Engineering Chemistry

2020 Edition
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 Republic of the Philippines
JOSE RIZAL
MEMORIAL STATE UNIVERSITY
The Premier University
in Zamboanga del Norte
Main Campus, Dapitan City

Compiled and Adapted by

Romie D. Laranjo, D. Eng.

Safety Rules in the Laboratory

The chemistry laboratory is a place to experiment and learn. You must assume
responsibility for your own personal safety and that of people working near you. Accidents are
usually caused by carelessness, but you can help prevent them by closely following the
instructions printed in this manual and those given to you by your instructor. The following are
some safety rules to help guide you in protecting yourself and others from injury in a laboratory.
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1. The chemistry laboratory is a place for serious work. Do not perform activities without your
instructor’s permission. Never work alone in the laboratory. Work only when your teacher is
present.
2. Study your lab activity before you come to the lab. If you are in doubt about any procedures,
ask your instructor for help.
3. Safety goggles and a laboratory apron must be worn whenever you work in the lab. Gloves
should be worn whenever you use chemicals that cause irritations or can be absorbed through
the skin.
4. Contact lenses should not be worn in the lab, even if goggles are worn. Lenses can absorb
vapors and are difficult to remove in an emergency.
5. Long hair should be tied back to reduce the possibility of it catching fire.
6. Avoid wearing dangling jewelry or loose, draping clothing. The loose clothing may catch fire
and either the clothing or jewelry could catch on chemical apparatus.
7. Wear shoes that cover the feet at all times. Bare feet or sandals are not permitted in the lab.
8. Know the location of the fire extinguisher, safety shower, eyewash, fire blanket, and first-aid
kit. Know how to use the safety equipment provided for you.
9. Report any accident, injury, incorrect procedure, or damaged equipment immediately to your
instructor.
10. Handle chemicals carefully. Check the labels of all bottles before removing the contents. Read
the labels three times: before you pick up the container, when the container is in your hand, and
when you put the bottle back.
11. Do not return unused chemicals to reagent bottles.
12. Do not take reagent bottles to your work area unless specifically instructed to do so. Use test
tubes, paper, or beakers to obtain your chemicals. Take only small amounts. It is easier to get
more than to dispose of excess.
13. Do not insert droppers into reagent bottles. Pour a small amount of the chemical into a beaker.
14. Never taste any chemical substance. Never draw any chemicals into a pipette with your mouth.
Eating, drinking, chewing gum, and smoking are prohibited in the laboratory.
15. If chemicals come into contact with your eyes or skin, flush the area immediately with large
quantities of water. Immediately inform your teacher of the nature of the spill.
16. Keep combustible materials away from open flames. (Alcohol and acetone are combustible.)
17. Handle toxic and combustible gases only under the direction of your teacher. Use the fume
hood when such materials are present.
18. When heating a substance in a test tube, be careful not to point the mouth of the tube at another
person or yourself. Never look down the mouth of a test tube.
19. Use caution and the proper equipment when handling hot apparatus or glassware. Hot glass
looks the same as cool glass.
20. Dispose of broken glass, unused chemicals, and products of reactions only as directed by your
instructor.
21. Know the correct procedure for preparing acid solutions. Always add the acid slowly to the
water.
22. Keep the balance area clean. Never weigh chemicals directly on the pan of the balance.
23. Do not heat graduated cylinders, burettes, or pipettes with a laboratory burner.
24. After completing an activity, clean and put away your equipment. Clean your work area. Make
sure the gas and water are turned off. Wash your hands with soap and water before you leave
the lab.

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25. Women that are, or may become pregnant should carefully determine, upon consultation with
your personal physician, if it is advisable for them to participate in the laboratory program. If
you are pregnant or are planning to become pregnant please inform your instructor.

Safety Contract
I HAVE READ ALL OF THE ABOVE, AND I AGREE TO CONFORM TO ITS
CONTENTS. (This is for your records. You don’t need to turn this in.)

Name: _______________________________________

Course:_______________

Student ID:____________

Section:_______________

Signature: _____________________________________ Room: _________

Date: _________________________

Lab Professor: ___________________

Writing a Laboratory Report

When scientists perform experiments, they make observations, collect and analyze data, and
formulate generalizations about the data. When you work in the laboratory, you should record all
your data in a laboratory report. An analysis of data is easier if all data are recorded in an
organized, logical manner. Tables and graphs are often used for this purpose.

Title: The title should clearly describe the topic of the report.
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Hypothesis: Write a statement to express your expectations of the results and as an answer to the
problem statement.

Materials: List all laboratory equipment and other materials needed to perform the experiment
.
Procedure: Describe each step of the procedure so that someone else could perform the experiment
following your directions.

Results: Include in your report all data, tables, graphs, and sketches used to arrive at your
conclusions.

Conclusions: Record your conclusions in a paragraph at the end of your report. Your conclusions
should be an analysis of your collected data.

Read the following description of an experiment. Then answer the questions.

All plants need water, minerals, carbon dioxide, sunlight, and living space. If these needs are not
met, plants cannot grow properly. A scientist wanted to test the effectiveness of different
fertilizers in supplying needed minerals to plants. To test this idea, the scientist set up an
experiment. Three containers were filled with equal amounts of potting soil and one healthy bean
plant was planted in each of three containers. Container A was treated with Fertilizer A,
Container B was treated with Fertilizer B, and Container C did not receive any fertilizer. All three
containers were placed in a well-lit room. Each container received the same amount of water
every day for 2 weeks. The scientist measured the heights of the growing plants every day. Then
the average height of the plants in each container each day was calculated and recorded in Data
Table 1. The scientist then plotted the data on a graph.

1. What was the purpose of this experiment?

______________________________________________________________________________

______________________________________________________________________________

______________________________________________________________________________

2. What materials were needed for this experiment?

______________________________________________________________________________

______________________________________________________________________________

______________________________________________________________________________

______________________________________________________________________________

3. Write a step-by-step procedure for this experiment.

______________________________________________________________________________

______________________________________________________________________________
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______________________________________________________________________________

______________________________________________________________________________

______________________________________________________________________________

______________________________________________________________________________

______________________________________________________________________________

______________________________________________________________________________

______________________________________________________________________________

______________________________________________________________________________

____________________________________________________________________________

4. Data Table 1 shows the data collected in this experiment. Based on these data, state a
conclusion for this experiment.

______________________________________________________________________________

______________________________________________________________________________

______________________________________________________________________________

______________________________________________________________________________

5. Plot the data in Data Table 1 on a graph. Show average height on the vertical axis and the
days on the horizontal axis. Use a different colored pencil for the graph of each container.

Table of Contents
Safety Rules in the Laboratory ..........................................................................3

Writing a Laboratory Report........................................…………………………...5

Laboratory Activities

1 Introduction to Chemistry

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 1.1 Familiarization of Laboratory Apparatus .........................................9

1.2 Laboratory Techniques and Safety…………………………………..21

1.3 The Bunsen Burner……………………………………………………...26

2 Matter and Energy

2.1 Mixing Alcohol and Water- A Thumb-Sucking Exercise………….31

2.2 Methods of Evaporation and Filtration Used to

Separate Mixtures.............................................................................34

2.3 Electrochemistry……………………………...………………………….39

2.4 Corrosion of Metals……………………………………………………...49

2.5 Radioisotope Dating…………………………………………………….55

3 Chemistry of Engineering Materials

3.1 Metallic and Ionic Crystal Lattices……………………………………61

3.2 Specimen Preparation and Microscopic Examination…………….74

3.3 Tensile Test……………………….………………………………………80

4 Chemistry of the Environment

4.1 Acid Rain…………………………………………..………………………89

4.2 Global Warming Issues and Effects………………………………….98

4.3 Determination of Dissolved Oxygen………………………………..104

4.4 Growth of Algae as a Function of Nitrogen Concentration…….109

ORATORY MANUAL

LAB MANUAL
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Activity 1.1
Familiarization of Laboratory Apparatus
Laboratory glassware and equipment are expensive. Familiarization of these equipment and
glassware is necessary. You must also adopt correct procedures for using glassware and other
pieces of equipment.

Objectives
• Draw the laboratory apparatus.
• Familiarize its uses

Materials
Drawing Instruments (Optional), Pencil, Ruler, short bond papers

Procedure
1. Draw the laboratory apparatus and equipment which are present in the laboratory.
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2. Identify the functions or uses of these apparatus and equipment.

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Name______________________________Course & Yr_________________Date____________

Data and Observations

Name______________________________Course & Yr_________________Date____________

Data and Observations

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Name______________________________Course & Yr_________________Date____________

Data and Observations

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Name______________________________Course & Yr_________________Date____________

Data and Observations

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Name______________________________Course & Yr_________________Date____________

Data and Observations

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Name______________________________Course & Yr_________________Date____________

Data and Observations

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Name______________________________Course & Yr_________________Date____________

Data and Observations

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Activity 1.2
Laboratory Techniques and Safety
Chemistry has been developed largely through experimentation. Chemistry courses use
laboratory experiences to demonstrate, clarify, and develop principles of chemistry. Behavior in
the laboratory is more structured than in the classroom. Certain rules of conduct pertaining to
safety and keeping a clean work environment must be followed at all times. You must also adopt
correct procedures for using glassware and other pieces of equipment. General safety rules are
summarized at the beginning of this lab manual. However, there often will be more specific safety
rules or special procedures to follow when performing an experiment. Your instructor will
provide these added instructions before you perform any lab activity. If you are unsure of any
procedure, always ask your instructor before proceeding. In this activity, you will practice some
laboratory techniques and apply laboratory safety rules. You will determine the mass of different
solid materials, measure the volume of a liquid, and separate mixtures of chemicals. You will also
review specific safety rules.

Pre-Lab
1. What is the safety rule concerning working alone in the laboratory?
2. What is the safety rule concerning the handling of excess chemicals?
3. What should you do if you spill a chemical?
4. Read the entire laboratory activity. Hypothesize what safety precautions will be needed to handle
the different chemicals and lab equipment in this experiment. Record your hypothesis.

Objectives
• Measure the mass of solid substances.
• Measure a volume of water.
• Separate components of a mixture through filtration.

Materials
table salt, sand, distilled water, 100-mL graduated cylinder, 250-mL beakers (2), 50-mL beakers
(2), balance, ring stand, ring, funnel, scoops (2), stirring rod, filter paper, weighing paper

Procedure
1. Using a scoop, transfer a small amount of table salt to a 50-mL beaker.

2. Measure the mass of a piece of weighing paper to 0.1 g using a laboratory balance. Record this
mass in Data Table 1.

3. Add about 5.0 g of table salt from the 50-mL beaker to the weighing paper. Record the mass of
the weighing paper and table salt to 0.1 g in Data Table 1.

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4. Transfer the table salt to the 250-mL beaker and place all excess table salt into an appropriate
waste container, as indicated by your teacher.
5. Using another scoop, transfer a small amount of sand to the second 50-mL beaker. Using the
techniques described in steps 2 and 3, measure out about 5.0 g of sand. Then transfer the sand to
the 250-mL beaker containing the table salt.

6. Using a 100-mL graduated cylinder, measure out 80 mL of distilled water. Measure the volume
of the water to 0.1 mL by reading at the bottom of the meniscus, as illustrated in Figure A.
Record the volume of water measured in Data Table 1.

7. Pour the water into the 250-mL beaker containing the table salt and sand. Using the stirring rod,
gently stir the mixture for 1 minute. Record your observations in Data Table 2.

8. Place a clean 250-mL beaker on the base of the ring stand. Attach the ring to the ring stand and
set the funnel in the ring so that the stem of the funnel is in the beaker. Adjust the height of the
ring so that the bottom of the funnel stem is approximately halfway up the beaker. Fold a piece of
filter paper as illustrated in Figure B. Place the folded filter cone in the funnel.

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9. To avoid splashing and to maintain control, you will pour the liquid down a stirring rod. Place the
stirring rod across the top of the 250-mL beaker that contains the mixture, as shown in Figure
B. The stirring rod should rest in the spout and extend several inches beyond the spout. Grasp the
beaker with your hand and place your index finger over the stirring rod to keep it in place. Slowly
pour the contents of the beaker into the filter cone, allowing the liquid to pass through the filter
paper and collect in the beaker.

10. While holding the beaker at an angle, use the water bottle to rinse the beaker and wash any
remaining solid from the beaker into the filter cone. Record your observations in Data Table 2.

11. Allow the filter cone to drain. Then remove the filter cone and carefully unfold the filter
paper. Place the filter paper on a watch glass and record your observations in Data Table 2.

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Name______________________________Course & Yr_________________Date____________

Data and Observations

• To find the “Mass of table salt,” subtract the “Mass of weighing paper” from the “Mass of
table salt + weighing paper.”

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• To find the “Mass of sand,” subtract the “Mass of weighing paper” from the “Mass of sand
+ weighing paper.”

Analyze and Conclude

1. Observing and Inferring Why were the excess reagents not put back into the original reagent
bottle?
______________________________________________________________________________
______________________________________________________________________________
______________________________________________________________________________

2. Comparing and Contrasting What differences were observed between the mixture of salt and
sand in the 250-mL beaker and the same materials after the water was added?
______________________________________________________________________________

______________________________________________________________________________

______________________________________________________________________________

3. Drawing a Conclusion Why were the samples of table salt and sand placed into 50-mL beakers
prior to weighing?
______________________________________________________________________________

______________________________________________________________________________

______________________________________________________________________________

4. Thinking Critically

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a. If one of the pieces of glassware is dropped and breaks, why is it necessary to clean up the
broken glass immediately?
______________________________________________________________________________

______________________________________________________________________________

______________________________________________________________________________

b. If one of the pieces of broken glass is dropped and breaks, why is it necessary to tell the
instructor immediately?
______________________________________________________________________________

______________________________________________________________________________

______________________________________________________________________________

5. Thinking Critically Why is it necessary to wear safety goggles and a lab apron while performing
experiments in the lab?
______________________________________________________________________________

______________________________________________________________________________

______________________________________________________________________________

6. Error Analysis What are some possible sources of error in this activity?
______________________________________________________________________________

______________________________________________________________________________
______________________________________________________________________________

Activity 1.3
The Bunsen Burner
During chemical or physical changes, energy is often transferred in the form of heat. This
transfer can be measured by a change in temperature. In this activity, you will test the effective
use of a Bunsen burner. You will vary the height of the position of a beaker of water above the
burner and observe how long it takes to boil the water. All other factors will be kept constant. The
intensity of the flame and the height of the platform used to hold the beaker of water will not
change. Because the intensity of the flame does not change, the amount of heat provided by the
flame will be a constant. In addition, a given amount of water will always require the same
amount of energy to boil.

