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TITLE Soap Preparation STARTING EXPERIMENT : Friday, 9th March 2012 EXPERIMENT DONE : Friday, 9th March 2012

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PURPOSE After the experiment done, the students are expected to be able to a) Making procedure for soap preparation

b) Predicting the reaction of soap preparation c) Explaining the difference of soap preparation using NaOH base and KOH base d) Making soap emulsion e) f) Explaining the form of water-oil emulsion process Determining the oil quality based on its peroxide number.

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THEORY In chemistry, soap is a salt of a fatty acid. Soaps are mainly used as surfactants for washing, bathing, and cleaning, but they are also used in textile spinning and are important components of lubricants. Soaps for cleansing are obtained by treating vegetable or animal oils and fats with a strongly alkaline solution. Fats and oils are composed of triglycerides: three molecules of fatty acids attached to a single molecule of glycerol. The alkaline solution, often called lye, brings about a chemical reaction known as saponification. In saponification, the fats are first hydrolyzed into free fatty acids, which then combine with the alkali to form crude soap. Glycerol, often called glycerine, is liberated and is either left in or washed out and recovered as a useful by-product according to the process employed. Soaps are key components of most lubricating greases, which are usually emulsions of calcium soap or lithium soaps and mineral oil. These calcium- and lithium-based greases are widely used. Many other metallic soaps are also useful,

including those of aluminium, sodium, and mixtures of them. Such soaps are also used as thickeners to increase the viscosity of oils. In ancient times, lubricating greases were made by the addition of lime to olive oil. Soap is a type of surfactant, made from oil or natural fat that has bipolar structure. Head part is hydrophilic and tail part is hydrophobic. Because of this characteristic, soap can release dirt that is usually fat from our body and clothes, forms emulsion of oil in water. Soap can be made as saponification by using alkaline is a triglycerides reaction with alkaline (NaOH atau KOH) that produce soap and glycerine. C3H5(OOCR)3 + 3 NaOH -> C3H5(OH)3 + 3 NaOOCR Saponification produces soap as main product and glycerine as side product, that also has value. Soap with lower mass molecule will be more soluble and has harder structure. Soap has higher solubility in the water, but soap doesnt dissolve to smaller particles but in ionic form. Soap is generally known in two states, liquid and solid soap. Main difference from those two types is alkaline that is used in saponification. Solid soap uses NaOH, while liquid soap uses KOH. Types of oil that is used also influences state of soap. Palm oil will produce harder soap than peanut oil, soybean oil and cotton seed oil.

Fat/oil Oil/fat is a lipid that has ester from glycerol. Vegetable oil or animal fat is used. Difference between oil and fat is their state in room condition. Oil is in liquid state in room temperature ( 28C), while fat in solid state. They are triglyceride compounds. Triglyceride that is used as mateial of soap preparation has fatty acid chain length between 12 until 18. If it is less than 12 it will irritate skin, but if it is more than 18, soap will be hard and difficult to dissolve in water. Unsaturated fatty acid which is too much such as oleic acid, linoleic and others will cause soap is easy to oxidize in atmospheric condition so it will be rancid. Amount of oil or fat used in soap making process should be limited for various reasons, such as economic feasibility, product specifications (soap is not

