GENERAL

CHEMISTRY
Laboratory Guide

This module provides guidelines for safety, Laboratory

Report and note book. It’s also providing students with
Laboratory manual for subject of General Chemistry
(CLD 10004).

FIRST EDITION
2009
 Laboratory Information

Before each lab session, you should prepare by reading the lab manual and the textbook required
reading. We expect you to have a good understanding of the purpose, details of the procedure,
the use of all chemicals and any significant hazards, and the underlying science of the experiment
when you come to lab.
 CONTENTS

Preface i

Laboratory safety Guidelines ii

Safety Declaration Form vi

Chemistry Laboratory Report Guidelines vii

Laboratory Notes Books Guidelines x

xi
Laboratory Technique

Experiment

1 Calibration of Volumetric Glassware 1

2 Empirical Formulas 9

3 Standardization of Sodium Hydroxide Solutions 15

4 Acids, Bases, Buffers and The Determination of pH 22

5 Redox Reactions 30

6 Qualitative Analysis of Common Ions 40

REFERENCES 56

APPENDICES 57
 PREFACE

This manual provides laboratory guidelines, safety declaration form, Chemistry Lab
Report guidelines and Laboratory manual for subject of General Chemistry (CLD 10004).

The primary purpose of this manual is to compile all necessary information regarding
laboratory component in one manual.

The manual contains four parts. Part 1 provides a description of laboratory guidelines and
safety declaration form. It is compulsory for student to understand all those guidelines
and submit safety declaration for recording purposes. Part 2 is laboratory report
guidelines containing all requirements such as format and arrangement in order to
produce good quality of laboratory report. Part 3 is guidelines for preparation of
laboratory notes book. Part 4 is emphasizes on basic laboratory skill including tools,
chemical as well basic technique in laboratory exercise. Part 5 is compilation of laboratory
manual that will provide student practical guidelines in General Chemistry.

There may be shortcomings which we had overlooked but hopefully these should not
hinder the process of enhancing laboratory skill.

Mohd Zulkhairi Abdul Rahim

 PART 1

LABORATORY SAFETY GUIDELINES

General Guidelines

1. Conduct yourself in a responsible manner at all times in the laboratory.

2. Be familiar with your lab assignment before you come to the lab. Follow all
written and verbal instructions carefully. If you do not understand a direction or
part of a procedure, ask the instructor before proceeding.
3. No student may work in laboratory alone. The lab instructor or co-coordinator
grant exceptions on a case by case basis.
4. When first entering a laboratory, do not touch any equipment, chemicals or other
materials in the laboratory area until you are instructed to do so.
5. Do not eat, drink beverages or chew gum in the laboratory. Do not use laboratory
glassware as containers for food or beverages.
6. Smoking is not allowed in any indoor area.
7. No music allowed in the laboratory. Radio (including walkman) and other
entertainment devices are not permitted.
8. No cellular phone is allowed in this laboratory.
9. Perform only those experiments authorized by the instructor. Never do anything
in the laboratory that is not called for the laboratory procedures or by your
instructor. Carefully follow all instructions, both written and oral. Unauthorized
experiments are prohibited.
10. Observe good housekeeping practices. Work areas should be kept clean and tidy
at all times.
11. Horseplay, practical jokes, and pranks are dangerous and prohibited.
12. Always work in a well-ventilated area.
13. Bring only your laboratory instructions, worksheets and report to the work area.
Other materials (books, purses, backpacks, etc) should be stored in the cabinet.
14. Know the locations and operation procedures of all safety equipment including
the first aid kit, eyewash station, safety shower, spill kit and fire extinguisher.
15. Be alert and proceed with caution at all times in the laboratory. Notify the
instructor immediately of any unsafe condition you observe.
16. Label and equipment instructions must be read carefully before use. Set up and
use the prescribed apparatus as directed in the laboratory instructions provided by
your instructor.
17. Experiments must be personally monitored at all times. You will be assigned a
laboratory station at which to work. Do not wander around the room, distract
other students or interfere with laboratory experiments or others.
18. Write your name and equipment use every time you come in to the laboratory in
the log book.
19. Defeating safety devices or using equipment in a manner other than that which is
intended will be grounds for dismissal from the lab.
 Clothing
1. Safety goggles and safety jacket must be worn whenever you work in lab.
2. Gloves should be worn whenever you use chemicals that cause skin irritations or
need to handle hot equipment.
3. Mask should be worn every time you prepare the chemicals.
4. Safety shoes and hard hat should be worn at all times while in the laboratory.
5. Contact lenses should not be worn in the laboratory unless you have permission
from your instructor.
6. Dress properly during a laboratory activity.
7. Long hair, dangling jewelry and loose or baggy clothing are a hazard in the
laboratory. Long hair must be tied back and dangling jewelry and loose or baggy
clothing must be secured.
8. Sandal, open-toed shoes, high heels or shoes with holes in the sols will not be
worn in the lab.
9. Short and skirts are not permitted.
10. Instructor and laboratory assistant have a right dismiss to you from the laboratory
if they found that you are not wearing proper safety clothing.

Handling Chemicals
1. Treat chemicals with respect and understand the chemicals you are using with
Material Safety Data Sheet (MSDS). The MSDS are available in the analytical
room.
2. All chemicals in the laboratory are to be considered dangerous. Do not touch,
taste or smell any chemical unless specifically instructed to do so.
3. Check the label on chemical bottles before removing any of the contents. Take
only much chemical are you need. Smaller amounts often work better than larger
amounts.
4. Label all containers and massing papers holding dry chemicals.
5. Never return unused chemicals to their original containers.
6. Never use mouth suction to fill a pipette. Use pipette bulb or pipette filler.
7. Acids must be handled with extreme care. Always add acids slowly to water, with
slow stirring and swirling, being careful of the heat produced, particularly with
sulfuric acid.
8. Handle flammable hazardous liquid over a pan to contain spills. Never dispense
flammable liquids anywhere near a flame or source of heat.
9. Never take chemicals or other materials from the laboratory area.
10. Take good care when transferring acids and other chemicals from one part of the
laboratory to another. Hold them securely and in the method demonstrated by the
instructor as you walk.
11. All wastes generated during the course of an experiment must be disposed of
according to the lab instructor’s directions.
12. Never mix chemicals in sink drains.
13. Sinks are to be used only for water and those solutions designated by the
instructor.
14. Solid chemicals, metals, matches, filter paper, and all other insoluble materials are
to be disposed of in the proper waste containers, not in the sink.
15. Checks the label of all waste containers twice before adding your chemicals waste
to the container.
16. Cracked or broken glass should be placed in the special container for “broken
glass”.
17. Keep hands away from your face, eyes, mouth and body while using chemicals.
Wash your hands with soap and water after performing all experiments.

Personal Hygiene
1. Wash hands before leaving the lab and before eating.
2. Gloves should be removed before leaving the lab, using telephones, or entering
common areas
Accidents and Injuries
1. Report any accidents (spill, breakage, etc) or injury (cut, burn, etc) to the
instructor immediately, no matter how trivial it may appear.
2. If you or your lab partners are hurt, immediately tell to the instructor.
3. If a chemical should splash in your eye(s), immediately flush with running water
from the eyewash station for at least 20 minutes. Notify the instructor
immediately.
4. Spills should be cleaned up immediately.

Handling Glassware and Equipment

1. Inserting and removing glass tubing from rubber stopper can be dangerous.
Always lubricate glassware (tubing, thistle tubes, thermometer, etc) before
attempting to insert it in a stopper. Always protect your hands with tower or
cotton gloves when inserting glass tubing into, or removing it from a rubber
stopper.
2. When removing an electrical plug from its socket, grasp the plug, not the
electrical cord.
3. Hands must be completely dry before touching an electrical switch, plug or outlet.
4. Examine glassware before each use. Never use chipped or cracked glassware.
5. Never use dirty glassware.
6. Do not immerse hot glassware in cold water; it may shatter.
7. Report damaged electrical equipment immediately. Look for things such as frayed
cords, exposed wires and loose connections. Do not use damaged electrical
equipment.
8. If you do not understand how to use a piece of equipment, ask the instructor for
help.
9. Be careful when lifting heavy objects. Lift comfortably, avoid unnecessary
bending, twisting, reaching out, and excessive weights, lift gradually and keep in
good physical shape.
10. Do not transfer a glassware form one laboratory to another without permission
from instructor.
 Heating Substances

1. Do not operate a hot plate by yourself. Take care that hair, clothing, and hands
are a safe distance from the hot plate at all times. Use of hot plate is only allowed
in the presence of the teacher.
2. Heated glassware remains very hot for a long time. They should be set aside in a
designated place to cool, and picked up with caution. Use tongs or heat protective
gloves if necessary.
3. Never look into a container that is being heated.
4. Do not place hot apparatus directly on the laboratory desk. Always use an
insulated pad. Allow plenty of time for hot apparatus to cool before touching it.
5. If leaving a lab unattended, turn off all ignition sources and lock the doors.