Pre-Lab
1. What are the constants in this experiment?
2. What are the variables in this experiment?

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3. Which measurement in this experiment is the dependent variable?
4. Read over the entire laboratory activity. Hypothesize about what the most effective position
above the flame will be. Record your hypothesis

Objectives
• Heat a beaker of water using a Bunsen burner.
• Measure distances using a ruler. • Measure temperature using a
thermometer.

Materials
100-mL graduated cylinder, 250-mL beakers (4), Bunsen burner, striker or matches, thermometer, ring stand,
ring, wire gauze, ruler, stopwatch or clock, beaker tongs or hot mitts, hot pad, distilled water

Procedure
1. Label four 250-mL beakers 1, 2, 3, and 4. Using a graduated cylinder, measure 100 mL of
distilled water into Beaker 1. Measure and record the temperature of the water in Data Table 1.
Repeat this process three more times for the remaining three beakers.

2. Set up a ring stand and attach the ring to the stand. Place the wire gauze on the ring to provide a
platform on which to place the beaker of water.

3. Use burner connector safety tubing to connect the Bunsen burner to the gas inlet. Make sure the
hose does not have any cracks or holes.

4. Light the burner by first turning on the gas flow and using the striker to ignite the gas. If you use
a match, light the match first before turning on the gas. Hold the match close to the bottom side
of the burner nozzle to light the gas.

5. When the flame is lit, adjust the gas flow and oxygen flow so that the flame is blue with an
inner light-blue cone. A yellow flame is too cool and needs more oxygen. Your teacher may
have additional directions on the operation of the Bunsen burner.

6. After you adjust the flame, move the burner to the ring stand and observe the height of the wire
gauze above the flame. Adjust the height so the wire gauze is approximately halfway up the
inner blue cone. Refer to Figure A, Test 1 height. Estimate the distance from the top of the
burner to the wire gauze with a ruler and record this distance as Test 1 in Data Table 2. This
will be your starting distance. Turn off the flame.

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7. Place Beaker 1 on the wire gauze. Ignite the flame and measure the time (in s) it takes for the
water to boil. Record this time in Data Table 2.

8. Turn off the flame and using beaker tongs and hot mitts, carefully remove the hot beaker of
water from the wire gauze and place it on a hot pad on your lab bench.

9. Turn on the flame and adjust the height so the wire gauze is now at the top of the inner blue
cone. Refer to Figure A, Test 2 height. Estimate the distance from the top of the burner to the
wire gauze with the ruler and record this distance in Data Table 2. Turn off the flame.

10. Repeat steps 6–8 using Beaker 2.

11. Turn on the flame and adjust the height so the wire gauze is now positioned the same distance
from the top of the inner blue cone as the top was positioned from the starting distance, halfway
up the inner blue cone. Refer to Figure A, Test 3 height. For example, if the starting distance
was 3 cm and the top of the inner blue cone is 6 cm, then the new position will be 9 cm above
the burner top. Estimate the distance from the top of the burner to the wire gauze with the ruler
and record this distance in Data Table 2. Turn off the flame.

12. Repeat steps 6–8 using Beaker 3.

13. Turn on the flame and adjust the height so the wire gauze is moved to a new position that is the
same distance increment as before. Refer to Figure A, Test 4 height. For example, if the starting
position was 3 cm, the height for test number 2 was 6 cm and the height for test number 3 was 9
cm, then the height for test 4 will be 12 cm. Estimate the distance from the top of the burner to
the wire gauze with the ruler and record this distance in Data Table 2. This will be your starting
distance. Turn off the flame.
14. Repeat steps 6–8 using Beaker 4.

15. When the beakers are cool, empty the water in the sink and dry the glassware.

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Name________________________________ Course & Yr_________________Date _________

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Data and Observations

Analyze and Conclude

1. Observing and Inferring Why did you turn off the burner between experiment setups?
______________________________________________________________________________

______________________________________________________________________________

______________________________________________________________________________

2. Thinking Critically Why is the height of the wire gauze the independent variable?
______________________________________________________________________________

______________________________________________________________________________

______________________________________________________________________________

3. Thinking Critically Why is the time to get the water to boil the dependent variable?
______________________________________________________________________________

______________________________________________________________________________

______________________________________________________________________________

4. Comparing and Contrasting What observed differences did you note among the results of the
four tests?___________________________________________________________________

______________________________________________________________________________

______________________________________________________________________________

5. Drawing a Conclusion Why did it take less time for the water to boil when the wire gauze was
placed at the tip of the inner blue cone?___________________________________________
______________________________________________________________________________

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______________________________________________________________________________

______________________________________________________________________________

6. Thinking Critically Why was it necessary to use beaker tongs or hot mitts to remove the beaker of
water after the test but not before the test?____________________________________

______________________________________________________________________________

______________________________________________________________________________

7. Error Analysis What are some sources of error in this activity?

______________________________________________________________________________

______________________________________________________________________________

______________________________________________________________________________

Activity 2.1
Mixing Alcohol and Water - A Thumb Sucking
Exercise

Despite its frivolous-sounding title, this exercise will provide you with an opportunity to
speculate about what must be happening on the molecular level when these two simple substances
are mixed.

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Pre-Lab
1. Very little introduction will be given to this exercise.
2. You are to perform two rather simple operations
3. The hazard level is low in this exercise. However, there is a risk of splashing alcohol in the eyes,
and, as is usual, goggles are required.
4. Also, the use of your thumb to close off the top of a test tube, as called for here, is not allowed in
any future work. 3. Record your hypothesis.

Objectives
• Observe the phenomena involve.
• Speculate about an explanation.

Materials
Ethyl alcohol, deionized water, 2 small test tubes, plastic wash bottles

Procedure
1. Remove two small (10-cm) test tubes from your locker along with a small beaker to hold them
upright. Locate two plastic wash bottles: one, containing deionized water, will be unlabeled;
and the other, containing ethyl alcohol, will be labeled with that name, along with the warning
"Flammable!” There won’t be a flame in today's activity, but you should be aware that alcohol, like
many non-aqueous solvents, will burn.

2. Fill one test tube about half full with water from the unlabeled wash bottle.

3. Now fill it to the top with alcohol from the labeled wash bottle (A). Do this carefully. Try not
to mix the two liquids unnecessarily. (They will dissolve in each other, given the chance, but it
is possible to layer the alcohol above the water.)

4. When the tube is "brimful", slide your thumb over the top of the tube carefully so that no
bubbles of air are trapped. (Again, we will not use our thumbs this way in any further chemical
work. It is not good for the thumb or the chemical study. Here, there is no hazard, and direct
contact is necessary to the study.)

5. Be sure your thumb is squarely and firmly positioned on top. Now invert the tube once or twice
and return to the original position, keeping your thumb on top. Observe any changes in
appearance inside the tube and any sensations in your thumb. (Some people find that they can
suspend the tube from their thumb without supporting it! But keep your free hand underneath,
just in case!).

6. Discard the solution into the proper waste container.

7. Try the experiment again, but this time, add the alcohol first, and then fill with water (B).

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Name________________________________ Course & Yr_________________Date _________

Data and Observations

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1. In your lab write-up, describe what you saw and experienced in the two different exercises.
Please use complete sentences.
______________________________________________________________________________

______________________________________________________________________________

______________________________________________________________________________

2. What is your explanation for what happened in A, and for the difference in behavior between A
and B? You are not expected to know the whole story. Any hypothesis, however "wild" is
invited.
______________________________________________________________________________

______________________________________________________________________________

______________________________________________________________________________

3. Do you get the same effect? If not, why not? Refer to Procedure # 7.
______________________________________________________________________________

______________________________________________________________________________

______________________________________________________________________________

Activity 2.2
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Methods of Evaporation and Filtration Used to
Separate Mixtures
Is bottled water safer than tap water? Studies have revealed that phthalates, chemicals
known to affect hormones, can come from the plastic material of the bottled water. In addition, at
least 25% of bottled water contains tap water inside. These studies suggest that consumers should
become more aware of what they are drinking. Besides chemical contaminant concerns, the
shipment and production of plastic bottled water have environmental consequences. Simply
moving large amounts of bottled water from one location to another creates global warming and
other types of air pollution. The production of plastic bottled water requires millions of barrels of
crude oil each year that affects the environment as well. The environment is also impacted by the
disposal of plastic bottles. Most of the bottles are either sent to landfills or left as unclaimed trash
instead of being recycled. If bottled water is environmentally unfriendly, then drinking tap water
may be a better alternative. However, consumers may be reluctant to trust the water coming out of
their faucets unless there is scientific evidence that tap water is safe to drink. The separation of
unwanted particulates from a mixture plays a major role in filtration systems.

Materials
Saturated NaCl solution, Filter paper, 1 M Na2CO3 Vanillin, 1 M CaCl2, Büchner funnel, 6 M HCl

Safety Precaution
Be cautious with the acids and bases used in this experiment. Dispose all chemicals as instructed.

Procedures Part 1. Separation of Mixtures by Evaporation

1. Weigh and record the mass of a clean and dry evaporating dish using an analytical balance.

2. Pour onto the evaporating dish approximately 5 mL of a saturated NaCl solution.

3. Reweigh and record the evaporating dish with the NaCl solution on it.

4. Set up a heating apparatus similar to the illustration below (Figure A).

5. Choose an appropriate size beaker that will hold the evaporating dish directly on top.

6. Add several (about 3 – 5) boiling chips into the beaker to avoid bumping.

7. Fill the beaker half full with tap water.

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 Figure A: A heating apparatus.

8. Place the evaporating dish with the saturated NaCl solution directly on top of beaker.

9. Turn on the flames from the Bunsen burner and heat until there is no apparent liquid on the
evaporating dish. Turn off the flames.

10. Carefully remove the evaporating dish and the beaker from the heating apparatus.

11. Place the evaporating dish back on the wire gauze.

12. Apply a very gentle flame (approximately 2 minutes) underneath the wire gauze to completely
evaporate any residues of liquid that may remain on the evaporating dish.

13. Allow the evaporating dish to cool and weigh the dish. Repeat the heating, cooling, and
reweighing process until constant mass is reached.

14. Calculate the mass percent of NaCl in the saturated NaCl solution.

Part 2. Separation of Mixtures by Gravity Filtration

1. Add 10 mL of 1.0 M sodium carbonate into a 150 mL beaker.

2. Into the same beaker, add 10 mL of 1.0 M calcium chloride and stir the mixture with a glass
stirring rod.

3. Write a balanced chemical equation for this mixture.

4. Set up a gravity filtration setup similar to the illustration below (Figure B). Make sure to wet
the filter paper with deionized water to ensure that it sticks well to the funnel.

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5. Using the glass stirring rod as a guide, pour the sodium carbonate and calcium chloride mixture
directly into the center of the funnel. Make sure to point the glass stirring rod directly into the
middle of the funnel without touching the filter paper.

6. Any solids will be retained by the filter paper while liquids will flow through due to gravity.
The liquids will be collected underneath into a beaker.

7. When the filter paper appears dry, remove it from the funnel.

8. Open up the filter paper completely and transfer some solids to a watch glass.

9. Add 3 drops of 6 M HCl to the solids on the watch glass.

10. Write a balanced chemical reaction for the observed reaction.

Figure B: A gravity filtration setup.

Part 3. Separation of Mixtures by Vacuum Filtration

1. Place a 250 mL Erlenmeyer flask on an analytical balance and press “Tare.”

2. Weigh and record the mass of 0.8 g to 1 g of vanillin into the 250 mL Erlenmeyer flask on the
analytical balance.

3. Remove the Erlenmeyer flask from the balance and add approximately 50 mL of deionized
water and vigorously stir to dissolve as much vanillin as possible.

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4. Using the flames from a Bunsen burner, gently heat the solution in the flask until all the solids
dissolve. Do not allow the solution to boil. Turn off the flames and allow the solution to cool
for several minutes.

5. Put the Erlenmeyer flask into an ice bath. As the solution cools down in the ice bath,
crystallization should occur. If there are no signs of crystals forming when the flask feels cold,
insert a glass stirring rod into the flask and gently scrap at the bottom.

6. Once crystallization is complete, assemble a vacuum filtration setup similar to the illustration
below (Figure C).

Figure C: A vacuum filtration setup.

7. Obtain an appropriate size filter paper that fits well at the bottom of the Büchner funnel. Weigh
the filter paper using an analytical balance. Place the filter paper at the bottom of the Büchner
funnel and wet it with deionized water.

8. Turn on the water line where the rubber hose is attached, as this will create a suction effect.

9. Rinse the crystals in the Erlenmeyer flask with approximately 5 mL of ice-cold water and
carefully pour the crystals into the center of the Büchner funnel.

10. If there are crystals still remaining in the Erlenmeyer flask, rinse them with an additional 5 mL
of ice-cold water and pour them into the Büchner funnel.

11. When the crystals appear to be dry, turn off the water line to stop the suction and carefully
remove the filter paper from the Büchner funnel.

12. Place the filter paper containing the crystals on watch glass and allow it to dry in the lab drawer.

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13. In the next lab class, weigh and record the mass of the filter paper containing the vanillin.

