ADAMSON UNIVERSITY

College of Engineering
Chemical Engineering Department
M a nila

Physical Chemistry for

Engineers 1
Laboratory Manual

Prepared by:

Committee for Laboratory Manual of the Chemical Engineering Department

 Table of Contents:

Course Des cription (i)

Policies and Guideli nes on t he use of ChE/Chem Laboratori es (ii)

Ins truction f or Preparing Laboratory Reports (iii)

Experiment Title
No.

1 Determi nat ion of Molar Volume and Evaluation of the

Univers al Gas Const ant

2 Molecul ar Wei ght Dete rmination by Vapor Density

Method

3 Meas urem ent of Densit y

4 Meas urem ent of Viscosity

5 Calorimetr y: Measureme nt of Heat of Reaction

6 Meas urem ent of Ref ractive Index

7 Polarimetr y

8 Spectrophotometry
 PHYSICAL CHEMISTRY FOR ENGINEERS - I
(Laboratory)

Course Description:

This laboratory course deals accompanying Physical Chemistry 1 (lecture) covers the
experiments concerning fundamental physical properties such as density, viscosity, melting
point, surface tension, determination of optical properties by applying the principles of
colorimetry/turbidimetry, spectrophotometry, refractometry, and polarimetry. This course will
also deal with important colligative properties, namely boiling point elevation and freezing point
depression.

No. of hours : 3 hours per week

Course Credit Units : 1 unit

Course Objectives:

After completing this course, the students must be able to:

1 Develop sound judgment in interpreting and correlating experimental data based on

the principles learned in Physical Chemistry.
2 Develop initiative, resourcefulness, and leadership by demonstrating full
responsibility in performing the experiments assigned.
3 Acquire laboratory skills by following accepted laboratory handling and waste
disposal techniques.
4 Develop safety consciousness by observing proper laboratory techniques at all times
while working in the laboratory.
 POLICIES AND GUIDELINES ON THE
USE OF CHEMICAL ENGINEERING/CHEMISTRY LABORATORIES

1. Chemical Engineering laboratories are open for equipment review and other preparatory work
from 8 am to 5 pm Monday through Friday. Equipment may only be operated and chemicals
will be dispensed during scheduled laboratory hours. Written approval of the faculty adviser,
laboratory coordinator, and ChE chairperson are required for anyone (e.g. research students) to
use the laboratory during Saturdays or to operate equipment on non-scheduled laboratory days.

2. For the use of equipment, computers, and chemicals, students and faculty members must sign
in the log books for proper monitoring of the equipment.

3. No equipment is to be operated until the approval of the instructor and laboratory coordinator
has been obtained at the check-in meeting. Only the equipment pertaining to the assigned
experiment is to be operated. All members of a group are to be properly informed on the safety
aspects of their assigned experiment and to be familiar with the safety aspects of surrounding
experiments. Before any apparatus can be operated in the laboratory, the group must have a
second on-site safety check-in.

4. Students are required to prepare handling and storage procedures of chemicals and materials to
be used and waste disposal/treatment procedures approved by the faculty adviser and
laboratory coordinator prior to any experiment.

5. Transfer or movement of equipment or devices from the laboratories will not be allowed
without approval of advance notice (at least 2 days before the request schedule) from the
laboratory coordinator.

6. In borrowing glassware and accessories of the equipment, equipment and in using laboratory
facility, students must accomplish Form A (Request for the Use of Laboratory Facilities and
Equipment) with the signature of the professor.

7. In case of breakages, damages, or losses:

(A) A student accomplishes three copies of the Breakage Forms/Charge Slip Form (Form B)
duty signed by all members of the group.
(B) The student requests the signature of the instructor and returns the form to the laboratory
personnel.
(C) The laboratory personnel indicate the price of the damaged or lost item.
(D) The students are given one week to replace the items with the same brand or
specifications. If the students fail to replace the said item, the item is then forwarded to
the Cashier’s Office for payment.
(E) After payment, the students return the forms to the laboratory personnel with the
photocopy of the official receipt.
(F) They must be advised to keep the original receipt for future reference.

8. Students should always wear their laboratory gowns or aprons when working in the laboratory.
Safety goggles and safety gloves must also be worn whenever applicable. Students must also
observe proper attire specifically closed footwear to protect them from spilled chemicals or hot
fluids. Neckties, dangling clothing or jewelry and other unsafe items are prohibited.
9. Sleeping is prohibited in the laboratory. Violation of this rule will result in dismissal from the
laboratory for that day.

10. Horseplay of any sort is absolutely prohibited in the laboratory.

11. As a general rule, eating, drinking, chewing gum, and smoking are not allowed inside
laboratories.

12. All safety precautions must be followed at all times.

13. No operating equipment will be left unattended. At least two members of the group must be
present while the equipment is operating.

14. The laboratory floor must be kept dry, clean, and uncluttered at all times. Any spills should be
cleaned up immediately.

15. All injuries, accident, hazardous situation, losses, leaks, malfunctions or breakages must be
reported to the laboratory personnel or professor immediately.

16. All chemicals must be transported in a safety carrier. All mercury and alcohol thermometers
and more than one item of glassware must be transported in a bucket or other suitable
container.

17. The students are expected to be familiar with the safety aspects of all chemicals used in the
laboratory.

18. Listening to radios, walkman, MP3’s, MP4’s, etc. is strictly prohibited in the laboratory.

19. Playing computer games; using and recharging of cellular phones; or viewing DVD’s is
prohibited in the laboratory.

20. Applying cosmetics are prohibited in the laboratory.

21. Precautions should be taken to prevent long hair from being entangled in moving parts of the
equipment.

22. A violation notice will be issued by the Laboratory Coordinator or Laboratory Student
Assistant or by the assigned Laboratory Professor to any student found violating any of these
rules and regulations.

23. Any SERIOUS VIOLATION of any of these safety rules or laboratory policies may lead to
immediate dismissal from the laboratory. A person who repeatedly disregards the safety rules
or laboratory policies for at least 3 times will be called in for disciplinary action with the ChE
chairperson. A penalty that suits the violation may be imposed and, at the discretion of his/her
laboratory professor, the student’s grade may be severely affected.

Other policies may be given as situation arises and in consideration of our best interest. It is
expected that these sets of policies serve as a guide for us to work safely and efficiently.
 Instructions for Preparing Laboratory Reports

The report must be prepared and will be graded according to the following outline:

Subject Marks

1. Title page 2

2. Abstract 12

3. Introduction 3

4. Theoretical Background 5

5. Procedure 4

6. Results 8

7. Discussion of Results 24

8. Conclusions and Recommendations 8

9. Literature Cited 2

10 Nomenclature 2

Appendices

A1 Raw Data 5

A2 Analysis of data & Sample Calculation 20

Organization & neatness 5

Total: 100

1. Title Page

The Title page should be separate from the rest of the report. It should contain:
a. The name of the experiment
b. The number of course
c. The date when the experiment was run
d. The name of the writer and his co-workers, ID number, and his group number
e. The name of the instructor to whom the report is submitted
f. The date of submission of report

2. Abstract
The abstract should be informative, and should be written in about three to five sentences. It
should cover all phases of the investigation. It must include the following:
a. An introductory statement about the subject matter
b. Briefly describe what was done.
c. Present some selected result (numerical values, if possible).
d. If possible, present some percentage errors in experimental results in comparison with
theoretical values. While writing the abstract, it should be kept in mind that you should not refer
to any graph or table.