Ended the Experiments

1. At the end of the laboratory sessions, you should;
 Shut-off main gas outlet
 Turn-off the water inlet
 Desk top, floor area and sink are clean
 All equipment is cool, clean and arranged
2. All equipment use should be flushed using de-ionized water.
 SAFETY DECLARATION FORM

The Dean/Head of Campus

Universiti Kuala Lumpur
Malaysian Institute of Chemical and Bioengineering Technology
Lot 1988, Vendor City Industrial Area
Taboh Naning, 78000 Alor Gajah
Malacca

Dear Sir,

SAFETY DECLARATION

I ………………………………..………………………………………………………….
ID No ………………………. declare that I have read and understood the safety rules and
regulations in UniKL MICET. I hereby agree to abide by all the rules and regulations
stated in the safety guidelines.

9. I hereby understood the contents and will disciplinary action will be taken against
me, if I do not abide by the stated rules.

9. I am fully responsible for all my actions during laboratory sessions.

Thank you.

Yours faithfully,

……………………………….
Name:
Matrix No:
Subject:
Date:
 PART 2

CHEMISTRY LAB REPORT FORMAT

You should type your lab report. Make sure that you check your document for any spelling
errors. Each lab report is worth 100 points. You should also read the student handbook on the
subject of plagiarism. Your data and observations will be similar, but your interpretations
should not be written identically. You may not copy another student’s lab report in part or in its
entirety. If you are found guilty of this infraction, you and the person from whom you copied
will both lose points or shared total marks. In extreme cases or repeated offenses, both students
may receive a zero for the lab.

Title

Use a separate title page. Include the title of the experiment, YOUR NAME, and the date.
Also clearly indicate the name(s) of your lab partner(s).

Summary/Abstract (not more than 1 page)

It should be written after conclusion of experiment OR project. Its cover briefly about
Introduction, Objectives, Methodology, Result & discussion, Conclusion

Objectives

State the objectives of the experiment or report (point form)

Example:

The objective of the experiments was …….

Introduction

Background to the work / experiment

Example:

The purpose of this experiment was to identify the present of heavy metal in river water by
using Atomic Absorption Spectroscopy (AAS). AAS is ………….

Theory / formula used in the experiment. Do not just copy word for word from the lab handout.
The introduction should be of 1– 3 pages.
Materials

List the chemicals and equipment needed to perform the experiment.

Procedure

Write the procedure in chronological order. Again, DO NOT COPY DIRECTLY from the lab
handout. Rearrange your procedure become a passive sentence.

Example:

Prepare 0.5M NaOH solution (from manual)

0.5M NaOH was prepared (your report)

Result & Discussion

Analyze all data qualitative and quantitative. Then transfer finding into Table, Graph,
Histogram and Pie chart if necessary. This includes any observations. Make sure that your
graphs have titles, labeled axes with units, and legends. You should include the proper units
with any numbers, as well as use the proper number of significant figures based upon the lab
equipment used. DO NOT place any calculations or data analysis in this section. It may be a
good idea to reproduce here any data tables that you completed during the lab. Base on above
point, discuss on your findings and relate to your theory and objective of experiment.

Example:

Table 1: X vs. Y

Samples X (unit) Y (unit)

A
B
C
D
 50
45 y = 4.4557x + 0.9714
40 R2 = 0.9893

parameter X (unit)
35
30
25
20
15
10
5
0
0 2 4 6 8 10 12
parameter Y (unit)

Figure 1: Relationship between X and Y

Conclusions

This is the most important section. Please include the summary of the results and relate in brief
the findings / results with the theory. Answer the questions, “What did you learn?”, “Did I
accomplish the purpose?”, “How would I improve the experiment next time?”.
Recommendation is optional. The conclusion should be one paragraph of 5 – 7 sentences.

References

Write down any sources such as your textbook, the Internet, electronic
encyclopedia, books, etc. that you used.

 A list of lab manuals, books, reports, journal, world wide web (www) etc.
 Arrangement (year, alphabetical order)
 Author, title, publisher, year, chapter or page number

Example:

Smith J.M and Van Hess H.C., Introduction to Chemical Engineering Thermodynamics,
McGraw-Hill, New York, 2001, p229

Appendix

Here is where you attach any material that you think is pertinent to the lab report such as
summary of calculation involved. Also answer any questions here that are in the lab report.
You do not have to re-write the questions, but label and number them appropriately.
 PART 3

LABORATORY NOTEBOOKS

You are required to use a bound notebook in CLD 10004 Lab to record all primary data and
observations. You should prepare your notebook before coming to lab by writing the title
of the experiment on a new numbered page, summarizing relevant information from the
lab manual, and starting calculations involving molar masses, etc. Take note of theoretical
ideas and special instructions given by your instructor at the start of each experiment. Your
notebook should be a complete record of your work in lab. Notes should be able to understand
in the future, not just during the current experiment. Good note taking in lab is a valuable skill
that you can learn with a little effort and practice.

Guidelines to be followed:
1. Always bring your notebook with you to lab. You will be graded on the completeness of
your previous note taking and your preparation for the current experiment. You may use
your notebook during a lab quiz.
2. Number the pages sequentially and reserve space at the beginning for a table of contents.
3. Take your notebook during laboratory hours and record all values directly in it – not on
loose scraps of paper.
4. Specify each measured quantity by name and include the units.
5. If you make a mistake in your notebook, simply draw a solid line through the error and write
the correction nearby.
6. Tables greatly simplify data entry; they should be set up before coming to lab.
7. Write down all observations if necessary – don’t rely on your memory.
8. Save time by doing trial calculations in your notebook before filling out any report sheets.
9. Save time by making preliminary sketches of graphs (flow Chart) on the ruled lines in your
notebook.
 PART 4

LABORATORY TECHNIQUES

Handling chemicals

1. SAFETY IS THE PRIORITY. Take every precaution to prevent chemical from coming
into your skin and clothing..
2. All volatile or hazardous chemicals such as concentrated acid are placed in the fume
cupboards. Chemical that are less hazardous are placed on shelves or benches. It is wise to
assume all chemical are hazardous.
3. Before using any chemical ,reads labels carefully
4. Take only the necessary amount of chemical required for your experiment..
5. NEVER return unused chemicals to their respective bottles to avoid contaminations.
6. Discard excess chemical into appropriate waste bottles.
7. Keep the reagent shelf and laboratory balance clean and neat. Clean up any spills
immediately.
8. Wash hands thoroughly before leaving the laboratory.

Handling Apparatus

Cleaning Glassware

A11 glassware must be thoroughly cleaned before being used. use laboratory detergent and tap
water. The glassware is then rinsed first several times with tap water and finally with several
small portions of deionised water. Make sure the entire inner surface of the glassware is rinsed
each time. The glassware is clean if it is coated with a uniform and unbroken film of water. No
droplets will stick to the glass surface. Invert the glassware over a paper towel. Do not wipe or
blow dry for this may be a source of contamination. It is seldom necessary to dry the inner
surface of glassware before use (burettes, pipettes, volumetric flasks, graduated cylinders). An
organic solvent may be used for removing grease films.

Mass Measurement

Different kinds of balances are available with different degrees of sensitivities. Figure 1 is an
electronic top-loading balance, sensitivity of t 0.001 g and Figure 2 is an electronic analytical
balance, sensitivity of 0.0001 g. After placing the weighing paper or a clean, dry container
(beaker or weighing bottle) on the balance pan, the balance can be zeroed or tarred out. The
sample is then placed on the paper or container and the balance reading will give the mass of
the sample directly.
Several guidelines on the proper use of a balance are:

 Handle with care; balances are expensive.

 Be certain that the balance is levelled and zeroed before use.
  Never place any reagent directly on the balance pan. Always use weighing paper or a
clean, dry container.
 Never weigh hot or warm objects.
 Record your measurement with the proper number of significant
 figures directly onto your Report Sheet.
 After you are done, zero the balance and close the balance doors (for
 the analytical balance). Clean the balance and balance area of any
 spilled chemical.

Figure 1 Fiqure 2

 Use tongs or paper strips to handle glassware o avoid contact between glass and skin.
 For transferring small quantities of solid reagent, first dispense the reagent into the
inverted screw cap. Then transfer the reagent from the cap to the container. Return the
excess reagent from the screw cap to the reagent bottle.
 Weighing by difference
This is a method for determining a series of sample weights (for example in the
standardization of NaOH). The weighing bottle and its contents are first weighed.
Transfer the sample into a container (Erlenmeyer flask for example) by gently tapping
the weighing bottle with its top. The bottle and the remaining contents are then weighed.
This may be repeated to get the desired amount of sample.

