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Experiments in General Chemistry 1

Senior High School Department


Science, Technology, Engineering and Mathematics Strand

Course Moderators:

Nian Beceral, MSc.


Lindley Susi, Msc.

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TABLE OF CONTENTS

Experiment 1: Determination of 6
an unknown compound

Experiment 2: On the nature of 7


physical and chemical change

Experiment 3: On separation of 8-9


mixture into its component
substances
Experiment 4: Density and 10-12
Exercise on pipetting

Experiment 5: Stoichiometry of 13
precipitation reaction

Experiment 6: Diff. types of 14-15


chemical reactions

Experiment 7: Hydrocarbons 16-21


and biomolecules

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INTRODUCTION

The primal goal of the laboratory course is to correlate experimental observations with the
principles and fundamental concepts in chemistry. Furthermore, the laboratory component of
the subject features experiments that will provide due chance for the students to make careful
observation (qualitative) and quantitative measurements under specified laboratory conditions
in lieu that they will depict and discover patterns of regularity and cross-examine these by
inductive and deductive methods of reasoning with the fundamental concepts given in the
lecture.

The program flow consists of three phases: the pre-lab, the actual experimentation and post-
lab.

Pre-lab phase: This phase involves the careful planning of the experiment to be performed
beforehand. Formulation and conversion of methods into schematic diagrams, firm
understanding of the objectives of the experiment, anticipation to the type of data that may be
gathered and background knowledge of the chemicals to be used are expected in this phase.

Actual experimentation (Lab-phase): This phase involves the execution of the specified method
for the experiment to be performed. Data gathering, establishment of experimental set-ups and
actual observations are expected to be seen in this phase.

Post lab (Analysis and Examination): A laboratory investigation doesn’t end with the
completion of the procedure and observation of the experimental results. After all the
substantial data has been compiled, these should be analyzed and evaluated if it successfully
answers and reflects the objectives and correlated with the fundamental principles of chemistry.

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Basic Laboratory safety and guidelines
Laboratory safety principle: It should be reiterated that the laboratory is considered as an
unsafe place to begin with. Moreover, it is a place where the theoretical underpinnings are
concretized into a directly observable material in order to supplement and facilitate the sound
grasp of scientific principles. As such, the use of this significant facility in the university is
structured under certain norms and regulations.

The following precautions and safety regulations will be strictly enforced throughout the course
of the experimentations for General chemistry 1 intended for Senior High School of the De La
Salle University Dasmarinas campus.

1. Never perform or begin touching any tool, reagent (chemical) you see in the laboratory
without the direction, supervision and authority of your instructors.

2. Observe proper laboratory outfit which includes the laboratory gown, protective eye goggles,
and closed toe shoes. Likewise, for those sporting considerably long hair, it is advised that they
bring and wear a hairnet during the course of experimentation.

3. Observer proper decorum. The laboratory is neither a park nor a playground where you could
loiter, hang with your friends and perform actions which are very unlikely of its context.

4. Observe if the chemicals you are using are properly labeled.

5. Keep open flames away from highly volatile and flammable solvents. Examples of these are
acetone, chloroform,

6. Use protective gloves if necessary (e.g. handling of highly hazardous chemicals).

7. Know by heart the location of the following: the eyewash, shower, first aid kit, fire
extinguishers and fire exits.

8. Clean up chemical spills on working bench immediately.

9. Dispose chemical wastes properly in their designated waste bottle.

10. Wearing of contact lens, metal accessories and make-up is highly discouraged in the course
of experimentation.

12. Practice the habit of good data or logbook management.

13. Golden rule: Safety in the lab is a communal responsibility. Let us work hand in hand
towards a safe but effectual conduct of experimentations.

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Definition of terms:

1. Hazard- defined as the potential of a substance to cause or induce harm. It is an inherent


property of a substance and thus, cannot be reduced.

2. Risk- could be defined as the probability that a substance used will cause harm. Compared to
hazards, risk can be minimized by ways such as using smaller or reducing the amounts used and
taking appropriate precautionary measures in handling (e.g. transferring acids or reactions
involving caustic substances should be performed in the fume hood).

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Experiment 1
Determination of an unknown compound

Reagents: Glassware/ equipment:

Corn starch Test tubes


Baking soda (NaHCO3) Test tube rack
Sodium chloride (NaCl) Droppers
Table sugar (Sucrose- C12H22O11) Weighing paper
Assigned unknown compound (A, B, C, D) Graduated cylinder (10 mL)
1 M NaOH microspatula
1M CH3COOH
Potassium iodide (KI) solution

Objectives:
1. Determine the physical properties and some chemical properties of the unknown compound
that will be assigned to the learners.

