Imam Muhammad ibn Saud Islamic University

College of Science
Department of Chemistry

LABORATORY MANUAL
For
GENERAL CHEMISTRY
CHM 101

Collected and Prepared by Chemistry Dept. Staff

Modified and Revised by:
Dr. Abdulrahman G. Alhamzani
Dec, 2023

2nd Semester (1445)

Spring 2024

1
 Table of Contents
Laboratory Rules and safety .............................................................................................................. 3
Some Chemical Hazard Symbols ......................................................................................................... 4
Lab Safety Definitions ......................................................................................................................... 5
Overview of Laboratory Glassware and Apparatus ............................................................................. 6
Experiment 1: Basic laboratory techniques ........................................................................................ 8
Experiment 2: Density of liquids ..................................................................................................... 15
Experiment 3: Density of Solids ...................................................................................................... 19
Experiment 4: The chemical composition by mass percentage ....................................................... 22
Experiment 5: Stoichiometry: Mass to mass relationship ................................................................ 25
Experiment 6: Preparation of primary standard and dilution rules .................................................. 27
Experiment 7: Determination of the empirical formula ................................................................... 31
Experiment 8: Strong acid-strong base titration ............................................................................... 35
Experiment 9: Reactions in Aqueous Solutions ............................................................................... 38
Experiment 10: Precipitation reaction & Limiting reactant ............................................................. 41
Experiment 11: Weak base-strong acid titration .............................................................................. 44
Experiment 12: Vinegar Analysis, Mass % ..................................................................................... 47
Experiment 13: Oxidation reduction reactions................................................................................. 49
Experiment 14: Redox titration of Fe2+ ............................................................................................ 53
Experiment 15: Ideal Gas Law ......................................................................................................... 55
Experiment 16: Determination of the specific heat of metal ...................................................... 59

2
 Laboratory Rules and safety
The following rules are designed for your safety in the laboratory. The Laboratory Supervisor
is required to enforce these rules and has the full backing of the Department of Chemistry Staff
and Faculty. Violations of these rules will result in expulsion from the laboratory.
1- Approved safety goggles must be worn by all persons at all times.
2- Lab Coats of 100% cotton are required upon entering lab.
3- Eating, drinking, and smoking are strictly prohibited in the laboratory at all times.
4- Closed-toe, closed-heel shoes that cover the entirety of the foot must be worn at all times
(sandals are not allowed)
5- Clothing that completely covers your arms and legs must be worn at all times in the
laboratory.
6- Confine long hair while in the laboratory. Hair can catch on fire while using open flames
7- Avoid rubbing your eyes unless you know that your hands are clean.
8- Never taste anything. Never directly smell the source of any vapor or gas. Instead, use your
fingers to waft the odor to your nose
9- Do not touch chemicals with your hands. Spatulas will be provided for handling solid
materials.
10- Do not sit on the lab benches.
11-Do not pour any chemicals into a sink without authorization from the instructor
12- Learn the location and how to operate the nearest eyewash fountain, safety shower, fire
extinguisher, and fire alarm box.
13-Mouth suction must never be used to fill pipets. Always use a bulb to fill pipets
14- Consider all chemicals to be hazardous unless you are instructed otherwise
15-You may use gloves
16- The student must have at least ONE UNGLOVED HAND when outside the laboratory. Only
use the ungloved hand to open doors
17- Keep your working area clean
18- Do not put chemicals back into reagent bottles, this may contaminate the reagent. Never
return excess material to reagent bottles.
19-All accidents, injuries, explosions, or fires must be reported at once to the lab supervisor.
20-Do not wear contact lenses in the laboratory
21- If a chemical gets on your skin, immediately wash the affected area with large quantities
of water.
22- Visitors are not permitted in lab.
23-Always pour acids into water, not water into acid, because the heat of solution will cause
the water to boil and the acid to spatter
24- Put all toxic or flammable waste into the appropriate waste container(s) provided in your
laboratory.
25- Never use reagents from unmarked (not labeled) bottle,

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Some Chemical Hazard Symbols

4
 Lab Safety Definitions
Carcinogen: The substance has been found to cause cancer in animals or humans.
Caustic The substance is a strong base. Caustic substances cause burns to human
flesh and eat holes in clothing.

Corrosive The substance is a strong acid Corrosive substances cause burns to human
flesh. They also break down certain fibers (including cellulose, the polymer
found in cotton).

Flash point The temperature at which the vapor above a liquid forms an explosive
mixture with air. Ignition results in a flash (or explosion) rather than a flame

Irritant The substance will irritate skin, eyes or mucous membranes. The fumes may
cause you to sneeze.

Mutagen The substance causes genetic damage (mutations) to cells with which it
comes in contact. Mutagens in the bloodstream can adversely affect germ
cells, causing genetic defects in offspring. Normally we will not use known
mutagens.
Pyrophoric Pyrophoric materials ignite spontaneously in air below about 45oC. They
will also ignite nearby inflammable materials.

Smelly The substance has an objectionable odor. Smelly substances should be

handled only in the hood: this includes cleaning glassware contaminated
with them. If they need to be weighed. They must be weighed in closed
containers
Teratogen The substance causes developmental abnormalities in unborn babies:
therefore, pregnant women should not be exposed to it. We do use some
suspected teratogens: if you think you might be pregnant you should inform
the instructor immediately.
Toxic The substance is poisonous.
Mutagen The substance causes genetic damage (mutations) to cells with which it
comes in contact. Mutagens in the bloodstream can adversely affect germ
cells, causing genetic defects in offspring. Normally we will not use known
mutagens.

5
Overview of Laboratory Glassware and Apparatus

6
7
 Experiment 1: Basic laboratory techniques
Introduction:
In this experiment, you will practice some laboratory techniques and apply laboratory safety
rules. You will determine the mass of different solid materials and measure the volume of a
liquid, you are expected to be familiar with how mass and volume measurements are carried
out and how an evaluation of the measurements is reflected in the number of significant figures
recorded.

(A) Mass Measurement:

The balance is used to determine the mass of an object. The centigram balance is conveniently
used when an accuracy of 0.01g is required.

Figure 1. Balances in Chemistry Labs

• The top loader balances are precise enough to read ± 0.001g.

• The analytical balances are the most accurate balances commonly used in the modern
laboratories for accurate quantitative work (with accuracy± 0.0001g).
Certain general rules must be followed to have long life for balance
1. Keep the balance and the area near balance clean.
2. Tare (zero) the balance prior to taking any measurements.
3. Never place any chemical directly on the balance pan: always use a
piece of weighing paper. Liquids must be weighed in a closed container.
4. Never take the mass of hot objects (only at room temperature)

Procedure
1. Zero the balance after cleaning the pan.
2. Measure the mass of a clean dry 50 mL beaker to the nearest ± 0.001g
3. Remove the beaker from the pan. Again, clean the balance pan and zero the balance.
4. Weigh the same beaker as before (step 2) and record the result.
5. Repeat steps 3 and 4 one more time.
6. From the three mass measurements, calculate the average mass of the beaker.
7. Repeat steps 3 and 4 using a second balance (just one weighing).

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B- Measuring liquid volumes
Many laboratory glassware are used for liquid volume measuring.

Figure 2. Class ware for Liquids measurements

9
How to read the volume from graduated cylinder and burette?
When liquid is placed into a burette or graduated cylinder, a meniscus is formed. This is a
curved layer of liquid (either curved up as in mercury or down as in the case of water). A
volume is read at the very bottom (or very top) of the meniscus, as can be seen in Figure1-1
below. Properly reading the meniscus will provide you with the volume of the liquid contained
in the graduated cylinder or burette.

Figure 3. Reading volume in Cylinder or Burette

Figure 4. Types of meniscus.

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Procedure
1- Take a 50 ml graduated cylinder, place it on the balance pan, zero the balance.
2- Add distilled water to the graduated cylinder (add gradually) to 30.5 g
3- Read the volume (record the volume with the proper significant figures)

(C) Length measurement

The same length (of the same object) can be measured to different significant figures
according the device of measurements. Look at the ruler measurements shown below,
the length can be 0.6 m in (a), 0.61 m in (b), or 0.607 m in (c). It depends on the degree
of precision. The total number of digits in a given number, including the last digit
whose value is uncertain, are called the Significant figures.
In (a) you have 1 significant figure, in (b) you have 2 Sig. Fig., and in (c) you have 3 Sig.
Fig.

Procedure
You will be given several measuring devices allowing you to measure the length of
various objects in the lab.

D- Simple filtration (Gravity)

Gravity filtration is the simplest method of separating a solid from a liquid, after
selection of a funnel and receiver of a size which is appropriate for the quantity of
liquid to be filtered, the filter paper should be prepared; fold the paper in two then
refold in the same direction matching up the previous fold. Continue in this way until
four folds have been produced. Turn the paper over and matching up the previous
folds continue to make another four folds. Then press the folds together until the paper
forms a cone (this process is shown in the figure below). place the filter paper in the
funnel and wet it with small amount of water(solvent),

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Decant a portion of the liquid down a glass rod held vertically above the center of the
filter paper (Figure 1-3), do not fill the funnel (2/3 only), allow the filter paper enough
time to dry.