Preparing solution

The preparation of an aqueous solution begins with either a solid reagent or a more
concentrated solution. Never insert a pipette, spatula or dropping pipette directly into the
reagent bottle. Always transfer the amount needed into another container. Solutions are usually
prepared in volumetric flasks (Figure 3).

 Fill the flask about a third or half fully with water.

 Add the solid or more concentrated reagent slowly, while swirling, into the flask.
 After the solid has dissolved, add water (drop wise when close to the
 mark) to the calibration mark.
  Insert the stopper securely; invert the flask several times to ensure that the solution is
homogenous.

Figure 3

Transferring Liquids and solutions

Transfer a liquid or solution from the reagent bottle with the aid of a stirring rod. Hold a
stirring rod against the opening of the reagent bottle and pour down the stirring rod which
should be touching the inner wall of the receiving container as shown in Figure 4.

Figure 4: Transferring liquids

Reading a meniscus

For measurement of liquids in graduated cylinders, pipettes,, burettes and volumetric flasks,
the volume of liquid is read at the bottom of its meniscus (Figure 4)
.

Figure 4:Reading a meniscus

Pipetting a liquid

Filling the pipette

Place the pipette tip well below the surface of the liquid to be pipette.(Figure 5a). Draw liquid
into the pipette until the level is above the calibration mark. Wipe the exterior of the pipette
free of adhering liquid. Touch the tip of the pipette to the wall of the reagent container and use
the pipette pump to drop the liquid level to the calibration mark (Figure 5b) while holding the
pipette in a vertical position. Then place the pipette tip within the receiving vessel and remove
the pipette pump from the pipette to deliver the liquid. The pipette tip should touch the wall to
avoid splashing. When free flow of the liquid st the tip against the inner all for - 10 seconds.
DO NOT BLOW OUT or shake out the liquid remaining at the tip of the pipette (Figure 5c).
Rinse the pipette several times with deionised water if no longer needed. Drain each rinse
through the tip.

Figure 5
Titrating

Make sure you begin with a clean burette. Close the stopcock. Rinse the burette with about 5
mL of deionised water and then the titrant. Roll each rinse around the burette to make sure the
liquid rinses the inner wall of the burette. Empty each rinse through the burette tip. Figure 6a
shows the titration set-up. Close the stopcock. Using a clean funnel, fill the burette to above the
zero mark. Releases liquid briefly to remove any bubbles in the tip. Allow 10 - 15 seconds for
the titrant to drain from the wall. Record the volume of the titrant to the nearest  0.01 mL.
Figure 6b is titration technique.

(a) (b)

Figure 6
Recording Data

 Record all data and observation directly into notebook in ink. Neatness is desirable.
 Supply each entry or series of entries with heading and label.
 Specify each measured quantity by name and include the units.
 Tables greatly simplify data entry; they should be set up before coming to lab.
 Record all data and observation directly into notebook in ink. Neatness is desirable.
 Supply each entry or series of entries with heading and label.
 Specify each measured quantity by name and include the units.
 Tables greatly simplify data entry; they should be set up before coming to lab.
Others Laboratory equipment
 PART 5

EXPERIMENT 1

CALIBRATION OF VOLUMETRIC GLASSWARE

OBJECTIVES

• To calibrate a 10 mL volumetric pipette.

• To calibrate a 25 mL volumetric pipette.
• To calibrate a 100 mL volumetric flask.
• To calibrate a 50 mL measuring cylinder.

INTRODUCTION

Volumetric glassware is marked with TD for ‘to deliver’ and TC for ‘to contain’ and also
with the temperature at which the calibration applies. For greatest accuracy, volumetric
glassware should be calibrated to measure the volume that is actually contained in or delivered
by a particular piece of glassware. The calibration is done by measuring the mass of water
contained in or delivered by the glassware. The density of water at a particular temperature is
used to convert mass into volume. Pipettes and burettes are calibrated to deliver specific
volumes; whereas, volumetric flasks are calibrated on a to contain basis.

EXPERIMENTAL PROCEDURE
You must use three complete trials for each of the calibration.

1) Calibration of a volumetric pipette (10 ml and 25 ml).

a) Obtain a transfer pipette. If distilled water does not drain uniformly but leaves droplets
of water in the inner surface, the pipette should be cleaned. Use a cleaning solution or
detergent to clean the pipette (ask your instructor). Please make sure you have read
(Laboratory techniques) or have been shown the correct way of pipetting by your
instructor.

b) The water used for calibration should be in thermal equilibrium i.e same
temperature with the surroundings. The temperature should be recorded at uniform
intervals. Weighing to the nearest milligram will be satisfactory and the use of a top
loading balance is sufficient. Weighing bottles or small conical flasks with a stopper
can be used as containers to hold the calibration liquid.

i. Weigh an empty weighing bottle to the nearest milligram.

ii. Fill the pipette to the mark with distilled water.

 iii. Drain the water by gravity (remove pipette bulb or pump) into the weighing bottle
and cap the bottle to prevent evaporation.

iv. Weigh the bottle again to find the mass of water delivered from the pipette.

v. Use the following equation to convert mass to volume:

True (actual) Volume = (grams of water) x (volume of 1 g of H2O in Table 4.1)

Notes:

 Repeat the procedure another 2 times

 Perform the above procedure on each of the pipette.

2) Calibration of a volumetric flask (100 ml).

a) Get a 100 mL volumetric flask. Make sure the flask is clean and dry. (Dry the flask
by clamping the flask in an inverted position at room temperature if necessary. Do not
dry a volumetric flask in an oven. Very seldom volumetric flasks need to be dried).
Weigh the flask to the nearest milligram.

b) Fill the flask to the mark with distilled water and weigh again.

c) Calculate the mass of water contained in the flask.

d) Convert the mass of water to volume

3) Calibration of a measuring cylinder (50 ml)

Calculate the mass of water contained in the cylinder and convert it to volume
by the procedure you think most appropriate.

Table 1: Volume occupied by 1.000g of water weighed in air

Temperature,°C Volume, mL at ToC

20 1.0028
21 1.0030
22 1.0033
23 1.0035
24 1.0037
 25 1.0040
26 1.0043
27 1.0045
28 1.0048
29 1.0051
30 1.0053
31 1.0056
32 1.0058
33 1.0061

Standard Deviation ( σ )
Sample Standard Deviation

The standard deviation value represents the average distance of a set of scores from the mean.
It is a statistical measure of the precision for a series of repetitive measurements. The sample
standard deviation, s, is the positive square root of the sample variance.

Where is the sample, is the mean of the sample and N is sample size
 RESULTS

A) DATA:

i) 10 mL pipet
Trial 1 Trial 2 Trial 3

Mass of container + water (g) :

Mass of container (g) :

Mass of water (g) :

Temperature (˚C) :

Actual volume (mL) :

Average volume (mL) :

Standard deviation, σ :

Relative standard deviation (σ / x ) :

ii) 25 mL pipet
Trial 1 Trial 2 Trial 3

Mass of container + water (g) :

Mass of container (g) :

Mass of water (g) :

Temperature (˚C) :

Actual volume (mL) :

Average volume (mL) :

Standard deviation, σ :

Relative standard deviation (σ / x ) :

iii) 100 mL volumetric flask

Trial 1 Trial 2 Trial 3

Mass of flask + water (g) :

Mass of flask (g) :

Mass of water (g) :

Temperature (˚C) :

Actual volume (mL) :

Average volume (mL) :

Standard deviation, σ :

Relative standard deviation (σ / x ) :

iv) 50 mL measuring cylinder

Trial 1 Trial 2 Trial 3

Mass of flask + water (g) :

Mass of flask (g) :

Mass of water (g) :

Temperature (˚C) :

Actual volume (mL) :

Average volume (mL) :

Standard deviation, σ :

Relative standard deviation (σ / x ) :

[4 x 15 marks]
 Discussion

(Hints: Discuss on your findings and relate to your theory and objective of experiment)

[10 marks]
Conclusion

(Hints: Conclusion should contain summary of the results, sum up what you have learned
from the lab. The conclusion should be one paragraph of 5 – 7 sentences).

[10 marks]
 Appendix

Questions

1. Please tell in simplest way what a calibration is.

[4 marks]

2. Draw a flowchart for the calibration of 50 mL measuring cylinder.

[10 marks]
5. A 50 mL pipet delivers 49.960g of water at 27 0 C. Calculate the volume delivered by
this pipet at 28 0 C (given 1.000g of water weigh in air occupies 1.0048 mL at 28 0 C )

[6 marks]

Total Marks = 100

 EXPERIMENT 2

EMPIRICAL FORMULAS

OBJECTIVE
To determine the empirical formula of a compound formed by a combination reaction.
INTRODUCTION

The empirical formula of a compound is the formula written with the smallest whole number
ratio of moles of the elements in the compound. The percentage composition of a compound
will enable to obtain the empirical formula. To determine the empirical formula experimentally,
the following is required:

 Determine the mass of each element in the compound.