14. Calculate the percent recovery of vanillin.

Name________________________________ Course & Yr_________________Date _________

Data and Observations

1. An evaporating dish weighs 44.3170 grams. After 8.5 mL of salt water was added to the dish,
the combination of the dish and salt water weighed 52.987 grams. The dish was then heated
until a constant mass of 44.5990 grams was obtained. What was the mass percent of salt
dissolved in the salt water?
______________________________________________________________________________

______________________________________________________________________________

______________________________________________________________________________

2. What is meant by “constant mass”? How is this important?

______________________________________________________________________________

______________________________________________________________________________

______________________________________________________________________________

3. Distillation is performed to purify water from tap water. In this experiment evaporation, gravity
filtration, and vacuum filtration were methods used to separate homogeneous mixtures. Would
it be safe to drink purified sewage water if these methods were used to separate water from
unwanted substances?
______________________________________________________________________________

______________________________________________________________________________

______________________________________________________________________________

34
Activity 2.3
Electrochemistry
Oxidation is the loss of electrons and reduction is the gain of electrons. These processes occur
simultaneously in reactions referred to as redox reactions. A voltaic cell uses a spontaneous redox
reaction to generate electrical energy. An electrolytic cell uses electrical energy to drive a non-
spontaneous reaction. Both of these cells use two electrodes that are placed in an electrolyte
solution. The anode is the electrode where the oxidation half reaction takes place and the cathode
is the electrode where the reduction half reaction takes place. Each half-reaction takes place in its
own half-cell and the two half reactions are physically separated. An external circuit connects the
half-cells and a salt bridge used to maintain electrical neutrality completes the circuit.
The potential difference between the anode and the cathode in a cell is known as the
electromotive force or EMF of the cell. It is also referred to as the cell potential and is denoted the
symbol Ecell.
Consider for instance a cell constructed using zinc and copper electrodes. The standard reduction
potentials for these two electrodes are given below.

A spontaneous redox reaction will result when the electrode with the higher reduction potential
undergoes reduction reaction. Since the copper electrode has the higher reduction potential, it is
the electrode that becomes reduced and is therefore at the cathode and consequently the zinc
electrode is at the anode.

The two half reactions and the overall cell reaction in this instance may be written as follows:

The cell potential, E°cell is given by:

E°cell = E°RED (cathode) − E°RED (anode) Equation 1

35
According to Equation 1, the cell potential for the electrochemical cell that results in a spontaneous
redox reaction using zinc and copper electrodes is given by:

E°cell = 0.34 – (-0.76) = 1.10 V

A schematic representation of this cell is given below in Figure 1.

Figure 1 Electrochemical Cell

The line diagram for the electrochemical cell shown in Figure 1 is written as follows:

Zn|Zn2+||Cu2+|Cu

Under standard conditions, the molarities of the electrolyte solutions are assumed to be 1M and the
standard temperature is assumed to be room temperature, 25°C or 298 K. The cell potential
calculated under these conditions is the standard cell potential E° cell given by Equation 1.

However, if the concentrations of the electrolyte solutions are different from 1M, the non- standard
cell potential, E, is calculated using the Nernst Equation, given in Equation 2.

0.0592
E E= −o logQ Equation 2
n
In Equation 2, “n” is the number of electrons transferred from the anode to the cathode in the redox
process and Q is the reaction quotient. In the example shown above for the zinc/copper
electrochemical cell, n = 2 and Q is obtained from the overall cell equation.

Zn2
Q = Cu2++

36
The free energy change for a redox reaction is related to the cell potential according to Equation 3
below.

ΔG = − nFE Equation 3

In Equation 3, ΔG is the free energy change and “F” is the Faraday’s constant (96,485
Coulombs/mol).

Pre-Lab
Provide a purpose, and a brief summary of the procedure in your lab notebook before coming to
lab.

Objectives
• Construct an electrochemical cell.
• Measure the cell potential for an electrochemical cell.
• Calculate the free energy change for an electrochemical cell using the measured cell potential
value.

Materials
Zinc, copper, and silver electrodes, 0.2 M solutions of Zn2+, Cu2+, Ag+, 2 M ammonium nitrate

Electrochemical cell kit (from the stockroom)

Procedure

1. Obtain an Electrochemical Cell kit from the stockroom. Make sure that the electrodes are sanded.

2. Construct the cell using the following procedure:

a. Insert the two medicine droppers into the two holes of the provided rubber stopper.

b. Place a small piece of cotton plug at the tip of each medicine dropper.

c. Place the electrode inside the medicine dropper and surround the electrode with the
appropriate electrolyte solution.

d. Place the medicine dropper and the stopper set up on a plastic cup containing aqueous
ammonium nitrate solution.

37
e. The entire set up should look similar to that shown in Figure 2 below.

Figure 2 Electrochemical Cell Laboratory Setup

f. Construct each cell shown in Table 1 below.

38
 g. NOTE: In cells 1, 2, and 3 the 0.2 M solutions of electrolytes provided may be used as
is.

h. NOTE: In cells 4 – 7, 0.01 M solutions of electrolytes are needed. In order to prepare

these solutions, add ONE drop of 0.2 M solution to 19 drops of deionized water.

i. NOTE: Replace the cotton and NH4NO3 for each cell.

3. Measure the cell potential of each constructed electrochemical cell to the nearest millivolt.

4. Repeat the entire experiment to obtain a duplicate set of readings.

5. Discard all the waste into a large waste beaker. Empty the contents of the waste beaker into a waste
container provided by the instructor.

39
Name________________________________ Course & Yr_________________Date _________

Data and Observations

1. Calculation of theoretical values of E cell & ΔG: For each write the cathode and anode
halfreactions and the overall reactions. Refer to tables of standard reduction potentials and
calculate the standard cell potential. Using Equation 2, calculate the non-standard cell potential E,
based on the concentrations used in the experiment. Also calculate ΔG for each cell using
Equation 3. Cell number 1 is shown below as an example.

Cell Number 1: Zn|Zn2+(0.20M)||Cu2+(0.20M)|Cu

40
Cathode: Cu2+(aq) + 2e− → Cu(s) E°RED = +0.34 V
Anode: Zn(s) → Zn2+(aq) + 2e− E°RED = −0.76 V

Overall: Zn(s) + Cu2+(aq) → Zn2+(aq) + Cu(s) E°cell = 0.34 – (-0.76) = 1.10 V

Q = CuZn22++ = 0.200.20 =1

E E= −o 0.0592 logQ=1.10−
0.0592 log(1) =1.10V n 2

ΔG = − nFE = − 2 × 96485 × 1.10 = -212267 J/mol = -212 kJ/mol

Cell Number 2: Cu|Cu2+(0.20M)||Ag+(0.20M)|Ag

Cell Number 3: Zn|Zn2+(0.20M)||Ag+(0.20M)|Ag

41
Cell Number 4: Zn|Zn2+(0.20M)||Cu2+(0.010M)|Cu Cell Number 5: Zn|Zn2+(0.010M)||Cu2+(0.20M)|
Cu

Cell Number 6: Zn|Zn2+(0.20M)||Ag+(0.010M)|Ag Cell Number 7: Zn|Zn2+(0.010M)||Ag+(0.20M)|

Ag

42
2. Determine the experimental value of ΔG for each cell using Equation 2 and the
experimental value of Ecell (average from two trials).

3. Enter the experimental (average from two trials) and theoretical values of E cell and ΔG for
each cell and calculate the percent error in the experimental value in each case.

43
4. Using the zinc/copper cell diagram shown in Figure 1 as an example, draw labeled
diagrams for the other two cells used in this experiment.

Copper/Silver Cell

Zinc/Silver Cell

44
Activity 2.4
Corrosion of Metals
Objective
The objective of this experiment is to measure the corrosion rate of two different metals and to
show the effectiveness of the use of inhibitors to protect metals from corrosion.

Background
The importance of corrosion can be seen in daily life. Corrosion causes accidents in industry, on
highways, and in homes. It is wasteful financially, costing industrialized nations 45% of their
gross domestic products annually. A little knowledge of electrochemistry, material science and
corrosion could save nations some 25% of this loss.
Corrosion engineering is the application of science and art to prevent or control corrosion
damage in a safe and economical manner. To perform this function properly, the corrosion
engineer must rely on experimental research. This is because the major aspects of corrosion
engineering are largely empirical in nature. A body of theory exists that can be very helpful in
solving corrosion problems, but in the final analysis, most decisions are based on the results of
empirical tests.

Corrosion tests are conducted for a number of reasons including:

1. Establishing corrosion mechanisms.
2. Defining corrosion resistance of materials and how to develop new corrosion resistant alloys.
3. Estimating service life of equipment.
4. Developing corrosion protection processes.
5. Defining the critical potential values for materials in various environments.

Theory
Anodes and Cathodes:
In analyzing corrosion, the first thing that must be determined is whether a metal reacts with its
environment. If so, the nature of the reaction must be understood. It is generally accepted that
corrosion processes are caused by the formation of electrochemical cells. The electrochemical
reactions in these cells can be divided into two reactions:
1. Anodic reactions
2. Cathodic reactions
where each reaction is called a half-cell reaction. In the anodic reaction, metal goes into solution as
an ion. The reaction is generally written as:

M → Mn+ + ne-

where M is a metallic element, e- is an electron and n is the valence of the metal as an ion. An
example of this is Zinc where:

Zn → Zn2+ + 2e-

45
 In the cathodic reaction, electrons provided by the anode, flow through the metal until they reach
the cathode where they can be combined with positively charged ions. In acidic solutions this
reaction is:

2H+ + 2e- → 2H → H2 (gas)

and in neutral solutions the reaction is:

O2 + 2H2O + 4e- → 4OH-

Both the anodic and cathodic reactions must occur simultaneously for a corrosion process to
proceed. If both reactions are not occurring then a charge builds up and the corrosion process
stops. The anodic reaction is generally the simple case of a metal going into solution. However a
variety of cathodic reactions are encountered depending on the conditions of the process
involved. Table 1 shows several examples of different cathodic reactions. Note that in all of the
cathodic reaction electrons are absorbed.

Table 1 - Possible Cathode Reactions in Different Galvanic Cells

––––––––––––––––––––––––––––––––––––––––––––––––––––––––––––––––––––––
Cathode Reaction Example
2H+ + 2e- → 2H Acid Solutions
O2 + 2H2O + 4e- → 4OH- Neutral and alkaline solutions
O2 + 4H+ + 4e- → 2H2O Using both O2 and H+ in acid solutions
3+ - 2+
M +e →M When Ferric ions are reduced to ferrous
2+ -
M + 2e → MO When iron is placed in a Cu salt solution the
electron from solution of the iron reduces Cu
ions to metallic Cu
––––––––––––––––––––––––––––––––––––––––––––––––––––––––––––––––––––––

The electrode potential in the electrochemical cell

When an ideal metal is placed in an electrolyte, an electrode potential develops that is related to
the tendency of the material to give up electrons. To measure this tendency, we measure the
potential difference between the metal and a standard electrode using a half-cell.

The standard reference electrode is a half cell with a known constant potential. Different
standard reference electrodes are used depending on the solution environment. Some standard
electrodes are the standard hydrogen electrode (SHE) and the saturated calomel electrode (SCE).

Standard expressions for corrosion rate

In most cases, aside from contamination problems, the primary concern where corrosion is
present, is the life (usually in years) of metals in question. A good corrosion rate experiment
should include:
1. Familiar units.
2. Easy calculations with a minimum opportunity for errors.
3. Ready conversion of data to life in years.
4. Penetration.
5. Whole numbers without cumbersome decimals.

46
Mils penetration per year (mpy) is the most commonly used corrosion rate expression. One
formula used to calculate the corrosion rate is:

534 x W
mpy = ––––––––
DxAxT

where:
W = weight loss (g)
D = density of the specimen, g/cm 3
A = area of specimen, sq. in.
T = exposure time, hr.

The corrosion rates of resistant materials generally range between 1 and 200 mpy. The relative
corrosion resistance of a material can be evaluated using the following criteria:

Relative Corrosion Resistance mpy

outstanding <1 excellent 1-5 good 5-20 fair 20-50
poor 50-200
unacceptable >200

Consider a car engine block with and without the addition of antifreeze, as an example of a
corrosion rate problem. Engine blocks are generally made from low carbon steel that corrodes
when exposed to tap water. This is the brown rust that is often seen in cooling systems containing
water only. The corrosion reactions for low carbon steel are:

Fe --> Fe2+ + 2e-

Fe2+ --> Fe3+ + e-

O2 + 2H2O + e- --> 4OH-

2Fe + 2H2O + O2 --> 2Fe2+ + 2OH- --> 2Fe(OH)2

2Fe(OH)2 + H2O + 1/2 O2 --> 2Fe(OH)3 (rust)

The electrochemical technique is used to study the corrosion rate of low carbon steel in tap water
instead of using the weight loss technique. This is because the former is a very rapid method of
obtaining data while the latter technique is a very lengthy process. In the electrochemical process
the corrosion rate is measured by measuring the current density, J:

I
J = ––
A

where I is the current in microamps (μA) and A is the area in cm2. The corrosion rate can be
calculated from this using the relationship:

47
 1 mpy = (1/n ) J

where n is the valence of the metal involved (M → Mn + + ne-).

Procedure

CAUTION: BE SURE YOU UNDERSTAND HOW TO OPERATE THE

EQUIPMENT BEFORE BEGINNING THE EXPERIMENT

If you are not familiar with the equipment ask for help from your instructor. DO NOT
START INDISCRIMINATELY MAKING ADJUSTMENTS TO THE EQUIPMENT.

Your group will be provided with samples of 1018 steel and brass. Prepare the sample (metal
exposed side) for metallographic observation (polish/grind using 400 grit, 600 grit sandpaper and
1 micron powder). Check the specimens under the microscope to be sure that they are well
polished. Observe the surface of each specimen before and after corrosion takes place. Take
photos.

CAUTION: The equipment used to measure corrosion rates is very delicate. Use extreme care
when handling.

