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GENERAL CHEMISTRY
LABORATORY MANUAL
QAFQAZ UNIVERSITY
QAFQAZ UNIVERSITY LABORATORY MANUAL
In all chemical work it is essential that good records be keptotherwise work may
notebook while the work is in progress. Loose scraps of paper are unacceptable as places
to record results. In many industrial laboratories, each day's work is signed by the
colleague. One reason for keeping good records is to have the information available for
later use.
The notes of the students in this course are to be kept in a similar way. A bound
notebook with pre-recorded page numbers must be used. A spiral notebook is not
the notebook. Each exercise should start on an unused page in the notebook. At the start
of each day's work, the date should be recorded. Records are always kept in ink. In the
event that an error is made in recording an observation or a data point, the erroneous
words or numbers should be crossed out and the correct information written nearby.
The Laboratory Report is the means whereby you convince the instructor that you
conducted the experiment thoughtfully and learned something in the process. Below are
1. Header, containing Date and Time on left side, title of experiment in center,
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QAFQAZ UNIVERSITY LABORATORY MANUAL
your name, lab partner's name. TA's name, and section on right hand side.
2. Title of experiment.
data should be recorded in the notebook while the work is in progress. Scraps
5. Calculations from your data used to obtain your results. These should be
6. Results: Clearly indicated so the instructor can find them. Use a table if
appropriate.
Your laboratory report will be due one week from the date of completion.
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LESSON 1
Lab Dress: Beginning on the first day of lab, everyone MUST have approved goggles, long-
sleeved shirts which cover the midriff, long pants, and shoes with closed toes and
heels (no sandals, slides, etc.). (Basically, you should have as little exposed skin as
possible.) Anyone not wearing the appropriate attire will not be allowed into lab.
Fires: Most organic materials including you, your hair, and your clothing are
flammable. Know the location of the safety showers, fire extinguishers, and fire
blankets.
Floods: Be careful with drain hoses and leaky faucets.
Injuries: Blood is always a sure sign of bad laboratory technique. Check all glassware for cracks,
sharp edges, or star cracks before using it.
Any injury no matter how trivial, should be reported to the lab instructor.
Spills: Notify the lab instructor of any spills which occur during the lab. Minor spills can be
cleaned by students, but do not try to clean up reagent or solvent spills yourself; some
of these materials require special care in their disposal.
Clean up any spills immediately.
Behavior: Do not eat, drink, smoke, or chew gum in the lab.
Work only at your assigned desk.
Do not perform experiments other than those which are scheduled for that day.
No horseplay will be tolerated.
Wastes: Throw away trash in the appropriate containers.
Follow the directions of your instructor for discarding wastes from that days work.
These instructions must be followed carefully; disposing of chemical wastes in the
wrong way may result in dangerous reactions (or at least a foul-smelling lab or a
foul-smelling chemist). Always ask if youre unsure.
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Broken glass should be discarded in the designated waste containers. NEVER throw
glass away in the trash cans!
Reagents: Do not move reagent bottles from their assigned place.
Always recap reagent bottles! Some reagents decompose when exposed to the
atmosphere for a period of time.
Do not stick anything into the reagent bottles. If a spatula is provided for that purpose,
be sure that the same spatula is used in the same bottle.
If you pour out or weigh out too much of any reagent or solvent from the bottle, do
NOT put the excess back in the bottle. This will risk introducing contaminants into the
main supply of the reagent. Unused or excess reagents should be disposed of in the
appropriate waste container.
When an experiment calls for water, use deionized water provided in the wash bottles
on the lab benches unless the directions specifically call for tap water. USE ONLY
TAP WATER IN HOT WATER BATHS!
Never add water to acid!
Never add boiling chips or activated carbon to hot liquids!
Fume Hoods: Fume hoods are used when a procedure may produce smoke or strong odors.
Keep the fume hoods clean! Do not leave weighing paper lying around in the hood
after youre finished with it.
Balances: Keep the balances clean. Immediately clean up any chemicals which are spilled on
the balances, or around the balance area.
Do not leave stray pieces of paper or glassware around the balances.
Equipment: Bunsen burners, ring stands, clamps and O-rings, and buret clamps are available on the
side shelves. At the end of the laboratory period, clean the desk space and return
burners, clamps, and ring stands to their assigned spaces.
Glassware: Hot glass looks exactly like cold glass.
Check all glassware for cracks, sharp edges, or star cracks before using it. (I know I
said this already, but it bears repeating.)
Cleaning up: Clean up your bench before leaving.
Be sure that the gas, water, and electric hotplate/stirrers are turned off. Return all
glassware and hardware to their respective drawers, and return ringstands to the shelves
on the side of the lab.
Wash your hands after leaving the laboratory, or at any time you think that chemicals
may have come in contact with your hands.
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Foreword
This laboratory sequence is designed to illustrate some of the principles involved in performing
scientific measurements, handling chemicals, and performing chemistry experiments. In some cases, the
experiments in the lab are designed to introduce you to concepts before you cover them in the lecture
course, and in some cases, the experiments will reinforce concepts already covered in the lecture course.
Pay attention to the directions that your lab instructor gives you concerning the assignments
which must be completed before the lab. In many cases, there will be Pre-Lab Assignments that must be
done on the computer before you can participate in that days lab.
Laboratory Equipment
The following is a list of all of the glassware that should be found in the Glassware and Hardware
drawers:
See Figure 1 for an illustration of some of this glassware and equipment. (The glassware on this
figure is not drawn to scale.) Other equipment that you will need during this lab will be provided as it is
needed.
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Clay Triangle Crucible with lid Crucible Tongs Split Rubber Stopper
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LESSON 2
Introduction to Density
Introduction
The purpose of this experiment is to understand the meaning and significance of
the density of a substance. Density is a basic physical property of a homogeneous
substance; it is an intensive property, which means it depends only on the substance's
composition and does not vary with size or amount. The determination of density is a
nondestructive physical process for distinguishing one substance from another. Density
is the ratio of a substance's mass to its own volume.
m mass
_____ _________
d = =
V Volume
In the metric system the unit of density for a liquid or solid is measured in g/mL or g/cm 3.
The cm3 volume unit used with solids is numerically equal to mL volume unit used with
liquids. That is, 1 mL = 1 cm3. In this experiment you will determine the density of
several liquids and compare the physical properties of those liquids.
Which is heavier, a pound of aluminum or a pound of lead? The answer, of course,
is neither, but many people confuse the words "heavy" and "dense." "Heavy" refers to
mass only. Density is the mass of a substance contained in a unit of volume. Lead is a
very dense metal and contains a large quantity of matter in a small volume, while
aluminum, being much less dense, contains a smaller quantity of matter in the same
volume.
The volume of 20.0 grams of lead is 1.77 mL. The mass of lead contained in each
mL is its density.
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immersed in the water. The object displaces a volume of water equal to its own volume.
