... 27
Experiment VI : Formula and Composition of a Hydrate ............................ 29
Experiment VII : Acid-Base Titrations ........................................................... 34
Experiment VIII : Oxidation Reduction (Redox) Titrations ........................ 37

3
LAB SAFETY RULES

Safety rules are guidelines designed to help keep YOU safe when experimenting. Some
equipment and chemicals in the laboratory carry a potential risk and can cause serious harm.
The following rules are the basic rules that should be followed in the general biology lab.
DO’s
Be prepared: Before the biology lab, you should be knowledgeable about any lab exercises
that will be performed. You should read your lab manual to know exactly what you will be
doing.
Clothing: Wearing a lab coat protects you potential damage from chemical or biological
spills. Also wearing proper shoes can protect your feet in case something gets broken. Sandals
or any type of open-toed shoes are not recommended. You should wear a lab coat during the
laboratory session and long hair must be tied at back.
Gloves: Laboratory gloves must be worn when dealing with chemicals, blood and other
biological samples. They will be provided by the assistants.
✓ Be aware when dealing with chemicals and working with fire. Warn assistants
immediately if something goes wrong.
✓ Ensure that all communal materials and equipment are clean after use
✓ Rinse out all your glassware before you put it out for washing.
✓ Ask before doing anything when you don’t understand.
DO NOT’s
✓ Do not eat, drink, chew gum and smoke in the lab.
✓ Do not taste any chemicals or substances and do not use your mouth for pipetting
substances.
✓ Do not handle broken glass with bare hands.
✓ Do not pour chemicals down the drain without permission.
✓ Do not leave any heated materials unattended.
✓ Do not place flammable substances near heat.
✓ Do not perform your own experiments unless given permission.
✓ And please do not touch any equipment in the lab without the supervision of the instructor
or the teaching assistant.
TAKING NOTES
One of the most important necessities in the laboratory is to take notes properly. It is not
possible to remember everything you have done. So you should have a notebook for only
laboratory and note everything elaborately. The obtained data, especially results, are crucial
for preparing an effective lab report. A good laboratory notebook provides anyone who read it
to perform same experiment successfully. Please notice the following rules when taking notes.
✓ Keep your notes on a proper notebook
✓ Write heading and date for each experiment
✓ Write down everything that you used and what you done
✓ Write down results properly
✓ Do not forget every observation is important

4
Experiment I : Properties of Pure Substances

Purpose: To observe several changes in matter carefully and to determine the type of change.

Theory: Matter can be classified as follows:

Matter
Pure substances Mixtures

1 ) elements 1 ) heterogeneous mixtures

(e.g. Na, Fe, Cu) (e.g. sand + water, lime + water)

2 ) compounds 2 ) homogenous mixtures

(e.g. NaC1, CaCO3) (e.g. sugar + water, salt + water)

Pure substances have their own chemical and physical properties. A compound can be
identified by using the following properties.
Physical properties: Melting point, boiling point, density, solubility, color, crystal structure,
physical state, etc.
Chemical properties: The reactions that the compound undergoes under different conditions.
In some cases a substance can undergo a change that we can observe easily.

In a physical change, the appearance of a substance changes, but the composition and
identity stays the same. Examples:
• boiling of water to produce steam
• dissolving of sugar in water
• melting of iron at high temperature
• breaking of a glass into small pieces
In a chemical change, a change in the composition and identity of a substance occurs, new
products are formed:
• burning of wood to give CO2 and water
• rusting of iron to give iron oxide
• electrolysis of water to give H2 and O2
Chemical reactions cannot be reversed easily.
A chemical reaction is indicated by any of the following observations:

5
• change of color
• formation of a precipitate
• evolution of a gas, production of heat, light, or sound

Procedure: Substances to be tested are given below:

* salt (NaCl)
* oxalic acid (H2C2O4)
* sugar (C6H12O6)
* ammonium Hydrogen Phosphate ((NH4)2HPO4)
* copper(II) sulfate (CuSO4)

For the given substances, the following tests will be applied:

1) Changes caused by heat
2) Solubility in water
3) Checking acidity or basicity of their solutions

1) Take a very small amount of the compound (size of a pea), put it in a dry test tube and
start to heat on the Bunsen burner.

