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Scientific Soapmaking

Kevin M. Dunn

Summer 2010

$Revision: 1.1 $

Acknowledgements
Copyright 2010 Kevin M. Dunn

Acknowledgements

Mike Lawson/Columbus Foods

Scientific Soapmakers

Why Teach Soapmaking?

Why Teach Soapmaking?

Thriving cottage industry

Why Teach Soapmaking?

Why Teach Soapmaking?

Thriving cottage industry

Soapmakers generally come from a cooking/craft background

Why Teach Soapmaking?

Why Teach Soapmaking?

Thriving cottage industry

Soapmakers generally come from a cooking/craft background

Soapmakers are interested in the chemistry of their craft

Why Teach Soapmaking?

Why Teach Soapmaking?

Thriving cottage industry

Soapmakers generally come from a cooking/craft background

Soapmakers are interested in the chemistry of their craft

If gen-ed students can imagine themselves as soapmakers, they


will become interested in the chemistry

Why Teach Soapmaking?

Why Teach Soapmaking?

Thriving cottage industry

Soapmakers generally come from a cooking/craft background

Soapmakers are interested in the chemistry of their craft

If gen-ed students can imagine themselves as soapmakers, they


will become interested in the chemistry

Experiments are designed to solve real-world problems

Lets Make Soap

Lets Make Soap

1000 g Delight (an oil blend)

288 g Lye (500 ppt NaOH)

Lets Make Soap

Lets Make Soap

1000 g Delight (an oil blend)

288 g Lye (500 ppt NaOH)

But how are we to weigh?

Weighing Synthetically

Weighing Synthetically

Place bottle of lye on balance

Press tare button

Use cup to transfer lye to jug of oil

What if we overshoot?

What about the lye in the cup?

Lets Make Soap

Lets Make Soap

1000 g Delight (already weighed)

288 g Lye (weigh synthetically into oil)

Lets Make Soap

Lets Make Soap

1000 g Delight (already weighed)

288 g Lye (weigh synthetically into oil)

Shake vigorously for 60 seconds

Pour into styrofoam cups

Measure temperature

Oil and Water

Oil and Water

Glyceryl Trilaurate

Glyceryl Trilaurate

O
O

O
O

O
O

Saponification

Saponification

Saponification

Saponification
O

NaOH
O

NaOH

NaOH

Na

O
OH

OH
O

OH

Na

O
Na

O
O

Saponification

Saponification

Oil + 3 NaOH = Glycerol + 3 Soap

Each molecule of oil requires 3 molecules of NaOH

Saponification

Saponification

Oil + 3 NaOH = Glycerol + 3 Soap

Each molecule of oil requires 3 molecules of NaOH

What happens if you provide only 2 molecules of NaOH?

Saponification

Saponification

Oil + 3 NaOH = Glycerol + 3 Soap

Each molecule of oil requires 3 molecules of NaOH

What happens if you provide only 2 molecules of NaOH?

What happens if you provide 4 molecules of NaOH?

Saponification

Saponification

Oil + 3 NaOH = Glycerol + 3 Soap

Each molecule of oil requires 3 molecules of NaOH

What happens if you provide only 2 molecules of NaOH?

What happens if you provide 4 molecules of NaOH?

We measure oil and NaOH by weight, not by molecules

Saponification

Saponification

Oil + 3 NaOH = Glycerol + 3 Soap

Each molecule of oil requires 3 molecules of NaOH

What happens if you provide only 2 molecules of NaOH?

What happens if you provide 4 molecules of NaOH?

