You are on page 1of 32

FE 101 GENERAL CHEMISTRY LABORATORY SHEET

(2011-2012)

INTRODUCTION
Science is a unique field of study based on experiment. And the one purpose
of the laboratory is to make you aware that chemistry is an experimental science.
Your department requires you to spend time each week working in a chemistry
laboratory. There are three significant reasons why students must have actual
experience with scientific experimentation
First, scientific conclusions are reached by the results of experimental
observations carried out carefully. Second you should have manipulative skills in
performing quantitative experiments. Third, you need to develop the ability to record
and keep your experimental results and observations.
In this text some basic exercises have been selected with following criteria:
1. To show the relationship between experimental measurement and chemical
theory.
2. To teach basic laboratory technique
3. To give you skill to interpret numerical data.
You should make a special effort to develop the ability to observe what is actually
happening and then try to understand and explain it. Finally, during laboratory you
should try to learn new concepts just as in lecture.

GENERAL INSTRUCTION
The following instructions are to acquaint and guide you in the procedure to be
followed in performing and reporting laboratory experiments.
A. PROMPTNESS: At the beginning of each laboratory period some time will be
devoted to a discussion of the work for the day. If tardy, you will, of course, miss some
of the discussion. In addition, the assignment for the following week will be given
during this discussion period.
B. PREPARATION: Your assignments will be given one week in advance, it is
expected that you will acquaint yourself with the objective and procedure for each
experiment to be performed in any given week. Careful planning of your work will
enable you to understand each experiment and to complete it with a minimum of
wasted effort.
C. CLEANLINESS AND ORDERLINESS: The condition of your laboratory table and
equipment is some indication as to whether you are a good student. Therefore, your
instructor will consider these factors in his (her) appraisal of your work.

D. CHEMICALS: Use only the quantity of each chemical that is necessary for each
experiment. Do not pipette from reagent bottles directly. Do not pour chemicals back
into reagent bottles.

E. QUESTIONS: Do not hesitate ask questions to your instructor. However, you are
expected to make certain you can not answer questions with some additional thought
before you monopolize his (her) time.
F. RECORDING DATA: There are at least good for writing a good laboratory notebook.
a) This is a laboratory course. Therefore, your work in the laboratory, which is
represented partially by this record of your experience in the laboratory, is the most
important factor in your course grade.
b) More important to you is the fact that you learn a great deal about experiment when
you "write it up".
c) Most important of all; you learn how to write a good research report; a good
research report is an essential requirement for a good scientist. A research report is
valuable to only when you can tell at a glance exactly what you did on a particular date
why you did it. Your book should be intelligible to another scientistas well, particularly
your instructor in this course.
What are the elements of a good notebook ?
It is suggested that you use a bound report, not a loose leaf. Use ball point pen rather
than pencil. If possible, paste or stable examples of things such as spectrum records
directly in your notebook. However, do not hand in them loosely folded around the
pages. Each experiment should be written with the following points in mind:
1- Name of Experiment:
2- Name of Partners :
3- Date:
4- Purpose:
5- Materials:
6- Procedure (Method):
7- Results: (Your Data)
8- Discussion:
9- References:
10- Appendix (graphs, shapes us.)

Statement of purpose: A brief statement of the purpose of carrying out the


experiment.
State the principle(s): involved in the experiment. Briefly, not more than several
sentences. Include relevant chemical equations.
Procedure: Refer to the appropriate pages in the laboratory manual unless you
change the experimental procedure. If you do change it, state the changes and your
reasons why.
Your data and results: These include tables, graphs, drawings, calculations, and so
forth. Organize these as well as possible and as neatly as possible. Try to present
some of your results in the form of a graph, wherever possible, or if more appropriate,
a table. The labeling of the graphs must be clear and unambiguous. For example: Be
sure to label both ordinate and abscissa and to title the graph with a clear legend. Use
circles around your data.
Concise discussion of data and conclusion : Briefly discuss results in terms of
expectations, outline reasons for "unexpected" results. Be precise and clear. Mention
possible sources of error. Provide a single statement of conclusions from the
experiment. Be sure to read your report carefully after it is written to be sure you know
what is said.
G. REPORTS: A written report will be due one week after the completion of each
experiment. This report is be written on a "Report" and handed to the instructor.

