Chemistry 1 and 2 WRITE SHOP

K-12 SENIOR HIGH INDUSTRY LINKAGE REPLICATION PROJECT
K-12 SENIOR HIGH

INDUSTRY LINKAGE
REPLICATION PROJECT
for Grade 11 and 12 (STEM)
A Compilation of Activities and Experiments

for Grade 11 and 12 Students (STEM)
of
ICCP GROUP FOUNDATION, INC. MARJORIE B. REGALADO-TEACHER III

2
MARJORIE B. REGALADO
Teacher III
CABUYAO NATIONAL HIGH SCHOOL
A project of ICCP Group Foundation

“K-12 Senior High Industry Linkage Replication Project”
Noted:
MARIBETH G. HERRERO TEODORA M. GALANG

Head Teacher III Master Teacher I
Senior High School Coordinator Senior High School Coordinator
DR. JUANITO Y. DE RAMOS

Principal III
Cabuyao Nationa High School
Material contained in this publication is compiled from electronic sources.

Credits ar due to the authors.

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Table of Contents

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Grade: 11
Semester: 1st
and 2nd
Subject Title:
General Chemistry
1&2
LEARNING COMPETENCY
Determine the density of liquids & solids. (STEM_GC11MT-Ib-14)
CONTEXTUALIZED LEARNING COMPETENCY

Determine the density of liquid used in the semiconductor industry.
DENSITY
Key Concepts
• Density is a measure of how tightly packed and how heavy the molecules are in an

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object.
• Defined as mass per unit volume.
Equation: Density = mass
m
or D= volume
• A measure of the amount of mass in a V
certain volume.
• This physical property is often used to identify and classify substances.
• It is usually expressed in grams per cubic centimeters, or g/cm3.
• The density of a liquid determines whether it will float on or sink in another liquid.
• A liquid will float if it is less dense than the liquid it is placed in.
• A liquid will sink if it is more dense than the liquid it is placed in.
Things to be done!
Students will observe three industrial liquids stacked on each other and conclude that
their densities must be different. They will predict the relative densities of the liquids and
then measure their volume and mass to see if their calculations match their observations
and predictions.
Objective
Students will be able to determine whether a liquid will sink or float in water by
comparing its density to the density of water.
Safety
Wear properly fitting goggles. When using isopropyl alcohol, read and follow all
warnings on the label. Isopropyl alcohol is flammable. Keep it away from any flames or
spark sources. Wash hands after the activity.
Materials for Each Group
• Balance
• Isopropyl alcohol, 70% or higher
• Water
• Graduated cylinder
• 2 identical tall clear plastic cups
• 2 tea light candles
Notes about the Materials
Isopropyl alcohol
The demonstrations and activity work best with 91% isopropyl alcohol solution, which is
available in many grocery stores and pharmacies. If you can’t find 91% solution, 70%

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will work, but make sure your candle will not sink in it.
ENGAGE
1. Show that different liquids have different densities.
Activity Sheet
Density: Sinking and Floating Liquids
Materials
• Balance
• Water
• 2 identical tall clear plastic cups
• 2 tea light candles
Procedure
Part 1
Demonstrate the density of two liquids with sinking
and floating
www.middleschoolchemistry.com
1. Use a graduated cylinder to measure 50 mL of water and pour it into a clear plastic
cup.
2. Measure 50 mL of isopropyl alcohol and pour it into another identical clear plastic cup.
3. Place a tea light candle in a cup with water and another tea light candle in a cup with
alcohol.
4. Observe what will happen to the candle.
Q1. Do water and alcohol have the same or different densities?

Q2. Which liquid is more dense?
Q3. How do you know?
Part 2
Demonstrate the density of two liquids by
comparing the mass of equal volumes
5. Remove the candles from each liquid and tell
students that each cup contains the same volume
of liquid.
6. Carefully place the cups of water and alcohol

on opposite ends of a balance.
www.middleschoolchemistry.com
Q4. Explain how this demonstration proves that water is more dense than alcohol. Be

7
sure to mention both volume and mass.
EXPLORE
2. Demonstrate that liquids can float or sink in other liquids by making a density column
with water, oil, and alcohol.
Materials
• Water
• Vegetable oil
Note: If you would like the liquids to be more visible, add 1

drop of food coloring to the water and another drop of a
different color to the alcohol.
Procedure
7. Pour about 15 mL of water into the graduated cylinder.
Gradually add about 15 mL of oil. Then slowly pour about 15
mL of alcohol on top. The liquids should form layers in the
graduated cylinder.
8. The layered liquids in the graduated cylinder and point out
that the alcohol floats on the oil while the water sinks.
9. Draw your observation. www.middleschoolchemistry.com
Q5. Why does the alcohol float on the oil?

Q6. Why does the water sink in the oil?
ACTIVITY
Question to investigate
Why does water sink in oil, and alcohol float in oil?
Materials for each group

• Water
• Vegetable oil
• Isopropyl alcohol
• Balance that measures in grams
Procedure
1. Find the mass of an empty graduated cylinder. Record the mass
in grams in the chart on the activity sheet.
2. Pour 20 mL of water into the graduated cylinder. Try to be as
accurate as possible by checking that the meniscus is right at the
20-mL mark.
3. Weigh the graduated cylinder with the water in it. Record the

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mass in grams.
4. Find the mass of only the water by subtracting the mass of the empty graduated
cylinder. Record the mass of 20 mL of water in the chart.
5. Use the mass and volume of the water to calculate density. Record the density in g/cm3
in the chart.
6. Follow steps 2–5 for alcohol and then oil. Be sure to measure the oil last because it
does not rinse easily from the graduated cylinder.
Water Alcohol Oil

Mass of graduated cylinder + liquid (g)
Mass of empty graduated cylinder (g)
Mass of liquid (g)
Density of liquid (g/cm3 )
1. How do the densities you calculated explain why water sinks in oil and alcohol floats
on oil?
2. Look at the layered liquids in the illustration. Write most, least, or in-between in the
chart below to describe the density of each liquid.
EXPLAIN
3. Compare the density of water, alcohol, and oil on the molecular level.
Alcohol Oil Water

Atoms mostly carbon and carbon and hydrogen oxygen and hydrogen
hydrogen
and oxygen
Mass of Atoms Oxygen is heavier and smaller
than carbon
Density less dense than oil more dense than oil
Arrangement of alcohol molecules do water molecules are very
atoms not pack very tightly attracted to each other and pack
together very close together

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EXPLAIN IT WITH ATOMS & MOLECULES
Water molecules are smaller and have less mass than alcohol and oil molecules. Explain
why water is more dense than alcohol and oil.
Extend
Try this!
Liquid Layers
Imagine that the liquids on the right have the following densities:
15g/cm3 10g/cm3
3
3g/cm 9g/cm3
7g/cm3 12g/cm3
Match the colors to the correct densities by writing the corresponding densities beside the
colored liquid.
Review
1. What is the formula for density?
2. What happens if you pour together liquids that have different densities?
3. Will the liquid on the top have the highest or lowest density?
4. Will the liquid on the bottom have the highest or lowest density?
EXTRA EXTEND
Chemical Used in Semiconductor Industry
Introduction
Liquid chemicals are use in the semiconductors industry in many

applications such as the manufacture of microchips and the growth of
crystals.
The production requirements of this High Tech industry impose the

massive setting up of clean rooms for the various processes of
manufacture and treatments including chemical ones.
Wet chemistry is one of the most important technological stages in

the realization of electronic devices.
Semiconductors chemistry is mainly organized around the chemical

treatment by solvents and acido-basic attacks of semiconductors.
Chemistry of solvents : the main chemicals used during this stage are
trichloroethylene, acetone, isopropanol and also other alcohols such
as denatured ethanol.

10
1
The typical applications are the cleaning, the degreasing of the semiconductors and the shrinkage of
residual resins (acetone).
2
Chemistry of acids and bases : the acid chemical agents used can be sulphuric acid, nitric acid,
orthophosphoric acid, hydrochloric acid,hydrobromic acid or even citric acid.
3
Solutions prepared associate sometimes a base (to oxidize the semiconductor) to an acid (to attack this
oxide): hydrogen peroxide, ammonium hydroxide, sodium hydroxide or potasium hydroxide (mainly
used for the attack of silicon).
Activity
Solve the following problems.
1. Trichloroethylene
Liquid trichloroethylene evaporates quickly into the air.
It is nonflammable and has a sweet odor. The two major
uses of trichloroethylene are as a solvent to remove
grease from metal parts and as a chemical that is used to
make other chemicals, especially the refrigerant. To
determine the density of trychloroethylene a flask is foist
weighed empty (108.6g). It is then filled with 125ml of
the trichloroethylene to give a total mass of 291.4g.
What is the density of trichloroethylene in grams per
milliliter?
Solution:
2. Acetone
1. What is the mass of a flask filled with acetone
(d = 0.792 g/cm3) if the same flask filled with
water (d = 1.000 g/cm3) weighs 75.20 gram? The
empty flask weighs 49.74 g.
Solution:

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3. Isopropanol/Isopropyl alcohol
Isopropyl alcohol ( rubbing alcohol) has a density
of 0.785 g/ mL. What is the mass of 3.75 L of
isopropyl alcohol? What volume would 125 g of
isopropyl alcohol occupy?
Solution:
Isopropyl alcohol (IPA) is one of the most

commonly used organic solvents in the
semiconductor industry. Silicon wafers are dried
after surface cleaning in the manufacturing
process and IPA is frequently used during the
drying step. The purity of IPA used is critical
since these materials come in direct contact with
the silicon wafers and any contaminants present at
this stage could be detrimental to the overall
performance of the final product.
4. sulfuric acid
Calculate the density of sulfuric acid if Sulfuric acid is a strong drain cleaner and can be found in
35.4 mL of the acid weighs 65.14 g.
Solution:

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5. nitric acid
You measure out 5.00 mL of concentrated nitric
acid, HNO3. It weighs 7.10 g. What is the density
of concentrated nitric acid? [Note. This refers to
common lab “concentrated nitric acid”, which is
about 70% (w/w) HNO3.]