2. Compare the physical and chemical properties of the known compound with the respective
assigned unknown.

3. Identify the unknown compound by comparing its physicochemical properties with the set or
known compounds.

Procedure:
1. Note the appearance, color and characteristic odor of the compounds that will be given.

2. Place a micro-spatulaful of baking soda, sodium chloride, table sugar, corn starch and your
assigned unknown into 5 separate test tubes. Observe proper labeling.

3. In each test tube containing their designated and known compounds, add in separate set ups
the following: 5 mL each of 1 M NaOH solution, 1M CH3COOH, KI solution and H2O.

4. Record your observations.

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Experiment 2
On the nature of physical and chemical change: Effects of heat on some solids

Reagents: Glassware/equipment:

bismuth carbonate powder Test tubes


ammonium dichromate Test tube rack and holder
magnesium ribbon Wire gauze
Tripod
Bunsen burner
microspatula

Objectives:

1. Describe the effect of heat to solid samples.

2. Infer whether a physical or chemical change has occurred after heating the samples.

Procedure:

1. Take note of the appearance of the solids samples provided.

2. Place separately in clean dry test tubes a micro-spatulaful of the solids except the Mg ribbon.
Gently heat each solid. Then, subject the sample to more intense heat. Note all the changes
taking place.

3. For the Mg ribbon, place one to two pieces on top of the wire gauze. Heat it directly. Wear
eye goggles.

4. Allow the solids to cool. Note again their appearance after cooling.

Format for the data table:

Solid samples Appearance prior Behavior during Appearance after Inference


to heating heating heating and cooling (Physical or
chemical change?)

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Experiment 3

On separation of mixture into its component substances

Reagents: Glassware and equipment:

Iron fillings / nails Beaker


Sand Magnet
gravel Funnel
Soil Filter paper
dH2O (distilled water) erlenmeyer flasks

Objectives:

1. To resolve or separate the mixture into its component substances


2. To correlate the concept of particle size in deciding what type of separation techniques must
be employed given a mixture of substance to resolve

A. Simple filtration

Procedure:

1. Place a micro-spatulaful of soil or sand in a beaker.

2. Add 20 mL water to the sand or soil contained in the beaker. Mix well.

3. Prepare a fluted filter paper. (This will be demonstrated by the course facilitator).

4. Place a funnel on the erlenmeyer flasks.

5. Place the fluted filter paper in the funnel.

6. Poor gently the soil or sand mixture in the filtration set-up. Guide the mixture using the
stirring rod.

7. Don’t disturb the set-up and allow the filtration to proceed until all the liquid part is collected
or separated from the solid component of the mixture.

8. Observe if there are remaining sand or soil in the filtrate.

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B. Decantation

Procedure:

1. Place a handful of rice grains in a beaker.

2. Add approximately 20-30 mL of water. Mix well

3. Carefully separate the liquid portion of the rice mixture and collect it to a separate beaker.

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Experiment 4
Relationship of mass to volume (density) and exercise on pipetting

A. Relationship of mass to volume


Reagents: Glassware/equipment/others:

Soda Top loading balance


dH2O Graduated cylinder
methylene blue Marble
rose Bengal Gravel (1-3 pcs)
pipette

Objectives:

1. To measure the mass and volume of an unknown solid or liquid at room temperature.

2. To determine the relationships that exists between the mass and volume of a substance.

Procedure:

For liquid sample:

1. Weigh a clean dry 10 mL graduated cylinder and record its mass.

2. Measure into the weighed graduated cylinder 2 mL of assigned liquid sample.

3. Weigh the graduated cylinder containing the liquid sample. Record the mass.

4. Make a 2nd and third determination by repeating steps 1 to 3.

5. Return the samples to the properly labeled bottles.

For solid sample:

1. Weigh the assigned solid sample and record its mass.

2. Half fill the 10 mL graduated cylinder with water. Record the exact volume of water.

3. Drop slowly the assigned solid into the graduated cylinder. Record the new volume of the
system.

4. Make a 2nd and third determination by repeating steps 1 to 3.

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Format for the data table:

Liquid Determination
1 2 3
Vol. of unknown liquid
Mass of empty cylinder
Mass of empty cylinder and
liquid
Mass of liquid
Mass to volume ratio
Ave. mass to volume ratio

Solid:(indicate sample type) Determination


1 2 3
Vol. of water
Vol. of water and solid
Vol. of solid
Mass of solid
Mass to volume ratio
Ave. mass to volume ratio

B. Exercise on pipetting (Practical exam)

Glassware/ equipment:

Pipet
Test tube
Test tube rack

Objectives:

