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Al al-bayt University Faculty of Science

Department of Chemistry

CHEM – LAB – 106

Prepared By: Dr. Qutaiba Abu-Salem


Department of Chemistry
General Chemistry Laboratory (403106)

Credit hours: 1

Perquisite: Chemistry (403102 )

Evaluation: (subject to change )

Mid-Term Exam and Quizzes: 30%

Reports: 20%

Final Exam: 50%

Course Contents:

Introduction: Laboratory Apparatus, Safety, and Techniques

Exp.1: Density

Exp.2: Physical Separation of Mixtures

Exp.3: Limiting Reactant

Exp.4: Colligative Properties: Determination of Molecular Weight by Freezing


Point Depression

Exp.5: Acid-Base Titration

Exp.6: Chemicals In Everyday Life

Exp.7: Qualitative Analysis of Insoluble Chlorides Ag+, Pb+2, Hg2+2

Mid-Term Exam

Exp.8: Calorimetry

Exp.9: Spectrophotometric Determination of an Equilibrium Constant

Exp.10: Solubility Product Constant And Common-Ion Effect

Exp.11: Quantitative Yield of a Redox Reaction

Exp.12: Determination of Rate Law


If you have to miss a lab . . .

Missed Labs: Unexcused absences will result in a grade of zero for the lab missed.
No make-up labs will be allowed for unexcused absences.

Excused absences result in the averaging of the student's other lab grades and
substituting this average grade for the lab missed.

Unexcused absences result in a 0 (zero) for that lab meeting's quiz grade and
technique grade.

Lab Reports

Lab reports consist of data, observations and calculations. We do not want students to
spend a lot of time writing long lab reports. Be clear, be concise. You will not impress
your TA by copying pages from the Manual or Text; you will impress your TA if they
can easily read and understand what you write. You must think about what happened
in lab and make conclusions on what you saw, and not what the book says.

Evaluation (performances in the laboratory - "technique")

You will be evaluated at the end of the term and will be worth 5% of your overall
grade. The "technique" grade is basically an "attendance" grade. Attendance in this
case means not simply physical presence, but whether or not you are paying attention
to what you are doing. The maximum number of points will be awarded to students
who:

 Show up on time.
 Use the equipment properly.
 Are fully prepared for lab.
 Follow all safety rules.
 Perform laboratory functions safely and efficiently.
 Work carefully in the lab to avoid breakage, spills, contamination, and
fire.
 Properly dispose of waste.
 Clean up their bench and common work areas.
 Isolate pure product and in high yield.

You can ask your TA how to do a procedure and not be penalized by losing points.
You are here to learn to do inorganic chemistry lab techniques, and you cannot do this
if you do not ask questions. If you constantly ask your TA what to do next, you are
not able to perform the experiments.

The technique grade is assigned by your TA. It may or may not be assigned each lab
meeting; your TA may keep simple plus and minus notes in their grade record.
Technique grade cannot be assigned on the basis of your lab report; it must be
assigned according to visual observations of each student in lab. Yes, it is subjective.
You may be doing stellar work most of the time and your TA does not see you until
you drop your flask.
Laboratory Safety Rules
Keeping the lab safe is the number one priority and it is everyone’s
responsibility. Before you begin, read safety rules in your lab book. The following
rules are very important for your safety as well as the safety of other students. Please
read them carefully and follow them each laboratory period.

 Appropriate white Lab-coat must be worn in the lab.


 Eye protection must be worn at all times in the lab.

Contact lenses must not be worn in the lab. Solvent vapors can get trapped behind
hard lenses and remain in contact with your eyes for extended periods. Soft lenses can
dissolve and be fused to your eyes. This is not pleasant. Please wear your goggles.

 To avoid skin exposure in case of spills, shorts and open toed shoes
(sandals) are not allowed.
 Never taste anything. Never directly smell the source of any vapor.
 Memorize the location of all exits, showers, eye washes, fire
extinguishers, and fire blankets.
 Always pour acids into water and not vice verse.
 No food or beverages are allowed in the lab.
 Perform all reactions producing gases or unpleasant odor in the fume
hood.
 Be certain that there are no flammables in the area when lighting a
flame.
 Be alert for hazards in the lab. Do not proceed with any experiment
until you understand the hazards involved.
 Report all injuries to your instructor, even if they appear to be minor.
 Do not come into contact with any of the solvents or reagents used in
this lab other than soap and water. Remove gloves and wash hands
before leaving lab.
 Clean up all chemical spills (this includes drips on bottles) and all
broken glassware immediately.
 Do not leave any bottle uncapped.
 Dispose of all wastes as directed. (Ask before you dump.)
 Do not come to the lab unprepared.
COMMON LABORATORY APPARATUS

Beakers are useful as a reaction container or to hold liquid or solid


samples. They are also used to catch liquids from titrations and filtrates
from filtering operations

Bunsen Burners are sources of heat

Burets are for addition of a precise volume of liquid. The volume


of liquid added can be determined to the nearest 0.01 mL with
practice.

Clay Triangles are placed on a ring attached to a ring stand as a


support for a funnel, crucible, or evaporating dish.

Droppers are for addition of liquids drop by drop

Erlenmeyer Flasks are useful to contain reactions or to


hold liquid samples. They are also useful to catch filtrates.
Glass Funnels are for funneling liquids from one container
to another or for filtering when equipped with filter paper.

Graduated Cylinders are for measurement of an amount of


liquid. The volume of liquid can be estimated to the nearest
0.1 mL with practice

Hot Plates can also be used as sources of heat when an


open flame is not desirable.

Pipets are used to dispense small quantities of liquids.

Ring stand with Rings are for holding pieces of


glassware in place.

Test Tubes are for holding small samples or for containing


reactions
Test tube holders are for holding test tubes when tubes
should not be touched

Tongs are similar in function to forceps but are useful for


larger items.

Dilution mark Volumetric Flasks are used to measure precise volumes of liquid or to
make precise dilutions

Wash bottles are used for dispensing small quantities of


distilled water.

Watch glasses are for holding small samples or for


covering beakers or evaporating dishes.

Wire Gauze on a ring supports beakers to be heated by


Bunsen burners
LABORATORY EQUIPMENT

Balances are used to determine the mass of a


reagent or object.

Spectrophotometers are used to measure the


absorbance or transmittance of a liquid sample.

Fume Hoods are used to ventilate noxious or harmful


gases.
COMMON LABORATORY TECHNIQUES

Reading a Meniscus

In all volumetric glassware (pipet, buret,


volumetric flasks, graduated cylinder, etc.), it is
necessary to read the level of a liquid. A liquid
46
in a small-diameter container will form a meniscus 46.33
or curve at the surface of the liquid. Usually this
meniscus curves downward to a minimum at the
center. To read the level of the liquid properly,
the eye should be at the same level as the bottom
47
of the meniscus. Sometimes a white card or a white
card with a black mark on it will help a person to 100
see the meniscus clearly. For volumetric flasks
and transfer pipets, the volume of the glassware is Buret
exact when the bottom of the meniscus is even with
the etched line. In a graduated cylinder or a
buret, the volume is read from the graduations 91.7
etched on the glass. To read the volume correctly, 90
visualize the distance between the tenths of
milliliter marks as divided into ten equal amounts.
The volume is then found by reading the number of Graduated
tenths of milliliters and estimating hundredths of
Cylinder
milliliters.

Care of Reagents

The reagents used by all of the students can be


contaminated by one careless student. Never put
anything back into the reagent bottle. A certain
amount of liquid can be obtained in several ways. 1)
Pour from the reagent bottle into a beaker and draw up 6M NaOH
the liquid into a pipet from the beaker. 2) Pour from the
beaker into a graduated cylinder to within 0.1 ml of the
desired amount, adding the last drop with an eyedropper Copper
Sulfate
filled from a beaker. Only use appropriately labeled
spatulas for each reagent bottle. Pour the solid into a
beaker, onto weighing paper, or into a weigh boat. Never
pour excess back into the bottle. Reagents are to remain on the plastic on the center
bench. This will 1)prevent spills and accidents from occurring at your work area, 2)save
time for everyone because all of the chemicals will be relatively easy to find in a central
location, and 3)make clean-up easier if a spill does occur. When you are finished using
a chemical, replace the lid! A mix-up of lids could also contaminate an expensive
chemical.
Care and Use of Balances

Each of the balances you will be using costs somewhere in the neighborhood of $2000 to
$2500. Therefore, care must be exercised in using them. Below is a simple outline that
will help you to use the balance more effectively, safely, and will assist in reducing the
speed at which the Stockroom Manager’s hair is turning prematurely gray.
1. Select a suitable container (usually a weigh boat, weigh paper, or glassware) to
weigh the chemical in.
2. Remove the balance cover.
3. Place the container on the balance pan and replace the balance cover. Replacing
the balance cover will greatly reduce fluctuations in the balance reading!
4. Allow the balance reading to stabilize. Zero the balance by pressing the TARE
button or bar which is located at the front of the balance. DO NOT hold down the
tare button/bar! This will cause the balance to change units and you may end up
weighing your chemical in units other then grams which will cause your data to be
in error!
5. Remove the balance cover and carefully transfer the desired chemical to the
container. If you use a spatula, use only a clean, dry spatula for obtaining dry
chemicals. If you should spill a chemical on the balance pan, use the brush that is
attached to the balance to clean the balance pan IMMEDIATELY! Chemicals left
on the balance pan will corrode the pan.
6. Replace the balance cover and allow the balance reading to stabilize. In the event
you weigh out too much chemical, remove the excess to a secondary container.
NEVER return a chemical to its original container! There will always be some left
over. Try to find someone else who needs it before disposing of it.
7. Discard chemicals as directed in each experiment (See the Safety and Disposal
section for each experiment).
8. Record the balance reading in your notebook.
9. Remove the container from the balance pan and replace the balance cover.
10. Replace the appropriate lids on all reagent bottles when finished.
Titration

The titration procedure is accomplished by adding


small amounts of one reactant to a beaker or flask
containing the other until the reaction is completed. In an
acid-base reaction, the reaction is complete when the
amount of acid equals the amount of base. The
experimenter is aware of this condition by the change in pH
that occurs. The change in pH is indicated by a color
change of an indicator or by a pH meter. In other types of
reactions, the completion of the reaction is usually also
indicated by a color change. Titrations are often
accomplished using a buret. A small amount (~ 5 - 10 mL)
of the solution is used to rinse a clean buret. The rinse
solution is discarded. The buret is filled to just below the zero
mark. The liquid level is read and recorded as the initial volume. A
buret has zero at the top as shown in the figure on page 12. Small
amounts of the solution are allowed to flow out of the buret into the
flask by turning the stopcock. Often localized color changes will be evident for a short
period of time. Mixing the solution by swirling the flask will usually cause the color to
return to the original color. As the color lasts longer, the next addition of solution needs
to be smaller. Close to the endpoint (reaction completion), the additions are one drop at
a time. When the endpoint is reached, the liquid level is read and recorded as the final
volume. The volume added is the final volume minus initial volume.

Using A Bunsen Burner

Lighting the Bunsen burner - Make sure the


rubber tubing is connected to the Bunsen
burner and the gas jet. Turn the gas valve High Temp.
until it is parallel to the gas jet. You should be
Cool Inner Region
able to hear the gas flow. Use a flint striker to
cause a spark and ignite the gas.
Adjusting the Bunsen burner - First, adjust
the height of the flame using the gas valve at
the bottom of the burner. For a clean burning
flame, more air is required than is available
from the gas exhaust. The air vents can be Air Vents
adjusted to produce an inner blue cone in the
flame with no yellow tip. Too little air produces Gas
a sooty, orange-yellow tipped flame that is Valve To Gas Outlet
quite noisy. Too much air supply may cause
the flame to separate from the burner and
even blow itself out. The ideal working flame
is bluish-green with a light blue cone and it
burns quietly.
Experiment (1)

Density
Objectives:
1. Use measuring tools correctly.
2. Read and record measurements correctly (significant digits and unit).
3. Associate metric units with the quantities being measured.
4. Determine the density of a liquid and solid.

Introduction:
Density is a measure of a substance’s mass-to-volume ratio. For liquids and solids,
density is usually expressed in units of g/mL or g/cm3; these are equivalent since 1 mL is
exactly equal to 1 cm3. Density is an intensive property meaning that a substance’s density
will be the same regardless of the size of a sample. For example, steel has a density of 7.85
g/cm3 whether you have a tiny steel bar or a large steel bar. The mass and volume of each
piece will be different, but the mass-to-volume ratio is the same.
The density can be measured by two different techniques: 1) volume calculation based on
water displacement and 2) volume calculation using measurements of the radius and length of
the cylinder using caliper or ruler. The volume of a solid can also be determined by
displacement. A solid that is more dense than water will sink and displace a volume of liquid
equal to the volume of the solid object. Such a volume measurement is typically made in mL.
(Remember, 1 mL = 1 cm3.)
In this laboratory, you will practice taking measurements and recording them to the
correct degree of uncertainty while determining the density of various samples. Density is
defined as mass per unit volume and can be calculated using the equation:

Mass of Sample  m
Density= or D = 
Volume of Sample  V

1 Chemistry 106 Experiment 1


Significant Figures and Metric Conversions
Significant figures are important in describing the accuracy of a measurement. The
following rules paraphrased from your textbook will help you determine the number of
significant figures in a measurement.
1. All nonzero digits are significant. 3.467 cm has 4 sig figs
2. Zeros between nonzero digits are significant. 2.07 mL has 3 sig figs
3. Zeros beyond the decimal point at the end of a number are significant. 6.00 mL has 3 sig
figs
4. Zeros preceding the first nonzero digit in a number are not significant. 0.0341 g has 3 sig
figs
5. The number of sig figs is the number of digits shown when the number is written in
scientific notation.

