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Manual Lab 403106
Manual Lab 403106
Department of Chemistry
Credit hours: 1
Reports: 20%
Course Contents:
Exp.1: Density
Mid-Term Exam
Exp.8: Calorimetry
Missed Labs: Unexcused absences will result in a grade of zero for the lab missed.
No make-up labs will be allowed for unexcused absences.
Excused absences result in the averaging of the student's other lab grades and
substituting this average grade for the lab missed.
Unexcused absences result in a 0 (zero) for that lab meeting's quiz grade and
technique grade.
Lab Reports
Lab reports consist of data, observations and calculations. We do not want students to
spend a lot of time writing long lab reports. Be clear, be concise. You will not impress
your TA by copying pages from the Manual or Text; you will impress your TA if they
can easily read and understand what you write. You must think about what happened
in lab and make conclusions on what you saw, and not what the book says.
You will be evaluated at the end of the term and will be worth 5% of your overall
grade. The "technique" grade is basically an "attendance" grade. Attendance in this
case means not simply physical presence, but whether or not you are paying attention
to what you are doing. The maximum number of points will be awarded to students
who:
Show up on time.
Use the equipment properly.
Are fully prepared for lab.
Follow all safety rules.
Perform laboratory functions safely and efficiently.
Work carefully in the lab to avoid breakage, spills, contamination, and
fire.
Properly dispose of waste.
Clean up their bench and common work areas.
Isolate pure product and in high yield.
You can ask your TA how to do a procedure and not be penalized by losing points.
You are here to learn to do inorganic chemistry lab techniques, and you cannot do this
if you do not ask questions. If you constantly ask your TA what to do next, you are
not able to perform the experiments.
The technique grade is assigned by your TA. It may or may not be assigned each lab
meeting; your TA may keep simple plus and minus notes in their grade record.
Technique grade cannot be assigned on the basis of your lab report; it must be
assigned according to visual observations of each student in lab. Yes, it is subjective.
You may be doing stellar work most of the time and your TA does not see you until
you drop your flask.
Laboratory Safety Rules
Keeping the lab safe is the number one priority and it is everyone’s
responsibility. Before you begin, read safety rules in your lab book. The following
rules are very important for your safety as well as the safety of other students. Please
read them carefully and follow them each laboratory period.
Contact lenses must not be worn in the lab. Solvent vapors can get trapped behind
hard lenses and remain in contact with your eyes for extended periods. Soft lenses can
dissolve and be fused to your eyes. This is not pleasant. Please wear your goggles.
To avoid skin exposure in case of spills, shorts and open toed shoes
(sandals) are not allowed.
Never taste anything. Never directly smell the source of any vapor.
Memorize the location of all exits, showers, eye washes, fire
extinguishers, and fire blankets.
Always pour acids into water and not vice verse.
No food or beverages are allowed in the lab.
Perform all reactions producing gases or unpleasant odor in the fume
hood.
Be certain that there are no flammables in the area when lighting a
flame.
Be alert for hazards in the lab. Do not proceed with any experiment
until you understand the hazards involved.
Report all injuries to your instructor, even if they appear to be minor.
Do not come into contact with any of the solvents or reagents used in
this lab other than soap and water. Remove gloves and wash hands
before leaving lab.
Clean up all chemical spills (this includes drips on bottles) and all
broken glassware immediately.
Do not leave any bottle uncapped.
Dispose of all wastes as directed. (Ask before you dump.)
Do not come to the lab unprepared.
COMMON LABORATORY APPARATUS
Dilution mark Volumetric Flasks are used to measure precise volumes of liquid or to
make precise dilutions
Reading a Meniscus
Care of Reagents
Each of the balances you will be using costs somewhere in the neighborhood of $2000 to
$2500. Therefore, care must be exercised in using them. Below is a simple outline that
will help you to use the balance more effectively, safely, and will assist in reducing the
speed at which the Stockroom Manager’s hair is turning prematurely gray.
1. Select a suitable container (usually a weigh boat, weigh paper, or glassware) to
weigh the chemical in.
2. Remove the balance cover.
3. Place the container on the balance pan and replace the balance cover. Replacing
the balance cover will greatly reduce fluctuations in the balance reading!
4. Allow the balance reading to stabilize. Zero the balance by pressing the TARE
button or bar which is located at the front of the balance. DO NOT hold down the
tare button/bar! This will cause the balance to change units and you may end up
weighing your chemical in units other then grams which will cause your data to be
in error!
5. Remove the balance cover and carefully transfer the desired chemical to the
container. If you use a spatula, use only a clean, dry spatula for obtaining dry
chemicals. If you should spill a chemical on the balance pan, use the brush that is
attached to the balance to clean the balance pan IMMEDIATELY! Chemicals left
on the balance pan will corrode the pan.
6. Replace the balance cover and allow the balance reading to stabilize. In the event
you weigh out too much chemical, remove the excess to a secondary container.
NEVER return a chemical to its original container! There will always be some left
over. Try to find someone else who needs it before disposing of it.
7. Discard chemicals as directed in each experiment (See the Safety and Disposal
section for each experiment).