3. Introduction
This section should include few sentences discussing the physical and/or chemical principles
involved in the experiment.

4. Theoretical Background
This section should include the theory behind the experiment. It should also contain all those
equations, which are used to acquire a certain result. Theoretical correlations, which are used for
comparison with experimental results, should also be included.

5. Procedure
Here, you should briefly describe the actual step-by-step procedure you followed in running the
experiment. It should be written in your own words, e.g. the needle valve was manipulated in
order to adjust the liquid flow rate.

6. Results
The results should be presented in the form or Tables or graphs. The Table should contain the
results obtain from experiments and from theoretical knowledge. Comparisons should be
presented in terms, e.g. percent deviation.

7. Discussion of Results
In this section you should discuss you experimental results. Show how you make comparison
with the values obtained theoretically. Also discuss the deviation of experimental results from
theoretical values. The possible source of errors should also be mentioned. If the results are
obtained in terms of graphs, then interpret them also.

8. Conclusions and Recommendations

Conclusions are the series of numbered sentences which answer the questions posed in the end of
each experiments. Conclusions should also include the errors between the experimental and
theoretical values. What you have learned from the experiment should be mentioned as well.
Recommendations are the proposals for future work, e.g. suggested changes in equipment, study
of new variables, or possible experiments in relative fields. Like the conclusions, the
recommendations are usually listed by numbers, and each consists of only a sentence or two.
9. Literature Cited
Here, you should list the books, Journal’s articles, etc. used in writing your report and analyzing
the experiment. The reference should be completed (name of the book, author, volume, date of
publication, pages, etc.). References should be arranged alphabetically by author.

10. Nomenclature
The symbols, which are used in the report, should be defined in the nomenclature in alphabetical
order. The accompanying definitions must include proper units.

Appendices

All appendices and graphs should be attached at the end of the report.

A1. Raw Data:

It should contain the data on which the experiment was done.

A2. Analysis of Data and Sample Calculations:

This shows how the data/manipulated data is transformed into experimental results by using the
appropriate equations. Also, how the theoretical results are obtained using theoretical in terms of
percentage error. Sample calculations should contain each step, which is used to acquire certain
results.
 EXPERIMENT NO.1

DETERMINATION OF MOLAR VOLUME

AND UNIVERSAL GAS CONSTANT

The behavior of ideal gases is best explained using the Kinetic Molecular Theory developed in
1857 by Rudolf Clausius (1822-1888). According to this theory, gases are composed of minute
particles called molecules that move in random, chaotic motion. They collide with each other and
with the walls of the container, however, these collisions are said to be perfectly elastic that
results in the conservation of both momentum and kinetic energy. Furthermore, the attractive and
repulsive forces are assumed to be negligible. As such, ideal gases are said to exist at high
temperature and low pressure. In addition, the volume of all molecules of the gas is considered
negligible compared to the total volume in which gas is being contained. The relationships of the
pressure, volume and temperature of this hypothetical gas can be described by the ideal gas
equation as follows:

The constant, R is the universal gas constant whose units depend on the units of P, V, n and T.

Values of the Universal Gas Constant, R

The ideal gas equation has many applications which include the evaluation of the molar volume
at a given temperature and pressure as follows:

Many decomposition reactions produce gases such as hydrogen displacement reactions of metals
in acids. In the activity series of metals, any metal more active than hydrogen displace hydrogen
in the acid. When a gas is produced from a chemical reaction, this gas can be collected over
water. The gas collected is said to be saturated with water vapor such that its total pressure of
water at the given temperature.

In this experiment the molar volume of a gas evaluated using gas collected over water and
produced from hydrogen displacement reaction of a meal in an acid. The universal gas constant
is also evaluated from the experimental values of pressure, temperature and molar volume.
 EXPERIMENT NO.1

DETERMINATION OF MOLAR VOLUME

AND UNIVERSAL GAS CONSTANT

PRELAB EXERCISES

NAME: __________________________________________ DATE: _________________

PROFFESOR: ______________________________________ SCORE: ________________

1. Describe the behavior of ideal gases according to the Kinetic Molecular Theory.

2. Complete the following reactions:

a) (s) + (aq)
b) (s) + (aq)
c) 3(s)

d) 3(s)

3. An empirical equation that determines the vapor pressure ρ of any liquid at a given
temperature range is the Antoine’s Equation given as follows:

For water from , A= 8.10765, B= 1750.284 and C= 235.000. Using the

Antoine equation, calculate the vapor pressure of water at 25 .

4. Sodium carbonate decomposes according to the following reaction:

2 3(s) 2 (s) 2(g)

If 235.46mg of Na2CO3 decomposed completely and the gas produced is collected over
water at 1atm, calculate the volume of gas collected in mL. Vapor pressure of water
at is 23.756 mmHg.
 EXPERIMENT NO.1

DETERMINATION OF MOLAR VOLUME

AND UNIVERSAL GAS CONSTANT

Objectives
1. To determine the molar volume of a gas produced from a displacement reaction.
2. To experimentally evaluate the universal gas constant.

Apparatus
1. Acid Buret – 50mL
2. Beaker – 1L
3. Thermometer
4. Iron stand
5. Professional burette clamp
6. Cork stopper to fit the acid burette

Reagents
1. 10 ml concentrated HCl (12 M)
2. Distilled water
3. 0.20 g Magnesium ribbon
4. 0.20 g Zinc metal
5. Copper or nichrome wire

Procedure
1. Pour 10 mL of concentrated HCl in a burette.
2. Pour 40 ml water to the burette slowly sliding along the side of the burette to avoid
mixing of the two liquids.
3. Weigh 0.20 grams of magnesium metal and clip it in the nichrome wire.
4. Insert the cork in the buret. Invert the burette in a 1 L beaker half filled with water.
5. As soon as the metal reacts completely, measure and record the volume of the
hydrogen gas produced.
6. Repeat using 0.20 grams of zinc metal.
7. Repeat for three trials.
8. Record your data.