1. To familiarize themselves with the use of pipet.

2. To equip the learners with correct techniques on using the pipet.

3. To develop hand and eye coordination in relation to accuracy and precision in measurement.

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Procedure:

1. Draw the following volumes of the colored liquids (1, 5 and 10 mL) into separate test tubes.

2. Repeat step 1 5 times for each set test volume to be aspirated and transferred into
designated test tubes.

3. Prepare for the practical exam.

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Experiment 5
Stoichiometry of a precipitation reaction

Reagents Glassware/equipment

0.10 M AgNO3 solution Microwell plate


0.10 M K2CrO4 solution Beral pipette/ dropper
dH2O

Objectives:

1. To determine the combining ratio of Ag+ and CrO4 using the mole ratio method

2. To determine which ratio will produce the greatest amount of precipitate

Procedure:

1. Add 5 drops of distilled H2O to each of the 5 wells of the microwell plate.

2. Place the appropriate drops of the reagents in the well accordant to the table below:

Well 1 2 3 4 5

Drops of AgNO3 2 4 6 8 10

Drops of K2CrO4 10 8 6 4 2

3. Gently swirl the plate to facilitate the reaction.

4. Allow the precipitate to settle and identity the well with the greatest depth of precipitate.

5. Write the formula for the reaction and calculate the moles of silver nitrate and potassium
chromate.

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Experiment 6
Different types of chemical reactions

Reagents: Glassware/equipment:

Bi2(CO3)3 Wire gauze


Cu(NO3)2 Tripod
Al foil Bunsen burner
Mg ribbon Test tubes
1.0 M CuCl2 Droppers
0.1 M Zn(NO3)2 solution Microwell plate
0.1 M CuS04 solution
0.1 M HCl solution
0.1 M AgNO3
0.1 M BaCl2

Objectives:

1. To observe how substances undergo chemical change.

2. Write the balanced equations for all reactions.

3. Speculate the identity of the products of the chemical reactions.

Procedure:

Experiment involving solids

1. Place in a clean dry test tube a microspatulaful amount of Bi2(CO3)3 solid. Heat the test tube
gently first and then strongly. Observe the changes.

2. Place the Mg ribbon on top of the wire gauze. Heat it directly. Observe the changes. Use
forceps in placing the Mg ribbon on the wire gauze.

Experiment involving solids and liquids

1. Place Mg ribbon in test tube and add O.1 M HCl solution dropwise until the Mg ribbon is fully
immersed. Note the changes taking place.

2. Place Mg ribbon in another test tube and add 1.0 M CuCl2 solution dropwise until the Mg
ribbon is fully immersed. Note the changes taking place.

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3. Perform steps 1 and 2 but replace the Mg ribbon with Aluminum foil.

4. Mix 1 ml each of 0.1 M BaCl2 and 0.1 M AgNO3 in a micro test tube. Observe the formation of
precipitate.

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Experiment 7
Hydrocarbons and Biomolecules

A. Analysis of hydrocarbons

Objectives:

1. Differentiate various types of hydrocarbons (saturated, unsaturated, alipathic, aromatic)

2. Propose a scheme to discriminate hydrocarbon on the basis of its type

3. Depict an unknown hydrocarbon through simultaneous chemical tests

Reagents: Glassware and equipment:

1:1 H2SO4-HNO3 (Nitrating rgt.) Test tubes


5% Br2 in CH2Cl2 Droppers
2% aq. KMnO4 Water bath set at 500C
10% NaOH 500 mL beaker/thermometer
Reference stds. (toluene, hexane,
cyclohexane)
Unknown organic liquids

Procedure:

1. Nitration test (reaction 1) - Mix 5 drops sample with 8 drops nitrating rgt. and shake well. If
no visible change appears within 2 mins, heat in a water bath for 8 mins and dilute or add 20
drops water. Positive result: yellow oil/precipitate

2. Bromine test (reaction 2) – Mix 5 drops of sample with 3 drops of bromine rgt. If
decolorization occurs, add more bromine rgt. until substantial no change is observed. Note the
total drops of bromine rgt. added. Positive result: reagent decolorizes

Note: Bromine reagent has original orange color.

3. Basic oxidation (reaction 3) - Mix 5 drops sample with 3 drops 2% aq. KMnO4 and 2 drops 10%
NaOH. Warm the mixture for 2 mins in the water bath and note for change in color. Positive
result: brown ppt.