500 g written expressing 3 sig figs would = 5.00 x 102 g


500 g written expressing 2 sig figs would = 5.0 x 102 g
500 g written expressing 1 sig fig would = 5 x 102 g

In science the metric system is used almost exclusively. The basic unit of length is the
meter (m); of mass, the gram (g); of volume, the liter (l). The meter, the gram, and the liter are
related to larger and smaller units by multiples of 10. Prefixes are used for the unit of measure
expressing these multiples of 10.

Prefix Abbreviation Value x basic unit Some Conversion Factors


Kilo- k 1000 1 km = 1000 m
Deci- d 0.1 1 m = 10 dm & 1 km = 10,000 dm
Centi- c 0.01 1 m = 100 cm & 1 dm = 10 cm
Milli- m 0.001 1 m = 1000 mm & 1 cm = 10 mm

How does 1 kilometer compare to the other units in the metric system?

1 km = 1000 meters = 10,000 dm = 100,000 cm = 1,000,000 mm

Exact Numbers and Conversion Factors


Some numbers by their very nature are exact numbers. When you say you are holding
five beakers in your hand, you mean exactly five beakers, not six or four. Thus, if this figure 5
is used in a calculation, you may regard it as having as many significant figures as desired:

2 Chemistry 106 Experiment 1


5.0000… (an unlimited number). Another example of an exact number is a number used to
relate quantities (conversion factors) within the same system of units:
1.0000… m = 100.0000… cm. These are defined values and possess an unlimited
number of significant figures.

Uncertainty in Calculations:
Measured quantities are often used in calculations in lab. The precision of a calculation
is limited by the precision of the measurements on which it is based.
 Addition and Subtraction:

When measured quantities are used in addition or subtraction, the final answer is limited
by the least decimal place in which all digits are significant. In this example, The
tenths place (one after the decimal place) is the least decimal place.
Example: 32.01 m + 5.325 m + 12.1 m = 49.435 m
The sum of the numbers is 49.435, but the sum should be reported as 49.4 meters
because 12.1 m is only known to the tenths place.

 Multiplication and Division:

When experimental quantities are multiplied or divided, the answer is limited by the
number in the calculation with the fewest number of significant figures than any of the
original numbers.

Example: 25.624 g / 25 mL = 1.02616 g/mL

Your calculator will read 1.02616, but the final answer should be reported as 1.0 g/mL
because 25 mL only has 2 significant digits.

3 Chemistry 106 Experiment 1


Reading volumes in graduated cylinders, volumetric flasks, pipets,

and burets:
When water is measured in a narrow glass container the top of the water does not form a
straight line. It forms a curved line called a MENISCUS. To read the volume correctly, adjust
the apparatus so that the bottom of the meniscus is at eye level and record the volume at the
bottom of the meniscus.

4 Chemistry 106 Experiment 1


Procedure

Part A: Density of Liquids (Pure Water)


1. Obtain approximately 30 mL of known liquid using a small beaker.
2. Place a clean, dry and empty 50 to 100 mL beaker onto a digital scale. To “Zero” the
digital scale with the graduated cylinder on it, press the “Re-Zero” or “Tare” button.
3. Using a 10 mL pipette, obtain approximately 5 mL of the known liquid.
4. Read and record the liquid volume from the marks on the pipette, using the correct
number of significant figures.
5. Place the liquid into the dry beaker (from step 1). Determine and record the mass of the
liquid using the digital scale. Re-zero the scale.
6. Repeat the procedure, this time using approximately 8 mL of the liquid.
7. Repeat the procedure, this time using approximately 10 mL of the liquid.
8. Using your mass and volume measurements, determine the density of the liquid for each
liquid sample.
9. Calculate the average density value.

Part B: Density of Solids (Regular Solid)


1. Record your sample number (or letter).
2. Determine and record the mass of your sample using a digital scale. (Note: sample must
be either cylindrical or rectangular.)
3. If your sample is cylindrical, measure the diameter of the circular face and the height
(H). From the diameter, determine the radius (r) for the cylinder. The radius is ½ the
diameter of the circular face.
4. Using the formula V = π × r2 × H for a cylindrical solid, determine the volume of your
sample.
5. Calculate the density of your sample and record this value in the data table.

Irregular Solid
1. Using a 100 mL graduated cylinder, obtain roughly 20 to 30 mL volume of an irregular
solid sample.
2. Record your sample number (or substance name).
3. Determine and record the mass of your sample (be sure it’s dry).

5 Chemistry 106 Experiment 1


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 water volume.
6. Carefully place your solid 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 initial water volume (no metal)
from the final water volume (with metal).
9. Calculate the density of your sample.

6 Chemistry 106 Experiment 1


Experiment (1)
Density
Student Name: Lab. Section:

Student Number: Partner Name:

Data and Results:


Part A: Density of Liquids (Known Liquid Sample)

Trial 1 Trial 2
1. Mass of liquid ………g ………g
2. Volume of liquid ………mL ………mL
3. Density of liquid ………g/mL ………g/mL

4. Average density of liquid …………g/mL

Unknown Liquid Sample


1. Number of unknown ………………

Trial 1 Trial 2
2. Mass of liquid ………g ………g
3. Volume of liquid ………mL ………mL
4. Density of liquid ………g/mL ………g/mL

5. Average density of liquid …………g/mL

6. Identity of unknown (from Table B) ……………………

Show calculations for trial 1.

7 Chemistry 106 Experiment 1


Part B: Density of Solids (Regular Solid)
1. Sample number ………
2. Mass of sample ………g
3. Sample dimensions
Cylindrical diameter ………cm radius ………cm height ………cm
4. Volume of Sample* (Note: 1 cm3 = 1 mL) ………cm3 = ………mL
5. Density of sample* ………g/mL
6. Identity of unknown (from Table A) ……………………
Show calculations for all items marked with an asterisk (*).

Irregular Solid
1. Sample number ………
2. Mass of sample ………g
3. Initial water volume ………mL
4. Final water volume ………mL
5. Volume of sample* ………mL

6. Density of sample* ………g/mL

7. Identity of unknown (from Table A) ……………………


Show calculations for all items marked with an asterisk (*).

8 Chemistry 106 Experiment 1


Appendix 1: Accepted Density Values

The “CRC” (short for Chemical Rubber Company Handbook of Chemistry & Physics) is a
commonly used source of physical and chemical data. Among the information compiled in
this resource are the density values for all of the solid and liquid elements and numerous
compounds. Refer to this data when identifying your unknown substance.

A) Physical Constants of Inorganic Compounds (solids):

Substance Density (g/cm3)

lead 11.3
gold 19.3
copper 8.96
aluminum 2.70
iron 7.87
zinc 7.14
tin 7.265
potassium chloride 1.988

B) Physical Constants of Organic Compounds (liquids):

Substance Density (g/mL)

Chloroform 1.4788
1, 2-ethanediol 1.1135
glycerol 1.2613
Carbon tetrachloride 1.594
ethanol 0.7893
water 0.998

9 Chemistry 106 Experiment 1


Experiment (2)

Physical Separation of Mixtures

Objective:
To separate a heterogeneous mixture based on each component's physical
properties.

Introduction:
A mixture is a physical combination of two or more pure substances where
each substance keeps its own chemical identity. For example, each substance in
a salt-water mixture has the same chemical properties as its would have when
pure, the water is present as H2O molecules and the salt is present as sodium ions
(Na+) and chloride ions (Cl-).

Mixtures are either homogeneous or heterogeneous. A homogeneous


mixture is made up to two or more substances having uniform properties and
composition throughout the mixture. Air is an example of a homogeneous
mixture of gases. A heterogeneous mixture contains two or more separate
phases. Today's experiment involves a heterogeneous mixture.

The method chosen for separating the mixture is based on the differences in
the chemical and/or physical properties of the mixture's components. Some
common physical methods for separating a mixture's components include:

a- Distillation: vaporizing a liquid from a solid (or another liquid) and


condensing the vapor;

b- Crystallization: Forming a crystalline solid decreasing its solubility as a


result of cooling the solution, evaporating the solvent, or adding a solvent in
which it is less soluble so that solid crystals from;

1 Chemistry 106 Experiment 2


c- Extraction: removing a substance from a solid or liquid mixture by adding
a solvent in which the substance is more soluble;

d- Filtration: removing a solid substance from a liquid by passing the


suspension through a filter;

e- Centrifugation: removing a solid substance from a solution by means of a


centrifuge;

f- Sublimation: vaporizing a solid and recondensing its vapor (not all solids
sublime, however);

In this experiment, you will separate an unknown mixture of NH4Cl, NaCl,


and SiO2 using sublimation, extraction, and filtration methods. Some physical
properties of each chemical in the mixture are listed in Table-1 below.

Table (1): Physical Properties of Some Pure Substances

Solubility
Compound Molar Mass (g/100 g water Melting Point Appearance
at 25oC)

NaCl 58.44 35 801 White crystals

NH4Cl 53.49 37 Sublime at 340 White crystals

SiO2 60.08 0.0 > 1600 White crystals

2 Chemistry 106 Experiment 2


Practice Exercise:
A mixture weighs 9.8712g and contains 6.3164 grams of sodium chloride
and 3.4779 grams of silicon dioxide. The remainder of the mixture is ammonium
chloride. Calculate the percent by weight of each substance in the mixture.

1- Mass of mixture 9.8712 g

2- Mass of NaCl 6.3164 g

3- Mass of SiO2 3.4779 g

4- Mass of NH4Cl = mass of mixture – (mass of NaCl + mass of SiO2) = 0.0769 g

5- Percentage of NaCl = (Mass of NaCl/Mass of mixture) x 100% = 63.988%

6- Percentage of SiO2 = (Mass of SiO2/Mass of mixture) x 100% = 35.2335

7- Percentage of NH4Cl = (Mass of NH4Cl/Mass of Mixture) x 100% = 0.7790%

Experimental Procedure:
1- Weigh a clean, dry, evaporating dish and record its mass on the report
sheet.

2- Add about 2 g of the unknown mixture to the dish, weigh and record the
mass.

3- Place the evaporating dish (with sample) on a wire gauze.

4- Heat the dish slowly, but gradually increase the heat until the white fumes
of ammonium chloride stop vaporizing (approx. 15 minutes).

5- Cool the dish to room temperature, weigh, and record the mass on the report
sheet.

6- Add about 20ml of distilled water to the solid in the evaporating dish and
stir for about one minute. Decant the solution into a beaker. Add about 10
ml more of distilled water to the solid, stir again for about one minute, and
decant into the beaker. Repeat once the 10 ml washing and decant them
into the beaker.

3 Chemistry 106 Experiment 2


7- Get a fine porosity filter paper, weigh two of them and seal it into a
Buchner funnel with a small amount of distilled water. Have your
instructor approve your filtering apparatus. Transfer the decanted solution
in the beaker to the Buchner funnel. Rinse the solid with two sml portions
of water.

8- First air-dry the solid on the filter paper, and then in a 100oC constant-
temperature drying oven for about 10 minutes.

9- Allow to cool to room temperature, weigh, and record the mass on the
report sheet.

10- At the end of the laboratory period, wash the funnel and the evaporating
dish. Dispose of any sand in the waste beaker.

4 Chemistry 106 Experiment 2


Experiment (2)
Physical Separation of Mixtures
Student Name: Lab. Section:

Student Number: Partner Name:

Data and Results:


A- Data Unknown No. ……………..

1- Mass of evaporating dish. ……………. g

2- Mass of evaporating dish and unknown ……………. g


mixture

3- Mass of evaporating dish & unknown ……………. g


mixture after heating

4- Mass of filter papers ……………. g

5- Mass of filter papers & the solid ……………. g

B- Calculations and Results:

1- Mass of original mixture ……………. g

2- Mass of ammonium chloride in mixture ……………. g

3- Mass of sodium chloride in mixture ……………. g

4- Mass of silicon dioxide in mixture ……………. g

5- % NH4Cl in mixture ……………. %

6- % NaCl in mixture ……………. %

7- % SiO2 in mixture ……………. %

* Show your calculations below.

5 Chemistry 106 Experiment 2


Experiment (3)

Limiting Reactant

Objectives:
To determine the limiting reactant in a salt mixture.
To determine the percent composition of a salt mixture.

Techniques:
To effectively complete the experiment's objectives, review the following
techniques:
Technique 2d, 3 Transferring a liquid.
Technique 5 Decanting a liquid from a solid.
Technique 6 Flushing a precipitate from a beaker.
Technique 7 Folding filter paper for a filter funnel.
Technique 8 Filtering procedures.
Technique 19b Weighing on a balance,  0.001 g.

