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FACULTY OF CHEMICAL ENGINEERING

NAME : SITI FATIMAH BINTI


NGAGIMAN
(2011683532)
GROUP : EH 221 2B (GROUP 6)
EXPERIMENT : SOAP AND DETERGENT
DATE PERFORMED: 25TH MAY 2012
SEMESTER : 02
PROGRAMME : FACULTY OF CHEMICAL
ENGINEERING AND PROCESS
NO TITTLES
(EH 221)
ALLOCATED MARKS
MARKS (%)
1. ABSTRACT 5
2. INTRODUCTIONS 5
3. AIMS 5
4. THEORY 5
5. APPARATUS 5
6. METHADOLOGY/ 10
PROCEDURES
7. RESULTS 10
8. CALCULATIONS 10
9. DISCUSSIONS 20
10. CONCLUSION 10
11. RECOMMENDATIONS 5
12. REFERENCES 5
13. APPENDIX 5
TOTAL MARKS 100
REMARKS:
CHECKED BY:

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DATE

ABSTRACT:
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The experiment which is to prepare the soap and detergent had


been conducted on 25th May 2012. Basically, the experiment used to
prepare the soap and thus, to compare the properties between the soap
that had been prepared early with the synthetic detergent in the form of
precipitation, emulsification and cleaning abilities. Based on the
experiment that had been conducted, it can be concluded that the soap
has the properties of emulsifying oil whereas the detergent has not. This
is because the soap has the abilities of forming precipitates and it can be
seen clearly in the soap solution while doing the experiment. Whereas the
detergent has not forms precipitates at all. Thus, the experiment is
completed and successfully conducted.
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INTRODUCTION:

Soaps and detergents are used frequently in our daily life. We use
them in many kinds of ways. We use them to wash our hands and clean
our clothes without ever really paying attention on how they work.
Beneath the plain white surface of a bar of Ivory soap lies an intrigung
history and a powerful chemistry.

Actually, it is hard to say when soap was first invented. Some


hypothesize believe that the soap had been invented by the Babylonian
in 2800 BC where soap have been excavated in clay cylinders and the
Phoenicians around 600 BC. By 1500 BC Egyptians medical scrolls
recommend a soap made from alkaline salt and animals and vegetables
oil for skin conditions. In the early history, soap was used for the purpose
of cleaning textile fibres such as wool and cotton in preparation for the
dyeing process instead of personal hygiene.

Later, the ancient Roman discovered the cleaning power of soap


accidently. At Mount Sapo, where it a place for the animals were
sacrificed, rain mixed animal fats, wood ashes and clay in to the soil.
Then, incidently, women washing their clothes by the stream found it was
much easier to wash their clothes with some of this clay mixture. Legend
links Mount sapo with the process of soap making saponification.
Interestingly, although Romans are famous for their baths, they actually
did not use soap to wash. But they coated themselves in oils and after
that used a scraping tool called a strigil to clean their bodies. However,
bars of soap were found in the ruins of Pompeii and the archeologists
believe soap was used for the laundry and occasionally on the body.
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Figure 1.

Soap making was an established craft in Europe by the 7th century


and soap making center flourished in France, Spain and also Italy. In the
New World, soap makers found work in Jamestown as early as 1608.
Besides, most of the early settlers made their own soap by boiling ashes
and animal fats. As world growth, the soap industry continued to grow
fairly steadily until the 20th century. While in 1916, there was a chemical
break through that promised to change the role of soap for years to come.
Thus, the Germans, suffering from a shortage of materials, resorted to
synthetic detergent. As a result, it was succesful and by 1946 laundry
detergent became available to the entire American population. In 1953,
sales of detergent surpassed those of soap.

Actually, soap and detergents are very similar in their chemical


properties which is same function used to wash and clean a dirt.
However, there is a significant difference between them where the soaps
are produced from the natural products while the detergents are synthetic
or man-made.

In todays progressive world of science and technology, soap is


manufactured much like it was back then where the fats and oils are
technically heated with the presence of strong base which commonly
used is sodium hydroxide or potassium hydroxide to produce fatty acid
salts and glycerol in a process termed as saponification process. As a
matter of fact, the salt of a fatty acid is the soap, which is a soft and waxy
material that brush up the ability for cleaning purpose of water. While
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processing of soap, a positive ion, usually Na + or K+ and a negative ion


usually the anions of long-chained carboxylic acids yielded by the
hydrolysis of either animals or vegetables fats.

