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Laboratory Guide
ANALYTICAL &
ORGANIC
CHEMISTRY
This module
provides guidelines for
CLB
10803
safety, Laboratory Report and note
Laboratory Information
Before each lab session, you should prepare by reading the lab manual, reference
book and summarized it in a jotter book. 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
10
Experiment
1
13
16
20
23
REFERENCES
26
APPENDICES
27
PREFACE
This manual provides laboratory guidelines, safety declaration form, Chemistry Lab Report
guidelines and Laboratory manual for subject of Analytical & Organic Chemistry (CLB
10803).
The primary purpose of this manual is to compile all necessary information regarding
laboratory component in one manual.
Students are compulsory to read and understand all the laboratory guidelines provided in this
manual. The safety declaration form should be submitted to the lecturer/instructor before you
start the first experiment.
In the laboratory report format, there are report writing guidelines and requirements that you
have to follow to produce a good quality of lab report.
Laboratory Jotter Notes you are required to prepare a jotter note for each experiment. In the
jotter note, you have to write the basic information of the experiment, the procedure and all
primary data and observations during the experiment. You should prepare the jotter note
BEFORE coming to the lab and submit to the lecturer/instructor BEFORE you leave the lab
on the day of experiment.
Clothing
1.
2.
Safety goggles and safety jacket must be worn whenever you work in lab.
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.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
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.
All chemicals in the laboratory are to be considered dangerous. Do not touch, taste or
smell any chemical unless specifically instructed to do so.
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.
Label all containers and massing papers holding dry chemicals.
Never return unused chemicals to their original containers.
Never use mouth suction to fill a pipette. Use pipette bulb or pipette filler.
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.
Handle flammable hazardous liquid over a pan to contain spills. Never dispense
flammable liquids anywhere near a flame or source of heat.
Never take chemicals or other materials from the laboratory area.
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.
All wastes generated during the course of an experiment must be disposed of according to
the lab instructors directions.
Never mix chemicals in sink drains.
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.
2.
1.
2.
3.
4.
Report any accidents (spill, breakage, etc) or injury (cut, burn, etc) to the instructor
immediately, no matter how trivial it may appear.
If you or your lab partners are hurt, immediately tell to the instructor.
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.
Spills should be cleaned up immediately.
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.
2.
3.
4.
5.
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.
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.
Never look into a container that is being heated.
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.
If leaving a lab unattended, turn off all ignition sources and lock the doors.
2.
Thank you.
Yours faithfully,
.
Name:
Matrix No:
Subject:
Date:
9
10
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
A
B
C
D
X (unit)
Y (unit)
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
encyclopedia, books, etc. that you used.
your
textbook,
the
Internet,
electronic
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.
12
EXPERIMENT 1
SAPONIFICATION REACTION OF FAT: SOAP PRODUCTION
OBJECTIVE
INTRODUCTION
The procedure of making soap involves the basic hydrolysis (saponification) of a fat.
Chemically, fats are referred to as triglycerides. They contain ester functional groups.
Saponification involves heating fat with an alkaline solution. The alkaline solution hydrolyzes
the fat to alcohol and the salt of a long chain carboxylic acid (soap).When common salt is added,
the soap precipitates. The soap is washed free of unreacted alkaline solution and molded into
bars.
O
R C
CH2
O
R'
CH
O
R'' C
Fat
CH2
3 NaOH
3R
HO
CH2
HO
CH
HO
CH2
+
O
Na
glycerol
13
Methods:
Preparation of Soap
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
Continue to draw air through the filter for a few minutes to partially
dry the product. Test your soap with the procedure below.
Analysis of Data
1.
Remove about 0.01 g of soap from the filter paper and placed it in a
clean 10 ml graduated cylinder
2.
Add 3 ml of distilled water, close the cylinder with your thumb and
shake the mixture vigorously for about 15 sec. After about 30 sec
standing, Record your observation. Note down the level of the
foam.
3.
4.
Then add 0.5 g of trisodium phosphate and shake the mixture again
for 15 seconds. After 30 sec. Again observe and record the result.
15
1.
EXPERIMENT 2
OBJECTIVE
(1) To determine max of Colourant (wavelength scan)
(2) To prepare a serial dilution and generate a standard calibration
graph for sample quantitation (photometric scan)
INTRODUCTION
Food coloring (colouring) is any substance that is added to food or drink
to change its color. Synthetic Food Colours, also known as Artificial
Food Colours, are manufactured chemically and are the most commonly
used dyes in the food, pharmaceutical and cosmetic industries. Besides
that, a growing number of natural food dyes are being commercially
produced, partly due to consumer concerns surrounding synthetic dyes.
Some examples include Caramel coloring (E150), made from caramelized
sugar, used in cola products and also in cosmetics. Annatto (E160b), a
reddish-orange dye made from the seed of the Achiote. A green dye made
from chlorella algae (chlorophyll, E140) and etc.
All those colourant can be analyze by using an ultraviolet/visible
spectrophotometer. Figure 1.0 below gives a schematic diagram of a
double beam spectrophotometer. Instruments for measuring the
absorption of U.V. or visible radiation are made up of the following
components; Sources (UV and visible), Wavelength selector
16
Figure 1.0
A=bc
Where;
= pathlength (cm)
c = concentration (M or mol/L)
17
18
1.
2.
3.
4.
For photometric scan, fill the cuvette as step no 3 but use the
serial dilution prepared and scan one by one. Record the
absorbance readings and look at the standard calibration graph
produced.
5.
Analysis of Data
The purpose of wavelength scan is to determine at what wavelength the
carmoisine able to absorb in the range of 200 nm to 700 nm. From
spectrum obtain, please identify max .