LABORATORY SAFETY RULES


The chemical laboratory has some hazards and a laboratory accident can not be
predicted . To avoid those following safety rules should be considered.
1. Responsible behavior is essential. The dangers of spilled acids and
chemicals and broken glassware created by thoughtless actions are too great
to be tolerated.
2. Wear suitable clothing and shoes. Shorts or bare feet leave large areas of
skin exposed to potential chemical burns. Long, full sleeves may drag in your
chemicals or catch on your equipment ; both the sleeves and the experiment
could be ruined. Long hair should not be worn loose, especially when you are
using a burner or centrifuge.
3. Take precautions to avoid cutting yourself. Discard cracked or chipped
glassware.
4. Dispose of waste chemicals as directed. Do not return any substances to
reagent bottles. Usually, your instructor will ask you place waste chemicals in
waste jars or to pour them down a sink with plenty of running water.
5. Perform no unauthorized experiments.
6. Do not smoke in the laboratory at any time.
7. Report all injuries to your instructor at once.
8. Always pour concentrated acid into water (not water into acid).

Experiment 1

Density of liquids
INTRODUCTION
In this experiment you will become familiar with how mass and volume
measurements are carried out. These mass and volume measurements will then be
used to determine the density of a salt solution and liquid water.
The density (mass per unit volume) of liquids can be determined by measuring
both the mass and the volume of a given sample. The density is a characteristic
property of a substance. As an intensive property it is independent of the quantity of
material measured since it is ratio of the mass of an object to its volume. It remains
constant unless the temperature or pressure is changed. For liquids a relatively small
change in temperature can affect the density appreciably, but a pressure change must
be quite great to have a measurable effect. In this experiment you will determine the
density of liquid water. Once this density and its change with temperature are known,
you can use the information to find out what volume should be occupied by a known
mass of water at a given temperature.
Calibration is the process by which a stated measure a mass or a volume is
checked for accuracy. Once a data such as concentration vs. density of the solution is
obtained, it is possible to plot a curve what we called a calibration curve. When such a
plot is obtained we can determine the density of a substance with a known
concentration, or the concentration of a substance with a known density.

PROCEDURE
A)
- Weigh an empty cylinder
- Add about 20 mL of distilled water in the clean graduated cylinder.
- Record the volume to the nearest 0.1 mL.
- Weigh the cylinder plus water on an analytical balance and record.
- Measure the temperature of the water
- Calculate the density.
- Compare the calculated density of the water with the values given in the table and
calculate the percent error.
- Obtain an unknown solution and determine the density of this unknown in a
similar way.
8

B)
- In clean dry containers, obtain approximately 25 mL of each of four different NaCl
solutions: 4, 8, 12, 16 % NaCl by weight.
- Determine the density of each solution as in Part A.
- Obtain a salt solution of unknown concentration of NaCl from your instructor and
determine its density.
- Plot a graph showing the density (on the vertical axis) vs. Concentration of NaCl
(horizontal axis).
- Using the graph, obtain a value for the concentration of NaCl for your unknown and
report it to your instructor.

Table-1 Density of water at different temperature.