If the solid material is soluble in water, another liquid, in which the solid is insoluble, is
used (e.g. carbon tetrachloride for salt).
Procedure
(Part 1) Density of water:
In any chemistry experiment, it is always advisable to calibrate your instruments
and to practice any new technique. The density of water can be found in the CRC
Handbook of Physics and Chemistry. You will learn the technique for measuring the
density of any liquid by experimentally determining the density of water then comparing
it to the actual value obtained from the CRC Handbook. You will need to pay close
attention to the proper use of a graduated cylinder and a balance.
Weigh a clean dry 25-mL or 50-mL graduated cylinder. Remove it from balance and add
15.0 mL of distilled water and read the volume to the nearest 0.1 mL (carefully observe
the bottom of the meniscus). Re-weigh the graduated cylinder now containing water.
Calculate the mass of water and the density of the water using the equation, d = m/V.
As with any experiment, you should always check how accurate your experimentally
obtained value is compared to the "true" or accurate value. This experimental error is
also known as percent error and it describes the percentage the experimental value is
off from the actual value.
actual value - experimental value
% error = _________________________ x 100
actual value
If you used the graduated cylinder and balance correctly, you should have an
experimental error less than 1%. If your error is greater that 2% repeat the above
experiment until you have a small percent error.
(2) Obtain either cottonseed oil or corn oil. Look up the actual density in the CRC
Handbook. Weigh a dry 25-mL graduated cylinder. Remove it from balance and add 10
mL of oil and read the volume to the nearest 0.1 mL (carefully observe the bottom of the
meniscus). Re-weigh the graduated cylinder now containing oil. Record the weight of oil
then calculate the density of the oil.
(3) Repeat the process with vinegar. Do not look up the density in a reference
book. It probably is not reported since vinegar is a mixture and not a pure substance.
On the report sheet, record the weight of vinegar then calculate the density of vinegar.
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Dispose of these test tubes in the sink and wash the test tubes with soap and water.
Scrub the oil test tubes well.
(OPTION 1) Using the Merck Index or CRC Handbook of physics and chemistry, look up
the density of the following metals. Your unknown solid may be one of these metals. .
Report the density and calculate your experimental error
Al Cu Fe Pb Sn Zn Yellow Brass Stainless Steel
(OPTION 2) The solid unknown may also be copper pennies from different years.
Obtain two sets (each set containing about 10 pennies) from two different years. Follow
the same directions as above except after placing the pennies into the graduated
cylinder, remember to gently tap the sides to free any trapped air bubbles. Share your
data with 3 to 4 other groups then make a graph showing the change in the density of
pennies over the years.
Experiment 3 - Density
Name_________________
_____________
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________________
________________
= _________________
Vinegar
1. Weight of a dry 25-mL graduated cylinder = ________________
________________
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(OPTION 1)
Identity of metal _____________ True density ____________g/mL Percent
error_____________ %
Identity of metal _____________ True density ____________g/mL Percent
error_____________ %
(OPTION 2)
Look up the density of pure copper.__________________
What trend is indicated by the graph of density vs. year?
Hypothesize how the trend in density compares to the compositional change in pennies?
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LESSON 3
DILUTION
PURPOSE
THEORY
In dilution, the amount of solute stays constant. Only the solvent is being added.
Since the amount of solute stays the same before and after dilution an equation can be written to
say the same thing mathematically:
Since the solutions in terms of molarity and volume, moles seem a natural way to work, since
multiplying molarity times volume in liters will give the moles of solute. In other words,
MV = moles of solute
If a subscript used 1 to specify the concentrated solution, or the solution before dilution, this can
be written:
Substituting,
M1V1 = M2V2
Laboratory Coat
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Graduated Cylinder
Beaker
Spatula
Funnel
Pipette
Wash bottle
Dropper
Rubber pipette bulb
300 ml water
PROCEDURE
When preparing a dilution, the first thing to do is wearing a laboratory coat for eliminating the
damages. Calculating the volume of necessary concentrated HCL.Find the volume of the water
which is necessary for dilution. Fill small amount of water into beaker for avoiding any
splashing. Then put HCL with using pipettes and with the help of rubber pipette bulb. Then
measure the volume of water which is the volume of solution and fill it up to solution volume.
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LESSON 4
competitors fireworks displays and had observed a new blue-green color present in some
of the chrysanthemums that they had not seen before. One of their spies had managed to
procure a portion of the material contained in the shell, and now the chemists in the
company could analyze it to find out what chemical compound was responsible for the
blue-green color. A metal containing compound was isolated from the material, and
qualitative analysis tests revealed the presence of both copper and chloride ions. The
precise ratio of copper to chloride now had to be determined in order to identify the
You will need to purchase the Signature Labs Series booklet from the bookstore
for this experiment. Read module STOI0386 (pp 1-7) before lab and prepare the pre-lab
outline of the procedure as usual, incorporating the changes to the procedure discussed
below (do not do the pre-laboratory assignment in the module). Use your lab notebook to
record your data and observations, not the data sheet provided in the module.
Work in pairs.
you will use a buret (see TECH II.E) to dispense 25.00 mL of the solution directly
into a 250 mL beaker. Record the initial and final buret readings. If you dispense
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more or less than 25.00 mL, use the exact volume along with the data on the reagent
bottle label to calculate the mass of copper chloride that is in your beaker.
2. To clean the piece of zinc, place 10 mL of 10% HCl solution in a 150 mL beaker.
Place the zinc strip in the hydrochloric acid. Let this sit for one or two minutes until
the dull surface of the zinc has become more lustrous. Using crucible tongs, flip the
metal over to expose the entire surface area to the acid. Pull the zinc out, rinse it under
running water and dry it thoroughly with a paper towel before weighing to the nearest
0.001 g. The HCl solution that remains in the beaker may be poured down the sink.
17. Hold the wire gauze underneath the watchglass as you carry it to the balance.
19. You should obtain two weights that agree to within 0.01 g. Be careful not to
overheat the copper during the drying process as this could lead to the formation of
should be performed a second time and just one of the following variables should be
changed:
Smaller amount of zinc used (cut a piece that weighs 0.7 g or less)
Before you begin the second procedure, make predictions about what, if any, differences you'll
see between the two procedures. Write these differences in your
notebook. These differences can include observations, the empirical formula obtained,
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the percent yield obtained or anything else you can think of. Give an explanation for
your predictions.
Each student must write his or her own report. Your report cannot be identical to
Calculations
Perform all of the calculations in the module (pp 7-8) for both your first and second
Questions
(Do not answer the questions in the module unless instructed to do so.)
1. Answer Post-Laboratory Question 1, parts (1) and (2), from page 9 of the module.
Answer this question for both your first and second experiments.
Answer this question for both your first and second experiments.
3. Did any results from the second experiment differ from the results of the first
experiment (either the empirical formula, the percent yield or other things)? If so,
provide an explanation for the differences. Did the difference(s) match your
prediction(s)?