Disposal of Chemical
1. Titrate acidic solution using 0.1 M NaOH and dispose resulting solution into the sink
with plenty of water.
NOTE:
1. Check for the leaks of the burette.
 EXPERIMENT NO.1

DETERMINATION OF MOLAR VOLUME

AND UNIVERSAL GAS CONSTANT

PRELIMINARY DATA SHEET:

Date: _______________ Score: _______

Group No.: __________

SIGNATURE

Leader: ________________________________ ___________________________

Members: _________________________________ __________________________

_________________________________ __________________________

_________________________________ _________________________

TRIAL TRIAL
DATA
1 2 3 1 2 3
Metal used
Atomic weight of metal
Mass of metal (mg)
Millimole of metal
Volume of hydrogen gas
collected (mL)
Barometric pressure
(mmHg)
Temperature (˚C)
Vapor pressure of water
(mmHg)
Molar volume (calculated)
(mL/mmol)
Gas constant (calculated)
(mL-mmHg/K-mol)
Molar volume (accepted)
(mL/mmol)
Gas constant (accepted)
(mL-mmHg/K-mol)
Percentage difference
SAMPLE CALCULATIONS:

Approved by: _______________________

PROFFESOR

Guide Questions and Problems

1. What is the other product of the reaction? Write the balanced reactions for this
experiment.

2. Why is it necessary to remove the bubbles before collecting the hydrogen gas?

3. What are the possible errors in the experiment? Account for the possible causes of
deviation of the calculated values from the expected values.
 EXPERIMENT NO. 2

MOLECULAR WEIGHT DETERMINATION BY VAPOR DENSITY METHOD

The molecular weight of an ideal gas can be calculated using the ideal gas equation:

Several methods are being employed to measure the molecular weight of gases at room
temperature .One of these methods is the Regnault’s method . In this method , a dry gas bulb of
300-500 bulb mL capacity is evacuated and weighed. At a definite temperature and pressure the
bulb is filled with gas and weighed . The bulb is then filled with a liquid of known density and
weighed.

Jean-Baptiste Dumas devised a method determining molecular weight in the vapor phase
of volatile liquids. Using this method, a retort-shaped bulb , having a small opening to capillary
tube is filled with air and weighed. The sample of liquid is drawn into the bulb by cooling it and
then immersed in a bath with temperature above boiling point of the liquid. Boiling allows
removal or excess air to complete vaporization of the liquid. The flask is then sealed. Cooled to
room temperature and weighed.

For a real gases , the Berthelot Equation can be used to estimate the molecular weight of
real gases at low temperatures.

MW= ρRT/P[1+ (9(P)(Tc)/128(Pc)(T))(1-6Tc^2/T^2)]

Another technique for molecular weight determination is the Method of Limiting

Densities. The density of a gas is determined at different pressures but constant temperature. At
zero pressure, ideal gas laws become exact for all gases and the molecular weight is determined
as follows:

MW=RT(ρ/P) at P=0

In this experiment the molecular weight of a gas is determined by vapor density method.
 EXPERIMENT NO. 2

MOLECULAR WEIGHT DETERMINATION BY VAPOR DENSITY METHOD

PRELAB EXERCISES

NAME: _________________________________________ DATE: _________________

PROFFESOR: ____________________________________ SCORE: ________________

1.Describe the following methods used for molecular weight determination:

a) Dumas Method
b) Regnault’s Method
c) Method of Limiting Density

2. The following data were taken in measuring the molecular weight of a certain gas by Regnault
Method:

Wt. of evacuated bulb= 42.5050 grams

Wt. of bulb + gas= 43.3412 grams
Wt. of bulb + water= 365.31 grams
Temperature=25°C
Pressure(corrected)=745 mmHg
Find the molecular weight of gas.
 EXPERIMENT NO. 2

MOLECULAR WEIGHT DETERMINATION BY VAPOR DENSITY METHOD

Objectives:

1. To determine the molecular weight of gas by vapor density method.

Apparatus:

1. 6 Erlenmeyer Flask- 250 mL

2. Water bath
3. Analytical balance

Reagents:

1. 15 ml Ethyl alcohol
2. 15 ml Ethyl acetate

Procedure:

1. Weigh a clean dry 250 mL Erlenmeyer flask.

2. Cover the mouth of the flask with an aluminum foil and pinch a hole using a small pin.
Secure the cover with a rubber band. Be sure the pin is small enough and nearly visible to
the naked eye.
3. Weight the empty flask with the cover.
4. Pour 5 mL of ethyl alcohol in the flask and cover with the aluminum foil,
5. Immerse the flask in water bath and maintain a temperature of 750C.
6. If all liquid in the flask vaporized, remove it from the bath and cool at room temperature.
7. Weigh the flask with the condensed liquid sample and measure its temperature.
8. To get the volume of the flask, fill it with distilled water up to the brim and measure the
volume in a graduated cylinder. Record also the temperature.
9. Make three trials.
10. Repeat using ethyl acetate.

Disposal of Chemicals:

1. Dispose resulting solution into the sink with plenty of water.

 EXPERIMENT NO. 2

MOLECULAR WEIGHT DETERMINATION BY VAPOR DENSITY METHOD

PRELIMINARY DATA SHEET

Date: _______________ Score: _______

Group No.: __________

SIGNATURE

Leader: ________________________________ ___________________________

Members: _________________________________ __________________________

_________________________________ __________________________

_________________________________ _________________________

DATA AND RESULTS:

DATA TRIAL
1 2 3 1 2 3
Compound
Mass of empty flask(g)
Mass of empty flask and
cover (g)
Mass of flask and
condensed liquid(g)
Mass of condensed
liquid(g)
Temperature of liquid(˚C)
Mass of flask with
distilled water (g)
Mass of distilled water(g)
Temperature of distilled
water (˚C)
Density of distilled water
Volume of
water=Volume of
flask(mL)
Barometric
pressure(mmHg)
Molecular weight of gas
average
SAMPLE COMPUTATIONS

Approved by:

Professor

Guide Questions and Problems:

1. Why is it necessary to dry flask completely before vaporizing the liquid?

2. What are the possible errors in the experiment? Account for the possible causes of deviation of

the calculated values from the expected values.

 EXPERIMENT NO. 3

MEASUREMENT OF DENSITY

One of the intensive properties of matter is density. It is defined as the ratio of mass and volume.
For solids and liquids, density changes with changing temperature and pressure. However, the
change may be considered negligible making them incompressible. For gases, changes in
temperature and pressure will cause a considerable change in its density. Specific gravity is the
ratio of the density of a substance and the density of a reference substance. Water at 4°C makes
the density of a substance numerically equal to its specific gravity for both solids and liquids. At
this temperature, the density of water is 1 g/mL. For gases, air is used as a reference substance.

Density of Some Liquids

Compound SG20°C/4°C Compound SG20°C/4°C Compound SG20°C/4°C
Acetone 0.791 Benzene 0.879 Glycerol 1.26050°C
CCl4 1.595 Methanol 0.892 (C2H5)2O 0.70825°C
Toluene 0.866 Ethanol 0.789 Butane 0.579

Densities of liquids may be measured by simply determining the mass of a

known volume of liquid. Some volume measuring devices may be used like
graduated cylinders and pipettes. Another device used to measure density is the
pycnometer. It is a special glass flask which is used for determining a relative
density of liquids. The bottle has a special glass stopper. The stopper has a hole
which allows liquid to overflow as the stopper is inserted so that it ensures an
accurate full fill every time. The bottle is weighed dry and filled with the liquid.
The procedure is repeated for another liquid and the density of the liquids is
compared.

For specific gravity measurements, Westphal Balance or Mohr’s Balance is used. This is used to
measure liquid densities heavier and lighter than water. A plummet is suspended from the beam
and placed in a cylinder containing the liquid sample. It works on the principle that the plummet
on the balance will be buoyed by the weight of liquid equal to the volume displaced. Riders are
placed on the beam in succession until the beam balances.