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Metal Etching
Solution:
Take it Further More

By Group
Make an interview or research on how your knowledge in density of liquids can be used in
semiconductor industry. Make a powerpoint presentation/demonstration of your report.
Para sa bayan!
RUBRICS FOR ASSESSMENT
Problem Solving
Criteria Points
5 4 3 2 1
Answer With 5 With 4 With 3 With 2 With 1 correct
correct correct correct with correct answer with
answer with answer with answer answer with correct units.
correct correct correct correct units.
units. units. units.
Part With 5 Whith 4 With 3 With 2 With 1 solution
solution solution solution solution
Neatness No erasure With 1-2 With 3-5 With 6-10 With more than
erasures. erasures. erasures 10 erasures.
Activity
Criteria Points
5 4 3 2 1
Procedure All the Only 1 2-3 4-5 procedures 6 and
proceduresh procedure is procedures are missing above
as been missing are missing produre
done are
missing
Timeliness Submitted Submitted Submitted the Submitted the Submitted
the result on the result 1- result 6-10 result 11-15 the result

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the time 5 minutes minutes late minutes late more than

late 15
minutes
late
Neatness No erasure With 1-2 With 3-5 With 6-10 With more
erasures. erasures. erasures than 10
erasures.
Student Powerpoint Presentation Rubric

Criteria
4- Exceeds 3- Meets Standard 2- Approach 1-Below Points
Standards Standards Standards
Oral Students are Students are faily Students are Students do not
Presentation well prepared. prepared. Volume is somewhat seem prepared.
Volume is loud loud enough. prepared. Volume is too
enough. Establish eye Volume is loud soft to be
Establish eye contact most of the enough. heard.
contact always. time. Team Establish eye Establish no
Team cooperation most of contact eye contact.
cooperation the time smooth. sometimes. Partners do not
always smooth. Team seem
cooperation cooperation.
sometimes
smooth.
Content All content on Most of the content There are Content is
Accuracy slides is is accurate. There many confusing on
accurate. are 1 to 2 factual inaccuracies in many of the
errors. the content slides.
Use of All slides have At least 5 of the Some of the Many of the
Graphics graphics to slides have graphics slides have slides have no
support all the to support all graphics but graphics.
information. information. don’t support
the
information.
Text-Font Font formats FonWednesday, Font formats Font formats
Choice and (e.g. Color and June 6, 2018t (e.g. Color and (e.g. Color and
Formatting style have been formats (e.g. Color style have been style have not
carefully and style have been carefully been carefully
planned to carefully planned to planned to planned to
enhance the enhance the enhance the enhance the
redability and readability and readability and readability and
content on all content on at least 4 content on at content on the
slides. of the slides. least 3 of the slides.
slides.

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Spelling and Project has no Project has between Project has Project has
Capitalization misspellings 1-2 misspellings between 3-4 more than 4
and/or and/or capitalization misspellings misspellings
capitalization errors on all slides. and/or and/or
errors on all capitalization capitalization
slides. errors on all errors on all
slides. slides.
http://www.slideshare.net/msedaghatian1/power-point-presentation-rubric-4088342

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Grade: 11
Semester: 1st
and 2nd
Subject Title:
General Chemistry
1&2
LEARNING COMPETENCY
Describe evidences that a chemical reaction has occurred. (STEM_GC11CR-If-g-36)
CONTEXTUALIZED LEARNING COMPETENCY

Describe evidences that a chemical reaction usually occured in industry.
Topic: Chemical Reactions and Chemical Equations in Industry

Sub-Topic: Industry Depends on Chemical Reaction
BEFORE, you learned

• Chemical reactions turn reactants into products by rearranging atoms
• Mass is conserved during chemical reactions
• Chemical reactions involve energy changes
NOW, you will learn

• How chemistry has helped the development of new technology
Introduction
Chemical Industry Processes and Chemical Reactions
Chemical processes are used in the chemical industry to transform raw materials into more specialized
products. The place where chemical products are produced is usually called chemical plant. The
chemical industry relies on the knowledge and investigation of the chemical properties of different
materials.
Chemistry is the study of the matter and the transformations of it. While
physics study matter from a more fundamental point of view, chemistry
focuses on its composition, behavior, reactions, structure and properties.
The study of the chemical reactions that affect matter gave humans the
possibility to turn useless materials into more valuable and useful
materials, through chemical transformations. Chemistry focuses on atoms,
molecules, substances, crystals and other kind of aggregates.
A chemical process is a method in which one or more chemicals or

chemical compounds are changed in some way. Let’s remember that a
chemical is a substance with a constant chemical composition and
characteristic properties, that cannot be separated into components by
physical separation methods, and without breaking chemical bonds.

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The basic reactions used in the chemical industry are: Oxidation, Reduction, Hydrogenation,
Dehydrogenation, Hydrolysis, Hydration reaction, Dehydration, Halogenation, Nitrification,
Sulfonation, Ammoniation, Alkaline fusion, Alkylation, Dealkylation, Esterification, Polymerization,
Polycondensation and Catalysis.
Activity
Directions: Write the proper coefficient to

balance the following chemical reactions.
1. Synthesis of ammonia.
Reaction: H2(g) + N2(g)  → NH3(g)
Hydrogen gas and nitrogen gas are combined in the presence of a catalyst at high temperature and
pressure to produce ammonia gas
Significance: Synthesis of ammonia leads to the

production of fertilizer (ammonium nitrate) and to
the production of ammunitions.
2. Combustion of hydrogen / Electrolysis of water

Reaction: H2(g) + O2(g)  → H2O(l)
Hydrogen gas and oxygen combine to produce liquid water.

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Significance: In the forward direction this is a

spontaneous reaction that explosively oxidized
hydrogen to water. It has a high activation energy
but once started it is very exothermic. Hydrogen is
a fuel. In the reverse direction this reaction is non-
spontaneous. Electricity can be used to "split"
water into hydrogen and oxygen. This is the basis
of the fuel cells in the hydrogen powered vehicle.
3. Combustion of methane (hydrocarbons)
Reaction: CH4(g) + O2(g) →
Methane gas and oxygen gas combine exothermically to produce carbon dioxide gas and water vapor.
Significance: Methane is the simplest of the hydrocarbons, all of which combine with oxygen and
undergo oxidation. If the oxidation is complete the products are carbon dioxide (a greenhouse gas) and
water. Incomplete combustion will produce carbon monoxide and carbon (soot). Methane is obtained
from underground and is from the decomposition of prehistoric plants and other organic matter. Fossil
fuels are burned (oxidized) to produce heat and provide energy for many machines and for cooking
and heating. There are serious concerns currently about the rapid increase of carbon dioxide in our
atmosphere.

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4. Wet Oxidation
Reaction: Pyrophoric and high pressure:
Si + O2 + H2 → SiO2 + H2O
Flash and bubbler:

Si + H2O → SiO2 + H2
Four methods of introducing water vapour are commonly used when water is the
oxidizing agent—pyrophoric, high-pressure, bubbler and flash.
Pyrophoric oxidation involves
the introduction and combustion
of a hydrogen/oxygen gas
mixture. Such systems are
generally called burnt hydrogen
or torch systems. Water vapour is
produced when proper amounts
of hydrogen and oxygen are
introduced at the inlet end of the
tube and allowed to react. The
mixture must be controlled
precisely to guarantee proper
combustion and prevent the
accumulation of explosive
hydrogen gas.
5. Synthesis of sulfuric acid
Reaction: S(s) + O2(g) + H2O(l) → H2SO4(aq)
Sulfur is first oxidized to sulfur dioxide and then to sulfur trioxide. This gas is bubbled through water
to produce sulfuric acid. There are other methods to synthesize this substance.

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Significance: Sulfuric acid is a very important

chemical and an indicator of a nation's industrial
strength. World production in 2004 was about 180
million tonnes. Most of this amount (~60%) is
consumed for fertilizers, particularly
superphosphates, ammonium phosphate and
ammonium sulfates. Sulfuric acid is needed to
dissolve very insoluble phosphate ores.
6. Equilibrium of carbonic acid and carbon dioxide gas.
Reaction: H2CO3(aq) → CO2(g) + H2O(l)
Carbonic acid breaks down to produce carbon dioxide gas and liquid water.
Significance: Carbon dioxide dissolves in water to
an extent determined by temperature and pressure.
When this occurs carbonic acid is formed which
lowers the pH of the water. Soda pop is a
carbonated drink - the acid counterbalances the
added sugars and gives the drink its fizzy quality.
As more carbon dioxide builds up in our
atmosphere the pH of the ocean is decreasing and
the ocean "sinks" this carbon dioxide (dissolves
it).
7. Biological formation of calcium carbonate.