Futhermore, the soap tends to decrease its melting point due to the
presence of double bond which known as unsaturated with fatty acids
materials. Thus, the compounds are in liquid form at room temperature.
Technically, the vegetable fats are relatively unsaturated and liquid under
the ordinary conditions, whereas animals fats are relatively more
saturated and solid or more-solid at the same temperature. Thus, double
bonds are said to lower the melting point of a fatty acid chain because its
cis-conformation chain by a Van der Waals attraction. Hence, a lower
temperature is required for these materials to form a solid crystal lattice.

If now we can see, there a variety of detergents can be found


today, which generally contain surfactants, a builder and other additives
such as bleaching agents and enzymes. The surfactants are the parts that
are responsible for the cleaning properties of that particular detergent.
Some of them may be cationic, ionic and non-ionic. The builders indeed
are compounds responsible for removing the corresponding calcium and
also the magnesium ions in hard water.

Furthermore, there are two detergents which may not be safe as it


may concern, mostly that contains phosphates. Such detergents will end
up in wastewater and cause excessive growth of algae and other aquatic
plants. When those die, bacteris that present in the dead matter consume
oxygen which then results in the lack of oxygen left for the fish and other
aquatics lives.
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AIMS AND OBJECTIVE:

For this experiment, we conducted to achieve the objective which


are to prepare a soap by using the mineral oils. Besides, the experiment
is conducted to study and compare the properties between the soap and
synthetic detergent in the form of precipitation, emulsification and also

cleaning abilities.
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THEORY:

Soap is a mixture of sodium salts of various naturally occuring fatty


acids. Air buubles added to a molten soap will decrease the density of the
soap thus it will float on the water. If the fatty acid salt has potassium
rather than a sodium, a softer lather is the result. This is because the bar
soap produced in the presence of sodium hydroxide while the liquid soap
is formed in the presence of potassium hydroxide.

Theorytically, the soap is produced by a saponification or basic


hydrolysis reaction of a fat or oil. Currently, sodium carbonate or sodium
hydroxide is used to neutralize the fatty acid and convert it to the salt.

In the other words, soap is a generic term for the sodium or


potassium salts of long-chain organic acid which is fatty acid that are
made from naturally occuring esters in animal fats and also the vegetable
oils. All organic acid contain the RCOOH functional group, where R is the
shorthen notation for the complex hydrocarbon which famously known as
alkyl group. The term for R is used because the group can be very large
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and for the addition for each chain has a litter effect for the chemical
reactivity. While for the ester it contain RCOOR functional group.

A soap is the sodium or potassium salt of a long chain fatty acid.


The fatty acid usually contain 12 to 18 carbon atoms which can be
expressed as term R. Solid soap usually consists of sodium salts of fatty
acids whereas liquid soaps usually are potassium salts of fatty acid.
Besides, the few examples of soaps are sodium fatty acid such as lauric
(vegetable oil), palmitic (palm oil), and stearic (animal fat).

Furthermore, the hydrocarbon chain in the soap may contain


saturated and unsaturated chains. Sodium salts are usually solid
therefore, most bars of soap are sodium salts. While potassium salts are
the basis of liquid soaps, shaving cream, and greases. Triglycerides is
formed by the combination of three molecules of fatty acid which are fats
and vegetable oils. Triglycerides included in the ester group which is
RCOOR which derived from three fatty acids. A triglyceride made from
three lauric acid molecules which shown as below:

General overall hydrolysis reaction:

Fat + NaOH glycerol + sodium salts/ fatty


acid
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Figure 2 - the hydrolysis of triglycerides

For the figure above, it formed by the saponification of a


triglyceride with the sodium hydroxide. Actually, saponification is a
process that produce soap usually from fats and lye. In the other words,
saponification involves base hydrolysis of triglycerides, which are esters
of fatty acid to produce a product which is sodium salt od a carboxylate.
Besides, saponification processes also produce glycerol.

The mechanism by which esters are cleaved by base involves


nucleophilic acyl substitution. Then the hydroxide anion, OH - adds to
attacks the carbonyl group of the ester. Then the intermediate product is
formed is orthoester.