In this experiment, the densities of various liquids are determined using different methods and
the effect of solute concentration to density is evaluated.
 EXPERIMENT NO. 3

MEASUREMENT OF DENSITY

PRELAB EXERCISES

NAME: _________________________________________ DATE: _________________

PROFFESOR: ____________________________________ SCORE: ________________

1. Differentiate density and specific gravity.

2. What are the SI and AES units for density?

3. If the specific gravity of a substance is 1.15, determine its density in lb m/ft3.

4. What are the factors affecting the density of gases?

5. Describe how density is measured in a pycnometer and a chain balance.

 EXPERIMENT NO. 3
MEASUREMENT OF DENSITY

Objectives:
1. To determine the density and specific gravity of liquids.
2. To be familiar with the use of Westphal balance and pycnometer.
3. To determine the effect of concentration of solute in the density of solutions.

Apparatus:
1. Pycnometer
2. Westphal Balance
3. Graduated Cylinder – 10 mL
4. Test Tubes
5. Analytical Balance

Reagents:
1. Distilled Water
2. 30 ml Ethyl Alcohol
3. 30 ml Ethyl Acetate
4. 30 ml Methyl Alcohol
5. 30 ml Liquid sucrose

Procedure:

A. Measurement of Mass and Volume

1. Weigh an empty, dry and clean graduated cylinder (10 mL) using an analytical balance.
2. Add 10 mL of the compound to be tested and weigh.
3. Measure the temperature of the liquid in the graduate cylinder.
4. Calculate the weight of the liquid sample of known volume and compute for its density.
5. Repeat using other liquid samples.

B. Measurement of Specific Gravity using Westphal Balance

1. Check the balance if it is level by adjusting the leg support until the bubble in the level
indicator is at the center.
2. Fill the cylinder with the liquid allowing the liquid to flow along the side of the container
to avoid formation of bubbles.
3. Place the plummet on the hook and carefully immerse it in the cylinder filled with the
liquid sample.
4. Unrest the arrest knob and place the rider on the notch of the balance.
5. Move the rider just before the pointer swings fully to the right.
6. Adjust the chain until the pointer points to the middle.
7. Read the specific gravity.
8. Repeat using other liquid samples.
C. Measurement of Density using the Pycnometer
1. Weigh an empty, dry and clean pycnometer. Be sure to include the cover in weighing.
Caution: In drying the pycnometer, do not include the cover.
2. Fill the pycnometer with distilled water until it overflows. Cover it, wipe the spilled
liquid completely and weigh.
3. Read the temperature. Determine the density from a table according to the temperature
read.
4. Calculate the volume of water based from the density and mass of the liquid in the
pycnometer. The volume of water is also the volume of the pycnometer.
5. Repear the above procedures for other liquid samples.

D. Effect of Solute Concentration to Density

1. Prepare 30 ml solutions of methanol, ethanol and sucrose with the following
concentrations: 10%, 30%, 50%, 70% and 90%.
2. Determine the density using the pycnometer and record its temperature.
3. Plot the density (g/mL) versus solute concentration.
4. From the plot, determine the density of pure methanol and ethanol.

Disposal of Chemicals
1. Place solutions in appropriately labeled containers.
2. Sucrose solutions may be disposed directly to the sink.
 EXPERIMENT NO. 3
MEASUREMENT OF DENSITY

PRELIMINARY DATA SHEET

Date: _______________ Score: _______

Group No.: __________

SIGNATURE

Leader: ________________________________ ___________________________

Members: _________________________________ __________________________

_________________________________ __________________________

_________________________________ _________________________

I. Measurement of Mass and Volume

COMPOUND

Mass of empty container (grams)

Temperature of liquid sample (°C)
Volume of Liquid Sample (mL)
Mass of empty container + liquid (grams)
Mass of liquid sample (grams)
Density of liquid sample (g/mL)

II. Measurement of Specific Gravity using Westphal Balance

COMPOUND

Temperature (°C)
Specific Gravity

III. Measurement of Density using Pycnometer

Mass of empty pycnometer grams
Mass of pycnometer + water grams
Temperature of water °C
Mass of water grams
Density of water g/mL
Volume of water = volume of pycnomter g/mL
 COMPOUND

Mass of pycnometer + liquid (grams)

Temperature of liquid sample (°C)
Volume of liquid sample (mL)
Mass of liquid sample (grams)
Density of liquid sample (g/mL)

IV. Effect of Solute Concentration to Density of Solutions

Solute Concentration COMPOUND
(%wt)
10%
30%
50%
70%
90%

Approved by: ____________________

PROFESSOR

Guide Questions and Problems

1. Discuss the possible sources of errors in the experiment.

2. Is it possible to determine the density of liquids at high temperature using

Pycnometer?
 EXPERIMENT 4

MEASUREMENT OF VISCOSITY

Viscosity is the measure of resistance of offered by a fluid to flow of another fluid. For gases, an
increase in the temperature and pressure results in the increase in viscosity. However, the
viscosity of gases in slightly affected at low pressures. For liquids, an increase in temperature
results in the decrease of viscosity.

Viscosities of liquids are measured using an Ostwald Viscometer or Falling Sphere Viscometer.
The operation of Ostwald Viscometer is governed by the Poiseuille Equation given as follows:

where P = pressure head

r = radius of the capillary tube
L = length of the capillary tube
V = volume of the fluid
T = time of efflux

Using a standard liquid, the ration of the viscosities yields

Another method employed to measure the viscosities of the liquids is the Falling Sphere
Viscometer. The viscometer consists of a cylindrical tube containing a liquid of density, . A
steel ball of radius, r and density, ρ is dropped through the neck of the tube. The time, t for the
steel ball to pass through the fixed points of length, L is measured and the viscosity, µ of the
liquid is calculated using Stokes’ Law as follows:

Stokes’ Law is applied for free settling in the laminar region. It is assumed further that the radius
of the ball used is greater than the distance between the molecules of the fluid. If the procedure is
repeated using a standard liquid, the equation is reduced as follows:
Fluids can be classified according to their rheological behavior. Rheology deals with the
relationship between the shear stress and shear rate ion a real fluid.

Consider a thin layer of fluid between two parallel plates at a distance apart.

Fixed Plate of Area, A

From the figure, the velocity, v increases as the distance, from the fixed plate increases

Similarly,
Where µ is the Newton’s coefficient of viscosity

Real fluids or viscous fluids are fluids of finite viscosity. Non-viscous fluids have zero viscosity
but are compressible. Viscous fluids can be classified as Newtonian and non-Newtonian
according to Newton’s law of Viscosity.

