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COLLEGE OF ARTS AND SCIENCES

General Chemistry for


Healthcare professions
Laboratory
Course Code: CHE 105L

Laboratory Manual
Spring 2023
College of Art and Science
By Mustafa Hussein

Revised by:
Dr. Jonathon Brooks

CHE105L Laboratory Manual Spring 2023 Page 1 of 44


Contents
Contents .......................................................................................................................................... 2
Introduction ..................................................................................................................................... 5
Lab Safety ....................................................................................................................................... 6
1. Scientific Method: Accuracy and precision ............................................................................ 8
Introduction ............................................................................................................................... 15
Sample calculations .................................................................................................................. 16
Procedure .................................................................................................................................. 16
Accuracy of the weighing ..................................................................................................... 16
Precision of different volume measuring techniques. ........................................................... 16
2. Properties and Changes of Matter ......................................................................................... 18
Objective ................................................................................................................................... 18
Introduction ............................................................................................................................... 18
Equipment and chemicals ......................................................................................................... 19
Safety precautions ..................................................................................................................... 20
Procedure .................................................................................................................................. 20
Mixing Liquids...................................................................................................................... 20
Dissolving a Solid in a Liquid .............................................................................................. 20
Mixing solutions ................................................................................................................... 20
Separation of mixtures .......................................................................................................... 20
3. Densities of Liquids and Solids ............................................................................................ 22
Objective ................................................................................................................................... 22
Introduction ............................................................................................................................... 22
Equipment and chemicals ......................................................................................................... 23
Safety Precautions ..................................................................................................................... 23
Procedure .................................................................................................................................. 23
Density of a liquid ................................................................................................................. 23
Density of a Regular Solid .................................................................................................... 23
Density of an Irregular Solid................................................................................................. 23
Calculations............................................................................................................................... 24
Density of a Liquid ............................................................................................................... 24

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Density of a Regular Solid .................................................................................................... 24
Density of an Irregular Solid................................................................................................. 24
4. Molar Volume of a Gas......................................................................................................... 25
Objective ................................................................................................................................... 25
Introduction ............................................................................................................................... 25
Sample calculations .................................................................................................................. 26
Safety Precautions ..................................................................................................................... 27
Procedure .................................................................................................................................. 27
5. Separation of Cations by Paper Chromatography ................................................................. 27
Objective ................................................................................................................................... 27
Introduction ............................................................................................................................... 28
Equipment and chemicals ......................................................................................................... 29
Safety Precautions ..................................................................................................................... 29
Procedure .................................................................................................................................. 30
Preparation of the Chromatogram ......................................................................................... 30
Analysis of the Chromatogram ............................................................................................. 30
Enhancement of the Chromatogram ..................................................................................... 30
6. Empirical formulae of a compound ...................................................................................... 31
Objective ................................................................................................................................... 31
Introduction ............................................................................................................................... 31
Sample Calculations.................................................................................................................. 31
Equipment and chemicals ......................................................................................................... 32
Safety precautions ..................................................................................................................... 33
Procedure .................................................................................................................................. 33
A Sulfide of Copper .............................................................................................................. 33
An Oxide of Tin .................................................................................................................... 33
Magnesium Oxide ................................................................................................................. 34
7. Titration of Acids and Bases ................................................................................................. 35
Objective ................................................................................................................................... 35
Introduction ............................................................................................................................... 35
Calculations examples .............................................................................................................. 36

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Example 1 ............................................................................................................................. 36
Example 2 ............................................................................................................................. 36
Chemicals and equipment ......................................................................................................... 37
Safety precautions ..................................................................................................................... 37
Procedure .................................................................................................................................. 37
Titration of Oxalic Acid with NaOH .................................................................................... 37
Titration of NaOH with unknown concentration of acid ...................................................... 38
8. Calorimetry: Calculating the Specific Heat of an Unknown Solid ....................................... 39
Objective ................................................................................................................................... 39
Introduction ............................................................................................................................... 39
Chemicals and equipment ......................................................................................................... 40
Procedure .................................................................................................................................. 40
Preparation for Calorimeter Runs ......................................................................................... 40
First Calorimeter Run ........................................................................................................... 40
Subsequent Calorimeter Runs ............................................................................................... 41
Calculations............................................................................................................................... 41
9. Qualitative Analysis of Some Common Ions........................................................................ 42
Objective ................................................................................................................................... 42
Introduction ............................................................................................................................... 42
Chemicals and Equipment ........................................................................................................ 42
Safety precautions ..................................................................................................................... 43
Procedure .................................................................................................................................. 43
Test for the Carbonate Ion (CO32-)........................................................................................ 43
Test for the Sulfate Ion (SO42-) ............................................................................................. 43
Test for the Phosphate Ion (PO43-) ........................................................................................ 43
Test for the Thiocyanate Ion (SCN-) ..................................................................................... 44
Test for Chloride Ion (Cl-) .................................................................................................... 44
Test for the Aluminum Ion (Al3+) ......................................................................................... 44
Test for the Copper (II) Ion (Cu2+) ....................................................................................... 44
Analysis of an Unknown Solution ........................................................................................ 44

CHE105L Laboratory Manual Spring 2023 Page 4 of 44


Introduction
This laboratory will introduce and guide you through the laboratory course. The laboratory manual
contains a small summary of the safety manual.
Each experiment contains an introduction describing the theory behind the experiment, any
important reactions, and some equations used to determine specific values in the experiments.

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1. Lab Safety
Safety is an essential part of working in a chemistry laboratory. You can avoid accidents if you
pay attention to what you're always doing, use good judgment, abide by safety regulations, and
follow instructions. A set of rules has been made and should ALWAYS be followed to protect
students, personnel, equipment, and the environment. The Laboratory safety rules have been
summarized below, but you must read the Laboratory safety manual and sign the authority letter
before entering the chemistry laboratory. Any action that contradicts these rules and regulations
might compromise your safety and the safety of colleagues, assistants, and Instructors. Think
wisely before attempting to put all these individuals at risk, be responsible.
• Students should not work alone without a supervisor in the laboratories.
• Always were a laboratory coat, gloves, and safety glasses. The Laboratory coat must be
buttoned, and the safety glasses must be worn when working in the laboratory.
• The students must only bring a notebook and a pen inside the laboratory. Bags and other
belongings must be placed outside the laboratory.
• Long hair should be tied back or pinned up and closed-toe shoes must be worn in the
laboratory. Contact lenses are prohibited in the laboratory.
• The laboratory benches should be wiped with 10 % bleach solution before and after
finishing and experiment.
• Do not eat, drink, or smoke in the laboratory.
• You should be aware of all available safety devices in the laboratory, their locations, and
how to use each.
• Never return poured chemicals to their original container and always handle volatile
chemicals inside a fume hood.
• Always follow the laboratory manual and your instructor/supervisor.
• No chemicals, reagents, or equipment must leave the laboratory.
• ALWAYS follow instructions from your supervisor and ask if you have any doubt. Better
safe than sorry.
The globally Harmonized System of Classification and Labelling of Chemicals (GHS) is an
international agreement of standards to replace local classifications and labelling systems round
the world. GHS include pictograms that are used for different chemicals indicating hazard
warnings. These pictograms can be found on chemicals in the lab and cleaning agents at home. All
GHS Hazard pictograms can be found in table 1 below. GHS also includes material safety data
sheets (MSDS) that provides information about the chemical, perspective to the hazards, and risk
management in the lab. The MSDS of the different chemicals can be found on the internet.

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Pictogram Code Pictogram Meaning
GHS01: Explosive Explosive compounds.

GSH02: Flammable Flammable gases, aerosols,


liquids, and solids.

GHS03: Oxidizing Oxidizing gases, liquids, and


solids.

GHS04: Compressed gas Compressed, liquefied,


refrigerated liquefied, or
dissolved gases.

GHS05: Corrosive Corrosive materials (strong


bases and acids)

GHS06: Toxic Toxic by all administration


routes (oral, dermal, and
inhalation).

GHS07: Harmful Skin and eye irritation.


Can have specific target
organ toxicity.

GHS08: Health hazard Used for respiratory


sensitization, carcinogenicity,
and reproductive and germ
cell toxicity.

GHS09: Environmental Hazard for the aquatic


hazard environment and have
environmental toxicity.