Introduction:
Two factors that limit the yield of products in a chemical reaction are (1)
the amounts of staring materials (reactants) and (2) the percent yield of the
reaction. Many experimental conditions-for example, temperature and pressure-
can be adjusted to increase the reaction's yield but because the chemicals react
according to fixed mole ratio (stoichiometrically), only a limited amount of
product forms from given amounts of starting materials. The reactant restricting
the amount produced is called the limiting reactant in the chemical system.
To better understand the concept of the limiting reactant, let's look at the
reaction studied in this experiment. The equation's molecular form is:
 Ba3 PO4 2  6 NaCl  30H 2 O............. (1)
2 Na3 PO4 .12H 2 O  3BaCl 2 .2H 2 O 
Since the reactant salts are soluble, Ba3 PO4 2 is insoluble, and NaCl soluble,
the ionic equation is:
 Ba 3 PO4 2  6Na   Cl   H 2 .......... (2)
6Na   2PO43  24H 2 O  3Ba 2  6Cl   H 2 O 
Presenting only the reacting ions in the reaction (removing spectator ions), we have:
 Ba3 PO4 2( s ) ......................(3)
2 PO43  3 Ba 2 

Two moles of phosphate ion from 2 moles of Na3PO4. 12H2O (F.W. = 380.2), or
760.4g reacts with 3 moles of barium ion from 3 moles of BaCl2. 2H2O (F.W. =

1 Chemistry 106 Experiment 3


244.2), or 732.6 g, producing 1 mole of Ba3(PO4)2 precipitate (F.W. = 602.0), or
602.0g, if the reaction proceeds to completion.
Suppose however only 700.0 g of Na3PO4.12H2O and 700.0 g of
BaCl2.2H2O dissolve in water and are mixed. How many grams Ba3(PO4)2 are
then produced? Since the equation reads in mole, not grams, the moles of each
reactant are first determined:
1molNa3 PO4.12 H 2O
700 .0 g Na3 PO4.12 H 2O   1.84 mol Na3 PO4.12 H 2O
380 .2 gNa3 PO4.12 H 2O
 1.84 mol PO43

1molBaCl2. 2 H 2O
700 .0 g Ba3Cl2. 2 H 2O   2.87 mol BaCl2. 2 H 2O
244 .2 gBaCl2. 2 H 2O
 2.87 mol Ba 2 

Equation 3.3: indicates that 2mol PO43 reacts with 3mol Ba 2  . With

1.84 mol PO43 present, is enough Ba 2  present for all of the PO43 to react?
Again, using Equation 3.3 and the 3:2 mol ratio of Ba 2  to PO43 .
3mol Ba 2 
1.84 mol PO43   2.76 mol Ba 2  reacts with 1.84 PO43
2mol PO43

Since only 2.76mol Ba 2  of the 2.87 mol Ba 2  added to the system reacts
with the 1.84 mol PO43 , PO43 is the limiting reactant, Ba 2  is the excess
reactant. In other words, all of the PO43 reacts, but not all the Ba 2  . An excess
of 2.87  2.76  0.11mol Ba 2 remains unreacted.

Once the limiting reactant is known, the theoretical yield of product is


calculated from the balanced equation. Since PO43 is the limiting reactant, we
determine the moles and grams of that are Ba3 PO4 2 that are expected to
precipitate:
2mol PO43 Produces 1mol Ba3 PO4 2 .
1.84mol PO43 Produces 0.920mol Ba3 PO4 2 .
 602.2 g 
1.84mol PO43 Produces  0.920mol    554 g Ba 3 PO4 2 .
 mol 
Thus 554 g of Ba3 PO4 2 form if the reaction proceeds to completion.

2 Chemistry 106 Experiment 3


In this experiment an unknown salt mixture of Na3PO4.12H2O and
BaCl2.2H2O is added to water where they form insoluble Ba3(PO4)2. Weighing
the initial salt mixture and the product's final weight, we determine the limiting
reactant and the salt mixture's composition.

Experimental Procedure:
Two trials are recommended for this experiment. To hasten the analyses,
weight duplicate unknown salt mixtures and simultaneously follow the procedure
for each. Label the beakers accordingly for Trial 1 and 2 to avoid intermixing
samples and solution.

A- Precipitation of Ba3(PO4)2:
1- Weigh on weighing paper (+0.001 g, Technique 19b) about 1.0g of an
unknown Na3PO4.12H2O-BaCl2.2H2O salt mixture (see your instructor).
Transfer it to a 400-mL beaker and add 200mL (0.2mL) of distilled (or de-
ionized) water. Stir the mixture with a stirring rod for about 1 minute and
then allow the precipitate to settle.
2- Cover the beaker with a watch glass and maintain the solution hot (80-
90oC) on a steam bath or with a low flame for 30 minutes (Figure 3.1).
Allow the precipitate to settle.
3- Decant (Technique 5) two 50-mL (0.2 mL) volumes of the supernatant
liquid into separate 100mL beakers, labeled beaker I and Beaker II. Save
for part B.

Figure (3.1): Warming the precipitate. Figure (3.2): Transfer of Ba3(PO4)2 precipitate
to filter

3 Chemistry 106 Experiment 3


4- The precipitate may be gravity-filtered (Techniques 7 and 8a) or vacuum-
filtered (Figure 3.2) using fine porosity filter paper, such as What man
No.42. See your instructor before continuing. Weigh (+0.001g) a piece of
filter paper and seal it into the filter funnel with a small amount of distilled
water. Discard the water in the receiving flask. Have your instructor
approve your filtering apparatus.
5- While the solution is hot, quantitatively transfer the precipitate (Technique
6) to the filter funnel. Remove any precipitate on the beaker's walls with a
rubber policeman and, with hot water, wash the precipitate on to the filter
(Technique 6). Rinse the precipitate with two 5.mL portions of hot water.
6- First air-dry the precipitate on filter paper, and then in a 100oC constant-
temperature drying oven overnight or until the next laboratory period.
Weigh (+0.001g) the precipitate and filter paper.

B- Determination of Limiting Reactant:


From the following two tests (Figure 3.3) we determine the limiting reactant
in the original salt mixture. Some cloudiness may appear in both tests but one
shows more definite precipitate formation.
1- Test for excess PO43 . Add 2 drops of Ba 2  0.5M (0.5m BaCl2) to the 50 mL
of supernatant liquid in Beaker!. If a precipitate forms, then PO43 is an
excess and Ba 2  is the limiting reactant.

Figure (3.3)

4 Chemistry 106 Experiment 3


Experiment (3)

Limiting Reactant
Student Name: Lab. Section:

Student Number: Partner Name:

Data and Results:


Trial 1 Trial 2

A- Precipitation of Ba3(PO4)2:

Unknown number …………..…………

1- Mass of salt mixture (g) ………… …………

2- Mass of filter paper (g) ………… …………

3- Mass of filter paper and Ba3(PO4)2 ………… …………

4- Mass of Ba3(PO4)2 (g) ………… …………

B- Determination of Limiting Reactant:

1- Limiting reactant in salt mixture ………… …………

2- Excess reactant in salt mixture ………… …………

Calculation:

1- Moles Ba3(PO4)2 Precipitated: M.Wt. = 602.2 g/mol ………… …………

2- Moles BaCl2.2H2O reacted ………… …………

3- Mass BaCl2.2H2O reacted (g): M.Wt. = 244.2 g/mol ………… …………

4- Moles Na3PO4.12H2O reacted (g): M.Wt. = 380.2 g/mol ………… …………

5- Mass Na3PO4.12H2O reacted (g): M.Wt. = 380.2 g/mol ………… …………

6- Mass of salt mixture A.1 (g) ………… …………

7- Mass of excess reactant, B.2 (g)#6-#3or#5 ………… …………

5 Chemistry 106 Experiment 3


8- Percent BaCl2.2H2O in mixture ………… …………

9- Percent Na3PO4.12H2O in mixture ………… …………

* Show your calculations for one trial below.

6 Chemistry 106 Experiment 3


Experiment (4)

Colligative Properties

Objective:
To determine the molar mass of a non-electrolyte compound in water by
measuring the freezing point of pure water and of solution.

Introduction:
The properties of a solution differ considerably from those of the pure
solvent. Those solution properties which depend primarily on the concentration
of solute particles rather than their nature are called colligative properties. These
properties include vapor pressure lowering, osmotic pressure, boiling point
elevation and melting point depression. The relationships among colligative
properties and solute concentration are best regarded as limiting laws. They are
approached most closely when the solution is very dilute. In practice, the
relationships are valid, for nonelectroytes to within a few percent at
concentrations as high as 1M.

Solutions usually boil at higher temperature and freeze at a lower


temperature than pure solvent. A good example of solutes used to decrease the
freezing point of water is ethylene glycol or called antifreeze which is added to
car's radiator to prevent freeze-up of water in winter and boiling in summer.

The change in boiling or freezing point is a direct result of vapor pressure


lowering. At any given temperature, a solution of a nonvolatile solute has a
vapor pressure lower than that of the pure solvent. Hence, a higher temperature
must be reached before the solution boils. Figure (1) illustrates this reasoning
graphically.

1 Chemistry 106 Experiment 4


Figure 1: Changes in boiling point and freezing point of water.

Figure 1 shows that the freezing point of solution is the temperature at


which the solvent in solution has the same vapor pressure as the pure solid
solvent. This implies that it is pure solvent that separate when the solution
freezes. The increase in boiling point, ∆Tb , (usually called boiling point

elevation) and the decrease in freezing point, ∆T f , (Freezing point depression)

are directly proportional to the number of solute particles per mole of solvent
molecules. ∆T = Tsolvent − Tsolution

∆Tb = K b x m ∆T f = K f x m

Where K b and K f are the solvent's molal boiling point and freezing point
constants respectively, which have the unit of oC.kg mol-1, and m is the molality
of the solution which is the number of moles of solute per one kilogram of
solvent.

Figure 2, cooling curve for a pure solvent, shows you see a steady decrease
in temperature followed by a dip which is followed by a slight rise in the
temperature. This dip is not unusual and results from supercooling during the
early stages of the freezing process that may occur before freezing. Supercooling
results when a solution cools below its normal freezing point without freezing.

2 Chemistry 106 Experiment 4


To prevent supercooling, steady stirring of the liquid is required. Once
solid begins to form, further crystallization usually occurs rapidly without
supercooling. In this example the dip is followed by a short plateau in the
temperature. This plateau is at the freezing point of the pure solvent as shown in
Figure 2.

When solute is added to the solvent the shape of the cooling curve
sometimes changes so that we don’t see a clear horizontal plateau, as shown in
cooling curve for solution (Figure 2). In this case we must draw a trend line
through the data points corresponding to the cooling of the liquid and a trend line
through the data points corresponding to the freezing of the liquid. The
temperature at the point where those two lines intersect is the freezing point of
the solution (see Figure 3).

Figure 2: Freezing curve for a pure solvent and solution.

3 Chemistry 106 Experiment 4


Figure 3: Solution cooling curve showing best fit straight lines through the two
portions of the curve discussed in the text.

Example:
What would be the freezing point and boiling point of a solution containing
65.0g of ethylene glycol (C 2 H 6 O 2 ) commonly used as an automotive antifreeze,
in 200.0 g of water. (for pure water K f = 1.86oC/m, K b = 0.52oC/m, T f = 0Co, T b
= 100oC).
Moles of C 2 H 6 O 2 = mass/molar mass = 65.0g/62.0 g/mol = 1.05 mol

M = moles of solute/kg of solvent = 1.05 mol/0.200 kg = 5.24 mol/kg

∆T f = K f x m = 1.86oC/m x 5.24m = 9.75oC

T f ( solution) = T f ( water ) − ∆T f

0-0.75 = 9.75oC the solution freezes at -9.75oC

∆Tb = K b x m = 0.52oC/m x 5.24m = 2.70oC

Tb ( solution) = Tb ( water ) + ∆T f

100 + 2.70 = 102.70oC; Tb ( solution) = Tb ( water ) + ∆T f

100 + 2.70 = 102.70oC the solution boils at 102.70oC

4 Chemistry 106 Experiment 4


In this experiment,, you will determine the formula weight of a non-
volatile, non-electrolyte compound in water by measuring the freezing point of
pure water and of solution.

Procedure:

A-Freezing point of pure solvent (H 2 O):


1- Prepare an ice bath by filling a 400 or 600 mL beaker 2/3 full with crushed
ice, a small amount of water and table salt.

2- Weigh an empty and dry 200-mL test tube, and add 30.0 mL of water. Place
a thermometer in the test tube (Figure 4) and record the temperature under
time = 0 seconds on the data sheet.

3- Insert the test tube deep into the ice bath, carefully stirring the solution
continuously with the wire stirrer, and record the temperature every 30
seconds on the data sheet.

4- Record the freezing point of water for 300 seconds (5 minutes): the
temperature at which two phases (ice and water) co-exist.

5- Using graph paper, plot temperature versus time and determine the freezing
point of water.

Figure (4): Freezing point apparatus.


5 Chemistry 106 Experiment 4
B- Freezing point of solution:
1- Remove the test tube from the cooling bath and melt the solidified water by
pouring tap water at its outside. Dry the outside and reweight.

2- Add 2.5 g of the solid unknown and carefully add it to the test tube. Stir the
mixture until the entire unknown has dissolved. Replace the thermometer and
record the temperature (time = 0) on the data sheet.