8. Record the balance reading in your notebook.
9. Remove the container from the balance pan and replace the balance cover.
10. Replace the appropriate lids on all reagent bottles when finished.
Titration
Density
Objectives:
1. Use measuring tools correctly.
2. Read and record measurements correctly (significant digits and unit).
3. Associate metric units with the quantities being measured.
4. Determine the density of a liquid and solid.
Introduction:
Density is a measure of a substance’s mass-to-volume ratio. For liquids and solids,
density is usually expressed in units of g/mL or g/cm3; these are equivalent since 1 mL is
exactly equal to 1 cm3. Density is an intensive property meaning that a substance’s density
will be the same regardless of the size of a sample. For example, steel has a density of 7.85
g/cm3 whether you have a tiny steel bar or a large steel bar. The mass and volume of each
piece will be different, but the mass-to-volume ratio is the same.
The density can be measured by two different techniques: 1) volume calculation based on
water displacement and 2) volume calculation using measurements of the radius and length of
the cylinder using caliper or ruler. The volume of a solid can also be determined by
displacement. A solid that is more dense than water will sink and displace a volume of liquid
equal to the volume of the solid object. Such a volume measurement is typically made in mL.
(Remember, 1 mL = 1 cm3.)
In this laboratory, you will practice taking measurements and recording them to the
correct degree of uncertainty while determining the density of various samples. Density is
defined as mass per unit volume and can be calculated using the equation:
Mass of Sample m
Density= or D =
Volume of Sample V
In science the metric system is used almost exclusively. The basic unit of length is the
meter (m); of mass, the gram (g); of volume, the liter (l). The meter, the gram, and the liter are
related to larger and smaller units by multiples of 10. Prefixes are used for the unit of measure
expressing these multiples of 10.
How does 1 kilometer compare to the other units in the metric system?
Uncertainty in Calculations:
Measured quantities are often used in calculations in lab. The precision of a calculation
is limited by the precision of the measurements on which it is based.
Addition and Subtraction:
When measured quantities are used in addition or subtraction, the final answer is limited
by the least decimal place in which all digits are significant. In this example, The
tenths place (one after the decimal place) is the least decimal place.
Example: 32.01 m + 5.325 m + 12.1 m = 49.435 m
The sum of the numbers is 49.435, but the sum should be reported as 49.4 meters
because 12.1 m is only known to the tenths place.
When experimental quantities are multiplied or divided, the answer is limited by the
number in the calculation with the fewest number of significant figures than any of the
original numbers.
Your calculator will read 1.02616, but the final answer should be reported as 1.0 g/mL
because 25 mL only has 2 significant digits.
and burets:
When water is measured in a narrow glass container the top of the water does not form a
straight line. It forms a curved line called a MENISCUS. To read the volume correctly, adjust
the apparatus so that the bottom of the meniscus is at eye level and record the volume at the
bottom of the meniscus.
Irregular Solid
1. Using a 100 mL graduated cylinder, obtain roughly 20 to 30 mL volume of an irregular
solid sample.
2. Record your sample number (or substance name).
3. Determine and record the mass of your sample (be sure it’s dry).
Trial 1 Trial 2
1. Mass of liquid ………g ………g
2. Volume of liquid ………mL ………mL
3. Density of liquid ………g/mL ………g/mL
Trial 1 Trial 2
2. Mass of liquid ………g ………g
3. Volume of liquid ………mL ………mL
4. Density of liquid ………g/mL ………g/mL
Irregular Solid
1. Sample number ………
2. Mass of sample ………g
3. Initial water volume ………mL
4. Final water volume ………mL
5. Volume of sample* ………mL
The “CRC” (short for Chemical Rubber Company Handbook of Chemistry & Physics) is a
commonly used source of physical and chemical data. Among the information compiled in
this resource are the density values for all of the solid and liquid elements and numerous
compounds. Refer to this data when identifying your unknown substance.
lead 11.3
gold 19.3
copper 8.96
aluminum 2.70
iron 7.87
zinc 7.14
tin 7.265
potassium chloride 1.988
Chloroform 1.4788
1, 2-ethanediol 1.1135
glycerol 1.2613
Carbon tetrachloride 1.594
ethanol 0.7893
water 0.998
Objective:
To separate a heterogeneous mixture based on each component's physical
properties.
Introduction:
A mixture is a physical combination of two or more pure substances where
each substance keeps its own chemical identity. For example, each substance in
a salt-water mixture has the same chemical properties as its would have when
pure, the water is present as H2O molecules and the salt is present as sodium ions
(Na+) and chloride ions (Cl-).
The method chosen for separating the mixture is based on the differences in
the chemical and/or physical properties of the mixture's components. Some
common physical methods for separating a mixture's components include:
f- Sublimation: vaporizing a solid and recondensing its vapor (not all solids
sublime, however);
Solubility
Compound Molar Mass (g/100 g water Melting Point Appearance
at 25oC)
Experimental Procedure:
1- Weigh a clean, dry, evaporating dish and record its mass on the report
sheet.
2- Add about 2 g of the unknown mixture to the dish, weigh and record the
mass.
4- Heat the dish slowly, but gradually increase the heat until the white fumes
of ammonium chloride stop vaporizing (approx. 15 minutes).