Fluids with constant viscosity at varying shear rate are called Newtonian Fluids. Non-Newtonian
fluids are those which viscosities are function of shear rate. Non-Newtonian fluid can be further
classified according to the manner their viscosities vary with shear rate. Real plastics are fluids
with constant viscosity at high shearing rate. Suspensions of clay in water behave like a real
plastic. Bingham plastics or ideal plastics behave like a Newtonian fluid only when introduced
with a minimum deformation (yield stress). Sewage sludge is a typical example of a Bingham
plastic. Pseudoplastics are fluids that have decreasing viscosity with rate of shear but its
viscosity becomes constant at high shear rate. These types of fluids are commonly gels like
polystyrene in organic solvents and metallic soaps in gasoline. Dilatant fluids are those with
viscosities increasing with shear rate. Quicksand, butter, starch suspensions are example of
dilatant materials.

This experiment will measure the viscosity of liquids using the Ostwald Viscometer and
Viscotester at different temperatures.
 EXPERIMENT 4

MEASUREMENT OF VISCOSITY

PRELAB EXERCISES

NAME: _________________________________________ DATE: _________________

PROFFESOR: ____________________________________ SCORE: ________________

1. Define viscosity and discuss the effect of pressure and temperature on the viscosities of
liquids and gases.

2. What are the SI and AES units for viscosity?

3. Describe how viscosity is measured in an Ostwald Viscosimeter and Falling Sphere

Viscometer?

4. The time of efflux of water through an Ostwald viscosimeter is 0.60 minutes. For the
same volume of an organic liquid of density 1.75 g/ml the time is 1.25 minutes. Find its
absolute viscosity at 20° C is 1 cP.

5. A steel ball of density 12.45 g/mL and 2 mm diameter requires 30 sec to fall a distance of
1 meter through a liquid of density 0.789 g/mL. Calculate the viscosity of the liquid in
Pa-sec.
 EXPERIMENT 4

MEASUREMENT OF VISCOSITY

Objectives
1. To measure the viscosity of liquids using the Ostwald Viscometer. and Portable
Viscotester.
2. To compare the measured values using two methods.

Apparatus
1. Ostwald Viscometers
2. Iron Stand
3. Iron Clamp
4. Suction Valve
5. Beaker
6. Graduated Cylinder- 10 mL
7. Pipette- 10 mL

Reagents
1. Distilled water
2. 10 ml Glycerol
3. 10 ml Ethyl alcohol
4. 10 Methyl alcohol
5. Starch solution
6. Catsup
7. Condensed Milk

Procedure

A. Measurement of Viscosity using Ostwald Viscometer

1. Clean the viscometer using chromic acid and wash thoroughly with distilled water.
2. Pas hot air to completely dry the viscometer, removing all bubbles or liquid that may
be present.
3. Pipette 5 mL of distilled water into the viscometer and measure its temperature.
4. Using an aspirator, draw the liquid to a point above the upper graduation (pointA)
5. Record the time for the liquid to pass the lower graduation of the viscometer (pointB)
6. Repeat for three (3) trials maintaining the same temperature.
7. Repeat the above procedure glycerol, methyl alcohol, and ethyl alcohol
 B. Measurement of Viscosity using Portable Viscotester (Vt-03)
1. Insert the threaded end of the rotor (available rotors are #3, #4, and #5) into the
connector hole and turn the rotor in counter-clockwise until it is completely
mounted.
2. Attached cup A to the unit and fill with starch solution up to the dip mark as
indicated in each rotor.
3. Level the instrument as indicated in the level indicator of the instrument
4. Release the clamp and urn on the power.
5. Read the viscosity according to the rotor used.
6. Use the following rotors according to the range of viscosities:
7. Repeat using catsup and condense milk

ROTOR NUMBER VISCOSITY RANGE SCALE

3 50-330 cP Lower scale
4 2-33 cP Upper scale
5 15-150 cP Middle scale

Disposal of Chemicals

1. Place used chemicals in labeled containers

 EXPERIMENT 4

MEASUREMENT OF VISCOSITY

PRELIMINARY DATA SHEET

Date: _______________ Score: _______

Group No.: __________

SIGNATURE

Leader: ________________________________ ___________________________

Members: _________________________________ __________________________

_________________________________ __________________________

_________________________________ _________________________

I. Measurement of Viscosity using Ostwald Viscosimeter

DISTILLED WATER Trial 1 Trial 2 Trial 3 AVERAGE
Temperature (o C)
Density (g/mL)
Viscosity (cP)
Time of Efflux (min)

COMPOUND

Temperature (o C)
Density (g/mL)
Viscosity (cP)
Time of Efflux (min)

II. Measurement of Viscosity using Portable Viscosity tester (Vt-03)

LIQUID SAMPLE

Temperature (o C)
Rotor Number
Viscosity (cP)
SAMPLE COMPUTATIONS:

Approved by: ________________

Professor

Guide Questions and Problems:

1. Discuss the possible source of errors in the experiment.

2. What are the factors affecting the viscosity of liquids?

 EXPERIMENT NO. 5

CALORIMETRY: MEASUREMENT OF HEAT OF REACTION

Calorimetry is the measurement of heat changes and a calorimeter is used to measure the heat
involved in any physical and chemical processes. The following heats of reaction can be
measured using a calorimeter:

a. Combustion
b. Dissolution, dilution or mixing
c. Neutralization etc.

There are two basic types of calorimeter: the open-type (constant pressure) and the bomb
calorimeter (constant volume). Figure 1 shows inner sections of various calorimeters:

Figure 1a. OPEN TYPE CALORIMETER Figure 1b. BOMB TYPE

CALORIMETER

From the statement of the First Law of Thermodynamics, the change in the internal energy is due
to the exchange of heat and work across the boundary of the closed system. Mathematically, U
= Q + W where U is the sum of the kinetic and potential energy at a system due to microscopic
position and movement and Q and W (equal to –P V) are heat and work that is either absorbed
or released, and done on or done by the system, respectively. The sign convention for Q and W
are assigned as follows:

HEAT (Q) WORK (W)

released by the system
- work done by the system -
(exothermic)
absorbed by the system
+ work done on the system +
(endothermic)
The enthalpy of a system is a thermodynamic function so defined to express U+PV in flow
processes. Thus, H = U + P V at constant pressure. Since U = Q – P V the two equations
can be simplified to:

H= U+P V=Q

H = QP

This simply implies that, heat released or absorbed at constant pressure is a measure of the
change in enthalpy of a system. Therefore, heat measured in an open-type calorimeter is a
measure of H.

At constant volume, V = 0…

U=Q–P V=Q

U = QV

Similarly, the heat released or absorbed at constant volume is a measure of the change in internal
energy so as in bomb calorimeters.

For solids and liquids, H is approximately equal to Usince changes in volume are assumed to
be negligible when heat and work are applied.

For gases, assuming that ideal behavior, the ideal gas equation can be applied thus,

H = U + ( ng)RT

Where ng = n gas, constant - n gas, reactant

In bomb calorimeters, reaction occurs in a vessel immersed in a known mass of water. The whole
assembly is insulated so as to avoid heat transfer from the surroundings. When a reaction
releases heat, water and the calorimeter absorb the heat. No heat is assumed to be dissipated to
the surroundings. In so doing, the temperature of water and the calorimeter will rise. A stirrer is
installed to ensure the uniformity of the temperature. Thus,

Qreaction + Qcalorimeter + Qwater = 0

Qreaction = - (Qcalorimeter + Qwater)

U = Qreaction = - [ (Ccal T) + (mc T)water ]

Heat Capacity (C) of a substance is the amount of heat required to raise the temperature of a
substance by one degree temperature. Specific Heat (c) is the amount of heat required to raise the
temperature of a unit-mass of a substance by 1 oC. A British Thermal Unit (BTU) is the heat
required to raise the temperature of 1 pound-mass of a substance by 1oF. Thus at constant
pressure, U = CvdT and at constant volume, H =CpdT.