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Reaction: Ca2+(aq) + CO3 2- (aq)  → CaCO3(s)
Calcium ions combine with carbonate ions to produce insoluble calcium carbonate.
Significance: Many sea creatures produce shells.
Birds and reptiles produce eggs with shells. All of
these shells are composed of calcium carbonate.
Over time these shells collect, are buried, and
produce limestone. If limestone is subjected to
heat and pressure it may undergo metamorphoses
into marble.
8. Rusting of iron.
Reaction: Fe(s) + O2(g)  → Fe2O3(s)
Iron metal combines with oxygen gas to produce iron (III) oxide.
Significance: Iron is the main ingredient of steel,
an alloy used in many structures. As oxygen
attacks iron it converts it to one of its oxides, iron
(III) oxide as shown here or iron(II) oxide or
some combination of the two. Rust varies in color
from red to yellow but it should be noted that it
does not stick to iron. It flakes off continuously
exposing more iron to oxygen. Finding ways to
stop iron from rusting has led to longer lasting
structures.
9. Production of hydrogen from the action of acid on metal.
Reaction: Zn + H2SO4(aq)  → H2(g) + ZnSO4(aq)
Zinc combined with sulfuric acid produces hydrogen gas and soluble zinc sulfate.

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Significance: One way of synthesizing some

hydrogen gas for use in the laboratory is to
liberate it from an acid using an active metal. Zinc
works well for this purpose.
10. Oxidation of alcohol.
Reaction: CH3CH2OH(l) + O2(g)  → CH3COOH(aq) + H2O(l)
Ethyl alcohol and oxygen produce acetic acid and water.

Significance: Wine becomes sour with age and
exposure to the air. This is due to the conversion
of alcohol to acetic acid (vinegar).

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SENIOR
HIGH
SCHOOL –
SCIENCE,
TECHNOLOGY, ENGINEERING AND MATHEMATICS (STEM) SPECIALIZED
SUBJECT
Grade: 11 Subject Title: General Chemistry 1 and 2
Learning Competency:
1. Determine the density of liquids & solids. STEM_GC11MT-Ib-14
Contextualized Learning Competency

1. Explain and describe the purpose and importance of calibration.
2. Explain and describe the methods of calibration.
3. Explain and describe the standards of calibration.
4. Explain and describe the purpose and imporatnce of calibration.
5. Graphing using EXCEL.
6. Work effectively in a work team.
Calibration of Volumetric Glassware

In this laboratory exercise, we will calibrate the three types of
glassware typically used by an analytical chemist; a volumetric flask,

24
a volumetric pipet and a buret. Over the course of this semester, we will use these tools extensively
when performing Gravimetric and Titrimetric Analyses. In order to avoid introducing Systematic
Errors into our measurements, each of these instruments must be properly calibrated. And, to reduce
the Random Errors inherent when using these instruments, their proper use must be thoroughly
understood. The quality of the measurements obtained from these tools depends heavily on the care
taken in calibrating and in using each instrument.
Volumetric Flask (http://en.wikipedia.org/wiki/File:Brand_volumetric_flask_100ml.jpg)
Pipettes (http://www.chem.yorku.ca/courses/chem1000/equipment/pipette.html)
Buret
In precise work it is never safe to assume that the volume delivered by or contained in any volumetric
instrument is exactly the amount indicated by the calibration mark. Instead, recalibration is usually
performed by weighing the amount of water delivered by or contained in the volumetric apparatus.
This mass is then converted to the desired volume using the tabulated density of Water:
Volume = mass / density (Eq. 1)
All volumetric apparati should be either purchased with a Calibration Certificate or calibrated by the
analyst in this manner.
Systematic Errors Affecting Volumetric Measurements

25
The volume occupied by a given mass of liquid varies with temperature, as does the volume of the
device that holds the liquid. 20oC has been chosen as the normal temperature for calibration of much
volumetric glassware.
Glass is a fortunate choice for volumetric ware as it has a relatively small coefficient of thermal
expansion; a glass vessel which holds 1.00000L at 15 oC holds 1.00025L at 25oC. If desired, the
volume values (V) obtained at a temperature (t) can be corrected to 20oC by use of:
V20 = V [1 + 0.000025 (20 - t)] (Eq. 2)
In most work, this correction is small enough it may be ignored. However, the thermal expansion of
the contained liquid is frequently of importance. Dilute aqueous solutions have a coefficient of thermal
expansion of about 0.025%/oC. A liter of water at 15oC will occupy 1.002L at 25oC. A correction for
this expansion must frequently be applied during calibration procedures.
Parallax is another source of error when using volumetric ware. A correction for this expansion must
frequently be applied during calibration procedures. Frequently, graduation marks encircle the
apparatus to aid in this.
(Quantitative Analysis, 4th Ed. by Conway Pierce, Edward L. Haenisch

and Donald T. Sawyer; John Wiley & Sons; 1948.)
Readings which are either too high or too low will result otherwise.
Tips for Correct Use of Volumetric Glassware

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Pipets
The Pipet is used to transfer a volume of solution from one container to another. Most Volumetric
Pipets are calibrated To-Deliver (TD); with a certain amount of the liquid remaining in the tip and as a
film along the inner barrel after delivery of the liquid. The liquid in the tip should not be blown-out.
Pipets of the "blow-out" variety will usually have a ground glass ring at the top. And, drainage rates
from the pipet must be carefully controlled so as to leave a uniform and reproducible film along the
inner glass surface. Measuring Pipets will be gradated in appropriate units.
Once the pipet is cleaned and ready to use, make sure the outside of the tip is dry. Then rinse the
pipet with the solution to be transferred. Insert the tip into the liquid to be used and draw enough of
the liquid into the pipet to fill a small portion of the bulb. Hold the liquid in the bulb by placing your
fore finger over the end of the stem.
(Quantitative Analysis, 4th Ed. by

Conway Pierce, Edward L. Haenisch
and Donald T. Sawyer; John Wiley &
Sons; 1948.)
Withdraw the pipet from the

liquid and gently rotate it at an angle
so as to wet all portions of the bulb.
Drain out and discard the rinsing
liquid. Repeat this once more.
To fill the pipet, insert it vertically in the liquid, with the tip near the bottom of the container. Apply
suction to draw the liquid above the graduation mark. Quickly place a fore finger over the end of the
stem. Withdraw the pipet from the liquid and use a dry paper to wipe off the stem. Now place the tip
of the pipet against the container from which the liquid has been withdrawn and drain the excess
liquid such that the meniscus is at the graduation mark.
Move the pipet to the receiving container and allow the liquid to flow out (avoiding splashing) of
the pipet freely. When most of the liquid has drained from the pipet, touch the tip to the wall of the
container until the flow stops and for an additional count of 10.
Volumetric Flasks
The Volumetric Flask is used to prepare Standard Solutions or in diluting a sample. Most of these
flasks are calibrated To-Contain (TC) a given volume of liquid. When using a flask, the solution or
solid to be diluted is added and solvent is added until the flask is about two-thirds full. It is important

27
to rinse down any solid or liquid which has adhered to the neck. Swirl the solution until it is
thoroughly mixed. Now add solvent until the meniscus is at the calibration mark. If any droplets of
solvent adhere to the neck, use a piece of tissue to blot these out. Stopper the flask securely and invert
the flask at least 10 times.
Burets
The Buret is used to accurately deliver a variable amount of liquid. Fill the buret to above the zero
mark and open the stopcock to fill the tip. Work air bubbles out of the tip by rapidly squirting the
liquid through the tip or tapping the tip while solution is draining.
The initial buret reading is taken a few seconds, ten to twenty, after the drainage of liquid has ceased.
The meniscus can be highlighted by holding a white piece of paper with a heavy black mark on it
behind the buret.
(Quantitative Analysis, 4th Ed. by Conway Pierce,

Edward L. Haenisch and Donald T. Sawyer; John Wiley
& Sons; 1948.)
Place the flask into which the liquid is to be drained on a white

piece of paper. (This is done during a titration to help visualize
color changes which occur during the titration.) The flask is swirled with the right-hand while the
stopcock is manipulated with the left-hand.
(Quantitative Analysis, 4th Ed. by Conway Pierce,
Edward L. Haenisch and Donald T. Sawyer; John Wiley
& Sons; 1948.)
The buret should be opened and allowed to drain freely until

near the point where liquid will no longer be added to the flask. Smaller additions are made as the end-

28
point of the addition is neared. Allow a few seconds after closing the stopcock before making any
readings. At the end-point, read the buret in a manner similar to that above.
As with pipets, drainage rates must be controlled so as to provide a reproducible liquid film along the
inner barrel of the buret.
Cleaning Volumetric Glassware
Cleaning of volumetric glassware is necessary to not only remove any contaminants, but to ensure its
accurate use. The film of water which adheres to the inner glass wall of a container as it is emptied
must be uniform.
Two or three rinsings with tap water, a moderate amount of agitation with a dilute detergent solution,
several rinsings with tap water, and two or three rinsings with distilled water are generally sufficient if
the glassware is emptied and cleaned immediately after use.
If needed, use a warm detergent solution (60-70 oC). A buret or test tube brush can be used in the
cleaning of burets and the neck of volumetric flasks. Volumetric flasks can be filled with cleaning
solution directly. Pipets and burets should be filled by inverting them and drawing the cleaning
solution into the device with suction. Avoid getting cleaning solution in the stopcock. Allow the warm
cleaning solution to stand in the device for about 15 minutes; never longer than 20 minutes. Drain the
cleaning solution and rinse thoroughly with tap water and finally 2-3 times with distilled water.
Pipets and burets should be rinsed at least once with the solution with which they are to filled before
use.
A General Calibration Procedure
As was noted above, volumetric glassware is calibrated by measuring the mass of Water that is
Contained In or Delivered By the device.
To obtain an accurate mass measurement, buoyancy effects must be corrected for. The amount of air
displaced by the standard weights of the balance is somewhat different than the amount of air
displaced by the weighed water. This difference leads to different buoyancies for these objects;
meaning the balance levels at a point other than when the two objects are of the same mass. This can