3- Determine the solution's freezing point in the same way as the solvent's was
found in Part A.

4- On your graph paper, plot temperature versus time and determine the
freezing point of the solution as before (see Figure 2).

6 Chemistry 106 Experiment 4


Experiment (4)

Colligative Properties
Student Name: Lab. Section:

Student Number: Partner Name:

Data and Results:


Trial 1 Trial 2

Part A. Freezing point of pure water:

Volume of water ……………. …………….

Freezing point of water ……………. …………….

Part B. Freezing point of Solution; Unknown No:…………….

Volume of water ……………. …………….

Mass of solute ……………. …………….

Freezing point of solution ……………. …………….

Calculations:

Molal freezing point depression constant for water = 1.86oC/ mol

Density of water = 1.00g/ mL

Mass of water in solution ……………. …………….

Mass of solute in solution ……………. …………….

Molar mass of unknown ……………. …………….

* Show all your calculations for Trial 1.

7 Chemistry 106 Experiment 4


Data - Temperature vs Time

Pure water

Time (sec) 0 30 60 90 120 150 180 210 240 270 300


Temperature
(oC)

Solution (Water +Unknown)

Time (sec) 0 30 60 90 120 150 180 210 240 270 300


Temperature
(oC)

Plot temperature versus time (cooling curve)

8 Chemistry 106 Experiment 4


Experiment (5)

Acid – Base Titration

Objectives:
1- To standardize sodium hydroxide solution.
2- To determine the molarity of strong acid solution.

Introduction:
Titration is a term used to describe an experiment in which one solution is
added to another using a burette. The two solutions contain to compounds which
react rapidly with each other. The solution in the burette is added until there is
evidence that the reaction between the two compounds is complete.
Acid-base reactions are one of the most common types of chemical
reactions. The reaction between an acid and a base can be represented by the
equation:
H (aq)  OH (aq)  H 2 O(l ) 1

This reaction is called a neutralization reaction, and proceeds sufficiently to


the right to be considered quantitative. Therefore, the titration can be used to
determine the concentrations of acidic and basic solutions. The titration is
performed by adding a basic solution from a burette to a measured quantity of an
acid solution until the number of moles of OH- is just equal to the number of
moles of H+. This is called the equivalence point of the titration, and is detected
by an indicator which changes color as close to the equivalence point. The
change in color is called the end point. As possible, the change in color is called
the end point of the titration.
In this experiment, you will first determine the molarity of an NaOH
solution by titrating against a primary standard acid (potassium hydrogen
phthalate which has precisely known concentration). Then you will use the
standardized NaOH solution to determine the molarity of a sulfuric acid (H2SO4)
solution of an unknown concentration.

1 Chemistry 106 Experiment 5


A- Standardization of NaOH solution:
The primary standard "potassium hydrogen phthalate"; KHC8H4O4(KHP);
is used to standardize the NaOH solution (to determine exactly the molarity of
the NaOH solution). A known weight of KHP is dissolved in distilled water and
titrated with NaOH solution in the presence of phenolphthalein as indicator. At
the end point (the color of phenolphthalein indicator is changed from colorless in
an acidic solution to pink in a basic solution):

Mass of KHP
Moles of KHP = moles of NaOH or  M NaOH VNaOH 
Mwt of KHP

Example (1):
In an acid-base titration, 20.15 mL of NaOH solution was required to
neutralize 0.491 g of KHP (molar mass = 204.23 g/mol). What is the molarity of
the NaOH solution?
Mass of KHP
 M NaOH VNaOH 
Mwt of KHP

0.491 g
 M NaOH  0.02015 L
204 .23 g / mol

M NaOH  0.119 mol / L

B- Titrating an unknown solution of sulfuric acid:


The standardized NaOH solution is used to determine the molarity of the
sulfuric acid solution. A known measured volume of H2SO4 is titrated against
the standardized NaOH solution using phenolphthalein as indicator. The
molarity of H2SO4 solution is determined from measuring the volume of the
standard NaOH solution needed to neutralizer the H2SO4 solution.

2 Chemistry 106 Experiment 5


At the end point:

Moles of OH- = moles of H+

Moles of NaOH = 2 moles of H2SO4

(MNaOH) (VNaOH) = 2(MH2SO4) (VH2SO4)

Example (2):
The standardized NaOH solution (0.119 M) was titrated against 28.10 mL
of H2SO4. The volume of the standardized NaOH solution needed to neutralize
the H2SO4 solution was 24.28 mL. What is the molarity of the H2SO4 solution?
( M NaOH ) (VNaOH )  2( M H 2 SO4 ) (VH 2 SO4 )

0.119M  24.28mL  2M H 2 SO4  28.10mL

M H 2 SO4  0.0512 M

Procedure:

A- Preparing an NaOH solution by dilution:


Pour about 50 mL of approximately 1 M NaOH solution into a 500 mL
volumetric flask that contains approximately 50 mL of distilled water. Close the
flask with the stopper and shake. Then add distilled water to bring the final
volume up to the mark etched around the nick of the flask. Close the flask again
and shake thoroughly to make solution uniform.

B- Standardizing the NaOH solution prepared by dilution:


1- Weigh, as accurate as possible, about 0.4 g KHP on a weighing paper and
transfer it to a clean 125-mL Erlenmeyer flask. Record the mass of KHP
on your report sheet.
2- Add about 50 mL of distilled water and swirl to dissolve the KHP and
then add a few droops of phenolphthalein indicator.
3- Clean a 50 mL burette with soap and water using a burette brush and
rinse it thoroughly first with tap water then with distilled water.

3 Chemistry 106 Experiment 5


4- Add about 3 mL of NaOH solution to the burette. Turn the burette to it is
nearly horizontal but do not let NaOH run out of the open end. While you
hold the burette nearly horizontally, roll it in your fingers so the base
solution touches every part of the inside of the burette. Hold it upright
and drain the base through the tip. Repeat this rinsing twice to completely
wet the burette with NaOH solution.
5- Remove air bubbles from the burette tip. There should not be any air
bubbles in the burette or in the burette tip.
6- Titrate. Read the level of the solution in the burette and record it in your
report sheet before you start. Add NaOH solution with continuous
swirling of the Erlenmeyer flask. Continue the titration until you reach
the end point (the color of the solution is changed to pink which lasts for
about 30 seconds). Read the level of the base solution in the burette and
record it in your report sheet. The difference between the initial and the
final readings is the volume of NaOH required to titrate (neutralize) the
acid.
7- Repeat the titration with a new 0.4 sample of KHP.

C- Titrating a sulfuric acid solution of an unknown concentration:


1- Pick up a sample of the unknown sulfuric acid solution from the
instructor.
2- Clean a 10-mL pipette and rinse it with distilled water. Then rinse the
pipette a couple of times with about 2 mL of the acid.
3- Transfer 10.0 mL of the acid solution using the pipette into a clean 125-
mL Erlenmeyer flask. Add about 10 mL of distilled water and one drop of
phenolphthalein indicator and titrate with the NaOH solution. Record the
volume for the NaOH solution used to reach the end point.
4- Repeat the titration with a new 25.0 mL sample if H2SO4 solution.

4 Chemistry 106 Experiment 5


Experiment (5)

Acid – Base Titration


Student Name: Lab. Section:

Student Number: Partner Name:

Data and Results:


Trial 1 Trial 2
A- Standardization of NaOH solution:
Mass of KHP (g) ……………. …………….
Moles of KHP (Mwt of KHP = 204.23g/mol) ……………. …………….
Initial reading of NaOH burette (mL) ……………. …………….
Final reading of NaOH burette (mL) ……………. …………….
Volume of NaOH used (mL) ……………. …………….
Moles of NaOH used ……………. …………….
Molarity of NaOH (mol/L) ……………. …………….
Average molarity of NaOH (mol/L) ……………. …………….

B- Titrating an unknown solution of Unknown No:…………


sulfuric acid
Trial 1 Trial 2
Volume of H2SO4 solution used (mL) ……………. …………….
Initial reading of NaOH burette (mL) ……………. …………….
Volume of NaOH used (mL) ……………. …………….
Average molarity of NaOH (mol/L) ……………. …………….
Moles of NaOH used ……………. …………….
Moles of H2SO4 ……………. …………….
Molarity of H2SO4 (mol/L) ……………. …………….
Average molarity of H2SO4 (mol/L) ……………. …………….

5 Chemistry 106 Experiment 5


* Show your calculations for trial 1 in part A and part B.

6 Chemistry 106 Experiment 5


Experiment (6)

Chemicals In Everyday Life


Objectives:
To identify the chemical constituents of some household items and some
common chemicals.

Introduction:
It is important to know the composition of common substances at home and
handle them safely. In case of an accident the fast action is important before
taking the injured person to the hospital if it is needed, identification of
substances can be done either by instruments or by chemical tests of identify
some household items.

Warning:
"Never mix household chemicals unless you know what you are doing.
Mixing chemicals sometimes produces explosion, fires, or other hazardous
reactions".

Procedure:

A- Glass Cleaner, ammonia (NH3):


It is dilute solution of ammonia, (NH3), which is tested by a red litmus
paper. Hold a wet red litmus paper over a 100 ml beaker (or large test tube)
containing household glass cleaner (ammonia). Record your observations.

B- Fertilizers, ammonium salts (NH 4 ) :

Some ordinary fertilizers contain ammonium compounds. Ammonium salts


are converted to ammonia by strong bases:

NH4( aq)  OH (aq)  NH3( aq)  H 2O(1)

The familiar odor of ammonia could be noticed. The ammonia can be


tested by a red litmus paper as described above. Hold a wet litmus paper over a

1 Chemistry 106 Experiment 6


test tube containing small amounts of solid fertilizer (0.5g), add 1ml of 8M
NaOH solution to the test tube. Note the smell of the evolved gas by fanning the
gas with your hand toward your nose. Record your observation.

C- Table Salt, Sodium Chloride (NaCl):


Table salt is mostly sodium chloride, NaCl. The test for Cl- is to convert it
to HCl by strong acids, such as H2SO4, and the produced HCl is tested by blue
litmus paper:
2 NaCl( s )  H 2 SO4( aq)  2HCl( g )  Na2 SO4( aq)

Another test for Cl- is to convert it to a white solid AgCl by treatment with
AgNO3(aq):

Cl(aq)  AgNO3( aq)  AgCl( s )  NO3( aq)

Place about 0.5g of table salt in a test tube, add two drops of concentrated
H2SO4 Solution. Note the smell of the gas. Test the gas by a wet blue litmus
paper. Dissolve about 0.5g of NaCl in a test tube by adding 1ml of distilled
water and a drop of 3M HNO3 solution, then add 4 drops of 0.1M AgNO3
solution. Record your observations.

D- Baking Soda, sodium bicarbonate (NaHCO3); Lemon Juice,

and Vinegar:
Baking soda is sodium bicarbonate (NaHCO3), which is a basic salt that can
be reacted with acids to form CO2(g):

NaHCO3( s )  H (aq)  Na(aq)  H 2O(1)  CO2( g )

The CO2(g) evolved helps to raise the cake or dough. Lemon juice is simply
citric acid, and vinegar is a dilute solution of acetic acid. Both acids react with
baking soda.
Place about 0.5g of baking soda in a test tube, add 1-2ml of lemon juice or
vinegar. Record your observations. The test for escaping CO2(g) can be done by
holding a drop of Ba(OH)2 solution at the tip of a dropper, and inserting the
2 Chemistry 106 Experiment 6
dropper down into mouth of the test tube. Clouding of the Ba(OH)2 drop is a
proof for the presence of CO2(g) due to the formation of BaCO3(s):
CO2( g )  Ba(OH )2( aq)  BaCO3( s )  H 2O(1)

E- Bathroom Cleaner, HCl:


Most bathroom cleaners are dilute solution of HCl. Test form HCl in
cleaners can be done by reacting the cleaner with limestone CaCO3, which will
evolve CO2(g):
HCl( aq)   CaCO3( s )  CO2( g )  CaCl2( aq)  H 2O(1)

The test for evolved CO2(g) can be done as described above (in part D).
Place about 0.5g of limestone, CaCO3, into a test tube. Add 1-2ml of the
bathroom cleaner, record your observations.

F- Bleach, Cl2 / Water:


Commercial bleach is a 5% solution of sodium hypochlorite, NaOCl. This
solution behaves as though only chlorine, Cl2, were dissolved in water. Cl2(g) is a
yellow green gas and it is considered as a strong oxidizing agent. It can be tested
by oxidizing I- to I2 and I2 reacts with starch to form a dark blue complex:

Cl2( g )  2 I (aq)  2Cl(aq)  I 2( aq)

I 2( aq)  starch  dark blue complex

Dissolve 0.5g of NaI or KI in 1ml of distilled water, add drops of starch


solution then add 5 drops of bleach. Record your observations.

Warning:
Bleach is a toxic material and has an irritating odor. Avoid direct contact
with skin.