In this experiment, the heat capacity of the calorimeter is determined along with the heats of
neutralization, dilution and neutralization using a constant pressure calorimeter.
 EXPERIMENT NO. 5

CALORIMETRY: MEASUREMENT OF HEAT OF REACTION

PRELAB EXERCISES

NAME:____________________________________________DATE:_____________________
PROFESSOR:_______________________________________SCORE:____________________

1, Calculate the standard enthalpy of reaction of the following:

a. C2H2(g) + O2(g)  2CO(g) + H2O(l)

b. NaOH(s) + HCl(g)  NaCl(s) + H2O(l)
c. H2SO4(l) + 2 NaOH(s)  Na2SO4(s) + H2O(l)

2. What are the two basic types of calorimeter? Differentiate these calorimeters.

3. Write the thermochemical equations of the following reactions at 25oC.

a. Formation of CH4(g)

b. Combustion of CH3OH(l)

c. Dissolution of SO3(g) in H2O

4. The molar heat of combustion of liquid ethyl alcohol is -1336.91 kcal/mole. If 300 mg of ethyl
alcohol is burned in a calorimeter causes a rise in temperature of 2.225oC. What is the total heat
capacity of the calorimeter?
 EXPERIMENT NO. 5

CALORIMETRY: MEASUREMENT OF HEAT OF REACTION

Objectives:

1. To measure the heat capacity of an improvised calorimeter.

2. To determine the heat of neutralization , solution and dilution

Apparatus:

1. 2 Thermometers
2. 2 Improvised calorimeter

Reagents:

1. Distilled water
2. 25 ml Concentrated hydrochloric acid
3. 15 ml Concentrated sulfuric acid
4. 80 ml 1M NaOH
5. 1.5 g NH4Cl

Procedure:

A. Thermometer Calibration
1. Label two thermometers as thermometer A and thermometer B to be used for calorimeter
A and calorimeter B, respectively.
2. Dip both thermometers in a beaker filled with distilled water. Record the temperature
readings on both thermometers.
3. For thermometer B, account for any difference and record difference as correction factor
in relation to thermometer A. add the difference to all readings of thermometer B.
otherwise subtract the difference from all readings of thermometer B.

B. Determination of Heat Capacity of Calorimeter

1. Dry the Styrofoam cups and fill calorimeter A with 25mL water at a temperature above
70oC and calorimeter B with 25 mL distilled water at room temperature.
2. With the cover and thermometer in place, transfer the contents of calorimeter B to
calorimeter A and cover it immediately.
3. Record the temperature reading of thermometer A until a constant value is attained that
lasts for two minutes.

C. Heat of Neutralization
1. Prepare 25mL of 1.0 M of HCl solution in calorimeter A and 25 mL of 1.0 M of NaOH
solution in calorimeter B. Allow to stand until both solutions attain room temperature.
 2. Quickly pour the contents of calorimeter B to calorimeter A.
3. Record the temperature reading of thermometer A until a constant value is attained that
last for two minutes.

D. Heat of Solution
1. Measure 400 mg of NH4Cl in calorimeter A and 50 mL of distilled water in calorimeter
B.
2. Pour water in calorimeter A to calorimeter and record the temperature reading of
thermometer A until a constant value is attained that lasts for two minutes.

E. Heat of Dilution
1. Measure 25 mL of distilled water in calorimeter A and 5 mL of concentrated sulfuric acid
in calorimeter B.
2. Pour the acid to calorimeter A and record the temperature reading of thermometer A until
a constant value is attained that lasts for two minutes.

Disposal of Chemicals

1. Combine solutions obtained from part C and E and titrate with 0.1 M NaOH and dispose
resulting solution directly to sink with plenty of water.
 EXPERIMENT NO. 5

CALORIMETRY: MEASUREMENT OF HEAT OF REACTION

PRELIMINARY DATA SHEET

Date: _______________ Score: _______

Group No.: __________

SIGNATURE

Leader: ________________________________ ___________________________

Members: _________________________________ __________________________

_________________________________ __________________________

_________________________________ _________________________

I. Thermometer Calibration

Thermometer A Reading
Thermometer B Reading
Correction Factor for Thermometer B

II. Determination of Heat Capacity of Calorimeter

TRIAL 1 TRIAL 2 TRIAL 3

Temperature of water in Calorimeter
A
(
Density of water in Calorimeter A
(g/mL)
Temperature of water in Calorimeter B
(
Density of water in Calorimeter B
(g/mL)
Temperature of mixture in calorimeter
A
Heat Capacity of Calorimeter A
III. Heat of Neutralization

TRIAL 1 TRIAL 2 TRIAL 3

Temperature of HCl(aq.) in Calorimeter
A
(
Temperature of NaOH(aq.) in
Calorimeter B
(
Temperature of mixture in calorimeter
A
Heat of Neutralization per mole H2O
produced

IV. Heat of Solution

TRIAL 1 TRIAL 2 TRIAL 3

Mass of NH4Cl (grams)
Temperature of H2O in Calorimeter
(
Density of water in Calorimeter B
(g/mL)
Heat of solution per mole NH4Cl
dissolved
Final temperature of solution (0C)

V. Heat of Dilution

TRIAL 1 TRIAL 2 TRIAL 3

Temperature of water in Calorimeter
A
(
Density of water in Calorimeter B
(g/mL)
Temperature of H2SO4(aq.) in
Calorimeter B
(
Temperature of mixture in calorimeter
A
Heat of Dilution per mole H2SO4
SAMPLE COMPUTATIONS:

Approved by :____________________
PROFESSOR
 EXPERIMENT NO. 6

MEASUREMENT OF REFRACTIVE INDEX

Refractive index is a measure of the extent of the bending (refraction) of light as it passes
through a transparent media, either towards or away from the normal. It is also defined as the
ratio of the velocity of a radiation at a particular frequency in a vacuum to that of a given
medium. Snell’s law governs the refraction of lights in various media. It states that the sine of the
angle of incidence and the sine of the angle of refraction are constant. Mathematically,

Consider the following:

Incident ray θi

air

glass

θr Refracted ray

It is observed that when light passes from a less dense medium, like air, to a denser medium like
glass, the beam of light is deflected towards the normal.

The extent of interaction between electromagnetic radiation and the medium through which it
passes is a measure of the medium’s refractive index. Mathematically, it can also be expressed as
Water a room temperature has a refractive index of 1.33. . This means that radiation passes
through water at a rate of c/1.33 or light travels 1.33 times slower in water than it does in a
vacuum.