Figure 3 - the mechanism of ester (1)

At this stage, the alkoxide is more basic than the conjugate base of
the carboxylic acid, and hence the proton is transfer rapidly and directly it
form a stabe carboxylic acid compound.

Figure 4 - the mechanism of ester (2)

After that, it continue by reaction between the RCOOH with the


alkoxide anion and then formed a product of carboxylic anion and a
alcohol. But with the presence of NaOH, the carboxylic acida are
converted to their sodium salts which is RCOO -Na+.
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The saponification of triglyceride produced 3 fatty acid which is


soap and the glycerol but the alkyl group in the triglyceride may or may
not have the same chain length which known as the number of carbons.

Figure 5 - the hydrolysis of triglycerides

Since the cleansing action of soaps depend upon the fact that they
ionize readily in water, how can you imagine if the ionic at the end
molecule is lost its charge. Thus, the soap would no longer clean and
emulsify the oil and dirt. But in facts, it would happen in hard and acidic
water. This is because the hard water contain metal cations such as Ca 2+
and Mg2+ that will react with the charged ends od the soaps and directly
form the insoluble salts.

As the conclusion, the synthetic detergent were developed to


overcome this kind of problems. Actually, the detergent has a similar to a
soaps in having an ionic and nonpolar end but it have a different structure
which have sulfonate end. The difference in polar groups is one of the key
distinctions between a soap and a synthetic detergent. The synthetic
detergent form micelles and cleanse in the same manner as soaps but if
it released into rivers and lakes it can cause explosive growth of algae.
Thus, it can cause decay of the aquatic ecosystem due to deoxygenation
from the decomposition of dead algae.
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A micelle is a spherical shape that is formed resulting from the


negatively charged heads on the soap molecules. They then orient
between them, where the non polar tails rearrange towards the centre of
the micelle and then the hydrophilic site facing the water. In the presence
of oil and dirt, the non-polar head interact with them and gathered it to
the centre of the micelle. Technically, this is how the soap works. When
rinsed with water, the micelle together qith the dirt washed away. Soap is
theoretically acting as an emulsifying agent, where emulsion is the
dispersion of a liquid in asecond immiscible liquid.

Figure 6 - the micelle of the soap

The structure below is a sodium lauryl sulfonate that contain in the


synthetic detergent. In facts the sulfonic acids are more stronger than
carboxylic acids, hence the synthetic detergent does not form any
precipitate in the acidic solution. Besides, in the hard water, the
detergent do not form insoluble salts compare with the soap. As a
conclusion, the synthetic detergents remain soluble in both acidic and
hard water.

Figure 7 - the structure for synthetic detergent


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REAGENTS:

1. Vegetable oil,
2. Ethanol
3. 6M sodium hydroxide
4. Saturated sodium chlorde
5. Synthetic detergent (dynamo)
6. CaCl2 solution
7. MgCl2 solution
8. FeCl2 solution
9. Mineral oils
10.1M hydrochloric acid
11.Tomato sauces.

APPARATUS:

1. Erlenmeyer flask
2. Measuring cylinder
3. Beakers
4. Magnetic stirrer
5. Glass rod
6. Retort stand and clamp
7. Vacuum filtration apparatus
8. Filter paper
9. pH meter
10.test tubes with racks
11.dropper
12.petri dish
13.cloth strips

PROCEDURES:

PART A: SOAP PREPARATIONS:

1. 12.5 ml of vegetable is placed in a 250 ml Erlenmeyer flask. 10mL


of ethanol and 12.5mL of 6M sodium hydroxide solution are added
to the flask. The mixture is stirred using a stirring bar to mix the
contents of the flask. The alcohol is carefully smelled by wafting it
towards our nose.
2. The 250 mL of flask is heated in a 600mL boiling water bath.
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Figure 8 - heating the mixture in the boiling water bath

3. The mixture is stirred continuously during the heating process to


prevent the mixture from foaming. If the mixture should foam to
the point of nearly overflowing, the flask is removed from the
boiling water until the foaming subsides, then the heating is
continued. The mixture is heated for 20-30 minutes or until the
alcohol odor is no longer detectable.