29
be corrected for using:
mtrue = mmeas + da ( (mmeas/d) – (mmeas/ds) ) (Eq. 3)
where ds is the density of the standard weights (8.47 g/cm3), da is the density of air ( 0.0012
g/cm3), and d is the density of the object being measured.
This mass data is then converted to volume data using the tabulated density of Water (See Appendix)
at the temperature of calibration. (In very accurate work, the thermometer must also be calibrated as
an incorrect temperature reading will lead to the use of an incorrect density for Water. This, in turn,
will give an inaccurate volume calibration.)
Finally, this volume data is corrected to the standard temperature of 20 oC. This can be accomplished
using the thermal expansion coefficient of Water; 0.00025/oC:
V20 = V [1 + 0.00025 (20 - t)] (Eq. 4)
Further details concerning calibration of laboratory glassware can be found in the NIST publication
“The Calibration of Small Volumetric Laboratory Glassware” by Josephine Lembeck; NBSIR 74-461.
This publication can be found at:
http://ts.nist.gov/MeasurementServices/Calibrations/upload/74-461.PDF
Thus, in this exercise we will calibrate a volumetric flask and a pipet and determine a buret Correction
Factor by calibrating each of these devices with Water. In each case, the measured mass of the
calibrating Water will be corrected for buoyancy effects and the resulting volume will be standardized
to 20oC.

30
Materials
1 5-mL or 25 mL Volumetric Pipet
1 50-mL Buret
1 25-mL Volumetric Flask
2 100-mL plastic beaker
Analytical Balance
Watch (any available timer)
8 inches x 13 inchesAluminum Foil
5 liters of Distilled water
Detergent liquid
10 mL Sulfuric Acid
Laptop or desktop for graphing (EXCEL)
Procedures
Begin by cleaning a 5 mL or
25 mL Volumetric Pipet, a 50
mL Buret, and a 25 mL
Volumetric Flask according to
the procedure outlined above.
It is imperative for the
purposes of calibration that
these glassware items be
cleaned such that Water
drains uniformly and does not
leave breaks or droplets on
the walls of the glass.
If detergent solutions are not sufficient to clean your glassware, a Cleaning Solution (Dichromate in
Conc. Sulfuric Acid) may be used. Consult you instructor before taking this step.

31
Once cleaned, the Buret should be filled with Distilled Water and clamped in an upright position and
stored in this manner until needed. The Volumetric Flask should be clamped in an inverted position so
that it may dry.
Calibration of a Pipet
Use your cleaned pipet. Note if this is a Class A or other device. Weigh a receiving container on the
Analytical Balance; a 100 mL plastic beaker with Aluminum Foil cover. Pipet distilled water into the
plastic beaker and reweigh it.
Record the temperature of the water used.
Repeat the procedure at least 2 more times. Dry the plastic beaker and re-weigh it for each replication.
Q1. Are you pipeting consistently and correctly?
Calculate the apparent mass and the buoyancy corrected mass of the water delivered for each time you
pipet. From this mass, and the density of water at the given temperature (See Appendix), (Q2)
calculate the volume of the water delivered. Correct the volume to 20 oC. Calculate the Average,
Standard Deviation and 90% Confidence Interval for your calibration result.
Show your solution.
Q3. Is your result within the listed tolerance for this pipet? (See Appendix)
Q4. What is the better question to ask?
Calibration of a Buret

32
Use your cleaned 50mL buret. Note if this is a Class A or other device. Fill the buret with water. Make
sure the tip is free of bubbles. Drain into a waste beaker until it is at, or just below, the zero mark.
Allow 10-20 seconds for drainage. Make an initial reading to a precision of at least 0.01 mL. Test for
tightness of the stopcock by allowing the buret to stand for 5 minutes and then re-reading the volume.
There should be no noticeable change in the reading.
Once the tightness of the stopcock is assured, refill the buret and again drain into a waste until it is at,
or just below, the zero mark. Allow for drainage. Touch the tip of the buret to the wall of the waste
beaker to remove the pendent drop of water. Make a volume reading.
Weigh a receiving container on the Analytical Balance; a 100 mL plastic beaker with Aluminum Foil
cover. Drain about 5 mL of water from the buret into the beaker. Allow 10-20 seconds for drainage.
Touch the tip of the buret to the wall of the beaker to again remove the pendent drop. Read the buret
and weigh the water.
Record the result.
Calculate the actual volume of water delivered by the buret in the same manner as outlined above in
the procedure on calibrating pipets. Calculate the Correction Factor by subtracting the apparent
volume delivered, as given by the buret readings, from the actual volume delivered. Repeat the
procedure at least once more. The two Correction Factors should agree within 0.04 mL. If they do not,
repeat the procedure again. Report the average Correction Factor for 5 mL.
Record the result.
Repeat this process for 15 mL, 25 mL, 35 mL, and 45 mL delivered.

33
Plot the Average Buret Correction Factor vs. Volume Delivered using Excel or some other graphing
software.
Label and store your buret properly; upright and filled with Distilled Water. This is the buret
you will use for the remainder of the course.
Calibration of a Volumetric Flask

Use your cleaned 25mL volumetric flask. Note if this is a Class A or other device. Weigh the flask
empty. Fill the flask to the mark and re-weigh it. Measure the temperature of the water used.
Repeat the procedure at least twice more.
Calculate the true volume of the flask using the method outlined above. Report the Average, Standard
Deviation, and 90% Confidence Interval for this result.
Q5. Is your result within the listed tolerance for this flask?
Q6. What is the purpose and importance of calibration?

34
Appendix - Density of Water
Temperature (oC) Density (g/mL)
10 0.9997026
11 0.9996084
12 0.9995004
13 0.9993801
14 0.9992474
15 0.9991026
16 0.9989460
17 0.9987779
18 0.9985986
19 0.9984082
20 0.9982071
21 0.9979955
22 0.9977735
23 0.9975415
24 0.9972995
25 0.9970479
26 0.9967867
27 0.9965162
28 0.9962365
29 0.9959478
30 0.9956502

35
Appendix - Tolerances for Class A Volumetric Glassware at 20oC
Pipets
Capacity (mL) Tolerances (mL)

0.5 0.006
1 0.006
2 0.006
5 0.01
10 0.02
20 0.03
25 0.03
50 0.05
100 0.08
Volumetric Flasks

5 0.02
10 0.02
25 0.03
50 0.05
100 0.08
250 0.12
500 0.20
1000 0.30
2000 0.50
Burets

5 0.01
10 0.02
25 0.03

36
50 0.05
100 0.20
With the exception of Graduated Cylinders, the Tolerances for Class B devices is typically twice that
of a Class A device. (ASTM E694)
SENIOR
HIGH
SCHOOL –
SCIENCE,
TECHNOLOGY, ENGINEERING AND MATHEMATICS (STEM) SPECIALIZED
SUBJECT
Grade: 11 Subject Title: General Chemistry 1 and 2
Learning Competencies:
1. Determine the pH of solutions of a weak acid at different concentrations and in the
presence of its salt. STEM_GC11AB-IVf-g-167
2. Determine the behavior of the pH of buffered solutions upon the addition of a small
amount of acid and base. STEM_GC11AB-IVf-g-168

1. Explain and describe the purpose and importance of calibration.
2. Explain and describe the methods of calibration.
3. Explain and describe the standards of calibration.
4. Explain and describe the purpose and imporatnce of calibration.
5. Graphing using EXCEL.
Standard Operating Procedures

OVERVIEW
In the following laboratory exercises you will be introduced to some of the glassware

37
and techniques used by chemists to isolate components from natural or synthetic mixtures
and to purify the individual compounds and characterize them by determining some of
their physical properties.
While working collaboratively with your group members you will become
acquainted with:
a) Volumetric glassware
b) Liquid-liquid extraction apparatus
OBJECTIVES
After finishing these sessions and reporting your results to your mentor, you should
be able to:
• Prepare solutions of exact concentrations
• Separate liquid-liquid mixtures
• Purify compounds by recrystallization
EXPERIMENT 1
Glassware Calibration, Primary and Secondary Standards, and Manual Titrations
PART 1. Volumetric Glassware Calibration

Volumetric glassware is used to either contain or deliver liquids at a specified
temperature. Glassware manufacturers indicate this by inscribing on the volumetric ware
the initials TC (to contain) or TD (to deliver) along with the calibration temperature,
which is usually 20°C1. Volumetric glassware must be scrupulously clean before use. The
presence of streaks or droplets is an indication of the presence of a grease film. To
eliminate grease from glassware, scrub with detergent solution, rinse with tap water, and
finally rinse with a small portion of distilled water.