 Calculate the number of moles of each element.
 Express the ratio of the moles of each element as integers.

For example, when a compound of nitrogen and oxygen is analyzed, it is found that the sample
contains 0.500g N and 1.142g O.

The numbers of moles of these elements are:

0.500g X 1 mol N = 0.0357 mol N ; 1.142g X 1 mol O = 0.0714 mol O
14.0g N 16.0g O

The mole ratio of nitrogen : oxygen is 0.0357 : 0.0714. The mole ratio in integers is 1 : 2
(divide each number by the smaller number i.e 0.0357 = 1 ; 0.0714 = 2 )
0.0357 0.0357

Hence, the empirical formula is NO2. The formula NO2 states that 14.0 g (1mol) of nitrogen
combines with 32.0 g (2 mol) of oxygen to form 46.0 g (1 mol ) of NO2.

In this experiment, a combination reaction of magnesium and oxygen is used to determine the
empirical formula of magnesium oxide. The initial mass of the magnesium and the mass of the
magnesium oxide formed are measured.

MATERIAL AND METHOD

Chemicals: Mg ribbon
A. Preparation of a clean crucible
1. Take a clean crucible and a lid and check the crucible for any crack or other flaws. If
any is found, request for another one.
 2. Place the crucible and lid on a clay triangle and heat with an intense flame for 5minutes.
3. Cool the crucible and lid to room temperature in a desiccator.
4. If the crucible is still dirty, move the whole setup to the fume cardboard and add 1-2
mL
6M HNO3 and gently heat the crucible, evaporate the acid to dryness.
5. Repeat heating with intense flame and subsequent cooling of the crucible.
6. When cool, remove the crucible and lid from the desiccator with tongs and weigh it
with the analytical balance (±0.0001g). Record the weight. Do not handle the crucible
with your fingers for the rest of the experiment (so that no dirt is transferred to it).

B. Combination Reaction of Magnesium (Mg) and Oxygen (O)

1. Prepare the sample:
a) Polish about 0.2-0.3 g of magnesium ribbon with steel wool.
b) Weigh the clean magnesium ribbon and record the weight to + 0.0001g. Curl the
ribbon and place it in the crucible.
c) Weigh the crucible, lid and magnesium. Record this weight to + 0.0001 g.

2. Heat the Sample in Air

a) Place the crucible with the magnesium ribbon and lid on the clay triangle
b) Heat slowly and lift the lid occasionally (now and then) to allow access of air to the
magnesium ribbon.

Caution: Rapid oxidation of the Mg will occur if too much air comes in contact with the
Mg and the Mg will burn brightly. If it does, place the lid immediately on the crucible,
allow it too cool and repeat the experiment from Part A.

3. To Complete Reaction
a) Continue heating until there is no change in the appearance of the magnesium ash in
the crucible.
b) Remove the lid. Continue heating the crucible and ash for about 30 seconds.
c) Remove the heat and cool the crucible to room temperature in a desiccator.
d) Take the mass of crucible, ash and lid and record it.

4. Test for Completeness of Reaction

a) Add a few drops of water to decompose any magnesium nitride that may have
formed.
b) Reheat the sample for 1 minute. Allow it to cool and repeat determination of the
mass of the crucible, lid and ash.
c) If this mass is greater than ±1% from that recorded in Part B.3; repeat Part B.4.
d) Wash the cool crucible with a dilute solution of 6 M HCl. Discard the solution into
the wash acids container. Rinse with tap water and then with deionised water.
5. Calculations
 a) Determine the ratio of the number of moles of magnesium to the number of moles of
oxygen.
b) Determine the formula of the pure compound.

Notes:
You must complete 3 trials of the experiment.
RESULTS
A) DATA:
No Trial 1 Trial 2 Trial 3
1 Mass of crucible + lid (g)
2 Mass of crucible + lid + Mg (g)
3 Mass of crucible + lid + Magnesium oxide:
1st measurement (g)
2nd measurement (g)
3rd measurement (g)
4 Mass of magnesium oxide (g)

(3 x 10 Marks)
Calculate the empirical formula of the compound for each trial.

The empirical formula of magnesium oxide: _____________________________

(3 x 10 Marks)
 DISCUSSION
(Hints: Discuss on your findings and relate to your theory and objective of experiment)

(10 marks)
CONCLUSION
(Hints: Conclusion should contain summary of the results, sum up what you have learned
from the lab. The conclusion should be one paragraph of 5 – 7 sentences).

(10 marks)
 Appendix

Questions

1. What is the difference between an empirical formula and molecular formula?

(5 marks)
2. Draw a flowchart for the determination of empirical formula of magnesium oxide

(5 marks)
4. A compound consisting of 62.02% C, 13.88% H and 24.10% N has a relative molecular
molecular mass of 116.21. What is the molecular formula?

(10 marks)
Total Marks = 100
 EXPERIMENT 3

STANDARDIZATION OF SODIUM HYDROXIDE SOLUTIONS

OBJECTIVES:

 To understand the applications of neutralization titration

 To standardize a sodium hydroxide solution with potassium hydrogen phthalate
 To understand the calculation for titration in order to get the concentration of the standard
solution

INTRODUCTION

In volumetric analysis which involves a titration, the volume of reagent needed to react with an
analyte is measured. Increments of the titrant from the burette are added to the analyte solution
until the reaction is complete.

Standardization

The concentration of titrant is known if it is prepared by dissolving a weighed amount of

pure reagent in known volume of solution. This reagent is called a primary standard. It
should be >>99.9% pure and stable when heated. The titrant may not be available as a primary
standard. However, the concentration of the titrant can be determined by titrating it with a
weighed primary standard. This procedure is called standardization and we call the titrant
a standard solution.
In this experiment your solution of NaOH will be standardized by titrating it against a very
pure sample of potassium acid phthalate (KHC8H4O4) of known mass.

NaOH (aq) + KHC8H4O4 (aq)  NaKHC8H4O4 (aq) + H2O (l)

Consider the following reaction:

aA + bB product

If VA ml of A with molarities MA, reacts completely with VB ml of B with molarities

MB in the titration, the relationship can be shown as,

MAVA a
--------- = --------
M B VB b
Practically, it is difficult to determine the equivalent point, thus a third substance called
indicator that gives a change when the substance is added with slightly excess quantity is used.
When the change occurs, it is known as the end point. It is not equal to the equivalent point.
The equivalence point occurs when the amount of titrant added is sufficient for a
stoichiometric reaction with analyte. What is actually measured is the end point which there is
change in color of the indicators used in the titration.

Volumetric analysis also can be used to determine the concentration of unknown solution.
It is based on the stoichiometry of the reaction involved. The reaction must rapid and complete.
In this method, a standard solution from the burette is added to a solution of unknown
concentration until the equivalent point is reached. To do this, you will accurately measure
with a burette the volume of your standards base that is required to exactly neutralize the acid
present in unknown.

MATERIALS AND METHODS

MATERIALS

Apparatus / Glassware

100 ml Erlenmeyer Flasks

50 ml Graduated Cylinder
Titration Set up
Spatula
Burette
Top loading balance  0.01g

Chemicals

50 % W/W NaOH
Potassium hydrogen phthalate, KHP
Distilled Water
 METHODS

1) Standardization of NaOH

i. Weigh accurately three samples of about 0.7 g to 0.9 g solid KHP into each of the
three clean, numbered Erlenmeyer flasks.

ii. To each flasks add 50 ml of distilled water from a graduated cylinder and shake the
flask gently until the KHP is dissolved. Add 2 drops of phenolphthalein to each
flask.

iii. Titrate each of them with the NaOH solution to the end point with the first
appearance of a faint pink color that persists for 15 second. The color will fade as
CO2 from the air dissolves in the solution.

iv. Calculate the average molarity, the standard deviation and relative standard
deviation (S/X)

11) Diluted Standardization NaOH

i. Prepare a diluted standardization NaOH (diluted 5 times) in a 250 ml

volumetric flask.

ii. Weigh accurately three samples of about 0.7 g to 0.9 g solid KHP into each
of the three clean, numbered Erlenmeyer flask.

iii. To each flask add 50 ml of distilled water from a graduated cylinder and shake
the flask gently until the KHP is dissolved. Add 2 drops of phenolphthalein to
each flask.

iv. Titrate each of them with NaOH solution to the end point with the first
appearance of a faint pink color that persist for 15 seconds. The color will fade
as CO2 from the air dissolves in the solution.

v. Calculate the average molarity, the standard deviation and relative standard
deviation (S/ X)
 RESULTS

1) STANDARDZIDATION OF NaOH SOLUTION

TRIAL 1 TRIAL 2 TRIAL3

Mass of KHP (g)

Final burette reading, NaOH (mL)

Initial burette reading, NaOH (mL)

Volume of NaOH (M)

Molarity of NaOH (M)

Average molarity of NaOH (M)

Standard deviation, σ

(Please show all calculation steps in your Jotter book)

11) DILUTED STANDARDIZED NaOH SOLUTION

TRIAL 1 TRIAL 2 TRIAL3

Mass of KHP (g)

Final burette reading, NaOH (mL)

Initial burette reading, NaOH (mL)

Volume of NaOH (M)

Molarity of NaOH (M)

Average molarity of NaOH (M)

Standard deviation, σ

(Please show all calculation steps in your Jotter book)

[2x 30= 60 marks]
 DISCUSSION

(Hints: Discuss on your findings and relate to your theory and objective of experiment)

[10 marks]

CONCLUSION

(Hints: Conclusion should contain summary of the results, sum up what you have learned
from the lab. The conclusion should be one paragraph of 5 – 7 sentences).