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Procedure:
1- Weigh exactly 5.00 g of sand (silica).
2- Transfer to a 200 ml beaker, add 100 ml distilled water
3- Filter the solid (un dissolved) sand, use a pre-weighed filter paper
4- Dry the sand in the oven
5- Take the mass of sand, calculate the recovery of the process.

𝒐𝒃𝒕𝒂𝒊𝒏𝒆𝒅 𝒎𝒂𝒔𝒔
𝑹𝒆𝒄𝒐𝒗𝒆𝒓𝒚 = × 𝟏𝟎𝟎
𝟓. 𝟎𝟎 𝒈

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 Helpful information for this experiment:

Table1: Equipment Accuracy

Equipment Accuracy
Top-loading balance ±0.001 g
Analytical balance ±0.0001 g
Beakers ± 1 mL or more
Graduated cylinder ±0.1 mL
Pipette ±0.02mL
Burette ±0.02mL

Table 2: SI units of measurements

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 Experiment 2: Density of liquids

Objectives:

✓ To determine the density of known liquids (water, ethanol, acetone).

✓ To identify an unknown liquid by determining its density.
✓ To compare the accuracy and precision of various types of volumetric glassware.

Materials Needed:
10-mL pipette and pump 100-mL (or 50 mL) graduated cylinder
50-mL beaker Eyedropper
Samples of known and unknown liquids Top-loading balance or analytical balance

Introduction:
Density is an intensive physical property obtained by dividing the mass of a material or object
by its volume (i.e., mass per unit volume).

𝑚𝑎𝑠𝑠 (𝑔)
𝐷𝑒𝑛𝑠𝑖𝑡𝑦 =
𝑣𝑜𝑙𝑢𝑚𝑒 (𝑚𝐿)

The SI base unit of mass is Kg and the volume unit is cubic meters (m3), but chemists generally
express mass in grams (g) and volume in cubic centimeters (cm3) or milliliters (mL).
The most commonly encountered density unit, then, is grams per cubic centimeter (g/cm3), or
the identical grams per milliliter (g/ml).

The mass of 1.000 L of water at 4 0C is 1.000 kg. Therefore, the density of water at 40C is:
1000𝑔
𝑑= = 1.000 𝑔/𝑚𝐿
1000 𝑚𝐿

However, at 20 0 C, the density of water is 0.9982 g/ml. The density of liquids is affected by
temperature.

Accurate measurements of volume and mass are very important in this experiment. Should a
mass or its constituent volume be misread, this affects the density calculation.
Once you determine a density experimentally, you will need to evaluate the precision and
accuracy of your results. We shall use a calculation called percentage to express precision and
a calculation called percent error to express accuracy. The necessary formulas are:

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Procedure:

Liquid Sample:
1. Measure the mass of empty 100-mL graduated cylinder onto a digital balance. Record the
mass (m1)
2. Pour 100 mL of water into the graduated cylinder. Try to be as accurate as possible by
checking that the meniscus is right at the 50-mL mark. Use a dropper to add or remove small
amounts of water.

3. Weigh the graduated cylinder with the water in it. Record the mass in grams (m2).
4. Find the mass of only the water by subtracting the masses. Mass of water = m2-m1. Record
the mass of 100 mL of water in the chart.
5. Use the mass and volume of the water to calculate density. Record the density in g/cm3 in
the chart.
6. Pour off water until you have 50 mL of water in the graduated cylinder. If you accidentally
pour out a little too much, add water until you get as close as you can to 50 mL
7. Find the mass of 50 mL of water. Record the mass in the activity sheet. Calculate and record
the density.
8. Next, pour off water until you have 25 mL of water in the graduated cylinder. Find the mass
of 25 mL of water and record it in the chart. Calculate and record the density.
9. Record your results in the table in results sheet.
10. Graph the variation of the mass vs. the volume of each liquid density.
11. Calculate the slope.

12. Calculate the average density value.

13. Calculate the % Error and % Range for your density values.
Unknown liquid sample:
1. Repeat the above steps using the unknown liquid.
2. To identify your unknown liquid, compare our results to those in the table on the last page
of this hand-out.
3.Use the data in Table 3 to identify your unknown liquid.

Note: you can repeat the procedure using a 50 ml burette; this will give more accurate results.

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 Report Sheet (Exp 2)
Student Name: …………………………………………………
Experiment Title: …………………………………………………………………..

Density of different volumes of liquid (water)

Volume of water 100 mL 50 mL 25 mL
Mass of graduated cylinder + water (g)

Mass of empty graduated cylinder (g)

Mass of water (g)

Density of water (g/mL)

Average density =

% range of density =

% error of density =

Volume vs Mass of water

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Density of unknown liquid using graduated cylinder.

Volume of water 100 mL 50 mL 25 mL

Mass of graduated cylinder + unknown liquid (g)

Mass of empty graduated cylinder (g)

Mass of unknown liquid (g)

Density of unknown liquid (g/mL)

Average density =

Identify your unknown? …………………………………………………………………………………………

% range of density =

% error of density =

Densities of some common liquids at 25 ͦ C

Liquid Density ( g/mL)

Water ( at 25 C) 0.9970
Acetic acid (4% solution) 0.9803
Olive oil 0.9100
Benzene 0.8760
Rubbing Alcohol 0.800
1, 2-ethanediol 1.1135
Glycerin oil 1.261
Corn oil 0.900
Gasoline 0.670

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 Experiment 3: Density of Solids
Objectives:
✓ To determine the density of unknown regular and irregular solids
✓ To identify an unknown metal by determining its density

Materials Needed:

100-mL (or 250 mL) graduated cylinders. 50-mL beaker

Samples of regular and irregular solids. Ruler
Top-loading balance or analytical balance.

Introduction:

The density of a substance is defined as its mass per unit volume. However, the specific gravity
of a substance is defined as the ratio of the mass or weight of the substance to the mass or
weight of an equal volume of water and is a pure number having zero dimensions (unitless). A
convenient method for determining densities or specific gravities is one which uses the
principle of Archimedes, namely, that when a body is immersed in a fluid there is exerted on
the body a vertical upward force equal to the weight of fluid displaced. For solid substances
that have specific gravity more than water, they will sink in water so it is easy to determine
their volumes, for regular solids (geometrical) their volume can be measured according to
their shape.
Cylindrical shape objects: volume = π r2h

Cubic shape objects: Volume = (length x width x height) = r3

Spherical shape: Volume = 4/3 π r3

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Procedure:

(1) Regular (Geometrical)Solid:

1. Record your sample number (or letter).

2. Determine and record the mass of your sample using a digital scale.
3. Determine (calculate) the volume of your regular solid sample using the appropriate
equation according to the shape of your sample.
4. Calculate the density of your sample and record this value in the data table.
5. Compare the density of your sample with those listed in table 1, identify the elemental
composition of your solid.

(2) Irregular Solid

1. Record your sample number (or letter).

2. Determine and record the mass of your sample (be sure it’s dry).
4. Add approximately 50 mL of water to a 100 mL graduated cylinder (or 30 mL water to a 50
mL graduated cylinder).
5. Read and record the exact water volume.
6. Carefully place your sample in the graduated cylinder with the water. Gently agitate the
graduated cylinder to eliminate trapped air bubbles.
7. Read and record the new water volume. This is the volume of the water and the metal
sample.
8. Calculate the volume of your sample by subtracting the final water volume (with metal)
from the initial water volume (no metal).
9. Calculate the density of your sample.

Table 1. Densities of some elements.

Element Density(g/mL)
Aluminum 2.7
Copper 8.92
Iron 7.874
Lead 11.34
Nickel 8.91
Silver (Ag) 10.49
Tin( Sn) 7.31
Zinc (Zn) 7.14

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 Report Sheet (Exp 3)
Student Name: ……………………………………………………. ID …………………………………….
Experiment’s Title: …………………………………………………………………………………………

1-Density of regular solid:

Description of your solid: (Cylinder, Cube, or Spherical shape)

Length Radius Volume Mass Density

Identity of metal: .........................................................................................................

% error in density: .....................................................................................................

Note: Consider the significant figures in your calculation and pay attention for units of
measurements

Description of solid: (Cylinder, Cube, or Spherical shape)

Side length Mass Volume Density

Identity of metal:........................................................................................................

% error in density:.....................................................................................................

2- Density of irregular solid

Physical description of the solid: .................................................