We measure oil and NaOH by weight, not by molecules

Each gram of oil should require a specific weight of NaOH for


complete saponification

Saponification Value

Saponification Value
Theoretical saponification value of glyceryl tristearate:
1 mol oil
? g KOH = 1000 g oil
890 g oil
= 189 ppt KOH

3 mol KOH
1 mol oil

56 g KOH
1 mol KOH

Experimental saponification value of tallow: 190-200 ppt

Saponification Value

Saponification Value
Theoretical sodium saponification value of glyceryl tristearate:
1 mol oil
? g NaOH = 1000 g oil
890 g oil
= 135 ppt NaOH

3 mol NaOH
1 mol oil

40 g NaOH
1 mol NaOH

Experimental sodium saponification value of tallow: 135-143 ppt

Saponification Value

Saponification Value
SV

= weight (mg) of KOH needed to saponify 1 g of oil

SSV
AR

= weight (mg) of NaOH needed to saponify 1 g of oil

= weight (mg) of alkali actually used to saponify 1 g of oil

Saponification Value

Saponification Value
SV

= weight (mg) of KOH needed to saponify 1 g of oil

SSV

= weight (mg) of NaOH needed to saponify 1 g of oil

AR

= weight (mg) of alkali actually used to saponify 1 g of oil

SV

of Delight is 211.5 ppt KOH

SSV

of Delight is 150.8 ppt NaOH

Saponification Value

Saponification Value
SV

= weight (mg) of KOH needed to saponify 1 g of oil

SSV

= weight (mg) of NaOH needed to saponify 1 g of oil

AR

= weight (mg) of alkali actually used to saponify 1 g of oil

SV

of Delight is 211.5 ppt KOH

SSV

of Delight is 150.8 ppt NaOH

Since Lye is 500 ppt NaOH, we have used an AR of 144 ppt


NaOH

Why?

Lye Discounting

Lye Discounting
11 Weeks Old

6
4
2
0
140

144

148

152

AR / ppt NaOH

156

TA / ppt NaOH

TA / ppt NaOH

1 Day Old
6
4
2
0
140

144

148

152

AR / ppt NaOH

156

Checking In

Checking In
What are the temperature and consistency of your soap?

Measurable quantities

Measurable Quantities

Finished soap
Total alkali
Moisture content
Hardness

Measurable quantities

Measurable Quantities

Finished soap
Total alkali
Moisture content
Hardness

Raw materials
Saponification value
Lye concentration
Free fatty acid

Free Fatty Acid

Free Fatty Acid

Real-world oils may contain free fatty acid

How can we measure it?

Titration

Titration

Titration

Titration

Add 50 mL ethanol to Erlenmeyer flask

Add 4-5 drops 1% phenolphthalein

Add 4.18 ppt KOH until solution is faintly pink

Solution is now neutral

Weighing Analytically

Weighing Analytically

Place coconut oil bottle on balance

Press tare button

Transfer 30-40 drops of oil to Erlenmeyer flask

Replace oil bottle on balance and read weight

Gravimetric Titration

Gravimetric Titration

Place 4.18 ppt KOH bottle on balance

Press tare button

Add KOH to Erlenmeyer flask until faintly pink

Replace KOH bottle on balance and read weight

Acid Value

Acid Value
YY.YY g standard
? g KOH = 1000 g oil
1.XX g oil

YY.YY
4.ZZ ppt KOH
AV =
1.XX

What is the Acid Value of your oil?

4.ZZ g KOH
1000 g standard

Acid Value

Acid Value
YY.YY g standard
? g KOH = 1000 g oil
1.XX g oil

YY.YY
4.ZZ ppt KOH
AV =
1.XX

What is the Acid Value of your oil?

Why did we get different values?

4.ZZ g KOH
1000 g standard

Free Fatty Acid

Free Fatty Acid

Free Lauric Acid = 3.570 AV

What is the Free Lauric Acid content of your oil?

Free Fatty Acid

Free Fatty Acid

Free Lauric Acid = 3.570 AV

What is the Free Lauric Acid content of your oil?

Which oil would saponify quicker?

Extended Investigations

Extended Investigations

Dreaded Orange Spots

Extended Investigations

Extended Investigations

Dreaded Orange Spots

Seizing

Extended Investigations

Extended Investigations

Dreaded Orange Spots

Seizing

Superfatting vs Discounting

Extended Investigations

Extended Investigations

Dreaded Orange Spots

Seizing

Superfatting vs Discounting

The Water Discount

Lye Concentration

Lye Concentration

What is the normal, correct, or standard lye concentration?