PROTECT YOUR EYES, DO NOT SMELL THE GASES.

Observe carefully the changes in the compound, and think about the type of change that has
occurred.

2) Take a small sample of the solid in a test tube, and fill more than half of it with water,
stir and observe.
* Is the solution homogenous?
* Is the solution heterogeneous?
* Is it a suspension?
If the solution is not homogenous, heat it slowly and observe again if there is any change or
not.
3) By using a glass rod, stir the solution from part (2), put a drop of solution on a litmus
paper, and see if the litmus paper changes its color.
* If red litmus paper turns blue the compound is BASIC
* If blue litmus paper turns red the compound is ACIDIC

6
* If no change occurs the compound is NEUTRAL
*** USE CLEAN GLASSWARE: if any impurity is present in the test tube, the result
could be wrong.

Get your unknown compound from your instructor, and try to identify it by using the same
tests stated above.

SAFETY

Ammonium Hydrogen Phosphate: Flush eyes with plenty of water for at least 15 minutes,
occasionally lifting the upper and lower eyelids. Get medical aid. Flush skin with plenty of
water for at least 15 minutes while removing contaminated clothing and shoes. Get medical
aid if irritation develops or persists. Wash clothing before reuse. Never give anything by
mouth to an unconscious person. Get medical aid. Do NOT induce vomiting. If conscious and
alert, rinse mouth and drink 2-4 cupfuls of milk or water. Remove from exposure and move to
fresh air immediately. If not breathing, give artificial respiration. If breathing is difficult, give
oxygen. Get medical aid if cough or other symptoms appear.

Oxalic acid: Harmful if inhaled. Can cause severe irritation and burns in nose, throat and
respiratory tract. Splashing solution into the eyes causes irritation. Swallowing can cause
severe internal pain, renal damage, convulsions, coma and even death.

Copper(II) sulfate: Hazardous in case of skin contact (irritant), of eye contact (irritant), of
ingestion, of inhalation. Check for and remove any contact lenses. In case of contact,
immediately flush eyes with plenty of water for at least 15 minutes. Cold water may be used.
Get medical attention. In case of contact, immediately flush skin with plenty of water. Cover
the irritated skin with an emollient. Remove contaminated clothing and shoes. Cold water
may be used. Wash clothing before reuse. Thoroughly clean shoes before reuse. Get medical
attention. Wash with a disinfectant soap and cover the contaminated skin with an anti-
bacterial cream. Seek immediate medical attention. If inhaled, remove to fresh air. If not
breathing, give artificial respiration. If breathing is difficult, give oxygen. Get medical
attention. Do NOT induce vomiting unless directed to do so by medical personnel. Never give
anything by mouth to an unconscious person. If large quantities of this material are
swallowed, call a physician immediately. Loosen tight clothing such as a collar, tie, belt or
waistband.

7
Name __________________
Partner’s name_______________ Date __________________

Pre Lab Questions:

1) What is the main difference between a chemical and a physical change? Give
examples of each.

2) What observations indicate that a chemical change has occurred?

3) How can you identify a solution as an acid or a base?

8
Name __________________
Partner’s name_______________ Date __________________

Report Questions:

1) Does heat always produce the same type of change? Support your answer by your
observations.

2) What do you think will happen if you dissolve a large amount of compound in part (2)?

3) Describe the safety precautions for this experiment.

4) If a substance gives out water vapor upon heating, what can we deduce from this result?

9
Name __________________
Partner’s name _______________ Date ________________

REPORT I

Heat action Type of change Solubility in Acidity /

observation Chem. / Phys. water Basicity
Salt
NaCl

Sugar
C6H12O6

Ammonium
Hydrogen
Phosphate
(NH4)2HPO4
Copper(II) sulfate
CuSO4

Oxalic acid
H2C2O4

Unknown no __
Formula
____________

10
Experiment II : Identification of Substances by Their Reactions

Purpose: To examine possible chemical reactions when compounds are mixed.