38
1 Skoog D.A., West D.M., Analytical Chemistry, 2nd Ed, pp. 89-91, Holt, Rinehart and
Winston (1965).
Volumetric flasks (TC)

A volumetric flask has a large round bottom with only one graduation mark
positioned on the long narrow neck.
The position of the mark facilitates the accurate and
precise reading of the meniscus. If the flask is used to
prepare a solution starting with a solid compound, add
small amounts of solvent until the entire solid dissolves.
Cap the flask with its stopper and invert it three times to
insure good mixing. If the temperature changes during
dissolution, wait until the flask reaches room temperature before proceeding to fill the
flask to the mark.
When filling the volumetric flask, stop the transfer of liquid when the liquid level is
about an inch below the graduation mark and invert the flask as you did previously to
homogenize the solution. Then use a Pasteur pipette to add liquid slowly to the mark.
Once liquid is filled to the mark, cap the flask with a stopper and mix as before.
Overfilling the flask above the graduation mark ruins the volume measurement. In this
case, the content inside the volumetric flask should be discarded.
Pipettes (TD)
A pipette bulb should be used to withdraw and deliver liquids when using a pipette.
In this course you will use graduated and volumetric pipettes according to the precision
required by the experiment. Graduated pipettes deliver different amounts of liquid by
making use of incremental
markings inscribed along the pipette. Volumetric pipettes deliver fixed amounts of liquid
indicated by a single graduation mark inscribed on them. The volumetric pipette
possesses an enlarged portion below the graduation mark in order to reduce the speed of

39
suction and allow a

precise volume reading.
Burettes (TD)
A burette is a long glass tube with a stopcock near the tip, which precisely controls
the rate of flow of liquid down the constricted tip of the burette.
Before use, burettes must be rinsed first with distilled water, then with a small
portion of the liquid to be measured as follows: add approximately 2 mL of liquid to the
burette, hold the burette horizontally and rotate it to allow the liquid to coat the entire
inside. Drain the liquid down the tip. When filling the burette using a funnel, make sure
the funnel is perfectly clean, the stopcock is closed, and the burette is over a waste
beaker. If you see air bubbles trapped inside the tip of the burette, eliminate them by
draining a few mL of the liquid out the tip while holding the burette diagonally. Your
mentor will demonstrate the correct way to rinse and fill the burette.
Depending on the type of glassware, the gravimetric calibration procedure at room
temperature consists of:
a) Determining the mass of distilled water that fills the TC-ware until the bottom of
the meniscus coincides with the graduation mark; or collecting the amount of water
delivered by the TD-ware in a tared beaker. Repeat the procedure at least three times to
assure reproducibility.

40
b) Measure the exact temperature of the water with a 0.1°C precision thermometer before
each measurement.
c) Calculate the calibrated volume using the density of water at the calibration
temperature
Warning: The Mettler balance has a capacity of 510g.
Statistical Analysis of Data

Your group will be assigned 4 or 5 pieces of glassware to calibrate. Each group member
should calibrate one piece of glassware. Your mentor will give you instructions about the
volumes to measure. Input the data from your notebook into the spreadsheet that
corresponds to each piece of glassware.
1. Record the name of the manufacturer. Fill up the information as in the example below.
VOLUMETRIC FLASK
Measured Measured mass Temperature of Density (g/mL) Calculated
Volume (g) water (°C) volume
(mL) (mL)
2. Using Excel compute the average, variance, and standard deviation for each piece of
glassware. Compute the same statistics for the mass determined with the Mettler balance
3. Find the uncertainty given by the glassware manufacturer and by the Mettler Company
4. Compare the values of the computed statistic with the uncertainty provided by the
manufacturers. Comment on the statistics given by the manufacturer.
5. Discuss the precision of the calibrated volume for each piece of glassware and for the
Mettler balance
6. Report your conclusions
PART 2. Solution Preparation: Primary and Secondary Standards

1. Tare two watch glasses and weigh on each a small amount of sodium hydroxide, NaOH
and potassium hydrogen phthalate, KHP, a monoprotic acid. Record the masses to the

41
nearest 1 mg. Leave the systems exposed to air for 25 minutes.

2. While you are waiting for the watch glass systems, take a 400 mL beaker of distilled
water and measure the pH of the water. Is this the value you expect? Boil the distilled
water uncovered with a stir bar for 10 minutes and let it cool to room temperature
covered with a watch glass. Measure the pH again.
Q7. Is there a difference in the reading obtained? If so, discuss why.
3. After time has elapsed, weigh the watch glasses and record your observations. Based
on the observations you made, decide which one of the two substances can be weighed
directly and dissolved in a well-measured volume of water to prepare a solution of exact
concentration.
4. Prepare a 10-1M solution of the substance you decided on in step 3.
5. Calculate the volume needed from this concentrated solution to prepare 250 mL of a
10-2M solution. Use a volumetric pipette to withdraw the aliquot calculated from the
concentrated solution.
Q8. Is it OK to use a graduated pipette to take the aliquot? Set this solution aside to
determine its exact concentration later.

42
PART 3. Standardization of Sodium Hydroxide Solution

After preparing a solution with the substance that changed while exposed to air, it is
necessary to perform a standardization (find the exact concentration of the solution) using
a procedure called TITRATION. The solution should be kept minimally exposed to air
after standardization. The TITRATION procedure entails reacting a volume of a solution
whose concentration is exactly known or a mass of solid with known molecular weight
with a volume of a solution which concentration is unknown. The volume of sodium
hydroxide solution used in a manual titration is the volume needed to reach the endpoint
of the titration (where the indicator changes color), while the one obtained from the
potentiometric titration is referred to as the equivalence point of the titration. At the
equivalence point the number of moles of titrant used is equal to the number of moles of
the titrated compound.
1. Add about 450 mL of distilled water to about 150 mL of NaOH (aq) solution provided
(note the approximate concentration of the NaOH(aq) from the bottle). Cover the bottle
and homogenize. Neither of these volumes needs to be exact since the solution will be
standardized. Keep the dilute solution covered as much as possible.
2. Weigh two samples of about 0.2-0.3 g of KHP (Potassium Hydrogen Phthalate, record
exactly the amount of KHP weighed) and quantitatively transfer them into two separate,
clean 250 mL Erlenmeyer flasks. Dissolve the samples in about 100 mL distilled water
(you may need to slightly heat for complete dissolution, but make sure the solutions cool
to room temperature before titrating) and add 2-3 drops of phenolphthalein indicator.
3. Rinse a clean burette with distilled water and then with small portions of the dilute
solution prepared in step 1. Discard the rinse solutions in the liquid waste container and

43
clamp the burette to the burette clamp. Fill the burette with the dilute solution prepared in
step 1.
4. Knowing the exact amount of KHP and its molar mass (204.22 g/mol).
Q9. Can you estimate the approximate volume of dilute sodium hydroxide solution
needed to reach the endpoint of the titration?
5. Titrate the KHP solution with the diluted NaOH solution from the burette, swirling
continuously, until the faint pink color lasts about 20 seconds. Each group member
should perform at least one manual titration.
6. Calculate the concentration of the solution from the volume used in each titration. If
the values of the volume used for each titration fall within the experimental error, use the
average value as the concentration of the solution. If the values are scattered showing low
precision, repeat the titration one more time.
RESULTS
Primary versus non-primary standard
Time(min) Mass NaOH (g) Mass KHP (g)
0
25
Observations:

44
Standardization of NaOH
Manual Titration
Trial 1 Trial 2 Trial 3
Weight of KHP used (g)
Initial burette reading (mL)
Final burette reading (mL)
Volume NaOH used (mL)
DISCUSSION
Q10. Discuss with your group whether the endpoint volume of the equivalence point
should be used to calculate the concentration of the titrated sodium hydroxide
solution.
Q11. What is the exact concentration of the sodium hydroxide solution?
Q12. Comment on the pH range at which phenolphthalein changes color.

45
Q13. Is phenolphthalein a good indicator for standardizing NaOH solutions against

KHP? Explain.
Q14. What is the purpose and importance of calibration?

46
EXPERIMENT 2
Liquid-liquid Extraction and Recrystallization
BACKGROUND
Extractions
Extraction is one of the oldest chemical operations known; it involves transferring a
solute from one phase to another. The preparation of a cup of tea or coffee represents a
process of extraction of flavor and odor components from dried material into water. When
a compound is extracted from a solid material into a liquid, the process is referred to as a
solid-liquid extraction; if the transfer occurs from one liquid into another is called
liquid-liquid extraction. Most organic synthetic procedures are followed by workups
employing extraction to isolate the product of interest.
How would a mixture of saccharin and NaCl be separated? Both are soluble in water.
However, saccharin is somewhat soluble in diethyl ether while salt is not. If you dissolve
the mixture in water and then add ether, two layers will form because ether and water are
immiscible. Most of the saccharin will be extracted into the ether layer. Notice that the
separation is not absolute. The salt and saccharin (the solutes) are distributed between the
two solvents, and a dynamic equilibrium is established. The ratio of the concentration of
a solute in a second solvent (e.g. ether) to its concentration in water is constant, called the
partition coefficient K:
Ksolute = Cether / Cwater

Cether and Cwater represent the molar concentration of the solute in ether and water
respectively.
This constant depends on the solvent used, the solute itself, and temperature. In this