Lye Concentration

Lye Concentration

What is the normal, correct, or standard lye concentration?

Ann Bramson, Soap: Making it, Enjoying it (1972)


25-27%, 26% average

Lye Concentration

Lye Concentration

What is the normal, correct, or standard lye concentration?

Ann Bramson, Soap: Making it, Enjoying it (1972)


25-27%, 26% average

Susan Cavitch, The Soapmakers Companion (1997)


26-29%, 27% average

Lye Concentration

Lye Concentration

What is the normal, correct, or standard lye concentration?

Ann Bramson, Soap: Making it, Enjoying it (1972)


25-27%, 26% average

Susan Cavitch, The Soapmakers Companion (1997)


26-29%, 27% average

Robert McDaniel, Essentially Soap (2000)


33-38%, 34% average

Lye Concentration

Lye Concentration

What is the normal, correct, or standard lye concentration?

Ann Bramson, Soap: Making it, Enjoying it (1972)


25-27%, 26% average

Susan Cavitch, The Soapmakers Companion (1997)


26-29%, 27% average

Robert McDaniel, Essentially Soap (2000)


33-38%, 34% average

Anne Watson, Smart Soapmaking (2007)


30-37%, 33% average

The Soap Formula

The Soap Formula

Lye = 50.00% NaOH, 50.00% distilled water

Coconut1000Lye348
Coconut1000Lye348Aq174
Coconut1000Lye348Aq348

The Soap Formula

The Soap Formula

Lye = 50.00% NaOH, 50.00% distilled water

Coconut1000Lye348 (50.00% NaOH Low-Water)


Coconut1000Lye348Aq174 (33.33% NaOH Medium-Water)
Coconut1000Lye348Aq348 (25.00% NaOH High-Water)

Processing Soap

Processing Soap

100 g oil + water + lye into 500 mL plastic bottle

Shaken 15 sec on a paint shaker

Gently swirled until trace

Poured into an Upland experimental mold

Incubated at 140F for 4 hours

Questions

Questions

What do we want to know?

Questions

Questions

What do we want to know?

Does the initial water portion affect the final moisture content?

Does it affect the curing time?

Does it effect the hardness of the soap?

Is there a danger of separation?

What Can We Measure?

What Can We Measure?

Moisture content of soap over time

Hardness of soap over time

Alkalinity of soap over time

Separation of soap

What Can We Measure?

What Can We Measure?

Moisture content of soap over time


Initially from formula, follow weight loss over time

Hardness of soap over time

Alkalinity of soap over time

Separation of soap

What Can We Measure?

What Can We Measure?

Moisture content of soap over time


Initially from formula, follow weight loss over time

Hardness of soap over time


Soil penetrometer

Alkalinity of soap over time

Separation of soap

What Can We Measure?

What Can We Measure?

Moisture content of soap over time


Initially from formula, follow weight loss over time

Hardness of soap over time


Soil penetrometer

Alkalinity of soap over time


Titration with 5 ppt citric acid

Separation of soap

What Can We Measure?

What Can We Measure?

Moisture content of soap over time


Initially from formula, follow weight loss over time

Hardness of soap over time


Soil penetrometer

Alkalinity of soap over time


Titration with 5 ppt citric acid

Separation of soap
Hardness of top and bottom of bar
Alkalinity of top and bottom of bar

Moisture

Moisture

Coconut1000Lye348Aq348

Total weight 1696 g

Water weight (174 + 348) = 522 g

Initial moisture = (522/1696) = 0.308 = 30.8% = 308 ppt

Moisture

Moisture

Coconut1000Lye348Aq348

Total weight 1696 g

Water weight (174 + 348) = 522 g

Initial moisture = (522/1696) = 0.308 = 30.8% = 308 ppt

Initial bar weight 141.32 g; Final weight 113.17 g

Weight loss (28.15/141.32) = 0.199 = 19.9% = 199 ppt

Final moisture = 308 - 199 = 109 ppt

Penetrometer

Penetrometer

Smaller foot used for hard soaps.

