Final Synthesis and Environmental Impact of Soap and Detergents

Synthesis and Environmental Impact of Soap and Detergents

Minyoung Kim

Chemistry 102 Laboratory, Section 32

Instructor: Chris Underwood

February 26, 2007

Abstract

This lab report describes the experiment in which the differences

between soaps made out of fat and oil and detergents are tested and

compared to determine which of the soaps and detergents is the most

environmental-friendly and the most cleaning. Through froth, cleaning

and solubility tests and titrations, the olive oil soap was determined to

be what people in the mountain region should use. It is the most soluble

soap in water out of all that were tested, and it also had the best

cleaning ability.

My signature indicates that this document represents my own work.

Outside of shared data, the information, thoughts, and ideas are my own

except as indicated in the references.

______________________________________________

1

Introduction

This laboratory project was to develop a safer and milder soap making

process that is more environment-friendly. The government has charged

the group to be sent to a remote mountain region where people still use

traditional lye soaps. The soap was identified as a possible source of

pollution. Not only did the soap cause the development of rashes on the

local residents’ skins, but it also varied a lot in quality; the soap would

form some sort of scum instead of lathering. Before beginning the

experiment, vegetable oils and olive oil were expected to create more

environmental friendly soaps than the solid fats; because both olive and

vegetable oils are known to be better than the solid fats, Crisco and lard,

to human body. Also, in Korean butcher shops, used vegetable oils are

brought in to be made into soaps which could be used for dish or laundry

washing purpose. Soaps made out of used oils tend not to lather much,

but their cleaning ability is as great as the regular chemically made

soaps. Although, used-oil soaps also hold some problems; they do not

dissolve into water as well as the regular soaps do, but they dissolve

better than the used oils. Thus, for the environment, it is better to turn

used-oil into soaps and use them rather than just discarding used-oil.

The laboratory group will create four different types of soaps out of

Crisco, Lard, Olive Oil, and Vegetable Oil with detergents to conduct

solubility tests and titration.

2

Results

Table 1: Soap Froth Test

Most to Least Froth

1 Crisco

2 Lard

3 Olive Oil

4 Vegetable Oil

Table 2: Soap Cleaning Test

Best to Worst

1 Olive Oil

2 Vegetable Oil

3 Lard

4 Crisco

Table 3: pH Test

Soaps Basic

Detergents Acidic

Pond Water Basic

Table 4: Solubility Test for Detergent #1

Acetone Slightly Soluble

Ethanol Soluble

Toulene Slightly Soluble

1M Hydrochloric acid Not soluble

6M Sodium Hydroxide Not soluble

Water Slightly Soluble

Table 5: Solubility Test for Detergent #2

3

Acetone Slightly Soluble

Ethanol Soluble

Toulene Slightly Soluble

1M Hydrochloric acid Not soluble

6M Sodium Hydroxide Not soluble

Water Slightly Soluble

Table 6: Solubility Test for Soaps

Soap

Solvent

Olive Oil Vegetable

Oil

Crisco Lard

Acetone Not Soluble Not Soluble Not Soluble Not Soluble

Ethanol Not Soluble Not Soluble Not Soluble Not Soluble

Toulene Slightly

Soluble

Not Soluble Slightly

Soluble

Not Soluble

Water Slightly

Soluble

Not Soluble Not Soluble Not Soluble

4

Table 7: Solubility Test for Fats

Fat

Solvent

Olive Oil Vegetable

Oil

Crisco Lard

Acetone Soluble Not Soluble Soluble Not Soluble

Ethanol Not Soluble Not Soluble Slightly

Soluble

Slightly

Soluble

Toulene Soluble Soluble Not Soluble Not Soluble

Water Not Soluble Not Soluble Not Soluble Not Soluble

Table 8: Anion/Cation Test

Present ion in the sample

water

Indication

Chloride White precipitate

Calcium Red flame

5

Graph 1: Titration of Lard

Lard

0

2

4

6

8

10

12

1 11 21 31 41 51 61 71 81 91 101 111 121 131 141 151 161 171 181 191 201 211 221 231 241