5- Cool the dish to room temperature, weigh, and record the mass on the report
sheet.
6- Add about 20ml of distilled water to the solid in the evaporating dish and
stir for about one minute. Decant the solution into a beaker. Add about 10
ml more of distilled water to the solid, stir again for about one minute, and
decant into the beaker. Repeat once the 10 ml washing and decant them
into the beaker.
8- First air-dry the solid on the filter paper, and then in a 100oC constant-
temperature drying oven for about 10 minutes.
9- Allow to cool to room temperature, weigh, and record the mass on the
report sheet.
10- At the end of the laboratory period, wash the funnel and the evaporating
dish. Dispose of any sand in the waste beaker.
Limiting Reactant
Objectives:
To determine the limiting reactant in a salt mixture.
To determine the percent composition of a salt mixture.
Techniques:
To effectively complete the experiment's objectives, review the following
techniques:
Technique 2d, 3 Transferring a liquid.
Technique 5 Decanting a liquid from a solid.
Technique 6 Flushing a precipitate from a beaker.
Technique 7 Folding filter paper for a filter funnel.
Technique 8 Filtering procedures.
Technique 19b Weighing on a balance, 0.001 g.
Introduction:
Two factors that limit the yield of products in a chemical reaction are (1)
the amounts of staring materials (reactants) and (2) the percent yield of the
reaction. Many experimental conditions-for example, temperature and pressure-
can be adjusted to increase the reaction's yield but because the chemicals react
according to fixed mole ratio (stoichiometrically), only a limited amount of
product forms from given amounts of starting materials. The reactant restricting
the amount produced is called the limiting reactant in the chemical system.
To better understand the concept of the limiting reactant, let's look at the
reaction studied in this experiment. The equation's molecular form is:
Ba3 PO4 2 6 NaCl 30H 2 O............. (1)
2 Na3 PO4 .12H 2 O 3BaCl 2 .2H 2 O
Since the reactant salts are soluble, Ba3 PO4 2 is insoluble, and NaCl soluble,
the ionic equation is:
Ba 3 PO4 2 6Na Cl H 2 .......... (2)
6Na 2PO43 24H 2 O 3Ba 2 6Cl H 2 O
Presenting only the reacting ions in the reaction (removing spectator ions), we have:
Ba3 PO4 2( s ) ......................(3)
2 PO43 3 Ba 2
Two moles of phosphate ion from 2 moles of Na3PO4. 12H2O (F.W. = 380.2), or
760.4g reacts with 3 moles of barium ion from 3 moles of BaCl2. 2H2O (F.W. =
1molBaCl2. 2 H 2O
700 .0 g Ba3Cl2. 2 H 2O 2.87 mol BaCl2. 2 H 2O
244 .2 gBaCl2. 2 H 2O
2.87 mol Ba 2
Equation 3.3: indicates that 2mol PO43 reacts with 3mol Ba 2 . With
1.84 mol PO43 present, is enough Ba 2 present for all of the PO43 to react?
Again, using Equation 3.3 and the 3:2 mol ratio of Ba 2 to PO43 .
3mol Ba 2
1.84 mol PO43 2.76 mol Ba 2 reacts with 1.84 PO43
2mol PO43
Since only 2.76mol Ba 2 of the 2.87 mol Ba 2 added to the system reacts
with the 1.84 mol PO43 , PO43 is the limiting reactant, Ba 2 is the excess
reactant. In other words, all of the PO43 reacts, but not all the Ba 2 . An excess
of 2.87 2.76 0.11mol Ba 2 remains unreacted.
Experimental Procedure:
Two trials are recommended for this experiment. To hasten the analyses,
weight duplicate unknown salt mixtures and simultaneously follow the procedure
for each. Label the beakers accordingly for Trial 1 and 2 to avoid intermixing
samples and solution.
A- Precipitation of Ba3(PO4)2:
1- Weigh on weighing paper (+0.001 g, Technique 19b) about 1.0g of an
unknown Na3PO4.12H2O-BaCl2.2H2O salt mixture (see your instructor).
Transfer it to a 400-mL beaker and add 200mL (0.2mL) of distilled (or de-
ionized) water. Stir the mixture with a stirring rod for about 1 minute and
then allow the precipitate to settle.
2- Cover the beaker with a watch glass and maintain the solution hot (80-
90oC) on a steam bath or with a low flame for 30 minutes (Figure 3.1).
Allow the precipitate to settle.
3- Decant (Technique 5) two 50-mL (0.2 mL) volumes of the supernatant
liquid into separate 100mL beakers, labeled beaker I and Beaker II. Save
for part B.
Figure (3.1): Warming the precipitate. Figure (3.2): Transfer of Ba3(PO4)2 precipitate
to filter
Figure (3.3)
Limiting Reactant
Student Name: Lab. Section:
A- Precipitation of Ba3(PO4)2:
Calculation:
Colligative Properties
Objective:
To determine the molar mass of a non-electrolyte compound in water by
measuring the freezing point of pure water and of solution.