[10 marks]
 Appendix

QUESTIONS

1. Define the terms below:

i. Titration

[2 marks]

ii. Titrant

[2 marks]

2. What volume of a 1.420 M NaOH solution is required to titrate 25.00 mL of a 4.50 M

H2SO4 solution?

2NaOH + 2NaOH  Na2SO4 + 2H2O 4

[6 marks]
3. Dilution is the procedure for preparing a less concentration solution from a more
concentrated solution. Please show a flow chart and calculation step on how to prepared a
diluted standardization NaOH (diluted 5 times) in a 250 ml volumetric flask

[10 marks]

Total Marks = 100

 EXPERIMENT 4

ACIDS, BASES, BUFFERS AND THE DETERMINATION OF pH

OBJECTIVES

1. To determine the pH of various concentrations of acids, bases and salts.

2. To learn the concept of buffers.

INTRODUCTION

In this experiment, the pH of various solutions of acids, bases and salts will be
determined using a pH meter.

Strong Acids and Bases

When a strong acid such as HCI or a strong base such as NaOH dissolves in water, it
dissociates completely into ions as shown in the equations below:-

+ -
HCI(g) + H O (1) H O (aq) + CI (aq)
2 3

NaOH(s) + H O (1) Na+(aq) + OH- (aq)

2

+
For a strong acid or strong base, the hydronium ion concentration, [H O ] and
3
hydroxide ion concentration, [OH-], is equal to the concentration of the acid and base
respectively. The hydronium ion concentrations are expressed logarithmically as pH
values. The letter p means –log
10.

+
pH = -log [H O ]
10 3

+
The lower the pH, the higher the concentration of [H O ] and hence the higher the
3
acidity.
 -14 -
Hydronium ion concentrations commonly range from 1.0 M to 10 M. [OH ] is related
+ 0
to [H O ] by the ion product of water, K which at 25 C has the value K =
3 w w
+ - -14
[H O ][OH ]= 1.0 x 10 , Therefore:
3

+ -
-log K = -log [H O ] – log [OH ] = 14.00
w 3

and

pKw = pH + pOH = 14.00

+ -
For a neutral solution, [H O ] = [OH ] = 10-7 M or pH = pOH = 7
3

Solutions with pH values less than 7 are acidic and solution with pH values greater than
7 are basic.

Weak Acids and Bases

Weak acids and bases do not dissociate completely in solution unlike strong acids and
bases. They ionize partially as shown for acetic acid and ammonia in the following
equations.

HC2H3O2(aq) + H2O(1) H O+(aq) + C2H3O2-(aq)

3

NH3(aq) + H2O(1) NH4+(aq) + OH-(aq)

The equilibrium constants for these reactions are known as dissociation or ionization
constants. The expressions for the dissociation constants for acetic acid and ammonia
are:

Acetic acid: Ka = [H3O+][C2H3O2 -]

-5
[HC H O ] = 1.75 x 10
2 3 2

Ammonia: K = [NH4+][OH-]
b

[NH ] = 1.75 x 10 -5
3
K is the acid dissociation constant and K is the base dissociation constant. From
a b
these expression, notice that the greater the percentage of ionization (the stronger the
acid or base) the larger the K value.
Salts of weak acids and bases

Soluble salts will dissociate completely into their ions when they dissolve in water.
The anions of strong acids and the cations of strong bases do not react with water.
However, the anions and cations of weak acids and bases react with water and this
process is called hydrolysis. For example, a solution of sodium acetate will be basic
due to the hydrolysis of the acetate ion as shown in the following equation:
- -
C H O (aq) + H O(1) HC H O (aq) + OH (aq)
2 3 2 2 2 3 2

Buffer

Buffers occur in many biochemical systems. Buffers resist pH changes, that is, they
prevent significant pH changes when an acid of base added to a system. They are
solution comprising of a weak acid and its conjugate base (such as acetic acid and
sodium acetate) or a weak base and its conjugate acid (such as ammonia and
ammonium chloride).

This experiment contains two parts.

In Part A, you will measure the pH values of several solutions. Calculate the [H 3O+]
and [OH] for each solution.

In Part B, you will compare the pH change in a buffer solution and a non buffer
solution when a strong base is added.

MATERIALS AND METHODS

Materials

Chemicals:

0.1 M HC1 0.05 M HC1

0.001 M HCI 0.1 M CH3CO2H
0.1 M NaOH 0.1 M NH3
0.1 M NaCl 0.1 NaOCOCH3
0.1 NH4Cl Vinegar sample, Coca Cola sample
Solution X and Y 1 M NaOH

Equipment:

pH Meter
Methods

A. pH measurement using a pH meter

Before any pH measurement of a solution is made, make a rough guess of the pH

value for the solutions, so that you get close to the correct value. Your technician
will show you how pH is to be measured with the pH meter.

B. Buffers

Two solutions X and Y will be given to you.

-3
X = 1 x 10 M HCI and Y = 0.1M CH CO H + 0.1 M
3 2
NaOCOCH
3
(Y is a solution containing two
compounds)

1. Transfer about 30mL of solution X to a small beaker.

2. Determine its pH with the pH meter.
3. With the pH electrode still in the solution, add 1 drop of 1 M NaOH, stir, and
read/ record the pH.
4. Add 9 more drops of 1 M NaOH, stir and read/record the pH again.
5. Add 15 more drops and read/record the pH.
6. Clean out the beaker and repeat the experiment with solution Y.

RESULT
A. pH measurements
+ -
*pH pH [H O ] [OH ]
No Solution 3
(predicted) (recorded)
1 0.1 M HCI

2 0.05 M HC1

3 0.001 M HCI

4 0.1 M CH CO H
3 2

5 0.1 M NaOH

6 0.05 M NaOH

7 0.1 M NH
3
 8 0.1 M NaCl

9 0.1 NaOCOCH
3

10 0.1 NH 4 Cl

11 deionised water

12 tap water

13 Vinegar

14 Coca Cola

*Please show your predict pH calculation steps in your Jotter book- if any

B. Buffers

Solution X Solution Y

Total drops of 1M NaOH pH Total drops of 1M NaOH pH

0 0

1 1

10 10

25 25

* Compare the pH changes obtained for solution X and Y with the addition of
NaOH. Explain if there is any difference

[60 marks]
 DISCUSSION

(Hints: Discuss on your findings and relate to your theory and objective of experiment)

[10 marks]

Conclusion

(Hints: Conclusion should contain summary of the results, sum up what you have learned
from the lab. The conclusion should be one paragraph of 5 – 7 sentences).

[10 marks]
 Appendix

QUESTIONS

1) What is the pH of a solution where the hydrogen ion Concentration is 10-3M?

[4 marks]

2) In NaOH solution  OH-  is 2.9 x 10 -4 M. calculate the pH of the Solution.

[4 marks]
3) Strong acids dissociate completely to H+ ions in aqueous solutions. Examples of strong
acids are HNO3.

HNO3 + H2O  H3O+ + NO3 –

Calculate the pH of HNO3 0.001 M

[4 marks]
+
4) Conversely, weak acid do not dissociate completely to H ions in aqueous solutions. All
organic acids are weak acids. Example is nitrous acid,

HNO2 + H2O  H3O+ + NO2 –

Calculate pKa and pH of 0.01 M nitrous acid, HNO2. (Ka = 5.1 x 10 -4 M).

[8 marks]
Total Marks = 100
 EXPERIMENT 5

QUALITATIVE ANALYSIS OF COMMON IONS

OBJECTIVES

* To perform specific test for identification of some common cations and anions.
* To identify the cations/anions present in unknown samples.