easily oxidized, easy foaming, and easily soluble), and others. Several types of oils or fats commonly used in soap making process include: 1. Palm Oil (palm oil). Palm oil is commonly used instead of tallow. Palm oil can be obtained from oil palm fruit ripening. Palm oil is reddish orange in color because of carotenoid pigments, so if you want to use as a raw material for making soap should be paled first. Soap which is made from 100% palm oil will be hard and difficult foaming. Therefore, if used as raw material for soap, palm oil should be mixed with other ingredients. 2. Coconut Oil (coconut oil). Coconut oil is a vegetable oil that is often used in soap making industry. Coconut oil is pale yellow and flesh obtained by extraction of dried fruit (copra). Coconut oil has a high saturated fatty acid content, especially lauric acid, so coconut oil is resistant to oxidation leading to rancidity. Coconut oil also contains fatty acids caproic, caprylic, and capric. 3. Palm Kernel Oil (palm kernel oil). Palm kernel oil is from palm kernel. Palm kernel oils contain fatty acids that are similar to coconut oil so it can be used as a substitute for coconut oil. Palm kernel oils contain higher unsaturated fatty acids and lower short-chain fatty acids than coconut oil 4. Stearine Palm Oil (palm oil stearin). Palm oil stearin is the extraction of oil produced from fatty acids from palm oil with the solvent acetone and hexane. Fatty acid content of oil is the largest in stearin. 5. Marine Oil. Marine oil derived from marine mammals (whales) and sea fish. Marine oils have unsaturated fatty acid content is quite high, so it must be partially hydrogenated before use as raw material. 6. Castor Oil (castor oil). This oil is derived from jatropha seeds and used to make transparent soap. 7. Olive oil (olive oil). Extraction of olive oil comes from olives. High-quality olive oil has a yellowish color. Soap derived from olive oil has the properties of the firm but gentle to the skin. 8. Mixture of oils and fats. Industrial soap makers making soap is generally derived from a mixture of different oils and fats. Coconut oil is often mixed with tallow because it has a complementary nature. Coconut oil contains high

lauric and myristic acid and can make a soluble soaps and foaming. High stearate and palmitate of tallow soap will harden the structure.

Alkaline A common type of alkali used in the saponification process is NaOH, KOH, Na2CO3, NH4OH, and Ethanolamines. NaOH, or commonly known as caustic soda in the soap industry, is the most widely used in the manufacture of hard soap. KOH is widely used in the manufacture of liquid soap because it is easily soluble in water. Na2CO3 (soda ash / sodium carbonate) is an alkali which is cheap and can saponify fatty acids, but cant saponify triglycerides (oils or fats). Ethanolamine is an alcohol amine compound group. Compound can be used to make soap from fatty acids. The resulting soap is very easily soluble in water, easily foamed, and can reduce water hardness. Soap made from coconut oil and ethanolamine showed easy foaming properties but is more commonly used soap as soap and detergent industry, not as a household soap. Mixing of different alkali is often done by the soap industry with the aim to get the soap with certain advantages.

Supporting Materials The raw materials used to help support the process of perfecting the soap saponification (making soap and glycerin precipitation) until the soap into products ready for market. 1) NaCl. NaCl is a key component in the process of making soap. NaCl content in the finished product is very small due to a too high content of NaCl in the bar of soap can harden the structure. NaCl is used typically in the form of salt water (brine) or solids (crystals). NaCl is used to separate products and glycerin soaps. Glycerin did not experience precipitation in the brine due to the high solubility, while the soap will precipitate. NaCl must be free of iron, calcium, and magnesium in order to obtain a quality soap. 2) Additives. Additives are substances added to the soap that aims to enhance the quality of soap products that attract consumers. Additive materials include: Builders, inert fillers, anti-oxidants, dyes, and perfumes.

3) Alcohol 96% or it could be called Ethanol (ethyl alcohol), serves as a solvent in the process of making transparent soap since it is easily soluble in water and fat. 4) 96% alcohol function is to make transparent soap becomes clear / clear. Actually 70% Alcohol (isopropyl alcohol) can also be used, but the end result of using this soap produces a turbid/cloudy. 5) Olive Oil is the basis of natural soap making, making soap into a durable, soft and prevent dry skin. Olive oil contains vitamins, minerals and proteins that function to prevent the loss of skin's natural moisture. 6) Stearic Acid is used to make natural soap (optional) and transparent soap, soap function is to harden and stabilize the foam. 7) Glycerin is the product of the hydrolysis reaction between vegetable oil with water to produce fatty acids. Glycerin is a humectant so it can function as a moisturizer on the skin. Glycerin is a liquid crystal clear, odorless and has a sweet taste.