Introduction:
The properties of a solution differ considerably from those of the pure
solvent. Those solution properties which depend primarily on the concentration
of solute particles rather than their nature are called colligative properties. These
properties include vapor pressure lowering, osmotic pressure, boiling point
elevation and melting point depression. The relationships among colligative
properties and solute concentration are best regarded as limiting laws. They are
approached most closely when the solution is very dilute. In practice, the
relationships are valid, for nonelectroytes to within a few percent at
concentrations as high as 1M.
are directly proportional to the number of solute particles per mole of solvent
molecules. ∆T = Tsolvent − Tsolution
∆Tb = K b x m ∆T f = K f x m
Where K b and K f are the solvent's molal boiling point and freezing point
constants respectively, which have the unit of oC.kg mol-1, and m is the molality
of the solution which is the number of moles of solute per one kilogram of
solvent.
Figure 2, cooling curve for a pure solvent, shows you see a steady decrease
in temperature followed by a dip which is followed by a slight rise in the
temperature. This dip is not unusual and results from supercooling during the
early stages of the freezing process that may occur before freezing. Supercooling
results when a solution cools below its normal freezing point without freezing.
When solute is added to the solvent the shape of the cooling curve
sometimes changes so that we don’t see a clear horizontal plateau, as shown in
cooling curve for solution (Figure 2). In this case we must draw a trend line
through the data points corresponding to the cooling of the liquid and a trend line
through the data points corresponding to the freezing of the liquid. The
temperature at the point where those two lines intersect is the freezing point of
the solution (see Figure 3).
Example:
What would be the freezing point and boiling point of a solution containing
65.0g of ethylene glycol (C 2 H 6 O 2 ) commonly used as an automotive antifreeze,
in 200.0 g of water. (for pure water K f = 1.86oC/m, K b = 0.52oC/m, T f = 0Co, T b
= 100oC).
Moles of C 2 H 6 O 2 = mass/molar mass = 65.0g/62.0 g/mol = 1.05 mol
T f ( solution) = T f ( water ) − ∆T f
Tb ( solution) = Tb ( water ) + ∆T f
Procedure:
2- Weigh an empty and dry 200-mL test tube, and add 30.0 mL of water. Place
a thermometer in the test tube (Figure 4) and record the temperature under
time = 0 seconds on the data sheet.
3- Insert the test tube deep into the ice bath, carefully stirring the solution
continuously with the wire stirrer, and record the temperature every 30
seconds on the data sheet.
4- Record the freezing point of water for 300 seconds (5 minutes): the
temperature at which two phases (ice and water) co-exist.
5- Using graph paper, plot temperature versus time and determine the freezing
point of water.
2- Add 2.5 g of the solid unknown and carefully add it to the test tube. Stir the
mixture until the entire unknown has dissolved. Replace the thermometer and
record the temperature (time = 0) on the data sheet.
3- Determine the solution's freezing point in the same way as the solvent's was
found in Part A.
4- On your graph paper, plot temperature versus time and determine the
freezing point of the solution as before (see Figure 2).
Colligative Properties
Student Name: Lab. Section:
Calculations:
Pure water
Objectives:
1- To standardize sodium hydroxide solution.
2- To determine the molarity of strong acid solution.
Introduction:
Titration is a term used to describe an experiment in which one solution is
added to another using a burette. The two solutions contain to compounds which
react rapidly with each other. The solution in the burette is added until there is
evidence that the reaction between the two compounds is complete.
Acid-base reactions are one of the most common types of chemical
reactions. The reaction between an acid and a base can be represented by the
equation:
H (aq) OH (aq) H 2 O(l ) 1
Mass of KHP
Moles of KHP = moles of NaOH or M NaOH VNaOH
Mwt of KHP
Example (1):
In an acid-base titration, 20.15 mL of NaOH solution was required to
neutralize 0.491 g of KHP (molar mass = 204.23 g/mol). What is the molarity of
the NaOH solution?
Mass of KHP
M NaOH VNaOH
Mwt of KHP
0.491 g
M NaOH 0.02015 L
204 .23 g / mol
Example (2):
The standardized NaOH solution (0.119 M) was titrated against 28.10 mL
of H2SO4. The volume of the standardized NaOH solution needed to neutralize
the H2SO4 solution was 24.28 mL. What is the molarity of the H2SO4 solution?
( M NaOH ) (VNaOH ) 2( M H 2 SO4 ) (VH 2 SO4 )
M H 2 SO4 0.0512 M
Procedure:
Introduction:
It is important to know the composition of common substances at home and
handle them safely. In case of an accident the fast action is important before
taking the injured person to the hospital if it is needed, identification of
substances can be done either by instruments or by chemical tests of identify
some household items.
Warning:
"Never mix household chemicals unless you know what you are doing.
Mixing chemicals sometimes produces explosion, fires, or other hazardous
reactions".
Procedure:
Another test for Cl- is to convert it to a white solid AgCl by treatment with
AgNO3(aq):
Place about 0.5g of table salt in a test tube, add two drops of concentrated
H2SO4 Solution. Note the smell of the gas. Test the gas by a wet blue litmus
paper. Dissolve about 0.5g of NaCl in a test tube by adding 1ml of distilled
water and a drop of 3M HNO3 solution, then add 4 drops of 0.1M AgNO3
solution. Record your observations.
and Vinegar:
Baking soda is sodium bicarbonate (NaHCO3), which is a basic salt that can
be reacted with acids to form CO2(g):
The CO2(g) evolved helps to raise the cake or dough. Lemon juice is simply
citric acid, and vinegar is a dilute solution of acetic acid. Both acids react with
baking soda.