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B. Analysis of complex biological molecules (macromolecules)

Objectives:

1. To characterize the nature of oil or fat sample using simple grease spot test and
saponification test.

2. To characterize monosacharrides using specific tests

B.1 Grease spot test

Reagents: Glassware/equipment:

Vegetable oil Filter paper


Lecithin (0.1 g per mL dichloromethane) Pasteur pipets
Dicholoromethane

Procedure:

1. Obtain a piece of filter paper. Divide it into four and label the 4 areas with “veg. oil”,
“lecithin”, H2O and DCM (dichloromethane) using a pencil.

2. Using Pasteur pipets, apply to each labeled area of the filter paper a drop of the
corresponding substance.

3. Warm the filter paper by placing it on a hot place that is set or adjusted to its lowest
temperature setting for 2-3 mins.

4. Record your observations.

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B. 2 Saponification test

Reagents: Glassware/equipment:

Vegetable oil Test tubes


Melted fat (butter) Pasteur pipets
3M NaOH Litmus paper
dH2O
conc. H2SO4

Procedure:

1. Label three (3) medium sized test tubes with “oil”, “fat” and “H2O”.

2. Place 8 drops of each sample into their corresponding test tubes

3. Add 10 drops of 3M NaOH solution to each test tube

4. Place the test tubes containing the reaction mixture in boiling water bath for 15-20 mins.

5. Remove the test tubes from the water bath, place them in a test rack and allow to coll at RT.

6. Add 5 mL of dist. Water to each test tube. Place a cork stopper to the tubes and mix to
facilitate chemical reaction.

7. Record your observations.

8. Acidify with a few drops of conc. H2SO4 solution (Check with blue litmus paper).

9. Mix with a stirring rod and note the materials which collect on top of the solution.

10. Dip a piece of red and blue litmus paper separately and record the pH (is it acidic or basic?)

11. Record your observations.

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B. 3 Specific tests for carbohydrates

Reagents: Glassware/equipment:

Unknown sugar Test tubes


20% standard slns. of : xylose, fructose, Pasteur pipette
glucose, galactose, lactose, maltose and Test tube rack
sucrose Water bath/hot plate
conc. HNO3
Benedict’s rgt.
Barfoed’s rgt.
Bial’s orcinol rgt.
Seliwanoff’s rgt.
20% NaOH
5% methyl ammnonium chloride
3M HCl
3M NaOH

B.3.1 Mucic acid test

Procedure

1. Label 8 medium sized test tubes with the standard sugar solutions and your assigned
unknown.

2. Place 10 drops of sugar solution in their respective tubes.

3. Add 10 drops of conc. HNO3 to each tube.

4. Plug the tubes with cotton and then heat them in a boiling water bath for 1 hr.

5. Let stand until the next laboratory period. Place tubes in your locker or store them in
refrigerator.

6. Note which standard sugars and unknown produce crystals.

B.3.2 Benedict’test

1. Label 8 medium sized test tubes with the standard sugar solutions and your assigned
unknown.

2. Place 10 drops of Benedict’s rgt. in each labeled tubes.

3. Add 5 drops of standard sugar solutions and unknown in their respective tubes.

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4. Heat the tubes in water bath until a muddy green suspension is observed which settles as
brick red precipitate.

5. Immediately remove the test tubes from the bath and cool them on rack

6. Record results. A negative result is obtained if no brick red precipitate is observed after >5
minutes of heating.

B.3.3 Barfoed’s test

1. Label 8 medium sized test tubes with the standard sugar solutions and your assigned
unknown.

2. Place 10 drops of Barfoed’s rgt. in each labeled tubes.

3. Add 5 drops of standard sugar solutions and unknown in their respective tubes.

4. Heat the tubes in water bath until a brick red precipitate is observed. Note the time when the
precipitate appears.

5. Immediately remove the test tubes from the bath and cool them on rack.

6. Record results. A negative result is obtained if no brick red precipitate is observed after >5
minutes of heating.

B.3.4 Bial’s Orcinol test

1. Label 8 medium sized test tubes with the standard sugar solutions and your assigned
unknown.

2. Add 5 drops of standard sugar solutions and unknown in their respective tubes.

3. Place 10 drops of Bial’s orcinol in each labeled tubes.

4. Heat the tubes in water bath until a blue-green solution is observed. Note the time when the
blue green solution precipitate appears.

5. Record the colors formed during the 5 minutes of heating.

6. Remove the test tubes from the bath.

7. Record results

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B.3.5 Seliwanoff’s test

1. Label 8 medium sized test tubes with the standard sugar solutions and your assigned
unknown.

2. Place 10 drops of seliwanoff’s rgt. in each labeled tubes.

3. Add 5 drops of standard sugar solutions and unknown in their respective tubes.

4. Immerse the tubes in boiling water bath.

5. Heat until cherry red solution is observed and then remove the tubes from the water bath

6. Note the time when the cherry red solution appears.

7. Record the results

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