Theory : Most inorganic chemical reactions may be classified in four groups:

1) Combination reactions: Direct union of two simple substances to form a third one.

A+B AB
Fe + S FeS

2) Decomposition reactions: Reverse of combination reactions. A complex compound is

decomposed into two or more simple substances.

AB A+B
2HgO 2Hg + O2

3) Single displacement reactions: Reaction of an element with a compound such that the
element replaces one of the elements in the compound and sets it free.

A + BC AC + B
Zn + 2 HC1 ZnCl2 + H2

4) Double displacement reactions: The positive and negative ions exchange partners. Such
reactions occur in solution and may result with
a) formation of a precipitate, or
b) formation of a gas

AB + CD AD + CB

NaC1 (aq) + AgNO3 (aq) NaNO3 (aq) + AgCl (s)

Na2CO3 (aq) + HC1 (aq) NaC1 (aq) + H2O (1) + CO2 (g)

11
In order to determine whether a precipitate forms, the following solubility rules should be
remembered:

General rules for solubility of ionic compounds in water

1) All salts of Na+, K+ and NH4+ are soluble.

2) All nitrates (NO3-), acetates (C2H3O2-) and chlorates (ClO3-) are soluble
3) All chlorides (Cl-), bromides (Br -) and iodides (I-) are soluble except those of Ag+, Pb++
and Hg2++.
4) All sulfates (SO4-2) are soluble except Ba++, Pb++ and Sr++.
5) All carbonates (CO3-2 ) and phosphates (PO4-3) are insoluble except Na+, K+, NH4+.
6) All hydroxides (OH-) and oxides (O-2) are insoluble except Na+, K+, NH4+ and Ba+2.
7) All sulfides (S -2) are insoluble except Na+, K+, NH4+, Ba+2 , Mg+2 and Ca+2.
How to dissolve an insoluble compound?

If a compound is insoluble in water, different methods should be tried to dissolve it. These
methods could be:
a) changing the pH of the medium
b) using redox reactions
c) forming soluble complexes

a) Changing the pH of the medium:

Among these alternative routes, the easiest way is to change the pH of the medium by using
strong acids (HC1, HNO3, H2SO4). It should be kept in mind that not all insoluble compounds
would be soluble in acids.

Water insoluble compounds can be divided in two groups;

i) acid insoluble ones ii) acid soluble ones

i) If a water insoluble compound contains the anion of a strong acid (i.e. Cl-, Br-, I-, SO4-2) it is
not possible to dissolve it by using a strong acid. For those compounds different methods
should be applied.

BaSO4 + HC1 NO REACTION

12
 AgC1 + HNO3 NO REACTION

ii) if the water insoluble compound contains the anion of a weak acid (i.e. CO3-2, S-2, O-2, OH-,
SO3-2, PO4-3 etc.) this compound can be dissolved by using a strong acid. In most cases the
anion will be destroyed in acid medium.

CaCO3 + 2 HC1 CaC12 (aq) + CO2(g) + H2O(l)

ZnS + 2 HC1 ZnC12 (aq) + H2S (g)

MgO + 2 HCl MgCl2(aq) + H2O(l)

The important point is the selection of the acid, since in some cases we could end up with
another insoluble compound.

BaCO3 (s) + H2SO4 (aq) BaSO4 (s) + CO2 (g) + H2O (1)

PbCO3 (s) + HC1 (aq) PbC12 (s) + CO2 (g) + H2O (1)

PbCO3 (s) + H2SO4 (aq) PbSO4 (s) + CO2 (g) + H2O (1)

b) Using redox reactions:

HNO3 is a good oxidizing agent, in some cases it acts in this way to take the anion away from
the medium, so the compound dissolves.

3 CuS (s) + 8 HNO3 (aq) 3 Cu( NO3)2 (aq) + 3 S(s) +2 NO (g) + 4 H2O (1)

c) Forming soluble complexes:

If the insoluble compound forms a complex with a reagent used, it will dissolve in it.