CHE105L Laboratory Manual Spring 2023 Page 7 of 44


Laboratory Equipment
Equipment Description Image
Beaker: A container where reactions are
carried out, solutions heated, and used to
transfer liquids. Typically, a waste beaker will
be placed on the working station and used for
liquid waste.

Erlenmeyer Flask (Conical Flask): Conical


shaped flask made of Pyrex, used to heat
solutions, chemical storage, undergo reactions
etc.

Wash/Spray bottle: flask containing deionized


water or 70 % ethanol (make sure to identify
the label). Used to clean the surface of the
working station or transfer water/ethanol to a
solution.

Graduated Cylinder: Used to measure


volumes of liquids. Comes in different sizes
and therefore it’s important to choose the
right graduated cylinder according to the
amount of liquid you need to measure.

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Volumetric flask: Used to measure and transfer
a specific amount of liquid very accurately.
Comes in different sizes.

Glass Pipettes: Used to measure and transfer


small volumes of liquids. Different sizes and
types of pipettes can be found inside the lab.
The most noticeable are graduated pipettes and
volumetric (transfer) pipettes.

Pipette pump: used to suck liquids inside the


pipette to measure and transfer the required
amount. The pump can be found in different
sizes.

Pasteur pipette: Small plastic or glass pipette


used to transfer drops or small amount of
liquids. Not as accurate as the glass pipettes.

Burette: Is a cylindrical glassware with a


stopcock on the bottom used to dispense a
known volume of liquid for titration
experiment.

Laboratory stand: A metal rod attached to a


heavy granite base. Used to attach different
clamps to hold different kinds of equipment.

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Support ring: Iron ring that can hold glassware
or other laboratory equipment. Must be
attached to the stand.

Burette clamp: Used to fix burette or other long


cylindrical objects into place. Must be attached
to the stand.

Pipestem triangle: used to place different


laboratory equipment like a crucible. Must be
placed on a support ring.

Wire gauze: Sheet of metal with a net pattern


with a ceramic center. Placed between the
Bunsen burner and glassware. Can be placed
on a support ring or a tripod

Bunsen burner: gas burner with a single gas


flame. Used to heat equipment, solutions etc.
Tripod: Stand with three legs used to support a
wire gauze or a pipestem triangle.

Heating plate: used as indirect heating of


solutions to a specific temperature.

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Evaporation dish: a small dish made of
porcelain. Used to evaporate solutions. Need to
be placed on a wire gauze.

Crucible: A ceramic container used to heat


metals or other compound to a very high
temperature. Can be placed on a pipestem
triangle.

Laboratory Tongs: used to gasp hot laboratory


equipment after heating.

Watch Glass: Circular piece of glass used to


evaporate liquids or to place solids while being
weighed.

Glass Funnel: Used to guide liquids and solids


to a small opening like an Erlenmeyer flask.

Büchner funnel + flask: a laboratory setup used


in filtration. This type of filtration is much
quicker than a standard filtration with a glass
funnel and filtration paper.

CHE105L Laboratory Manual Spring 2023 Page 11 of 44


Spatula: small stainless steel “scoop-like”
utensils used to transfer or scrape solids.

Stirring Rod: long glass cylinder with a


rounded end. Used to mix solutions.

Thermometers: Used to measure the


temperature of the environment, reaction, a
solution etc.

Test Tube: cylindrical tube with a closed


bottom. Used as a container to make small
reactions, heat a small amount of liquid etc.
transparent to make it easier to see the reaction.

Balance: is a scale for weighing. Different


balances exist depending on the accuracy and
precision of the mass needed for the
experiment.

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How to measure a liquid with the laboratory glassware: Meniscus point is formed when liquid
molecules adhere to the glassware's walls. This is referred to as adhesion. Always read the value
at the very bottom of the meniscus (fig. 1).

Figure 1 Proper reading of liquid volumes.

Laboratory Reporting
One of the goals of this course is to learn how to accurately and efficiently write a laboratory
report. This includes recording data and observations inside the laboratory, as well as writing a
report at home. The laboratory notebook is a critical component of this process since it will be
containing the data from the practical , poor reporting can lead to poor report preparation. A
notebook is essential in any research laboratory where data may need to be reviewed months or
years after it was collected, so full details are required. To write the data, no loose paper or scraps
should be used, and an ink pen must be used. The below requirements should be followed for your
notebook:
- Pages should be left for contents page to allow instructors to easily access findings
- Each lab session should be dated, and the title of the experiment must be indicated clearly.
- There should be a clear line between two lab sessions to avoid confusion of recording.
- Pages must not be removed from the notebook.
- Pages must be numbered.
- The notebook should include all experimental data (masses, reading etc.), any special
observations (colors)
- Use tables to organize data.
The number of significant figures depend on how accurate the measurement is. When measuring
volumes from graduated glass ware, estimate one digit beyond the marking. This is called the
estimated value. As shown in fig 2, the liquid is not 40 or 50 but something in between. This can
be estimated to 45 or even 43.

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Figure 2 uncertain value of a beaker with liquid.

The report should follow the lab report template and include following sections:
Introduction: Introduce the topic and describe the theory behind the experiment. At the end of this
section the purpose should be described.
Materials: Mention the equipment and reagents used to perform the experiment and mention
special safety cautions for the reagents. Try to use the GHS system to mention the safety hazards.
Method: This should tell a story of how you did the experiment. Try to white it in a chronological
order and avoid the use of bullet points. Use the story telling approach and describe what you did
in the lab and don’t copy directly from the lab manual since it can be counted as plagiarism. Past
tense should be used to describe what you did in the experiment e.g., “5 g of NaCl is added to the
solution”.
Results: The results should be described in text and should be in a chronological order. Always
show a sample calculation for each result and explain how to do the calculation. Use tables and
figures to organize your results and to make it easier to understand.
Discussion: This is the most important section in the report. This section should be used for result
interpretation and discussion. The discussion should describe what the results indicate and if it’s
acceptable with the theory, why did the does the result tell us, are there some unexpected results
and can they be explained, and what are the limitations of the experiment.
Conclusion: Used to sum up everything mentioned in the report and conclude. What did you find
out? Remember not to include any new information in this section.
Reference list: Mention all the references used in the report in an alphabetical order.

CHE105L Laboratory Manual Spring 2023 Page 14 of 44


1. Scientific Method: Accuracy and precision
Introduction
Precision and accuracy are one of the most important measures in the laboratory. Reproducibility
of an experiment is very important to prove a theory. These two terms might be used as synonyms,
but they mean something totally different in the scientific method.
Precision is a measurement of the reproducibility and how close the measurements are to each
other. The measurements do not have to be accurate to have a high precision. Accuracy on the
other hand is defined by how close the measurement is to the true value. The true value can be a
theoretical value that is determined by calculation or a reference value from a table or book. Fig.
1 shows a visualization of the principle of accuracy and precision.

Figure 3 Visualization of the concept of accuracy and precision.

Relative and percentage error is often used to determine the accuracy of the measured values from
the actual value by the following equation
𝑒𝑥𝑝𝑒𝑟𝑖𝑚𝑒𝑛𝑡𝑎𝑙 − 𝑎𝑐𝑡𝑢𝑎𝑙
𝑅𝑒𝑙𝑎𝑡𝑖𝑣𝑒 𝑒𝑟𝑟𝑜𝑟 =
𝑎𝑐𝑡𝑢𝑎𝑙

𝑒𝑥𝑝𝑒𝑟𝑖𝑚𝑒𝑛𝑡𝑎𝑙 − 𝑎𝑐𝑡𝑢𝑎𝑙
%𝑒𝑟𝑟𝑜𝑟 = ∗ 100
𝑎𝑐𝑡𝑢𝑎𝑙

The precision is determined by the standard deviation of a set of measurement. The standard can
be described as the amount of dispersion of a set of values. A low standard deviation (SD) indicates
that the values have a lower dispersion and are closer to the average value. To describe the SD, the
average/mean value must be defined. The average is the sum of all the values where the value is
represented by xi of the measurement divided by the number of collected measures (n).

𝑖𝑥𝑖
𝑎𝑣𝑎𝑟𝑎𝑔𝑒 = 𝑥 =
𝑛

The SD can be calculated by the following equation. n-1 is the degrees of freedom of the system.