Place about 0.5g of baking soda in a test tube, add 1-2ml of lemon juice or
vinegar. Record your observations. The test for escaping CO2(g) can be done by
holding a drop of Ba(OH)2 solution at the tip of a dropper, and inserting the
2 Chemistry 106 Experiment 6
dropper down into mouth of the test tube. Clouding of the Ba(OH)2 drop is a
proof for the presence of CO2(g) due to the formation of BaCO3(s):
CO2( g ) Ba(OH )2( aq) BaCO3( s ) H 2O(1)
The test for evolved CO2(g) can be done as described above (in part D).
Place about 0.5g of limestone, CaCO3, into a test tube. Add 1-2ml of the
bathroom cleaner, record your observations.
Warning:
Bleach is a toxic material and has an irritating odor. Avoid direct contact
with skin.
H- Unknown:
Receive an unknown solid from your instructor. The unknown contains one
of the following ions: CO32 , Cl , SO42 , or I-, Place a small amount of the
unknown in a dray test tube and add a drop of 18 M H2SO4. Use the following
table in determining the ion present in the unknown:
Ion Reaction
SO42 No Reaction
Observations:
A- Glass Cleaner:
1- Change of litmus paper : …………………………………
2- Reason for the change : …………………………………
B- Fertilizer:
1- Change of litmus paper : …………………………………
2- Describe the smell of gas : …………………………………
3- The smell is due to the formation of : …………………………………
C- Table Salt:
1- Describe the smell of the gas formed : …………………………………
2- The gas formed is……………… and it will turn a ……………… litmus paper
into ………………
3- When AgNO3 solution is added to the salt solution, a ……………… solid is
formed which is ………………
D- Baking Soda:
1- Observation from the addition of lemon juice or vinegar to baking
soda:………………
2- Observation and equation of holding a drop of Ba(OH)2: ……………………
E- Bathroom Cleaner:
1- Observation and equation of addition of the cleaner to limestone: ……………....
G- Drain Opener:
1- Observation from the addition to warm water to the drain opener:
2- The changes of litmus paper:…………………………………………………….
H- Unknown:
1- Unknown No. is: …………………………………………………………………
2- Unknown Ion: ……………………………………………………………………
3- Confirmatory tests: ………………………………………………………………
Objectives:
To Separate and identify of some insoluble chlorides: Ag+, Hg22+, and Pb2+
Introduction:
Qualitative analysis is a method of finding out what kind of chemicals
(compounds, elements or ions) are presented in a sample regardless of their
quantities or concentrations. Based on the physical and / or chemical behavior of
a certain chemical we will be able to determine whether this chemical is present
or not in an unknown sample. We usually use the expression positive test: test
which indicates that the substance is present, and negative test: test which shows
that the substance is not present in the sample or its concentration is too low to be
detected by this test. The evidence for a positive test is one or more of the
following observations:
a- Formation, disappearance or changing of a color.
b- Formation or disappearance of precipitate.
c- Formation of a gas.
d- Change in the temperature.
e- Change in the reading of an instrument.
In this experiment, you are going to identify some cations (Ag+, Hg22+ and
Pb2+) and detect them in unknown solutions. According to the solubility of their
chloride salts, these cations can be considered as insoluble chlorides. Thus by
adding a Cl- ion the insoluble salts (AgCl, Hg2Cl2 and PbCl2) precipitate and the
other cations stay in solution. The precipitate and the solution (supernatant) can
be separated after centrifugation, then the cations in each side can be identified
using certain chemical test.
This known solution contains all cations (insoluble chlorides) which you
are going to separate and analyze. Performing this analysis in a systematic way
(following the procedure step by step as shown below) is very important to
obtain correct results.
B- Test of Hg22+:
Ammonia, NH3, reacts with both Hg2Cl2 and AgCl. With Hg2Cl2 the
reaction produces a grey precipitate due to the formation of elemental black Hg(l)
and white mercury(II) amidochloride (HgNH2Cl). Reaction of AgCl with NH3
Hg (l ) HgNH 2 Cl NH 4 Cl (aq)
Hg 2 Cl 2 NH 3
Black White
To the precipitate (from step A above) add 10 drops of 6 M NH3, stir and
centrifuge the solution. Formation of a grey to black precipitate indicates the
presence of Hg22+. Transfer the supernatant solution to clean test tube and keep it
for the next step.
Ag ( NH 3 ) 2 Cl H
NH 4 AgCl ( s ) (white precipitat e)
Mark each action below to indicate if it is present (+ve) or absent (-ve) in your
unknown.
Ion Result (+ve or -ve)
a- Pb2+ ………………………
b- Hg22+………………………
c- Ag+ …………………………
Calorimetry
Objectives:
1- To determine the quantity of heat evolved in the neutralization of strong acid
with a strong base.
2- To determine the quantity and direction of heat flow for the dissolving of a
salt in water.