G- Drain Opener, NaOH/Al:


Drain opener is a mixture of solid sodium hydroxide and aluminum. When
this mixture comes in contact with NaOH dissolves readily and reacts with Al to
form H2 gas: 2 NaOH ( aq)  2 Al ( s )  6H 2 O(1)  2 Al (OH ) 4  2 Na(aq)  3H 2( g )

3 Chemistry 106 Experiment 6


NaOH solution dissolves the solid fats that clogs the drain, H2 gas build up
pressure which pushes wastes and dissolved fats down the drain.
Place about 0.5g of drain opener in a test tube, add 5ml of warm water and
shake well. Observe the formation of H2(g). Test form NaOH solution by a red
litmus paper. Record your observations.

H- Unknown:
Receive an unknown solid from your instructor. The unknown contains one
of the following ions: CO32 , Cl  , SO42 , or I-, Place a small amount of the

unknown in a dray test tube and add a drop of 18 M H2SO4. Use the following
table in determining the ion present in the unknown:

Table (1): Reaction of solid salts with concentrated H2SO4.

Ion Reaction

CO32  Colorless, odorless gas, CO2 evolved.

Cl- Colorless, pungent gas, HCl, evolve.

SO42  No Reaction

I- Violet vapors of I2 formed.

Perform additional test to help in identification of the ion present.

4 Chemistry 106 Experiment 6


Experiment (6)

Chemicals In Everyday Life


Student Name: Lab. Section:

Student Number: Partner Name:

Observations:
A- Glass Cleaner:
1- Change of litmus paper : …………………………………
2- Reason for the change : …………………………………

B- Fertilizer:
1- Change of litmus paper : …………………………………
2- Describe the smell of gas : …………………………………
3- The smell is due to the formation of : …………………………………

C- Table Salt:
1- Describe the smell of the gas formed : …………………………………
2- The gas formed is……………… and it will turn a ……………… litmus paper
into ………………
3- When AgNO3 solution is added to the salt solution, a ……………… solid is
formed which is ………………

D- Baking Soda:
1- Observation from the addition of lemon juice or vinegar to baking
soda:………………
2- Observation and equation of holding a drop of Ba(OH)2: ……………………

E- Bathroom Cleaner:
1- Observation and equation of addition of the cleaner to limestone: ……………....

5 Chemistry 106 Experiment 6


F- Bleach:
1- Observation from the addition of bleach to KI solution and starch:
The equation is …………………………………………………………………
2- The reaction is an oxidation-reduction, the element oxidized is:………………

G- Drain Opener:
1- Observation from the addition to warm water to the drain opener:
2- The changes of litmus paper:…………………………………………………….

H- Unknown:
1- Unknown No. is: …………………………………………………………………
2- Unknown Ion: ……………………………………………………………………
3- Confirmatory tests: ………………………………………………………………

6 Chemistry 106 Experiment 6


Experiment (7)

Qualitative Analysis of insoluble


chlorides: Ag+, Hg22+, Pb2+

Objectives:
To Separate and identify of some insoluble chlorides: Ag+, Hg22+, and Pb2+

Introduction:
Qualitative analysis is a method of finding out what kind of chemicals
(compounds, elements or ions) are presented in a sample regardless of their
quantities or concentrations. Based on the physical and / or chemical behavior of
a certain chemical we will be able to determine whether this chemical is present
or not in an unknown sample. We usually use the expression positive test: test
which indicates that the substance is present, and negative test: test which shows
that the substance is not present in the sample or its concentration is too low to be
detected by this test. The evidence for a positive test is one or more of the
following observations:
a- Formation, disappearance or changing of a color.
b- Formation or disappearance of precipitate.
c- Formation of a gas.
d- Change in the temperature.
e- Change in the reading of an instrument.
In this experiment, you are going to identify some cations (Ag+, Hg22+ and
Pb2+) and detect them in unknown solutions. According to the solubility of their
chloride salts, these cations can be considered as insoluble chlorides. Thus by
adding a Cl- ion the insoluble salts (AgCl, Hg2Cl2 and PbCl2) precipitate and the
other cations stay in solution. The precipitate and the solution (supernatant) can
be separated after centrifugation, then the cations in each side can be identified
using certain chemical test.

1 Chemistry 106 Experiment 7


I- Analysis of known solution:

This known solution contains all cations (insoluble chlorides) which you
are going to separate and analyze. Performing this analysis in a systematic way
(following the procedure step by step as shown below) is very important to
obtain correct results.

1- Separation of insoluble chlorides:


Obtain about 1 mL of the known solution in a small test tube (that can fit in a
centrifuge). Add 2-3 drops of 6.0 M HCl to this solution and then centrifuge the
solution. Decant the supernatant solution and keep the precipitate (AgCl, Hg2Cl2
and PbCl2) for part 2. The net ionic equations are:

Ag+ + Cl- AgCl(s) (AgCl is white, turning purple in light)


Hg22+ + 2Cl- Hg2Cl2(s) (Hg2Cl2 is white)
Pb2+ + 2Cl- PbCl2(s) (PbCl2 is white)
A slight excess of chloride ion is used to reduce the solubility of the
precipitates in accordance with the common ion effect. Even so the solubility of
lead chloride is sufficiently high for an appreciable concentration of lead ion to
remain in solution. A large excess of chloride ion should be avoided in order to
prevent the formation of soluble chloro complex ions which will dissolve the
precipitates. AgCl + Cl- AgCl2-

PbCl2 + 2Cl- PbCl42-

Hg2Cl2 + 2Cl- HgCl42- + Hg

2- Identification of insoluble chlorides:

A- Test for Pb2+:


Since PbCl2 is soluble in hot water but AgCl and Hg2Cl2 are not, Pb2+ can
be separated from Ag+ and Hg22+ by heating the solution. Wash the precipitate
obtained from part 1 by 1 mL of water then centrifuge and decant. Add 1 mL of
distilled water to the precipitate and heat the test tube in water bath for about 3
minutes. While the solution is hot centrifuge the mixture and transfer the

2 Chemistry 106 Experiment 7


supernatant solution to another test tube and save the precipitate for next step.
To the supernatant solution and few drops of 1 M K2CrO4. Formation of a
yellow precipitate indicates the presence of Pb2+.
PbCl2 + H2O Pb2+ + 2Cl-

Pb2+ + CrO42- PbCrO4

B- Test of Hg22+:
Ammonia, NH3, reacts with both Hg2Cl2 and AgCl. With Hg2Cl2 the
reaction produces a grey precipitate due to the formation of elemental black Hg(l)
and white mercury(II) amidochloride (HgNH2Cl). Reaction of AgCl with NH3

forms the soluble complex ion, Ag (NH3 ) 2 .

 Hg (l )  HgNH 2 Cl  NH 4  Cl (aq)
Hg 2 Cl 2  NH 3 
Black White

 Ag ( NH 3 ) 2( aq)  Cl (aq)


AgCl ( s )  2 NH 3( aq) 

To the precipitate (from step A above) add 10 drops of 6 M NH3, stir and
centrifuge the solution. Formation of a grey to black precipitate indicates the
presence of Hg22+. Transfer the supernatant solution to clean test tube and keep it
for the next step.

C- Test for Ag+:


Acidify the supernatant solution by adding few drops of 6 M HNO3, check
the acidity with blue litmus paper. Formation of a white precipitate indicates the
presence of Ag+ in the solution. The nitric acid converts the ammonia of the
silver complex ion equilibrium to ammonium ion:

Ag ( NH 3 ) 2  Cl   H  
 NH 4  AgCl ( s ) (white precipitat e)

3 Chemistry 106 Experiment 7


II- Analysis of unknown solution:
1- Ask your instructor for a sample of unknown solution of cations. Your
unknown solution may contain 1, 2, or 3 cations. Record your unknown
number on the report sheet.
2- Repeat the qualitative analysis tests described above and the reaction scheme

below to identify all cations (Ag+, Hg 22  ,Pb2+) present in your unknown


solution.

4 Chemistry 106 Experiment 7


Experiment (7)

Qualitative Analysis of Cations


Student Name: Lab. Section:

Student Number: Partner Name:

Unknown Number: …………………………

Mark each action below to indicate if it is present (+ve) or absent (-ve) in your
unknown.
Ion Result (+ve or -ve)

a- Pb2+ ………………………

b- Hg22+………………………

c- Ag+ …………………………

5 Chemistry 106 Experiment 7


Experiment (8)

Calorimetry

Objectives:
1- To determine the quantity of heat evolved in the neutralization of strong acid
with a strong base.
2- To determine the quantity and direction of heat flow for the dissolving of a
salt in water.

This experiment is designed to measure the heats of reaction of a series of


chemical reactions. There are several kinds of "heats of reactions", as an
example: heat of solution, heat of neutralization, heat of combustion, heat of
formation, etc. However, we will study only the first two of these:

1- Heat of Solution: It is the heat flow during the process of solution; as an


example when NaOH dissolves in water, hydrated ions are formed an heat is
released the solution absorbs this heat and, therefore increases in
temperature.

NaOH( s )  Na(aq)  OH (aq)  heat H1

Where the heat of solution in KJ is H1 .

2- Combined heat of solution and heat of neutralization: in a second reaction,


solid NaOH is reacted with an aqueous solution of HCl. During this
reaction, water and a dilute aqueous solution of sodium ions and chloride
ions are formed. This time both the heat of solution and the heat of
neutralization are released:

NaOH ( s )  H (aq)  Cl(aq)  H 2 O  Na(aq) Cl(aq)  Heat H 2

1 Chemistry 106 Experiment 8


3- Heat of neutralization: it is the heat evolved at constant pressure when acid is
neutralized with a base. It can be obtained from the two steps above. The
difference between the heat of reaction (obtained by dissolving solid NaOH
in aqueous HCl solution (step 2)) and the heat of solution (obtained by
dissolving solid NaOH in water (step 1)).

4- In another reaction (which we shall not perform in the lab.), we could add
distilled water to aqueous solution of sodium chloride. The heat released is
the heat of dilution. This effect was present in the reactions of step 1, 2 and
3 above; but we shall neglect this heat of dilution in our calculations because
it is smaller than the experimental errors expected in the measurement of the
other heats.

5- The final experiment of this laboratory class will be to determine the heat of
solution of an unknown salt, as in step 1 above.

Example (1):

2.00 g of solid CsOH is dissolved in 200.0 mL of water in a calorimeter.


The temperature of the water was raised from 22.3 to 23.4 oC. Calculate the heat
of solution in KJ/mol? (Assume the specific heat of solution to be 4.184 J/g.oC
and the density of solution to be 1.00 g/mL).

a- Temperature change, T  23.4  22.3  1.1o C.

b- Total mass of solution, m = (200.0 mL water) (1.00 g/mL) + 2.00g CsOH =


202.0g.

c- Heat absorbed by the solution = heat evolved by CsOH = mass of solution x


specific heat of solution x T = 202.0g x 4.184 J/ g.oC x 1.1oC = 930 J.

d- Moles of CsOH = mass / Molar mass = 2.00 g/149.9 mol/g = 0.01334mol.

e- Heat evolved per mole of CsOH = 930J/0.01334mol = 6.970 x 104 J/mol.

f- Heat of reaction in KJ/mol = -6.970 x104 J/mo x(1 KJ/103J) = -69.70 KJ/mol.

2 Chemistry 106 Experiment 8


Note: the minus sign shows that the reaction is exothermic; i.e. heat is given up
(evolved) by the system.
Example (2):
2.00 g of solid CsOH reacted with 200.0 mL of an aqueous solution of HCl
in a calorimeter. The temperature of the solution was increased from 22.3 to 24.3
o
C. Calculate the heat of reaction in KJ/mol? (Assume the specific heat of
solution to be 4.184 J/g.oC. And the density of solution to be 1.00 g/mL).
a- Temperature change, T  2.0 o C .
b- Total mass of solution = 202.0 g.
c- Heat absorbed by the solution = 1.69 x 103 J.
d- Moles of CsOH = 0.01334 mol.
e- Heat evolved per mole of CsOH = 1.27 x 105 J/mol.
f- Heat of reaction in KJ/mol = -127 KJ/mol.

Note: The difference in the heat of reaction (Example 2) and the heat of solution
(Example 1) is the heat of neutralization (Hn). So the heat of
neutralization of NaOH with HCl is -57.30 KJ/mol.

Hn is generally expressed in units of KJ/mol of acid (or base) reacted. Mass (g)
equals the combined masses of the two solutions. The heat of neutralization ,Hn,
is determined by (a) assuming the density and the specific heat of the acidic and
basic solutions are equal that of water, and (b) measuring the temperature, T ,
when the two are mixed:
Hn = mass of solution (g) x specific heat of solution (J/g.oC) x T ( oC )

3 Chemistry 106 Experiment 8


Procedure:
Assume that the density of all solution is 1.00 g/mL and their specific heat is
4.184 J/g.oC.

A- Determination of the heat of solution of NaOH (H1):


1- Add 100.0 ml of water to the calorimeter.

2- Close the calorimeter and stir the water until a constant temperature is
reached. Measure the initial temperature of water.

3- Weigh 2.0 g of NaOH. You should weight the NaOH fast, since it is very
Hygroscopic.

4- Add the solid NaOH to the 100 ml of water in the calorimeter and stir
gently until the maximum temperature reached.

B- Determination of the heat of reaction (H2):


1- Add 100.0 ml of 0.500 M HCL solution to the calorimeter.

2- Close the calorimeter and stir the solution until a constant temperature is
reached. Measure the initial temperature of solution.