Fluid Volume(mL)

pH

Run 1

Run 2

Run 3

Run 1: 0.64mLRun 2: 0.97mLRun 3: 0.2mL

Average: 0.60mLS: 0.39

M1*V1 = M2 *V2

M1 = (M2*V2)/V1

M1 = {(1)(0.6)}/(2)M1 = 0.3M

6

Graph 2: Titration of Olive Oil

Olive Oil

0

2

4

6

8

10

12

14

1 8 15 22 29 36 43 50 57 64 71 78 85 92 99 106 113 120 127 134 141 148 155 162 169 176 183 190 197 204 211 218

Fluid Volume (mL)

pH

Run 1

Run 2

Run 3


Average: 1.55mLS: .82

M1*V1 = M2 *V2

M1 = (M2*V2)/V1

M1 = {(1)(1.55)}/(2)M1 = 0.775M

7

Graph 3: Titration of Vegetable Oil

Veggie Oil

0

2

4

6

8

10

12

14

1 11 21 31 41 51 61 71 81 91 101 111 121 131 141 151 161 171 181 191 201 211 221 231 241 251 261 271 281 291 301

Fluid Volume (mL)

pH

Run 1

Run 2

Run 3



M1*V1 = M2*V2

M1 = (M2*V2)/V1

M1 = {(1)(0.91)}/(2)M1 = 0.455M

8

Graph 4: Titration of Crisco

Crisco

0

2

4

6

8

10

12

14

1 12 23 34 45 56 67 78 89 100 111 122 133 144 155 166 177 188 199 210 221 232 243 254 265 276 287 298 309 320

Fluid Volume(mL)

pH

Run 1

Run 2

Run 3



M1*V1 = M2*V2

M1 = (M2*V2)/V1

M1 = {(1)(0.25)}/(2)M1 = 0.125M

9

Graph 5: Titration of Pond Water

Titration of Pond Water

0

2

4

6

8

10

12

14

1 4 7 10 13 16 19 22 25 28 31 34 37 40 43 46 49 52 55 58 61 64 67 70 73

Fluid Volume (mL)

pH

pH vs Fluid Volume, Pond water 1 Run 1

pH vs Fluid Volume, Pond Water 2 Run 2

pH vs Fluid Volume, Pond Water 3 Run 3



M1*V1 = M2 *V2

M1 = (M2*V2)/V1

M1 = {(1)(.25)}/(2)M1 = 0.125M

10

Discussion

The tested fats were Crisco, Lard, Olive Oil, and Vegetable Oil. To

compare the difference between solid fats and liquid fats, the tested fats

solid vs. liquid ration was 1:1. Also, detergents were made to be

compared with soaps made out of fats mentioned above. As Table 1

shows, the solid fats produced more froth when shook. Table 2 shows

that oil fats generally cleaned better than solid fats. Solubility on

detergents #1 and #2 were tested the same (Table 4, 5). pH tests

(Table 3) indicated that both detergents and pond water were acidic

while soaps were tested to be basic. By conducting solubility tests on

soaps and fats, presented in Table 6, 7, it was clear that the properties

of fats were changed after going under the soap making synthesis. As

Table 6 and 7 shows, most fats were more soluble in the given solvents

than after they were turned into soaps. While conducting titration, a

mistake was made; instead of adding 2mL of the soap waste water to

198mL of water, whole beaker of waste water was titrated. The mistake

caused the titration to take much longer time than it should have. Other

group’s waste water had to be used instead, which created the

inconsistency of titration graphs 1 and 2. However, as the standard

deviations of each fat soap titration data (Graph 1, 2, 3, 4) shows, each

results were relatively close to each other. Also, each graph holds a

similarity with other graphs in its general shapes. 3 titrations of pond

water created the best result in consistency, giving only standard

deviation of 0.089. Pond water was identified to have calcium chloride in

it by the cation and anion tests. Not all the possible anion test was

conducted due to lack of time. Anion test for chloride reacted to give

white precipitate indicating the presence of chloride ion in the pond

water. Also, when put in the flame of a Bunsen burner, the water sample

gave a red flame indicating the presence of calcium ion in it (Table 8).