4. If the copper is heated too long, some of it will be transformed into copper oxide,
CuO. How would this affect the percent of copper that is calculated?
5. Discuss any errors that you may have made in the procedure and how they
affected the determination of the percent copper present in copper chloride and/or
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LESSON 5
EXPERIMENTAL GOALS:
The goal of this experiment is to observe a series of precipitation and neutralization reactions
(double displacement reactions) and deduce some of the properties of the ions involved in those
reactions. You will also observe a series of oxidation-reduction reactions, and draw some
conclusions about them.
INTRODUCTION:
In this lab, you will examine properties and reactions of ionic compounds in aqueous
solution. The focus will be on double displacement (precipitation and neutralization)
reactions, but some attention also will be given to oxidation-reduction (or redox) reactions.
From this experiment, you will learn that many of the properties of an ionic compound are due to
the properties of the ions that make up the compound.
Ionic compounds consist of a positive ion (cation) and a negative ion (anion). Some ions
are monatomic, consisting of a single atom with a positive or negative charge (Na+, Ca2+, Cl-,
O2-, etc.), and some are polyatomic, consisting of a cluster of atoms having an overall positive or
negative charge (NH4+, NO3-, CO32-, SO42-, PO43-, etc.). Each ion has its own characteristic color
and other properties. Many ions are colorless in aqueous solutions, or appear to be white if they
are part of a dry salt. Other ions have a definite color either in solution or as a dry salt, although
the color may change when the salt is dissolved in water. (For example, some copper salts are
green in the solid form, but blue when dissolved in water. The color of an ion may also be
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affected by the concentration of the solution.) If a compound consists of a red cation, for
example, plus a colorless anion, the compound will usually be red. If both cation and anion are
colorless, the compound will be colorless in solution, or appear white as a solid. If both are
colored, the compound will be a mixture or blending of the two colors. The color of a salt,
therefore, usually depends on the colors of the ions composing it. However, there are situations
when a cation and anion which are usually colorless form a colored solid salt when they are
combined. This is a result of the intimate contact between ions in the solid.
I. PRECIPITATION REACTIONS.
A precipitation reaction occurs when two ionic compounds react in an aqueous solution
to produce a precipitate, an insoluble substance which falls out of the solution. These reactions
are a type of double-displacement or metathesis reaction, because the cations and anions of the
reactants change partners in the products:
AB + CD AD + CB
The cations and anions have the same charges on both sides of the reactions, and the formulas of
the products of the reaction can therefore be predicted using the rules for writing the formulas of
ionic compounds.
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The formation of the insoluble precipitate is the driving force for these reactions: the
attractions between the cation and the anion in the precipitate are stronger than their attraction
for the solvent molecules. The other ions stay in solution as spectator ions, and do not
participate in the overall chemical change.
Just because we can write an equation for a precipitation reaction does not mean that the
reaction will actually take place. In order to predict whether a precipitation reaction occurs, we
use the solubility rules in Table 1 to determine whether any of the potential products of the
reaction are insoluble. If one of the products of the reaction is insoluble, the reaction occurs, and
must be balanced appropriately. (If one of the products is a nonelectrolyte like water, a weak
electrolyte, or a gas, the reaction is a neutralization reaction, which will be discussed in the next
section.) If no insoluble product (or weak electrolyte, gas, or nonelectrolyte) forms, then no
reaction (NR) takes place, and all of the ions remain in solution as spectator ions.
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For example, if we mix solutions of NaNO3 and KI, all we get is a mixture of dissolved
ions; no net reaction takes place because none of the potential products are insoluble in water:
(All of the ions in this reaction are spectator ions.) On the other hand, if we mix Pb(NO3)2 and
KI, a reaction does take place, producing a solid precipitate of PbI2:
There are three types of equations which are used to represent precipitation reactions. In
the overall reaction, all of the species are written in their usual ionic formulas (e.g., sodium
chloride is written as NaCl). In the complete ionic equation, all soluble strong electrolytes
(soluble ionic compounds, and strong acids) are dissociated into their separate cations and anions
(e.g., NaCl is written as Na+ and Cl-), while insoluble precipitates, weak acids, and molecular
compounds are left intact. In the net ionic equation, ions that are the same on both sides of the
equation are canceled out; these ions are called spectator ions, because they do not participate in
the overall chemical reaction that is taking place.
For example, consider the reaction between an aqueous solution of sodium chloride and
silver nitrate. One of the products of the reaction is insoluble silver chloride, so the reaction does
take place:
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According to the solubility rules, NaCl, AgNO3, and NaNO3 are soluble in water, so in the
complete ionic equation, they are dissociated into their ions. However, AgCl is insoluble, and is
left intact:
The spectator ions in the reaction are Na+ and NO3-, since they are the same on both sides of the
equation. The Ag+ and Cl- are different, because they are dissociated on the left side, but in an
insoluble precipitate on the right side. In the net ionic equation, Na+ and NO3- are canceled out,
which emphasizes the actual chemical change that takes place: the formation of insoluble silver
chloride:
Notice that the complete ionic equations and net ionic equations must be balanced, with respect
to the number of atoms, and with respect to the total charge. It is important to remember that the
cations and anions have the same charges on both sides of the reaction: precipitation reaction do
not involve changes in oxidation number (see section III).
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Acid-base reactions or neutralization reactions occur when an acid and base react to
form water, a weak electrolyte, or a gas. Like precipitation reactions, these reactions are a type
of double-displacement reaction.
For a strong acid (HA1) and base (MOH), this can be written as
H+ + A- + M+ + OH- M+ + A- + H2O(l)
Canceling the spectator ions M+ and A- gives the net ionic equation:
We will see the same net ionic equation for the reaction of any strong acid with any strong base.
The driving force for this reaction is the formation of a very stable water molecule. When one of
the species is a weak acid or base, one of the products is usually still water, but the net ionic
equation will be slightly different, since weak acids and bases do not dissociate:
Weve already seen one neutralization reaction: the reaction between acetic acid and
sodium hydroxide in the Titration of Vinegar lab is a neutralization:
Some acid-base reactions result in the formation of gases, either directly or in the
decomposition of an unstable intermediate. This removes ions from the solution, driving the
reaction to occur. For example, carbonic acid, H2CO3, is unstable, and falls apart to give water
and carbon dioxide gas, so any time carbonic acid is produced in a neutralization reaction, the
reaction takes place because of the formation of the carbon dioxide:
Other gases that can be produced in neutralization reactions include H2S(g), SO2(g) (from the
decomposition of H2SO3), HCN(g), and NH3(g) (from the dissociation of NH4OH).
1
Sometimes chemistry can be funny. This isnt one of those times.
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Neutralization reactions can also result in the formation of weak electrolytes, which also do not
dissociate. Usually, these will be weak acids2:
In the reaction classification scheme from the Reactions I lab, precipitation reactions and
neutralization reactions are types of double-displacement or metathesis reactions. In these
reactions, the cations and anions in two ionic compounds change partners:
AB + CD AD + CB
In order for a double-displacement to occur, one of four things must occur, otherwise, there is no
reaction (NR):
2. In neutralization (acid-base) reactions, an acid and a base form a salt and water, a gas
(CO2, SO2, H2S, HCN, or NH3), or a weak electrolyte (a weak acid).