TempC

Density(g/mL) TempC

Density (g/mL)

15

0.9979

26

0.9959

17

0.9977

28

0.9955

18

0.9975

29

0.9952

20

0.9972

31

0.9946

22

0.9968

33

0.9941

24

0.9964

35

0.9935

RESULTS
Calculate:
a) Density of water, percent error, density of unknown
b) Density of known solutions, density of unknown solution
density
(g/mL)

1.5

unknown
density

0.4
Concentration (salt%)

PRELAB QUESTIONS
1. Write the definition of the density and
a) Explain the effect of the temperature and pressure on the density of the
liquids. How does the density of liquids changes with the temperature?
b) Why do we need a great pressure change to observe a change in the density
of the liquids?
c) If we have a gas sample instead of liquids, do we need great pressure change
to have a measurable change in the density? Explain briefly.
d) If we have a solid sample instead of liquid or gas, does the density of this solid
change if we increase or decrease pressure too much?
2.
a) Suppose that, you measure the temperature of 20 mL of the water as 30C
when it is actually 20C. Find the minimum percent error in the calculation of
the density by using the table given above.

10

b) Suppose that you determine the mass of 41.2 mL of water as 41.052 g. at


28C. Calculate the density from the experimental values and match it with
the value given in the table. Calculate the percent error.
3. Plot the temperature vs. density values given in the table. Determine the
density of the liquid water at 16C, 21C, 23C and 25C.
4. What is the calibration? Explain briefly.

11

Date:

DATA SHEET
DENSITY OF LIQUID
a) Mass of graduated cylinder plus water...............
Mass of graduated cylinder alone....................
Volume of water in the cylinder.....................
Temperature of water................................
Mass of graduated cylinder plus unknown.............
Volume of unknown...................................
b) Mass of grd. cyl+ known NaCl soln.
Volume of NaCl in cylinder
Mass of grd. cyl.+ unknown soln.....................
Volume of unknown NaCl soln.........................

Name of student

Submitted to

12

Experiment 2

Solutions
INTRODUCTION
In this exercise the student will study various factors which affect the solubility and
the rate of solution. He will then observe the affect of a nonvolatile solute on the boiling
temperature of a liquid solvent.
Solutions are homogeneous mixtures. They are usually classified according to their
physical state. The component of a solution that is present in greatest quantity is
usually called the solvent, and all other components are called solutes. For a given
solution, the amount of solute dissolved in a given amount of solution is the
concentration of the solute. A dilute solution contains a small amount of solute, a
concentrated one contains large amount of solute. These terms are only relative and
do not covey any idea of how much of a given solute can be dissolved. The solubility of
a substance in a particular solvent at a specified temperature is the maximum amount
of the solute that will dissolve in a definite amount of solvent and produce a stable
system. A solution that contains this specific amount of solute is said to be saturated, if
it is contains less amount of this amount the solution is unsaturated. If the more than
the maximum amount of solute that can normally be contained at a given temperature
is dissolved (usually under special conditions), the solution is supersaturated.
Solubility varies from compound to compound. It can not be predicted quantitatively
even if you know a compounds formula, melting point, or other physical or chemical
properties. Solubility data have compiled by trial and error by actual experimentation.

PROCEDURE
A. Nature of Solute and Solvent:
-

test the solubility of sugar, sodium sulfate (Na2SO4), sodium chloride, paraffin and
iodine in each of the following solvents: water, alcohol and carbon tetrachloride. Use
2 - 3 mL of solvent and a lump of solute not more than half of the size of a pea.

- record the results of your tests in a table designating the substance as: soluble (s),
slightly soluble (ss) and insoluble (I) in each of the solvents.
B. State of Subdivision:
Select two of copper sulfate of about the same size. Grind one of the crystals into a
powder and the single crystal in separate test tubes. Add 2 mL of water to each test
tube and shake. Observe what happens.

13

PRELAB QUESTIONS
1- What are the factors that affect the solubility? Explain each factor.
2- What is the meaning of the term nonvolatile?
3- How can a nonvolatile solute affect the boiling temperature?
4- How does the solubility of a liquid and a gas changes with temperature? Does it
increase or decrease?

OUESTIONS
1.Discuss the solubility of sugar, sodium sulfate, sodium chloride, paraffin and iodine in
water, alcohol and carbon tetrachloride (CCl4 ) in terms of the nature of solute and
solvent by using the table obtained from Part A.
2. Compare and explain the rate of solution of the powder and the single crystal in
water in Part B of the experiment.