Pour about 400 cc tap water (room temperature) into the beaker that makes up the
electrochemical cell and add approximately one teaspoon of salt to form a solution. Then place
one prepared (steel or brass) specimen in the cell setup with the calomel standard reference
electrode and the counter electrode. Check to be sure that the counter electrode and the sample
surface are parallel (not touching).

Connect the leads from the EG&G VersaStat to the electrochemical cell. The Green wire
attaches to the working electrode (the sample), the Red wire attaches to the counter electrode,
and the White wire attaches to the reference electrode. Figure 1 below shows the EG & G
VersaStat equipment.

48
 Figure 1 EG&G Versastat II

If the machine is not already on, boot up the computer and at the DOS C:\> prompt type: corr
[ENTER].

When the title screen comes up hit any key to display the Main menu. Pick “ SetUp“ from the main
menu to display the Set up menu. Pick “Get Set Up”.

You will then be asked to “Enter setup filename for recall.” Type: 227L [ENTER].

The screen will now display the test parameters to be used for your experiment. Your group will
have to enter the correct sample area and specimen density in their respective fields on the test
Setup Screen.

Once the correct test parameters have been entered for your specimen, your group is ready to run
a test. Choose the Run command from the menu and turn the Cell Switch located on the front of
the EG&G Versa Stat to the ON position. A plot of your test will appear on the computer screen
once the test begins. The test runs for 15 minutes.

When the test stops, turn the Cell Switch to the OFF position. Always save your data before
beginning any further tests. To save your data first save your data on the C drive using the
“Save” command in the “File” menu. Next recall your data using the “Get Data” command in
the “File” menu. Finally, transfer the data to your flash drive in the A drive by choosing the
“Export Data” from the “File” menu. Type in a file name for your data including an A drive
path. (For example, you can type: a:\steel).

Repeat this procedure for the other metal (steel or brass) sample.

Next put about 400 cc of the prepared antifreeze/water mixture (50% ethylene glycol) into the
electrochemical cell and repeat the experiment for the remaining samples. Note the corrosion
inhibiting effect of the antifreeze. Normally, when antifreeze is added in small concentrations to

49
an environment, the corrosion rate decreases. In a sense, an inhibitor can be considered a
retarding catalyst. The effectiveness of an inhibitor can be measured based on:

Corrosion rate without inhibitor

Degree of effectiveness of inhibitor = ––––––––––––––––––––––––––
Corrosion rate with inhibitor

when a rate is determined using the mpy equation once the rate has plateaued.

Write Up

1. Write a memo report including the rate of corrosion for all samples in mpy (once the specimen's
rate levels off), and the degree of effectiveness of the inhibitor.

2. Graph the current density versus time.

3. Discuss the sources of error in this experiment.

Assignment

Glossary of Terms

Understanding the following terms will help in understanding this experiment. Define the following
terms:

1. Anode.

2. Anodic reaction.

3. Aqueous corrosion.

4. Cathode.

5. Cathodic reaction.

6. Composition cells.

7. Corrode.

8. Electrochemical cell.

9. Electrochemical corrosion.

50
10. Electrode potential.

11. Electrolyte.

12. Electromotive force series.

13. Galvanic corrosion.

14. Galvanic series.

15. Inhibitors.

16. Oxidation reaction.

17. Oxygen electrode.

18. Passivation.

19. Reduction reaction.

20. Water electrode.

Activity 2.5
Radioisotope Dating
The Zag meteorite fell in the western Sahara of Morocco in August 1998. This meteorite was
unusual in that it contained small crystals of halite (table salt), which experts believe formed by
the evaporation of brine (salt water). It is one of the few indications that liquid water, which is
essential for the development of life, may have existed in the early solar system. The halite
crystals in the meteorite had a remarkably high abundance of 128Xe, a decay product of a
shortlived iodine isotope that has long been absent from the solar system. Scientists believe that
the iodine existed when the halite crystals formed. The xenon formed when this iodine decayed.
For this reason, the Zag meteorite is believed to be one of the oldest artifacts in the solar system.
In this lab, you will use potassium-argon radiochemical dating to estimate the age of the Zag
meteorite and the solar system.

Objective
Determine the age of the Zag meteorite, using potassium-argon (K-Ar) radiochemical dating.

Materials
calculator
graph paper(4 sheets)

51
Pre-Lab
1. Suppose the initial number of nuclei of a radioactive nuclide is N0, and that the half-life is T.
Then the amount of parent nuclei remaining at a time t can be written as N1 = N0(1/2)(t/T). This
relationship is called the radioactive decay equation. What is the number of daughter nuclei
present at time t, expressed in terms of N0 and N1?

2. What is the ratio of daughter nuclei to parent nuclei at time t expressed in terms of N0 and N1?
Simplify the expression.

3. Use the radioactive decay equation to eliminate N0 and N1 from your answer to question 2.

4. 1940K decays to 20
40
Ar . 19
40
K has a half-life of 1.25 x 10 9 years and decays by positron (+10)
emission. Write the equation for this nuclear reaction.

Procedure
1. Data Table 1 shows a number of quantities that change with time in a radioactive
system. Column one shows the time, expressed in units of the half-life of the radioactive parent.
Column two shows the fraction of the original parent nuclei that remain after the indicated
number of halflives. Subtract the value in column two from 1.0 to obtain the fraction of the
original parent nuclei that have decayed to daughter nuclei. The final column is the ratio of
daughter nuclei to parent nuclei. Complete Data Table 1.

2. Plot a graph of daughter-to-parent ratio versus number of half-lives on the axes in Figure
A. Draw a smooth curve through the points.

3. The ratio of 40Ar to 40K was measured for four samples from the Zag meteorite. The
values obtained are shown in Data Table 2. Use your graph in Figure A to estimate how many
half- lives (to the nearest tenth of a half-life) have passed since the meteorite was formed.
Multiply number of half-lives by 1.25 x 10 9 years, the half-life of 40K, to obtain an estimate of the
age of the sample. Use the average value from the age determinations of all four samples to
estimate the age of the meteorite.

52
53
Name________________________________ Course & Yr_________________Date _________

Data and Observations

Figure A Daughter-to-Parent Ratio Versus Elapsed Time

54
Name________________________________ Course & Yr_________________Date _________

Average age (109 yr) =____________________________________________________________

Analyze and Conclude

1. Measuring and Using Numbers What is the average age of the Zag meteorite (in years)?

__________________________________________________________________________

2. Thinking Critically The K-Ar data for this experiment were obtained using a mass
spectrometer. In this process, a small sample is heated with a laser until its constituent atoms
vaporize and become ionized. A voltage is then applied that accelerates the charged ions
towards a detector. The lightest ions reach the detector first, and the numbers of ions of each
mass are identified and counted. There are a number of practical concerns that researchers
must address in order to be confident that the measurements truly yield an accurate age for the
object. List and explain a few possible concerns.

_________________________________________________________________________

______________________________________________________________________________

______________________________________________________________________________

____________________________________________________________________________

______________________________________________________________________________

_________________________________________________________________________

55
Name________________________________ Course & Yr_________________Date _________
______________________________________________________________________________

______________________________________________________________________________

______________________________________________________________________________
________________________________________________________________________

______________________________________________________________________________

___________________________________________________________________________

3. Comparing and Contrasting 14C decays to 14N with a half-life of 5730 years. This
reaction is used for radiochemical dating of a certain class of terrestrial objects. How many half-
lives of 40C have passed since the Zag meteorite formed?

_________________________________________________________________________

______________________________________________________________________________

______________________________________________________________________________

______________________________________________________________________________

4. Thinking Critically Based on your answer to question 3, explain why radiochemical

dating using carbon is an inappropriate technique for dating meteorites.

______________________________________________________________________________

______________________________________________________________________________

________________________________________________________________________

_________________________________________________________________________

____________________________________________________________________________

___________________________________________________________________________

______________________________________________________________________________

______________________________________________________________________________

56
Name________________________________ Course & Yr_________________Date _________

57
Assignment

1. A sample of spruce wood taken from Two Creeks forest bed near Milwaukee, Wisconsin,
is believed to date from the time of one of the last advances of the continental ice sheet into the
United States. The ratio of 14C to 12C in the sample was found to be 0.2446 of the atmospheric
value of this ratio. What is the daughter-to-parent ratio for the decay process in the sample?

2. What is the estimated age of the spruce wood sample? Show calculations that support
your answer.

58
Activity 3.1
Metallic and Ionic Crystal Lattices
Objectives
The purpose of this experiment is to construct models of the common metallic and ionic crystal
lattices and to study their characteristics.

Method

Historically, Styrofoam balls were connected with wooden toothpicks. Now we will use the Solid
State Model Kits to reproduce the following crystal lattices:

IONIC METALLIC

A. sodium chloride (rock salt) D. face centered cubic (Cubic close packed)
B. cesium chloride E. body centered hexagonal (Hexagonal close packed)
C. wurtzite (Hexagonal ZnS) F. body-centered cubic

By looking at these models, you will be able to identify many features of these lattices. Figure 1
shows the unit cells for the metallic crystal lattices and Figure 2 shows the unit cells for the ionic
crystal lattices.

Pre-Lab
(To be completed before coming to lab)

1. Write the equation for the volume, V, of a cube in terms of its side, s:

V =________________________________________

2. Write the equation for the volume, V, of a sphere in terms of its radius, R:

V =__________________________________________

59
3. Write the Pythagorean Theorem equation for a right triangle with sides a and b adjacent to the
right angle and hypotenuse c:

_____________________________________________

4. If a right triangle has two equal sides of length a, express the length of the hypotenuse c in
terms of a:
c =__________________________________________

5. For a cube with sides of length s:

a. Express the length of a diagonal across a face, FD, in terms of s:

FD =_______________________________________

b. Express the length of a diagonal through the body, BD, in terms of s:

BD =_______________________________________

6. Simplify 8 :

8 =_________________________________________

Procedure

You will use the Solid State Model Kit and the Instructions in the kit to answer the following
questions. Refer to the diagrams both here and in the Model Kit for assistance.

1. Find the instruction manual in your Model Kit. Read “Getting Started” along with the rest
of the information on pages 1-5.

60
2. Do the NaCl example on pages 6-7 using the Model Kit. This example takes you through
the questions step by step, while all other examples are abbreviated. You won’t have any
problems IF you have followed instructions 1 and 2!

3. Answer all of the questions for the NaCl example in part A below, then proceed with the
other parts. Answer all of the questions while you have the model in front of you for reference.

Introduction

The following are the simplest crystal lattice structures found in nature.

a. face-centered cubic b. body-centered hexagonal c. body-centered cubic

(cubic close-packed) (hexagonal close-packed)

Figure 1: Common metallic crystal lattice unit cells. Ion sizes not to scale

a. CsCl (simple cubic) b. NaCl (face-centered cubic)

Cesium Chloride Sodium Chloride (rock salt)

61
c. ZnS (face-centered cubic) d. ZnS (body-centered hexagonal)
Zinc Sulfide (zinc blende) Hexagonal Zinc Sulfide (wurtzite)

Figure 2 Common ionic crystal lattice unit cells for 1:1 salts. Ion sizes not to scale

CRYSTAL LATTICES

Construct each model using the Instructions in your Solid State Model Kit, answering questions
as you go. As you progress, have your work checked by the instructor. Be prepared to answer
questions about the information you have gathered.

Ionic Lattices

A. Sodium Chloride (Rock Salt), Octahedral Sites: Model A Follow

instructions on pages 6-7 of your Model Kit Instruction Manual.

Figure 3 The Na+ ion in the octahedral hole of the NaCl lattice.

1. What is the CN of X? (That is, how many Cl- ions are around each Na+ ion?) _____
This is known as the coordination number (CN) or number of nearest neighbors.

Figure 4 Sodium Chloride (Rock Salt). Smaller Na+ spheres in the octahedral holes of a
face-centered cubic lattice of Cl- spheres.

2. Within each unit cell, how many net Cl- ions are:

62
 a. on the corners (net number) _____

b, on the edges (do not count corners again) _____

c. within the faces _____

d. within the center _____

e. net total _____

3. Within each unit cell, how many net Na+ ions are:

a. on the corners (net number) _____

b. on the edges (do not count corners again) _____

c. within the faces _____

d. within the center _____

e. net total _____

4. The chloride ions alone describe what lattice? _______________________

5. The sodium ions alone describe what lattice? _______________________

6. Calculate the radius of the sphere that will touch all six surrounding spheres. Hint: tilt the
model until you see the plane of 4 spheres as shown.

small sphere of radius r

7. Calculate the radius ratio R/r (or r/R). ______

B. Cesium Chloride. Cubic Sites: Model B

Follow the instructions beginning on page 11 of the instruction manual.

Figure 5 The Cs+ ion in the cubic hole of the CsCl lattice

63
1. What is the CN of X? (That is, how many Cl- ions are around each Cs+ ion?) _____

Now complete the CsCl lattice.

Figure 6 Model B. Cesium Chloride, multiple unit cells

2. How many complete unit cells of CsCl are contained in this model? _____

3. Within each unit cell, how many net Cl- ions are:

a. on the corners _____

b. on the edges _____

c. within the faces _____

d. within the center _____

e. net total _____

4. Within each unit cell, how many net Cs+ ions are:

a. on the corners _____

b. on the edges _____

c. within the faces _____

d. within the center _____

e. net total _____

5. The chloride ions alone describe what lattice? _________________________

6. The cesium ions alone describe what lattice? _________________________

C. Hexagonal Zinc Sulfide (Wurtzite), Tetrahedral Sites: Model C

Follow the instructions on page 54 of the Solid State Kit Instruction Manual.