4. The paste like mixture is removed from the water bath and the
flask is cooled in a ice bath fro 10-15 minutes.

5. While the flask is cooling, the vacuum filtration apparatus is


assembled as shown in the figure below. The vacuum filtration
secured to a ring stand with a utility clamp to prevent the
apparatus from toppling over.
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Figure 9 - the vacuum filtration apparatus

6. A piece of filter paper is weighed to the nearest 0.001g and the


mass is recorded. The filter paper is placed inside the Buchner
funnel. The paper is moistered with water so that it fits flush in the
bottom of the funnel.
7. Once the flask has cooled, 150 mL of saturated sodium chloride
NaCl solution is added to the flask to salt out the soap.
8. The water at the aspirator is slowly turned on. The mixture from
the flask is poured into the Buchner funnel. Once all of the liquid
has filtered through the funnel, the soap was washed with 10 mL of
ice-cold water. The suction filtration is continued until all of the
water is removed from the soap.
9. The soap is removed from the funnel and pressed between two
paper towels to dry it. The filter paper and dried soap are weighed
and the mass is recorded to the nearest 0.001 g and the mass of
the soap determined by difference and then the mass is then
recorded.

PART B: COMPARISON OF SOAP AND DETERGENT PROPERTIES


(PRECIPITATION AND EMULSIFYING )

1. A stock soap solution is prepared by dissolving 2g of the prepared


soap in 100 mL of boiling distiiled water. The mixture is stirred until
the soap has dissolved and the solution is allowed to cool.
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2. Step 1 is repeated using 2 g of synthetic detergent. When both


solution are cool, the pH of each solution is determined using pH
meter.
3. Three test tubes are labelled as test 1, 2 and 3. 4 drops of minerals
oil are added to each test tube. 5 mL of distilled water is added to
test tube 1. 5 mL of stock solution is added to test 2 and 5 mL of
synthetic detergent is added to test tube 3.
4. Each solution is mixed by shaking and let stand for three to five
minutes. The solution, if any that emulsifies the oil by forming a
single layer is noted.
5. The mixtures are poured into the Waste Container. The three test
tubes are cleaned and dried.
6. Three more test tubes are labelled as test tube 1,2 and 3. 2mL of
stock solution is placed in each of the three test tubes. 2mL 1%
CaCl2 solution is added to test 1. 2mL of 1% MgCl2 solution is
added to test tube 2 while 2mL of 1% FeCl2 solution is added to
test tube 3. Each test tube is shaken to mix the solutions. The
observations are recorded.
7. 4 drops of mineral oils are added to each of the test tubes in step
6. Each test tube is shaken to mix the solutions and the solutions
are left to stand for three to five minutes. The solutions, if any, that
emulsifies the oil by forming a single layer is noted.
8. Step 6-7 is repeated using 2 mL of stock detergent solution. The
solutions that precipitated are observed.
9. The solution, if any, that emulsifies the oil by forming a single layer
is noted.
10.The mixtures are poured into the Waste Container. The test tube
are cleaned and dried.
11.5 mL of stock soap solution is poured in cine clean test tube and 5
mL of stock detergent solution in a second test tube. 1M HCl is
added one drop at a time to both solution until the pH in each tube
is equal to 3. The number of drops of acid added to each mixture is
counted. Any precipitate formed in either mixture is observed.
12.1 drop of mineral oil is added to each test tube in step 11. Each
test tube is shaken to mix the solution. Any emulsification formed
in either mixture is observed.
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PART C: COMPARISON OF CLEANING ABILITIES OF SOAP AND


DETERGENT.

1. The three beakers are cleaned, dried and labeled. Then 20 mL of


stock soap solution that from step 1 is placed in the first beaker.
After that, 20 mL of stock detergent solution from step 2 is placed
in the second beaker. 20 mL of tap water is added in a third beaker.
2. Three cloth test strips that have been soaked in tomato souce are
obtained and then one strip is placed in each of the beakers.
Repeatedly, each solution is stirred with a stirrer bar for 5 minutes.
3. The cloth strips is removed from the soap and detergent solution
and then the excess water is squeezed out. Each cloth strip is
observed and compared to determine their relative cleanliness.

RESULTS:

PART A : SOAP PREPARATION.