11

Calcium in water makes the water hard, which makes it harder for soaps

to lather in water. On the other hand, detergents lather whether it is in

hard or soft water. Hard water could be softened by putting lime in the

water or running water over an ion exchange resin (Helmenstine).

Detergents produced very harsh and dangerous exothermic reactions

while being created compared to the soaps. No harsh or dangerous

reactions were observed during the soap production. Also, it was proved

that the soaps were more environmentally friendly than the detergents,

because:

They were soluble in water;

Soaps are basic; when mixed with pond water, it neutralizes;

If detergents were mixed with pond water, the mixture would

become more acidic and harmful to human skin.

According to the data, Crisco had the lowest concentration (Graph 4),

its cleaning ability was the worst of the four (Table 2) and was not as

soluble in different solvents as shown in Table 6, although it shoed the

best lathering performance (Table 1). Thus, Crisco soap could not be

chosen to be the best soap. Lard was the next lowest in concentration

(Table 1). Also, it was one of the worst cleaning soaps (Table 2) and

was not soluble in water (Table 6). It was a competition between

vegetable oil and olive oil. Olive oil lathered and cleaned better than

vegetable oil (Table 1, 2), and its concentration was higher than that of

vegetable oil (Graph 2, 3). Lastly, the solubility was compared and olive

oil soap had better solubility than vegetable oil soap, which was tested

to be insoluble in all 4 of the given solvents (Table 6). Thus, hypothesis

was proven; soaps were better than detergents, and oil fat soaps were

better than the solid fat soaps.

Conclusion

12

According to the results from conducted solubility, froth, cleaning, and

solubility tests, it was determined that Olive Oil soaps should be used

instead of traditional lye soaps; the Olive Oil soap cleaned the best, was

relatively well lathering, was the most soluble in water, and had the

highest concentration rate out of all four types of soaps created. Also, it

was tested to be basic which would neutralize the pond water when

used; possibly protecting the remote mountain region people’s skin from

rashes. The remote mountain region people should not only use olive oil

to cook, but also use the left over or used olive oils to create better

soaps for them to use. If the people are worried that the soap might not

perform well because it does not lather well, they should know that it is

the soap mal-functioning; it is because of the hard water with calcium

they have in their area.

Experimental

Synthesis of the Soap

The group mixed 10g of fat(Crisco or Lard) or 10mL of oil(Olive oil

or Vegetable Oil) with 15mL of 6M sodium hydroxide with care,

added a small amount of glycerol and stirred the mixture with a

glass rod.

They brought up the solution to boil on heat for about 15-20

minutes until the solution became homogenous and thick paste.

Then, they added 50mL of saturated sodium chloride solution and

some ice to the cooled paste.

With a glass rod, the group mixed them vigorously so it would be

easier to filter the slurry.

After mixing, they used the suction filtration to filter the soap with

two 5mL portions of cold water.

13

They saved the waste water in a beaker and left the soap to air dry

a week.

Synthesis of the Detergent

A member of the group added 5mL of lauryl alcohol to 5mL of conc

sulfuric acid in a beaker with a great care while another member

added 3 drops of phenolphthalein to a beaker of 10mL 6M NaOH.

Then, they slowly combined two solutions together stirring

constantly until the pink solution turned clear.

They stirred the mixture for few more minutes on an ice bath

They filtered the solution to get the precipitated sodium lauryl

sulfate and dried the precipitate. They repeated the activity one

more time to create a second solution.