3- Weigh 2.0 g of NaOH. You should weight the NaOH fast, since it is very
Hygroscopic.

4- Add the solid NaOH to the HCL solution in the calorimeter and stir gently
until the maximum temperature is reached. Measure the maximum (Final)
temperature.

C- Determination of the heat of solution of an unknown salt:


1- Pick up an unknown salt from the instructor and record the unknown number
on the report sheet. You will be told the molar mass of the salt.

2- Repeat the procedures in part A, using 3.0g of the unknown salt in place of
NaOH.

4 Chemistry 106 Experiment 8


Experiment (8)

Calorimetry

Student Name: Lab. Section:

Student Number: Partner Name:

Data and Results:


Trial 1 Trial 2
Part A. Determination of the heat of solution of NaOH (H1)
Volume of water ……………. …………….
Mass of water ……………. …………….
Mass of NaOH ……………. …………….
Molar mass of NaOH 40.0g/mol
Moles of NaOH ……………. …………….
Mass of solution ……………. …………….
Initial temperature ……………. …………….
Final temperature ……………. …………….
H1 of solution ……………. …………….
Average H1 …………………….

Part B. Determination of the heat of reaction of NaOH (H2) and the heat of
neutralization:
Trail 1 Trial 2
Volume of HCl ……………. …………….
Mass of HCl ……………. …………….
Mass of NaOH ……………. …………….
Molar mass of NaOH ……………. …………….
Mass of solution ……………. …………….
Initial temperature ……………. …………….
Final temperature ……………. …………….

5 Chemistry 106 Experiment 8


H2 of solution ……………. …………….
Average H2 …………………….
Heat of neutralization(Hn = (H2 - H1) ……………. …………….
Average heat of neutralization …………………….

* Show all your calculations for Trial 1.

6 Chemistry 106 Experiment 8


Experiment (9)

Spectrophotometric Determination of an
Equilibrium Constant
Objectives:
1- To determine the equilibrium constant for the formation of a complex ion,
[Fe(H2O)5(SCN)]2+. This will be accomplished by using a spectrophotometer to
measure absorbance data, from which equilibrium concentrations can be
calculated with the Beer-Lambert Law, A =  l c.
2- To use graphing technique and data analysis to evaluate data.

Introduction:

Some processes (chemical or physical) go in one direction and are


irreversible, such as burning a piece of paper which produces, mainly, CO2 and
H2O. Another example is the reaction between a strong acid (such as HCl) and a
strong base (such as NaOH) to give a salt and water (eq 1).
irreversib le
HCl( aq)  NaOH( aq) 
 NaCl( aq)  H 2O(1)  (1)

There are many reactions that take place in solution that are equilibrium
reactions; that is, they do not go to completion, and both reactants and products
are always present. Examples of this type of reaction include weak acids such as
acetic acid dissociating in water, weak bases such as ammonia reacting with
water, and the formation of "complex ions" in which a metal ion combines with
one or more negative ions. We will study a reaction involving the formation of a
complex ion which occurs when solutions of iron(III) are combined with the
negative thiocyanate ion; they form a deep red color FeSCN2+ complex, in which
all species are soluble. The system studied is:

[Fe(H2O)6]3+ + SCN- [Fe(H2O)5(SCN)]2+ + H2O  (2)

1 Chemistry 106 Experiment 9


The Keq (equilibrium constant ) expresses the equilibrium position for a
chemical system. For example, a large equilibrium constant indicates the
equilibrium lies to the right. As with any equilibrium, the value of Keq will be the
same regardless of the initial concentrations of Fe3+ and SCN-, as long as the
temperature is constant. In this experiment you are going to calculate Keq by
determining the concentrations of Fe3+, SCN- and FeSCN2+ at equilibrium.
Because the concentration of H2O is essentially constant in dilute aqueous solutions,
we omit the waters of hydration; the equation becomes:

Fe3+ + SCN- Fe(SCN)2+


initial (i) A B 0
change () -x -x +x
equilibrium (eq) A-x B-x x

Its equilibrium expression is:


[ FeSCN 2 ]
K eq   (3)
[ Fe 3 ] [ SCN  ]

It is possible to follow this reaction and calculate the equilibrium constant


because the complex ion has a deep red color in solution, and therefore its
concentration can be determined using a spectrophotometer.
The experiment involves two major parts. First, a series of solutions of
2+ 2+
FeSCN must be prepared in which the concentration of FeSCN ions is known.
A spectrophotometer is used to measure the absorbance of light of each of these
2+
standard solutions, and then a graph of concentration of FeSCN vs. absorbance
is prepared. This graph serves as a calibration curve which will be used to
determine the concentration of the complex ion in solutions of unknown
concentration.
Secondly, a series of solutions is prepared in which varying amounts of
3+
the Fe ion and SCN- are present. The absorbance of each solution is measured
in the spectrophotometer, and the concentration of each substance present is
determined. These values are used to determine the equilibrium concentrations

2 Chemistry 106 Experiment 9


and equilibrium constant for the reaction. We will use several different initial
concentrations of the reactants to determine whether the equilibrium constant has
the same numerical value when the complex is formed under different
conditions.
1. Equilibrium Concentration of FeSCN2+. The principle of this technique is
based on absorbing light by certain chemical substances. When light passes
through solution of the red complex, FeSCN2+, the amount of light absorbed by
the complex at a wavelength of 447 nm is linearly related to the concentration of
FeSCN2+ in the solution according to Beer's law:

Absorbance at 447 nm (A) = constant x [FeSCN2+]………………..…. (4)

If the amount of light absorbed (represented by Astd) by a standard solution of


FeSCN2+ containing a known concentration of [FeSCN2+]std is measured then for
any equilibrium mixture the concentration [FeSCN2+]eq in the equilibrium
mixture can be calculated from the following relation:
[ FeSCN 2 ]eq  ( Aeq / Astd ) [ FeSCN 2 ]std  (5)

where Aeq is the absorbance of the equilibrium mixture and Astd is the absorbance
of the standard.
In preparing the standards, the Fe3+ concentration is much larger than SCN-
concentration. According to LeChatelier's principle, this should cause the
equilibrium in eq. 2 to shift far to the right; therefore the FeSCN2+ concentration
approximates the original SCN- concentration. In other words, we assume that
the position of equilibrium is driven so far to the right by the excess Fe3+ that all
of the SCN- is complexed, forming FeSCN2+.
2. Equilibrium Concentration of Fe3+. For each one mole of FeSCN2+
produced, one mole of Fe3+ must be consumed. The equilibrium concentration
of Fe3+ can be calculated as follow:
[ Fe 3 ]eq  [ Fe 3 ]in.  [ FeSCN 2 ]eq  (6)

3. Equilibrium Concentration of SCN-. In a similar way:


[SCN  ]eq  [SCN  ]in.  [ FeSCN 2 ]eq  (7)

3 Chemistry 106 Experiment 9


Example:
In an experiment a STANDARD solution of FeSCN2+ was prepared by
mixing 2.00 mL of 0.0045 M NaSCN with 8.00 mL of 0.20 M Fe(NO3)3 in 0.05
M HNO3 solution. Calculate the equilibrium constant for an equilibrium solution
prepared by mixing 4.00 mL of 0.0030 M solution of NaSCN with 6.00 mL of
0.0100 M Fe(NO3)3 solution. The absorbance of the standard solution is 0.48 and
the absorbance of the equilibrium solution was 0.36.
1. The Standard Solution Calculations:
a) The initial SCN- concentration:
(molarity of NaSCN) (Volume of NaSCN)
[ SCN  ]in 
total volume of the standardsolution
(0.0045 M ) (2.00 mL )
[ SCN  ]in 
10.00 mL

[SCN  ]in  9.0  10 4 M

b) FeSCN2+ concentration:
[ FeSCN 2 ]std  [SCN  ]in  9.0  10 4 M

2- The Equilibrium Mixture Calculations:


a) The initial Fe3+ concentration:
(molarity of Fe(NO 3 )3 ) (Volume of Fe(NO 3 )3 )
[ Fe3 ]in 
total volume of the solution
(0.010 M ) (6.00 mL )
[ Fe3 ]in   0.006 M
10.00 mL
b) The initial SCN- concentration:
(molarity of NaSCN) (Volume of NaSCN)
[ SCN  ]in 
total volume of the standardsolution
(0.0030 M ) (4.00 mL )
[ SCN  ]in   0.0012 M
10.00 mL

c) The equilibrium concentration of FeSCN2+:


We can use equation (6) and [FeSCN2+]std (from part 1 of this exercise) to

calculate [ FeSCN 2 ]eq

4 Chemistry 106 Experiment 9


[ FeSCN 2  ]eq  ( A eq / A std ) [ FeSCN 2  ]std

[ FeSCN 2  ]eq  (0.36 / 0.48) (0.0009 M )

[ FeSCN 2  ]eq  0.00068 M

d) The equilibrium concentration of SCN-:

[ SCN  ]eq  [ SCN  ]in  [ FeSCN 2 ]eq

[ SCN  ]eq  0.00052 M

e) The equilibrium concentration of Fe3+:

[ Fe3 ]eq  [ Fe3 ]in  [ FeSCN 2  ]eq

[ Fe3 ]eq  0.0053 M

f) The Equilibrium Constant:

[ FeSCN 2  ]eq
K eq 
[ Fe3 ]eq [ SCN  ]ec

0.00068 M
K eq 
(0.00052 M ) (0.0053 M )
Keq = 2.5 x 102 (2 significant figures)

CAUTION
All solutions contain nitric acid (for stability) which is very corrosive to
skin and eyes. Wash spills off yourself as quickly as possible. Neutralize spills
on the lab table with baking soda. Wash your hands before you leave the lab.

Procedure:
0.002 M Fe(NO3)3 - produces [Fe(H2O)6]3+ (or simply Fe3+) in solution
Stock solutions:
0.002 M KSCN - produces SCN- in solution

5 Chemistry 106 Experiment 9


A. The Standard Solutions:
1. Clean four 100-mL volumetric flasks very well, rinse then with distilled
water and let them drain. Pipet 2, 4, 6 and 8 mL of 0.00200 M NaSCN into
separate labeled 100-mL volumetric flasks. Pipet 25.0 mL of 0.200 M
Fe(NO3)3 into each flask and dilute to the 100 ml mark with 0.5 M HNO3.
These solutions establish a calibration curve for determining the equilibrium
FeSCN2+ concentration spectrophotometrically.

Solution 0.00200 M NaSCN 0.200M Fe(NO3)3 0.5M HNO3


1 2.0 mL 25.0 mL 73.0 mL
2 4.0 mL 25.0 mL 71.0 mL
3 6.0 mL 25.0 mL 69.0 mL
4 8.0 mL 25.0 mL 67.0 mL

Rinse the spectrophotometer cell (cuvet) twice with 1 mL of the solution,


which you are going to measure its absorbance, before doing any absorbance
measurement and then fill it approximately three-fourths full. Carefully dry
the outside of cuvet, removing water and fingerprints. Handle only its lip
thereafter. These cells are very expensive, use and handle them carefully.
Your instructor will demonstrate for you how to operate the
spectrophotometer

2. Make sure that the wavelength in the spectrophotometer is set at 447 nm.

3. Measure the absorbance for the blank solution (the solution that has only
0.500 M HNO3) and adjust the absorbance (A) to zero and the transmittance
(%T) to 100%.

4. Determine the absorbance (A) of each standard solution and record your
results in a table in your report sheet.

6 Chemistry 106 Experiment 9


B. The equilibrium solutions for determination of Keq:
1. Clean five 10 mL volumetric flasks very well, rinse them with distilled water
and let them drain. Label the flasks by numbers from 1-5. The table below
lists all the solutions and the quantities of the original solution to be added
(from burettes) to each flask.

Solution 0.00200 M 0.0020 M 0.50 M


Fe(NO3)3 NaSCN HNO3
1 5.0 mL 1.0 mL 4.0 mL
2 5.0 mL 2.0 mL 3.0 mL
3 5.0 mL 3.0 mL 2.0 mL
4 5.0 mL 4.0 mL 1.0 mL
5 5.0 mL 5.0 mL 0.0 mL

2. Measure the absorbance at 447 nm (A) for each solution by following the
same procedure above (step 2-5 in part A). Record the results in a table in
your report sheet.

7 Chemistry 106 Experiment 9


Experiment (9)
Spectrophotometric Determination of an
Equilibrium Constant
Student Name: Lab. Section:

Student Number: Partner Name:

A. The Standard Solutions:

Flask #1 Flask #2 Flask #3 Flask #4

[FeSCN2+]std = [SCN-]in
Absorbance (Astd)

Average Astd =…………………….

B. The Equilibrium Mixture:


Flask #1 Flask #2 Flask #3 Flask #4 Flask # 5

[Fe3+]in
[SCN-]in
Absorbance, A
[FeSCN2+]eq
[Fe3+]eq
[SCN-]eq
Keq

Average Keq: (K1 + K2 + K3 + K4 + K5)/5 = …………………….

Standard Deviation,  n 1, ( Error)  {[  ( K eq  K ) 2 ] / (n  1)}1 / 2 

K eq   n 1 

8 Chemistry 106 Experiment 9


Calibration curve for data collected in Part A:

9 Chemistry 106 Experiment 9


* Show one sample calculations of Keq for solution # 2 in part B.