Mass of filter paper 0.4692 g

Mass of petri dish + filter paper 2.0632 g

Mass of petri dish +filter paper + 51.2267 g


soap

Mass of soap recovered 49.1635 g

PART B : COMPARISON OF SOAP AND DETERGENT


PROPERTIES.
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Test (1) : The comparison of the pH value of soap and


detergent.

Name of the Soap prepared Dynamo


sample
Mass 2.0808 g 2.0810 g

pH value 10.086 8.050

Conclusion: The soap that had been prepared is more basic that
the detergent because the pH value of soap is more than the
detergent

Based on the result above, between soap and detergent, the pH


value of detergent is 8.050 while the soap is 10.086. Thus, the
soap prepared is more basic compare to the detergent.

Test (2) : The comparison of emulsification of soap and


detergent.

Test 1 Test 2
Test 3

Name Test 1 Test 2 Test 3


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Sample Distilled water Stock soap Stock detergent

Test 4 drops mineral 4 drops mineral 4drops mineral


oils + 5 mL oils + 5 mL stock oils + 5 mL
distilled water soap synthetic
detergent

Observation The solution form The solution The solution is


2 layer with water become milky and pale blue in color
at the bottom not form any and form 2 layer
while oil at the layer. with the oil at
upper part the upper part

Emulsificati No Yes No
on

Emulsification can be described as the solution that form is in a


single layer. Thus, based on the test above, the emulsification had
occured in the stock soap solution which is form milky in solution.
While the distilled water and stock detergent do not occur any
emulsification because there are oil layer at the upper part of the
solution for both samples.

Test (3) : The comparison of properties of soap and detergent


in hard solution.
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The solution of soap with 1) FeCl2, 2) MgCl2 and 3) CaCl2.

System Precipitate Oil emulsified


Soap Synthetic Soap Synthetic
detergent detergent

2 mL CaCl2 Colourless No Yes Form single


+ 4 drops with white layer
mineral oils precipitate

2 mL MgCl2 Milky and No Yes Form 2


+ 4 drops have a layers and
mineral oils white the oil at the
precipitate upper part

2 mL FeCl2 + Orange in No Yes Form single


4 drops solution layer
mineral oils and have
orange
precipitate

Based on the test above, the soap have the precipitate of


properties if compare with the synthetic detergent that does not
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formed any precipitate although react with either CaCl2, MgCl2 nor
FeCl2.
From the result above, we can observe that when soap mixed with
CaCl2, the soap solution change to colourless with the present of
white precipitate while the synthetic detergent change color into
light blue and does not have oil emulsified.
When mixed with MgCl2, the soap become milky solution and also
presence the white precipitate while the synthetic detergent only
change in very light blue color and consist of oil emulsification in
the form of 2 layers.
Lastly, the soap change into orange color in solution with the
presence of orange precipitate while compare to the synthetic
detergent it only change into yellowish color and does not form any
precipitate and also oil emulsified.

Test (4) : The comparison of soap and detergent in acidic


solution by using 1M HCl

Sample Soap Synthetic detergent


Initial pH 8.821 5.860

Final pH 3.010 3.015

Drops of 1M HCl 28 drops 16 drops

Observations The solution become The solution is clear and


milky while droping not form any precipitate
the HCl solution.

Add the mineral oil for both samples

Observations Form white Not change


precipitate

For the test in the acidic solution we can observe that the soap has
a high value of pH reading compare with the synthetic detergent
and the soap formed the precipitate when react with the acid and
not for the synthetic detergent.
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Test (5) : Cleaning comparison of a soap and detergent

The cleaning ability by 1) tap water, 2) synthetic detergent and


3) soap

Samples Tap water Synthetic Soap


detergent
Cleanliness Not clean Very clean Slightly clean

Observation No effect the Not effect the The solution


solution solution seen have a
precipitate

For the test above, it more concentrate to determine the relative


cleanliness for the tap water, synthetic detergent and soap.
Based on experiment conducted, the synthetic detergent shown
the high relative cleaanliness compare with the soap and the tap
water.
The relative cleanliness can be conclude as:
tap water < soap < synthetic detergent
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DISCUSSION:

In the saponification process, the fatty acid carboxylate ions are


formed in the presence of the strong base which is used sodium
hydroxide, NaOH for this experiment. Then, these carboxylate ions are
the conjugate bases of the fatty acids therefore, it is able to accept a
proton to formed the stable compound. When it placed into water, these
conjugate bases are able to accept the proton from any souces including
the water.