4- In another reaction (which we shall not perform in the lab.), we could add
distilled water to aqueous solution of sodium chloride. The heat released is
the heat of dilution. This effect was present in the reactions of step 1, 2 and
3 above; but we shall neglect this heat of dilution in our calculations because
it is smaller than the experimental errors expected in the measurement of the
other heats.
5- The final experiment of this laboratory class will be to determine the heat of
solution of an unknown salt, as in step 1 above.
Example (1):
f- Heat of reaction in KJ/mol = -6.970 x104 J/mo x(1 KJ/103J) = -69.70 KJ/mol.
Note: The difference in the heat of reaction (Example 2) and the heat of solution
(Example 1) is the heat of neutralization (Hn). So the heat of
neutralization of NaOH with HCl is -57.30 KJ/mol.
Hn is generally expressed in units of KJ/mol of acid (or base) reacted. Mass (g)
equals the combined masses of the two solutions. The heat of neutralization ,Hn,
is determined by (a) assuming the density and the specific heat of the acidic and
basic solutions are equal that of water, and (b) measuring the temperature, T ,
when the two are mixed:
Hn = mass of solution (g) x specific heat of solution (J/g.oC) x T ( oC )
2- Close the calorimeter and stir the water until a constant temperature is
reached. Measure the initial temperature of water.
3- Weigh 2.0 g of NaOH. You should weight the NaOH fast, since it is very
Hygroscopic.
4- Add the solid NaOH to the 100 ml of water in the calorimeter and stir
gently until the maximum temperature reached.
2- Close the calorimeter and stir the solution until a constant temperature is
reached. Measure the initial temperature of solution.
3- Weigh 2.0 g of NaOH. You should weight the NaOH fast, since it is very
Hygroscopic.
4- Add the solid NaOH to the HCL solution in the calorimeter and stir gently
until the maximum temperature is reached. Measure the maximum (Final)
temperature.
2- Repeat the procedures in part A, using 3.0g of the unknown salt in place of
NaOH.
Calorimetry
Part B. Determination of the heat of reaction of NaOH (H2) and the heat of
neutralization:
Trail 1 Trial 2
Volume of HCl ……………. …………….
Mass of HCl ……………. …………….
Mass of NaOH ……………. …………….
Molar mass of NaOH ……………. …………….
Mass of solution ……………. …………….
Initial temperature ……………. …………….
Final temperature ……………. …………….
Spectrophotometric Determination of an
Equilibrium Constant
Objectives:
1- To determine the equilibrium constant for the formation of a complex ion,
[Fe(H2O)5(SCN)]2+. This will be accomplished by using a spectrophotometer to
measure absorbance data, from which equilibrium concentrations can be
calculated with the Beer-Lambert Law, A = l c.
2- To use graphing technique and data analysis to evaluate data.
Introduction:
There are many reactions that take place in solution that are equilibrium
reactions; that is, they do not go to completion, and both reactants and products
are always present. Examples of this type of reaction include weak acids such as
acetic acid dissociating in water, weak bases such as ammonia reacting with
water, and the formation of "complex ions" in which a metal ion combines with
one or more negative ions. We will study a reaction involving the formation of a
complex ion which occurs when solutions of iron(III) are combined with the
negative thiocyanate ion; they form a deep red color FeSCN2+ complex, in which
all species are soluble. The system studied is:
where Aeq is the absorbance of the equilibrium mixture and Astd is the absorbance
of the standard.
In preparing the standards, the Fe3+ concentration is much larger than SCN-
concentration. According to LeChatelier's principle, this should cause the
equilibrium in eq. 2 to shift far to the right; therefore the FeSCN2+ concentration
approximates the original SCN- concentration. In other words, we assume that
the position of equilibrium is driven so far to the right by the excess Fe3+ that all
of the SCN- is complexed, forming FeSCN2+.
2. Equilibrium Concentration of Fe3+. For each one mole of FeSCN2+
produced, one mole of Fe3+ must be consumed. The equilibrium concentration
of Fe3+ can be calculated as follow:
[ Fe 3 ]eq [ Fe 3 ]in. [ FeSCN 2 ]eq (6)
b) FeSCN2+ concentration:
[ FeSCN 2 ]std [SCN ]in 9.0 10 4 M
[ FeSCN 2 ]eq
K eq
[ Fe3 ]eq [ SCN ]ec
0.00068 M
K eq
(0.00052 M ) (0.0053 M )
Keq = 2.5 x 102 (2 significant figures)
CAUTION
All solutions contain nitric acid (for stability) which is very corrosive to
skin and eyes. Wash spills off yourself as quickly as possible. Neutralize spills
on the lab table with baking soda. Wash your hands before you leave the lab.
Procedure:
0.002 M Fe(NO3)3 - produces [Fe(H2O)6]3+ (or simply Fe3+) in solution
Stock solutions:
0.002 M KSCN - produces SCN- in solution
2. Make sure that the wavelength in the spectrophotometer is set at 447 nm.
3. Measure the absorbance for the blank solution (the solution that has only
0.500 M HNO3) and adjust the absorbance (A) to zero and the transmittance
(%T) to 100%.
4. Determine the absorbance (A) of each standard solution and record your
results in a table in your report sheet.