AgC1 (s) + 2 NH4OH (aq) Ag(NH3)2+ (aq) + Cl- (aq) + 2 H2O

Al(OH)3 (s)+ NaOH (aq) Al(OH)4- (aq) + Na+ (aq)

13
Procedure: For the following compounds, you will carry out several reactions, and identify
the type of reactions that have occurred.

CuSO4, Na2CO3, Na2SO4, CaCO3, NH4C1,

1) Take a very small amount of the compound (size of a pea), put it in a test tube, use the
solubility rules and classify the compounds as soluble and insoluble. For the soluble ones,
prepare a solution by taking small amount of solid in a test tube and fill it with distilled water.
Shake well to have a homogenous solution.

3) Divide the solution into 3 test tubes

* to the first tube, add 0.2 M Ba(NO3)2 solution
* to the second tube, add 6 M HC1 solution
* to the last one add 6 M H2SO4 solution

Observe any change in the medium, write the reactions, and decide about the type of reaction
that has occurred.

4) If the compound is insoluble in water, try to dissolve it in 6 M HNO3 observe the solution
process well. If the compound dissolves in acid and you have a homogenous solution, repeat
the process in part (3).

5) Get your unknown (which will be one of the compounds listed above), and try to identify it
by using the same process.

14
 SAFETY

CuSO4: Harmful if inhaled or ingested. Copper salts are toxic in large amounts.

Pb(NO3)2 : Toxic if swallowed or inhaled. Lead salts can act as a carcinogen and systemic
poisons, building up in the body over an extended period.

NH4C1: Harmful if swallowed.

Ba(NO3)2 : Poisonous. Harmful if inhaled and in contact with skin and eyes. May be fatal
if swallowed.

HC1: Vapor irritates the respiratory system, eyes, and skin. Liquid burns eyes and
skin. Swallowing results in severe irritation. Avoid breathing the vapor; prevent contact with
eyes and skin.

HNO3: Harmful vapor, causes burns, and irritates the respiratory system. It is an
oxidizing agent, so contact with combustible materials may cause fires, causes severe burns,
prevent contact with eyes and skin.

H2SO4: Concentrated acid causes severe burns. Dilute acid irritates eyes and skin.
Swallowing would cause severe internal damage. Avoid breathing vapor, prevent contact with
eyes and skin.

DO NOT ADD WATER TO A CONCENTRATED SOLUTION, IT GIVES A STRONG

EXOTHERMIC REACTION

15
Name __________________
Partner’s name _______________ Date ________________

Pre Lab questions:

1) List some observations which indicate that a reaction has occurred?

2) How can you prepare BaSO4 in the lab? Which reagents do you prefer to use?

3) Classify the following reactions:

a) 2S + 3 O2 2SO3 __________
b) KC1O3 KC1 + 3/2 O2 __________
c) 2 Al + 6 HC1 2 AlCl3 + 3 H2 __________
d) 2 KOH + CaC12 Ca(OH)2 + 2 KC1 __________

4) Give the formula of a chemical substance which will

a) Dissolve KC1 but not AgCl __________
b) Dissolve CuCO3 but not BaSO4 __________
c) Dissolve FeS and also Ag2O __________
d) Dissolve MgO and also Ba(OH)2 __________

5) Give the formula of a chemical substance which will

a) Give a precipitate with KC1 and also with CuC12 __________
b) Give a precipitate with NaC1 and also with Na2CO3 __________
c) Give a precipitate with AgNO3 but not with Cu(NO3)2 __________
d) Give a precipitate with CuC12 but not with KC1 __________

16
Name __________________
Partner’s name _______________ Date ________________

REPORT II

Report Questions:

1) If the following reactions occur, what will be the products? Complete the reactions.

a) MgCO3 (s) + HNO3 (aq)

b) CuBr2 (aq) + Na2S (aq)

c) Ba (s) + O2 (g)

d) NaC1 (aq) + Zn( NO3)2 (aq)

e) BaSO4 (s) + Na2CO3 (aq)

2) What is a precipitate?

3) What is the first step to identify an unknown compound?