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𝑑2
𝑆𝐷 = 𝑠 = ↔ 𝑑 = 𝑥𝑖 − 𝑥
𝑛−1

Sample calculations
A test object has been weighed on different balances. The measured data and the calculated
statistical values are presented in the table below
Balance number Mass (g) = xm 𝑑 = 𝑥𝑚 − 𝑥 d2
1 10.21 -0.03 0.001
2 10.23 -0.01 0.000
3 10.20 -0.04 0.002
4 10.22 -0.02 0.001
5 10.29 0.05 0.002
6 10.25 0.01 0.000
7 10.30 0.06 0.003
The average is calculated by the following equation:
i xi 71.70
x= = = 10.243
n 7

The s can then be calculated by the following equation:

𝑑2 0.009
𝑠= = = 0.0390
𝑛−1 7−1

The standard deviation is typically shown as ±s, that describes the range where 95 % of all results
can be found. that concludes that the results should be shown as: 10.243 g ± 0.039

Procedure
1. Accuracy of the weighing
A. Obtain an unknown material from the instructor. Record the identification number.
B. Weigh the object with the two analytical balances and record your data (repeat 6 times).
C. Ask your instructor for the actual value.
D. Calculate the percentage error and the average weight of the unknown object.
E. Repeat the process with an high precision analytical balance.

2. Precision of different volume measuring techniques.


A. Weigh an beaker with a parafilm wrap on the analytical balance. Record the weight.
B. Add 10 ml of deionized water measured with a graduated cylinder into the beaker.

CHE105L Laboratory Manual Spring 2023 Page 16 of 44


C. Weigh the beaker with the parafilm and water. Record the weight.
D. Repeat step A-C 3 times.
E. Empty the beaker and re-weigh the beaker and parafilm.
F. Add 10 ml of deionized water measured by a volumetric transfer pipette to the beaker.
G. Weigh the beaker, parafilm and water. Record the weight.
H. Repeat step E-G 3 times.
I. Calculate the percentage error and the standard deviation (s), each data set.

CHE105L Laboratory Manual Spring 2023 Page 17 of 44


2. Properties and Changes of Matter
Objective
• Determine experimentally the solubility of a pure substance in a given liquid, or, in the
case of two liquids, determine their miscibility.
• determine which of two immiscible liquids is denser.
• Determine whether a chemical reaction happens when two solutions are combined, and
then explain your reasoning.
• Separate sand from water by filtration and salt from water by evaporation.

Introduction
Matter is any substance that takes up space and has a mass. A pure substance is a sample of matter
that has identical properties throughout while a mixture is has different properties throughout.
Chemists classify matter according to its physical and chemical properties and can be classified as
a mixture or a pure substance, depending upon its properties and composition. Properties can be
classified as physical and chemical properties.
Physical properties are attributes of a substance that may be observed without affecting the
substance's composition. Taste, color, physical state (solid, liquid, gas), and density are examples
of physical attributes. Physical change simply causes a visual change, not a change in
composition. Let’s consider boiling water. The composition of water does not change, but its
appearance (physical state) changes from liquid to gas.
Chemical properties describe a substance's behavior when it alters its composition through
reaction with other substances or decomposition into two or more other pure substances. Some
examples are the ability to burn or the ability to react with other compounds like water. In a
chemical change, substances are converted into new products having properties and compositions
that are entirely different from those of the starting materials. A piece of wood can undergo a
chemical change when the carbon in the wood react with the oxygen and forming two new products
(Carbon dioxide and water).
Miscibility is a chemical property and it’s the ability of two liquids to be mixed and has a uniform
appearance. If the mixed liquids have a uniform appearance the liquids are said to be miscible and
will be called a solution. If two liquids are not miscible (immiscible), two distinct layers will
form when they are poured together and will be called a mixture. The liquid with the lowest density
will "float" on top of the other. This rule is applied for both solids and liquids.
solubility is the ability of a solute to dissociate in a liquid to form a solution. The solubility is often
measured as a concentration. A saturated solution has reached an equilibrium and no more solute
can be dissolved but some solutes does not reach an equilibrium and then the substance are said
to be miscible and soluble.

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If the solid does not dissolve, it is said to be insoluble. When two solutions are combined, a
chemical change, or reaction, may occur in which new products form. If so, it will be evidenced
by one of several visible changes. Among them are:
- Precipitate formation: A solid substance that is frequently finely dispersed throughout the
solution. If the precipitate is allowed to stand, it will settle to the bottom of its container.
- Effervescence: The formation of a gaseous product. The gas produced bubbles out the
solution.
- The appearance of a color change. A color shift usually signals the creation of a product
with a color that was not initially present among the reactants. The color may be the same
as one of the reactants, but in a darker or lighter tone.
Different compounds can be separated from a mixture by a range of different techniques. some
techniques use the physical properties to separate mixtures like the solubility and boiling point.
Two of the most utilized types of separation techniques are filtration and evaporation. Filtration
separate compounds that are insoluble in the liquid while evaporation separate compounds soluble
in the liquid.

Equipment and chemicals


Item Quantities Needed
Trichloroethane 3ml
water
Xylene 2.5ml
Barium Chloride (BaCl2) 0.5g
Sodium Sulfate (Na2SO4) 0.5g
Barium Sulfate (BaSO4) 0.5g
Sodium Carbonate (Na2CO3) 1.0 g
Hydrochloric acid (HCl) 1ml
Copper(II) sulfate (CuSO4) 0.5g
Ammonia solution (NH3aq) or 1ml
NH4OH
Test tube
Dropper
Weighing balance
Test tube holder
Büchner funnel
Büchner flask
Rubber bung
Filter paper
Evaporation dish
Water aspirator
Sand
Sodium Chloride (NaCl)

CHE105L Laboratory Manual Spring 2023 Page 19 of 44


Safety precautions

Procedure
1. Mixing Liquids
A. Place about 20 drops of trichloroethane and 10 drops of water into a test tube.
B. Stir the mixture with a stirring rod.
C. Identify the two liquids if not miscible. Record your observations.
D. Repeat the process but in reverse (20 drops of water and 10 drops of trichloroethane).
E. Repeat the procedure with 20 drops of water and 10 drops of xylene.
F. Repeat the experiment with 20 drops of trichloroethane and 10 drops of something that
mixes with oil xylene.

2. Dissolving a Solid in a Liquid


A. Place a small quantity of barium chloride (BaCl2) with the tip of your spatula in a test tube
B. Add 10 ml of deionized water in the test tube.
C. Stir the content of the test tube with a stirring rod.
D. Notice your observations
E. If small amount does dissolve in the test tube, add more water to dissolve all the solid.
F. Repeat the procedure with sodium sulfate (Na2SO4)
G. Combine the content of the two test tubes (made in step C and step F). Record your
observations
H. Set the test tube aside for 5-10 min. record your observations after the waiting period.
I. Repeat A-D with BaSO4.

3. Mixing solutions
A. Dissolve a small amount of sodium carbonate (Na2CO3) in 2 ml of water in a test tube.
B. Add 2-3 drops of hydrochloric acid (HCl) solution to the content in the test tube. Record
your observation.
C. Add more HCl and record your observations.
D. Dissolve a small amount of copper(II) sulfate (CuSO4) in 2 ml of water
E. add concentrated ammonia solution NH3(aq) dropwise. Record your observations.

4. Separation of mixtures
A. Add enough sand in a 150 ml beaker to cover the bottom.
B. add roughly equal amount of sodium chloride (NaCl).
C. Add 50 ml of deionized water and stir well with a stirring rod.
D. Set up the Büchner funnel filtration setup according to the instructor’s demonstration.

CHE105L Laboratory Manual Spring 2023 Page 20 of 44


E. Stir the mixture and pour it into the Büchner funnel.
F. Rinse the sand with deionized water.
G. Remove the filter paper and let the sand dry on a paper towel.
H. Transfer some of the water in the Büchner flask to an evaporation dish.
I. Heat the evaporation dish on a tripod and wire gauze over a Bunsen burner.
J. Record your observations.