2. Measure the absorbance at 447 nm (A) for each solution by following the
same procedure above (step 2-5 in part A). Record the results in a table in
your report sheet.
[FeSCN2+]std = [SCN-]in
Absorbance (Astd)
[Fe3+]in
[SCN-]in
Absorbance, A
[FeSCN2+]eq
[Fe3+]eq
[SCN-]eq
Keq
K eq n 1
Objectives:
1- To determine the molar solubility and Ksp of Ca(OH)2.
2- To determine the molar solubility of Ca(OH)2 in the presence of added Ca+2.
Introduction:
Many common ionic compounds, which have a very limited solubility in
water, are called slightly soluble salts. A saturated solution of a slightly soluble
ionic compound produces a dynamic equilibrium between the compound and the
dissociated ions. However, because the compound is only slightly soluble, the
solution has a low concentration of ions. For example, in a saturated Ca(OH)2
solution, the equilibrium between Ca(OH)2(s) and the Ca+2(aq) and OH (aq) ions
lies far to the left because of its low solubility:
Ca(OH ) 2 (s) Ca 2 (aq) 2OH (aq)
Example (1):
If 2.42 x 10-4 g of BaSO4 is dissolved in 100 mL of water. Calculate Ksp of
BaSO4?
2.42 10 4
Mol BaSO4 1.04 10 6 M
233 .4 g / mol
1.04 10 6 mol
Morality of BaSO4 1.04 10 5 M
0.1L
[ Ba 2 ] [ SO42 ] 1.04 10 5
K sp [ Ba 2 ] [ SO42 ] (1.04 10 5 )2
K sp 1.1 10 10
M HCl VHCl M V
OH OH
M 2.2 10 2M
OH
1
[Ca 2 ] [OH ] 1.1 10 2 M
2
K sp 5.3 10 6
Example (3):
What is the molar solubility of AgCl in water and in a 0.010 M solution of
NaCl? Ksp AgCl is 1.7 x 10-10.
Ag Cl
AgCl
In pure water
X X
So the solubility of a salt is less in a solution that already contains one of its ions
than it is in pure water.
Procedure:
It is important to keep the bottles containing the Ca(OH)2 tightly capped
when not in use to prevent the solution from absorbing CO2. The reaction of
carbonic acid with the hydroxide ion will reduce the hydroxide ion concentration
and will precipitate CaCO3 (chalk), as shown in the equation below:
Ca(OH)2(s) + CO2(g) CaCO3(s) + H2O(l)
2- Rinse a clean 50-mL burette three times with 5 mL portions of 0.1M HCl
solution, then fill the burette with the acid.
3- Titrate the Ca(OH)2 solution prepared in step 1 with the 0.1M HCl
solution, the color of the indicator will change from yellow to red at the
end point. Record the volume of HCl used to reach this point.
effect:
Repeat Part A, steps 1-4, using saturated Ca(OH)2 solution to which
0.100M CaCl2 has been added.
Calculations:
Show your calculations for trial 1 from the titrations of Part A and Part B.
Objectives:
1- To observe an oxidation-reduction reaction.
2- To calculate the molar concentration of Cu2+ solution by using a redox
reaction.
Introduction:
Chemical reactions involving the transfer of electrons from one reactant to
another are called oxidation-reduction reactions or redox reactions. In a redox
reaction, two half-reactions occur; one reactant gives up electrons (undergoes
oxidation and it's called a reducing agent) and another reactant gains electrons
(undergoes reduction and it's called an oxidizing agent), resulting in changes in
oxidation number. The electrons are not shown in equation (1) because they are
neither reactants nor products but have simply been transferred from one species
to another (from Cu to Ag+ in this case), the total number gained must equal the
total number lost.
Cu ( s ) 2 Ag (aq) Cu (aq2 ) 2 Ag ............ (1)
Now the question is, why does a reaction such as equation 1 occur, whereas
another reactions such as, Cu( s ) H (aq) no reaction, does not occur?
Table (1). Activity Series of Metals: Metals arranged in order of decreasing ease
of oxidation.
Copper
Cu2 2e
Cu
Silver
Ag e
Ag
Gold
Au 3 3e
Au
From table (1), Zn is above Cu and H2, Thus, Zn metal will be easily
oxidized by both Cu2+ and H+ ions (i.e. the reactions proceed to completion
because zinc has a lower ionization energy). However, H2 is above Cu in the
series, and therefore Cu metal cannot be oxidized by H+ ions. Thus, if solid zinc
is added in excess to a solution of blue copper sulfate, the copper ions are
precipitated out of solution as solid copper, and zinc metal dissolves to form
aqueous zinc ions. As the copper ions are removed, the solution becomes less
blue, finally appearing colorless when all Cu2+ is precipitated. Any unreacted
zinc metal can be dissolved with dilute HCl, leaving copper as the only solid
2 Chemistry 106 Experiment 11
phase in the mixture. The copper can then be separated, dried and weighted. By
determining the mass of copper precipitated from a known volume of Cu2+
solution, it will be possible to calculate the molarity of Cu2+ solution. If the mass
of a known volume of Cu2+ solution is obtained, it is additionally possible to
calculate the density of the solution and the % by mass of copper in it.
In this experiment you will analyze a sample of Cu2+ of unknown molarity.