INTRODUCTION

[qualitative analysis is a set of procedures to detect the presence of a specific element/ion ]

Ionic compounds are of 2 types: soluble and insoluble. Soluble salts have high solubility values
whereas the insoluble salts have very low solubility values. Soluble salt dissociates into cation
and anion when it is put in water. When cation and anion of an insoluble salt are present
together in one sample, the 2 react forming the new salt which then appears as solid/precipitate
because of its low solubility.
Soluble salts: all nitrates , all chlorides except of Pb2+, Hg22+ and Ag+ and (refer to lecture )
Insoluble salts: most sulphate except of Na+, K+ and… (Refer to lecture notes)

This experiment contains two parts: Part A and Part B

1. Part A
In this experiment, you will perform specific test for identification of some common
cations

2. Part B

In this experiment, you will perform specific test for identification of some common
anions
 Part A

QUALITATIVE ANALYSIS OF COMMON CATIONS

The precipitating reagent used for the qualitative analysis of Pb2+, Hg22+ and Ag+ is chloride
ion (Cl‾) in acidic solution. The Cl‾ ion is obtained from dissolving in water soluble chlorides
eg. NaCl ; KCl.

The chlorides of Pb2+, Hg22+ and Ag+ (i) are white in colour and (ii) are insoluble in cold
water.

Solutions that have these ions in them are used to show the above TWO (2) Properties.

The precipitation reactions for these cations that occur are as follows:

Ag+(aq) + Cl-(aq)  AgCl(s)

Hg22+(aq) + 2Cl-(aq)  Hg2Cl2(s)

Pb2+(aq) + 2Cl-(aq)  PbCl2(s)

The PbCl2 dissolves in hot water. If the 3 chlorides are present together as a mixture, by
heating the mixture in some water i.e making it hot and then filter, the Lead (II) chloride
(PbCl2) can be separated from Ag Cl and Hg2Cl2.

PbCl2(s) HEAT
 Pb2+(aq) + 2Cl-(aq)

The Pb2+ ion in solution is tested by adding a solution of K2CrO4. Pb2+ ion forms a yellow
precipitate with the chromate ion, CrO42-.

Pb2+(aq) + CrO42-(aq)  PbCrO4(s)

yellow

The other two insoluble chlorides, AgCl and Hg2Cl2 can be separated by adding aqueous
ammonia solution. AgCl dissolves forming the complex ion, Ag(NH3)2+.

AgCl(s) + 2NH3(aq)  Ag(NH3)2+(aq) + Cl-(aq)

Ammonia also reacts with Hg2Cl2 to produce finely divided metallic mercury (black in colour)
and a compound, Hg(NH2)Cl (white in colour)

Hg2Cl2(s) + 2NH3(aq)  Hg(NH2)Cl(s) + Hg (l) + NH4+ (aq) + Cl-(aq)

white black
As this reaction occurs, the solid appears to change colour from white to black to grey.
The solution containing the Ag(NH3)2+ needs to be tested further to confirm the presence of
silver. Dilute HNO3 acid is added to the solution which destroys the complex ion and
reprecipitates silver chloride.

Ag(NH3)2+(aq) + 2H+(aq)  Ag+(aq) + 2NH4+(aq)

Ag+(aq) + Cl- (aq)  AgCl(s)
________________________________________________
Ag(NH3)2+(aq) + 2H+(aq) + Cl-(aq)  AgCl(s) + 2NH4+(aq)
white

MATERIALS AND METHODS

MATERIALS

Chemicals:

Known solutions with ions (separately and together):

Known Solutions with ions Label

containing Pb2+ I
2+
containing Hg2 II
containing Ag+ III
containing Ag+, Hg22+ and Pb2+ IV

6 M HCl acid
6 M acetic acid
0.1 M K2CrO4
6 M NH3
6 M HNO3
Unknown solution.
 METHODS

1.0 Qualitative Analysis of Pb2+ ions

a) Put 1 mL of the solution I in a small test tube .Then add 2 drops of 6 M HCl. Mix
thoroughly with your stirring rod. Note down your observation.
b) Place the test tube in boiling water bath. Leave the test tube in the bath for 3 minutes;
while stirring occasionally with a glass rod. Note down your observation.
c) Divide the hot solution into 2 test tubes.
d) Take one test tube to the tap and cool the tube under running water. Note down your
observation.
e) To the other tube, add 1 drop of 6 M acetic acid and a few drops of 0.1 M K2CrO4
Note down your observation. (PbCrO4 is yellow precipitate)

2.0 Qualitative Analysis of Hg22+ ions

a) Put 1 mL of the solution II in a small test tube .Then add 2 drops of 6 M HCl. Mix
thoroughly with your stirring rod. Note down your observation.
b) Place the test tube in boiling water bath. Leave the test tube in the bath for 3 minutes;
while stirring occasionally with a glass rod. Note down your observation.
c) Filter OR centrifuge the solutions
d) Put all the precipitate together into a test tube. Add 1 mL of 6 M NH3 and stir
thoroughly. Note down your observation.
e) Discard the solid that is formed into the proper waste container for solids.

3.0 Qualitative Analysis of Ag+ ions

a) Put 1 mL of the solution III in a small test tube .Then add 2 drops of 6 M HCl. Mix
thoroughly with your stirring rod. Note down your observation.
b) Place the test tube in boiling water bath. Leave the test tube in the bath for 3 minutes;
while stirring occasionally with a glass rod. Note down your observation.
c) Filter OR centrifuge the solutions
d) Put all the precipitate together into a test tube, add 1 mL of 6 M NH3 and stir
thoroughly. Note down your observation.
e) Add HNO3 drop wise, while stirring, to the supernatant until it is acidic to litmus
paper (blue to red) by dipping a glass rod into the test solution and touching it on the
litmus paper. Note down your observation.
4.0 Qualitative Analysis of Known Mixture (Pb2+, Hg22+ and Ag+ ions) and Unknown
Mixture

Test for Pb2+ ion

a) Put 2 mL of the solution IV (Known Solution) / Unknown Mixture in a small test

tube .Then add 4 drops of 6 M HCl. Mix thoroughly with your stirring rod. Note down
your observation.
b) Filter the mixture OR centrifuge the mixture. Ask your instructor for instructions on
how to use the centrifuge correctly. After centrifuge, in the test tube there will be a
layer of clear solution (supernatant) on top of a thin layer of white precipitate.
c) Add 1 more drop of 6 M HCl to the solution from filtration or to the supernatant
d) Centrifuge again if any additional precipitate forms. Pour the supernatant into another
test tube
e) Wash the precipitate from step (2) above with 1 to 3 mL of distilled water, i.e
f) add 1-3 mL of distilled water from a wash bottle to the precipitate in the test tube, stir,
centrifuge/filter and pour out the liquid (this liquid may be thrown away)
g) Add 3 mL distill water to the precipitate. Place the test tube in boiling water bath.
Leave the test tube in the bath for 3 minute; while stirring occasionally with a glass
rod. This should dissolve the PbCl2.
h) Centrifuge/filter the hot mixture. The precipitate is used for further tests for Hg22+
and Ag+.
i) Add 1 drop of 6 M acetic acid and a few drops of 0.1 M K2CrO4 to the supernatant.
2+
A yellow precipitate of PbCrO4 will form if Pb is present.

Test for Hg22+ ion

a) To the precipitate from step 4 (g) the previous test, add 1 mL of 6 M NH3 and stir
thoroughly.
b) Centrifuge and decant the supernatant into a small test tube. A grey to black
precipitate proves the presence of Hg22+. Discard into the proper waste container
for solids.

Test for Ag+ ion

a) Add 6 M HNO3 dropwise, while stirring, to the supernatant until it is acidic to litmus
paper (blue to red) by dipping a glass rod into the test solution and touching it on the
litmus paper. A white precipitate confirms the presence of Ag+.
 Part B

QUALITATIVE ANALYSIS OF COMMON ANIONS

In this experiment, qualitative tests for SO42-, PO43-, CO32-, S2-, CI- and NO3- ions will be
carried out. These ions: SO42-, PO43-, CO32-, S2-, CI‾ and NO3- are from the soluble salts.
These tests involve a particular chemical reaction for a particular anion. To test for a particular
anion in a solution, selected chemicals are added to the solution. If the anion is present, a
unique chemical reaction occurs which will produce a product with a particular color or
form, or a gas that can be identified. If the reaction does not occur, the anion is absent.

Sulfide ion, S2-

The sulfide ion is an anion of a weak acid, H2S. When a strong acid is added to a solution that
has S2- in it, gaseous H2S will be liberated. The reaction is represented by the chemical
equation:

S2-(aq) + H+ (aq) H2S(g)

The odour of H2S can be used for identification and can be further confirmed with the
formation of a black lead sulfide, PbS.