14

Date:
DATA SHEET
SOLUTION
Part A. The nature of solute and solvent

Na2S

NaCl

paraffin

iodine

Sugar

Water
Alcohol
CCl4
Part B. State of Subdivision
Write your observations.

Name of student

Submitted to

15

Experiment 3
Charless Law

16

17

18

Date:
DATA SHEET
CHARLESS LAW

Name of student

Submitted to

19

Experiment 4
Heat and Temperature

20

21

Date:
DATA SHEET
HEAT AND TEMPERATURE

Name of student

Submitted to

22

Experiment 5

pH and Indicators
INTRODUCTION
In this experiment, the student will become familiar with the practical aspects of pH
concept and indicators. He will learn how indicators are used to determine the pH of a
solution. Some principles concerning the dissociation of weak are also given.
-pH concept: The concentration of H+ in natural and biological environments, as
well as in all chemically oriented problems, highly important.
H2O----->H+(aq) + OH- Kw = 1.0*10-14

at 25C

Kw =[H+][OH-], where brackets denote concentrations in mole/L. As it is seen from the


value of the Kw, ion product of water, for pure water [OH-] = [H+] = 1*10-7. If an acid or a
base is present in water H+ deviates from the value of 1*10 -7 M. However [H+] and
[OH-] always equals Kw at constant temperature. The concentration of H+ may change
over a wide range of values are frequently expressed in terms of exponential numbers.
For this reason, a simpler form representation for H+ is provided as follows:
pH = -log[H+]
Example: What are the pH values for 0.1 M HCl and 0.1 M formic acid HCOOH?
a) HCl is a strong acid, it dissociates almost completely in aqueous solution. 0.1 M
HCl gives 0.1 M H- and 0.1 M Cl-.
HCl ------> H+ + Cl-

[H-] = 0.1 M

pH= -log(0.1) = 1

b) HCOOH is a weak acid, it does not dissociate completely in aqueous solutions.


Its dissociation depends on the following
[H+] [HCOO-]
HCOOH <-------> H+ + HCOO- Ka = -------------- = 2.0 *10-4
[HCOOH]
Ka is the dissociation constant for formic acid.
At equilibrium: x= dissociated HCOOH molecules, mole /L. If x moles of HCOOH
dissociated, it would give x moles of H+ and x moles of HCOO- ions. If the initial
concentration of formic acid is 0.1 M at equilibrium, it remains 0.1-x M.
(x)(x)
HCOOH <--------> H + HCOO Ka=---------=2*10-4
0.1 M
0.1-x
+

Initially

23

At equilibrium

0.1-x M

x in the denominator can be neglected since 2*10-4 << 0.1


x=[H+] = [HCOO-] =4.5*10-3 M

pH = 2.3

INDICATORS
Acid base indicators, in general, are organic molecules which are weak acids or
weak bases; they exhibit different colors in their protonated form, HIn, and
unprotonated form, In-. For an indicator of weak acid type, the ratio of [In-] to [Hin]
depends on [H+].
[H+][In-]
+
HIn <------> H + In
Ki = ------------[HIn]
where Ki is the dissociation constant for indicator HIn.
When HIn is the predominant species in the solution, the acid color of the indicator is
observed; on the other hand, the base color is observed when the predominant
species is In.
n general, depending on the slight ability of human eye the acid or base color can be
observed when the following conditions are met.
In1
---- = --- log(1/10)=-1 acid color is observed.
HIn
10
In10
---- = --- log(10/1)= 1 base color is observed.
HIn
1
Ki=[H+][In-]/[Hin]
[H+] = Ki[HIn]/[In-]

pH= pKi + log [In-]/[HIn]

pH < pKi

acid color is observed.

pH = pKi

base color is observed.

pH > pKi

color transition range.