CHE105L Laboratory Manual Spring 2023 Page 21 of 44


3. Densities of Liquids and Solids
Objective
• Calculate the density of a liquid or a solid from experimental data.

Introduction
Density is a physical property of liquids and solids, which is defined as its mass per unit volume.
𝑚𝑎𝑠𝑠
𝐷𝑒𝑛𝑠𝑖𝑡𝑦 =
𝑣𝑜𝑙𝑢𝑚𝑒

According to this equation, density is equal to the ratio of the mass of a sample of a substance to
the volume it occupies. The density of a solid is normally expressed in grams per cubic centimeter
(g/cm3) while the density of a liquid in grams per milliliter (g/ml), and the density of a gas in
grams per liter (g/l).
As shown in Equation 4.1, the density is determined by dividing the mass with the volume. Mass
is measured by the usual weighing techniques. A graduated cylinder can be used to gauge a liquid's
volume. A solid with a regular geometric shape, such as a rectangular block, cylinder, or sphere,
can have its dimensions measured with a ruler, and the volume can then be determined using those
measurements. When a solid with an irregular shape is submerged in a liquid, the volume of the
liquid that is displaced can be used to calculate the solid's volume.
In Part 1 of this experiment, you will be asked to determine experimentally the density of a known
substance and then to calculate the percent error in your determination. Percent error is defined by
the following equation:
𝑒𝑟𝑟𝑜𝑟
𝑃𝑒𝑟𝑐𝑒𝑛𝑡 𝑒𝑟𝑟𝑜𝑟 = ∗ 100
𝑎𝑐𝑐𝑒𝑝𝑡𝑒𝑑 𝑣𝑎𝑙𝑢𝑒

The ‘‘error’’ is the difference between the experimental value and the accepted value. Error is
expressed as an absolute value, i.e., a numerical value without regard for algebraic sign. Absolute
value is indicated by enclosing the quantity between vertical lines. Thus Equation 4.2 becomes
𝑒𝑥𝑝𝑒𝑟𝑖𝑚𝑒𝑛𝑡𝑎𝑙 𝑣𝑎𝑙𝑢𝑒 − 𝑎𝑐𝑐𝑒𝑝𝑡𝑒𝑑 𝑣𝑎𝑙𝑢𝑒
𝑃𝑒𝑟𝑐𝑒𝑛𝑡 𝑒𝑟𝑟𝑜𝑟 = ∗ 100
𝑎𝑐𝑐𝑒𝑝𝑡𝑒𝑑 𝑣𝑎𝑙𝑢𝑒

CHE105L Laboratory Manual Spring 2023 Page 22 of 44


Equipment and chemicals
Item Quantities Needed
Ethanol 8ml
Unknown liquid 8 ml
Water
Unknown irregular solids 2
10 ml graduated cylinder 2
100 ml graduated cylinder 1
Parafilm 2
Rectangular or square shape Objects 3

Safety Precautions

Procedure
1. Density of a liquid
A. Weigh a 10-mL graduated cylinder and a piece of plastic wrap.
B. Add roughly 8 ml of ethanol into the cylinder.
C. Measure and record the volume to nearest 0.1 ml.
D. Measure the mass of the container and ethanol on an analytical balance.
E. Calculate the density.
F. Repeat the procedure with the unknown liquid

2. Density of a Regular Solid


A. Record the color of the unknown regular solid.
B. Weigh the solid on an analytical balance. Record the mass
C. Measure the volume of the solid.
D. Determine the density of the regular solid.
E. Repeat the procedure with all the regular solids.

3. Density of an Irregular Solid


A. Place 20-25 ml of water into the cylinder and record the volume
B. Weigh the cylinder and water. Record the mass.
C. Place the unknown solid into the graduated cylinder.
D. Record the volume to the nearest 0.1 ml.
E. Weigh the cylinder, water, and the unknown solid on a centigram balance. Record the
mass.

CHE105L Laboratory Manual Spring 2023 Page 23 of 44


F. Repeat Steps 3A and 3E for 3 unknowns.

Calculations
1. Density of a Liquid
The mass of the liquid can be found by calculating the difference between the weight of the empty
container and the container + liquid. The accepted value for the density of 1,1,1-trichloroethane is
1.34 g/ml.

2. Density of a Regular Solid


The volume of a rectangular solid is calculated by this equation: 𝑉 = 𝑙 ∗ 𝑤 ∗ ℎ
The volume of a cylinder and a sphere can be calculated by following equations:
𝜋𝑑2 ℎ
𝑉𝑐𝑦𝑙𝑖𝑛𝑑𝑒𝑟 =
4

π = 3.14159265
𝜋𝑑3
𝑉𝑆𝑝ℎ𝑒𝑟𝑒 =
6

Once you have calculated the volume of the unknown solid, its density may be found by using the
first equation in the introduction.

3. Density of an Irregular Solid


Both the mass and the volume of the sample are found by difference. Density is again calculated
by using the first equation in the introduction.

CHE105L Laboratory Manual Spring 2023 Page 24 of 44


4. Molar Volume of a Gas
Objective
• Use experimental values to calculate a hydrogen's molar volume at room pressure and
temperature.

Introduction
The number of liters that one mole of a gas takes up is known as its molar volume. This experiment
aims to quantify the volume occupied by a predetermined number of moles of hydrogen gas. The
molar volume of a gas depends on the temperature and pressure.
The temperature may be ignored since the experiment is conducted at a fixed temperature (room
temperature) therefore the relationship between the pressure and volume can be described by
Boyle's Law, which describes the quantitative relationship between pressure and volume of a fixed
quantity of gas at a constant temperature:
𝑃𝑉 = 𝑐𝑜𝑛𝑠𝑡𝑎𝑛𝑡 𝑜𝑟 𝑃1 𝑉1 = 𝑃2 𝑉2

P is the pressure, V is the volume, and numbers 1 and 2 refer to the first and second measurement
of the gas sample. Each gas in a mixture exerts a specific amount of pressure on its own. The
partial pressure is the pressure that an individual component of the gas mixture would exert if it
took up the entire volume at the specified temperature. This can be expressed mathematically by:
𝑃 = 𝑝1 + 𝑝2 + 𝑝3 +. ..

P is the total pressure of the mixture and p1, p2, and p3 are the partial pressures of the compounds
in the mixture. This phenomenon is known as Dalton’s Law of Partial Pressures.
A "wet" gas—a gaseous mixture—is created when a confined gas that has been formed comes into
contact with water and gets saturated with water vapor. Tables can be used to find the relationship
between temperature and the partial pressure of water vapor (table 1).
Temperature (°C) Vapor Pressure (torr) Temperature (°C) Vapor Pressure (torr)
17 14.5 23 21.1
18 15.5 24 22.4
19 16.5 25 23.8
20 17.5 26 25.2
21 18.6 27 26.7
22 19.8 28 28.3

The Hydrogen, in this experiment, will be formed by the reaction of Magnesium with hydrochloric
acid (HCl). The volume of hydrogen generated can be measured by a eudiometer (a glass

CHE105L Laboratory Manual Spring 2023 Page 25 of 44


measuring tube). The volume of dry hydrogen at room temperature can be corrected and measured
by Dalton’s and Boyle’s Laws. The mass of aluminum reacted with the hydrochloric acid can be
used to calculate the number of moles of hydrogen formed by stoichiometry and the molar volume
of hydrogen in room temperature can then be determined.

Sample calculations
H2 was collected over water at 26 °C. 0.0796 g of Magnesium has been used to form the H2 gas,
the total pressure was 747 torr, and the volume was 80.5 ml.
Reaction equation: Mg + 2 HCl → H2 + MgCl2
Determine the pressure of dry H2 at 26 °.C:
The pressure of dry H2 can be calculated by using Dalton’s Law of Partial Pressure since water
vapor pressure at 26 °C is 25.2 torr:
𝑃 = 𝑝𝐻2 + 𝑝𝐻2 𝑂 → 747 𝑡𝑜𝑟𝑟 = 𝑝𝐻2 + 25.2 𝑡𝑜𝑟𝑟 → 𝑃𝐻2 = 722 𝑡𝑜𝑟𝑟

How many moles of hydrogen has been produced?


Mg has a molar mass of 24.3 g/mol. The reaction indicates that one mole of magnesium is needed
to produce one mole of H2.
0.0769 𝑔 𝑀𝑔
= 0.00317 𝑚𝑜𝑙 𝑀𝑔 = 0.00317 𝑚𝑜𝑙 𝐻2
24.3 𝑔/𝑚𝑜𝑙

Calculate the volume of dry H2 in room pressure (762 torr).


Since we know the volume of dry H2 in 722 torr, Boyle's Law may be applied.