With this, the refractive index different concentrations of solutions of different density can be
determined. This will serve as a standard solution. It is however noted that the refractive index is
directly proportional to the concentrations of a solution. Thus, if plotted, a linear plot may be
obtained and the concentration of unknown solutions can be obtained by interpolation.

This experiment deals with measurement of refractive index using a refractometer. Refractive
indices of various concentrations of solutions will be determined as standards for determining
concentrations of unknown samples.
 EXPERIMENT NO. 6

MEASUREMENT OF REFRACTIVE INDEX

PRELAB EXERCISES

NAME: _______________________________________ DATE: _______________

PROFESSOR: _________________________________ SCORE: _____________

1. Discuss the different regions of the electromagnetic spectrum and the quantum change of
these regions.
 EXPERIMENT NO. 6

MEASUREMENT OF REFRACTIVE INDEX

Objectives

1. To measure the refractive index of solutions

2. To compare the measured values using two methods

Apparatus

1. Leica Abbe Mark II Refractometer

2. Dropper
3. Test tube

Reagents

1. Sucrose
2. Ethyl Alcohol

Procedure

A. Calibration with distilled water

1. Place two to three drops of distilled water on the

measuring prism and let it stand for three minutes
to attain temperature stability.
2. Turn the mode selector switch to refractive index
position.
3. Focus the eyepiece until the crosshair appears
clearly.
4. Rotate the adjustment control clockwise until the
shadow line meets the crosshair. Using the
dispersion correction wheel, obtain the sharpest
color-free shadow line.
5. Press the read button and record the temperature and refractive index.
6. If the instrument is properly calibrated. The reading should be 1.3330 or less 0.0001
for each degree above 20 degrees Celsius.

B. Measurement of Refractive index of solutions

1. Prepare solutions of ethyl alcohol and sucrose to make solutions with concentrations
10% to 90% in 10% interval.
 2. Before replacing each solution to be tested, clean the prism surface by two drops of
distilled water and wipe with clean cloth.
3. Obtain an unknown sample from your instructor and determine.

Disposal of Chemicals

1. Alcohol and sucrose solutions may be disposed directly to the sink.

 EXPERIMENT NO. 6

MEASUREMENT OF REFRACTIVE INDEX

PRELIMINARY DATA SHEET

Date: _______________ Score: _______

Group No.: __________

SIGNATURE

Leader: ________________________________ ___________________________

Members: _________________________________ __________________________

_________________________________ __________________________

_________________________________ _________________________

I. Calibration using Distilled Water

DISTILLED WATER TRIAL 1 TRIAL 2 TRIAL 3 AVERAGE

Temperature ( )
Refractive Index

II. Measurement of Refractive Index of Solutions

LIQUID SAMPLE

CONCENTRATIONS REFRACTIVE TEMPERATURE REFRACTIVE TEMPERATURE

INDEX INDEX
10%
20%
30%
40%
50%
60%
70%
80%
90%
 LIQUID SAMPLE

UNKNOWN REFRACTIVE CONCENTRATIONS REFRACTIVE CONCENTRATIONS

SAMPLES INDEX INDEX
Unknown 1
Unknown 2
Unknown 3
Unknown 4
Unknown 5

Approved by: ______________

Professor

Guide Questions and Problems:

1. What are the possible sources of error in the experiment?

2. What is the effect of concentration on the refractive indices of solutions?

GRAPHS

Refractive index vs. Concentration

SUCROSESOLUTIONS

Refractive index vs. Concentration

ETHANOL SOLUTIONS
 EXPERIMENT NO. 7

POLARIMETRY

A compound is considered to be optical active if it can bend a plane of a polarized light.

Polarimetry is a sensitive and non-destructive technique to measure optical activity of organic
and inorganic compounds. The molecular structure and the concentration of the chiral molecule
in a compound determine the degree o optical rotation. The specific of an optical active
substance is defined mathematically by Biots law given as follows:

[α]λT = αTλ / LC

where: [α]λT = specifical rotation at wavelength, λ and temperature T.

αTλ = optical rotation

L = optical path length

C = concentration in g/mL

Polarimeter is the nstrument used to study optical rotation of chiral molecules. A polarimeter is
equipped with a light source providing light vibrating in all planes. A fixed polarizer then
isolates light vibrating in all single plane, projects the lights through a tube filled ith a solution of
chiral compound, and measures the amount of rotation.

In this experiment, the optical activity of sugar solutions will be determined along with lactose
content of whole milk and skimmed milk.

Source:

http://www.tadjhizyaran.org/Portals/0/polarimeter/polarimeter.jpg
 EXPERIMENT NO. 7

POLARIMETRY
Objectives
1. To be familiar with the operation of the polarimeter
2. To determine the angle of rotation on an optically active compound
3. To determine the lactose content of whole milk and akimmed milk

Apparatus
1. SR-6 Polarimeter
2. Beaker

Reagents
1. Table Sugar
2. Milk
3. Chocolate
4. Wine

Procedure

A. Determination of Specific Rotatory Power

1. Turn the polarimeter on by pressing the red on/off switch of the transformer. The
sodium lamp is lit by pressing the yellow button.
2. Turn the vernier so that the “O” is opposite the “O’ of the circular scale.
3. Adjust the magnifying lens through the measuring field such that the dividing line
between the half shadows is in focus and the half shadows appear with equal
brightness.
4. If the point on the circular scale is not exactly on the “O” of the vernier, record such
difference and account this difference in subsequent readings.
5. Using a 190.09 mm tube, remove the cap from the other end of the tube and fill the
tube completely with the sugar solution avoiding any formation of air bubbles.
6. When the tube is completely filled, slide the clean and dry glass cover disc from the
side of the tube across the opening.
7. With a dry gasket in the cap, close the end of the tube.
8. To eliminate room light, rotate the light shield over the measuring chamber.
9. If the darker half shadow is to the left, then test substance is levorotatory substance,
otherwise, a dextrorotatory substance.
10. Turn the in the same direction as the rotation until both shadows appear in equal
brightness.
11. Read the degree of rotation from the circular scale.

B. Determination of Lactose in Milk

1. Dissolve 40grams of KI in 200 mL of water and 55 grams of HgI in a 500 mL
volumetric flask. Dilute with water up to the mark.
2. Add 7.5 mL of 20% H2SO4 and 7.5 mL of HgI solution to 50 mL of whole milk and
skimmed milk.
 3. Filter the resulting solution and add water until the volume is 100 mL
4. Determine the angle of rotation, α using the polarimeter and calculate the lactose
concentration from the formula with f = 0.94 for whole milk and 0.97 for skimmed
milk.
c = ( 100 / 1.9009 x 17.5º ) α f

Disposal of Chemicals
1. Place used chemicals in labeled containers
 EXPERIMENT NO. 7