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DESIGN OF EXPERIMENT Tools and Materials 1. 2. 3. 4. 5. 6. 7. 8. 9. Balancer Beaker Glass Measuring Glass Stirrer Pipette Test tube Water Bath Palm Oil Coconut oil

10. Ethanol 11. Concentrated KOH solution 12. Concentrated NaOH solution 13. Glycerin 14. Olive Oil

15. Concentrated NaCl solution 16. Concentrated KCl solution Procedure of Soap Preparation 1.4 gram NaOH Dissolve in 3.3 mL of water Hot NaOH Solutio Waited until cool NaOH Solution

1 gram stearic acid Entered into 10 gram palm / coconut oil Mixture Heated until T = 70oC Cooled until T = 50oC Stirred Added by 4 gram glycerin Added by NaOH solution Added by 12 gram alcohol Heated and stirred until the solution become colorless Added 1 mL Olive Oil Poured into mould Soap

Procedure of Soap Emulsion 0.1-0.2 gram of Soap Soap solution

3 mL aquadest Added by 5 drops palm oil Added by 2 mL palm soap solution Shake Emulsion Waited until form 2 layers Not the time needed Time

3 mL aquadest Added by 5 drops palm oil Added by 2 mL coconut soap solution Shake Emulsion Waited until form 2 layers Not the time needed Time

3 mL aquadest Added by 5 drops coconut oil Added by 2 mL palm soap solution Shake Emulsion Waited until form 2 layers Not the time needed Time

3 mL aquadest Added by 5 drops coconut oil Added by 2 mL coconut soap solution Shake Emulsion Waited until form 2 layers Not the time needed Time

3 mL aquadest Added by 5 drops palm oil Shake Emulsion Waited until form 2 layers Not the time needed Time

3 mL aquadest Added by 5 drops coconut oil Shake Emulsion Waited until form 2 layers Not the time needed

Time

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DATA Treatment Result NaOH = white solid. The color of NaOH solution is colorless. The tube wall becomes hot. Hypothesis There is exothermic reaction: NaOH (s) + H2O (l) NaOH (aq) Conclusion The reaction between crystal NaOH and water is an exothermic. It releases heat, so the tube wall becomes hot.

1.4 gram NaOH Dissolved in 3.3 mL water 1.4 gram NaOH Waited until cold NaOH Solution

1 g stearic acid Entered into 10 gram palm oil Mixture Heated until T = 70oC Cooled until T = 50oC

Stearic Acid = solid white granule Palm Oil : Thick yellow solution The mixture of stearic acid and palm oil is yellow. After heated the stearic acid dissolves in palm oil. Glycerin :

The stearic acid dissolves in palm oil at T = 70oC Alcohol can dissolve the mixture of glycerol and soap. There is saponification reaction: CH2OCOR + NaOH RCOONa + CH2OH

The melting point of stearic acid is 70oC. Alcohol is emulgator of glycerine and soap mixture. The soap that is made from palm oil is hard.

Added by Colorless thick NaOH (++) solution After cooled the solution soap becomes Alcohol : hard. Stirred Colorless solution. Added by After added by 4 gram NaOH, glycerin, glycerin and alcohol the mixture is like a Added by gel. 12 gram After heated alcohol again, the mixture become solution Heated and the color is and clear yellow. stirred Olive Oil : Thick until the (+) yellow (++) solution solution become colorless After added by olive oil, the color Added 1 of solution mL olive becomes thick oil yellow (++). Poured into mould Soap The texture of soap is hard.

1 g stearic acid Entered into 10 gram coconut oil Mixture Heated until T = 70oC Cooled until T = 50oC

Coconut Oil : Thick white rather yellow solution The mixture of stearic acid and coconut oil is pale white. After heated the stearic acid dissolves in coconut oil. After added by NaOH, glycerin, and alcohol the mixture is like a

The stearic acid dissolves in palm oil at T = 70oC Alcohol can dissolve the mixture of glycerol and soap. There is saponification reaction: CH2OCOR + NaOH RCOONa + CH2OH

The melting point of stearic acid is 70oC. Alcohol is emulgator of glycerine and soap mixture. The soap that is made from palm oil is soft.

Added by gel. NaOH After heated solution again, the mixture become solution Stirred and the color is pale white Added by 4 gram After added by glycerin olive oil, the color of solution Added by becomes pale 12 gram yellow. alcohol The texture of Heated soap is soft. and stirred until the solution become colorless Added 1 mL olive oil Poured into mould Soap

After cooled the soap becomes soft.