For example, in the reaction between elemental iron (Fe) and copper(II) ions (Cu2+), two
electrons are transferred from Fe to Cu2+, producing Fe2+ and elemental Cu. These processes
may be represented by half-reactions that show the separate oxidation and reduction processes:
Notice that when the oxidation and reduction half-reactions are added together, the electrons
cancel out.
2
Remember, the six strong acids are HCl, HBr, HI, HNO3, HClO4, and H2SO4. Any other acid is (for now)
considered to be a weak acid.
3
A common mnemonic device for this is LEO GER (a lion growling): Loss of Electrons is Oxidation, Gain of
Electrons is Reduction.
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oxidation
The oxidizing agent is the substance that causes oxidation to occur by accepting
electrons. The oxidizing agent itself becomes reduced. The reducing agent is the substance
that causes reduction to occur by losing electrons. The reducing agent itself becomes oxidized.
In general, metals tend to act as reducing agents (lose electrons), and nonmetals tend to act as
oxidizing agents (gain electrons). In the previous example, Fe is the reducing agent, and Cu2+ is
the oxidizing agent.
We can keep track of whether a reaction is a redox reaction, and what specifically is
being oxidized or reduced, by using oxidation numbers (aka oxidation state). The rules for
assigning oxidation numbers are listed in Table 2. (Note that oxidation number is not the same
thing as charge!!!!!)
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Examples:
Na Na is zero because it is an atom in its elemental state.
H2 H is zero because it is an atom in its elemental state.
Cl2 Cl is zero because it is an atom in its elemental state.
+
Na Na is +1 because it is a monatomic ion, which has the same oxidation number as its
charge.
Ca2+ Ca is +2 because it is a monatomic ion.
2-
O O is -2 because it is a monatomic ion.
Cl- Cl is -1 because it is a monatomic ion.
H2SO4 H is +1, O is -2, so for the oxidation numbers to add up to 0, S must be +6.
ClO4- O is -2, so for the oxidation numbers to add up to -1 (the charge on the polyatomic
ion), Cl must be +7.
ClO2- O is -2, so for the oxidation numbers to add up to -1 (the charge on the polyatomic
ion), Cl must be +3.
ClO3 O is -2, so for the oxidation numbers to add up to 0 (the charge on the molecule), Cl
must be +6.
HCl H is +1, so Cl must be -1.
CaH2 Ca is +2, so H must be -1. (H is bonded to a metal in this case.)
H2O H is +1, and O is -2.
H2O2 H is +1, and O is -1 since this is a peroxide. (This can be seen if you try to apply
rules 5b and 5c: with H = +1 and O = -2, the oxidation numbers add up to -2, which
is not the charge on H2O2. Since rule 5b takes priority over rule 5c, H must be +1,
and since rule 3 takes priority over rule 5c, this forces O to be -1 for the oxidation
numbers to add up to 0.)
NaCl Na is +1 and Cl is -1. (This is an ionic compound, so the oxidation numbers of
monatomic ions are the same as their charges.)
Cl2O O is -2, which forces Cl to be +1 for the oxidation numbers to add up to 0.
HOBr H is +1 and O is -2, which forces Br to be +1.
SO2 O is -2, which makes S +4.
SO42- O is -2, which makes S +6 for the oxidation numbers to add up to -2.
NH3 H is +1, which makes N -3.
NO2 O is -2, so N must be +4 for the oxidation numbers to add up to 0.
-
NO3 O is -2, so N must be +5 for the oxidation numbers to add up to -1.
NaNO3 Na is +1, O is -2, so N must be +5 for the oxidation numbers to add up to 0. (Notice
that the oxidation number on N is the same as for the previous example, since this is
the same polyatomic ion.)
K2Cr2O7 K is +1, and O is -2; each Cr must have an oxidation number of +6.
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The oxidation number concept gives us another way to define redox reactions: A redox reaction
is one in which the oxidation numbers of species change. Oxidation is an increase in oxidation
number, and reduction is a decrease in oxidation number. Any reaction in which oxidation
numbers change is a redox reaction. If no oxidation numbers change, the reaction is not a redox
reaction.
S + O2 SO2
0 0 +4 -2
S: 0 +4 oxidized
O: 0 -2 reduced
A + BC AC + B
The more active metal A is oxidized (it is the reducing agent), while the less active metal B is
reduced (it is the oxidizing agent). The species C, usually either a monatomic anion or a
polyatomic anion, is a spectator ion in the process.
Combustion reactions are also examples of redox reactions; the carbon atoms in the
hydrocarbons are oxidized to the +4 state in carbon dioxide, while molecular oxygen is reduced.
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Combination and decomposition reactions may be redox reactions, although not all of
them are: check to see if the oxidation numbers change to determine whether or not the reaction
is a redox reaction.
PROCEDURE:
All the salts listed in Part A of the report sheet are water soluble. Solutions of these salts have
been prepared, and are on display in the laboratory. Observe the color of each solution, if any,
and by deduction determine if the color (for colored compounds) is due to the cation, the anion,
or both. (For example, the NaCl solution is colorless, so if you see some other ionic solution
containing Na+ that has a color, the color is not due to the presence of Na+.) Record the formula
and charge for the cation and anion in each of the compounds (e.g., Na+), and its color.
In part A, all the compounds were solutions of soluble salts. All ions have some salts (that is,
combinations with other ions) that are soluble. Nearly all ions also have some salts that are
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QAFQAZ UNIVERSITY LABORATORY MANUAL
insoluble (although, as you will see, there are some exceptions). The solubility of a given salt,
therefore, depends on both ions. In the two exercises below you will produce precipitates by
combining ions. With the knowledge of the colors of ions you have gained in part A, and by
observing the colors of the precipitates and solutions in Part B, you should be able to determine
which ions have precipitated and which have remained in solution.
For this part, use solutions in dropping bottles. The centrifuge may be used to aid in the settling
of the precipitate. Its use will be explained by the instructor.
1. To 5 drops of silver nitrate solution in a test tube, add 5 drops of copper(II) chloride solution
and shake vigorously. Let settle, or centrifuge. Note the colors of the precipitate and the
resulting solution. From part A deduce which ions have gone to the precipitate and which
have remained in solution. Fill in the required information on the report sheet.
2. Repeat, using 10 drops of copper(II) sulfate solution and 5 drops of barium chloride solution.
If you are uncertain about your observations, repeat the test with 15 drops CuSO4 and 5 drops
BaCl2.
You now know that certain combinations of ions are soluble (part A), and that at least two
combinations are insoluble (part B). On the report sheet are listed pairs of solutions. Using the
information obtained in Parts A and B, and some logical thinking, try to predict the formula of
the precipitate that forms (if any), the color of the solution, and the color of the precipitate. If
Parts A and B provide you with no information with which to make a prediction, you should
write no prediction possible.