Trial Mass (g) Volume (mL) Density (g/mL)

1

Average
density

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 Experiment 4: The chemical composition by mass percentage
Objectives:
✓ To determine the percent, by mass, of water in a hydrated compound
✓ To Determine the chemical formula of the unknown hydrated compound

Materials Needed:
− One of these chemicals: (CuSO4 · 5H2O, BaCl2 · 2H2O, MgSO4 · 6H2O, Na2CO3 · 2H2O, or
Na3PO4 · 12H2O
− Crucible
− Oven
− Top-loading balance or analytical balance

Introduction:

A hydrated salt is a solid ionic compound that contains water molecules within its crystalline
lattice structure. When ionic compounds are prepared in water solution and then isolated as
solids, the crystals often have molecules of water trapped in the structure. Frequently, the
water is chemically bonded less tightly than other bonds within the compound. By heating the
hydrated salts, all of the water is released from the solid and evaporated. The compound
remaining after evaporating all of the water is called the anhydrous compound, a substance
that is “without water.” The mass of the original hydrate must equal the sum of the mass of
water driven away and the mass of the anhydrous compound left behind.

For example, suppose you heated 1.0 g of BaCl2‫ ﮲‬xH2O, after heating you are left with 0.860g
of the anhydrous compound, then the mass of water is the difference:

• (lost) = 1.0 - 0.863 = 0.137 g

• moles of H2O = 0.137 ÷ 18 = 0.0076 mol
• moles of anhydrous (BaCl2) = 0.860 ÷ 208.23 = 0.0041mol
• ratio of H2O : BaCl2
0.00778 : 0.0041
2 : 1
• So, the formula is: BaCl2 • 2H2O
• The mass % of H2O = (0.137 ÷ 1) × 100 = 13.7 %
• theoretical % H2O = [(2 x 18) ÷ 244.26] × 100 = 14.7 %

Procedure:
1. Weigh and record the mass of a clean and dry crucible using a top loading balance (w1).
2. Obtain an unknown compound. The unknown compound may be one of the followings:
(MgSO4•6H2O, CuSO4•5H2O, MnSO4•H2O, or Na2CO3•2H2O).
3. Add 1 g of the unknown compound into the crucible and Weigh (w2).

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4. Place the crucible containing the sample on the oven 100 oC. and heat for 30-40 min.
5. Then, remove the crucible out the oven, and allow it to cool for 10 min.
6. When the crucible is no longer hot, weigh and record the mass of the crucible with lid and
sample (w3).
7. Determine the chemical formula of the unknown compound.

% water in the compounds

Compound % water

CoSO4 · 6H2O (6 ×18) / [(6 ×18+ 4(16) +32.0+58.9)] × 100%= 41%

BaCl2·2H2O (2 ×18) / [137.3+2(35.45) +2(18)] = 14.7%

MgSO4·6H2O (6 ×18)/ [ 24.3+32.065+4(15.99) +6(18)] =47.3%

Na3PO4·12H2O 12(18)/ [3(22.98) +(30.97) +4(15.99) +12(18)] = 56.9%

CuSO4·5H2O 5(18)/ [5(18) + 4(15.99) +32.06+63.54)] = 36%

Na2CO3·2H2O 2(18) / [2(22.98) +12 = (3 ×16) + 2(18) = 25.3%

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 Report Sheet (Exp 4)

Student Name: …………………………………………………………

Experiment’s Title: ……………………………………………………

▪ Mass of crucible (w1)

▪ Mass of crucible + compound (w2)

▪ Mass of compound wc = (w2 – w1)

▪ Mass of crucible + compound after heating (w3)

▪ Mass of water ww = wc – w3

▪ % water = (ww / wc ) × 100

▪ Identify your compound?

▪ % error of water content:

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 Experiment 5: Stoichiometry: Mass to mass relationship
Objectives:
▪ To verify experimentally the mass and mole relationships between reactants and products.

Materials Needed:
small beakers Tong Glass rod
burette Gradated cylinders Top loading balance
Solid, pure NaHCO3, solution of 0.5M Na2CO3 solution of 0.5M CaCl2
Solution of 3M HCl

Introduction:
The mass to mass relationship is used to predict the amount of product that results when
using specific amount of reactant in known chemical reaction. In this experiment one reactant
is the solid NaHCO3, and the other is the solution of HCl which should be added gradually to
dissolve all the solids of NaHCO3. The calculations will rely on the amount of solid NaHCO3.

NaHCO3 (s) + HCl(aq) → NaCl(aq) + H2O(l) + CO2 (g)

According to the balanced equation 1 mole NaHCO3 produces 1mole of NaCl (using HCL in
excess). In term of mass stoichiometry, 84 grams of NaHCO3 produces 58.4 grams of NaCl.

Another reaction will also be studied by the same method. However, because one product
here is insoluble we will start with aqueous solutions of both reactants.

CaCl2 (aq) + Na2CO3→ CaCO3(s) + 2NaCl

In this reaction 1mole CaCl2 produces 1 mole CaCO3 , by using excess Na2CO3 then 110.98 g
CaCl2 produce 100.08 g CaCO3

Procedure:
Part A: Reaction of NaHCO3 with HCl
1- Measure the mass of a small clean and dry Erlenmeyer flask.
2- Add about 1.0 g of NaHCO3 to the flask, and re-mass the flask and record the exact mass of
NaHCO3 to the nearest 0.001 g.
3- Use dropper to add about 2-3 ml of 3M HCl, drop by drop, until all bubbling stops., add 10
more drops.
4- Evaporate your solution, using a hot plate, to dryness.
5- Allow the flask to cool, take its mass again.

Part B: Reaction of CaCl2 with Na2CO3

1- Take a small, clean and dry beaker
2- From burette No.1 add exactly 10 ml of 0.5M CaCl2 solution.
3- From burette No.2 add 15 ml of 0.5M Na2CO3 solution, to the same beaker
4- Stir your solution for about 1 minute (using glass rod)
5- After settling the precipitate, perform a simple filtration on a pre-weighed filter paper
6- Dry the precipitate and filter paper in the oven for 1 hour.
7- Measure the mass of filter paper and precipitate.

25
 Report sheet (Exp 5)
Student Name: ……………………………………………………………………. ID ………………………………………….
Experiment’s Title: ……………………………………………………………………………………………………………..

Part A:
1- Mass of empty Erlenmeyer flask

2- Mass of Erlenmeyer flask and NaHCO3

3- Mass of NaHCO3

4- Mass of Erlenmeyer flask and product (NaCl)

5- Mass of product (NaCl)

6- Theoretical mass yield of NaCl:

(58.4 ÷ 84) × mass NaHCO3 (step 3) =

7- Percentage yield:
(step5 ÷ step 6) × 100 =

8- Show the calculation for the theoretical mass based on moles stoichiometry
....................................................................................................................................................................................................
....................................................................................................................................................................................................
....................................................................................................................................................................................................
....................................................................................................................................................................................................

Part B:
1- Moles of CaCl2 in 10 ml (M × V) =
2- Mass of CaCl2 in 10 ml
(moles × M mass) = ( step1 × 110.98 g/mol)=

3- Mass of filter paper

4- Mass of filter paper and product (CaCO3)

5- Mass of CaCO3 (step4 - step3)

6- Theoretical yield of CaCO3

(100.08 ÷110) × mass CaCl2 (step 2)
7- Percentage yield:
(step5 / step 6) × 100%

8- Show the calculation for the theoretical mass based on moles stoichiometry
....................................................................................................................................................................................................
....................................................................................................................................................................................................
...................................................................................................................................................................................................

26
 Experiment 6: Preparation of primary standard and dilution
rules
Objectives:

• To prepare and standardized the exact concentrations of primary standard

• To apply the roles of dilution

Materials Needed:
Beakers Gradated Volumetric flask Erlenmeyer Burettes
cylinders flask
Top loading Methyl orange phenolphthalein
balance indicator indicator

- Highly pure Na2CO3

- Unknown 0.3M HCl solution (must be diluted)

Introduction:

Primary standards are chemicals usually salts or acid salts of high purity, they
are stable, non-hygroscopic and have a reasonable high molecular weight. A primary
standard can be used to make a standard solution whose concentration is accurately
known. Potassium hydrogen phthalate (KHP): KHC8H4O4, mol wt. = 204.23 g/mol is
very well known as a primary standard acid used for the titration of base, while the
sodium carbonate (Na2CO3, mol wt. = 105.99 g/mol) is known as a primary standard
for the titration of acids.
In this experiment, a standard solution of sodium carbonate (Na2CO3) will be
prepared and used to determine the exact concentration of a hydrochloric acid
solution (HCl). This equation is used to calculate the molarity of the prepared solution:
𝑚𝑎𝑠𝑠 1
𝑀= ×
𝑀. 𝑚𝑎𝑠𝑠 𝑉𝑜𝑙𝑢𝑚𝑒
The neutralization of sodium carbonate by hydrochloric acid is a two-step
process: . In the first step, one mole of sodium carbonate reacts with one mole of
hydrochloric acid:

In the first step, Na2CO3 (aq) + HCI (aq) → NaHCO3 (aq) + NaCl (aq)
In the second step NaHCO3 (aq) + HCI (aq) → NaCl (aq) + CO2 (g) + H2O (l)
Over all equation Na2CO3 (aq) + 2HCI (aq) → 2 NaCl (aq) + CO2 (g) + H2O (l)

Each of these reactions has an equivalence point. The pH at the first equivalence point
of this reaction happens to correspond very closely to the pH range where
phenolphthalein changes color, but is well above the pH range of methyl orange. The
27
pH at the second equivalence point of this reaction happens to correspond very closely
to the pH range where methyl orange changes color, but is well below the pH range of
phenolphthalein. The overall reaction can be written as:

Na2CO3 (aq) + 2HCI (aq) → 2 NaCl (aq) + CO2 (g) + H2O (l)

The calculation based on the second equivalent point, 1mole of Na2CO3 reacts with 2 moles of
HCl.