Titration

Titration

How many grams of acid required to titrate a given weight of


soap?

Total Alkali

Total Alkali
Y.YY g acid
5 g H3Cit
? g NaOH = 1000 g soap
1.XX
g soap 1000 g acid

3 mol NaOH 40.00 g NaOH


1 mol H3Cit
192.12
1 mol NaOH
g H3Cit 1 mol H3Cit
Y.YY
TA = 3.123
ppt NaOH
1.XX

Palm Oil

Palm Oil

Low, Medium, and High Water soaps

Identical in other respects

Moisture and hardness measured weekly for 60 days

Alkalinity measured at beginning and end

Palm Oil

Palm Oil
Batch Code
KMD2007.12.27
A Palm1000 Lye286
B Palm1000 Lye286Aq143
C Palm1000 Lye286Aq286

111
200
273

Moisture
A
B
C

200

30
Days

Alkali (ppt NaOH)


Initial
Final
Top Bottom Top Bottom
1.8
4.9 0.3
0.9
1.8
1.4 -1.7
-0.2
0.5
0.3 -1.7
-0.1
Hardness

10

100
0

54
60
74

kg/scm

300
ppt

Moisture (ppt)
Initial Final

60

5
0

30
Days

60

Coconut Oil

Coconut Oil
Batch Code
KMD2008.1.8

Moisture (ppt)
Initial Final

D Coconut1000Lye348
E Coconut1000Lye348 Aq174
F Coconut1000Lye348 Aq348
Moisture
D
E
F

200

Hardness
10

100
0

30
Days

41
88
109

kg/scm

300
ppt

129
229
308

Alkali (ppt NaOH)


Initial
Final
Top Bottom Top Bottom
0.4
0.5 -0.6
-0.3
-0.1
-0.2 -1.7
-1.0
0.1
0.2 -1.8
-0.4

60

5
0

30
Days

60

Olive Oil

Olive Oil

Medium and high water soaps separated

What can I do to accelerate trace?

Olive Oil

Olive Oil

Medium and high water soaps separated.

What can I do to accelerate trace? Add clove oil.

Olive Oil

Olive Oil
Batch Code
KMD2008
Olive1000Lye264
Olive990 Clove10 Lye259
Olive990 Clove10 Lye259 Aq130
Olive990 Clove10 Lye260 Aq260
Moisture
1.7A
3.5A
3.5B
3.5C

300
ppt

104
103
187
256

200

30
Days

Alkali (ppt NaOH)


Initial
Final
Top Bottom Top Bottom
0.3
0.2 -3.2
-0.4
-0.4
-0.7 -0.7
-0.7
-0.4
-0.4 -0.8
-0.7
-0.7
6.2 -1.1
-0.2
Hardness

10

100
0

36
43
61
67

kg/scm

1.7A
3.5A
3.5B
3.5C

Moisture (ppt)
Initial Final

60

5
0

30
Days

60

Delight

Delight

Delight = Olive390Palm280Coconut280Castor50

Delight

Delight
Batch Code
KMD2008.2.17

Moisture (ppt)
Initial Final

A Delight1000Lye288
B Delight1000Lye288 Aq144
C Delight1000Lye288 Aq288

112
201
274

Alkali (ppt NaOH)


Initial
Final
Top Bottom Top Bottom
-0.2
0.2 -1.0
-0.4
-0.4
0.3 -3.1
-0.9
-0.9
0.9 -3.7
-1.3

48
89
104

Moisture
A
B
C

200

10
kg/scm

300
ppt

Hardness

100
0

30
Days

60

5
0

30
Days

60

Delight

Gel Phase

Delight1000Lye288Aq50
Tmax 151F after 180 minutes
Never reached gel phase
Total alkali: 1.3 ppt (top), -0.2 ppt (bottom)