As a reminder, the relationships involving concentration, density, and % by mass
are listed below (in the present experiment, the solute is Cu2+).
Molar concentration = moles of solute / liters of solution.
Density = mass of solution (g) / solution volume (mL).
And by mass = mass of solute (g) / mass of solution (g).
Practice Exercise:
A student pipette 10.00 ml of CuSO4 solution, having an unknown molarity
and a density of 1.040 g/mL at 25oC, into a beaker and added 1.50 g of zinc
powder. The mixture was stirred occasionally over a period of about 5 minutes,
and then 10 mL of 6 M HCl was added. When bubbles stopped evolving, the
mixture was quantitatively transferred to a pre-weighed filtering crucible (mass =
10.8275g) which was connected to an aspirator. The reddish metal that separated
was washed with water and acetone. The crucible-with-metal was dried in an
oven at 100oC for 5 minutes, cooled, and found to weight 11.3459 g. Calculate
the molarity and % by mass of Cu2+ in the CuSO4 solution. Calculate the
molarity and % by mass of Cu2+ in the CuSO4 solution.
………………………………………………………………………………………
………………………………………………………………………………………
………………………………………………………………………………………
* Write the net ionic equation for the dissolution of zinc by dilute HCl:
………………………………………………………………………………………
………………………………………………………………………………………
………………………………………………………………………………………
Objectives:
1- To determine the rate law for the redox reaction
2- To use a graphical analysis of the experimental data.
2 I H 2O2 2 H
I 2 2 H 2O
Introduction:
The rate of a chemical reaction describes how quickly the reactants
disappear and the products form, and expressed as mol L-1 s-1. For the
hypothetical reaction, A2 2 B2
2 AB2 the rate can be measured by
observing the rate of disappearance of either A2 or B2, or the rate of appearance
of AB2, depending on which species is the easiest to detect and monitor during
the reaction. The rate of a reaction is related to the concentration of reactants by
the rate expression, for the above reaction the rate expression or the rate law is:
Rate k [ A2 ] p [ B2 ]q
Rate expression or rate law where k is the specific rate constant, varies with
temperature but its value is independent of reactant concentrations. The
2 I H 2O2 2 H
I 2 2 H 2O
Rate k [ I ] p [ H 2O2 ]q
a. Determination of p:
To determine p, [H2O2] is kept constant and [I-] is changed, and therefore,
Taking the logarithms of both sides: log ( Rate) 1og k plog [ I ] log c .
Combining all constants, we have an equation for a straight line:
log ( Rate ) plog [ I ] c
y mx b
b. Determination of q:
Where C' equals log k' + log[I-]p. Therefore, a plot of log(Rate) versus log [H2O2]
yields a straight line with a slope equal to q.
equation 1: 2 I H 2O2 2 H
I 2 2 H 2O
To prevent an equilibrium from being established in equation 1, the S2O32− is
present to react with the I2 as it is being formed.
equation 2: 2S2O32 I 2
2 I S4O62
The reaction rate is then followed by observing the time required for a
quantitatively measured amount of S2O32− to react is the time lapse for the
appearance of the deep-blue solution. This, in turn, measures the rate of I2
production (mol I2/ time), which is affected only by the initial concentrations of
H2O2 and I-.
2.5 10 4 mol
rate 2.8 10 6 mol / s
90 s
15 0.2
[I ] 0.04 M from M1V1 M 2V2
75
25 0.1
[ H 2O2 ] 0.033 M
75
Table (1): Composition of test solutions (All volumes are measured in mL)
Solution A
Test Solution B
Distilled 0.02M
solution Buffer 0.3M KI Starch 0.1M H2O2
water Na2S2O3
1 61.5 12.5 5.0 1 5.0 15
2 56.5 12.5 10.0 1 5.0 15
3 51.5 12.5 15.0 1 5.0 15
4 41.5 12.5 15.0 1 5.0 25
5 31.5 12.5 15.0 1 5.0 35
1- In a clean and dry 250 Erlenmeyer flask or 250-mL beaker add components
of solution A required for test 1. Measure the volumes of KI and Na2S2O3
using either a pipet or a buret. Stir thoroughly and record the temperature.
V (mL ) M
1. Number of moles of S2O32 .
1000
( mol I 2 )
3. The rate of reaction
t
mol I 2
rate .
t (sec)
4. Calculate the initial concentrations of I- and H2O2. Note that the total volume
of reaction's mixture = 100 mL.
0.3M V (mL )
[ I ]i
100
0.1 M V (mL )
[ H 2O2 ]i
100
2. Plot on linear graph paper log (mol I2/t) vs log [H2O2] for test solution 3, 4,
and 5 (these solutions have constant concentrations of I-). Draw the best
straight line and calculate the slope which gives the order of reaction, q, with
respect to H2O2.
moles I 2
Rate k [ I ] p [ H 2O2 ]q
t (sec)
To determine k' for the five solution. Calculate the average values of k'.
Report Sheet:
A. Data
Solution Temp. 1 2 3 4 5
B. Calculations
Using graphing calculators (page 11), determine the slope of the following lines.
Then write the rate law for the reaction.
Rate = ____________________________
1 2 3 4 5