64
 Figure 7. The Zn2+ ion in the tetrahedral hole of the hexagonal ZnS lattice.

1. What is the CN of X? (That is, how many S2- ions are around each Zn2+ ion?) ______

2. How many complete unit cells of ZnS are contained in this model? ______

3. Within each unit cell, how net many S2- ions are:

a. on the corners _____

b. on the edges _____

b. with in the faces _____

c. within the center _____

d. net total _____

4. Within each unit cell, how many net Zn2+ ions are:

a. on the corners _____

b. on the edges _____

c. within the faces _____

d. within the center _____

e. net total _____

Metallic Lattices

D. Face-Centered Cubic (FCC) or Cubic Close-Packed: Model D

Follow the instructions on page 27 of the Solid State Model Kit Instruction Manual.

65
Figure 8. Model A. Face-Centered Cubic.

1. How many spheres are directly touching the sphere marked with an "X" above? _____

2. Within the unit cell, how many (net number) spheres are:

a. on the corners (net contribution) net no.= __________

b. within the faces (do not count the corners again) net no. = __________

c. in the center net no. = __________

d. total all number of spheres in the unit cell ____________

3. FCC is one of the two close-packed lattices. In one of these, every other layer is the same,
called ABAB packing. This means that for every sphere in the 1st layer, there is a sphere right
above it in the 3rd layer. In the other type of close packing, spheres repeat every third layer,
called ABCABC packing. In this arrangement, each sphere in the 1st layer does not have a
sphere right above it until the 4th layer.

Is the packing in FCC, ABAB or ABCABC? ______________

(Hint: the four layers you have made are NOT the close packed layers. In order to see the packing
type, use the cube made by the first three

4. What are the relationships among the sides (a, b, c) in the

FCC unit cell (equal or unequal) _____

5. What are the angles (, , ) in the FCC unit cell? _____

Use the diagram of the face-centered cubic lattice below to answer the following questions.

66
 Face-centered cubic (FCC)

6. How many net spheres are in the unit cell? ______

7. What is the volume of a sphere in terms of R, the sphere radius? ______

8. What is the total volume occupied by the spheres in the unit cell in terms of R?

9. What is the face diagonal (corner-to-corner distance on face) in terms of R?

10. What is the value of S in terms of R? Use the Pythagorean Theorem on the right triangle
given. Show work below.

11. Give the volume of the cube in terms of S.

67
12. Give the volume of the cube in terms of R.

13. Calculate the percent of occupied space.

% occupied = (Vspheres/Vcube) x 100%

E. Bodv-Centered Hexagonal or Hexagonal Close-Packed (HCP): Model E

Follow the directions on page 24 of the Solid State Model Kit Instruction Manual.

Figure 9 Model E. Body -Centered Hexagonal .

1. What is the coordination number (number of nearest neighbors) in the hexagonal close packed
lattice? ______

2. Within the unit cell, how many (net number) spheres are:

a. on the corners (net contribution) net no. = _____

b. within the faces net no. = _____

c. in the center (inside the cell) net no. = _____

d. total net number of spheres in unit cell

_____

68
3. Is the packing in HCP ABAB_________ ABABC_________?
(Hint: the four layers you have made ARE the close packed layers in the hexagonal close-packed
lattice.)
4. What are the relationships among the sides (a, b, c) in the HCP unit cell (answer: equal or
unequal)? _____

5. What are the angles (, , ) in the HCP unit cell? _____

F. Body -Centered Cubic (BCC): Model F

Figure 10 Model F. Body -Centered Cubic.

1. What is the coordination number (number of nearest neighbors) in the body-centered cubic
lattice? _____

2. Within the unit cell, how many (net number) spheres are:

a. on the corners (net contribution) net no = _____

b. within the faces (do not count the corners again) net no =
_____

c. within the center net no =

_____

d. total net number of spheres in unit cell

_____

3. The body-centered spheres in the neighboring unit cells are only 14% farther away than those
touching the body centered sphere in this cell. Such spheres are called next nearest neighbors.
How many next nearest neighbors are in the BCC lattice? ______

4. What are the relationships among the sides (a, b, c)

in the BCC unit cell (equal or unequal)? ______

5. What are the angles (, , ) in the BCC unit cell?

______

69
Use the two diagrams of the body-centered cubic lattice below to-answer the following questions.

Body-centered cubic
6. How many net spheres are in the unit cell? _____

7. What is the volume of all the spheres in the unit cell, in terms of R? _____

8. What is the body diagonal (BD) of the cube in terms of R? Note: the central sphere
touches each corner sphere. _____

9. What is the face diagonal (FD) of the cube in terms of S? Use Pythagorean theorem on the
right triangle which has FD as the hypotenuse. Show your work below. _____

10. What is the value of S in terms of R? Use the Pythagorean theorem on the right triangle which
has BD as the hypotenuse. Use your values of BD in terms of R and FD in terms of S. Show
your
work below. _____

11. Give the volume of the cube in terms of R. _____

70
12. Calculate the percent of occupied space. _____

13. Which type of packing is more efficient? ______FCC or ______ BCC

Post-Lab

1. Cesium chloride structure

a. Why is it not proper to say that CsCl has a body-centered cubic structure?

b. Thallium (I) chloride crystallizes in the cesium chloride lattice, as shown in Fig. 5. The
shortest distance between the center of a Tl + ion and the center of a Cl- ion is 333
pm.

1) What is the length of the edge of a unit cell of TlCl? Hint: How many TlCl diameters
equal one body diagonal?

2) What is the density in g/cm3 of TlCl?

2. Superconductors. Given the idealized unit cell for the structure of a superconductor
shown below to be orthorhombic, answer the following questions.

71
 a. How many copper atoms are there per unit cell? (Show calculations.)

b. What is the number of oxygens per unit cell? and Y? and Ba?

c. What is the formula for this superconductor?

d. The coppers in this unit cell occupy two different kinds of sites. Based on the number
of each of these types and the formula for the compound, what are the oxidation states
for copper in this compound?

The following Questions will likely require some research and reading outside of our
textbook! Go dig out the information that you need!

3. a. What makes a substance a superconductor?

b. Give the properties of superconductors.

4. Explain why ionic solids are brittle and metals are malleable.

72
5. Explain why metals decrease in conductivity with a rise in temperature while
semiconductors increase in conductivity with temperature.

6. How does the band theory explain luster of metals and heat conductivity? Include labeled
diagrams in your answer.

Activity 3.2
Specimen Preparation and Microscopic
Examination
Objectives:
1. Familiarization with the procedure for preparation of a material specimen for microscopic
examination.
2. Familiarization with compound optical microscopes and metallography.
3. Examination of surface characteristics of engineering materials.
4. Grain size determination of metals.

Background:
The preparation of a metallurgical specimen generally can be divided into a series of stages:
sectioning, mounting, grinding and polishing, and etching.

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Sectioning

Sectioning is the removal of a small representative volume of material from the parent piece. The
microstructure of the material must not be altered in the process. Cold work and heat are the two
most likely conditions that can quickly bring about structure changes. Quite obviously operations
such as sawing that generates heat or shearing that introduces cold work are not preferable for
sectioning. Cutting using a bonded abrasive wheel with coolant offers the best solution to
minimize or eliminate heat and deformation.

Mounting

Metallurgical specimens are mounted primarily for (1) convenience in handling and (2)
protection and preservation during subsequent grinding and polishing. Two methods are
frequently used: compression mounting and cold mounting.

Compression mounting is done by mounting the specimen in a cylinder of hard polymer under
pressure and elevated temperature in a molding machine (Figure 1). The method is often preferred
when speed and a relatively hard mounting is required. For metallurgical examination, specimens
are usually molded in cylinders 1, 11/4, or 11/2 inches in diameter.

Compression molding materials are (1) thermosetting or (2) thermoplastic polymers. Bakelite and
diallyl phthalate fall into the first category while transoptic material into the second. By
definition, thermosetting materials require heat and pressure during the molding cycle, and
therefore may be ejected at high molding temperature. Transoptic materials remain molten at high
temperature and become transparent with increasing pressure and decreasing temperature.

Molding pressure, temperature, and time duration are the major variables involved in
compression mounting. By equipment design, temperature may be held constant leaving pressure
and time duration as variables.
Cold mounting is done by placing the specimen at the center of a metal or pyrex ring on a glass
plate and pouring liquid mounting material into the ring to cover the specimen. Allow the
mounting material to cure at room temperature for 60 to 90 minutes before removing the ring.
The method offers particular advantages when a specimen is too delicate to withstand the pressure
and heat involved in compression molding. With cold mounting, large groups of specimens may
be easily prepared in a short time.
Common types of cold mounting material include (1) epoxides (2) polyesters and (3) acrylics.
These materials are two-component types consisting of a resin and a hardener. Since the curing
process (polymerization) is an exothermic reaction the mixing by volume or weight ratios of each
type is critical.

Grinding and Polish

Grinding and polish are accomplished by sequential coarse grinding, medium grinding, and
rough and final polishing. The specimen should be carefully rinsed before proceeding from one
operation to the next.

Coarse grinding is done on a wet-belt grinder with 120 and 240 grit belts. The purpose of coarse
grinding is to obtain a flat surface free from previous cutting tool marks.

74
 Medium grinding is accomplished using successively finer grits of metallographic grinding
paper. The paper is supported on a hard, flat surface such as glass or steel. The specimen is moved
along the length of grinding paper without rotation or a rocking motion. When grinding is
completed on one grit the scratches should all run in the same direction. Before proceeding to the
next finer grit the specimen should be washed to avoid brining large particles to the finer grit. The
specimen is rotated 90 degrees between grits so that scratches from each successively finer grit
run at right angles to those from the previous one. The polishing on a grit is complete when
coarser scratches from previous grit have been totally removed.

Rough and final polishing is accomplished on cloth-covered wheels charged with fine abrasive
alumina particles suspended in water. Nylon cloth and 1.0-m alumina particle size are used for
the rough polish; a velvet cloth and 0.05-m particle size for the final polish. A few drops of
water are added to the rotating wheel to improve polishing action and cleanliness. Initially the
specimen is held at one position on the wheel, without rotation, until most of the previous
grinding marks are removed. The specimen can then be rotated slowly, counter to the wheel
rotation, until only scratches from the alumina are visible. The final polish should be completed at
a slow speed on a different polishing wheel.

Etching

The specimen surface is fairly smooth immediately after the final polish. A smooth surface
deflects lights from the illuminator in the metallurgical microscope along the same direction
showing no contrast and cannot reveal surface characteristics. Surface characteristics such as
different phases, inclusions, porosity, cracks, intergranular corrosion can be revealed by etching.
Etching is defined as the process to reveal structural details by preferential attack of a metal
surface with an acid or other chemical solutions.

Experimental Procedure:

1. Obtain a steel specimen from the instructor and remove as much surface scale as possible.
The steel specimen has been heat treated to form a desired structure for this exercise.

2. Mount the specimen in a phenolic cylinder using a compression mounting press. Watch
carefully the demonstration of the use of compression mounting press. Appropriate molding
pressure and time should be used in the process.

75
 Figure 1 A compression mounting press.

3. Prepare the specimen by coarse grinding on a wet-belt grinder, hand polishing on four
successively finer grits of polishing paper, and fine polishing on two polishing wheels with 1.0-
m and 0.05-m alumina powders. Rinse the specimen thoroughly between steps.

4. Etch the steel specimen by immersing it in a nital solution (5% concentrated nitric acid in
alcohol). Start with 5 seconds of immersion. Rinse the specimen with water, dry with paper
towel, immerse briefly in alcohol, and blow dry the specimen with a blow dryer.

5. Examine the specimen under microscope and identify the surface features. The specimen
surface may be overetched or underetched. An overetched specimen surface shows patches of
dark color with no identifiable features. On the other hand, a shiny, smooth surface with little or
no surface features revealed indicates an underetch. Repeat the final polishing to remove the
damaged surface and etching for less time if the specimen is overetched. In the case of underetch,
repeat the etching step to enhance the contrast.

76
 Figure 2 A metallurgical microscope.

Microscope Focusing Procedure

1. Initially the lowest power objective lens is used for focusing the specimen. Turn the
lowestpower objective lens into place. If necessary, turn the coarse stage height control to
lower the sample stage to make room so the objective lens can be turned into place.

2. Turn the stage height focusing control to position the specimen about half a centimeter under
the objective lens.

3. Look through the eyepieces and use the focusing controls (coarse and fine stage height
controls) to bring the specimen into appropriate focus.

4. Scan the specimen surface by moving the stage using the stage position controls and select the
areas that may warrant more complete study at higher magnification.

5. Turn the higher-power objective into place.

6. Adjust the stage height using the fine control until the specimen comes into sharp focus. Be
sure that the objective lens does not touch the specimen surface at any time. Otherwise the
objective lens may be scratched and permanently damaged.

7. A drop of oil on specimen surface usually is needed at higher magnification (greater than
X2000) to help with focusing.

77
Photographing Microstructure

A Polaroid Land camera mounted on the Bausch & Lomb microscope is to be used to photograph
specimen surface characteristics.

Figure 3 A Bausch & Lomb microscope equipped with a Polaroid Land camera

Procedure for photographing

1. Place the sample (inverted) on sample stage and bring the sample surface into focus at the
desired magnification. Place a drop of oil at the center of sample to enhance focusing, if
needed.

2. Check the Polaroid camera to ensure there are instant films in it.

3. Turn the visual observation knob clockwise to PHOTO.

4. Set the Shutter Speed with the Shutter Speed Control. Ask the instructor for the appropriate
shutter speed.

5. Press the COCK OR CLOSE button.

78
6. Press the Release button.

7. Pull the exposed film envelop out of the camera and time the development before removing the
photograph. Development time can be determined from the information sheet that comes with
the film.
Assignment:

1. Watch the demonstration of specimen preparation and microscope operation procedures

carefully.

2. Obtain a sample from the instructor and prepare the sample for microscopic examination
following the procedure of mounting, grinding, polishing, etching, observation under a
microscope, and photographing.

3. Keep a hard copy (photograph) of the sample as observed under the microscope. Record the
important information such as sample material, processing history, and photo magnification on
the back of the photograph.

