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CHEMISTRY
Laboratory Guide
FIRST EDITION
2010
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 i
Experiment
REFERENCES 14
APPENDICES 15
PREFACE
This manual provides laboratory guidelines, safety declaration form, Chemistry Lab
Report guidelines and Laboratory manual for subject of Organic Analytical Chemistry
(CLB 10803).
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 quidelines 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 compilation of laboratory manual that will provide
student practical guidelines in Organic Analytical Chemistry.
There may be shortcomings which we had overlooked but hopefully these should not
hinder the process of enhancing laboratory skill.
General Guidelines
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.
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.
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.
Thank you.
Yours faithfully,
……………………………….
Name:
Matrix No:
Subject:
Date:
PART 2
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).
It should be written after conclusion of experiment OR project. Its cover briefly about
Introduction, Objectives, Methodology, Result & discussion, Conclusion
Objectives
Example:
Introduction
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
Procedure
Write the procedure in chronological order. Again, DO NOT COPY DIRECTLY from the lab
handout. Rearrange your procedure become a passive sentence.
Example:
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
parameter X (unit)
35
30
25
20
15
10
5
0
0 2 4 6 8 10 12
parameter 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 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 a 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 a
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
EXPERIMENT 1
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 HO CH2
O
R C O CH 2
O + 3 NaOH 3R C O Na +
R C O CH HO CH
Sodium salt of an acid (soap)
O
R C O CH 2
Fat HO CH2
glycerol
MATERIAL AND METHODS
Materials
Chemicals:
Apparatus:
Conical Flasks Hirsch / Buchner funnel
Beaker Watch glass
Filter funnel
METHODS
Preparation of Soap
1. Prepare a NaOH solution (about 0.25 g sodium hydroxide dissolved in a mixture of 1.0
ml of distilled water and 1.0 ml of 95% ethanol)..
2. Place about 0.25 g of fat in a 50 ml conical flask and add the prepared sodium hydroxide
solution to the flask.
3. Heat the mixture in a in a bath of 100 oC.
4. Cover the flask with some aluminum foil to help reduce evaporation. Swirl the
Erlenmeyer flask every few minutes. Use tong to do this.
5. The soap will precipitate from the boiling mixture within 20 minutes.
6. If you observe that some alcohol and water is evaporating from the flask, you may
add up to 0.4 ml of a 50 % water/alcohol mixture to replace the solvent.
7. Heat the mixture for a maximum time of 25 minutes.
8. Place 4 ml of NaCI solution in a 15 ml beaker and transfer the saponified mixture from
flask to beaker.
9. Stir the mixture while cooling the beaker in an ice-water bath.
10. Collect the prepared soap on a Hirsch funnel of ice cold distilled water to remove excess
NaOH.
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. Add 5 – 10 drops of 4% calcium chloride solution to the soap mixture from a Pasteur
pipette .Shake the mixture for 15 sec and allow it to stand for 30 seconds. Record your
observation on the effect of addition the calcium chloride.
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.
APPENDIX
1. Reaction of fat with NaOH will produced long chain carboxylic acid (soap) in form of
Bar. What would be happen if sodium Hydroxide (NaOH) is replaced by Potassium
hydroxide (KOH).
EXPERIMENT 2
OBJECTIVE
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.
A=εbc
b = pathlength (cm)
c = concentration (M or mol/L)
This relationship between absorbance, A and ε bc is known as Beer’s Law. Beer’s Law is
successful in describing the absorption behavior of dilute solutions only. At high
concentrations, absorbance of the solution does not obey Beer’s Law and is no longer
proportional to C.
In this experiment you are going to conduct two main applications which are wavelength
scanning and photometric scanning.
MATERIALS AND METHODS
Materials
Chemicals
100 ppm colorant stock (100 ml), Unknown (two), Distilled water
Apparatus
Perkin – Elmer UV/Vis Spectrophotometer Lambda EZ210, Sample cuvettes, path length 1
cm, Volumetric flask 50 ml (five) , Pipette 5 ml, 10 ml and 25 ml (one each),Rubber bulb
(three),Beaker 100 ml (one),Graduated cylinder 50 ml (one),Dropper (one),Labeling
sticker,Tissue paper
Methods
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 λmax .
2. What is the volume needed to prepare a 50 ppm of carmoisine from a 100 ppm of
carmoisine in 100 ml volumetric flask?
Objective :
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:
Isocratic HPLC system with UV detector, C18 column, Vacuum, Funnel, 0.45 µm filter paper
0.45 µm filter syringe,100 µL syringe,60 mL syringe,Volumetric flask
Chemicals
Caffeine 1000 ppm standard (stock solution), Methanol (HPLC grade), Double distilled water
(filtered with 0.45 µm filter paper), Soft drink sample
Methods:
3. After preparing the serial dilution and sample, your instructor will brief on standard
operating procedure of HPLC.
Analysis of data
1. Use standard benzoic acid /caffeine retention time to identify the benzoic
acid/caffeine peak and then record their retention time.
2. By using above information, clarify and justify the present of benzoic acid/caffeine in
the soda sample.
3. Record different concentration of standards peaks area and construct a standard
calibration curve (concentration vs peak area).
4. Measure the caffeine peak in the soda sample chromatograph, and use standard
calibration curve (concentration vs peak area) to determine the concentration of
Benzoic acid/ caffeine in the soda sample.
Note: All raw data must be record in table form.
1. Why does the syringe have to be carefully rinsed before each use?
2. Retention of caffeine in standards. How could you be identify a peak in the soda was
caffeine and not another substance by using retention time?
EXPERIMENT 4
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, R’COOR. Small chain side groups give very aromatic compound, while long –
chain side groups form waxy compounds.
Chemical:
Ethanol, Glacial acetic acid, Conc. sulfuric acid, 30% Sodium carbonate solution, Calcium
chloride, Granular anhydrous Calcium chloride, anti-bumping granules.
Apparatus:
Round bottom flask, Water condenser, retort stand, separating funnel
Methods
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.
Appendix
1. Reaction of acetic acid with ethanol to produce will produce ethyl ethanoate and water.
Based on that the reaction, how many grams of ethyl ethanoate would be produced if 50
ml of ethanol were react with 50 ml acetic acid? (given ethanol: 0.8 g/ml and acetic acid :
1.06 g/ml and ethyl acetate: 0.9g/ml). Calculate the percentage yield if 50.0 g of ethyl
ethanoate was obtained from the experiment.
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 105 m3/s
Pressure