The purpose of photometric scan is to determine the concentration (single
component) of an unknown sample, after generating a working 'standard
curve' from a series of known standards (known concentration). Record
the absorbance readings for a series of prepared dilution generate
standards calibration curve and identify concentration of unknowns.
All calculation must show in detail.
19
EXPERIMENT 3
INTRODUCTION:
High Performance Liquid Chromatography (HPLC) is a chemistry based
tool for quantifying and analyzing mixtures of chemical compounds. It
can be used to separate compounds that are dissolved in solution. HPLC
instruments consist of a reservoir of mobile phase, a pump, an injector, a
separation column, and a detector. Compounds are separated by injecting
a plug of the sample mixture onto the column. The different components
in the mixture pass through the column at different rates due to
differences in their partitioning behavior between the mobile liquid phase
and the stationary phase.
The area of this peak (in relation to the area of other peaks) is
proportional to the concentration of that particular species in the sample.
The identity can also be found by comparing the sample peaks to
standards. Identical substances (peaks) will have identical retention
times.
MATERIALS AND METHODS
Materials:
21
22
23
EXPERIMENT 4
ORGANIC SYNTHESIS: FORMATION OF ESTER
OBJECTIVE
INTRODUCTION
Chemist use organic synthesis to make larger amounts of useful natural
compounds and to invent totally new compounds. Depending on the
choice of R and R, we have a variety of the final ester, RCOOR. Small
chain side groups give very aromatic compound, while long chain side
groups form waxy compounds.
O
R C
OH + R'
Carboxylic
acid
OH
heat
alcohol
R C
OR' + H2O
Ester
water
Apparatus:
Round bottom flask, Water condenser, retort stand, separating funnel
Methods
1. Set up a reflux system.
2. Mix 50 ml of 95% ethanol and 50 ml of glacial acetic acid thoroughly
in a 250 ml round bottomed flask. Add slowly with cooling and
shaking 10 ml of concentrated H2SO4. Ensure that the mixture is
homogenous, and then fit the flask with a reflux water condenser
and boil the mixture gently for 10 minutes. Cool the flask and its
content.
3. Rearrange the position of the condenser for distillation set up.
4. Put a few boiling chips in the flask. A filter flask, whose side arm is
joined to a rubber tube leading over the edge of laboratory bench, is
used as a receiver. Ethyl acetate is highly flammable. Therefore any
vapors should be conducted off the table towards the floor. Distilled
off about 2/3 of the mixture.
5. Transfer the distillate to a separating funnel and add about 25 ml of
30 % Na2CO3 solution. Stopper the funnel, invert it and shake it,
opening the stopcock from time to time. Allow the two layers to
separate. Carefully run off and reject the lower layer, ensuring
that the sodium carbonate is removed as completely as possible.
6. Prepare a solution of 25 g of calcium chloride in 25 ml of water.
Add if to crude ethyl acetate in the funnel. Shake vigorously. Allow
the mixture to separate. Run off the lower aqueous as completely as
possible.
7. Run the ethyl acetate into a small conical flask. Add a few lumps of
granular anhydrous calcium chloride. Shake occasionally until the
liquid is clear.
8. Decant the liquid some anti bumping granules. Arrange for
distillation (with a 0 100oC thermometer in the apparatus). Pre
25
Analysis of data
1.
From mass of acid, determine the percent yield of your final product
(Show all calculation in detail)
2. Interpret the FTIR of this compound. Identify the principles peaks.
3. Interpret Gas chromatography result.
26
REFERENCES
1. Francis A Carey, Organic Chemistry, 7th Edition, McGraw Hill
ISBN : 0073311847 / 9780073311845
2. T.W. Graham Solomon,Organic Chemistry, 8th Edition, Wiley
QD253.2.S65 2004
3. Douglas A. Skoog, Donald M. West and F. James Holler,
Fundamentals of Analytical Chemistry, 8th ed., Saunders College
Publishing, 1997.
QD75.22.F86 2003
4. Mohan, Jag, Organic Analytical Chemistry: Theory and Practice,
Alpha Science International, Ltd, 2004
ISBN : 0849339529 / 9780849339523
5. Mohan, Jag, Organic Spectroscopy: Principles and Applications,
Alpha Science International, Ltd.
ISBN : 0849339529 / 9780849339523
27
APPENDICES
28
Mass
1 lbm = 0.453592 kg
1 ton = 2000 lbm
1 kg = 2.20462 lbm
Volume
1 ft3 = 0.028317 m3
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 105 m3/s
Force
1 lbf = 4.448222 N
1N = 0.224809 lbf = 1 kg.m/s2
Density
1kg /m3 = 0.062428 lbm/ ft3
Pressure
1 pascal (Pa) = 1 N/m2
1 atm = 760 mmHg = 760 torr
1 atm = 101.325 KPa
Table 1.0 Characteristic Infrared Absorption frequencies
Bond
C-H
Compound Type
Alkanes
CH3 Umbrella Deformation
C-H Alkenes
Aromatic Rings
C-H Phenyl Ring Substitution Bands
Phenyl Ring Substitution Overtones
C-H Alkynes
700-610(b) bend
C=C Alkenes
1680-1640(m,w)) stretch
CC Alkynes
2260-2100(w,sh) stretch
1260-1000(s) stretch
29
3640-3160(s,br) stretch
3600-3200(b) stretch
3000-2500(b) stretch
3500-3300(m) stretch
1650-1580 (m) bend
C-N Amines
1340-1020(m) stretch
CN Nitriles
2260-2220(v) stretch
30