Procedure:
PART A: Preparation of known molarity of Na2CO3
1- Weigh exact mass (in the range 0.25 to 0.4 g) of pure Na2CO3 (record exact weight to three-
digits).
2- Transfer your sample into 100-mL volumetric flask. Make sure you transfer all of your
sample (Na2CO3, M. mass (106 g/mole).
3- Add about 50 mL water, and dissolve the sample by shaking. Be sure that your sample is
completely dissolved.
4- Fill the flask to within about 1 cm of the calibration mark, and then add the water dropwise,
using a dropping pipette, as shown in the figure belowJ:

Figure 5. Filling Volumetric flask.

5- Stopper the flask and invert it several times to ensure a homogeneous (evenly mixed)
solution.
6- Calculate the molarity of Na2CO3 solution.

PART B: Dilution of Concentrated acids

7- Take about 3 to 5 mL of the concentrated HCl, 3M, and transfare it into 100-mL volumetric
flask, then add water until the calibration mark.
8- Calculate the molarity of the prepared HCl by using the dilution rule:
Mconc. × Vconc. = Mdil. × Vdil.

PART C: Titration the diluted acid with Na2CO3

9- Clean and wash a burette using your diluted HCl solution, then Fill the burette with your
diluted HCl solution, take the initial HCl reading(usually start from zero).
10- Pipette 20 ml of the Na2CO3solution, and transfer it into Erlenmeyer flask, add few drops
of phenolphthalein indicator.
28
11- Titrate the Na2CO3 solution ( in Erlenmeyer flask) to the colorless solution (endpoint 1).
12- Add few drops of methyl orange indicator to the Erlenmeyer flask, and continue the
titration to the second end point (color changes from yellow to red).
13- Read the volume of HCl.
14- Repeat the titration for two more samples of Na2CO3 solution.

29
 Report Sheet (Exp 6)
Student Name: ………………………………………………………………………………………………………….
Experiment’s Title: …………………………………………………………………………………………………..
PART A: Preparation of known molarity of Na2CO3
• Mass of pure Na2CO3 = …………………… g
• Mol. mass of pure Na2CO3 = …………………… g /mol
• Volume of volumetric flask = …………………… L
• Calculate the Molarity of pure Na2CO3 = …………………… M
𝑚𝑎𝑠𝑠 1
𝑀𝑜𝑙𝑎𝑟𝑖𝑡𝑦 = ×
𝑀. 𝑚𝑎𝑠𝑠 𝑉𝑜𝑙𝑢𝑚𝑒
PART B: Dilution of Concentrated acids
Use the following equation to calculate the concentration (molarity) of diluted HCl.
M conc. × V conc. = M dil. × V dil.
• Volume of Conc. HCl =
• Concentration of Conc. HCl =
• Concentration of dil. HCl =
• Volume of dil. HCl =
………………………………………………………………………………………………………………………………………………………
………………………………………………………………………………………………………………………………………………………
………………………………………………………………………………………………………………………………………………………
………………………………………………………………………………………………………………………………………………………

PART C: Titration the diluted acid with Na2CO3

Trail No. Volume of Moles of Volume of Moles of HCl Conc. of Concentration

Na2CO3 Na2CO3 diluted HCl (mol) diluted HCl of original
(mL) (mol) (mL) (mol/L) HCl(mol/L)

1
2
3
Average of Concentration
Show the calculations:
………………………………………………………………………………………………………………………………………………………
………………………………………………………………………………………………………………………………………………………
………………………………………………………………………………………………………………………………………………………
………………………………………………………………………………………………………………………………………………………

30
 Experiment 7: Determination of the empirical formula
Objectives:
• Determine the expected formula for the ionic oxide when Mg reacts with O 2
• Find the theoretical and actual yields of MgxOy
• To evaluate possible sources of errors

Materials Needed:
- Magnesium turnings or ribbon
- Porcelain crucibles
- Bunsen burner
- Beakers
- Top loading balance
-Distilled water bottle

Introduction:

When magnesium and oxygen are heated together, they readily undergo a chemical
change (reaction):

magnesium + oxygen → magnesium oxide (1)

From the masses of magnesium and oxygen that combine, we can calculate the
empirical formula of magnesium oxide. If magnesium is heated in open air, its
reaction with oxygen is rapid and spectacular. The metal catches fire, burning with an
intense white flame and with production of white smoke. We can slow down the
reaction by limiting the supply of oxygen that reaches the magnesium by putting a
cover on the crucible that contains the magnesium sample.
Our procedure in this experiment is complicated by another fact. Magnesium is
such an active metal that it reacts with the relatively inactive element nitrogen to form
magnesium nitride. This occurs in competition with the reaction of magnesium with
oxygen, so it is called a "side reaction. We add water to the crucible contents at the end
of the first heating period to decompose magnesium nitride( reaction 2) and then we
heat again to speed up the decomposition of magnesium hydroxide (reaction 3) and to
evaporate any excess water.

magnesium nitride + water → magnesium hydroxide + ammonia (2)

magnesium hydroxide → magnesium oxide + water vapor (3)

we add water to the crucible contents at the end of the first heating period. We then
heat again to speed up reactions (3) and (4) and to evaporate any excess water.

Procedure
31
1. Heat a clean, dry porcelain crucible with cover on a clay triangle (supported on a
ring stand), using a direct flame, for about 3 minutes. This is to make certain that the
crucible is dry.

2. Turn off the burner, and let the crucible and cover cool. Leave the crucible and
cover resting on the clay triangle.

3. Weigh the empty, dry crucible and cover on the digital balance.

4. Weigh about 0.3 g of magnesium metal( should be shine), place in the crucible, and
weigh the crucible, lid and magnesium together.

5. Heat the crucible gently for 5 minutes, Use your crucible tongs to lift the cover
slightly every 30 seconds to admit air. If the Mg starts glowing brightly when the cover
is lifted, quickly cover the crucible, remove the Bunsen burner, and wait one minute
beforecontinuing to heat.

6. Heat the covered crucible strongly for 15 minutes, lifting the cover occasionally.
7. Continue heating, as necessary, to completely react the magnesium (to form white
ash), then allow the crucible to cool.

8. To the contents of the cooled crucible, add 10 drops of deionized water.

9. Partially cover the crucible (leave a slight crack) and heat gently for 2 minutes, then
heatstrongly for 10 minutes. Allow the crucible and contents to cool to room
temperature.

10. Weigh the crucible and contents (magnesium oxide).

32
 Report sheet (Exp 7)
Student’s Name: …………………………………………………………
Experiment’s Title: ………………………………………………………………………..

Empirical Formula

Trial Mass of Mass of Mass of Mass of Mass of Mass Moles Moles Empirical
No. empty crucible magnesium crucible product of of Mg of formula
crucible and lid (g) and lid (g) oxygen (mole) oxygen
and lid with with (g) (mole)
(g) magnesium product
(g) (g)
1

Hints:
Mass of magnesium = column3- column2
Mass of product= column5 -column2
Mass of oxygen = column6-column 4

Show in details, a sample calculation:

.....................................................................................................................................................................................
.....................................................................................................................................................................................
.....................................................................................................................................................................................
.....................................................................................................................................................................................
.....................................................................................................................................................................................
.....................................................................................................................................................................................
.....................................................................................................................................................................................
.....................................................................................................................................................................................
.....................................................................................................................................................................................
.....................................................................................................................................................................................
.........................................................................................................................................................................

33
Questions:
1. The percent by mass composition of a salt was found to be 56.58% potassium,
8.68% carbon, and 34.73% oxygen. What is the empirical formula of this salt?

2. A compound containing iron and sulfur was formed by combining 2.233 g of iron
with 1.926 gof sulfur. What is the empirical formula of the compound?

34
 Experiment 8: Strong acid-strong base titration
Objectives:
• To know how to perform the strong acid-strong base titration
• To know how to determine and observe the end point
• To calculate the concentration of unknown NaOH solution.