Check your predictions by mixing together about 5 drops of each solution in a test tube. If the
results do not confirm your predictions, experiment a little by trying the reaction with different
relative amounts of the two solutions (for example, 3 drops of one with 10 of the other, or vice
versa). Record your observations of what happened in the Observation column on the report
sheet. Dispose of the waste in as directed on the data sheet.
D. Neutralization Reactions.
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E. Oxidation-Reduction Reactions.
1. Place a pinch of Cu metal powder into a small test tube and heat it over a Bunsen burner.
When you are finished, put the used test tube in the waste beaker near the Cu metal
powder and solid Cu(NO3)2.
2. Place a few crystals of copper(II) nitrate in a test tube and heat strongly. Observe
carefully and note any gases produced or new solids formed. Can you identify the gas?
Put the used test tube in the waste beaker near the Cu metal powder and solid Cu(NO3)2.
3. Place a small piece of zinc into a test tube containing 2 mL of 6 M HCl. Test for H2 gas
by holding a burning splint near the mouth of the test tube; a popping sound indicates the
presence of H2. If the test is negative, heat the test tube gently to increase the production
of H2, which is indicated by increased bubble formation, and retest for the presence of H2.
Put the solution in the solution waste container labeled with a C. After rinsing in tap
water, dispose of any residual zinc in the waste basket.
4. Place an inverted test tube, filled with water, into a 100-mL beaker of water. Your
instructor will demonstrate this procedure. Now place a piece of calcium metal in the
water and collect the gas that is evolved in the inverted test tube. Bring the test tube to a
lighted Bunsen burner.
5. Place a piece of copper wire into 2 mL of concentrated HCl; carefully observe for signs
of reaction. Place the same piece of copper wire into 2 mL of concentrated HNO3;
carefully observe for signs of reaction. Put the solutions in the solution waste container
labeled with a C.
6. Place a piece of copper wire into a solution of mercury(II) chloride, HgCl2. Wait a few
minutes; taking care not to touch the end of the wire with your hands, wipe off the
wire with a paper towel. Report any changes that you have seen on the surface of the
wire before or after the procedure. Place the Hg-contaminated materials in the beaker
labeled for that purpose. Wash your hands before proceeding to the next experiment.
7. Place an iron nail into copper(II) sulfate solution. Observe any color changes that occur.
The copper coated nail can be disposed of in the waste basket, or kept as a souvenir.
8. Place copper wire into an iron(III) chloride solution. Observe what happens. Rinse the
copper wire and return it to beaker from which it came.
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LAB REPORT
Chemical Reactions II: Reactions of Ions in Solution
Salt Color of Solution Cation & Its Color Anion & Its Color
Sodium chloride, NaCl Colorless Na+, colorless Cl-, colorless
Copper(II) chloride, CuCl2
(Dropper Bottle)
Cobalt(II) Nitrate, Co(NO3)2
Potassium iodide, KI
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The color of the precipitate is __________, and it has the following formula _____________.
The color of the solution is __________, and the ions in the solution are ________________.
The color of the precipitate is __________, and it has the following formula _____________.
The color of the solution is __________, and the ions in the solution are ________________.
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KNO3 and
AgNO3
(Waste B)
CoCl2 and
AgNO3
(Waste B)
KNO3 and
CuCl2
(Waste C)
AgNO3 and
NaCl
(Waste B)
K2SO4 and
Cu(NO3)2
(Waste C)
Pb(NO3)2
and
K2CrO4
(Waste B)
Pb(NO3)2
and KI
(Waste B)
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QAFQAZ UNIVERSITY LABORATORY MANUAL
1. List all the colored cations that were encountered in the entire experiment.
3. Draw a general conclusion about the place of colored cations in the periodic table.
4. At least one of the cations in this experiment is an apparent exception to the rule. Which one
is it?
5. There are two colored anions in this experiment. Which are they, and do they follow the
same rule?
D. Neutralization Reactions.
1. Write the molecular, ionic, and net ionic equations for the reaction between HCl and NaOH.
2. What evidence was there that a chemical reaction between HCl and NaOH occurred?
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3. Write the molecular, ionic, and net ionic equations for the reaction between HCl and
NaHCO3.
4. What evidence was there that a chemical reaction between HCl and NaHCO3 occurred?
E. Oxidation-Reduction Reactions.
1. What physical evidence was there that a chemical reaction occurred? Write a balanced
equation for the reaction.
2. Describe the results of heating copper nitrate, Cu(NO3)2. Can you identify any of the
products? (Recall the reactions of Cu with nitric acid.) Write a balanced equation for the
reaction.
3. Describe the results of adding zinc to HCl. Write the equation for this reaction. Did you
observe the formation of both products in the reaction? If not, why not? (Observe means to
see evidence of a new substance such as a color change, formation of a precipitate, or gas
evolution.) What could you do if you wanted actually to observe all the products?
4. Write an equation for the reaction of calcium metal with water. Did you observe both
products here? What was the appearance of the products? Is the solution acidic or basic?
How do you know?
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5. Does copper wire react with HCl? What part of the HNO3 does the Cu react with?
6. What do you observe when you place the copper wire in the solution of HgCl2?
7. What do you observe when you place a sample of iron into the CuSO4 solution? Write the
reaction (if any) for what happens.
8. What do you observe when you place the copper wire in the solution of FeCl 3? Write the
reaction (if any) for what happens.
9. List the elements that were studied in these reactions (Cu, Hg, Fe, H, and Zn) in order
decreasing chemical activity: an element listed on the left will replace those listed on the
right, and not vice versa. Compare to the activity series in the procedure. [If you cannot
decide the order for two specific elements, you may need to design and perform an additional
test to resolve the problem check your procedure with your instructor before proceeding.]
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LESSON 6
Conservation of Mass
Reactants Products
Mass of O2 ____________g
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Purpose: In this lab, you will start with three different solutions. The combined
masses of the three solutions and their containers will be measured before and
after two reactions. In the first reaction, you should find that the reactants and
products have the same mass. In the second, they will not. Observe these
reactions carefully to better understand and explain conservation of mass.
REACTION 1:
a. Pour test tube A, containing the calcium chloride (CaCl2) into the flask to
observe the first reaction:
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QAFQAZ UNIVERSITY LABORATORY MANUAL
c. replace all stoppers and reweigh the apparatus to record the new mass
of the experimental materials on your data table
REACTION 2:
a. Carefully pour test-tube B, containing the sulfuric acid, into the flask to
observe the second reaction:
c. replace all stoppers and reweigh the apparatus to record the new mass
of the experimental materials on your data table.
Conclusion Questions:
1. What evidence that a chemical reaction has occurred was observed when the
solutions were mixed together in Reaction 1?