Solubility Tests

The group prepared a little bit of acetone, ethanol, toulene, 1M

hydrochloric acid, 6M sodium hydroxide and water in separate test

tubes.

To see the solubility of each soap and detergents they had

created, they took small amounts of dried soap (or detergents)

and mixed it with prepared liquids.

They covered the test tubes with cover films and shook them to

see the solubility of each solvent.

Titration

Using a Power Link interface, the group could record the difference in pH

as the fluid volume increased.

They had to set the drop counter above the hotplate/stirrer and

mount a burette 1cm above the rectangular hole in the drop

counter.

Then, the drop counter was connected to the Power Link interface.

14

Calibration

To calibrate, they put water into the burette, set a waste beaker

underneath the drop counter, and opened up to flush any air

bubbles there were.

After dispensing few mL of water, they closed the burette and

refilled it with more water.

After the set up was complete, they opened Data Studio in their

computer to start calibration while noticing their starting volume in

the burette.

They slowly opened the burette to avoid any liquid surges and

collected about 10mL of water in the waste beaker before noticing

the final volume to stop the flow of drops.

Using Data Studio, they read data from the sensor and the

calibration was complete.

Titration

A group member put 1M Hydrochloric Acid into the burette and

flushed any air bubbles there were while the other member put a

magnetic stirrer into a mixture of their soap waste water from the

week before and water. They used 2mL of soap waste water to mix

with water bringing the total volume of the solution to 200mL.

They put their titrant beaker on the hotplate/stirrer and turn the

stirrer onto medium speed.

Once the stirrer was set, they inserted the pH probe into one of

the round holes in the drop counter making sure that the sensor of

the pH probe is fully immersed in the solution and connected the

sensor to Power Link interface.

Then, they opened Data Studio to graph the pH vs. Fluid Volume of

the titration and started their titration.

15

On the graph, from the point where the base turns to acid, they

waited until the graph flattened out and stop the flow of acid to

finish their titration.

Anion/ Cation Test

Anion Test

Chloride

o A group member placed 1mL of the water sample in a test

tube and added 1mL of 6 M HNO3 and 1mL of AgNO3

solution.

The formation of a white precipitate (AgCl) indicated the

presence of chloride ion in the tested sample.

Cation Test

A group member put a clean nichrome wire in the flame of a

Bunsen burner to clean it.

Then, the wire was dipped into the water sample.

Dipped nichrome wire was put back into the flame to observe the

color in the flame, indicating the presence of a certain cation in

the water sample.

The group member referred to the table below (Cooper) to find

what the color present means.

Flame Coloration

Element Color Intensity

Barium Pale Green Low

Calcium Red Medium

Potassium Pale Violet Low

Sodium Brght Yellow High

Strontium Crimson Red Medium

Lithium Carmine Red Medium

Copper Blue-Green Medium

16

Magnesium None None

References

Cooper. Melanie M., Cooperative Chemistry Laboratories, McGraw-Hill

New York, NY, 2003, p 60-62.

Drop Counter Setup and Calibration. Melanie Cooper. Video images,

2006. <http://people.clemson.edu/~terry/Site/Podcast/B895F694

-C0B2-4B9D-9D40-F1A98E59523D.html>.

Power Link Introduction. Melanie Cooper. Video images, 2006.

<http://people.clemson.edu/~terry/Site/Podcast/D5C0F522-

629B-4E14-8E28-E4922F0D182E.htm>.

“Synthesis and Environmental Impact of Soap and Detergents.”

General Chemistry Laboratory Homepage. 2005. Clemson

University. 22 Jan. 2007 <http://chemed.clemson.edu/genchem

/labs.htm>.

Titration Using Probes Voice. Melanie Cooper. Video images, 2006.

<http://people.clemson.edu/~terry/Site/Podcast/35089BF7-9EF4-

4C5C-BFF0-AC67F93866F8.html>.

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Final Synthesis and Environmental Impact of Soap and Detergents

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