4. Include the photograph in the report and identify all the features observed.

5. Determine the ASTM grain size using the photograph. Show the measurement and calculation
in the report.

6. Determine the Vickers microhardness of pearlite and ferrite in the specimen. Show the data in
the report.

79
Activity 3.3
Tensile Tests
Whether a metal is used in an automobile, a bridge, a building or a space vehicle, an important
requirement is its ability to withstand and transmit stress. This ability is usually evaluated by
tensile tests on standard specimens cut from the particular material. Tensile tests determine the
strength characteristics as well as plasticity characteristics.
The term "tensile test" refers to the test in which a prepared specimen is subjected to a gradually
increasing uniaxial load until final fracture occurs. Tensile tests are carried out on standard
specimens of circular or rectangular cross section. The ends of the specimen are gripped and
increasing tensile load is applied to cause the specimen to elongate. The applied load and the
change of a gage length on specimen are recorded simultaneously, and used to develop a
characteristic stress-strain curve. Useful mechanical properties can then be determined from the
stress-strain curve. A schematic stress-strain diagram with property determination for metals is
shown in Figure 1.

80
Figure 1 – A schematic stress-strain curve for metals. Typically, an offset of 0.002 (or 0.2%) is
used to determine the 0.2% offset yield strength.

The elongation of the specimen initially is proportional to the increasing load, as described by
Hooke's law, resulting in a straight stress-strain line segment Then, at a certain load, the
proportionality between the specimen elongation and the applied load is interrupted, causing the
stress-strain curve to deviate from the previous straight line. The stress corresponding to the point
on the curve where the proportionality ends is termed proportionality limit. In the stress range up
to the proportionality limit the material behaves elastically where the elongation can be fully
recovered upon release of the load. The slope of the straight stress-strain line can be taken as the
modulus of elasticity E, ratio of stress to strain from Hooke's law:

 =E or E = (1)

where  is stress and  is strain.

With the applied load close to or greater than the proportionality limit, plastic deformation is
formed in the material; the specimen does not restore to its original dimensions after the applied
load is removed. The transition from the region of elastic deformation to that of plastic
deformation occurs gradually; the stress-strain curve deviates from the straight stressstrain line
gradually. It is practically impossible to determine a definite location on the stressstrain curve that
marks the transition. Instead, a yield point is determined using a specified residual strain
(typically 0.2%) and modulus of elasticity as shown in Figure 1. The stress corresponding to the

81
yield point is termed (0.2% offset) yield strength of the material. Note that there will be
permanent strain (0.2%) when the load is increased to the yield point and fully removed.
Increasing the load above the yield point causes uniform plastic deformation throughout the
specimen (within gage length) and results in work hardening of the material. As the material
hardens, the load required to elongate the specimen increases until it reaches a maximum level as
shown in Figure 1. The stress corresponding to the peak on the stress-strain curve is termed
Ultimate tensile strength. The ultimate tensile strength marks the point of transition from uniform
plastic deformation to localized plastic deformation in a small (usually the weakest) region along
the length of the specimen. The local yielding results in a more appreciable local contraction of
the cross section with the formation of a "neck". Therefore, the tensile strength characterizes the
resistance of a metal to plastic deformation. The reduced cross sectional area results in increased
local stress which develops still more local yielding, and therefore decreasing load needed to
break the specimen.
Tensile test is among the simplest of all the mechanical tests. Useful properties directly observed
and those that can be estimated from tensile tests include: modulus of elasticity, yield strength,
tensile strength, ductility in % elongation or % reduction in area, modulus of resilience, and strain
hardening exponent.

Tensile Strength = (Maximum Load)/(Original Cross Sectional Area) (2)

Yield Strength (y ) = Stress at which a material exhibits a specified deviation from
proportionality of stress and strain. An offset of 0.2% is often used. (3)

Modulus of Elasticity ( E ) = slope (ratio of stress to strain) of linear stress-strain curve in

the elastic region. (4)
Percent Elongation = [(Change in gage Length)/(Original Gage Length)] x 100

− 
= l fl o lo  x100 (5)

Percent Reduction in Area = [(Change in Cross Sectional Area)/(Original Area)] x 100

− f
 A A0

= Aox100 (6)

Modulus of Resilience = Energy absorbed and released during elastic deformation

= Area under the stress-strain curve up to yield strength

82
 y 1 1  y  y2


=   d = 2 yy = 2 y  E = 2E (7)
0

The stress and strain used in Equations (1) to (7) are termed engineering stress and engineering
strains when original gage length and original cross sectional area are used. In reality, the cross
sectional area changes due to Poisson’s effect continuously resulting in a somewhat different
stress and strain during the test. For more realistic account of the real stress and strain, true stress
and true strain may be calculated using Equations (8) and (9).

True Stress ( )  t = (1+ ) (8)

True Strain ( )t = ln(1+) (9)

Using Equations (8) and (9), an engineering stress-strain curve may be converted to true stress-
true strain cure. The segment of true stress-strain curve between true yield strength and true
tensile strength can be described by a polynomial expression in the form

 t =K tn (10)

where the exponent n is work hardening exponent that describes the ease with which a metal can
be work hardened (or strain hardened). The value of the work hardening exponent can be
determined by soling two simultaneous equations from two arbitrary points on the true stress-
strain curve between yield point and ultimate tensile point as

logt1 

t2 
Strain Hardening Exponent (n) = (11)
logt1 
t2 

83
Figure 2 – (a) A Qtest/50 universal testing machine, (b) Important manual controls on the
Qtest/50 universal testing machine.

84
 Figure 3 – The Qtest/50 UTM and control system.

Objectives:
1. Familiarization with a computer-controlled universal testing machine (UTM), standard tensile
test and test procedure.
2. Observation of the tensile behavior of metal and polymer materials.
3. Determination of material properties from stress-strain curves obtained from tensile tests.

Materials:
Universal Testing Machine, metal and polymer specimens

Procedure:

Operating Procedure for Tensile Test on QTest/50

Follow the procedure carefully to avoid damages to the testing system and injury to the user. Read
each step description entirely before executing a step. No students should be allowed to operate
the system without faculty supervision in the laboratory.

1. Make sure you know where the red emergency stop button is located on the machine.
Pressing the emergency stop button once will bring the machine to a quick stop. DO NOT
press the emergency stop button a second time, unless really necessary, which may cause the
crosshead to return rapidly to its starting position.

2. Install the correct type of sample grips. Make sure the connector pins are in place.

85
3. Turn on the testing system. Always turn on the testing machine before the computer. The
toggle power switch is on the right side (lower right corner) of the machine.

4. Turn on the monitor and the computer in that order.

5. Measure dimensions of the sample: width, thickness (same as width for a bar sample), and
gage length (axial length in which the diameter, width, or thickness is constant).

6. Double click on the TestWorks QT v2.00 folder, then the TestWorks QT2.02 icon to load
the control program. A User Login window will appear.

7. Enter MEM for both User Name and Password, and click OK, or press Enter. Additional
functions on the toolbar near the top of the screen are activated.

8. Click on the Test button. A new set of functions appears in the toolbar. Select the Simple
Tensile Test (English) method from the drop-down menu for the Method. A load meter
(10000 lb cell), a Crosshead Position meter and a Handset window appear.

9. Click on the Calibrate button on the toolbar. A small Calibrate window appears. Select
LOAD from the sensor list and 10000 lb cell.

10. Make sure only sample grips and fixtures (if any) are attached to the load cell, then click on
the Calibrate button followed by the OK button. The automatic calibration starts and finishes
in a few seconds.

11. Click on OK when the calibration is complete.

12. Click on Exit in the small Calibrate window to return to the Test window.

13. Click on Sample button on the toolbar. Enter a Sample ID for your sample and click OK. It is
a good idea to have a sample ID that is short and self-explanatory.

14. Use the following procedure to install the specimen in the testing machine.
a) Screw one end of the specimen in the upper grip (assuming a rod sample is being
used).

b) Remove the lower grip and screw it onto the lower end of the specimen.

c) Lower the sample (with the lower grip attached) to about ½ inches above the lower
grip connector by pressing the green Jog Down button.

d) In the Handset window, enter a speed of 2 (In/Min). Click on Down followed by Stop
to lower the grip in to the connector while guiding the grip with hands. Insert the
fastening pin when the holes are lined up.

86
 e) Change the speed to an even slower speed (0.01 In/Min) and adjust the crosshead
position using Up (or Down) and Stop buttons to take out slacks, leaving the specimen
under a small load (~50 lb for metal samples, ~10 lb for polymers).

f) Zero the Crosshead Position meter by clicking on the Zero button.

15. Click on Inputs button on the toolbar. An Inputs window appears.

a) Select Test (under Category).

b) Click to highlight Crosshead Speed and enter an appropriate crosshead speed (consult
Table 1 for suggested speed), highlight Load Limit HI and enter 8000 Lb, and
highlight Ext (ion) Limit HI and enter 30.0 In.

Table 1 – Suggested crosshead speed for various materials. Note that the suggested speeds are not
ASTM standard speeds. These speeds are suggested so that a test may be finished in a reasonable
length of time in a class period.

c) Select Specimen from Category and enter specimen dimensions.

d) Select Calculation category, enter sample gage length.

e) Select Information, enter information about the specimen material.

f) Click on OK, the Inputs window disappears.

16. Click on the Window button on the toolbar to bring up Graphics Window.

17. For Y-Axis Setup, click to select Auto Scale Max, LOAD form Channel 1 drop-down menu ,
Lb as unit for Y-Axis, 0 for Minimum, 500 for Maximum, and 0 for Decimals.

18. For X-Axis Setup, click to select Auto Scale Max, EXTENSION from Channel 1 drop-down
menu, In as unit for X-Axis, 0.00 for Minimum, 0.05 for Maximum, 2 for Decimals, and 0.00
for X-Offset.

19. Click on OK to return to the Test window.

87
20. Click on Run button. A Required Inputs window appears. Enter correct gage length and
click on the Save/Next button. Enter the same speed as that used in Inputs for crosshead speed
and click Save/Next button. The OK button lights up.

21. Click on OK to start the test. A Warning! Message appears.

22. Click on OK again to start. A separate X-Y Curve window appears showing the LOAD-
vs.EXTENSION data. The scales are programmed to change automatically with increasingly
larger applied load and extension.

23. Wait until the test is complete. Do Not try to change crosshead speed during the test. DO
NOT press the spacebar on the keyboard. Pressing the spacebar will cause the machine to
terminate the test. Observe the “necking” phenomenon of the sample and relate it to the
change in the curve shown in the X-Y Curve window.

24. Click on File. The Test window returns.

25. For polymer samples, unscrew the tightening screws in the grips and remove the sample. Go
to step 28. For metal samples, go to step 26.

26. Use the green Jog Up button to move the crosshead upward to provide enough room for the
removal of sample (broken pieces).

27. Remove both broken specimen pieces from grips.

28. Click on the Exit button to return to the main TestWork QT window.

29. Click on Output button. A listing of samples appears. Click to highlight your sample.

30. Click on the Export button to activate the Export Options window.

31. In the Export Options window, click to select Curve. Click OK to bring up the Select
Sample window.

32. In the Select Sample window, enter sample ID and click OK. The sample ID should be
identical to that on the list. Select sample 1 (the only one with your sample ID) and click OK.
A Select Channel window appears.

33. In the Select Channel window, click to select Extension and Load. Click OK. A Select
Delimiter window appears.

34. In the Delimiter window, select Tab and click OK. An Enter Filename window appears.

35. Insert a formatted 31/2-inch floppy disk in drive a of the computer. In the space under Enter
Path/Filename window, enter a:\filename.xls (DO NOT forget the .xls file extension) and click
OK. It takes a few seconds to export the test data in Microsoft Excel spreadsheet file format to the
disk in drive a.

88
36. After the data transfer is complete, click on Cancel to exit the Export Options window.

37. Click Exit to return to the main TestWorks QT window.

38. Click on Exit followed by Yes button to exit the program. It is a good idea to check the data
files on a different computer to make sure thy are complete before exiting the program.

39. Exit Windows.

40. Turn off the computer and the monitor in that order.

41. Turn off the machine. Note: Always turn off the computer before the testing machine.

Assignment:

1. Obtain samples from the instructor. Measure and record the initial dimensions of the samples.

2. Perform the tensile tests with the samples provided following the procedure described in the
handout. Record the type of material and measure sample dimensions before any test. After
each test, save the test data in Excel format (file name with extension .xls) for data reduction
using Microsoft Excel spreadsheet.

3. For the metal sample, use Excel spreadsheet to plot an engineering stress-strain tensile behavior
curve from the collected data and determine the following material properties: a) modulus of
elasticity,

b) 0.2% offset yield strength,

c) ultimate tensile strength,

d) fracture strength,

e) ductility in percent elongation and percent area reduction, and

f) modulus of resilience.

4. For the metal sample, plot a true stress-strain tensile behavior curve up to engineering ultimate
tensile strength of the material and determine the expression ( t =K tn ) that describes the
strain hardening behavior. Note: the expression is valid only between yield strength and
ultimate tensile strength.

5. For the polymer samples,

a. prepare an engineering stress-strain curve for each of the polymer samples and relate
the changes in curves to the physical changes in the sample during the tensile testing,
and

89
 b. estimate the short-term modulus of elasticity of each material.

6. Describe the differences between the tensile behavior of the metal sample and that of polymer
sample you had observed.

Activity 4.1 Acid

Rain
Carbonic acid occurs when carbon dioxide gas dissolves in rain droplets of unpolluted air:

(1) CO2(g) + H2O(l) H2CO3(aq)

Nitrous acid and nitric acid result from a common air pollutant, nitrogen dioxide (NO 2). Most
nitrogen dioxide in our atmosphere is produced from automobile exhaust. Nitrogen dioxide gas
dissolves in rain drops and forms nitrous and nitric acid:

(2) 2NO2(g) + H2O(l) HNO2(aq) + HNO3(aq)

Sulfurous acid is produced from another air pollutant, sulfur dioxide (SO 2). Most sulfur dioxide
gas in the atmosphere results from burning coal containing sulfur impurities. Sulfur dioxide
dissolves in rain drops and forms sulfurous acid:

(3) SO2(g) + H2O(l) H2SO3(aq)

In the procedure outlined below, you will first produce these three gases. You will then bubble the
gases through water, producing the acids found in acid rain. The acidity of the water will be
monitored with a pH Sensor.