2. What evidence that a chemical reaction has occurred was observed when the
solutions were mixed together in Reaction 2?
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3. Compare masses recorded before and after each reaction. If there are
differences in mass, provide an explanation for these differences?
4. Does your data verify the Law of Conservation of Matter? How could you
modify these procedures to bring the results more in line with the law?
5. When you burn logs in a fireplace, the resulting ashes weigh less than the logs.
Provide an explanation for this that reinforces the Law of Conservation of Mass
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LESSON 7
Theory: Hot tea can dissolve more sugar than iced tea, and warm
water dissolves less oxygen than cold water. The maximum amount of
any solute that can dissolve in a given amount of
solvent is called its solubility, and this depends on the
temperature.
Procedure:
6. Place test tube 1 in the hot-water bath. With a glass stirring rod, stir
the KCl mixture until all the solid has dissolved. At this point, remove
the stirring rod and rinse it. Take the thermometer out of the hot
water bath, quickly wipe any excess drops of water from it, and place it
into the test tube while it is still warm.
7. Carefully hold the test tube up to a light. Watch for the very first
signs of crystallization, and then immediately note the temperature. If
crystallization begins too quickly, or you do not catch it the instant it
begins, re-dissolve the precipitate and repeat until you are able to
determine the temperature at which the crystallization begins. Record
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QAFQAZ UNIVERSITY LABORATORY MANUAL
this in the data table. If you are working with a partner, the second
person should be setting up test tube 2.
8. Repeat steps 6 and 7 for all five test tubes. For test tube 5, it will be
necessary to use an ice bath to effect crystallization. Simply place 3 or
4 pieces of ice in a beaker and fill half way with water.
Data Table
Crystallization
Test Tube Mass - Mass of = Mass of Volume = Concentrat
of Pan (g) Sample of ion (g/mL) Temperature (C)
Samp (g) Water
le + (mL)
Pan
(g)
- = =
- = =
- = =
- = =
- = =
Calculations:
Conclusion:
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QAFQAZ UNIVERSITY LABORATORY MANUAL
LESSON 8
Objectives
1. To determine the percentage of water in barium chloride dihydrate.
Discussion
A hydrate salt is composed of anions (negative ions) and cations (positive ions) which are
surrounded by and weakly bonded water molecules. Each hydrate salt has a fixed number of
water molecules associated with it, called waters of hydration or water of crystallization. When
a salt holds waters of hydration, we call it a hydrated salt or a hydrate (hydrate from hydor, the
Greek word for water).
Barium chloride dihydrate, BaCl22H2O, has two waters of crystallization, or two waters of
hydration. Other hydrates have waters of hydration ranging from one to twelve. Upon heating, a
hydrate decomposes and produces an anhydrous salt and water (in the form of steam).
BaCl22H2O (s ) BaCl2 (s) + 2 H2O (g)
The theoretical percentage of water is found by dividing the water of crystallization mass, 36.0
amu, by the hydrate mass, 244.3 amu.
The experimental percentage of water in a hydrate is found by comparing the mass of water
driven off to the total mass of the compound, expressed as a percentage.
A 1.250 g sample of barium chloride dihydrate has a mass of 1.060 g after heating. Calculate the
experimental percentage of water.
Calculate the water of crystallization for an unknown hydrate that is found to contain 30.6 %
water. The formula mass of the anhydrous salt (AS) is 245 amu.
Solution: The unknown hydrate is 30.6 % water. subtracting from 100 %, the hydrate must be
69.4 % anhydrous salt. If we make the sample 100 g, the mass of water is 30.6 g and the
anhydrous salt 69.4 g. to calculate the moles of water and the anhydrous salt (AS)
To find the water of crystallization, simply divide the mole ratio of water to anhydrous
salt.
The water of crystallization is always a whole number, therefor the formula for the
unknown hydrate is AS6H2O.
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QAFQAZ UNIVERSITY LABORATORY MANUAL
PROCEDURE
In this lab, you will find the experimental percentage of water in BaCl22H2O, you will also find
the percentage of water in an unknown hydrate and then calculate the water of crystallization of
the unknown (the formula mass will be provided).
1. Obtain a porcelain crucible from the stockroom, rinse with water, and heat on a clay
triangle for five minutes over a direct flame to remove any surface moisture. Use crucible
tongs when handling hot crucibles.
2. Weigh the cool, dry crucible and lid. Record the weight on the data sheet.
3. Place between 1.0 and 1.5 g of BaCl22H2O in the crucible and reweigh the crucible, lid
and contents. Record the mass on the data sheet. Calculate the weight of the hydrate.
Record the mass of the hydrate on the data sheet.
4. Place the crucible back on the clay triangle with the lid almost covering the crucible. Heat
gently at first, then with a hot flame for 10 minutes. Allow the crucible to cool until it is
cool to the touch. Weigh the crucible and lid and record the mass on the data sheet.
5. Complete the calculations to determine the percent water in the compound. Show the
calculations on the data sheet.
6. Dispose of the BaCl22H2O. Repeat the procedure as Trial 2 on the data sheet.
1. Obtain an unknown hydrate from the stockroom and record the unknown number on the
data sheet.
2. Repeat the above procedure (Part A) and report the average percentage of water in the
unknown hydrate.
1. Get the formula mass of the unknown hydrate from the stockroom, and calculate the water
of crystallization. Show calculations on the data sheet.
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QAFQAZ UNIVERSITY LABORATORY MANUAL
Name_______________________________ Instuctor___________________________
DATA SHEET
Trial 1 Trial 2
Average ________________%
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Trial 1 Trial 2
Average ________________%
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QAFQAZ UNIVERSITY LABORATORY MANUAL
LESSON 9
SEPARATION OF A MIXTURE
Introduction: This experiment separates a mixture using the physical property of solubility.
You will learn decantation and filtration, and will use a Bunsen burner to evaporate a liquid.
You will use the Law of Conservation of Mass to check your accuracy
Background: Mixtures are combinations of substances in which the components keep their
individual characteristics, can be mixed in variable proportions and can be separated by simple
physical means. Contrast this with the composition of compounds that are inseparable by
physical changes.
Some of a mixtures components have physical properties like melting point, boiling point, or
solubility that allow us to selectively remove one component from the mixture. Then the
percentage of each component in the original mixture can be calculated.
Example: A student has a mixture of NaCl(s) and I2(s) weighing 2.75 grams. She heats the
mixture, which turns the solid iodine into a purple gas. The salt remains as a solid. After cooling
the salt, it weighs 1.59 g. To find the mass of iodine in the original sample, the student assumes
that the difference in mass of the mixture and the salt is the mass of the iodine originally present.
Thus: (2.75 g mixture 1.59 g salt) = 1.16 g iodine
The percent of iodine in the mixture:
(1.16 g iodine / 2.75 g mixture) x 100 = 42.2% iodine in this mixture.