Materials Needed:
- Burette - Pipette - Beakers - Gradated cylinders
- x M HCl solution (unknown concentration)
- 0.05 M NaOH solution (exact concentration)
- 0.5 % phenolphthalein indicator
Introduction:
Acids were first recognized as a class of substances that taste sour, for example lemon juice
and vinegar are considered as acids because of their sour taste due to their contents of citric
acid and acetic acid, respectively.
Bases, sometimes called alkalis, are characterized by their bitter taste and slippery feel to the
touch (e.g., soap).
Bronsted-Lowry definition of acids and bases, acid is a "proton donor" and base is a "proton
acceptor". For example, when an acid HA dissolves in water, the following reaction occurs:

HA + H2O  A- + H3O+
The acid HA loses its proton to produce A-(conjugate base), while water acts as a base, it
accepts the proton and produces H3O+ (conjugate acid).

Some examples of strong acids: HCl, HNO3, HClO4, HBr, HClO3 and HI.
Some examples of strong bases include all hydroxides of group IA (LiOH, NaOH, KOH .......) and
some hydroxides of group IIA such as Ca (OH)2, and Ba (OH)2.
Acid-Base titration (or neutralization reaction) is the determination of the concentration of an
acid or base by exactly neutralizing it with a base or an acid of known concentration.
As illustrated in the figure below:

Figure 6. Illustration of titration setup

35
The acid is usually placed in a titration flask (Erlenmeyer flask) and the base in a burette. The
solution in the burette is called the titrant. The titrant is delivered from the burette to the
titration flask until the solution in the flask is neutralized.
The phenolphthalein indicator is added to the acid in the receiver. The titration is started by
adding base from the burette until pink color appears (end point). End point is the
neutralization point in the strong acid -strong base titration.
In this experiment, an unknown solution of NaOH will be titrated with known
concentration of HCl solution.
Chemical equation of this reaction is HCl (aq) + NaOH(aq) → NaCl(aq) + H2O(l)
Ionic equation is H+ + Cl- + Na+ + OH- → Na+ + Cl- + H2O(l)
The net ionic equation is H+ + OH-→ H2O(l)

Procedure:

1-Wash a 50-mL burette with water and distilled water.

2- Using a clean funnel, fill the burette with the NaOH solution.
3- Check for the presence of bubbles or empty space at the end of burette.
4- Read the volume by viewing the bottom of the meniscus with the aid of a black line drawn
on a white card. (initial volume).
5-Pippet exactly 20 ml of your unknown HCl solution into Erlenmeyer flask.
6- Add few drops of phenolphthalein indicator to the HCl solution.
7- Place a sheet of white paper beneath the Erlenmeyer flask (HCl).
8- Slowly add the NaOH titrant to the HCl solution in the Erlenmeyer flask.
9- Continue addition of the NaOH until the appearance of pale-pink color. The color persists
for 30 seconds).
10- Read the final volume of burette, and record it in the results sheet
11- Repeat the procedure for more two samples of HCl solution.
12- Calculate the concentration of your unknown HCl solution.

36
 Report Sheet (Exp 8)
Student Name: …………………………………………………………….. ID ………………………………
Expr. Title: …………………………………………………………………………………………………………

Trial Initial Burette Final Burette Vol. NaOH Moles NaOH Vol. HCl Moles HCl Molarity
No. Reading Reading (mL) (mol) (mL) (mol) HCl
(mol/L)

1 20

2 20

3 20

Average molarity of HCl

Calculations:

……………………………………………………………………………………………………………………………
……………………………………………………………………………………………………………………………
……………………………………………………………………………………………………………………………
……………………………………………………………………………………………………………………………
……………………………………………………………………………………………………………………………
……………………………………………………………………………………………………………………………
……………………………………………………………………………………………………………………………
……………………………………………………………………………………………………………………………
………………………………………………………………………………………………………………………..

37
 Experiment 9: Reactions in Aqueous Solutions
Objectives:
• To become familiar with writing equations for metathesis reactions, including net ionic
equations.
• To observe and represent these reactions using balanced chemical equations.

Materials Needed: concentrations are not critical in this experiment (not quantitative)

• 12 Small test tubes • 1.0 M hydrochloric acid • 0.1 M copper (II) sulfate
• 1.0 M sodium acetate • 0.1 M nickel chloride • 0.1 M barium chloride
• 0.1 M potassium chloride • 0.1 M sodium sulfide • 1.0 M sulfuric acid
• 1.0 M sodium carbonate • 1.0 M ammonium chloride • 0.1 M silver nitrate
• 0.1 M sodium phosphate • 0.1 M lead nitrate • 0.1 M cadmium chloride
• 1.0 M sodium hydroxide • 0.1 M sodium nitrate

Introduction:

Reactions in aqueous solutions occur in biological systems such as our bodies, in our homes as
well as in water bodies such as ocean, river.... and in many industrial applications. Metathesis
reaction which is known as "double displacement," or "partner exchange." is very common in
aqueous solution. The general formula for such reaction is:
AB + CD → AD + CB
the reactants AB and CD are assumed to be completely dissociated in aqueous solution, the
evidence of the occurrence of the reaction can be:
1- The formation of precipitate (un soluble product).
2- The liberation of a gas.
3- The formation of weak acid or weak base.
4- The formation of water molecule.

A Typical example of metathesis reaction is that of KCl with AgNO3

KCl (aq) + AgNO3 (aq) → AgCl (s) + KNO3 (aq)

this equation is known as molecular equation, the salts AgNO3, KCl and KNO3 are strong
electrolytes and are completely dissociated in solution, we can write the equation as follows:

K++ Cl- + Ag+ +NO3-→ AgCl(s) + K+ + NO3-

This form is known as the ionic equation, ions of K+, NO3- are appeared in both sides of the
equation (reactants and products), they are known as spectator ions and can be eliminated,
the following net ionic equation is formed:

Cl- + Ag+→ AgCl (s)

In this experiment you will examine various reactions, and you will decide whether those
reactions occur or not.

38
Procedure:

In the table below, mix the two reactants in test tube.

Take around 2 ml of reactant-1 in the test tube, then add 2 ml of the reactant-2.
Record your observation (formation of precipitate, gas, heat, color change), in the results
sheet.
Reaction # Rectant-1 Reactant-2
1 0.1 M BaCl2 0.1 M CuSO4
2 0.1 M Pb(NO3)2 0.1 M NaBr
3 0.1 M Pb(NO3)2 0.1 M NaBr
4 0.1 M Ni(NO3)2 3 M NaOH.
5 solid CaCO3 3 M HCl
6 0.2 M NH4NO3 3 M NaOH
7 1M NH4Cl 1M NaOH
8 0.5 M NaOAC 1M HCl
9 0.1 M Pb(NO3)2 H2SO4
10 0.1 M Ba(NO3)2 0.1 M Na2SO4
11 0.1 M NH4NO3 0.1 M Na2SO4

39
 Report sheet (Exp 9)
Student name: …………………………………………………………
Experiment Title: ……………………………………………………………………………………………………..

Fill in the following table for each reaction

Reaction # 1 1
Molecular equation BaCl2(aq) + CuSO4(aq) →BaSO4(aq) + CuCl2(aq)
observations CuSO4 is blue solution, the BaCl2 solution is colorless. When mixed,
white precipitate gradually settled out from a blue solution.
Ionic equation Ba2+(aq) + 2Cl-(aq) + Cu2+(aq) + SO42-(aq) → BaSO4(s) + 2Cl-(aq) + Cu2+(aq)
Net ionic equation Ba2+(aq) + SO42-(aq) → BaSO4(s)
Reaction # …….. 2
Molecular equation
observations
Ionic equation
Net ionic equation
Reaction # …….. 3
Molecular equation
observations
Ionic equation
Net ionic equation
Reaction # …….. 4
Molecular equation
observations
Ionic equation
Net ionic equation
Reaction # …….. 5
Molecular equation
observations
Ionic equation
Net ionic equation
Reaction # …….. 6
Molecular equation
observations
Ionic equation
Net ionic equation

40
 Experiment 10: Precipitation reaction & Limiting
reactant
Objectives:

• To know how to carry out precipitation reaction

• To know how to perform quantitative filtration of solid product
• To know how to write a balanced equation for precipitation reaction
• To calculate the % yield of the reaction

Materials Needed:
- Lead Nitrate solution, Pb (NO3)2, 0.1M,
- Potassium iodide KI solution 0.5M, Burette No .2
- Beakers
- burettes
- Simple filtration apparatus (gravity)
- Oven
- Top-loading balance

Introduction:

Consider the precipitation reaction of barium phosphate, Ba3(PO4)2, from the

reaction of barium chloride with sodium phosphate, Na3PO4

First write balanced molecular equation: 3BaCl2 +2 Na3PO4 → Ba3(PO4)2 + 6 NaCl

then apply the solubility rules: 3BaCl2(aq) +2 Na3PO4(aq) → Ba3(PO4)2(s) + 6 NaCl(aq)
and write the ionic equation: 3Ba2+ + 6Cl- + 6Na+ + 2 PO4 -3 → Ba3(PO4)2 (s) + 6Na+ + 6Cl-
Finally, the net ionic equation is: 3Ba2+ + 2 PO4 -3 → Ba3(PO4)2 (s)
Na+ and Cl- are spectator ions.