𝑃1 𝑉1 = 𝑃2 𝑉2 → 722 𝑡𝑜𝑟𝑟 ∗ 80.5 𝑚𝑙 = 762 𝑡𝑜𝑟𝑟 ∗ 𝑉2 → 𝑉2 = 76.3 𝑚𝑙

What is the molar volume of hydrogen at room temperature?


Divide the calculated volume in atmospheric pressure with number of moles H2.
𝑚𝑙
(76.3 𝑚𝑙/1000 )
𝑙 = 24.1 𝐿 𝐻 /𝑚𝑜𝑙
2
0.00317 𝑚𝑜𝑙

Chemicals and equipment


Item Quantities Needed
6 M Hydrochloric acid (HCl) 10ml

CHE105L Laboratory Manual Spring 2023 Page 26 of 44


Magnesium pieces 0.07-0.08g
Steel wool
Copper wire
Deionized water 100ml
Water 1000ml
500ml cylinder
1 l beaker
Eudiometer/gas measuring tube
One hole rubber stopper
Utility clamp
LabQuest 3 (temperature +
atmospheric pressure sensor)
Safety Precautions

Procedure
A. Clean a small piece of Magnesium (0.07-0.08 g) with steel wool.
B. Weigh the Magnesium with an analytical balance.
C. Fold the Magnesium to a loosely shaped ball.
D. Wrap the Magnesium ball with a copper wire (no large holes should be present, or the
Magnesium can escape doing the reaction). Leave 10-12 cm copper wire unraveled.
E. Fill a 1000 ml beaker with deionized water.
F. Pour 10 ml of 6 M hydrochloric acid in the a 100 ml graduated cylinder.
G. Slowly pour deionized water down the side of the graduated cylinder (hold the cylinder at
an angle). Fill it to the top.
H. Lower the copper-wrapped Magnesium ball into the Beaker.
I. Place a piece of parafilm on the graduated cylinder.
J. Invert the cylinder quickly into the beaker while placing your hand over the cylinder.
K. Allow the reaction to proceed.
L. Adjust the graduated cylinder until the water level inside the cylinder and the beaker are
the same.
M. Record the volume of gas, the atmospheric pressure and temperature in the laboratory.

5. Separation of Cations by Paper Chromatography


Objective
• Separate a mixture of ions by paper chromatography and calculate their RF values.

CHE105L Laboratory Manual Spring 2023 Page 27 of 44


• Analyze an unknown mixture of ions by paper chromatography.

Introduction
Chromatography is an analytical technique used to separate chemical substances from a
mixture. The individual compounds can then be collected and analyzed. Different types of
chromatography techniques has been developed for separation and isolation like liquid
chromatography, gas chromatography, affinity chromatography etc. but all of these follows
the same principle.
Chromatography, which means ‘‘the graphing of colors,’’ gets its name from the early
experiments of Tswett, who, in 1906, succeeded in separating a mixture of colored pigments
obtained from leaves. A solvent mixture, carrying the pigments, was allowed to pass through a
glass column packed with chalk. At the end of the experiment, the pigments were separated into
colored bands at various distances from the starting level. This method is now known as column
chromatography. Paper Chromatography is used for separating chemicals based on their
different affinity towards the stationary and mobile phase. . This technique is commonly used in
crime scenes or in laboratories to identify an unknown compound by comparing it to known
compounds.
The filter paper is referred to as the stationary phase or adsorbent. The mixture of solvents used
to carry the substances along the paper is called the mobile phase, or solvent system. In practice,
a sample of the solution containing the substances to be separated is dried on the paper. The end
of the paper is dipped into the solvent system so that the sample to be analyzed is slightly above
the liquid surface. As the solvent begins to soak the paper, rising by capillary action, it transports
the sample mixture upward. Each component of the mixture being separated is held back by the
stationary phase to a different extent. Also, each component has a different solubility in the mobile
phase and therefore moves forward at a different speed. A combination of these effects causes each
component of the mixture to progress at a different rate, resulting in separation.
In a given solvent system, using the same adsorbent at a fixed temperature, each substance can be
characterized by a constant retention factor, RF. By definition,
𝐷𝑖𝑠𝑡𝑎𝑛𝑐𝑒 𝑓𝑟𝑜𝑚 𝑜𝑟𝑖𝑔𝑖𝑛 𝑡𝑜 𝑐𝑒𝑛𝑡𝑒𝑟 𝑜𝑓 𝑠𝑝𝑜𝑡
𝑅𝐹 =
𝐷𝑖𝑠𝑡𝑎𝑛𝑐𝑒 𝑓𝑟𝑜𝑚 𝑜𝑟𝑖𝑔𝑖𝑛 𝑡𝑜 𝑠𝑜𝑙𝑣𝑒𝑛𝑡 𝑓𝑟𝑜𝑛𝑡

where the origin is the point at which the sample was originally placed on the paper and the solvent
front is the line representing the distance travelled by the solvent from baseline.

CHE105L Laboratory Manual Spring 2023 Page 28 of 44


2 cm

Figure 4 Developed Chromatogram

Equipment and chemicals


Item Quantities Needed
Mn2+ solution (optional)
Fe3+ solution
Co2+ solution
Ni2+ solution (optional)
Cu2+ solution
Acetone 9 ml
6 M HCl 1 ml
Con. NH3 5 ml
Capillary tubes
Chromatography/filter paper
250 ml Beaker
500 ml beaker
Watch glass
Pencil
Metal ruler
Heat lamp or air blower
Binder clip
Stirring rod
Spray machine
Fume hood

Safety Precautions

CHE105L Laboratory Manual Spring 2023 Page 29 of 44


Procedure
A. In a fume hood, combine 9 ml of acetone and 1 ml of 6 M HCl in a 250 ml beaker. swirl
the solution around to mix.
B. Close the beaker with a watch glass.
C. Lay a chromatographic/filter paper (5*10 cm) on a piece of tissue.
D. Draw a line 1 cm from the bottom of the filter paper.
E. Make 3 (3 for standard solutions, one for a mixture of the 3 solutions, and 2 unknown
solutions) marks on the line starting on the line (see fig. 1)
F. Label each mark with the three cations in front of you.
G. Repeat D-E with a new chromatography paper.
H. Label the marks with a mixture of the three cations and the last two with unknown mixtures
(UM1 and UM2).

1. Preparation of the Chromatogram


A. Apply a drop of the appropriate solution on the mark drawn on the chromatographic papers.
B. Let the drop dry and repeat the “spotting” process a 3-4 times.
C. Let the paper dry.
D.
E. Place a binder clip on the end of the chromatography paper.Place the stirring rod inside the
binder clip.
F. Place the filter paper into the developing chamber and close the chamber with the plastic
wrap (don’t let the filter paper touch the walls of the chamber).

2. Analysis of the Chromatogram


A. When the eluent front reaches 1-2 cm from the top of the filter paper remove the plastic
wrap and place the filter paper on a dry tissue.
B. Mark the eluent front with a pencil and let the filter paper dry completely.
C. Record the color of each band.

3. Enhancement of the Chromatogram


A. Place the filter paper in the ammonium chamber and cover with the plastic wrap.
B. When the Cu2+ band turns a deep blue color, remove the chromatogram, and circle any new
bands.
C. Mark the center of each band. Record the color of each metal ion after removing the filter
paper from the ammonia chamber.

CHE105L Laboratory Manual Spring 2023 Page 30 of 44


6. Empirical formulae of a compound
Objective
• Prepare a compound and collect data from which you can determine the mass of each
element in the compound.
• From the mass of each element in a compound, determine its simplest formula.