90
Objectives

In this experiment, you will observe the formation of four acids that occur in acid rain:

• carbonic acid, H2CO3

• nitrous acid, HNO2
• nitric acid, HNO3
• sulfurous acid, H2SO3

Materials

Windows PC Solid NaNO2

Vernier computer interface Solid NaHCO3
Vernier LabQuest 2 Solid NaHSO3
Vernier pH Sensor 1.0 M HCl with 2 mL plastic dropper
Wash bottle with distilled water 3 2 mL plastic droppers
Rubber stopper, size 00 3 special glass sample vials
Beakers, 600, 400, 250, 150, mL Tap water
3 20 X 150 mm test tubes

Procedure

Safety First! Wear goggles. Avoid ingesting dust from solids and breathing gasses produced.
The glass bulb at the tip of the pH sensor is fragile, so please do not hit it.

1. Think safety continuously!

2. Label the three clean medium (20 x 150 mm) test tubes with the formula of the solid they will
contain: “NaHCO3”, “NaNO2”, and “NaHSO3”. Label the three special (for this experiment)
clean glass sample vials with the formula of the gas that will be dissolved in the 6 mL water
that they will contain: “CO2”, “NO2” and “SO2”. You can use a 150-mL beaker to support the
test tubes.

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3. Using a clean metal scoop, place some solid NaHCO 3.in the tube labeled “NaHCO 3”. Add
enough NaHCO3 to fill the curved bottom end of the test tube.

4. Repeat the Step 3 procedure to add solid NaNO 2 and NaHSO3 to the other two appropriately
labeled test tubes. CAUTION: Avoid inhaling dust from these solids.

5. Fill the clean 250 mL beaker about half full with clean tap water.

6. Carefully unscrew the little plastic bottle on the pH sensor and carefully place it upright on the
lab bench so that the storage solution does not spill. The glass bulb at the end of the pH sensor
is very fragile, so be careful not to hit it with anything. Carefully slip the plastic bottle cap off
from the cylindrical wall of the pH sensor. Wash the pH sensor by squirting deionized water
from a wash bottle onto the shaft and around the bulb. A 600 mL beaker serves as a good
waste container to collect the wash water as it runs off the pH sensor. After washing, place the
pH sensor in the 250 mL half full beaker of clean tap water. Screw the lid on the plastic bottle
and place the 00 rubber stopper in the hole to prevent spilling the storage solution. Set this
plastic bottle, with lid on and rubber stopper in the hole, in a safe place to prevent spilling
until the end of the experiment, when you have finished with the pH sensor and will store it
for future use. Figure 1 shows the Vernier pH Sensor.

Figure 1 Vernier pH Sensor

7. Using a 10 mL graduated cylinder, measure 6.0 mL of clean tap water into the clean sample
vial labeled “CO2”.

8. With the pH sensor connected to CH1 on the side of the LabQuest 2 interface, calibrate the
pH meter using pH 7 and pH 4 buffers. Go to the “Experiment” tab on the menu and click on
“Calibrate”. Click “Calibrate Now”. Immerse the pH meter into the pH 7 buffer, enter 7.00,
and hit “Keep”. Do the same for the pH 4 calibration.

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 Figure 2 Vernier LabQuest 2

9. Prepare the computer for data collection by opening by clicking on “File” in the upper left
corner of the menu bar and select “open”. A screen appears with the vertical axis of the graph
scaled with pH from 0 to 10 pH units. The horizontal axis has time scaled from 0 to 100
seconds. Change the 100 seconds time duration to 1000 seconds, by going to the
“Experiment” tab on the menu and clicking on “Data Collection”. Change the time interval
for collection to 1000 seconds. Check to see that the input display at the lower right in the
meter window shows a pH value between 6 and 9 for the water.

10. Remove the pH sensor from the 250 mL beaker of tap water, and rinse it with deionized
water, allowing the rinse water to collect in the 600 mL beaker waste container. Transfer the
pH sensor to the sample vial (labeled “CO 2”) with the 6 mL of tap water. The pH sensor in the
sample vial is very unstable vertically and tips over, so place the sample vial, with pH sensor
inserted, into a 400 mL beaker to provide vertical stability. Very gently stir the pH sensor in
the 6 mL tap water in the sample vial. Note that in a minute or so the pH in the meter display
window is becoming somewhat constant.

11. Click on “Collect” and start collecting pH data on the tap water sample.

12. Using the 2 mL plastic dropper provided with the reagent bottle 1.0 M HCl, add about 1 mL
(1/2 full dropper, about 20 drops) of 1.0 M HCl to the test tube with the solid NaHCO 3. Try to
wash powder stuck on the walls of the test tube to the bottom as you add the 1.0 M HCl.
Fizzing is observed as carbon dioxide, CO 2, is generated in this tube. Squeeze the bulb of a
clean 2 mL plastic dropper and insert the tip and stem of the dropper into the test tube and
release the squeezing as the bulb end gets close to the open end of the test tube. Note that the
bulb of the 2 mL plastic dropper catches at the mouth of the test tube, preventing the dropper
from touching the solution at the bottom of the test tube and providing somewhat of a seal at
the open end of the test tube. The dropper must not touch the solution at the bottom of the test
tube. Very gently swirl the test tube that now contains NaHCO 3 and HCl and dropper. Place
the test tube with dropper in the 150-mL beaker, to prevent spillage.

13. With the 2 mL plastic dropper still inserted into the test tube, squeeze the bulb of the dropper
completely flat several times to completely fill the dropper with the CO 2 gas that is in the test
tube. You want to collect CO2 gas only in the dropper and not any of the solution.

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14. Without depressing the bulb. gently, quickly, remove the 2 mL plastic dropper from the test
tube, wipe the stem clean with tissue and insert the stem of the 2 mL dropper into the sample
vial with the pH sensor and 6 mL tap water. Push the plastic dropper into the sample vial
along the side wall of the pH sensor, using the stem (not the bulb) to push the tip of the
dropper through the tap water to the bottom of the sample vial.

15. Very slowly completely squeeze the bulb of the dropper so that the CO 2 gas slowly bubbles
through the tap water. Do this 8 to 10 times so that the tap water drawn up into the dropper is
repeatedly contacted with the residual CO2 gas in the dropper.

16. Hold the bulb on the plastic 2 mL dropper squeezed tightly as you withdraw the stem of the
dropper from the sample vial, so that no solution remains in the stopper. Very slowly, gently
stir the solution (tap water with gas bubbled through) in the glass sample vial with the pH
sensor. Look at the graph which has been monitoring the pH during Steps #9 through #14.
Observe the constant pH of the tap water only at the earlier times, the decrease in pH as the
CO2 gas was bubbled through and the falling value of the pH with the slow gentle stirring of
the solution. Continue to follow the falling pH with very gentle stirring until the pH becomes
constant (may be 6 to 8 minutes or more).

17. When the pH becomes constant, you may click on “Stop” to stop collecting data, if the 1000
second time has not already elapsed.

18. Record on your data sheet the best constant initial value of the pH of the tap water just before
you inserted the dropper with CO2 gas (initial pH value, before CO2 was added) and the best
constant final value for the pH after adding the CO 2 gas, followed with the gentle stirring
(final pH value after CO2 was added and pH stabilized). You will find using the “x=?” button
below the menu at the top of the screen is a good help in determining the pH values that you
must record from the constant regions on the graph. If you wish to examine these values
another way, click the Statistics button, and examine the minimum and maximum values in
the pH box displayed on the graph. Make certain that you have recorded the initial and final
pH values in your data table.

19. After recording your data, remove the pH sensor from the glass sample vial, rinse it with
deionized water (collecting the waste water in your 600 mL waste container) and return it to
the 250 mL beaker half full of tap water. Set aside the CO 2 labeled glass sample vial and
“NaHCO3” labeled test tube for washing later.

20. To gather data on sulfur dioxide, SO 2, start again like at Step #7, using the 10 mL graduated
cylinder to measure 6.0 mL of clean tap water into the clean sample vial labeled “SO 2”.

21. Repeat Steps similar to #10 through #19, with this time adding about 1 mL of 1.0 M HCl to
the test tube containing solid NaHSO 3, and appropriately using “NaHSO 3“ in place of
“NaHCO3 and “SO2“ in place of “CO2“. Of course, SO2 is generated in this test tube. Do not
breathe the SO2 gas.

22. To gather data on nitrogen dioxide, NO2, start again like at Step #7, using the 10 mL
graduated cylinder to measure 6.0 mL of clean tap water into the clean sample vial labeled
“NO2”.

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23. Repeat Steps similar to #10 through #19, with this time adding about 1 mL of 1.0 M HCl to
the test tube containing solid NaNO2, and appropriately using “NaNO2“ in place of “NaHCO3
and “NO2“ in place of “CO2“. Of course, NO2 is generated in this test tube. Do not breathe the
NO2 gas.

24. If time permits, repeat the entire experiment. Appropriately discard wastes to protect the
environment as you clean the test tubes and sample vials with tap water, followed by
deionized water rinse. Then start again with NaHCO 3 as in step #3.

25. To finish this experiment: Rinse the pH sensor with deionized water, unscrew the cap on the
plastic storage bottle, take out the 00 rubber stopper, slip the cap carefully onto the cylindrical
wall of the pH sensor (be careful of the glass bulb!) and then screw the plastic bottle with the
storage solution onto the pH sensor with cap so that the glass bulb is submersed in the storage
solution. Be sure the cap is screwed on tightly to prevent leakage of storage solution. If some
loss of storage solution has occurred so that the bulb cannot be submersed in the storage
solution, please take the sensor and bottle to the instructor for special handling. The pH sensor
is permanently damaged if it is not stored under the storage solution.

26. Appropriately discard wastes to protect the environment. Wash and rinse other glass apparatus
and return the special glass sampling vials.

DATA

Enter the sample data report form below in your notebook before coming to lab. During the
experiment, record all data (with proper units and number of significant digits) directly into
your notebook in ink. Show sample calculations for all calculated data for at least one trial if
multiple runs were made.

For repeated experiments:

95
CALCULATIONS AND DATA ANALYSIS

Show the following calculations and answer the questions in your notebook.

1. For each of the three gases, calculate the change in pH (∆pH), by subtracting the final pH from
the initial pH. Record these values in the Data and Calculations table.

2. In this experiment, which gas caused the smallest drop in pH?

3. Which gas (or gases) caused the largest drop in pH?

4. Coal from western states such as Montana and Wyoming is known to have a lower percentage
of sulfur impurities than coal found in the eastern United States. How would burning low-
sulfur coal lower the level of acidity in rainfall? Use specific information about gases and acids
to answer the question.

5. High temperatures in the automobile engine cause nitrogen and oxygen gases from the air to
combine to form nitrogen oxides. What two acids in acid rain result from the nitrogen oxides in
automobile exhaust?

96
6. Which gas and resulting acid in this experiment would cause rainfall in unpolluted air to have a
pH value less than 7 (sometimes as low as 5.6)?

7. Why would acidity levels usually be lower (pH higher) in actual rainfall than the acidity levels
you observed in this experiment? Rainfall in the United States generally has a pH between 4.5
and 6.0.

Assignment

1. How many gallons of gas do you use per year?

I put ______(x)_ gallons of gas every _______(y)__ days. 365x/y = ______ gallons per year.

Convert from gallons to mL to determine mL/year. (1 gallon = 3.785 L)

2. Follow the steps to calculate how much CO2 results in one year in moles, kg, L, and classrooms
from your personal gas consumption.

97
a. Assume gasoline is C8H18. Write a balanced equation for the combustion reaction of gasoline in
air.

b. Determine moles of CO2 from your mL of gasoline in #1 using the balanced equation.
(dC C = 0.75g mL)
8 18

c. Determine kg of CO2 from b.

d. Determine Volume (in L) using PV = nRT (assume 20oC and 0.75 atm).

e. Determine the number of classrooms this volume of CO 2 would completely fill (assume 1200
sq.ft. x 10ft room).

98
3. The US uses about 21 million barrels of oil per day. The world used about 86 million barrels of
oil per day. Calculate how many kg and L of CO 2 are produced in the world each day from
gasoline. (Neglect all natural gas, coal and biofuels burned and any energy used to process long
chains into shorter chain hydrocarbons) (1 barrel = 42 gallons).

Activity 4.2
Global Warming Issues and Effects
You have seen the movie “An Inconvenient Truth”. Now you are asked to research on the
Internet and develop an understanding of the probable causes for the current apparent heating the
earth’s atmosphere and climatic changes.