11 Chemistry 106 Experiment 9


Experiment (10)

Solubility Product Constant And


Common-Ion Effect

Objectives:
1- To determine the molar solubility and Ksp of Ca(OH)2.
2- To determine the molar solubility of Ca(OH)2 in the presence of added Ca+2.

Apparatus and Chemicals:


125-mL Erlenmeyer flasks (3) Saturated solution of Ca(OH)2.
50-mL burette (3 g per 100ml H2O).
25-mL pipette (3 g of Ca(OH)2 and 1 g of
CaCl2.2H2O per 100 mL H2O).
0.1M HCL Methyl orange indicator.

Introduction:
Many common ionic compounds, which have a very limited solubility in
water, are called slightly soluble salts. A saturated solution of a slightly soluble
ionic compound produces a dynamic equilibrium between the compound and the
dissociated ions. However, because the compound is only slightly soluble, the
solution has a low concentration of ions. For example, in a saturated Ca(OH)2
solution, the equilibrium between Ca(OH)2(s) and the Ca+2(aq) and OH  (aq) ions
lies far to the left because of its low solubility:
Ca(OH ) 2 (s)  Ca 2 (aq)  2OH  (aq)

The equilibrium expression for this reaction is:


[Ca 2 ] [OH  ]2
Kc 
[Ca (OH )2]

Since in a heterogeneous equilibrium the concentration of solid Ca(OH)2 is


a constant for a given temperature, we can rewrite the expression as:
K sp  K c [Ca(OH)2 ]  [Ca 2 ][OH  ]2

1 Chemistry 106 Experiment 10


Ksp is called the solubility product constant or, more simply, the equilibrium
constant of a slightly soluble ionic compound.
A saturated Ca(OH)2 solution is filtered to remove solid Ca(OH)2 and the
OH  ion is titrated with a standard HCl solution to determine the number of
moles and its concentration. According to the equation for each mole of Ca(OH)2
that dissolves, one mole Ca+2 and 2 moles OH  are present in solution. Thus by
finding the [OH  ], the [Ca+2], Ksp and molar solubility of Ca(OH)2 can be
calculated. The molar solubility of Ca(OH)2 = [Ca+2] = 1/2 [OH  ].
The pH of the saturated solution is measured which allows an additional
means to calculate the equilibrium [OH  ] and then calculate the [Ca+2], Ksp and
molar solubility.
We use the same procedure to determine the molar solubility of Ca(OH)2
with Ca+2 added (an ion common to the slightly soluble salt equilibrium).
However, since Ca+2 is added from an external source [Ca+2]  1/2 [OH  ]. The
[Ca+2] is determined by the concentration added from the external source. The
[OH  ] is determined by the dissolving of the Ca(OH)2 so the molar solubility of
Ca(OH)2 = 1/2 [OH  ].

Example (1):
If 2.42 x 10-4 g of BaSO4 is dissolved in 100 mL of water. Calculate Ksp of
BaSO4?

2.42  10 4
Mol BaSO4   1.04  10  6 M
233 .4 g / mol

1.04  10 6 mol
Morality of BaSO4   1.04  10 5 M
0.1L

From the equilibrium: BaSO4 ( s)  Ba 2   SO42 

[ Ba 2  ]  [ SO42  ]  1.04  10 5

K sp  [ Ba 2  ] [ SO42  ]  (1.04  10 5 )2

K sp  1.1  10 10

2 Chemistry 106 Experiment 10


Example (2):
50.0 mL of a saturated solution of Ca(OH)2 required 11.0 mL of 0.1M HCL
to reach the methyl orange end point at 25oC. What is the value of Ksp for
Ca(OH)2.

Ca(OH )2 ( s)  Ca2  (aq)  2OH (aq)

M HCl  VHCl  M V
OH  OH 

11.0  0.1  50.0  M


OH 

M  2.2  10 2M
OH 

1
[Ca 2  ]  [OH  ]  1.1  10  2 M
2

K sp  [Ca2  ] [OH  ]2 (1.1  10 2 ) (2.2  10 2 )2

K sp  5.3  10 6

The Common Ion Effect:


As we mentioned earlier, in saturated solutions of slightly soluble salts
there is a dynamic equilibrium between the solid salt and its dissolved ions. The
addition of an ion common to the salt will shift the equilibrium to the left and the
solubility of the salt decreases, this according to Le Chatelier's principle.

Example (3):
What is the molar solubility of AgCl in water and in a 0.010 M solution of
NaCl? Ksp AgCl is 1.7 x 10-10.
 Ag   Cl 
AgCl 
In pure water
X X

K sp  ( x) ( x)  x 2  1.7  10 10 ; [ Ag  ]  [Cl  ]  x ; Molar solubility =1.3 x 10-5 M.

In a 0.01 M solution of NaCl : [ Ag  ]  x, and [Cl  ]  0.010  x  0.01M .


K sp  ( x) (0.010)  1.7  10 10 Molar solubility  x  1.7  10 8 M .

So the solubility of a salt is less in a solution that already contains one of its ions
than it is in pure water.

3 Chemistry 106 Experiment 10


In this experiment you will determine the solubility product constant for
Ca(OH)2 by titrating OH- with a standard HCl solution. Also, the molar
solubility of Ca(OH)2 is to be determined in the presence the common ion, Ca2+.

Procedure:
It is important to keep the bottles containing the Ca(OH)2 tightly capped
when not in use to prevent the solution from absorbing CO2. The reaction of
carbonic acid with the hydroxide ion will reduce the hydroxide ion concentration
and will precipitate CaCO3 (chalk), as shown in the equation below:
Ca(OH)2(s) + CO2(g)  CaCO3(s) + H2O(l)

A- Determination of Ksp and molar solubility of Ca(OH)2:

1- Decant the settled saturated Ca(OH)2 solution into a 125-mL Erlenmeyer


flask. Rinse 25-mL pipette with 2 mL of this solution, and transfer 25.0
mL of the solution using the pipette into a clean 125-mL Erlenmeyer flask
(do not let it stand around in the air for long periods of time to avoid
reacting with the CO2 and forming CaCO3). Add 2 drops of methyl orange
indicator and measure the temperature of the solution.

2- Rinse a clean 50-mL burette three times with 5 mL portions of 0.1M HCl
solution, then fill the burette with the acid.
3- Titrate the Ca(OH)2 solution prepared in step 1 with the 0.1M HCl
solution, the color of the indicator will change from yellow to red at the
end point. Record the volume of HCl used to reach this point.

4- Repeat titration with a new 25.0 mL sample of Ca(OH)2 solution.

B- Solubility of Ca(OH)2 in presence of Ca2+, the common ion

effect:
Repeat Part A, steps 1-4, using saturated Ca(OH)2 solution to which
0.100M CaCl2 has been added.

4 Chemistry 106 Experiment 10


Experiment (10)
Solubility Product Constant And Common-Ion Effect

Student Name: Lab. Section:

Student Number: Partner Name:

Data and Results:


Trial 1 Trial 2
A- Ksp and molar solubility of Ca(OH)2
Temperature of solution (o C) ………… …………
Burette reading, final (mL) ………… …………
Burette reading, initial (mL) ………… …………
Volume HCl used (mL) ………… …………
Concentration of standard HCl solution (M) ………… …………
Mole HCl added ………… …………
Mole OH- in saturated Ca(OH)2 solution ………… …………
Volume of saturated Ca(OH)2 solution (L) ………… …………
[OH-1] at equilibrium (mol/L) ………… …………
[Ca +21 at equilibrium (mol/L) ………… …………
Ksp of Ca(OH)2 from the titration = [Ca+2] [OH-]2 ………… …………
Average Ksp of Ca(OH)2 from the titration ……………………
Molar solubility of Ca(OH)2 from the titration ………… …………

5 Chemistry 106 Experiment 10


B- Solubility of Ca(OH)2 in presence of Ca+2
Trial 1 Trial 2
Temperature of solution (oC) ………… …………
Burette reading, final (mL) ………… …………
Burette reading, initial (mL) ………… …………
Volume HCl used (mL) ………… …………
Concentration of standard HCl solution (M) ………… …………
Mole HCl added ………… …………
Mole OH- in saturated Ca(OH)2 solution ………… …………
Volume of saturated Ca(OH)2 solution (L) ………… …………
[OH-1] at equilibrium (mol/L) ………… …………
Molar solubility of Ca(OH)2

Calculations:
Show your calculations for trial 1 from the titrations of Part A and Part B.

6 Chemistry 106 Experiment 10


Experiment (11)

Quantitative Yield of a Redox Reaction

Objectives:
1- To observe an oxidation-reduction reaction.
2- To calculate the molar concentration of Cu2+ solution by using a redox
reaction.

Introduction:
Chemical reactions involving the transfer of electrons from one reactant to
another are called oxidation-reduction reactions or redox reactions. In a redox
reaction, two half-reactions occur; one reactant gives up electrons (undergoes
oxidation and it's called a reducing agent) and another reactant gains electrons
(undergoes reduction and it's called an oxidizing agent), resulting in changes in
oxidation number. The electrons are not shown in equation (1) because they are
neither reactants nor products but have simply been transferred from one species
to another (from Cu to Ag+ in this case), the total number gained must equal the
total number lost.
Cu ( s )  2 Ag (aq)  Cu (aq2 )  2 Ag ............ (1)

According to this equation, Cu increases its oxidation number form 0 to +2


by losing 2 moles of electrons per mole of Cu, it is oxidized and is called a
reducing agent:
Cu ( s )  Cu (aq2 )  2e  ........ (2)

Ag+ decrease its oxidation number from +1 to 0 by gaining 1 mole of


electrons per mole of Ag+; it is reduced and it's called an oxidizing agent:
Ag (aq)  e   Ag ( aq) .................................... (3)

Now the question is, why does a reaction such as equation 1 occur, whereas

another reactions such as, Cu( s )  H (aq)  no reaction, does not occur?

1 Chemistry 106 Experiment 11


To answer this kind of question, we can get some help from what is called
an activity series, which is a list of metal arranged in order of decreasing ease of
oxidation, (table (1)). The activity series can be used to predict the outcome of
reactions between metals and either metal salts or acids. [Any metal on the list
can be oxidized by the ions of elements below it]. For example, copper is above
silver in the series. Thus, copper metal will be oxidized by silver ions, equation
(1). Whereas, copper is below hydrogen in the series. Thus, copper metal will
not be oxidized by acids.

Table (1). Activity Series of Metals: Metals arranged in order of decreasing ease
of oxidation.

Metals Oxidation reaction


Sodium
 Na   e 
Na 
Zinc
 Zn 2   2e 
Zn 
Iron
 Fe2   2e 
Fe 
Hydrogen  2H   2e 
H2 

Copper
 Cu2   2e 
Cu 
Silver
 Ag   e 
Ag 
Gold
 Au 3  3e 
Au 

From table (1), Zn is above Cu and H2, Thus, Zn metal will be easily
oxidized by both Cu2+ and H+ ions (i.e. the reactions proceed to completion
because zinc has a lower ionization energy). However, H2 is above Cu in the
series, and therefore Cu metal cannot be oxidized by H+ ions. Thus, if solid zinc
is added in excess to a solution of blue copper sulfate, the copper ions are
precipitated out of solution as solid copper, and zinc metal dissolves to form
aqueous zinc ions. As the copper ions are removed, the solution becomes less
blue, finally appearing colorless when all Cu2+ is precipitated. Any unreacted
zinc metal can be dissolved with dilute HCl, leaving copper as the only solid
2 Chemistry 106 Experiment 11
phase in the mixture. The copper can then be separated, dried and weighted. By
determining the mass of copper precipitated from a known volume of Cu2+
solution, it will be possible to calculate the molarity of Cu2+ solution. If the mass
of a known volume of Cu2+ solution is obtained, it is additionally possible to
calculate the density of the solution and the % by mass of copper in it.
In this experiment you will analyze a sample of Cu2+ of unknown molarity.
As a reminder, the relationships involving concentration, density, and % by mass
are listed below (in the present experiment, the solute is Cu2+).
Molar concentration = moles of solute / liters of solution.
Density = mass of solution (g) / solution volume (mL).
And by mass = mass of solute (g) / mass of solution (g).

Practice Exercise:
A student pipette 10.00 ml of CuSO4 solution, having an unknown molarity
and a density of 1.040 g/mL at 25oC, into a beaker and added 1.50 g of zinc
powder. The mixture was stirred occasionally over a period of about 5 minutes,
and then 10 mL of 6 M HCl was added. When bubbles stopped evolving, the
mixture was quantitatively transferred to a pre-weighed filtering crucible (mass =
10.8275g) which was connected to an aspirator. The reddish metal that separated
was washed with water and acetone. The crucible-with-metal was dried in an
oven at 100oC for 5 minutes, cooled, and found to weight 11.3459 g. Calculate
the molarity and % by mass of Cu2+ in the CuSO4 solution. Calculate the
molarity and % by mass of Cu2+ in the CuSO4 solution.