Introduction
During the late 1700s, chemists experimented with different elements form compounds. By
measuring the mass of a metal before reaction and the mass of metal oxide after reaction, chemists
were able to determine the formulas of metal oxide compounds. Chemical compounds are
composed of atoms of different elements. The atoms are held together by chemical bonds.
An empirical formula is the simplest ratio moles of each element in the compound. At times it may
be the same as the molecular formula; often, however, the molecular formula shows the simple
number of each atom in the molecule. For example, the empirical formula for benzene is CH while
the molecular formula is C6H6 the simplest formula of the compound benzene (C6H6) is simply
CH, indicating that the ratio of carbon atoms to hydrogen atoms is one to one. The empirical
formula can be determined experimentally by knowing the amount of each element in the
compound. In the experiment two elements with known mass will be combined and exposed to
high heat to react and form a compound. The mass of the compound can then be determined. The
ratio of moles between different elements can be calculated and the empirical formula can then be
determined.
During the late 1700s, chemists experimented with elements to see how they reacted to form
compounds. In particular, they were interested in the reactions of metals as they combined with
oxygen gas in the air. . ds. It has been shown experimentally that the ratio of moles of the elements
in a compound is nearly always a ratio of small, whole numbers. A few exceptions are known as
nonstoichiometric compounds. The simplest whole number ratio of atoms in a compound is
referred to as the simplest formula or the empirical formula. At times it may be the same as the
molecular formula; often, however, the molecular formula is an integral multiple of the simplest,
empirical formula. For example, the simplest formula of the compound benzene (C6H6) is simply
CH, indicating that the ratio of carbon atoms to hydrogen atoms is one to one.

Sample Calculations
A piece of aluminum is ignited in a suitable container, yielding an oxide. Calculate the simplest
formula of the oxide from the following data:
Mass of container 17.84 g
Mass of container + aluminum 18.38 g
Mass of container + compound 18.86 g

CHE105L Laboratory Manual Spring 2023 Page 31 of 44


1. Mass of each element from data:
𝑀𝑎𝑠𝑠 𝑜𝑓 𝑐𝑜𝑛𝑡𝑎𝑖𝑛𝑒𝑟 + 𝑎𝑙𝑢𝑚𝑖𝑛𝑢𝑚 − 𝑀𝑎𝑠𝑠 𝑜𝑓 𝑐𝑜𝑛𝑡𝑎𝑖𝑛𝑒𝑟 = 18.38𝑔 − 17.84𝑔 = 0.54𝑔 = 𝑀𝑎𝑠𝑠 𝑜𝑓 𝑎𝑙𝑢𝑚𝑖𝑛𝑢𝑚
𝑀𝑎𝑠𝑠 𝑜𝑓 𝑐𝑜𝑛𝑡𝑎𝑖𝑛𝑒𝑟 + 𝑐𝑜𝑚𝑝𝑜𝑢𝑛𝑑 − 𝑀𝑎𝑠𝑠 𝑜𝑓 𝑐𝑜𝑛𝑡𝑎𝑖𝑛𝑒𝑟 + 𝑎𝑙𝑢𝑚𝑖𝑛𝑢𝑚 = 18.86𝑔 − 18.38𝑔 = 0.48𝑔 = 𝑜𝑥𝑦𝑔𝑒𝑛 𝑚𝑎𝑠𝑠

2. Moles of each element:


𝑚𝑎𝑠𝑠 𝐴𝑙 0.54 𝑔
= 𝑔 = 0.020 𝑚𝑜𝑙 𝐴𝑙
𝑚𝑜𝑙𝑎𝑟 𝑚𝑎𝑠𝑠 𝐴𝑙 26.98
𝑚𝑜𝑙
𝑚𝑎𝑠𝑠 𝑂 0.48 𝑔
= 𝑔 = 0.030 𝑚𝑜𝑙 𝑂
𝑚𝑜𝑙𝑎𝑟 𝑚𝑎𝑠𝑠 𝑂 15.999
𝑚𝑜𝑙

3. Simplest formula ratio:


Obtain the ratio of atoms by dividing the number of moles of each atom by the smallest
number of moles.
𝑚𝑜𝑙 𝑂 0.02 𝑚𝑜𝑙
= = 1.5
𝑚𝑜𝑙 𝐴𝑙 0.03 𝑚𝑜𝑙

Which means that the ratio of Oxygen to Al is 1.5:1. The empirical formula must be a
whole number and therefore the formula is Al2O3.

Equipment and chemicals

Item Quantities Needed


Weighing balance
Option 1
Copper wire 2g
Sulfur 2g
crucible
Bunsen burner
Clay triangle
Wire gauze
Fume hood
Ring stand with support
Utility clamp
Crucible tongs

Option 2
Tin foil 2g
Nitric acid (HNO3) 5 ml

CHE105L Laboratory Manual Spring 2023 Page 32 of 44


crucible
Bunsen burner
Clay triangle
Wire gauze
Fume hood
Ring stand with support
Utility clamp
Crucible tongs

Safety precautions

Procedure
1. A Sulfide of Copper
A. Place a clean porcelain crucible and lid on a clay triangle.
B. Heat slowly first and then strongly about 4-5 min.
C. Cool the crucible and lid on a wire gauze
D. After cooling weigh the crucible and lid. Record the mass
E. Place around 1.5-2 g of copper wire in the crucible and weigh them with the lid.
F. Add 1-1.5 g of powdered sulfur on the copper wire.
G. Place the lid and begin heating (should be done in fume hood).
H. Heat slowly first and increase to moderate flame.
I. When sulfur no longer burns, heat the crucible strongly for 5 min.
J. Set the container aside to cool (DON’T open the lid).
K. Lift the lid and observe the contents.
L. If sulfur is still present, heat the crucible until no sulfur is present.
M. With the container and record the mass of the container and the compound.
N. Calculate and find the empirical formula of the compound.
O. Discard the content of the container when your calculations are corrected by the lab
instructor.
P. Before discarding, press the content to the bottom of the crucible.

2. An Oxide of Tin
A. Heat and weigh the crucible as instructed in in 1A-D.
B. Place 1-1.15 g of tin foil into the crucible. Weigh the crucible, lid, and the content.
C. Add Nitric acid (HNO3), in a fume hood until a white paste is formed.
D. Heat the crucible with a mild flame.

CHE105L Laboratory Manual Spring 2023 Page 33 of 44


E. After the liquid has evaporated, heat for 5 more min in a hot flame.
F. Cool and weigh the crucible.
G. Calculate and find the empirical formula of the compound.
H. Discard the content of the container when your calculations are corrected by the lab
instructor.
I. If the empirical formula is not accepted: add more nitric acid and follow the above steps.

3. Magnesium Oxide
A. Heat and weigh the crucible as instructed in in 1A-D.
B. Place a small piece (0.5-0.7 g) of magnesium into the crucible. Weigh the crucible, lid and
container.
C. Heat the crucible without the lid.
D. As soon as the magnesium begins to burn, replace the lid.
E. When the magnesium no longer burns, open the lid a little bit and heat strongly for 5 min.
F. Let the crucible and its content cool, add 10 drops of deionized water, and heat gently.
CAUTION: SPATTERING MAY OCCUR.
G. Heating the crucible and its content for 5-8 min with a strong flame.
H. Finish heating the crucible with a strong flame for 5-8 min.
I. Cool and weigh the crucible.
J. Calculate and find the empirical formula of the compound.

CHE105L Laboratory Manual Spring 2023 Page 34 of 44


7. Titration of Acids and Bases
Objective
• Calculate the molarity of the diluted solution using the volume of a solution with a known
molarity and the volume to which it is diluted in water.
• Calculate how many grams of a known solid base or acid are needed for the reaction given
the approximate molarity and volume of an acid or base solution to be used in a titration.
• Calculate the molarity of the base or acid solution using the volume of a base or acid
solution that reacts with a weighted amount of a primary standard acid or base.
• Perform acid–base titrations reproducibly.

Introduction
Titration is one of the most known analytical techniques to identify a concentration of an unknown
solution, called an analyte, with a solution who has a known concentration called a titrant. This
titration method utilizes the neutralization reaction between an acid and a base to reach the
equivalence point. The equivalence point is the pH value where the solution contains the same
number of moles H+ and OH-. When the solution reached the equivalence point, the pH will change
dramatically from the pH of the analyte to the pH of the titrant as shown in figure 1. To find the
equivalence point a suitable indicator is added to the analyte. It indicates the endpoint of the
reaction by changing color.

In this experiment you must determine the concentration of an acid solution by a sodium hydroxide
solution of known concentration. since solid sodium hydroxide has the property to absorb moisture
from the air it is not possible to weigh the solid accurately. By titrating the solution with a primary
standard solution of oxalic acid dihydrate (H2C2O4 • 2H2O). The reaction between the acid and
base is.