4) a) List 3 pairs of compounds, which will give a precipitate when mixed as

homogenous solutions.

b) List 3 pairs of compounds which will not form a precipitate when mixed in
solution form.

5) a) When is it permissible to taste a chemical?

b) Why should you wear safety glasses during an experiment?

c) What should you do if you spill a chemical on yourself?

17
Name __________________
Partner’s name _______________ Date ________________

REPORT II

salt solubility addition of addition of addition of

H2O/HNO3 Ba(N03)2 HC1 H2SO4

CuSO4

Na2CO3

Na2SO4

CaCO3

NH4C1

Unknown
Name

------------

18
Experiment III : Preparation of Solutions

Purpose: To be familiar with mole, molarity and molar mass concepts and to acquire ability
for preparing solutions.

Theory:

Procedure:
Disssolve 0.58 g nac in 100 ml water
A. Prepare 100 ml of 1 M NaCl solution (Sample 1)
add 12.5 ml water
B. Take half of the solution you have prepared and dilute it to get a solution of 0.8 M.
1Mx50 ml= 0.8
(Sample 2). MxV2

C. Mix 20 ml of Sample 1 with 30 ml of Sample 2. (Sample 3)

D. Fill in the table in report section using the correct units

19
Name __________________
Partner’s name _______________ Date ________________

Report Questions:

Part A
1. How many moles of NaCl should be in 100 ml of solution?

0.1 mol

2. How many grams is it?

5.844 g

Part B
1. How many moles are in half of Sample 1?

0.05 mole

2. How many moles should you have in Sample 2?

0.8mol

3. In what volume of solution should these moles be?

20
Part C
1. How many moles are there in 20 ml of Sample 1?

0.02 mol

2. How many moles are there in 30 ml of Sample 2?

0.024 mol

3. What is the total number of moles and the total volume?

212.5 ml

0.154 mol

4. What is the molarity of the mixture? (Sample 3)

0.88 mol/L

Part D
Sample 1 Sample 2 Sample3
Mass of solute 5.844 g 2.92 g 0.257 g
Volume of solution 100 ml 50 ml
62.5 ml
Molarity of solution 1M 0.8M 0.88 M

21
Experiment IV : Stochiometry of a Chemical Reaction

Purpose: To understand the principles of stoichiometry and the concept of theoretical and
actual yield.

Theory: Mole ratios of reactants, products, their physical states etc. for any chemical reaction
can be obtained from the balanced equation.

2 Ag2O (s) 4Ag (s) + O2(g)

AgNO3 (aq) + NaCl (aq) AgCl (s) + NaNO3 (aq)

For all reactions the reactants are combined in a given ratio, and if one of them is in excess, it
will remain as unreacted in the medium. The reactant which is completely used up in the
reaction is called the limiting reactant; the one which remains is called the excess reactant.
The amount of the product should be calculated according to the limiting reactant.
The amount of the product calculated from the balanced equation of the reaction is the
theoretical yield of that reaction. Most reactions, however, do not go to completion. In
practice we always get less. The amount of the product produced at the end of the reaction is
the actual yield.

actual yield
% yield of the reaction = x 100
theoretical yield

In this experiment the following reaction will be carried out and the percent yield will be
calculated.

FeCl3 (aq) + 3 K2C2O4.H2O (aq) 3 KCl (aq) + K3Fe(C2O4)3.3H2O

Ferric chloride + potassium oxalate potassium chloride + potassium ferritrioxalate trihydrate

22
Procedure:

Synthesis of K3Fe(C2O4)3.3H2O
1. Weigh out 4 g of K2C2O4.H2O into a 100 mL beaker and add 8 mL of distilled water.
Heat to dissolve the compound, do not boil.
2. Measure exactly 4 mL of FeCl3 solution, which is prepared so that it contains 0.4 g of
FeCl3 in one mL of solution. Add the FeCl3 solution into the beaker while the solution
is still hot. The mixture will turn green.
3. The expected product is soluble in hot medium, but forms a precipitate when cooled.
Put the beaker in the ice bath, and wait for complete precipitation.
4. Weigh a filter paper, and then filter the contents of the beaker using a funnel and a
filter paper. The precipitate remains on the filter paper, and the solution is drained off.
Wash the precipitate with small amount of water.
5. Carefully lift out the filter paper, try to take the excess water from it by using a piece
of paper towel.
6. Wait for the compound to dry (preferably overnight) and weigh the product.