To find the percent of salt in the mixture:
Procedure: WEAR YOUR GOGGLES! Weigh a clean dry evaporating dish to the
nearest 0.01gram. Also weigh a clean dry 250 mL beaker. Record the code # of the
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QAFQAZ UNIVERSITY LABORATORY MANUAL
sand/salt mix you are using. Weigh a 1.5 to 3 g mixture sample in the evaporating dish.
All weighings should be to two decimal places.
Add about 20 to 25 mL of
the stirring rod. Set up your funnel in a clay triangle on a tripod or iron ring over the beaker
and fit a piece of folded filter paper into the funnel. Wet the paper with a little deionized
water and set the funnel with filter paper in a clay triangle mounted on an iron ring attached
to a ring stand or a tripod.
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QAFQAZ UNIVERSITY LABORATORY MANUAL
Decant the liquid from the evaporating dish into the filter and funnel (leaving the sand in
the evaporating dish) and collect the filtrate (the liquid that passed through the filter) in the
beaker. Add 20 mL of water to the evaporating dish, decant & filter. Repeat once more. Then,
set aside the evaporating dish. (CAREFUL! Dont spill out the sand that remains in the dish.)
Squirt some water (just a few milliliters!) from your wash bottle over the filter paper and let this
drain into the beaker. Rinse the filter with small portions of water three times. Test the filtrate
as follows.
Catch a few drops of the liquid dripping out of the funnel in a small test tube. Add 1-2 drops
of 0.1M AgNO3 solution to the filtrate in the test tube (NOT to the whole portion of filtrate!). If
the mixture turns a cloudy white, salt may still be in the filter paper. Rinse the sand in the
evaporating dish two more times and test again. If still cloudy, some Cl still remains on the filter
paper. It is reasonable to stop rinsing when 120-150 mL water has been used.
Lift out the filter paper, open it up and rinse any sand granules that might have been trapped
on the paper back into the evaporating dish. Use a little deionized water from your wash bottle
to transfer any sand you find. Let the sand granules settle again in the evaporating dish, and then
decant as much water, without spilling any sand, as you can. Dry the dish with the damp sand by
placing it over the beaker as shown. Place the beaker with the salt solution on wire gauze
mounted on an iron ring over a Bunsen burner.
Weigh the beaker with the dried salt. After the first heating and cooling, these items can be
placed in an oven or gently flame dried for a few minutes, cooled and weighed again.
Never weigh an item while it is hot or even warm; it should be close to room temperature.
Disposal: The sand can be tossed in the trash and the salt rinsed into the sink.
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QUESTIONS
1. Many students do not recover 100% of the original mixture. Describe at least two possible
problems that could cause less than 100% recovery of the mixture.
2. A student received a mixture that actually contained 50.0% salt and 50.0% sand. At the end
of the experiment, this student calculated that his sample was composed of 45.2% salt and
54.8% sand. What might he have done (or not done correctly) during the experiment to
cause this error in his results?
However, this student spills her sand sample out of the evaporating dish before weighing it. If
the student believes in the Law of Conservation of Mass, what should have been the weight of
the evaporating dish with the sand in it? Show your work.
4. A student receives a sample of a mixture with three components, solid iodine that is removed
first from the mixture by evaporation, solid salt that is dissolved to separate it from the third
component, and solid sand. The salt and sand are dried and weighed but the iodine escapes
as a gas and is not recovered. The student starts with 8.35 g of mixture and recovers 2.37 g
of salt and 4.11 g of sand. What is the percent of each component in the original mixture?
Show your work. (Attach a separate sheet of paper, if necessary
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QAFQAZ UNIVERSITY LABORATORY MANUAL
LESSON 10
Unsaturated solution: All of the solute is dissolved, volume of solvent could hold more
solute at those conditions.
Supersaturated solution: If heat saturated solvent and add more solute dissolved. If
cooled to o original temperature and the solute remains in solution=supersaturated
solution.
Two liquids are miscible if they dissolve completely in each other whatever the
proportions of the components.
When two liquids are immiscible if they do not dissolved in each other.
Size, shape and charge of particles i.e. ionic, polar and nonpolar properties of matters
affect miscibility.
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- PROCEDURE
To begin with, take 12 test tubes in test tube rack. Make group of them. Four tubes for group of
solute and 3 tubes for group of solvent. Put four solutes (Na2SO4,NaCl,I2,sugar)
into test tubes. Put one solute in each three tube. Then fill that tubes with
solvents(CCl4,C2H5OH,water). Watch for changing. And take note if it is dissolved or not. Then
take 2 test tube and fill them with 1 ml water. After this step, put 2 ml of alcohol into one tube
and put ether on the other tube. Record the results of those tests according to their miscibility as
miscible or immiscible.
In the beginning of the experiment, there are two components in test tubes. After few seconds,
some of the test tubes apperance change into heterogeneous form to homogeneous form.solution
is heteregeneous. Sugar dissolved in water,on the other hand, in alcohol not much sugar
dissolved and in carbon tetrachloride neither sugar nor Na2SO4 dissolved. Na2SO4 slightly
soluble in alcohol and insoluble in carbon tetrachloride. NaCl is soluble in water,slightly soluble
in alcohol and insoluble in carbon tetrachloride.I2 is insoluble in water,soluble in alcohol and
carbon tetrachloride. The other experiments is miscibility. This experiment demonstrated that
water and alcohol is miscible and water and ether is immiscible.
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QAFQAZ UNIVERSITY LABORATORY MANUAL
LESSON 11
calculate H.
Objectives After completing this experiment, students should be able to do the following:
1. Define:
2. Given the heat capacity of a calorimeter system, the moles of reactants participating in the
reaction, and
the temperature change for the reaction, find the values for q and H for the reaction.
INTRODUCTION
The energy changes that accompany chemical reactions are nearly always reflected by the
release or
absorption of heat. There are many practical and theoretical reasons for studying the quantitative
aspects
You will measure the enthalpy change for three reactions. The enthalpy change, H, under our
lab
conditions is equal to the amount of heat lost or gained during the reactions. First, you will
measure the
enthalpy change that occurs when solutions of sodium hydroxide (NaOH) and hydrochloric acid
(HCl) are
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QAFQAZ UNIVERSITY LABORATORY MANUAL
mixed. Then you will measure the enthalpy change that occurs when solutions of ammonia
(NH3) and
hydrochloric acid are mixed. Third, you will measure the enthalpy change that occurs when
solutions of
The chemical reactions that will occur during this experiment are given in the following
equations:
The three chemical reactions that will occur in this experiment are examples of bases reacting
with acids.
You will learn much more about acids and bases in General Chemistry II. For now, simply
recognize
The heat evolved or absorbed during these reactions will be measured with a coffee-cup
calorimeter. In
order to determine the enthalpy change from a measured change in temperature, you will have to
utilize
the fundamental concepts of calorimetry and thermochemistry. You may or may not have gotten
to this
point in the lecture portion of the class, but you can refer to the Appendix at the end of this
experiment for
a step-by-step description and examples of the calculations you will perform in order to
determine the
enthalpy change for the three reactions, H1, H2, and H3. You should determine these with
units of
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kJ/mol. Once you have determined your individual H values, class data will be pooled in order
to 2
determine average H values for each of the three reactions. You will report your values and the
class
averages on the report sheet. Post-lab question 2 asks you to consider the value for H3 more
closely.