Mass of Cu = 11.3459 – 10.8275 = 0.5184g = mass of Cu2+ in the solution


moles of Cu2+ = mass/molar mass = 0.5184/63.55 = 9.157 x 10-3 mol
[CuSO4] solution = mole/volume = 8.157 x 10-3 / 10 x 10-3 = 0.8157 M
% by mass = mass of Cu2+ in the solution / total mass of solution
= mass of Cu2+ in the solution / (Volume x density)solution
= [0.5184g / (10 ml x 1.040 g/ml)] x 100% = 4.985%

3 Chemistry 106 Experiment 11


Experimental Procedure:
1- Pick up a CuSO4 solution of unknown concentration from the Instructor.
2- Pipette 100 ml of unknown solution into a clean, dry, and preweighed 50 ml
beaker. Weigh the beaker and solution. Measure the room temperature.
Record your measurements on the Report Sheet.
3- Add about 1 g (an excess) of granulated zinc to the Cu2+ solution and stir
with the glass rod. The mixture should be stirred occasionally until the blue
color disappears. Note: solid zinc should still be present at this time.
4- Add approximately 15 ml of 6 M HCL to the beaker and stir occasionally
until the bubbles stop evolving. The solid zinc should all be dissolved by
this time, leaving brown copper solid.
5- Weigh a filter paper, and set-up the suction filtration apparatus.
6- Transfer the reaction mixture from the beaker to the filtering Buchner funnel.
7- Wash the copper twice with distilled water, and once with about 5 ml of
acetone. Then let the aspirator pull air through the funnel until all obvious
liquid is gone.
8- Dry the copper solid in the oven for about 10 minutes. Allow to cool to
room temperature, and weigh the solid copper. Record the mass of solid
copper on the report sheet.
9- Calculate the density, the morality, and the % by mass of copper in the
solution.

4 Chemistry 106 Experiment 11


Experiment (11)
Quantitative Yield of a Redox Reaction

Student Name: Lab. Section:

Student Number: Partner Name:

Data and Results:


A: Data Unknown NO: ………………
Volume of CuSO4 solution …………… ml
Mass of CuSO4 …………… g
Room temperature …………… oC
Mass of filter paper …………… g
Mass of Filter paper + Cu …………… g
Mass of Cu …………… g

B- Results (show your calculations on the next page, with units):


Density of CuSO4 solution ……………
Molarity of CuSO4 solution ……………
% by mass of Cu in solution ……………
* Write the net ionic equation for the replacement of Cu2+ by Zn2+ in aqueous
solution:

………………………………………………………………………………………

………………………………………………………………………………………

………………………………………………………………………………………

* Write the net ionic equation for the dissolution of zinc by dilute HCl:

………………………………………………………………………………………

………………………………………………………………………………………

………………………………………………………………………………………

5 Chemistry 106 Experiment 11


Show your calculations below:

6 Chemistry 106 Experiment 11


Experiment (12)

Determination of a Rate Law

Objectives:
1- To determine the rate law for the redox reaction
2- To use a graphical analysis of the experimental data.

2 I   H 2O2  2 H  
 I 2  2 H 2O

Apparatus and Chemicals:


250-mL Erlenmeyer flask (5) Thermometer
250-mL beakers (5) 0.1M H2O2
50-mL graduated cylinder 0.3M KI
Pipette 0.02M Na2S2O3
Burette Starch
Stirring rod Buffer containing 0.5M HC2H3O2
Stop watch and 0.5M NaC2H3O2
Graph papers

Introduction:
The rate of a chemical reaction describes how quickly the reactants
disappear and the products form, and expressed as mol L-1 s-1. For the

hypothetical reaction, A2  2 B2 
 2 AB2 the rate can be measured by
observing the rate of disappearance of either A2 or B2, or the rate of appearance
of AB2, depending on which species is the easiest to detect and monitor during
the reaction. The rate of a reaction is related to the concentration of reactants by
the rate expression, for the above reaction the rate expression or the rate law is:

Rate  k [ A2 ] p [ B2 ]q

Rate expression or rate law where k is the specific rate constant, varies with
temperature but its value is independent of reactant concentrations. The

1 Chemistry 106 Experiment 12


superscripts p and q are the order of the reaction with respect to A2 and B2
respectively. p and q are always determined experimentally for a given reaction,
and there is no relation between their values and the coefficients in the chemical
equation. The overall reaction order is p + q.
One of the objectives of chemical kinetics is to determine k, p, and q. In
this experiment you will determine the rate law for the reaction between
hydrogen peroxide and potassium iodide in aqueous solution:

2 I   H 2O2  2 H  
 I 2  2 H 2O

In this reaction H2O2 oxidizes I- to I2 in the presence of H+ ions, the rate of

reaction can be expressed as: rate  k [ I  ] p [ H 2O2 ]q [ H  ]r .

This reaction is very rapid to be detected when the concentration of H+ is greater


than 0.001 M. However, if the concentration is less than 0.001 M, the reaction
occurs at a measureable rate. The concentration of H+ is maintained constant
during the reaction at a concentration of 1 x 10-5 M by using a buffer solution of
sodium acetate / acetic acid solution. As [H+] is consumed during the reaction,
the buffer equilibrium shifts to the right to supply additional [H+], Therefore,
CH3CO2H CH3CO2- + H+
the reaction rate is independent of the H+, and the rate law becomes:

Rate  k  [ I  ] p [ H 2O2 ]q

a. Determination of p:
To determine p, [H2O2] is kept constant and [I-] is changed, and therefore,

Rate  k  [ I  ] p . c c is a constant = [H2O2]q

Taking the logarithms of both sides: log ( Rate)  1og k   plog [ I  ]  log c .
Combining all constants, we have an equation for a straight line:
log ( Rate )  plog [ I  ]  c
y  mx b

2 Chemistry 106 Experiment 12


Therefore, a plot of log (Rate) Versus log [I-] yields a straight line with a slope
equal to p.

b. Determination of q:

To determine q, the concentration of [H2O2] varies, while [I-] is kept constant,


and the logarithmic form of the rate law is:

log(Rate)  q log [ H 2O2 ]  C 

Where C' equals log k' + log[I-]p. Therefore, a plot of log(Rate) versus log [H2O2]
yields a straight line with a slope equal to q.

3 Chemistry 106 Experiment 12


c. Measuring reaction rate:
To follow the rate of the reaction, two solutions are prepared:

Solution A: Solutions of KI, S2O32− (thiosulfate), starch and acetic acid-sodium


acetate buffer are prepared.
Solution B: H2O2
When solution A and B are mixed, H 2O2 reacts with I−:

equation 1: 2 I   H 2O2  2 H  
 I 2  2 H 2O
To prevent an equilibrium from being established in equation 1, the S2O32− is
present to react with the I2 as it is being formed.

equation 2: 2S2O32   I 2 
 2 I   S4O62 

As a result, I− is regenerated and maintains a constant concentration during the


course of the reaction until all of the S2O32− is consumed. When the S2O32− has
completely reacted in the solution, the I2 then reacts with the starch to form a
deep-blue I2•starch complex.

equation 3: I2(aq) + starch → I2•starch

The reaction rate is then followed by observing the time required for a
quantitatively measured amount of S2O32− to react is the time lapse for the
appearance of the deep-blue solution. This, in turn, measures the rate of I2
production (mol I2/ time), which is affected only by the initial concentrations of
H2O2 and I-.

The number of moles of I2 = 1/2 the number of moles of S2O32  , as indicated in

equation 2 between I2 and S2O32  .

4 Chemistry 106 Experiment 12


Example:
25mL of a buffer solution and starch were added to 15mL of 0.2M KI. To
this solution, 10 mL of 0.05M Na2S2O3 was added. When 25 mL of 0.1M H2O2
was added a blue color appeared after 90 seconds. Calculate the measured rate
and the rate constant for this reaction? Assume a first order reaction with respect
to both I- and H2O2, i.e. rate = k[I-] [H2O2].

Rate = mol I2 / time (s)


1 1
mol I 2  mol S 2 O32  ( ) (10 / 1000) (0.05)  2.5  10 4 mol
2 2

2.5  10 4 mol
rate   2.8  10 6 mol / s
90 s

Total volume of solution after mixing = 25 + 15 + 10 + 25 = 75 mL

The, initial concentrations of I- and H2O2 are calculated as follows:

15  0.2
[I  ]   0.04 M  from M1V1  M 2V2 
75
25  0.1
[ H 2O2 ]   0.033 M
75

Using the rate law for the reaction we have:

2.8  10 6 mol / s  k (0.04 mol L1 ) (0.033 mol L1 )

and k  2.12  10 3 mol 1L2 s 1

5 Chemistry 106 Experiment 12


Procedure:
Use clean and dry glassware, do not dry glassware with paper towels.

A. Preparation of solutions of reactants:


The following Table summarizes the preparation of the test solutions
required for this experiment, Each test is performed by mixing two solutions A
and B. Solution A contains the I- reactant in addition to buffer, starch, and
Na2S2O3. Solution B contains the H2O2 reactant.

Table (1): Composition of test solutions (All volumes are measured in mL)

Solution A
Test Solution B
Distilled 0.02M
solution Buffer 0.3M KI Starch 0.1M H2O2
water Na2S2O3
1 61.5 12.5 5.0 1 5.0 15
2 56.5 12.5 10.0 1 5.0 15
3 51.5 12.5 15.0 1 5.0 15
4 41.5 12.5 15.0 1 5.0 25
5 31.5 12.5 15.0 1 5.0 35

1- In a clean and dry 250 Erlenmeyer flask or 250-mL beaker add components
of solution A required for test 1. Measure the volumes of KI and Na2S2O3
using either a pipet or a buret. Stir thoroughly and record the temperature.

2- Measure 15mL of 0.1 M H2O2 (solution B) in a clean and dry 50-mL


graduated cylinder and transfer quickly to the Erlenmeyer flask. The
reaction begins where. H2O2 is added to solution. A. After mixing start
timing immediately in seconds with a watch or clock until the blue color of
I2. starch appears. Stop timing and record time elapsed to the nearest second.

3- Repeat steps 1 and 2 for test solutions 2, 3, 4 and 5 as described in Table 1.

6 Chemistry 106 Experiment 12


B. Calculations:
Refer to the Report sheet and calculate the following:

V (mL )  M
1. Number of moles of S2O32   .
1000

2. Number of moles of I 2  (1 / 2) moles S2O32  .

 ( mol I 2 )
3. The rate of reaction 
t

Since initial mol I2 = 0, and initial time = 0, we have:

mol I 2
rate  .
t (sec)

4. Calculate the initial concentrations of I- and H2O2. Note that the total volume
of reaction's mixture = 100 mL.

0.3M  V (mL )
[ I  ]i 
100

0.1 M  V (mL )
[ H 2O2 ]i 
100

5. Calculate the logarithms of rate, [I-]i, and [H2O2]i.

7 Chemistry 106 Experiment 12


C. Determination of reaction order:
1. Plot on linear graph paper log (mol I2/t), i.e. log rate versus log [I-]i for test
solutions 1, 2, and 3 (these solutions have constant concentrations of H2O2).
Draw the best straight line through the three points. Calculate the slope of
the straight line. The value of the slope is the order of the reaction, p, with
respect to I-.

2. Plot on linear graph paper log (mol I2/t) vs log [H2O2] for test solution 3, 4,
and 5 (these solutions have constant concentrations of I-). Draw the best
straight line and calculate the slope which gives the order of reaction, q, with
respect to H2O2.

D. Determination of the rate constant, k':


Use the values of p and q (obtained from part C) and the rate law equation:

moles I 2
Rate   k  [ I  ] p [ H 2O2 ]q
t (sec)

To determine k' for the five solution. Calculate the average values of k'.

8 Chemistry 106 Experiment 12


Experiment (12)
Determination of a Rate Law

Student Name: Lab. Section:

Student Number: Partner Name:

Report Sheet:

A. Data

Solution Temp. 1 2 3 4 5

1. Solution Temperature ______ ______ ______ ______ ______


(oC)

2. Time for color change, ______ ______ ______ ______ ______


Δt (sec)

B. Calculations

1. Mol S2O32  reacted ______ ______ ______ ______ ______

2. Mol I2 produced ______ ______ ______ ______ ______

3. Rate = Δ(mol I2) / Δt ______ ______ ______ ______ ______

4. log (Δ(mol I2) / Δt) ______ ______ ______ ______ ______

5. [I-]i (mol/L) ______ ______ ______ ______ ______

6. log [I-]i ______ ______ ______ ______ ______

7. [H2O2]i (mol/L) ______ ______ ______ ______ ______

8. log [H2O2]i ______ ______ ______ ______ ______

9 Chemistry 106 Experiment 12


C. Determination of the reaction order, p and q for each reactant

Using graphing calculators (page 11), determine the slope of the following lines.
Then write the rate law for the reaction.

log (Δ(mol I2) / Δt) vs log [I-]i = Slope = p = ______________

log (Δ(mol I2) / Δt) vs log [H2O2]i = Slope = q = ______________

Rate = ____________________________

D. Determination of k' The specific rate constant for the reaction

1 2 3 4 5

1. Values of k' _______ _______ _______ _______ _______

2. Average value of k' : ______________

E. Show your calculations for solution 1

11 Chemistry 106 Experiment 12


log (Δ(mol I2)/ Δt) vs log [I-]i

log (Δ(mol I2)/ Δt) vs log [H2O2]i

11 Chemistry 106 Experiment 12

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