POLARIMETRY

PRELAB EXERCISES

NAME: ________________________________________ DATE: _________________

PROFESSOR :__________________________________ SCORE:________________

1. Define the following:

a. Optical isomerism
b. Chiral substance
c. Racemic mixtures

2. Differentiate and give examples of compounds that are dextrorotatory and levrotatory.

3. Disuss the operation of polarimeter.

 EXPERIMENT NO. 7

POLARIMETRY

PRELIMINARY DATA SHEET

Date: _______________ Score: _______

Group No.: __________

SIGNATURE

Leader: ________________________________ ___________________________

Members: _________________________________ __________________________

_________________________________ __________________________

_________________________________ _________________________

I. Measurement of specific Rotatory Power of Sugar Solutions

CONCENTRATION ANGLE OF ROTATION SPECIFIC
OF SUGAR AVERAGE ROTAORY
SOLUTION (g/mL) POWER
TRIAL 1 TRIAL 2 TRIAL 3

II. Determination of Lactose in Milk

WHOLE MILK SKIMMED MILK

Angle of Rotation
Lactose Content
SAMPLE COMPUTATIONS

Approved by :____________________
PROFESSOR
 EXPERIMENT NO. 8

SPECTROPHOTOMETRY

Spectrophotometry involves the analysis of a substance based on their absorbance of

light. Every atom and compound absorbs a distinct set of light wavelengths. Spectrophotometry
measure the amount of light of specific wavelengths absorbed by a compound. If a beam of light
passes through a glass container filled with liquid, the emergent radiation is always less powerful
than that entering. If the energy absorbed is greater for some visible wavelengths than for others,
the emergent beam will appear colored. The absorption of radiant energy by matter can be
described using Beer’s Law.

Consider a block of an absorbing material of concentration, c and thickness, b:

PO P

dx

-∫ dP/P= ac ∫ dx where a= molar absorptivity limits: P,P o ; b, 0

dx
Integrating between limits: -ln P/Po = abc

A= log Po / P A= absorbance or A=log 1/T εbc T=transmittance

Spectrophotometers are usually with one or more light sources. These light sources produce the
full spectrum of visible light (wavelengths from 380-750 nm), ultraviolet light (100-380 nm), or
infrared light (103-106 nm). When the light sparks the prism, it diffracts each wavelength of light
at different angles, thus spatially separating each wavelength. The beam of light then passes
through the sample in a glass or quartz cuvette of specific dimensions. Light transmitted by the
sample enters a photodetector, resulting in an electrical signal which is proportional to the
intensity of light. The electrical signal is converted into either an analog or digital display. A
spectrophotometer is equipped with a photodetector that measures that amount of light passing
through the sample. Readings from the spectrophotometer can be expressed in terms of either %
absorbance (amount of light absorbed by the sample) or % transmittance (the amount of light
passing through the sample).

In this experiment, the color of the beam at different wavelengths is observed and the
concentration of unknown solutions is determined using the Beer’s Law plot.
 EXPERIMENT 8

SPECTROPHOTOMETRY

PRELAB EXERCISES

NAME: ________________________________________ DATE:______________________:

PROFESSOR:___________________________________ SCORE:_______________________:

1. Describe the operation of spectrophotometer.

2. Discuss the different factors that affect the absorbance of a solution.

3. A solution containing 4.48 ppm KMnO4 has a transmittance of 0.576 in a 1.00 cm cell at
52 nm. If the transmittance of a known solution is 0.0735 calculate the concentration of
the unknown KMnO4 solution in ppm.
 EXPERIMENT NO. 8

SPECTROPHOTOMETRY

OBJECTIVES;

1. To determine the color imparted at different wavelengths

2. To determine the absorption spectrum of a solution

3. To prepare Beer’s Law plot and determine the concentration of an unknown solution
through this plot.

APPARATUS:

1. Spectophotometer

2. Cuvette

REAGENTS:

1. Cobalt (II) nitrate

2. Potassium permanganate

PROCEDURE:

A. Initial Set-up

1. Turn the instrument on by flipping the toggle switch on the lower right of the back of
the instrument.

2. Allow at least 15-30 minutes for the instrument to warm up.

3. After warm-up, select %T by pressing the MODE keypad.

4. Open the sample chamber lid and place a blank cuvette.

5. Move the shutter to the closed position and press CAL in the keypad.

6. At this point, the display will be updated to zero.

B. Color of Visible Radiation

1. Place a strip of paper near the light source and move the shutter to the open position.

2. Observe the color of the beam in 50 nm intervals from 400 nm to 800 nm.

C. Visible Spectrum of a Solution

1. Fill one cuvette with distilled water and another cuvette with 0.01 M Co(NO 3)2 to
about 2/3 of the total volume of the cuvette

2. Set the thumbwheel to the cuvette containing water and adjust the wavelength of the
spectrophotometer to 375 nm and 100% transmittance.

3. Rotate the thumbwheel to the test solution and set the wavelength to 375 nm and read
the absorbance and transmittance.

4. Repeat measurement of absorbance and transmittance of the standard solution from

wavelengths 400 nm to 800 nm at 25 nm interval. Before starting with new
measurement, recalibrate using distilled water.

5. Repeat using 0.001 M KMnO4

6. Plot the absorbance (and transmittance) versus wavelength of the solution

D. DETERMINE OF CONCENTRATION USING ABSORBANCE VALUES

1. From the maximum absorbance obtained in the previous procedure, recalibrate the
spectrophotometer using distilled water 100%T.

2. Take the absorbance of the following solutions and obtain a plot of absorbance with
concentration.
 KMnO4 Co(NO3)2

CONCENTRATIONS (M) CONCENTRATIONS (M)

0.01 0.050

0.001 0.030

0.0001 0.010

0.0001 0.005

From the Beer’s Law Plot, determine the concentrations of unknown samples.

DISPOSAL OF CHEMICALS

1. Titrate KMnO4 solutions with 0.1 M Na2C2O4 to the faintest pink color and dispose to the
sink with plenty of water.

2. Return cobalt solutions to properly labeled containers.

 EXPERIMENT 8

SPECTROPHOTOMETRY

PRELIMINARY DATA SHEET

Date ___________________ Score ____________

Group No. ______________

SIGNATURE

Leader _______________________ _________________________

_______________________ _________________________

_______________________ _________________________

_______________________ _________________________

I. COLOR OF VISIBLE RADIATION

WAVELENGTH COLOR WAVELENGTH COLOR

400 650
450 700
500 750
550 800
600

II. VISIBLE SPECTRUM OF A SOLUTION

WAVELENGTH ABSORBANCE WAVELENGTH ABSORBANCE WAVELENGTH ABSORBANCE

375 520 670
400 530 680
410 540 690
420 550 700
430 560 710
440 570 720
450 580 730
460 590 740
 470 600 750
480 620 760
490 640 770
500 650 780

III. DETERMINATION OF CONCENTRATION USING ABSORBANCE VALUES

POTASSIUM PERMANGANATE
CONCENTRATION (M) ABSORBANCE
0.01
0.001
0.0001
0.00001

UNKNOWN
CONCENTRATION

COBALT (II) NITRATE

CONCENTRATION (M) ABSORBANCE
0.05
0.030
0.010
0.005

UNKNOWN
CONCENTRATION

APPROVED BY: ____________________

PROFESSOR
 GRAPHS
Absorbance

Wavelength (nm)
Transmittance

Wavelength (nm)
 GRAPHS
Absorbance

Wavelength (nm)
Transmittance

Wavelength (nm)