The limiting reactant is the reactant that runs out first, this means that it is
completely consumed during a chemical reaction, and it produces the least amount of
product.
Chemicals react according to fixed mole ratios (stoichiometric), so only a
limited amount of product can form from given amounts of starting materials. The
maximum theoretical yield of a chemical reaction is dependent upon the limiting
reagent thus the one that produces the least amount of product is the limiting reagent.
For example, if we mix 10 ml of 0.15M Na3PO4 with 5 ml of 0.2M BaCl2 then we
got the followings:
• Moles of Na3PO4= moles of PO4-3= MNa3PO4 × V Na3PO4 = (10/1000) × 0.15= 1.5 ×10-3
mol
• Moles of BaCl2= moles of Ba2+ = MBaCl2 × V BaCl2= (5/1000) × 0.2= 1.0 ×10-3 mol
What is the limiting reagent?
3Ba2+ + 2 PO4 -3 → Ba3(PO4)2 (s)
✓ 3moles of Ba2+ produces 1mole of the precipitate Ba3(PO4)2, then,

41
 ✓ ×10-3moles of Ba2+ produce 3.333×10-4moles of the precipitate Ba3(PO4)2
In the other hand,
✓ 2 moles PO4 -3 produce 1mole of the precipitate Ba3(PO4)2, then
✓ 1.5 ×10-3moles of PO4 -3 produce 7.5×10-4 moles of the precipitate Ba3(PO4)2.
Because Ba2+ produces the least amount of precipitate, it is the limiting reactant.
The theoretical yield (g), we should got of 3.333×10-4 moles of the precipitate
Ba3(PO4)2, :
(moles × molar mass) = (3.333×10-4 × 601.9 g/mole) = 0.2 g.
In the experiment, we may get less than the theoretical yield, suppose that we got only
0.16g, then the percentage yield = (actual yield / theoretical yield) × 100 = ( 0.16/0.2) × 100
= 80%.

In today's experiment we will apply the concepts of limiting reactant, theoretical and
% yield to the following precipitation reaction:
Pb(NO3)2 +2 KI → PbI2 (s) + 2KNO3
all of the reactants and product are water soluble except lead iodide, PbI2 (s)
The net ionic equation is:
Pb2+ + 2I- → PbI2 (s)
Procedure:

(1) Obtain a pre-cleaned and dried small beaker

(2) Take exactly 10 ml of 0.1 M Pb(NO3)2 pour in the beaker.
(3) Add exactly 5 ml of 0.5 M KI or NaI to the first solution. A yellow solid precipitate
should be formed (PbI2).
(4) Weigh a dry filter paper.
(5) Put the filter paper in funnel, and filtrate the yellow precipitate.

(6) Dry the filter paper in oven for 30 min.

(7) Weigh the filter paper with precipitate again, find the mass of your precipitate (by
difference), be sure that your product is getting dried.
(8) Determine the limiting reactant and the theoretical yield.
(9) Calculate the % yield of your reaction.

42
 Report Sheet (Exp 10)
Student Name: ………………………………………………………………….. ID:
………………………………..
Experiment Title: ……………………………………………………………………………………………………..

1- Moles of Pb2+ in 10 ml of 0.1M Pb(NO3)2 = (MPb(NO3)2 × VPb(NO3)2) = ………………………….

2- Moles of I- in 5ml of 0.5M KI= (MKI × VKI) = ......................................................................................

3- Moles of the precipitate (PbI2) would be produced from Pb2+ = ………………………………

(note the stoichiometric ratio) Pb2+ + 2I- → PbI2 (s)

4- Moles of the precipitate (PbI2) would be produced from I- =

……………………………………

(note the stoichiometric ratio)

5- Which ion (Pb2+ or I-) produce the least amount of (product) precipitate (compare step

3 and 4)

.................................................................................................................................................................................

6- The limiting reactant is ..........................................................................................................................

7- Theoretical yield of precipitate: .........................................................................................................

8- Mass of filter paper...................................................................................................................................

9- Mass of filter paper and precipitate..................................................................................................

10- Mass of precipitate (actual)..............................................................................................................

11- Percentage yield of reaction: (step10/ step 7) × 100%= ....................................................

43
 Experiment 11: Weak base-strong acid titration
Objectives:
• To know how to follow this type of reactions by suitable indicator
• To determine the concentration of the weak base.
• To apply the roles of dilution

Materials Needed:
- Burette
- Pipette
- Erlenmeyer flask
-Volumetric flask
- Beakers
- Gradated cylinders
- Ammonia aqueous solution 2M
- HCl 0.25M
- Methyl red or Bromocresol green indicators

Introduction:
Ammonia (NH3) is a weak base in aqueous solution, it can be found in house
hold cleaners with a mass percentage of 2-5%. As a base, ammonia reacts with
hydrochloric acid according to the following equation:
NH3 + HCl → NH4Cl
In the titration of ammonia with HCl, at the equivalent point all of the ammonia
is converted to the NH4Cl salt which has acidic criteria, and this lead to shift the
equivalent point far from pH 7 as in strong acid-strong base titration. As can be
shown from the titration curve below( figure ......) the choice of proper indicator
is very important to give accurate results, the indicator should response to pH
change in the range (6-4), the best choices could be the Bromocresol green (
blue to yellow) , Bromophenol blue ( blue to green) or methyl red( yellow to
red). Other indicators may have margin of errors.

44
 .
Figure:11-1

Procedure:

1-Use a pipette to transfer exactly 10 ml of concentrated ammonia solution to

100 ml volumetric flask.
2-Add multi- portions of distilled water to the 100ml volumetric flask shake
very well
3- Continue the addition of distilled water to mark(100 ml)

4-Transfer exactly 25 ml of this diluted solution to Erlenmeyer flask, add few

drops of suitable indicator( Methyl red or bromocresol green).
5- Titrate with 0.25 M HCl to the end point indicated by color change of the
indicator, Bromocresol green ( blue to yellow) , Bromophenol blue ( blue to
green) or methyl red( yellow to red).

6- Repeat the steps(4-5), for a total of 3-times.

7- Calculate the molarities of diluted ammonia solution

8- from the concentration of diluted ammonia calculate the concentration of

original ammonia solution

45
 Report Sheet (Exp 11)

Student Name: …………………………………………..

Experiment Title: …………………………………………………………………

Weak base-strong acid titration

Ammonia- titration

Trial No. Volume of Volume of Moles of moles of Molarity Molarity of

diluted titrant HCl diluted NH3 ofdiluted concentrated
ammonia HCl M* V NH3 NH3
(ml) (ml) mol/L mol/L

1 25

2 25

3 25

M
Average

Show a detailed sample calculations for any trial of the three ones?
.....................................................................................................................................................................
.....................................................................................................................................................................
.....................................................................................................................................................................
.....................................................................................................................................................................
.....................................................................................................................................................................
.....................................................................................................................................................................
...................................................................................................................................................

46
 Experiment 12: Vinegar Analysis, Mass %
Objectives:

• To perform the weak acid-strong base titration

• To determine the mass percentage of acetic acid in vinegar

Materials Needed:
- Erlenmeyer flask - Beakers
- Gradated cylinders (10 ml) - Burettes
- Vinegar solution - Standardized 0.25 M NaOH solution
- Top loading balance

Introduction:
Most commercial vinegars contain 4-5% (w/v) acids expressed as acetic acid
(CH3COOH). The principal acidic constituent of vinegar is acetic acid. However, other
organic acids are also present. The total quantity of acids can be readily determined
by titration with standard base using phenolphthalein as an indicator.
The neutralization reaction is:
CH3COOH + NaOH → CH3COONa + H2O
because the acetic acid is weak, the net ionic equation is:
CH3COOH (aq) + -OH (aq) → CH3COO- (aq) + H2O (l)
It is important to mention that at the endpoint the formation of the CH3COONa salt
(sodium acetate) will shift the equilibrium slightly, but because of the basic property
of this salt the phenolphthalein indicator will work properly in this area.

Procedure:
1- Obtain a small beaker (pre-cleaned and dried), take its weight on a top-loading
balance or zero the balance on this weight.
2-Transfer about 5-7 ml of vinegar to the small beaker, record exactly the weight of
vinegar. (in the range 5 -8 g).
3- Transfer the vinegar solution from the beaker to Erlenmeyer flask.
4- Rinse the beaker (3-times) with portions of distilled water (amount of distilled
water is not critical ...about 5-7 ml each time), now you have approximately a total of
20-30 ml.
5- Add few drops of phenolphthalein (Ph.Ph.) indicator to the vinegar solution.
6- Using a clean funnel, fill the burette with the 0.25 M NaOH solution.
7- Titrate the vinegar solution, with 0.25 M NaOH solution (from the burette) until the
pale-pink color, record the volume of NaOH.
8- Repeat steps 1-7 (for a total of 3-replicates).
9- Calculate the % (w/w) of acetic acid in vinegar.