CHE105L Laboratory Manual Spring 2023 Page 35 of 44


2𝑁𝑎𝑂𝐻𝑎𝑞 + 𝐻2 𝐶2 𝑂4 𝑎𝑞 → 2𝐻2 𝑂𝑎𝑞 + 𝑁𝑎2 𝐶2 𝑂4 𝑎𝑞

An approximately 1 M sodium hydroxide has been made but you have to calculate the precise
concentration of sodium hydroxide by diluting the solution and perform a titration with oxalic acid
hydrate.
The number of moles of a concentration can be calculated by following equation
𝑚𝑜𝑙𝑒𝑠
𝑣𝑜𝑙𝑢𝑚𝑒 𝑙𝑖𝑡𝑒𝑟 ∗ 𝑀𝑜𝑙𝑎𝑟𝑖𝑡𝑦 = 𝑚𝑜𝑙𝑒𝑠
𝑙𝑖𝑡𝑒𝑟
The calculations in the pre-laboratory study assignment must be done and accepted by the lab
instructor before proceeding with the experiment.

Calculations examples
Example 1
25.0 ml of a 12 M solution has been diluted to a volume of 500 ml. calculate the number of moles
in the 25 ml solution and the concentration of the final 500 ml diluted solution.
The number of moles in the 25 ml solution can be calculated by using the equation in the
introduction:
𝑚𝑜𝑙
0.025 𝑙 ∗ 12 = 0.30 𝑚𝑜𝑙
𝑙

The concentration of the diluted solution can be calculated since the number of moles in these two
solutions don’t change.
𝑚𝑜𝑙 0.3 𝑚𝑜𝑙 𝑚𝑜𝑙
0.50 𝑙 ∗ 𝑥 = 0.3 𝑚𝑜𝑙 → = 0.6
𝑙 0.5 𝑙 𝑙

Example 2
If a sample of oxalic acid weighing 1.235 g requires 42.5 mL of the base for neutralization,
determine the molarity of a NaOH solution.
The of moles of oxalic acid must be calculated by the weight of the oxalic acid and the molar mass.
Notice that you should use the molar mass of oxalic acid dihydrate and not only oxalic acid.
1.235 𝑔 𝐻2 𝐶2 𝑂4 ∙ 2𝐻2 𝑂
𝑔 = 0.0098 𝑚𝑜𝑙 𝐻2 𝐶2 𝑂4 ∙ 2𝐻2 𝑂
126 𝐻2 𝐶2 𝑂4 ∙ 2𝐻2 𝑂
𝑚𝑜𝑙

CHE105L Laboratory Manual Spring 2023 Page 36 of 44


Then we can determine the moles of NaOH required to reach the equivalence point in the titration
since we need 2 moles of NaOH for each mole of oxalic acid (the reaction can be found in the
introduction).
2 𝑚𝑜𝑙 𝑁𝑎𝑂𝐻
0.0098 𝑚𝑜𝑙 𝐻2 𝐶2 𝑂4 ∗ = 0.0196 𝑚𝑜𝑙 𝑁𝑎𝑂𝐻
1 𝐻2 𝐶2 𝑂4

The molarity of the NaOH solution can now be determined since we know the number of moles
of NaOH present and the volume of the solution.
0.0196 𝑚𝑜𝑙 𝑁𝑎𝑂𝐻 𝑚𝑜𝑙
= 0.461 𝑀 𝑁𝑎𝑂𝐻
0.0425 𝐿 𝐿

Chemicals and equipment


Item Quantities Needed
Sodium Hydroxide (NaOH) 4g
500 ml Beaker
500ml Storage bottles
Oxalic Acid dihydrate 3g
(H2C2O4.2H2O)
Erlenmeyer flasks 6
buret 1
Phenolphthalein 1g
Magnetic stirrer
Deionized water
Hydrochloric acid (HCl) 60 ml
Acetic Acid 60 ml
Glass funnel 1

Safety precautions

Procedure
1. Titration of Oxalic Acid with NaOH
A. Calculate the mass of oxalic acid dihydrate (H2C2O4• 2H2O) needed to neutralize 15 ml of
0.2 M NaOH solution.
B. Add 75 ml of the oxalic acid solution into the three Erlenmeyer flasks.

CHE105L Laboratory Manual Spring 2023 Page 37 of 44


C. Rinse the burette with deionized water and then with 10 ml of the NaOH solution.
D. Discard and rinse again with the 10 ml NaOH solution.
E. Fill the burette with the NaOH solution (let the liquid flow through the tip to calibrate the
burette).
F. Add 3-5 drops of phenolphthalein and a stirring bar to each oxalic acid solution.
G. Start the stirring at moderate speed and start adding NaOH. Slow down the pouring 5 ml
before the calculated volume needed to reach the equivalence point.
H. The titration is complete when the pink color persists for 30 seconds. Record the burette
reading.
I. Adjust the volume of NaOH in the burette and repeat the titration.
J. Calculate the results of the tree titrations. The instructor must correct the calculations
before proceeding with the next part of the exercise.

2. Titration of NaOH with unknown concentration of acid


A. Clean and prepare the buret according to 1A.
B. transfer 10.0 ml of the unknown acid solution with a bulb pipet into each of three 250 ml
Erlenmeyer flasks.
C. Add 50 ml of deionized water and 3-5 drops of phenolphthalein to the unknown solutions.
D. Titrate each sample slowly until the pink color appears.
E. If the titrations yield more than 0.2 ml of each other: Run two additional titrations.
F. Calculate the molarity of the unknown acid. The calculations must be approved by the
instructor.

CHE105L Laboratory Manual Spring 2023 Page 38 of 44


8. Calorimetry: Calculating the Specific Heat of an
Unknown Solid
Objective
• Calculate the specific heat of an unknown solid element by measuring the heat exchanged
in a calorimeter.

Introduction
Chemical reactions involve the release or consumption of energy, usually in the form of heat. Heat
is measured in the energy units, Joules (J). It is a derived unit, having a base unit of kg*m2/sec2.
Commonly kilojoule (kJ) is used.
When heat energy passes between an object and its surroundings the “heat content” in that object
changes and that’s called the Heat flow. It is proportional to the mass of the object and its change
in temperature and therefore becomes an equation. The proportionality constant called specific
heat is introduced in the equation as shown below.
𝑄 = 𝑚𝑎𝑠𝑠 𝑠𝑝𝑒𝑐𝑖𝑓𝑖𝑐 ℎ𝑒𝑎𝑡 ∆𝑇 = 𝑚 ∗ 𝑐 ∗ ∆𝑇

Q is the heat flow in joules, m is mass in grams, c is specific heat in joules per gram degree (J/g*°C)
and ΔT is the temperature change or final temperature minus initial temperature.
Specific heat is a property of a pure substance. It is the number of joules of energy that are required
to raise the temperature of 1 g of the substance by 1°C. The specific heat of water is 4.18 J/g*°C.
This value is used often in calorimetry experiments.
When a ‘‘hot’’ object comes into contact with a ‘‘cold’’ object, heat flows from the hot object to
the cold object. The hot object raises the temperature of the cold object, and the cold object cools
the hot object. Eventually, they reach the same intermediate temperature.
Heat flow between objects can be measured in a calorimeter. A perfect calorimeter is an isolated
segment of the universe that allows no heat to flow to or from its contents during an experiment.
It follows from the law of conservation of energy that, in a perfect calorimeter,
𝑄=0
Where ∑Q is the sum of all changes in heat content within the calorimeter. We will assume that
the calorimeters we use are “perfect”. In this experiment, you will measure the specific heat of two
metals, one known and the other unknown. The known metal will be copper, which has a specific
heat of 0.38 J/g*°C. The percent error from this know value will be calculated and the known
specific heat of water will be used to calculate the specific heat of the unknown metal. The heat
flow of the water and the unknown metal should be 0 and therefore:
𝑄𝑤 − 𝑄𝑚 = 0 → 𝑄𝑤 = −𝑄𝑚
Substituting the expressions in the heat flow equation and the above equation gives:
𝑚𝑤 ∗ 𝑐𝑤 ∗ ∆𝑇𝑤 = − 𝑚𝑚 ∗ 𝑐𝑚 ∗ ∆𝑇𝑚

CHE105L Laboratory Manual Spring 2023 Page 39 of 44


Chemicals and equipment
Item Quantities Needed
800ml beaker 3
Deionized water 2L
Hot plate 1
Copper piece 1
Unknown metal 1
Weighing balance
Crucible tongs 1
Thermometer 1
Calorimeter 1

Procedure
1. Preparation for Calorimeter Runs
A. Place 500 ml of tap water into the beaker and set it on the table.
B. Place 400 ml of deionized water in another 500 ml beaker. Heat the water to boiling. Make
two of those.
C. Select an unknown metal and record the identification number.
D. Weigh the unknown metal and a piece of copper. Record the measurements.
E. Place the unknown metal and the copper in the heated water.
F. Boil the water and metals for 30 minutes.
G. If the water level doesn’t cover the metals completely, replenish from the second beaker.
H. Record the temperature of the boiling water.
I. place a thermometer in the Styrofoam cup and stabilize the thermometer with a buret
clamp.