H2S + Pb (OOCCH3)2 PbS (s) + 2 HOOCCH3

black
Sulphate ion, SO42-

It forms a white finely divided precipitates with barium ion. The reaction is represented by the
chemical equation:

Ba2+ (aq) + SO42- (aq) BaSO4(s)

The precipitate, BaSO4, is not soluble in acidic solutions. (An acidic solution of Ba2+ ions
is used to test for the presence of SO42- ion)

Carbonate ion, CO32-

Acidification of a solution that contains carbonate ions will liberate carbon dioxide which is
colourless and odourless gas. The reaction is represented by the chemical equation:

CO32-(aq) + 2H+(aq) H2O(I) + CO2(g)

The carbon dioxide gas is bubbled through an alkaline solution containing calcium ion, carbonate is
produced and a white precipitate of calcium carbonate is formed. The reaction is represented by
the chemical equation:

CO2(g) + 2OH-(aq) + Ca2+(aq) CaCO3(s) + H2O(1)

Phospate ion, PO43-

The presence of the phospate ion is detected through the formation of a characteristic
precipitate i.e. a yellow precipitate. An acidic solution is necessary. Ammonium molybdate
solution is added to the test solution. An excess of ammonium ion is added to favour
formation of a yellow precipitate of ammonium phosphomolybdate. The reaction is as
follows:-

3NH4+(aq) + 12MoO42-(aq)+ 3H+ + PO43-(aq) 21H+(aq) + (NH4)3PO412MoO(s).

yellow

Sulfide ion interferes with this test. If it is present in the test solution, it should be removed by
adding HCI to the solution than boiling it to drive out the H2S gas.

Chloride ion, Cl-

Chloride ion is precipitated as a white precipitate of silver chloride with the addition of silver
nitrate solution. The reaction is as follows:-

Ag+(aq) + CI-(aq) AgCI(s)

The presence of chloride ion is further confirmed by adding ammonia solution to dissolve the
silver chloride by the formation of soluble, complex ion, Ag(NH3)2+ and CI-. AgCI will
precipitate out again with the addition of nitric acid.

AgCI(s) + 2NH3(aq) Ag(NH3)2+(aq) + CI-(aq)

Ag(NH3)2+(aq) + CI-(aq) + 2H+(aq) AgCI(s) + 2NH4+(aq)

Nitrate ion, NO3-

All nitrate salts are soluble in aqueous solutions. The identification of nitrate does not involve
the formation of a precipitate. The ‘brown ring’ test is used. The brown ring is formed when
the nitrate ion is reduced to nitric oxide, NO, by iron (II) in an acidic solution. The reaction is
as follows:-

Conc.H2SO4
NO3-(aq) + 3Fe2+(aq) + 4H+(aq) 3Fe3+(aq) + NO(aq) + 2H2O(1)

The nitric oxide, NO, reacts with excess iron(II) ions to form a brown complex ion, Fe(NO)2+
at the interface of the aqueous layer and the concentrated acid layer.

Fe2+ (aq) + NO(aq) Fe(NO)2+(aq)

An excess of iron (II) ions is essential for this test

 MATERIALS AND METHODS

MATERIALS

Chemicals:

0.5 M ammonium molybdate (8.8g/100mL)

0.02 M Ca(OH)2
0.1 M BaCI2
Lead acetate,[Pb(CH3COO)2] paper
Saturated FeSO4 (0.16 g mL-1 FeSO4-7H2O)
6M HCI, 6M HNO3, 6M NH3, 3M H2SO4
Concentrated H2SO4 acid
Known Solutions

Solutions containing ions Label

0.1 M Na2S (freshly prepared) I

0.1 M Na2SO4 II
0.1 M Na2CO3 III
0.1 M Na3PO4 IV
0.1 M NaCI V
0.1 M AgNO3 VI

Unknown Solution

Note:

 Acids and bases used in this experiment are corrosive. Be sure to wash them off
immediately if you get them on your skin.
 METHODS

1.0 Test for suphide ion.

a) To about 2 mL of solution I, add an excess of 6 M HCI. You might notice a smell of

rotten eggs with the H2S gas given off.
b) Moisten a piece of lead acetate paper and place it over the mouth of the test tube, then
c) heat the test tube gently in the fume hood. Formation of PbS will cause the paper to
darken.

2.0 Test for sulphate ion.

a) To about 2 mL of solution II, add a few drops of 6 M HCI until the solution is acidic to
litmus paper i.e. dip a glass rod in the test solution and touch it on the litmus paper.
b) Add 1 mL of 0.1 BaCI2. White precipitate of BaSO4 will form.

3.0 Test for carbonate ion.

a) Obtain a rubber stopper fitted with a bent glass tube for the 15 cm test tube. Fill the test
tube with about 3 mL of solution III.
b) Insert the end of the bent glass tube into another test tube filled with 0.02M Ca(OH)2.
c) Lift the stopper and add a few drops of 6 M HCI to the solution.
d) Close the stopper immediately and heat the test tube gently over a low flame to boiling
point to drive any CO2 gas produced into the Ca(OH)2 solution. Do not let any of the
boiling liquid go through the tube into the Ca(OH) 2 solution.
e) A white precipitate formed in the Ca(OH) 2 solution indicates the presence of CO32- ion.

4.0 Test for phosphate ion.

a) In a 15cm test tube, mix about 1 mL of 0.5 M (NH4)2MoO4 [ ammonium molybdate]

reagent with 1 mL 6M HNO3.
b) Add 2 mL of solution IV. A yellow precipitate of (NH4)3PO4-12MoO3 formed slowly
or after warming a few minutes in warm water bath at 60oC .
* If S2- ion is present in your unknown solution, acidify 2 mL of your unknown
solution with 6 M HCI. Boil it to remove all the H2S gas. Then add it to the clear
molybdate solution.
5.0 Test for chloride ion.

a) Add a few drops of 6 M HNO3 to 2 mL of solution V to make it slightly acidic (test

with litmus paper as in 2).
b) Add 1 mL of 0.1M AgNO3. If no precipitate is formed, this will indicate there is no CI-
ion in your unknown solution.

6.0 Test for nitrate ion.

 a) Acidify (test with litmus paper) 2 mL of solution VI with 3 M H2SO4.
b) Add 1 mL of saturated FeSO4 (freshly prepared).
c) Hold the test tube at about a 45o angle and with a dropper (slowly and carefully), add 1
mL of concentrated H2SO4 acid down the side of the test tube. Do not draw
concentrated H2SO4 acid into the bulb of the dropper.
d) Do not agitate the solution. The more dense concentrated H2SO4 acid will be below the
aqueous layer. Avoid mixing the concentrated acid with the rest of the solution.
e) Allow the mixture to stand for a few minutes. A brown ring of Fe(NO)2+ at the
interface confirms the presence of NO3- ion.

Note:
 Use a fresh 2 mL sample of your unknown solution for each test. Use 15 cm test tubes
for the tests.
 RESULTS
Part A

i) Qualitative Analysis of Common Cations (Known Sample)

Record Your Observation and write an equation as return in introduction if any

Solution I II III IV

+ Cl─

Ppt. in water
And heat

Cool the
Hot solution

Hot solution
+ H+/ CrO4─

Ppt. + NH3,
then + HNO3

Ppt. + NH3

ii) Qualitative Analysis of Common Cations (UnKnown Sample)

Record Your Observation and write an equation as return in introduction if any

 Solution Unknown Sample

+ Cl─

Ppt. in water
And heat

Cool the
Hot solution

Hot solution
+ H+/ CrO4─

Ppt. + NH3,
then + HNO3

Ppt. + NH3

Unknown solution code :

Cations present :
 Part B

QUALITATIVE ANALYSIS OF COMMON ANIONS

i) QUALITATIVE ANALYSIS OF COMMON ANIONS (Known Sample)

Anions Chemical change observed Equation for observed

Known precipitate/gas/colour change Reaction
Sample Yes / No

S2-

SO42-

CO32-

PO42-

CI-

NO3-
ii) QUALITATIVE ANALYSIS OF COMMON ANIONS (Unknown Sample)

Anions Chemical change observed Equation for observed

Known precipitate/gas/colour change Reaction
Sample Yes / No

S2-

SO42-

CO32-

PO42-

CI-

NO3-

Unknown solution code :

Anions present :

(60 Marks)
 DISCUSSION

(Hints: Discuss on your findings and relate to your theory and objective of experiment)

[10 marks]

Conclusion

(Hints: Conclusion should contain summary of the results, sum up what you have learned
from the lab. The conclusion should be one paragraph of 5 – 7 sentences).

[10 marks]
 Appendix

1. Define what is meant by Qualitative analysis and Give three example of its application in
industry

[5 marks]

2. Complete the following flow chart by referring theory as return in Qualitative analysis of
common cations above (Part A)
Pb2+, Hg22+, Ag+

6 M HCl

White precipitate Solutions with other

AgCl, PbCl2, Hg2Cl2 ions

Add hot water

White precipitate Solution contains

AgCl, Hg2Cl2 _______D___________

Add______A_______ Add _____B______

______E______________ shows_____J______

____F________ Solution contains

shows ______G___________

____H__________ Add _____C______

____I______________ shows _______K_________

Fig. 2.1 Flowchart for qualitative analysis of Pb2+, Hg22+ and Ag+.