Delight

Gel Phase

Delight1000Lye288Aq50
Tmax 151F after 180 minutes
Never reached gel phase
Total alkali: 1.3 ppt (top), -0.2 ppt (bottom)

Delight1000Lye288Aq100
Tmax 156F after 165 minutes
Very dry vaseline at 145F after 210 minutes
Total alkali: 0.5 ppt (top), 0.1 ppt (bottom)

Delight

Gel Phase

Delight1000Lye288Aq200
Vaseline with beads of oil at 151F after 195 minutes
Tmax 154F after 210 minutes
Total alkali: -0.2 ppt (top), 4.0 ppt (bottom)

Delight

Gel Phase

Delight1000Lye288Aq200
Vaseline with beads of oil at 151F after 195 minutes
Tmax 154F after 210 minutes
Total alkali: -0.2 ppt (top), 4.0 ppt (bottom)

Delight1000Lye288Aq250
Tmax 156F after 165 minutes
Jello with layer of oil at 156F after 180 minutes
Total alkali: -0.2 ppt (top), 8.7 ppt (bottom)

Delight

Gel Phase
Moisture Content (ppt)
200

Temperature (oC)

100
80
60

200

neat (gel)

160

curd + neat

120

40
20
0

300
Temperature (oF)

100

80

curd (solid)
Aq0

Aq144

Aq288

40

Soap phases determined by Differential Scanning Calorimetry

Conclusions

Conclusions

Does the initial water portion affect the final moisture content?

Conclusions

Conclusions

Does the initial water portion affect the final moisture content?
Probably not, though moisture may take more than 60 days to
equilibrate.

Conclusions

Conclusions

Does the initial water portion affect the final moisture content?
Probably not, though moisture may take more than 60 days to
equilibrate.

Does it affect the curing time?

Conclusions

Conclusions

Does the initial water portion affect the final moisture content?
Probably not, though moisture may take more than 60 days to
equilibrate.

Does it affect the curing time? Yes, more water initially lengthens the curing time.

Conclusions

Conclusions

Does the initial water portion affect the final moisture content?
Probably not, though moisture may take more than 60 days to
equilibrate.

Does it affect the curing time? Yes, more water initially lengthens the curing time.

Does it effect the hardness of the soap?

Conclusions

Conclusions

Does the initial water portion affect the final moisture content?
Probably not, though moisture may take more than 60 days to
equilibrate.

Does it affect the curing time? Yes, more water initially lengthens the curing time.

Does it effect the hardness of the soap? Yes, high-water soaps


are softer initially, but may equilibrate to the same final hardness as low-water soaps.

Conclusions

Conclusions

Does the initial water portion affect the final moisture content?
Probably not, though moisture may take more than 60 days to
equilibrate.

Does it affect the curing time? Yes, more water initially lengthens the curing time.

Does it effect the hardness of the soap? Yes, high-water soaps


are softer initially, but may equilibrate to the same final hardness as low-water soaps.

Is there a danger of separation?

Conclusions

Conclusions

Does the initial water portion affect the final moisture content?
Probably not, though moisture may take more than 60 days to
equilibrate.

Does it affect the curing time? Yes, more water initially lengthens the curing time.

Does it effect the hardness of the soap? Yes, high-water soaps


are softer initially, but may equilibrate to the same final hardness as low-water soaps.

Is there a danger of separation? Yes, high-water soaps are more


prone to separation than low-water soaps.

Checking In

Checking In
What are the temperature and consistency of your soap?

Scientific Soapmaking Class

Teaching Scientific Soapmaking


Economically

Spring 2010, 26 students

Scientific Soapmaking Class

Teaching Scientific Soapmaking


Economically

Spring 2010, 26 students

Each student paid $50 fee.