This question relies on the fact that you can use your values for H1 and H2 to calculate H3
directly.
Note the following relationship among the studied reactions: If Rxn. 1 is combined with the
reverse
of Rxn. 2, the third equation is generated. This relationship provides the basis for using Hess's
law
of heat summation. The post-lab question asks you to attempt to predict the enthalpy change for
the
third reaction by combining the enthalpy changes for the first and second reactions.
PROCEDURE
1. Obtain exactly 50.0 mL of the 3.0 M solution of HCl in a clean, dry graduated cylinder. Pour
the
liquid into your coffee-cup. Rinse the graduated cylinder with distilled water from your wash
bottle. Dry the cylinder. Obtain exactly 50.0 mL of the 3.0 M NaOH using the graduated
cylinder.
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2. Measure the temperature of the solution in the coffee-cup. Record this temperature as the
initial
temperature, Ti
4. Immediately, place the top on the calorimeter and begin swirling the cup. Do not stir the cup
with
the thermometer!
5. Record the temperature to the nearest 0.1 C at the times listed in your data table.
6. Repeat the procedure of the HCl-NaOH reaction for trials involving the following acid base
pairs
and amounts:
7. Using Excel, obtain a scatter plot of the temperature (y-axis) against the time (x-axis) on one
set
of axes. Print out your plots without performing a linear regression. Manually extrapolate your
results to the time of mixing (time = 0 s) on the y-axis. This is done by drawing a straight line
through your points and extending it back to t=0. The temperature at which your line crosses the
axis is Tf
8. Calculate H in units of kJ/mole for each reaction. Use 430 J/C for the heat capacity of the
calorimeter plus contents. See the appendix for an explanation of this calculation.
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LESSON 12
Exothermic means to release heat. Its etymology stems from the Greek suffix thermic,
meaning to heat, and the Greek prefix exo-, meaning outside. It refers to a transformation in
which a system gives heat to the surroundings: Q < 0. When the transformation occurs at
constant pressure: H < 0; and constant volume: U < 0. If the system undergoes a
transformation which is both exothermic and adiabatic, its temperature increases.
Endothermic means to absorb heat. Its etymology stems from the Greek suffix thermic,
meaning to heat, and the Greek prefix endo-, meaning inside. It refers to a transformation in
which a system receives heat from the surroundings: Q > 0. When the transformation occurs at
constant pressure: H > 0; and constant volume: U > 0. If the surroundings do not supply heat,
an endothermic transformation leads to a drop in the temperature of the system.
Laboratory Coat
Laboratory Scale
Test tube
Test rube rack
Test tube holder
Thermometer
Stirrer
Clamp
Hot plate
Test tube brushes
Graduated cylinder
Beaker
Spatula
Funnel
Volumetric flask
Wash bottle
Dropper
Distilled water
Tap water
KNO3
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B- PROCEDURE
First, fill a beaker three-fourths of tap water and heat it. Calculate 2 gr of KNO3 with
laboratory scale and put it into test tube. Fill that test tube with distilled 5 ml water. When tap
water is boiled, put the test tube which has KNO3 and water mixture into beaker with
thermometer. Watch for dissolving. When all KNO3 dissolved record the temperature. Then start
cooling it down. When KNO3 starts to begin crystallized, record the crystallization temperature.
There is heteregeneous mixture in the test tube first. After few second it starts to dissolve
slowly. When it penetrated into boiled water KNO3 starts to dissolve faster. In 72 degree of
celcius, all KNO3 in the test tube dissolved. After cooling it down, there is crystals in the bottom
of the test tube. And the temperature is 26 degree of celcius.
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LESSON 13
Aspirin synthezise
Materials
3.0 g salicylic acid
6 mL acetic anhydride*
5-8 drops of 85% phosphoric acid or concentrated sulfuric acid*
distilled water (about 50 mL)
10 mL ethanol
1% iron III chloride (optional, to test purity)
*Use extreme caution when handling these chemicals. Phosphoric or sulfuric acid
and acetic anhydride can cause severe burns.
Equipment
filter paper (12.5 cm)
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3. Gently swirl the flask to mix the solution. Place the flask in a beaker of warm water for
~15 minutes.
4. Add 20 drops of cold water dropwise to the warm solution to destroy the excess acetic
anhydride.
5. Add 20 mL of water to the flask. Set the flask in an ice bath to cool the mixture and speed
crystallization.
6. When the crystallization process appears complete, pour the mixture through a Buckner
funnel.
7. Apply suction filtration through the funnel and wash the crystals with a few milliliters of
ice cold water. Be sure the water is near freezing to minimize loss of product.
8. Perform a recrystallization to purify the product. Transfer the crystals to a beaker. Add 10
mL of ethanol. Stir and warm the beaker to dissolve the crystals.
9. After the crystals have dissolved, add 25 mL of warm water to the alcohol solution.
Cover the beaker. Crystals will reform as the solution cools. Once crystallization has
started, set the beaker in an ice bath to complete the recrystallization.
10. Pour the contents of the beaker into a Buckner funnel and apply suction filtration.
11. Remove the crystals to dry paper to remove excess water.
12. Confirm you have acetylsalicylic acid by verifying a melting point of 135C.
13. You can compare the actual and theoretical yield of acetylsalicylic acid
based on the initial quantity of salicylic acid. Can you identify the limiting
reactant in the synthesis?
14. You can compare the quality of the synthesized aspirin with commercial
aspirin and salicylic acid. Add one drop of 1% iron III chloride to separate
test tubes containing a few crystals of each substance. Observe the color:
Pure aspirin would show no color, while salicylic acid or traces of it in
impure aspirin will show a purple color.
15. Examine the aspirin crystals under a microscope. You should see white
small-grained crystals with obvious repeating units.
16. Can you identify the functional groups in salicylic acid? Can you predict
how these groups affect the properties of the molecule and how the body
reacts to it? Salicylic acid has an -OH group (an alcohol) and a carboxyl
group -COOH (an organic acid). The acid portion of the molecule is one of
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Why do you think the aspirin was washed with distilled water? How did this
affect the end product? How did this affect the actual product yield? Washing
the aspirin removed most of the unreacted salicylic acid and acetic anhydride to
yield a purer product. Some product was dissolved and lost in the washing
process. Cold water was used to miminize dissolving the product.
How did the synthesis use different temperatures to affect solubility of aspirin?
At higher temperatures (warm water), molecules have more kinetic energy and
collide with each other more often to interact with water molecules, increasing
the solubility of the aspirin. The ice bath slowed the molecules, allowing them
to more easily stick together and "fall out" of solution or crystallize.
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