99
Greenhouse Gases and Global Warming

Objectives
• Explore some of the factors influencing the debate about global warming and the greenhouse
effect
• Apply principles learned in Chemistry 101 to a current environmental controversy. Including:
a. Insights into the interaction of radiation with matter and how this affects the earth’s
climate
b. Explore how humans might contribute to the greenhouse effect
c. Investigate how infrared spectroscopy is used to identify certain atmospheric Gases

Background:

The temperature of the Earth’s surface is controlled by many different factors. One of these is the
radiation absorption by gases in the atmosphere, referred to as the Greenhouse Effect. One of the
primary energy inputs is direct radiation from the sun. Much of this radiation lies in the visible
region of the spectrum. The atmosphere does not absorb most of this radiation and it strikes the
ground or ocean surface where some of it is absorbed and some is reflected back into space. The
absorbed radiation warms the surface. Warm objects radiate energy in the infrared region of the
spectrum. If gases in the atmosphere absorb this infrared energy, it does not get back out into
space. Thus the atmosphere acts like a blanket, or a greenhouse, making the surface warmer. The
atmospheric blanket moderates the surface temperature and prevents extreme changes between
high daytime temperatures and frigid nighttime ones. The gas most frequently cited as important
in the greenhouse effect is CO2. The CO2 concentration in the atmosphere has increased from the
burning of fuels. There is concern that this CO 2 increase is leading to a warming of the climate,
which might result in a variety of serious effects. In this experiment we will study CO 2 and look
at some aspects of its contribution to the greenhouse effect.
Changes in the vibrational and rotational motions of polyatomic molecules are the main results of
the absorption of heat by gases. The direct absorption of infrared radiation occurs only if there is
a change in the dipole moment of the molecule. An n-atom molecule (where n is the # of atoms)
may be described as having 3n – 6 vibrational motions, or vibrational modes as they are called
(3n – 5 for linear molecules). Changing dipole moments for any of these vibrational modes result
in that mode absorbing infrared radiation. The absorption bands in the infrared spectrum are
related to these vibrational modes. Using the 3n-6 formula, water has 3 vibrational modes, as
shown below:

Consider the dipole moment as the molecule undergoes each of these motions. Does it change? If
so, the vibration will result in an absorption in the infrared region. Infrared absorption frequencies

100
for several atmospheric gases are given in Table I. Note that wavelength (in μ) =10,000/ cm -1
Table I: Principal IR Absorptions for Various Atmospheric Gases

Assignment (Laboratory Discussion)

1. Research and describe in your own words the effects of Greenhouse Gases, and why they
are heating the earth over time. [hint: see… http://www.ucar.edu/learn/1_3_1.htm]

101
2. What are the relative average atmospheric abundances for the most important
contributors to heating the atmosphere? What is a pollutant and explain the difference between a
primary and secondary pollutant. [hint: see sites like…
http://www.ace.mmu.ac.uk/eae/Global_Warming/Older/Concentrations.html], and their rate of
change. [http://www.mindfully.org/Air/2006/UN-Greenhouse-Gas3nov06.htm]

3. From the identified pollutants, distinguish between anthropogenic, biogenic, and

geogenic sources.

4. Research and list what are the relative global warming potential effects for each of the
gases that you have listed in 2.[http://www.eia.doe.gov/oiaf/1605/gwp.html]

a. Research and explain using blackbody radiation curves, why these gases have the
potential to warm the earth.

b. Based upon your research and the film that you saw, list what actions we as Americans
must undertake to prevent future potentially catastrophic results from Global Warming.
What are the current efforts that the USA government is undertaking to control
greenhouse gases? (You might want to visit the EPA climate change website)

c. Explain in your own words what does carbon sequestration means and implies.

A place to start might be these websites:

(US EPA site)
http://yosemite.epa.gov/oar/globalwarming.nsf/content/impacts.html

(USGS site)
http://www.nrmsc.usgs.gov/research/global.htm

(NASA site)
http://earthobservatory.nasa.gov/Study/WaterVapor/water_vapor.html

(California site)
http://climatechange.ca.gov/

(NRDC Site)
http://www.nrdc.org/globalWarming/f101.asp

(Pew Center)
http://www.pewclimate.org/global-warming-basics/

And many, many more sites can be found with a Google search. In addition, here is an interesting
website that will allow you to estimate your own Carbon Footprint.
http://www.bp.com/extendedsectiongenericarticle.do?categoryId=9008204&contentId=7 015209

102
Additional Practice Exercises

1. You are traveling to London in October and you found out that temperature at that time of the
year is usually around 15 °C, which is different than the usual 75 °F in Southern California
during that time of the year. Compare these two temperatures using the Kelvin (K) scale?

2. Some athletes have as little as 3% percent body fat. If such a person has a body mass of 45 kg,
how much body fat does that person have?

3. If body fat has a density of 0.94 mg/L and 3.0 L of fat are removed in a liposuction, how many
pounds of fat were removed from the patient?

103
4. What is a cholesterol level of 0.00185 kg/L in the standard units of mg/dL?

5. An object has a mass of 11.2 oz. When it is submerged into a graduate cylinder initially
containing 27.82 mL of water, the water level rises to 0.07778 L. What is the density (g/mL) of
the object? (16 oz = 1 lb)

104
Activity 4.3
Determination of Dissolved Oxygen

Objective:
The aim of the experiment is to determine the quantity of dissolved oxygen present in the given
sample(s) by using modified Winkler’s (Azide modification) method.

Principle
Dissolved Oxygen (D.O.) levels in natural and wastewaters are dependent on the physical,
chemical and biochemical activities prevailing in the water body. The analysis of D.O. is a key
test in water pollution control activities and waste treatment process control.
Improved by various techniques and equipment and aided by instrumentation, the Winkler (or
iodometric) test remains the most precise and reliable titrimetric procedure for D.O. analysis. The
test is based on the addition of divalent manganese solution, followed by strong alkali to the water
sample in a glass-stoppered bottle. D.O. present in the sample rapidly oxidizes in equivalent
amount of the dispersed divalent manganous hydroxide precipitate to hydroxides of higher
valency states. In the presence of iodide ions and upon acidification, the oxidized manganese
reverts to the divalent state, with the liberation of iodine equivalent to the original D.O. content in
the sample. The iodine is then titrated with a standard solution of thiosulphate. The following
reactions are involved:

MnSO4 + 2KOH → Mn(OH)2 + K2SO4

2Mn (OH)2 + O2 → 2MnO(OH)2

(DO) Basic manganic oxide (brown ppt)

2MnO (OH)2 + H2SO4 → MnSO4 + H2O + [O]

(Nascent oxygen)

2KI + H2SO4 + [O] → K2SO4 + H2O + I2

I2 + 2Na2S2O3 → 2NaI + Na2S4O6

Sodium Sodium
thiosulphate tetrathionate

Apparatus
1. 300 mL capacity bottle with stopper

105
2. Burette 3. Pipettes, etc.

Reagents
1. Manganous sulphate solution (MnSO HO4 4 2 )
2. Alkali-iodide azide reagent
3. Conc. sulphuric acid (36 N)
4. Starch indicator
5. Standard sodium thiosulphate solution (0.025N)
6. Standard potassium dichromate solution (0.025N)

Procedure

1. Add 2 mL of manganous sulphate solution and 2 mL of alkali-iodide azide reagent to the 300
mL sample taken in the bottle, well below the surface of the liquid.
(The pipette should be dipped inside the sample while adding the above two reagents.)

2. Stopper with care to exclude air bubbles and mix by inverting the bottle at least 15 times.

3. When the precipitate settles, leaving a clear supernatant above the manganese hydroxide floc,
shake again.

4. After 2 minutes of settling, carefully remove the stopper, immediately add 3 mL concentrated
sulfuric acid by allowing the acid to run down the neck of the bottle.

5. Restopper and mix by gentle inversion until dissolution is complete.

6. Measure out 203 mL of the solution from the bottle to an Erlenmeyer flask. As 2 mL each of
manganese sulphate and azide reagent have been added, the proportionate quantity of yellow
solution corresponds to 200 mL of sample is

= =203ml

7. Titrate with 0.025 N sodium thiosulphate solution to a pale straw colour.

8. Add 1–2 mL starch solution and continue the titration to the first disappearance of the blue
color and note down the volume of sodium thiosulphate solution added (V), which gives
directly the D.O. in mg/L.

Observation
Sample × Standard sodium thiosulphate solution (0.025N) (Starch indicator)

106
General calculation

Volume of hypo solution used in titration = V mL

Normality of hypo solution (sodium thiosulphate) = 0.025 N

Applying normality equation

N1V1 (water) = N2V2 (Hypo)

N1 × 200 = (0.025) × V

N1 = 𝑉
8000

Strength of dissolved oxygen = Normality × Equivalent wt of oxyen

= 𝑉
x 8 g L-1 = 𝑉 x 8 x 1000 mg L-1 = 1 V ppm
8000 8000

Result: The amount of dissolved oxygen in water sample is ….ppm

107
Name________________________________ Course & Yr_________________Date _________

Analyze and Conclude

1. Observing and Inferring Most of the critical conditions related to dissolved oxygen deficiency
occur during summer months. Why?
______________________________________________________________________________

______________________________________________________________________________

______________________________________________________________________________

2. Thinking Critically Why do we use 0.025 N sodium thiosulphate solution for the titration?
______________________________________________________________________________

______________________________________________________________________________

______________________________________________________________________________

3. Discussion Discuss the environmental significance of dissolved oxygen.

______________________________________________________________________________

______________________________________________________________________________

______________________________________________________________________________

108
______________________________________________________________________________

______________________________________________________________________________

______________________________________________________________________________

______________________________________________________________________________

______________________________________________________________________________

4. Drawing a Conclusion The turbulence of water should be encouraged. Why?

______________________________________________________________________________

______________________________________________________________________________

______________________________________________________________________________

______________________________________________________________________________

5. Draw the oxygen saturation curve.

109
6. Error Analysis What are some sources of error in this activity?
______________________________________________________________________________

______________________________________________________________________________

______________________________________________________________________________

Activity 4.3
Growth of Algae as a Function of Nitrogen
Concentration
Freshwater comes from many sources, including lakes, rivers, and municipal reservoirs.
However, daily activities of life often leave these water sources polluted and unfit for personal
consumption or use in industry.
Nitrogen and phosphorus compounds are among the most common pollutants. They contribute to
pollution by causing algae and bacteria in the water to reproduce rapidly. When these organisms
die, the decomposition process depletes oxygen in the water, killing fish and other aquatic life. In
this lab, you will investigate the effect of nitrates on algae.

Objectives
• Determine how the level of nitrogen affects algal growth.
• Identify how much nitrogen is present in water, using algal growth as an indicator.

Materials
algae culture light source
stock solutions of aluminum foil
0.3M NaNO3, test-tube rack
0.6M NaNO3, dropper
0.9M NaNO3 china marker

110
unknown NaNO3 solution 10-mL graduated cylinder
distilled water
15-mm x 150-mm test tubes (5)

Pre-Lab
1. What are sources of nitrogen and phosphorus pollution in Earth’s freshwater?
2. Why is light needed for algal growth?
3. Read the entire laboratory activity. Hypothesize why the growth of algae may indicate the
concentration of nitrogen pollutants in water. Record your hypothesis.

Procedure

1. Using a china marker, label five test tubes as follows and place them in the test-tube rack.
Label test tube 1, Unknown; test tube 2, 0.0M NaNO3; test tube 3, 0.3M NaNO3; test tube 4,
0.6M NaNO3; and test tube 5, 0.9M NaNO3.

2. Add 10 mL of unknown solution, supplied by your teacher, to test tube 1.

3. Add 10 mL of distilled water to test tube 2.

4. Add 10 mL of the appropriate NaNO3 stock solution to each of test tubes 2, 3, and 4.

5. Place 10 drops of algal culture into each test tube, and cover the open end of all test tubes with
a small piece of aluminum foil.

6. Record the appearance of each test tube in Data Table 1.

7. Place the test tubes under the light source as your teacher directs.

8. Check each test tube daily for 10 days, and record the appearance of each test tube in Data
Table 1.

111
Name________________________________ Course & Yr_________________Date _________

Data and Observations

112
Analyze and Conclude

1. Observing and Inferring What happened in each test tube over the course of the 10 days?
______________________________________________________________________________

______________________________________________________________________________

______________________________________________________________________________

113
2. Comparing and Contrasting What was the difference in sodium nitrate concentration among
test tubes 2–5?
______________________________________________________________________________

______________________________________________________________________________

______________________________________________________________________________

3. Drawing a Conclusion What can you conclude about the amount of algal growth and the nitrate
concentration in test tubes 2–5?
______________________________________________________________________________

______________________________________________________________________________

______________________________________________________________________________

4. Drawing a Conclusion What can you conclude about the amount of pollution, in the form of
NaNO3, that was present in the Unknown, test tube 1? Explain.
______________________________________________________________________________

______________________________________________________________________________

______________________________________________________________________________

5. Predicting What would you predict to be the immediate response of algal growth if the amount
of pollutants was allowed to keep increasing?

_____________________________________________________________________________

_____________________________________________________________________________

_____________________________________________________________________________

6. Recognizing Cause and Effect Why do nitrates increase growth of algae?

_____________________________________________________________________________

_____________________________________________________________________________

_____________________________________________________________________________
7. Error Analysis What could be done to improve the precision and accuracy of your
investigation?___________________________________________________________________

______________________________________________________________________________

______________________________________________________________________________

114
Assignment:

1. Why is it not possible to completely eliminate algae blooms from the water supply?

2. In ponds where there are viable fish and plant populations, algae are seldom seen. Explain why
this might happen.

3. People who have backyard ponds often keep snails and tadpoles in the ponds. Explain the
purpose of these organisms.

References

Askeland, D. R., Fulay, P.P., and Wright, W. J. (2010). The Science and Engineering of
Materials, Sixth Edition. Stamford, CT:Cengage Learning, Inc.

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Callister, W. D. (2007). Materials science and engineering: an introduction (7 th Edition). New
York, NY: John Wiley & Sons, Inc.

Callister, W. D.(2001). Fundamentals of materials science and engineering: an interactive e

• text (5th Edition). New York, NY: John Wiley & Sons, Inc.

Chemistry: Matter and Change Laboratory Manual Student Edition. Glencoe/McGraw-Hill 8787
Orion Place Columbus, OH 43240-4027

General Chemistry Laboratory Manual (2015). California State University, Sacramento

M.S. & Armando Rivera, Ph.D. General Chemistry 101 Laboratory Manual Khuu,
A. & Rivera, A. General Chemistry 101 Laboratory Manual

Santhi, G. and Saravanan, R. Engineering Chemistry Laboratory Manual -1. Department of

Chemistry, CMS College of Engineering and Technology, Appachigoundanpathy, Coimbatore.

Las Positas College Chemistry Faculty and Staff (2012). Las Positas College Chemistry 1A Lab
Manual Fall AB

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