2. First Calorimeter Run


A. Transfer 100 ml of the beaker in 1A to your calorimeter with a graduated cylinder.
B. Record the temperature of the water when the temperature has remained constant for about
1 min.
C. lift the piece of copper, using crucible tongs, above the beaker with the boiling water for
two seconds.
D. Lower the copper piece slowly into the calorimeter (be sure it’s completely submerged.
E. Stir the water with a glass stirring rod. Record the highest temperature reached before it
begins to drop.
F. Pour the water from the calorimeter into the sink. Place the copper back into the boiling
water.

CHE105L Laboratory Manual Spring 2023 Page 40 of 44


3. Subsequent Calorimeter Runs
Pour exactly 100 mL of water into your calorimeter. Repeat Steps 2B through 2F, using the
unknown metal.
Repeat the calorimeter runs again with the copper and the unknown metal.

Calculations
Calculate the specific heat of the metal for each run of the experiment, using equation in the
introduction, in which the specific heat is the only unknown. Find the percent error for the copper,
using the equation:
𝐸𝑥𝑝𝑒𝑟𝑖𝑚𝑒𝑛𝑡𝑎𝑙 𝑣𝑎𝑙𝑢𝑒 − 𝐴𝑐𝑐𝑒𝑝𝑡𝑒𝑑 𝑣𝑎𝑙𝑢𝑒
𝑃𝑒𝑟𝑐𝑒𝑛𝑡𝑎𝑔𝑒 𝑒𝑟𝑟𝑜𝑟 = ∗ 100
𝐴𝑐𝑐𝑒𝑝𝑡𝑒𝑑 𝑣𝑎𝑙𝑢𝑒

Find the average specific heat for the two runs with the unknown metal.

CHE105L Laboratory Manual Spring 2023 Page 41 of 44


9. Qualitative Analysis of Some Common Ions
Objective
• Conduct tests to confirm the presence of known ions in a solution.
• Analyze an unknown solution for certain ions.

Introduction
When we analyze an unknown solution, two questions come to mind: (1) what ions are present in
the solution, and (2) what is their concentration? The first question can be answered by performing
qualitative analysis, and the second by quantitative analysis. These two categories are known
as analytical chemistry. Analytical chemistry is one of the essential chemical courses that serve
as the foundation for future pharmacy specialists to study pharmaceutical chemistry,
pharmacognosy, forensic chemistry, drug technology, and so on.
To find out what ions are in the solution is to test for the presence of each possible component by
adding a reagent that will cause the component if present to react in a certain way. Difficulty arises
especially in complex mixtures, because one component may interfere with the analytical test for
another component. Although interferences are common, many ions in mixtures can usually be
identified by simple tests.
In this experiment, an unknown mixture of ions will be analyzed. The mixtures contain one or
more of these ions: CO32-, CL-, SCN-, SO42-, PO43-, Cu2+, Al3+. First, you will perform the various
tests designed to detect the presence of individual ions. Once you have observed these specific
reactions, you will obtain the unknown solution from your instructor. Then, taking small portions
of this solution, you will run each reaction again to determine which ions are present and which
are absent.

Chemicals and Equipment


Item Quantities Needed
1 M Hydrochloric Acid (HCl) 4ml
1 M Sodium Carbonate 1g
(Na2CO3)
0.5 M Sodium sulfate (Na2SO4) 1g
1 M Barium Chloride (BaCl2) 1g
1 M Nitric acid (HNO3) 4ml
Sodium Phosphate (Na3PO4) 2g
0.5 M Ammonium Molybdate 1g
[(NH4)2MoO4]
3 M Acetic Acid (HC2H3O2) 10ml
0.5 M Potassium Thiocyanate 1g
(KSCN)
0.1 M Iron(III) chloride (FeCl3) 1g

CHE105L Laboratory Manual Spring 2023 Page 42 of 44


0.5 M Sodium Chloride (NaCl) 1g
0.1 M Silver Nitrate (AgNO3) 1g
1 M Ammonia (NH3) 4ml
0.5 M Aluminum Chloride 1g
(AlCl3)
0.5 M Copper sulfate CuSO4 1g
Catechol violet reagent 1ml
Unknown solution
150 ml beaker
Test tube 10
Hot plate
Blue litmus paper
Red Litmus paper
Safety precautions

Procedure
add 100 ml of deionized water into a beaker and heat it to boiling. Replenishing the water from
time to time when it becomes necessary.

1. Test for the Carbonate Ion (CO32-)


Add 10 drops of 1 M Hydrochloric acid, HCl, to 10 drops of 1 M sodium carbonate, Na2CO3, in a
test tube. Bubbles of colorless and odorless gas (CO2) appear indicating the presence of the
carbonate ion.

2. Test for the Sulfate Ion (SO42-)


A. Add 10 drops of 1 M hydrochloric acid, HCl, to 10 drops of 1 M sodium sulfate, Na2SO4,
in a test tube.
B. Add 4 drops of 1 M barium chloride
C. White, powdery precipitate indicates the presence of sulfate ions.

3. Test for the Phosphate Ion (PO43-)


A. Add 10 drops of sodium sulfate, Na3PO4, to a test tube.
B. Add 1 M nitric acid, HNO3 until the solution is acidic (test with universal pH paper).
C. Add 5 drops of 0.5 M ammonium molybdate, (NH4)2MoO4.
D. Heat the test tube in hot water.
E. Powdery, light-yellow precipitate indicates the presence of the phosphate ion.

CHE105L Laboratory Manual Spring 2023 Page 43 of 44


4. Test for the Thiocyanate Ion (SCN-)
A. Add 10 drops of 0.5 M potassium thiocyanate, KSCN, into a test tube
B. Add 10 drops of 3 M acetic acid, HC2H3O2, and stir the solution with a stirring rod.
C. Transfer 1-2 drops of 0.1 M iron (III) Chloride, FeCl3, into the test tube. The formation of
deep red color indicates the presence of thiocyanate ions.

5. Test for Chloride Ion (Cl-)


A. Add 5 drops of 1 M nitric acid, HNO3, 10 drops of 0.5 M sodium chloride, NaCl, and 2-3
drops of 0.1 M silver nitrate, AgNO3, into a test tube.
B. The white precipitate indicates the presence of silver ions.
C. Add 10 drops of the solution just made in another test tube.
D. Add 10 drops of 1 M nitric acid to the test tube and boil the solution until the volume is
reduced to half.
E. Perform the chloride ion test as previously explained. This will eliminate any interference
if thiocyanate ions are present.

6. Test for the Aluminum Ion (Al3+)


A. Add 10 drops of 0.5 M aluminum chloride, AlCl3 to a test tube
B. Add 1 M ammonia, NH3 dropwise into the test tube until the solution is basic (remember
to stir the solution and test the solution with universal pH paper).
C. A white, gelatinous precipitate indicates aluminum hydroxide, Al(OH)3.
D. Add 3 M acetic acid, HC2H3O2, until the precipitate dissolves.
E. Add 2 drops of catechol violet reagent and stir.
F. A blue solution indicates the presence of aluminum ions.
Another method:
A. Add 10 drops of 0.5 M Aluminum chloride, AlCl3 to a test tube.
B. add ammonia dropwise until a white gelatinous precipitate indicates the presence of
aluminum ions.

7. Test for the Copper (II) Ion (Cu2+)


A. Add 10 drops of 0.5 M copper (II) sulfate, CuSO4 in a small test tube.
B. Add dropwise concentrated ammonia, NH3, into the test tube.
C. A deep blue color indicates the presence of copper (II) ions in the solution.

8. Analysis of an Unknown Solution


A. Analyze the unknown solution by repeating the following test with the unknown solution.
The solution contains more than one ion.

CHE105L Laboratory Manual Spring 2023 Page 44 of 44

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