Safety:
FeCl3: Corrosive, it can cause burns on the skin. Harmful if swallowed or inhaled.

23
Name __________________
Partner’s name _______________ Date ________________

Pre Lab Questions:

1) In a precipitation reaction, the amount of precipitate is always less than what is expected.
Could you give any reason for this observation?

2) Reaction of 1.5 g of CaCl2 with 3.4 g of AgNO3 gives 2.5 g of AgCl, Write the reaction
and calculate the percent yield of the reaction.
(CaCl2 = 111 g/mole AgNO3 = 170 g/mole AgCl = 144 g/mole)

3) How many grams of ZnSO4 would form by the action of H2SO4 on 52 g of Zn? What will
be the volume of 4 M H2SO4 needed to have a complete reaction?
(Zn = 65 g/mole S = 32 g/mole O = 16 g/mole)

24
Name __________________
Partner’s name _______________ Date ________________

REPORT IV

Report Questions:
1) It would be easier to dry the product in the oven, but we prefer to leave it on the bench and
dry it in open air. What could be the reason for this?

2) Suggest some improvements to this experiment.

3) 3 mL of 0.100 M Pb(N03)2 reacted with 12 mL of 0.100 M K2CrO4 .

Calculate the mass of precipitate, lead chromate (PbCrO4), and also the concentrations of ions
remaining in solution. (PbCrO4 = 323 g / mole)

25
Name __________________
Partner’s name _______________ Date ________________

REPORT IV

Mass of K2C2O4.H2O ____________

Volume of FeCl3 solution used ____________
Mass of filter paper ____________
Mass of filter paper + product ____________
Mass of product ____________

Calculations:

Mass of FeCl3

Moles of FeCl3

Moles of K2C2O4.H2O

Name and number of moles

of the excess reactant

Moles of product collected

Moles of product it the yield

of reaction were 100%

% yield of the reaction

26
Experiment V : Preparing Solutions Through Serial Dilutions

Purpose: To be familiar with mole, molarity and preparation of dilutions to acquire ability for
preparing solutions.

Theory: A dilution is a reduction in the concentration of a solution. A serial dilution is a

series of repeated dilutions that provides a geometric dilution of the original solution. Serial
dilutions are used extensively in biochemistry and microbiology.

Dilution equation M1V1 = M2V2

Procedure A:
• Take 1 ml of 0.1 M HCl put in a test tube.
• Add 9 ml of distilled H2O (dilution I)
• Take 1 ml from first solution add 9 ml of distilled H2O.
• Repeat this steps till (dilution VI)

Procedure B:
• Take 1 ml of 0.1 M NaOH put in a test tube.
• Add 9 ml of distilled H2O (dilution I)
• Take 1 ml from first solution add 9 ml of distilled H2O.
• Repeat this steps till (dilution VI)

27
Name __________________
Partner’s name _______________ Date ________________

REPORT V

Calculated pH Observed pH
0.1 M HCl
Dilution I
Dilution II
Dilution III
Dilution IV
Dilution V
Dilution VI

Calculated pH Observed pH
0.1 M NaOH
Dilution I
Dilution II
Dilution III
Dilution IV
Dilution V
Dilution VI

28
Experiment VI : Formula and Composition of a Hydrate

Purpose: To determine the percentage of water in a hydrated compound and to find the
formula of the hydrate.

Theory: Hydrates are crystalline compounds in which one or more molecules of water are
combined with each formula unit of salt. This water of hydration is not bounded tightly into
the crystalline structure and can be driven off by heating a sample of a hydrate.

If the hydrate is colored, a color change usually results upon heating.

heat
CuSO4.5H2O (s) CuSO4 (s) + 5H2O (g)
blue white
heat
NiSO4.7H2O (s) NiSO4 (s) + 7H2O (g)
green yellow

Most salts are white, so a color change will not be seen.