For the hard water, it can be known as the water that consist of
calcium ion, Ca2+ and magnesium ions, Mg2+. These ions are leached from
the ground water flowing over rock formations containing limestone and
also other minerals. Thus, the hard water interferes with the cleaning
action of soap. That why when the soap is react with the mineral ions that
contain in the hard water, it will formed the precipitate. So that, the
precipitate leaves a deposit on clothes, skin and hair.

The synthetic detergents have undeniably replaced soap for many


cleaning jobs around the home. Thus, the development of synthetic
detergent by chemist actually was a great advantage for people with
relatively hard tap water in their homes.

However, although the synthetic detergent have the advantages


compare to the soap, but there is a significant issue regarding the use of
synthetic detergent that is the biodegradability of some of its
components. In fact, many of the surfactants initially used in detergents
were not biodegradable whereas soaps are biodegradable, apparently can
be degraded by bacteria.

From the observations obtained from the experiement, the soap


form the precipitate in all of the solutions added which are CaCl2, MgCl2
and FeCl2 as well emulsifies the oil. So that, this may not appear as a
good characteristics for the soap as the cleaning agent if there formed
precipitate and emulsifies oil on the cloth.

Furthemore, compare to the detergent, it is a better cleaning agent


because it not formed any precipitate while react with the mineral that
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may be contains in the hard water. Besides, this is because the detergent
can cleaned without involving any precipitate or oil emulsification.

CONCLUSION:

Followed by the objectives of the experiment which are to prepared


the soap and used to compare the properties of soap and detergent
which are precipitation, emulsification and cleaning abilities. thus, the
soap is succesfully prepared and all the comparison of properties had
been observed and recorded.

For the test 1 which is to compare the pH value of soap prepared


with the detergent. The soap has a high value of pH reading if compare
with the detergent which the reading recorded is 10. 086 while the pH
value for detergent that had been recorded is 8.050. Thus, it can be
concluded that the soap is more alkaline than the detergent.

Next for the second test, which is to compare the oil emulsification
for the 3 kinds of samples which are distilled water, soap solution and
also synthetic detergent. From the observations, the distilled water and
the synthetic detergent do not emulsified the oil while the soap
emulsified the oil which formed the solution milky. Thus, this can be
concluded that the soap is not the good cleaning agent which has the
properties of emulsification of oil.

In addition, for the test 3 and 4 which are to compare the soap and
detergent in the formed of precipitation and emulsification in the hard
and acidic solution. From the experiment conducted, it can be concluded
that the soap has the properties of emulsifying oil whereas the detergent
has not. Besides, the soap solution seen clearly can be observed formed
the precipitate when react with the hard water and also the acidic
solution whereas the detergent does not form any precipitate in all tests
that had been conducted in the experiment.

For the lastly test which is cleaning abilities between 3 types of


samples which are tap water, soap and detergent. From the result and
figure above, we can make a conclusion that the synthetic detergent is
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the most good of cleaning agent compare to the tap water and soap
which do not clean the cloth strips that contain tomato sources cleanly.

RECOMMENDATIONS:

There are a few recommendations that will significantly produce


better observations which will not deviate much from the theoretical
observations.

Firstly, the experiment should be repeated twice in order to get


more accurate observations. This is because if the experiments are
conducted twice, thus the observations might be more convincing when
the average is taken.

The most important, use a safety equipment and avoid contact


with any chemical reagents involved. If there a contact with the chemical,
directly wash the hands and dont forget to wash hand agains before
leaving the laboratory.

While doing the experiment, focus and recorded any change of the
solution and for the color change prepared the white paper as the
background. Thus, the color change can be observed clearly and then it
must be recorded.
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REFERENCES:

1. Experiment in General Chemistry Featuring Measuring Net, Bobby


Shanton, Lin Zhu, C.H.Atwood, 2005, Brooks/Cole Laboratory
Series,USA.
2. Organic Chemistry(third editions), R.T.Morrison & R.N.Boyd,1973,
Allyn and Bacon,Boston.
3. Fundamentals of General, Organic and Biological Chemistry (third
edition), J.McMurry, M.E. Castellion,1999.Prentice Hall,Inc.Upper
Saddle Rier,New Jersey.

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