47
 Report Sheet ( Exp 12)
Student Name: . . . . . . . . . . . . . . . . .. . . . . . . . . . . . .
Experiment Title: …………………………………………………………………

Trial mass of Vol. of NaOH moles of NaOH moles of Acetic mass of Mass % of
No. vinegar (mL) (mol) acid in vinegar acetic acid acetic acid
(g) (mol) (g) in vinegar
1

Average =

Hints:
• Volume of NaOH = final burette reading - initial reading
• Moles NaOH = MNaOH x VNaOH
• Moles acetic acid = Moles NaOH (1:1 mole ratio)
• Mass acetic acid = moles (acetic acid) x Molar mass (acetic acid)
[Molar mass (acetic acid) = 60 g/mole]

………………………………………………………………………………………………..
………………………………………………………………………………………………..
………………………………………………………………………………………………..
………………………………………………………………………………………………..
………………………………………………………………………………………………..
………………………………………………………………………………………………..
………………………………………………………………………………………………..
………………………………………………………………………………………………..
………………………………………………………………………………………………..
………………………………………………………………………………………………..
………………………………………………………………………………………………..
………………………………………………………………………………………………..
………………………………………………………………………………………………..
………………………………………………………………………………………………..
………………………………………………………………………………………………..
………………………………………………………………………………………………..
………………………………………………………………………………………………..
………………………………………………………………………………………………..
………………………………………………………………………………………………..
………………………………………………………………………………………………..

48
 Experiment 13: Oxidation reduction reactions
Objectives:
To predict the patterns of redox reactions and their behavior.
To observe and represent these redox reactions using balanced chemical equations

Materials Needed:
Copper turnings 6M HCl 6M HNO3 0.5 M H2SO4
0.1M NaHSO3 0.1M KMnO4 0.1M KI 0.1 M FeCl3

Introduction:
Oxidation-Reduction reactions (or Redox) reactions, are a type of chemical
reaction that involves a transfer of electrons between two species. In such reactions,
the oxidation number of a molecule, atom, or ion change by gaining or losing an
electron.
In order to write the balanced redox equation, the equation is divided in two
cells (half), the oxidation part and the reduction part, each half is balanced separately
and the number of electrons in the last step must be the same in the two cells before
their combining.
For example, of how to balance a redox reaction is shown below:
I2 + S2O32- → S4O62- + I-
1-Split the reaction in two halves:
I 2 → I- reduction

S2O32- → S4O6 oxidation

2-Balance each half, the main atom, (oxygen atom by adding H2O, hydrogen atom by
adding H+ and finally the net charge by adding electrons)
I2 → 2I- reduction add 2e to be I2 + 2e- → 2I-
S2O32- → S4O6 oxidation add 2e in the right to be 2S2O32- → S4O6-2 + 2e-
Summation: I2 + 2S2O32- → S4O62- + 2I-
Another example is the reaction of KCr2O7 and H2O2 in acidic solution:

and the balanced equation:

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Procedure:

A- Cu and HCl (aq)

Place a small amount of copper (pieces) in a small test tube in the hood. Add
about 5 mL of 6M HCl. Look for a reaction over a period of 5 minutes or so.
Note the color of the fumes above the test tube.

B-Cu and HNO3(aq)

Repeat the procedure of System 1, but substitute 5 mL 6 M HNO 3 for HCl

C-NaHSO3 and KMnO4

In a large test tube, add 0.1 M NaHSO3 (2 mL) + 3 drops of 0.5 M H2SO4; then
add 10drops of 0.1 M KMnO4, drop by drop. The sign of reaction will be the
loss of the permanganate color.

D-KI and FeCl3

In a large test tube place 0.1 M KI (2 mL) + 0.1 M FeC13 (2 mL)
Note the color and the formation of any precipitate of I2(s). the precipitation
process may be slow.

50
 Report sheet (Exp 13)
Student Name: ………………………………………………………..
Experiment Title: ……………………………………………………………………………………….

1-Write balanced redox equations for the four reactions

A- ......................................................................................

B-.......................................................................................

C-......................................................................................

D-.......................................................................................

2- Determine the oxidizing and reducing agent in each reaction

A-.............................................................................................

B-...............................................................................................

C-..............................................................................................

D-..............................................................................................

3- What evidences of forming gases in the reaction of Cu with HCl and HNO3?

………………………………………………………………………………………………………………
………………………………………………………………………………………………………………
………………………………………………………………………………………………………………
………………………………………………………………………………………………………………
………………………………………………………………………………………………………………
………………………………………………………………………………………………………………

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Questions:
Q1: For each of the following reactions, tell whether or not it is a redox reaction

1- Mg(s) + 2 HCl(aq) →MgCl2(aq) + H2(g)

2- Cu(s) + 2 AgNO3(aq) →Cu(NO3)2(aq) + 2 Ag(s)

3- MgO(s) + 2 HCl(aq) →MgCl2(aq) + H2O(l)

4- NaHCO3(s) + HC1(aq) →NaCl(aq) + H2O(l) + CO2(g)

5- Fe(s) + Cl2(g) →FeCl3(s)

Q2: Determine the oxidation number of underlined element in the following

ions or compounds:

1- H2O2 2- K2C2O4 3- SO4-2 4- Cr2O7-2 5- IF5

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 Experiment 14: Redox titration of Fe2+
Objectives:

• To determine the concentration of unknown Fe2+ solution

• To know some properties of KMnO4 solution

Materials Needed:
- Burettes - Beakers - Erlenmeyer flasks
- Pipettes - H2SO4 - H3PO4
- 0.02 M of KMnO4 solution - Unknown Fe solution (freshly prepared)
2+

Introduction:

The iron content of different samples can be determined (quantified) by the titration
with standardized solution of potassium permanganate (redox reaction). In this
reaction potassium permanganate is employed as an oxidizing agent, it is inexpensive
and readily available. The reagent itself is used as an indicator. For the above reaction
to be feasible, all of iron must be in the 2+ oxidation state Fe (II) and the sample
solution that contains iron should be acidic. The Phosphoric acid is added to Fe(II)
solution before starting the titration, it forms the colorless complex Fe(HPO4)+, this
give a sharper end point by preventing the formation of the yellow Fe(III) solution.
In today’s experiment, Fe2+ will be oxidized by KMnO4according to the following
balanced equation:
MnO4— + 8H+ + 5Fe2+→ 5Fe3+ + Mn2+ + 4H2O ( In acidic medium)
In this case 1 mole of KMnO4 reacts with 5 moles Fe2+.
******Precaution: Potassium permanganate is a strong oxidizing agent and can be
damaging to skin, eyes, and clothing. Wash thoroughly after handling *******

Procedure:
1- Obtain your (unknown) solution of Fe2+,
Note: the iron solution is prepared using sulfuric acid, which is damaging to the
skin, eyes, and clothing.
2- Transfer exactly 20 m l of this solution (Fe2+) to Erlenmeyer flask.
3- Add approximately 1 ml (by plastic dropper) of concentrated H3PO4
4- Titrate with 0.02 M KMnO4 (from burette) to the first appearance of a permanent,
pale pink color. Record the exact volume of KMnO4
5- Repeats steps (2 & 4) for 2 more trials

53
 Report Sheet (Exp 14)
Student Name:. …………………………………………………………………..
Expr. Title: …………………………………………………………………………………………………………

Redox titration of Fe2+

Trial Volume of Volume of Moles of Molarity of

moles Fe2+
No. Fe2+ KMnO4 KMnO4 Fe2+
(mol)
(mL) (mL) (mol) (mol/L)

1 20

2 20

3 20

Average M

Questions:
Q1: Write the molecular, ionic and net ionic equations, given this word
equation for a chemical reaction:
barium hydroxide + sulfuric acid →barium sulfate + water

Q2: Iron oxides found in iron ores can be reduced to metallic iron when reacted
with carbon monoxide. The equation for this reaction is:
Fe2O3 + 3CO→ 2Fe + 3CO2
a.) How many kilograms of elemental iron can be formed if 16.0 kg Fe2O3 is
reacted with 10.0 kg CO?

b.) How many kg of CO2 will be produced in the reaction described in 5a?

54
 Experiment 15: Ideal Gas Law
Objectives:

• To apply the ideal gas law

• To demonstrate the use of various units of pressure (P),volume ( V), temperature(T)
and gas constant (R)
• To identify the unknown gaseous material ( unknown volatile liquid)

Materials Needed:
- Erlenmeyer flasks
- Thermometer
- Beakers
- Gradated cylinder
- Top loading balance
- Aluminum foil
- Rubber band
- Stand and clamp
- Volatile liquid( B.P less than 90 ͦ C)acetone, or methanol, hexane, diethyl ether...