Some compounds absorb water from the air and form a hydrate spontaneously. These
compounds are known hygroscopic or deliquescent.

In some hydrates, the water of hydration is bonded so weakly that it tends to escape even at
room temperature to form the anhydrous form. Such hydrates are efflorescent.

Procedure:

PART A: Deliquescence and Efflorescence

1. Place a few crystals of Na2SO4.10H2O on a watch glass, and observe its appearances
for about one hour, write the equation.
2. On another watch glass, place a few crystals of sodium acetate (NaC2H3O2), observe
its appearance over at least one hour and write the reaction.

29
PART B: Find the hydrated formula of BaCl2.XH2O

1. Clean a 100 mL beaker or watch glass, and place it in an oven at 250°C-300°C.

2. Wait for 15-20 minutes. Take it out, cool and weigh it carefully.
3. Place 2-3 g of BaCl2.XH2O in it, weigh carefully again, and place it in the oven to
evaporate the water of hydration.
4. After half an hour, take the beaker out, cool ad weigh it.
5. Place it back in the oven for 15 min, take it out, cool and weigh it again. Compare the
results between the two weighings, if there is a big difference; repeat the heating
process once again.
6. Calculate the formula.

30
Name __________________
Partner’s name _______________ Date ________________

Pre Lab Questions:

1. Why must the beaker be cleaned before weighing?

2. Why must the beaker heated and allowed to cool before weighing?

3. What happens if you weigh the beaker while it is still hot?

31
Name __________________
Partner’s name _______________ Date ________________

REPORT VI

Report Questions:

1. Mass percent of water in a hydrate of MnCl2 is 36.41%. Find the formula of the
compound. (MnCl2=126 g/mole, H2O=18 g/mole)

2. Suppose you got a large difference between the two weighing after heating, what
should you do? What happens if you stopped there and calculated the results?

3. 1.500 g of BaCl2.2H2O is heated for a while. Calculate the mass of water removed.
(assuming that the compound is completely dehydrated) (BaCl2=208 g/mole)

4. 2.500 g of hydrated CaSO4 loses 0.523g of water when heated. Calculate the mass
percent of water in the compound and the formula of the hydrate. (CaSO4 = 136
g/mole)

32
Name __________________
Partner’s name _______________ Date ________________

REPORT VI

Part A: Write your observations and explain what happened to the compound.

Part B: Formula of BaCl2.XH2O

Mass of beaker ____________________

Mass of beaker + hydrated BaCl2 ____________________

Mass of hydrated BaCl2 ____________________

Mass of beaker + anhydrous BaCl2 (first weighing) ____________________

Mass of beaker + anhydrous BaCl2 (second weighing) ____________________

Mass of anhydrous BaCl2 ____________________

Moles of BaCl2 ____________________

Mass of water ____________________

Moles of water ____________________

Percentage of water ____________________

Formula of hydrate ____________________

33
Experiment VII : Acid-Base Titrations

Purpose: To introduce volumetric analysis, acid and base reactions, and solution
stoichiometry.

Theory: In certain chemical analysis, it is necessary to determine the concentration of ions in

the solution. This can be done either by using instrumental methods such as atomic adsorption
spectroscopy, ion selective electrodes or by volumetric analysis, in which the volumes of
reactants need to be measured exactly.

The objective in volumetric analysis is to determine the volume of a standard reagent needed
to react completely with the analyte. Some of the terminology used in volumetric analysis is:

Titration is the process in which a solution is added drop by drop from the buret into a
solution in a flask.
Buret is the volumetric glassware used for titration.
Standard solution is a solution with an exactly known concentration.
Standardization is the process to find out the exact molarity of the solution prepared.
Equivalence point is the point where the reactants are in stoichiometric ratio. This is a
theoretical point, which cannot be determined exactly. The aim is to reach the equivalence
point as close as possible. To see the equivalence point an indicator is used.
Indicators are chemical substances which change color depending on the medium.
Some examples are:
Phenolphthalein colorless in acid, pink in base
Methyl orange yellow in acid, pink in base
End point is the point when the indicator changes color, warning to stop titration.
Titration error is the difference between the end point and the equivalence point.