Soap Solution : 0.1-0.2 gram of White turbid Soap Dissolved in 6-8 mL of water Soap solution

3 mL aquadest

Oil + Aquadest : can not mix well

Added by 5 drops After Shake : palm oil Appear bubble, the solution Added by become 2 mL homogeneous

Palm Soap can be as an emulsifying agent so, it can make oil-water mixture become homogeneous

Palm Soap is emulsifying agent.

palm soap solution Shake Emulsion Waited until form 2 Layers Note the time needed Time

Time to separate into two layers : 15 second

3 mL aquadest

Oil + Aquadest : can not mix well

Added by 5 drops After Shake : palm oil Appear bubble, the solution Added by become 2 mL homogeneous coconut soap Time to separate solution into two layers : Shake 40 second Emulsion Waited until form 2 Layers Note the time needed Time

Coconut Soap can be as an emulsifying agent so, it can make oil-water mixture become homogeneous

Coconut Soap is emulsifying agent

3 mL aquadest

Oil + Aquadest : Added by can not mix well 5 drops palm oil After Shake : The solution become Emulsion straight to be

Oil and Aquadest can not be emulsion because there is no emulsifying agent

Soap is emulsifying agent, the mixture of oil and water can not mixed perfectly

Waited until form 2 Layers Note the time needed Time

separate Time to separate into two layers : 2 second

3 mL aquadest

Oil + Aquadest : can not mix well

Added by 5 drops After Shake : coconut Appear bubble, oil the solution become Added by homogeneous 2 mL palm Time to separate soap into two layers : solution 20 second Shake Emulsion Waited until form 2 layers Note the time needed Time

Palm Soap can be as an emulsifying agent so, it can make oil-water mixture become homogeneous

Palm Soap is emulsifying agent.

3 mL aquadest

Oil + Aquadest : can not mix well

Added by 5 drops After Shake : coconut Appear bubble, oil the solution become Added by homogeneous 2 mL coconut Time to separate soap into two layers : solution 50 second

Coconut Soap can be as an emulsifying agent so, it can make oil-water mixture become homogeneous

Coconut Soap is emulsifying agent

Emulsion Shake Waited until form 2 Layers Note the time needed Time

3 mL aquadest

Oil + Aquadest : can not mix well

Added by 5 drops After Shake : The coconut solution is straight oil become separate Emulsion Waited until form 2 Layers Note the time needed Time Time to separate into two layers : 5 second

Oil and Aquadest can not be emulsion because there is no emulsifying agent

Soap is emulsifying agent, the mixture of oil and water can not mixed perfectly

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ANALYSIS The aim of the experiment is to understand the procedure of soap preparation that made from palm oil. The first done is making NaOH solution from 1.4 gram of solid NaOH dissolved in 3.3 mL aquadest in the reaction tube. The original form of NaOH is solid white, while the aqaudest is colorless aqueous. The result of this reaction is occurring hot temperature in the wall of the reaction tube. The solution is colorless. The hot temperature occurs because the reaction of NaOH and aquadest is exothermic reaction. It means that this reaction is releases heat. This NaOH solution is let until it cooled. The chemical reaction is written :

NaOH (s) + H2O (l) NaOH (aq) The next step is by mixing 1 gram of stearic acid with 10 gram palm oil. The original state of stearic acid is solid white granule, while the palm oil is thick clear yellow solution. The stearic acid is used to harden and stabilize the foam soap. Than, this mixture is heated in order the stearic acid will dissolve completely. The heating process is maintain in 70oC temperature to prevent the completely oxidation of oil that can make brown color. The result of this step is thick clear yellow solution, This is closely related to the peroxide value to determine the degrees of damage to the oil or fat caused by autooxidation. This mixture is let until the temperature decrease to 50oC. Then, it is added with NaOH solution that has been made, 4 gram Glycerin, and 12 gram of Alcohol. The original state of glycerin is thick (++) colorless solution, while the alcohol is colorless solution. Addition of NaOH solution is to neutralize the acid function as NaOH is alkaline. If the base point to use is NaOH, the resulting soap will manifest themselves hard, whereas if the base used is KOH, the resulting soap will manifest soft. Glycerine is a humectants that can be used as moisturizer for skin. While the function of alcohol is as solvent in transparently soap preparation because its