47
particular case Ksaccharin is a large number because saccharin is more soluble in ether
than water while Ksalt is a small number because salt is slightly soluble in ether. Using
this constant, one can show that extracting a component from a mixture several times
with small portions of solvent is more efficient than extracting it with one large portion.
The separatory funnel is the tool of trade for liquid-liquid extraction. In order to
increase the surface area between the two layers, and speed the attainment of equilibrium,
the separatory funnel is shaken and vented. The organic layer (ether) is then separated
from the aqueous layer, and dried. Any water dissolved in the ether can be removed by
utilizing a drying agent such as anhydrous magnesium sulfate (MgSO4) and filtering off
the hydrate (MgSO4•xH2O) that forms. Another way to dry an ether layer is to wash it
with saturated NaCl solution (brine) before adding drying agent. The brine transfers the
water from the ether layer to the aqueous layer. The dry ether solution is evaporated by a
rotary evaporator (see the Instrumentation Guide) and the solute remains in the flask. If
the ether is not properly dried, the remaining solute in the flask will be moist.
Other organic solvents that are used in extractions include ethyl acetate
(CH3CO2C2H5), methylene chloride (CH2Cl2), chloroform (CHCl3), hexane
(CH3(CH2)4CH3), and benzene (C6H6). Benzene and chloroform are usually avoided as
solvents due to their carcinogenic nature. Methanol and ethanol are not useful extraction

48
solvents because they are miscible with water and will not form a separate layer.
Chloroform and methylene chloride are denser than water, while most other organic
solvents are not as dense as water. Therefore, the organic layer could be above or below
the aqueous layer depending on the organic solvent used. If you are not sure which layer
is the organic or the aqueous layer, perform the water drop test: add a drop of either layer
on top of a watch glass filled with water. The aqueous layer will readily mix with water.
You may need to add several drops, as some solvents have a small, but significant,
solubility in water.
The formation of an emulsion is a common problem when performing extractions.

An emulsion is a stable dispersion of one liquid in a second immiscible liquid. Emulsions
delay the separation of two liquids, making it necessary to “break” the emulsion. This can
be done mechanically
(settlers, cyclones, centrifuges, filtration through Celite) or chemically (addition of salt or
a saturated NaCl solution called brine). The addition of salt increases the surface tension
of the droplets and increases the density of the aqueous layer, thereby forcing separation.
If one of the solvents being used is water, the addition of a saturated aqueous sodium
chloride solution will help destroy the emulsion. You should avoid shaking a solution that
tends to form emulsions.
Depending on the impurities being removed extractions can be classified as :
• Aqueous extraction
• Acidic extraction
• Basic extraction
Aqueous Extraction
An organic mixture is extracted with water to remove highly polar materials such as
inorganic salts, strong acids or bases, and low molecular weight polar substances.
Normally, water extractions are used immediately following extractions of a mixture with
either an acid or base to ensure that all traces of the acid or base have been removed.

49
Acidic Extraction
Extracting an organic mixture with a dilute acid (5% HCl) removes any basic
impurities such as amines. Bases are converted to their cationic salts by the acid.
This cationic salt can be converted to its neutral form by adding base to the acid extract.
Basic Extraction
Extracting an organic mixture with a dilute base (5% sodium bicarbonate or NaOH)
converts any strongly acidic impurities to their anionic salts.
This anionic salt then can be regenerated by acidifying the basic extract. If a weak acid is
present, extracting an organic mixture with a stronger dilute base (5% NaOH) will
convert weak acids to their anionic salts:

50
This anionic salt then can be regenerated to its neutral form by acidifying the basic
extract.
Purification by Recrystallization
The technique of recrystallization is used to purify inorganic and organic compounds in
the solid state. Essentially, impurities are separated from the desired product by selecting
a solvent, or a solvent mixture, that will keep the impurities in solution at all
temperatures, thus prohibiting these impurities from precipitating along with the product
crystals. The goal is to prepare a saturated solution of solute in the solvent at its boiling
point and allow it to cool. If the solvent or solvent mixture is properly chosen, the
compound will have decreased solubility at lower temperatures, and the solution will
precipitate crystals as it cools.
Recrystallization Using a Single Solvent

Ideally, the solute is very soluble in the solvent at its boiling point, but virtually insoluble
at 0°C. Usually, recrystallization is carried out by first dissolving the solid in a boiling hot
solvent. Next, the solution is cooled below room temperature, and the crystals that crash
out are collected by vacuum filtration. To do this the substance to be recrystallized is
placed in an Erlenmeyer flask and a minimal amount of hot solvent is added to dissolve
the solid, as the solvent is heated to maintain it at its boiling point. The solution is then
allowed to slowly cool to room temperature undisturbed. Allowing crystals to grow
slowly is important because crystals consisting entirely of the same repeating unit will
have the most uniform and strongest intermolecular interactions. For pure crystals to
grow, however, there must exist a thermodynamic equilibrium between solid- and
dissolved-phase solute. If the solution is shocked and cooled rapidly, crystals will grow
haphazardly and are more likely to incorporate impurities.
Once recrystallization is complete, the crystals must be separated from the mother
liquor via suction filtration, washed a few times with the appropriate ice-cold solvent (to
discourage the now-recrystallized solid from dissolving) and dried either in air or in a
desiccator.

51
Recrystallization Using Solvent Mixtures

In many cases, a single solvent does not fit the above requirement satisfactorily, and
as a result, a mixture of solvents is used. By using a solvent mixture, we are attempting to
create a solvent system that closely resembles an ideal solvent as shown in the Figure
below.
In this situation, a solvent is chosen that will readily dissolve the solid. After
dissolution, the system is filtered to remove any solid impurities (if necessary). A second
solvent miscible with the first, but in which the solute has little solubility, is then added
dropwise to the hot solution to achieve saturation. The first solvent in the dual solvent
system readily dissolves the solidat high temperatures. However, at the boiling point of
this first solvent, the solution is not saturated, and thus, this single solvent does not
exhibit ideal behavior. Upon addition of the second solvent, the solution approaches
saturation at the boiling point of this solvent system. This new dual solvent system best
approaches ideal solvent behavior.
General Procedure
The material to be recrystallized is dissolved in the minimum amount of the solvent in
which the compound is most soluble at its boiling point. While the solution boils, the
solvent in which the compound is less soluble is added drop wise until it just turns the

52
solution cloudy. If necessary, a little of the more-soluble solvent is added to clear the
mixture; as the mixture cools, the desired compound will crystallize out. When using
mixed solvents keep in mind that that they must be miscible so that separate layers do not
form.
Table 1. Some Miscible Solvent Pairs For Recrystallization

Methanol - Water
Ether - Acetone
Ethanol - Water
Ether - Petroleum Ether
Ether - Methanol
Methylene Chloride - Methanol
Ethyl Acetate – Hexanes
Ethyl Acetate - Ether
In this list, the first solvent listed is the principal solvent used to dissolve the “impure”
crystals. The second solvent, present in significantly lower quantity, enables saturation of
the solution and thus initiates the gradual precipitation.
Melting Points
Once an organic solid has been isolated, the melting point range is measured to establish
the compound’s identity and purity. The melting point of a solid compound is the
temperature at which a phase transition from solid to liquid occurs. This is a
demonstration of colligative properties, which can be rationalized by the lowering of the
vapor pressure of pure liquids due to the presence of impurities. It should be apparent that
the impurity must be soluble in the compound in order to cause a melting point
depression; i.e., an insoluble impurity such as sand or charcoal will not depress the
melting point. The impurity does not need to be a solid. It can be a liquid such as water or
an organic solvent. Melting points are generally measured and reported as a range rather
than asa single discrete temperature.

53
EXPERIMENTAL OUTLINE
In this experiment you will separate a mixture of aspirin and an unknown that is either
acetanilide or phenacetin by making use of their solubility and acid-base properties. You
will purify the unknown by recrystallization and determine which of the two substances it
is based on its melting point.
PROCEDURE
PART 1. Separation of Aspirin and Unknown
Before you begin, discuss how you might separate a mixture of aspirin and either
acetanilide or phenacetin with you group. How can you take advantage of the acid-base
properties of the compounds and their solubilities in aqueous and organic solvents?
1. Weigh about 3 g of the unknown mixture and transfer to a clean, dry 125 mL
Erlenmeyer flask. Dissolve in approximately 50 mL dichloromethane. Dichloromethane
may be harmful if ingested, inhaled, or absorbed through the skin. Minimize contact with
the liquid and handle it under the fume hood.
2. Prepare at least 100 mL of a saturated sodium bicarbonate solution (about 10% w/v).
Addyour solution from step 1 to a seperatory funnel and extract the aspirin in two 25 mL
portions of NaHCO3. Your mentor will demonstrate the proper use of a seperatory funnel.
Collect the organic and aqueous layers in separate Erlenmeyer flasks. Why will aspirin be
extracted into the aqueous layer?
3. Set your organic layer aside. Slowly add 6 M HCl to your aqueous layer while stirring
until the pH is about 2. Cool the solution and filter off the solid by vacuum filtration.
Wash your solid with cold distilled water and dry to constant mass. Take the melting
point.
4. Dry your organic layer with sodium sulfate and gravity filter into a pre-weighed

54
roundbottom flask. Evaporate the solvent using a rotovap and determine the mass of solid
you obtain. Determine the melting point of your crude solid.
PART 2. Recrystallization of Unknown

5. Dissolve your solid in a minimal amount of boiling water in an Erlenmeyer flask. Why
is an Erlenmeyer flask ideal for recrystallizations?
6. If the solution is colored, add a small amount of activated carbon and gravity filter the
hot solution into a second flask. Add additional hot solvent to your solution before
filtering and use a funnel pre-heated with vapors from your boiling solvent to prevent
recrystallization and loss of product.
7. Heat your solution until the solute is completely dissolved and then allow it to cool to
room temperature. Cool for 10-15 minutes on an ice bath to complete the recrystallization
and collect the crystals by vacuum filtration.
8. While your solution cools, convince yourself that water is an appropriate solvent for
recrystallization by performing three solubility tests. Take about 10 mg of your crude
unknown (the tip of a spatula) and place in a test tube with about 0.3 mL of either
distilled water, hexanes, ethyl acetate, acetone, or ethanol. Observe the degree to which
the solid dissolves at room temperature, at 0°C, and at the solvent’s boiling point.
9. After your recrystallized unknown is sufficiently dry, determine its melting point and
identify it as either acetanilide or phenacetin. Confirm your results by grinding a 50/50
mixture of your unknown and a pure sample of the compound you suspect, and determine
the melting point. How does this technique work to confirm your result?