Procedure:

Part A:
1) Clean a buret, rinse it with NaOH solution and then fill it with NaOH solution.

34
 2) Weigh out 0.1 – 0.2 g of KHP exactly and place it in an erlenmeyer flask. KHP is a
monoacidic (only one ionizable H+) compound and has a high molecular weight
(204.23). Add 50 mL of distilled water and 3-4 drops of phenolphthalein indicator.
Shake the contents and make sure that all the solid has dissolved completely.
3) Record the initial buret reading, and start to add NaOH solution from the buret into the
flask drop by drop and observe carefully the point when the color changes to light
pink. This color should stay for at least 30 seconds. Read the buret again and record.

Part B:
1) Procedure will be same as in Part A, except an unknown acid will be used instead of
KHP. Use the molarity of NaOH from part A, and calculate the molarity of the acid.

35
Name __________________
Partner’s name _______________ Date ________________

REPORT VII

Report Questions

1) Define standardization

2) Indicate the difference between end point and equivalence point.

Part A
Mass of KHP __________
Moles of KHP __________
Volume of NaOH used __________
Moles of NaOH __________
Molarity of NaOH __________

Part B
Volume of NaOH used __________
Moles of NaOH __________
Molarity of the acid __________

Calculations and reactions:

36
Experiment VIII : Oxidation Reduction (Redox) Titrations

Purpose: To determine the mole ratio of reactants in a redox reaction.

Theory: Many oxidation reduction reactions serve as a basis for volumetric quantitative
analysis.

Potassium permanganate, KMnO4, is a strong oxidizing agent. Permanganate, MnO4-, is an

intense dark purple color. Reduction of purple permanganate ion to the colorless Mn+2 ion,
the solution will turn from dark purple to a faint pink color at the equivalence point. No
additional indicator is needed for this titration. The reduction of permanganate can be
controlled by the acidity of the medium. To have desired reduction to Mn+2 the reaction is
carried out in dilute H2SO4 solution. Acid prevents the formation of an insoluble MnO2 and
ensures the reduction to Mn+2.

MnO4- + 5e- + 8H+ Mn2+ + 4 H2O

MnO4- + 3e- + 4H+ MnO2 + 2 H2O (not wanted)

In this experiment, permanganate will be reduced by oxalate, C2O42- in acidic conditions.

Oxalate reacts very slowly at room temperature so the solutions are titrated hot to make the
procedure practical. The unbalance redox reaction is shown below.

MnO4- + C2O42- → Mn2+ + CO2

Procedure:
Standardization of a KMnO4 solution

1. Weigh 1 g of KMnO4 exactly and dissolve it in 200 mL of distilled water in a

volumetric flask. The salt dissolves slowly and forms a very dark solution. Be sure to
dissolve completely. Add 25 ml 2 M H2SO4 and complete to 250 mL by adding more
water.

37
2. Fill a burette with the KMnO4 solution to be standardized.
3. Pipette 20 mL of the standard oxalic acid (0.05 M) solution into a 250 mL flask and
add about 20 mL of 2 M H2SO4.
4. Warm the flask to about 80°C and titrate the permanganate solution against the oxalic
acid solution. Add the KMnO4 solution fairly slowly or manganese (IV) oxide (a
brown solid) may form instead of manganese (II) ion. The end point is reached when
the addition of one drop of permanganate solution produces a permanent pink color.
Record your results.
5. Repeat the titrations until consistent results are obtained.

38
Name __________________
Partner’s name _______________ Date ________________

REPORT VIII

Mass of KMnO4 ___________

Molarity of oxalic acid solution ___________

Molarity of KMnO4 _______________

Titrations
Average 1 2
Final reading
Initial reading
Titration volume

Report Questions

1. From the average volume of KMnO4 solution used, calculate the concentration of the
solution.

2. What is the purpose of using H2SO4?

3. Write the overall reaction.

39