characteristic that easy to solve in both water and oil. In the other hand, alcohol here is used as emulgator. The mixture was formed gel and not became a unity. The mixture then heating and stirred until form clear yellow solution and dissolve completely. The next step is let this soap solution cooled to add the olive oil. The function of olive oil is as additive compound that can give aroma to the soap. The original state of olive oil is thick yellow (++) solution. The final result of this solution is thick yellow (+) solution that poured into mould. After a couple time, the soap is harder. The second experiments aimed is to understand the procedure of coconut oil soap preparation. The tool, material and the procedure is same with the palm oil soap preparation, and just changing palm oil into coconut oil. The original state of coconut oil is thick white rather yellow solution and become thick clear solution after mixed with staeric acid, NaOH, Glycerin, and Alcohol. The final result of this soap solution is yellow solution because of addition of olive oil. The smell of this solution is not good, and the soap produced is soft. Coconut oil has high quantity of saturated fatty acid so this oil is resistant to oxidation which can cause rancidity in oil. The overall reaction of soap preparation is:

Oil

Glycerin

Soap

The next experiments is to understand the emulsion characteristic of soap. The procedure is by mixing 3 mL aquadest with 5 drops of palm oil. This mixture is divided into three tubes. The first treatment is added by palm soap solution that makes from 0.1-0.2 gram of soap that has been made with 6-8 mL hot water, the second treatment is added by coconut soap solution, and the final treatment is added nothing. The mixture is shake strongly, and let to make separating layer while the time is recorded. The time recorded to palm soap treatment is 15 second, coconut soap is 40 second, and without soap treatment is 2 second. Then, the emulsion is changed into coconut oil with same treatment above. The time recorded for palm soap treatment is 20 second, coconut soap is 50 second, and without soap treatment is 5 second. This is shows that the soap that has been made can emulsifying the water and the oil, shown from the time for soap treatment is longer than without soap treatment. And, the coconut soap can emulsifying perfectly than palm soap, shown from the time for coconut soap treatment is longer than palm soap treatment in both emulsifying water with palm oil and water with coconut oil.

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CONCLUSION The soap preparation can be done by mixing a base with oil and added with alcohol as an emulgator. The result of palm oil soap is form hard soap while the result of coconut oil soap can not make hard soap. The soap that is made can emulsify the water and oil mixture The reaction of soap preparation is :

10. ANSWERING QUESTION 1) How to make the hard and soft soap? Hard Soap 1.4 gr NaOH Dissolve in 3.3 mL of water Hot NaOH Solution Let until cool NaOH Solution

1 gram Stearic Acid Added with 10 gram Palm Oil Mixture Heated and stir until the stearic acid dissolve completely Let until its temperature reach 50oC Stir Added with NaOH solution, stir Added with 4 gram Glycerin, stir Added with 12 gram Alcohol, stir Heated until form homogenous solution

Soap Solution Dried Hard Soap Soft Soap 1.4 gram KOH Dissolve in 3.3 mL of water Hot KOH Solution Let until cool KOH Solution

1 gram Stearic Acid Added with 10 gram Palm Oil Mixture Heated and stir until the stearic acid dissolve completely Let until its temperature reach 50oC Stir Added with KOH solution, stir Added with 4 gram Glycerin, stir Added with 12 gram Alcohol, stir Heated until form homogenous solution

Soap Solution Dried Hard Soap 2) Write the complete reaction of soap preparation! The reaction of soap preparation is:

3) How to make a soap emulsion? 0.1 - 0.2 gram soap that has been made Dissolve in 6-8 mL hot water Soap Solution