Introduction:

The ideal gas law (PV = nRT) indicates that the observed properties of a gas sample
[pressure (P), volume (V), and temperature (T)] are directly related to the quantity of gas in
the sample (n, moles).This law serves as the basis for the Dumas Method for the
determination of molecular weight of some gases. In Dumas method, a small amount of
liquid is placed in a container with a very small hole. The liquid is then heated in a constant
temperature bath, such as a boiling water bath, until all the liquid vaporizes. Excess vapor
escapes via the hole in the container( see figure 16-1). Assuming ideal gas behavior, use the
pressure of the vapor (P), its volume (V), and
its temperature (T) to determine the moles of vapor in the Erlenmeyer flask. If the mass (m)
of the gas is also known, and this is also easily measurable, we can then determine its
Molecular Weight: MW = m / n , where m is the mass in gram and n is the number of
moles.

55
Figure 15-1: Apparatus for determination of the molar mass of a volatile liquid

Procedure:

1- Obtain a clean and dry 125ml Erlenmeyer flask.

2- Cut a square of aluminum foil, to serve as a cover.

3- Weigh the Erlenmeyer flask, aluminum foil and the rubber band together.

4. Prepare a hot water bath by filling a 1 L beaker half full of water, heat to
boiling on a hot plate.

5- Obtain your unknown liquid, take 2-3 ml of this liquid , add to the Erlenmeyer flask.

6- Cover the flask with the foil cover, secure with the rubber band, and punch a small hole
in the foil cover with a pin.

7- Clamp the flask assembly into the water bath(boiling) so that flask is as far down as
possible in the bath.( figure 8)

8- When it appears that all the unknown liquid has vaporized, and the flask is filled with
vapor, continue to heat for 3-5 more minutes.

56
9- Remove the flask from water bath, Allow the flask to cool to room temperature, and dry
it on the outside gently with a paper towel. Liquid will reappear in the flask as the vapor
in the flask cools.

10- Measure the temperature of boiling water, and the atmospheric pressure in the lab.

11- Weigh the flask along with its contents.

12- Repeat the determination by adding another 2-3-mL sample of unknown liquid.( Do not
wash the flask for the second trial)

13- After two successive trials, measure the volume of Erlenmeyer flak by filling it with
water and measuring the volume of water with a 100 mL graduated cylinder

14- Now, you have the P, V, T and mass of the unknown liquid( vapor), calculate its
molecular weight and try to identify it.

57
 Report Sheet ( Exp 15)
Student Name: ………………………………………..
Experiment’s Title: …………………………………………………..
……………………………………………………………………….

1- Mass of empty Erlenmeyer flask, foil and rubber band together:.....................g

2- temperature of boiling water..........................C

3- Atmospheric pressure in lab...........................atm

4- Mass of Erlenmeyer flask, foil, rubber band and condensed vapor..........................g.

5- Mass of the gas occupied the Erlenmeyer flask,( step 4-
step1),................................................g
6- The volume of gas( volume of Erlenmeyer flask)..................L

7- Number of moles of condensed gas, (apply PV/RT), .......................mole

6- Molecular weight of the liquid ( vapor),(m/n) (step5/step7)..........................g/mole

7- Possible compound:................................................

Questions :

Q1: If 2.31 g of the vapor of a volatile liquid is able to fill a 498-mL flask at 100.EC and
775 mm Hg, what is the molecular weight of the liquid? What is the density of the
vapor under these conditions?

Q2: Calculate the molecular weight of a gas if 35.44g of the gas stored in a 7.5 L tank
exerts a pressure of 60 atm at a temperature of 35.5 ͦ C?

58
 Experiment 16: Determination of the specific heat of
metal
Objectives:
• To apply the first law of thermodynamic "conservation of energy"
• To determine the specific heat of metal
• To identify the metal

Materials Needed:
- Constant pressure calorimeter, "Coffee cup"
- Thermometer
-Tong
- Beakers
- Gradated cylinders
- Various metallic samples (15-35 g)
- Top loading balance

Introduction:

The specific heat of capacity is defined as the amount of heat needed to rise the
temperature of one gram of substance by one degree. Specific heat capacities of
various materials are often listed in textbooks. Standard metric units are
Joules/kilogram. Kelvin (J/kg/K). More commonly used units are J/g/°C.

Specific heat capacities provide a means of mathematically relating the amount

of thermal energy gained (or lost) by a sample of any substance to the sample's
mass and its resulting temperature change. The relationship between these
four quantities is often expressed by the following equation.

Q = Sp. m. ΔT
where Q stands for the amount or quantity of heat transferred in or out of
object, Sp is the specific heat capacity of the substance(object), m is the mass of
object and ΔT is the temperature change of the object.
Heat flowsspontaneously from an object at a high temperature to an object at a
lower temperature if the two objects are thermally in contact. Heat flow is
ordinarily measured in a device called a calorimeter which is simply a
container with insulating walls, to prevent heat lost to the surroundings.
Within the calorimeter, chemical reactions may occur or heat may pass from
one part of the contents to another. The specific heat of a metal can readily be
measured in a calorimeter. if a known mass of metal at high temperature( T1) is
poured in a calorimeter which contain water with known mass and

59
temperature( T2,where T2<T1), then heat flows from metal to water, at
equilibrium they reach Tf, by applying the law of conservation of energy:
Heat lost by metal = heat gained by water
- [Spmetal× mass metal × (Tf-T1)] = Spwater× mass water × ( Tf-T2)

we can calculate the specific heat of metal.

Procedure:
1- Obtain your unknown metal, take its mass( ±0.001g)
2- Place the metal in boiling water( measure the temperature of
boiling water) for 10 minutes.
3- Measure about 100 ml of distilled water, take the exact mass, pour in the
calorimeter, measure and record the temperature of water.
4- Remove the hot metal( use forceps) and immediately place it in the
calorimeter
5- Stir the water carefully, and record the highest temperature.

60
 Report Sheet (exp 14)
Student name: ………………………………
Expr Title: ……………………………………………………………………

Specific heat of metal

Unknown No. or description: .........................................................................

Trial Mass of T/ Mass of T/ T ΔT ΔT Specific
No. metal/g metal water/ water equilibrium metal wate heat of
ͦ C g ͦ C ͦ C r metal

Average Specific heat capacity

Show a sample calculation:( choose any trial )

.....................................................................................................................................................................
.....................................................................................................................................................................
.....................................................................................................................................................................
.....................................................................................................................................................................
.....................................................................................................................................................................
.....................................................................................................................................................................
.....................................................................................................................................................................
.....................................................................................................................................................................
..............................................................................................................

Note: specific heat capacity of water = 4.18 J/g.ͦ

61
Questions:

Q1:It takes 585 J of energy to raise the temperature of 125.6 g mercury from 20
degrees C to 53.5 degrees C. Calculate the specific heat capacity and the molar
mass capacity of mercury.

Q2:Determine the final temperature when a 25.0g piece of iron at 85.0°C is

placed into 75.0grams of water at 20.0°C. The specific heat of iron is 0.450
J/g°C. The specific heat of water is 4.18 J/g°C.

Q3:What is the final temperature after a 21.5 gram piece of ice at 0 is placed
into a Styrofoam cup with 125.0 grams of water initially at 76.5oC? Assume no
loss or gain of heat from the surroundings.

62
References
Lab 2 &3:
http://www.ccri.edu/chemistry/courses/chem_1030/flanagan%20campus/Ex
periments/Density.pdf
http://web.gccaz.edu/~rob2108739/Density%20of%20Water/Accuracy%20a
nd%20Precision%20of%20Glassware%20Fall%202013.pdf
https://www.mdc.edu/kendall/chmphy/Experiment2.pdf

Lab
4:http://web.clark.edu/sbrookhart/Chem_121_Lab/Lab_Handouts_files/121H
ydrateS10.doc.pdf
Lab 5:
http://www.smc.edu/projects/28/Chemistry_10_Experiments/Ch10_Stoichio
metry.pdf
Lab 6: http://classes.uleth.ca/201203/chem24102/Expt%203_12_2938.pdf
Lab7 : http://web.clark.edu/amixon/110/W11_PercentComp.pdf
Lab8:
http://www.kimia.um.edu.my/images/kimia/lab%20manual/level1/Physical
%20/Expt%201%20Manual.pdf
https://www.smc.edu/AcademicPrograms/PhysicalSciences/Documents/Che
mistry_12_Experiments/titration%20experiment%203-13.pdf

Lab9: http://www.csus.edu/indiv/m/mackj/chem1a/lab/pdfs/exp_3.pdf

Lab 10: http://scienceattech.com/wp-content/uploads/2010/05/PbI2-

Synthesis.pdf
Lab 11: http://www.foothill.edu/attach/psme/sinha.titrationcurves.pdf

Lab12: https://scilearn.sydney.edu.au/fychemistry/LabManual/E10.pdf
Lab13:
http://cms.cerritos.edu/uploads/cshimazu/Chem%20112/Experiments/Oxida
tion-_Red_Exp._chem_112_no_Pb_.pdf
Lab 14:
http://www.colby.edu/chemistry/CH145/CH145L/CH141exp52009.pdf
Lab 15: http://www.laney.edu/wp/lschaleger/files/2015/10/7-Specific-Heat-
of-a-metal.pdf

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