55
K to 12 BASIC EDUCATION CURRICULUM SENIOR HIGH SCHOOL – SCIENCE,

TECHNOLOGY, ENGINEERING AND MATHEMATICS (STEM) SPECIALIZED SUBJECT
Grade: 12 Quarter: 1st and 2nd

Subject Title: General Physics 1
LEARNING COMPETENCY
1. Solve measurement problems involving conversion of units, expression of measurements in
scientific notation STEM_GP12EU-Ia-1
2. Differentiate accuracy from precision STEM_GP12EU-Ia-2
3. Differentiate random errors from systematic errors STEM_GP12EU-Ia-3
4. Use the least count concept to estimate errors associated with single measurements
STEM_GP12EU-Ia-4

1. Can measure with vernier caliper, micrometer and spherometer.
Length Measurement: A Vernier Caliper,

Micrometer Screw, and Spherometer
Purpose of the Experiment
The purpose of this experiment is for students to understand the operating principles and
usages of various length measurement instruments and to learn to address errors in the
measurement. In general, the most frequently used length measurement instrument is the
meter scale or rule. However, meter scales possess the following innate disadvantages:
1. Poor accuracy (the smallest scale marking or division is 1/10 cm, and any length below
this scale can only be estimated).
2. Inability to measure the radius of curvature for spherical surfaces.
To overcome these drawbacks, we typically use more precise measurement instruments:

1. Vernier caliper
2. Micrometer screw
3. Spherometer

56
These instruments are used for various purposes and will be used frequently in other
experiments. Although the vernier caliper and the micrometer screw have already been
introduced briefly in high school curricula, we hope that students can use this experiment
as an opportunity to develop a comprehensive understanding of length measurement.
These instruments are used for various purposes and will be used frequently in other
experiments. Although the vernier caliper and the micrometer screw have already been
introduced briefly in high school curricula, we hope that students can use this experiment
as an opportunity to develop a comprehensive understanding of length measurement.
Experimental Principle
A. Vernier caliper
Figure 1
The vernier caliper consists of a main scale and a vernier scale, and enables readings
with a precision of 1/200 cm. Figure 1 shows that the main scale is fitted with Jaws C and
D on either side, with the straight edges connecting C and D vertically to the main scale
forming a right angle. Simultaneously, Jaws E and F are fitted on the vernier scale, which
moves over the main scale. When the jaws of the main and the vernier scales contact each
other, the zeros of both scales should coincide. If the zeros do not coincide, a zero point

57
calibration must be performed instantly. The distance between C and E or between D and
F is the length of the object that is being measured.
We first use an example to demonstrate how to read the vernier caliper, followed by
simple equation readings.
Figure 2
Figure 3
The vernier scale in Figure 2 is graduated into 20 divisions or scale markings, which
coincide with the 39 smallest divisions on the main scale (i.e., 39 mm). Assuming the
length of one division on the vernier scale is S, then S can be obtained as follows:
20S = 39

58
S = 1.95 mm. (1)
In Figure 3, the zero on the vernier scale is located between 18 and 19 mm on the main
scale, whereas the 11th division on the vernier coincides with the 40 mm on the main
scale. Thus, AB is the length of the object, and
AB = AC − BC (2)
where the length of AC is 40 mm and BC is the length of the 11 divisions on the vernier
scale. Therefore,
AB = 40 − 11 × S = 40 − 11 × 1.95 = 18.55. (3)
However, although these calculations are easy, repeating them in each reading is time
consuming. In fact, some contemplation enables vernier caliper reading to be as direct
and rapid as straight ruler reading. We hereby convert (3) into (4).
AB = 18 + 11 × ( 2 − 1.95) = 18 + 11 × 0.05 (4)
Where 18 represents the division (i.e., 18 mm) on the main scale that precede the location
where the zero on the vernier scale points in Figure 3. Furthermore, 11 represents the
division on the vernier scale that coincides with a division on the main scale. A closer
look indicates that 0.05 is marked on the vernier caliper. Thus, a reading of the vernier
caliper can be obtained rapidly following these steps:
1. Determine that the zero on the vernier scale is located between divisions n and n+1 on
the main
scale;
2. Identify division m on the vernier scale as coinciding to a certain division on the main
scale;
3. Determine how many units M one division on the vernier scale is equivalent to. This
unit is typically displayed on the vernier scale. For example, Figure 3 shows that one

59
division on the vernier scale is equal to 0.05 mm. (Note: when we say that one division
on the vernier scale is equal to 0.05 mm, this does not mean that one division on the
vernier actually measures 0.05 mm. The actual length of one division on the vernier scale
shown in Figure 3 is in (1)). If the vernier caliper does not show how many divisions a
scale marking or divisions on the vernier scale is equivalent to, we can obtain this
information through calculations. The method is specified in a subsequent passage.
4. The reading should be n + m × M (A closer inspection shows that the value of m × M
is displayed on the vernier caliper. Therefore, a vernier caliper reading is as simple as a
straight ruler reading, and we can obtain the measurements instantly).
In labs, vernier calipers possess various specifications. For example, the one shown
in Figure 3 contains a vernier scale, whose 20 divisions coincide with the 39 smallest
divisions on the main scale. We provide the following examples to demonstrate how to
calculate how many divisions one marking on the vernier scale equals.
Example 1: The 20 divisions on the vernier scale coincide with the 39 smallest markings
on the main scale (mm). Thus, the length of one division on the vernier scale is
S = = 1.95 39
20
Therefore, one division on the vernier scale is equal to 2 - 1.95 = 0.05 mm.
Example 2: Ten divisions on the vernier scale coincide with 9 smallest divisions on the
main scale (mm). Thus, the length of one division on the vernier scale is
S= = 0.9 9
10
Therefore, one division on the vernier scale is equal to 1 - 0.9 = 0.1 mm.
Regarding the vernier calipers in this lab, we have summarized the following rules by
which we can obtain what one division of the vernier scale equals.
1. When the smallest division on the main m scale is M and n divisions on the vernier
n
scale are equal to m divisions on the main scale, the actual length of the smallest
division on the vernier scale is S= M.

60
2. is not an integer. And the value of is m between integers R-I and R,

that is R - 1 << R. n
m
3. One division on the vernier scale is n
m equal to D = (R - ) x M.
n
B. Micrometer screw
Figure 4 shows a micrometer screw, where A is an anvil fixed to the frame (F), and
the spindle (B) channels through F and the sleeve (S) to connect to a revolvable thimble
(T) and a ratchet (H). S is marked with precise divisions, and the periphery of T is
graduated into 50 equal parts. For one revolution of T, it moves forward or backward half
a division on the sleeve, that is, 0.05 cm (metric micrometer screw). Therefore, one
division on the periphery of T equals 0.05/50 = 0.001 cm.
Figure 4
The ratchet is designed to ensure that the object that is placed between the anvil and
the spindle undergoes a certain amount of pressure, but that the pressure does not cause
significant object deformation, which would affect the precision of the measurement.
Therefore, rather than directly turning the thimble to compress the object during
measurement, we should turn ratchet (H) for adjustments.
We will use an example to demonstrate the usage of micrometer screws.
Figure 5 shows the positions of S and T when the length of an object is Y. The edge of T

61
is located between 9.5 and 10.0 mm on S, and the reading on T is 33.5. Therefore, the
distance between the edge of T and the 9.5 mm on S is
33.5 × mm = 0.335 mm. 1

100
Thus, the length of the object is
Y = 9.5 + 33.5 × = 9.835 mm. 1

100
Figure 5
C. Spherometer
Spherometers are used to measure 1 the thickness of thin objects or the radius
100
of curvature of objects. Its structure and operating principles are similar to those
of a micrometer screw. Figure 6 shows that a straight ruler (S) is placed on a tripod (T)
and a circular disc is located on top of the screw (I). The circular scale (G) is graduated

62
into 100 equal parts or divisions. For one rotation of the circular scale, it advances or
recedes by 0.1 cm on S. Therefore, each division of G is equal to x 0.1 = 0.001 cm.
To measure a spherical surface, first place the three legs (ABC) of the spherometer
on the surface, and adjust the screw so that F is in contact with and fixes the surface. If
the spherical glass being measured is positioned as shown in Figure 7, assuming its radius
of curvature is R, the spherometer is located at points A, B, C, and D, and the tip of the
central angle is at D. We assume that h is the distance between D and D', which is the
center of the equilateral triangle formed by A, B, and C, the sides of Triangle ABC are s,
and the distances between D' and A, B, and C are all r.
Figure 6
Based on the relationship of similar triangles, we obtain