3 mL Water Added with 5 drops of oil

3 mL Water Added with 5 drops of oil Added with soap solution

Mixture Shaked strongly Let it for a while Oil separating layer 4) Explain the process of soap emulsion! Emulsion, in physical chemistry, mixture of two or more liquids in which one is present as droplets, of microscopic or ultramicroscopic size, distributed throughout the other. Emulsions are formed from the component liquids either spontaneously or, more often, by mechanical means, such as agitation, provided that the liquids that are mixed have no (or a very limited) mutual solubility. Emulsions are stabilized by agents that form films at the surface of the droplets (e.g., soap molecules) or that impart to them a mechanical stability (e.g., colloidal carbon or bentonite). Soaps are sodium or potassium fatty acids salts, produced from the hydrolysis of fats in a chemical reaction called saponification. Each soap molecule has a long hydrocarbon chain, sometimes called its 'tail', with a carboxylate 'head'. In water, the sodium or potassium ions float free, leaving a negatively-charged head. Soap is an excellent cleanser because of its ability to act as an emulsifying agent. An emulsifier is capable of dispersing one liquid into another immiscible liquid. This means that while oil (which attracts dirt) doesn't naturally mix with water, soap can suspend oil/dirt in such a way that it can be removed. The organic part of a natural soap is a negatively-charged, polar molecule. Its hydrophilic (water-loving) carboxylate group (-CO2) interacts with water molecules via ion-dipole interactions and hydrogen bonding. The hydrophobic (water-fearing) part of a soap molecule, its long, nonpolar

hydrocarbon chain, does not interact with water molecules. The hydrocarbon chains are attracted to each other by dispersion forces and cluster together, forming structures called micelles. In these micelles, the carboxylate groups form a negatively-charged spherical surface, with the hydrocarbon chains inside the sphere. Because they are negatively charged, soap micelles repel each other and remain dispersed in water. Grease and oil are nonpolar and insoluble in water. When soap and soiling oils are mixed, the nonpolar hydrocarbon portion of the micelles break up the nonpolar oil molecules. A different type of micelle then forms, with nonpolar soiling molecules in the center. Thus, grease and oil and the 'dirt' attached to them are caught inside the micelle and can be rinsed away.

5) Explain the difference between soap using NaOH and KOH as a base! Soaps are water-soluble sodium or potassium salts of fatty acids. Soaps are made of fats and oils, or their fatty acids, by treating them chemically with a strong alkali. These fatty acids are weak acids composed of two parts: A carboxylic acid group consisting of one hydrogen atom, two oxygen atoms, and one carbon atom, plus a hydrocarbon chain attached to the carboxylic acid group. The common alkalis used in soap making are sodium hydroxide also called caustic soda, and potassium hydroxide also called caustic potash. Saponification of fats and oils is the most widely used soap making process. This method involves heating fats and oils and reacting them with a liquid alkali to produce soap and water plus glycerine. When the alkali is sodium hydroxide, a sodium soap is formed. Sodium soaps are "hard soaps". When the alkali is potassium hydroxide, a potassium soap is formed. Potassium soaps are softer and are found in some liquid hand soaps and shaving creams.

11. REFERENCES

Anonym. 2012. Soap. en.wikipedia.org/Soap.htm (accessed at 13th March 2012)

Anonym. 2011. Komponen Pembuatan Sabun. www.sabuncair.com/2011/10/komponenpembuatan-sabun.html (accessed on 12th March 2012)

Helmenstine, Anne Marie. How Soap Cleans. http://chemistry.about.com/od/cleanerchemistry/a/how-soap-cleans.htm (accessed on Thursday, 15th March 2012 at 8.42 pm)

Rohman, Saepul. 2009. Bahan Pembuatan Sabun. http://majarimagazine.com/2009/07/bahan-pembuatan-sabun/ (accessed at 12th March 2012)

Spurlock, D. 2012. Synthesis of Soap Course Notes. http://homepages.ius.edu/Dspurloc/c122/soap.htm (accessed on Thursday, 15th March 2012 at 8.42 pm)

12. ATTACHMENT

Solid NaOH

NaOH Solution

Olive Oil

Glycerin

Mixture of Oil and NaOH after heating process

Palm Oil soap solution before adding Olive Oil

Coconut Oil soap solution before adding Olive Oil

Palm Oil soap solution after adding Olive Oil

Coconut Oil soap solution after adding Olive Oil