Every indicator has a specific color, in terms of pH units, depending on its K i value. In
practice, this range may equal to or less than 2 pH units.
Example: Phenolpthalein an acid base indicator, has a color transition range of pH =
8.0 to pH = 10.0. It is colorless when it is in acidic medium. Its base color is pink. If one
drop of phenolpthalein solution is added to 5*10-3 M NaOH solution, what would the
color of this solution become?
Solution:
[OH-] = 5*10-3 M
[H+] = 1*10-4/5*10-3 = 2* 10-12 M
24

pH = 11.70
11.7 > 10 base color, solution becomes pink.

PROCEDURE
1. Take 10 mL of 0.1 M HCl. What is the pH of this solution?
2. Dilute 1 mL of 0.1 M HCl with 9 mL of distilled water to give 10 mL of a solution
with pH=2.
3. In a similar way, prepare solutions of pH=3, pH=4 and pH=5.
4. Divide each of the five of the solutions above into two parts. Now, you have two
sets of solutions. Keep these ten solutions until you finish through step 9.
5. Test each of the five solutions in the first set with one drop of thymol blue
indicator. Record the colors observed. Note: thymol blue can not be used after
pH=2.8.
6. In a similar way, test the second set with methyl orange indicator. Record the
colors observed.
7. Obtain a sample of an unknown acid, test it with each of the indicators, estimate
its pH.
8. Obtain 5 mL of 1 M acetic acid, CH3COOH. Test it with each of the indicators
and estimate its pH value to the nearest 0.5 pH unit. Calculate Ka for acetic acid.
9. Obtain 5 mL of 0.01 M acetic acid and determine its pH. Calculate Ka.
10. When you diluted 1 M acetic acid to 0.01 M, did H change by a factor of 100?
Explain.
11. Take 10 mL of 0.1 M NaOH, and determine its pH.
12. By using 0.1 M NaOH, prepare a series of solutions from pH=10 through
pH=13. Divide each of these five solutions into three parts. Now you should
have three sets of solutions.
13. Test each of sets above with three different indicators; one with
phenolphtalein, one with alizarin yellow and one with tropolin O, use one
drop of indicator for each test. Record the colors observed.
14. Obtain a sample of an unknown base. Test it with each of the indicators,
estimate its pH.

25

PRELAB QUESTIONS
1- Write definition of the following terminology:
a) pH and pKi
b) acidity
c) indicator
d) strong acid and strong base
e) weak acid and weak base
2- What is the difference between the pH and acidity?
3- Find the indicators and their working pH range from the library.
4- Suppose that 100 mL of 0.5 M HAc (Acetic acid) and 50 mL of 2 M CaCl 2 are
mixed at room temperature to prepare a brine solution for pickling. What will be the
theoretical pH of this mixture?
(Ka for HAc = 1.8*10-5)
5- Write a brief procedure for the experiment in your own words

26

Date:
DATA SHEET
pH and Indicators
pH
Thymol blue

Methyl orange
pH of Unkown:
pH of 1.0 M Acetic acid:
PH of 0.01 M Acetic acid:

pH
Phenolphthalein
Alizerin yellow
Tropolin O

pH of Unkown base:

Name of student

Submitted to

27

Experiment 6

Acids - Bases
INTRODUCTION
Neutralization is the reaction between an acid and a base in chemically equivalent
amounts and titration is the process of mixing measured volumes of reacting solutions
in such manner that one can determine when chemically equivalent amounts of
reactants are present. The purpose of titration is to determine the concentration of a
solution of unknown strength. The concentration of one of the solutions , expressed as
molarity , in this case, must be known. After titration the molarity of other solution can
be calculated. In titration process, the reagent is slowly added to the unknown from a
burette until the end point is reached. The end point is marked by a color change,
formation of a precipitate etc. The titration may involve either an acid base or an
oxidation - reduction reaction.
Solutions Preparation of Standard
a) A measured quantity of reagent is placed in a flask of known volume.
b) Distilled water is then added until a measured volume of solution has been
prepared.
For example, to make a 0.10 M NaOH solution one would weigh out 4.00 grams of
NaOH, place this in volumetric flask, and add distilled water until one liter of solution is
obtained.
End Point
The end point is the point where the number of equivalents of reagent added is just
sufficient to react with all the unknown. This point is usually determined by a color
change in an indicator. In some cases the reagent or unknown is colore, and a color
change may be observed without the presence of an indicator.
The Burette
The burette must be clean before use. It should first be rinsed three times with
distilled water. Since the water remaining in the burette would dilute the standard
solution the burette must then be rinsed two or three times with 5 mL of the standard
solution. The burette is then filled to above the graduated portion and clamped
vertically to a ring stand. The outside is dried and checked for leaks. If there are air
bubbles below the stopcock, they may be eliminated by running out a small quantity of
the standard solution. To read the burette, observe the surface of the liquid, called
meniscus. Adjust the lowest part of the meniscus to the zero graduation line by running
out the excess solution. In order to get consistent results your eye must be at the level
of he meniscus when a reading is made. For colore solutions use the top of the
solution instead of the meniscus.
As the end point is approached the standard solution should be added one drop at
a time. You should have practice until you have learned this technique.

28

PROCEDURE
1. Determination of Concentration of HCl Solution:
- Using a pipet place 10 mL of a known concentration of Na 2CO3 solution in each
of two flasks.
- Add two drops of methyl orange indicator to each of the flasks and mix the
solution with a gentle shaking.
- Fill your burette with HCl as instructed above.
- Place one of the Erlenmeyer flasks under the tip of the burette.
- Handle the stopcock of the burette with your left hand while shaking the flask
gently with your right hand.
- Carefully run HCl from the burette into the Na 2CO3 solution until the end point is
reached.
- The end point is the first appearance of a permanent red color.
- To prevent the effect of dissolved CO 2 on the pH, boil the mixture for a few
minutes.
- After cooling the solution add a few drops of HCl until the end point is observed
again.
- Record the volume of HCl added.
- Titrate the solution in the second flask following exactly the same procedure. Try
to detect the end point as closely as possible.
- Calculate the molarity of the HCl solution.
2. Quantitative Determination of NaOH:
- Using a pipet, add 10 mL of 0.1 M NaOH to each of two erlenmeyer flasks.
- Add two drops of methyl orange to each flask and titrate just as you did with
sodium carbonate, Na2CO3.
- It is not necessary to boil the solution.
- Calculate the molarity of the NaOH solution and compare your result with the
actual concentration.

29

3. Unknown
You will be given an unknown solution of NaOH. Titrate this solution just as you did
above and calculate the number of grams of NaOH in the solution.

PRELAB QUESTIONS
1-Explain the meaning of the following terms
a) Titration
b) End Point
c) Standard Solution
d) Meniscus
2-Explain the preparation of 500 mL of 0.3 M standard NaOH solution.
(MW of NaOH = 40 g/mole)
3- Write a brief procedure for the experiment in your own words.

OUESTIONS
1- How does dissolved CO2 affect the end point in the titration of Na 2CO3 with HCl?
Explain by using chemical formulas. Does the pH decrease or increase in the presence
of dissolved CO2?
2- Why did you carry out the same procedure with two times for the titration of
Na2CO3 and NaOH? Were the results same with each other? If not what can be the
reason of obtaining different results?

30

Date:

DATA SHEET
ACIDS AND BASES
1.Volume of Na2CO3 pipetted

Initial burette reading for acid

Final burette reading for acid

2.Volume of NaOH pipetted

Initial burette reading for acid

Final burette reading for acid

3.Initial burette reading for acid

Final burette reading for acid

Name of student

Submitted to

31

RESULTS
1.Volume of Na2CO3 used

Equivalents of Na2CO3 us

Volume of acid used

Normality of acid

Average

2.Volume of base used

Equivalents of base used

Volume of acid used

Normality of base

Average

3.Volume of acid used

Equivalents of acid used

Mass of base

32