63
ΔADD' ~ΔD"AD'
AD'：DD' = D"D' : AD' r : h = (2R - h) : r
∴R=+ rh
2
2h2
Furthermore, ABC is an equilateral triangle, the side length of which is s;
therefore
= r sin 60o = r r2 = ss3

2
32
∴R=+ sh
2
6h2
Laboratory Instruments
1. Vernier caliper
2. Micrometer screw
3. Spherometer
4. Hollow cylinders (several)
5. Watch glass (several)
6. Plate glass

64
7. Coins (self-prepared)
Experimental Procedure
A. Vernier Caliper
1. Zeroing
a. Close the jaws of the vernier caliper and read the zeros;
b. Repeat the action five times and calculate the means of the errors and the
standard deviations.
2. Measure the thicknesses and diameters of the coins five times, respectively,
and calculate the means of the measurements and the mean standard deviations.
3. Use the results from Steps 1 and 2 to calculate the volume of the coins
(including the means and mean standard deviations).
4. Select a random hollow cylinder and measure its outer and inner diameters
and depths five times, respectively, and calculate the means and mean standard
deviations.
5. Use the results from Steps 1 and 4 to calculate the volume of the hollow
cylinder (including the means and mean standard deviations).
B. Micrometer Screw
1. Perform zeroing, same as Step A.-1, and identify the means of the errors and standard
deviations.
2. Same as Step A.-2. (Measure the same coin as the one used in Step A)
3. Same as Step A.-3.
C. Spherometer
1. Zeroing: Place the spherometer on plate glass and ensure that A, B, C, and F are all
contacting the glass. Read the zeros. Repeat the measurement five times and calculate the
means of the errors and standard deviations.
2. Select a random watch glass, place the spherometer on the spherical surface of the

65
glass, and ensure that the tips of the four legs are in contact with the surface. Read the
scale measurement. The difference between zero and this value is h. Repeat this action
five times and calculate the means of h and mean standard deviations.
3. Place the four legs of the spherometer on flat paper simultaneous. Apply a little
pressure to press the tips to leave marks on the paper. Use these marks to obtain the side
length s of Equilateral Triangle ABC. Repeat the measurement five times and calculate
the means of s and standard deviations.
4. Based on these results, calculate the radius of curvature of the watch glass (means and
mean standard deviations).

66
Questions for Reflection

1. Using the vernier calipers and the micrometer screw to measure the same object, which
method will yield a more precise result? Why?
________________________________________________________________________
________________________________________________________________________
________________________________________________________________________
________________________________________________________________________
________________________________________________________________________
2. Can we use the spherometer to measure the radius of curvature of a concave mirror? If
yes, please demonstrate how to modify the equations.

67
________________________________________________________________________
________________________________________________________________________
________________________________________________________________________
________________________________________________________________________
________________________________________________________________________
3. Based on the statistics of the experiments, please explain how to determine the
significant figures of the results.
________________________________________________________________________
________________________________________________________________________
________________________________________________________________________
________________________________________________________________________
________________________________________________________________________
K to 12 BASIC EDUCATION CURRICULUM SENIOR HIGH SCHOOL – SCIENCE,

TECHNOLOGY, ENGINEERING AND MATHEMATICS (STEM) SPECIALIZED SUBJECT
Grade: 12 Quarter: 3rd and 4th
Subject Title: General Physics 2

68
LEARNING COMPETENCY
1. Draw circuit diagrams with power sources (cell or battery), switches, lamps, resistors (fixed and
variable) fuses, ammeters and voltmeters STEM_GP12EM-IIIf-47
2. Evaluate the equivalent resistance, current, and voltage in a given network of resistors connected in
series and/or parallel STEM_GP12EM-IIIg-48

1.
2.
Electrical Symbols

69

70
Safety and Health Guide for the Microelectronics Industry
References:
Http://preparatorychemistry.com/Bishop_Book_4_eBook.pdf
Chemical Industry Processes and Chemical Reactions. Inquima.
<http://www.inquimica.com/chemical-industry-processes-chemical-reactions.html>
(June 7, 2016
Ten Important Chemical Reactions <http://justonly.com/chemistry/pdfs/ten_reactions.pdf> (June

7, 2016)
https://www.google.com.ph/search?
q=methane&biw=1368&bih=623&source=lnms&tbm=isch&sa=X&ved=0ahUKEwjUquOcpZXNAh
VFppQKHQp8CFYQ_AUIBigB#tbm=isch&q=methane+gas+uses&imgrc=WBh4qQmpCQUhHM
%3A
https://books.google.com.ph/books

71
Profile
Personal Data
Name: Marjorie Brondo-Regalado
Date of Birth: April 20, 1986
Place of Birth: Sta. Cruz, Laguna
Civil Status: Married
Religion: Jehovah’s Witness
Sex: Female
Parents: Herman B. Brondo and Estrella D. Burac
Husband: Rowell G. Regalado
Daughter: Eliyah Julienne B. Regalado
Educational Background:
Primary : Stma. Cruz Elementary School, Sta. Cruz, Laguna
Secondary: Pedro Guevara Memorial National High School,

Sta. Cruz, Laguna
Tertiary: Laguna State Polytechnic University, Sta. Cruz, Laguna

Course: Bachelor of Secondary Education Major in Chemistry
Masters: Laguna State Polytechnic University, Sta. Cruz, Laguna

Course: Master of Arts in Teaching Science and Technology
Complete Academic Requirement (33 units)
Organization: SEAL (Science Educators Association of Laguna)
Achievements: Coach of Different Contests

Rank 10 KAPNAYAN 2016 Quiz Contest (National Level)
3rd Place KAPNAYAN 2016 Essay Writing
1st Place Division Science Quiz Contest 2014
3rd Place Division Science Quiz Contest-Teacher Category 2015

72

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K-12 SENIOR HIGH INDUSTRY LINKAGE REPLICATION PROJECT

K-12 SENIOR HIGH

A Compilation of Activities and Experiments

ICCP GROUP FOUNDATION, INC. MARJORIE B. REGALADO-TEACHER III

A project of ICCP Group Foundation

MARIBETH G. HERRERO TEODORA M. GALANG

DR. JUANITO Y. DE RAMOS

Material contained in this publication is compiled from electronic sources.

ICCP GROUP FOUNDATION, INC. MARJORIE B. REGALADO-TEACHER III

ICCP GROUP FOUNDATION, INC. MARJORIE B. REGALADO-TEACHER III

CONTEXTUALIZED LEARNING COMPETENCY

ICCP GROUP FOUNDATION, INC. MARJORIE B. REGALADO-TEACHER III

Materials for Each Group

Notes about the Materials

ICCP GROUP FOUNDATION, INC. MARJORIE B. REGALADO-TEACHER III

Q1. Do water and alcohol have the same or different densities?

6. Carefully place the cups of water and alcohol

ICCP GROUP FOUNDATION, INC. MARJORIE B. REGALADO-TEACHER III

sure to mention both volume and mass.

Note: If you would like the liquids to be more visible, add 1

Q5. Why does the alcohol float on the oil?

Materials for each group

ICCP GROUP FOUNDATION, INC. MARJORIE B. REGALADO-TEACHER III

Water Alcohol Oil

Alcohol Oil Water

ICCP GROUP FOUNDATION, INC. MARJORIE B. REGALADO-TEACHER III

EXPLAIN IT WITH ATOMS & MOLECULES

Chemical Used in Semiconductor Industry

Liquid chemicals are use in the semiconductors industry in many

The production requirements of this High Tech industry impose the

Wet chemistry is one of the most important technological stages in

Semiconductors chemistry is mainly organized around the chemical

ICCP GROUP FOUNDATION, INC. MARJORIE B. REGALADO-TEACHER III

Solve the following problems.

ICCP GROUP FOUNDATION, INC. MARJORIE B. REGALADO-TEACHER III

Isopropyl alcohol (IPA) is one of the most

ICCP GROUP FOUNDATION, INC. MARJORIE B. REGALADO-TEACHER III

ICCP GROUP FOUNDATION, INC. MARJORIE B. REGALADO-TEACHER III

Take it Further More

RUBRICS FOR ASSESSMENT

ICCP GROUP FOUNDATION, INC. MARJORIE B. REGALADO-TEACHER III

the time 5 minutes minutes late minutes late more than

Student Powerpoint Presentation Rubric

ICCP GROUP FOUNDATION, INC. MARJORIE B. REGALADO-TEACHER III

ICCP GROUP FOUNDATION, INC. MARJORIE B. REGALADO-TEACHER III

CONTEXTUALIZED LEARNING COMPETENCY

Topic: Chemical Reactions and Chemical Equations in Industry

BEFORE, you learned

NOW, you will learn

A chemical process is a method in which one or more chemicals or

ICCP GROUP FOUNDATION, INC. MARJORIE B. REGALADO-TEACHER III

Directions: Write the proper coefficient to

Reaction: H2(g) + N2(g)  → NH3(g)

Significance: Synthesis of ammonia leads to the

2. Combustion of hydrogen / Electrolysis of water

Hydrogen gas and oxygen combine to produce liquid water.

ICCP GROUP FOUNDATION, INC. MARJORIE B. REGALADO-TEACHER III

Significance: In the forward direction this is a

3. Combustion of methane (hydrocarbons)

Reaction: CH4(g) + O2(g) →

ICCP GROUP FOUNDATION, INC. MARJORIE B. REGALADO-TEACHER III

Flash and bubbler:

5. Synthesis of sulfuric acid

Reaction: S(s) + O2(g) + H2O(l) → H2SO4(aq)