A, B, C – reagents that need to be added.

D, E, F, G, H – ions in solution or precipitate formed.
I, J, K – ion present
[15 marks]
 REFERENCES

Chang, R (2007), Chemistry, 9th ed., McGraw Hill

Raymond Chang with Brandon Cruickshank, (2005), Chemistry ,8th ed., Boston: McGraw Hill.
John McMurry, Robert C. Fay, (2001), Chemistry , 3rd ed, Prentice Hall.
Ebbing, D. ,(1996), General Chemistry, 5th ed., Houghton 4. Barrows.
Zumhal,(2007),Chemistry,7th Edition, Houghton Miffin
 EXPERIMENT 6

REDOX REACTIONS

OBJECTIVES
• To observe and predict products of oxidation-reaction reactions.
• To determine the relative reactivity of a series of metallic elements.

INTRODUCTION

Redox reactions involve a transfer of electrons. If the oxidation number of any element has
increased, the element has lost electrons and has been oxidized. In such reactions, another
element must have gained electrons and has been reduced. It has also experienced a decrease in
oxidation number. A reducing agent donates electrons for the reduction of another
substance. An oxidizing agent is a substance that gains electrons and causes the oxidation
of another substance in a redox reaction. This experiment focuses on a single replacement
reaction.

For the reaction,

Zn(s) + Pb (NO3)2(aq)  Pb(s) + Zn (NO3)2(aq)

Lead is reduced to its elemental form. Zinc is oxidized to its form. Therefore zinc metal is a
more active reducing agent than lead metal. If no reaction occurs when a metal is put unto
a solution, then the elemental form of metal in solution is a better reducing agent than the metal
put into the solution.

For the reaction,

- -
F2 (g) + 2 Br (aq)  2F (aq) + Br2(1)

Fluorine is reduced and bromine is oxidized to its elemental form. Therefore fluorine is a
more active oxidizing agent than bromine. If no reaction occurs when an oxidizing agent is
put into a solution, then the oxidized form of the negative ion already in solution is a better
oxidizing agent.

This experiment contains two parts: Part A and Part B

 1. Part A

In this experiment, you will first determine the relative reducing activities of Cu,
Fe, H, Mg and Zn.

2. Part B

you will observe and study several redox reactions

A redox reaction is divided into two half reactions, an oxidation and a reduction.

MATERIALS AND METHODS

MATERIALS

Chemicals:

Copper metal
Magnesium ribbon
Zinc metal
Steel wool
0.1 M CuSO4

3 M H2SO4 acid

0.1 M ZnSO4

0.01 M KMnO4

0.01 M K2Cr2O7

0.1 M Fe(NH4)2(SO4)2

0.1 M K2C2O4

6 M H2SO4 acid
 METHODS

Part A
Metal as reducing agents

3. Label four test tubes 1-4 (15mL test tubes)

2
4. Put a 1 cm piece of copper metal into the first test tube.
5. Put a 2 cm long piece of magnesium ribbon into the second test tube.
2
6. Put 1 cm piece of zinc metal into a third test tube.
7. Put a small ball of steel wool into the fourth test tube.
8. Add a few millilitres of 0.1 M CuSO4 to each test tube. Note if there is any reaction.
If a reaction occurs, write a balanced equation for the reaction. If not, write NR, for no
reaction.
9. Discard the used metal squares in the waste container.
10. Rinse the tubes with deionised water, and test some new metal squares in the
same way as before with 3 M H2SO4 acid.
11. Hold a lighted splint over any test tube in which bubbling occurs.
12. Clean the test tubes as before and test each metal square with 0.1 M ZnSO4
solution.

Part B

Redox reactions

1. Clean and label 4 small test tubes (3 mL test tubes)

2. Place 1 mL of each solution listed as Solution X in Table 5.1 into the test tubes.
3. Slowly add up to 1 mL of Solution Y until a permanent change is observed. Some
reactions may be slow.
4. Record your observations for each mixture that shows a reaction.
5. Write balanced redox reactions for any reaction observed. Underline the
oxidising agent in each reaction. The half reactions are given in Table 5.2.
6. Dispose of the test solutions into waste containers provided. Rinse the test tubes with
tap water.
Table 5.1 Solutions for redox reactions

Tube Solution X Solution Y

1 0.01 M KMnO4 + 2 drops 6 M H2SO4 Drops of 0.1 M Fe(NH4)2(SO4)2

2 0.01 M KMnO4 + 2 drops 6 M H2SO4 Drops of 0.1 M K2C2O4

3 0.01 M K2Cr2O7 + 2 drops 6 M H2SO4 Drops of 0.1 M Fe(NH4)2(SO4)2

4 0.01 M K2Cr2O7 + 2 drops 6 M H2SO4 Drops of 0.1 M K2C2O4

Table 5.2 Half reactions

- +
Mn04 (aq) + 8H (aq) + 5e
-
 2+
Mn (aq) + 4H20(l)
Purple light pink
to colourless

Cr2O7 (aq) + 14H (aq) + 6e 

2- + - 3+
2Cr (aq) + 7H2O(1)
Orange dark green

2+
Fe (aq)  3+
Fe (aq) + e
-

Light green red brown

to colourless

2-
C2O4 (aq)  2CO2 (g) + 2e
-

colourless colourless
 RESULTS

Part A

Metal as reducing agents

Test Tube No 0.1 M CuSO4 3 M H2SO4 0.1 M ZnSO4

1 (Copper)

2 (Magnesium)

3 (Zinc)

4 (Steel wool)

Metals as reducing agents

1. If a reaction occurs, complete and balance the equation. Write NR if there is no
reaction observed. Assume elemental iron will react to form iron (II).

Balanced Equation

CuSO4(aq) + Cu(s)

CuSO4(aq) + Mg(s)

CuSO4(aq) + Zn(s)

CuSO4(aq) + Fe(s)

H2SO4(aq) + Cu(s)

H2SO4(aq) + Mg(s)

H2SO4(aq) + Zn(s)

H2SO4(aq) + Fe(s)
 ZnSO4(aq) + Cu(s)

ZnSO4(aq) + Mg(s)

ZnSO4(aq) + Zn(s)

ZnSO4(aq) + Fe(s)

2. Arrange the four metals and hydrogen in the order of their activities beginning with the
best reducing agent and ending with the poorest reducing agent.

i.
ii.
iii.
iv.
v.
 Part B

Solution for redox reaction

Test tube Solution X Observation and Redox Reaction Equation (if any)

0.1 M Fe( NH4)2(SO4) 0.1 M K2C2O4

1 0.01 M KMnO4

2 drops 6 M H2SO4

2 0.01 M KMnO4

2 drops 6 M H2SO4

3 0.01 M K2Cr2O7

2 drops 6 M H2SO4

4 0.02 0.01 M
K2Cr2O7

2 drops 6 M H2SO4

(60 Marks)
 DISCUSSION

(Hints: Discuss on your findings and relate to your theory and objective of
experiment)

[10 marks]

Conclusion

(Hints: Conclusion should contain summary of the results, sum up what you have
learned from the lab. The conclusion should be one paragraph of 5 – 7 sentences).

[10 marks]
 Appendix

1. The following reaction does not occur spontaneously:

2+ -
Pb (aq) + 2Cl (aq)  Pb(s) + Cl2(g)
2+
Which is the more active oxidising agent, Pb or C12 ?

(2 marks]

13. Elemental Zn reacts with a aqueous Ni(II) chloride to give zinc chloride and
nickel.

a. Which is the more active metal (better reducing agent) zinc or nickel?

[2 marks]

b. Write down the oxidation and reduction half reactions and net ionic equation for the
system.

[6 marks]
3. When iron metal is placed in a solution containing lead (II) ion, iron (II) and lead metal
are produced.

a. Which is the more active metal, iron or lead?

[4 marks]

b. Write down the oxidation and reduction half reactions and the net ionic equation
for the system.

[6marks]

Total Marks = 100

 APPENDIXS

Mass Force
1 lbm = 0.453592 kg 1 lbf = 4.448222 N
1 ton = 2000 lbm 1N = 0.224809 lbf = 1 kg.m/s2
1 kg = 2.20462 lbm

Volume Density
1 ft3 = 0.028317 m3 1kg /m3 = 0.062428 lbm/ ft3
1 L = 0.001 m3
1 m3 = 35.32 ft3
1 cm3 = 0.06102 in3
1 gal =0.0037854 m3
1 gal/min = 6.31 x 10‾5 m3/s

Pressure

1 pascal (Pa) = 1 N/m2

1 atm = 760 mmHg = 760 torr
1 atm = 101.325 KPa
THIS IS THE END OF THE LABORATORY MANUAL ~