Scientific Soapmaking Class

Teaching Scientific Soapmaking


Economically

Spring 2010, 26 students

Each student paid $50 fee

Students self-organized into four firms

Scientific Soapmaking Class

Teaching Scientific Soapmaking


Economically

Spring 2010, 26 students

Each student paid $50 fee

Students self-organized into four firms

Firms bought all equipment and supplies at list price

Scientific Soapmaking Class

Teaching Scientific Soapmaking


Economically

Spring 2010, 26 students

Each student paid $50 fee

Students self-organized into four firms

Firms bought all equipment and supplies at list price

Students kept 90% of the soap produced

Scientific Soapmaking Class

Teaching Scientific Soapmaking


Economically

Spring 2010, 26 students

Each student paid $50 fee

Students self-organized into four firms

Firms bought all equipment and supplies at list price

Each student kept more than $50 worth of soap

Department kept all equipment and leftover suppliesno net


cost to the Department

Scientific Soapmaking Class

Teaching Economic Soapmaking

90 min lecture, 90 min lab each week

Scientific Soapmaking Class

Teaching Economic Soapmaking

90 min lecture, 90 min lab each week

4 weeks startup, 5 weeks production, 4 weeks R&D

Scientific Soapmaking Class

Teaching Economic Soapmaking

90 min lecture, 90 min lab each week

4 weeks startup, 5 weeks production, 4 weeks R&D

Production period approximately one 8-hr day

Scientific Soapmaking Class

Teaching Economic Soapmaking

90 min lecture, 90 min lab each week

4 weeks startup, 5 weeks production, 4 weeks R&D

Production period approximately one 8-hr day

Juried soap sale used to sell production soap

Scientific Soapmaking Class

Teaching Economic Soapmaking

90 min lecture, 90 min lab each week

4 weeks startup, 5 weeks production, 4 weeks R&D

Production period approximately one 8-hr day

Juried soap sale used to sell production soap

Each firm used GnuCash to track income and expenses

Scientific Soapmaking Class

Teaching Economic Soapmaking

90 min lecture, 90 min lab each week

4 weeks startup, 5 weeks production, 4 weeks R&D

Production period approximately one 8-hr day

Juried soap sale used to sell production soap

Each firm used GnuCash to track income and expenses

495 bars produced, 382 bars sold for $1746

Scientific Soapmaking Class

Teaching Economic Soapmaking

90 min lecture, 90 min lab each week

4 weeks startup, 5 weeks production, 4 weeks R&D

Production period approximately one 8-hr day

Juried soap sale used to sell production soap

Each firm used GnuCash to track income and expenses

495 bars produced, 382 bars sold for $1746

Return on Equity: 47%, 88%, 102%, 118%

Scientific Soapmaking Class

Juried Soap Sale

Rack used for curing, then displaying production soap

Scientific Soapmaking Class

Juried Soap Sale

Each firm set up a display of products with prices

Scientific Soapmaking Class

Juried Soap Sale

Each firm set up a display of products with prices

Each juror had $30 to spend

Scientific Soapmaking Class

Juried Soap Sale

Each firm set up a display of products with prices

Each juror had $30 to spend

Jurors kept the soaps they selected

Scientific Soapmaking Class

Juried Soap Sale

Each firm set up a display of products with prices

Each juror had $30 to spend

Jurors kept the soaps they selected

For each soap selected, 9 more sold at the same price

Scientific Soapmaking Class

Juried Soap Sale

Each firm set up a display of products with prices

Each juror had $30 to spend

Jurors kept the soaps they selected

For each soap selected, 9 more sold at the same price

Firms were allowed to change prices daily

Scientific Soapmaking Class

Juried Soap Sale

Each firm set up a display of products with prices

Each juror had $30 to spend

Jurors kept the soaps they selected

For each soap selected, 9 more sold at the same price

Firms were allowed to change prices daily

No real money changed hands, 90% of soap returned

Scientific Soapmaking Class

Juried Soap Sale

Each firm set up a display of products with prices

Each juror had $30 to spend

Jurors kept the soaps they selected

For each soap selected, 9 more sold at the same price

Firms were allowed to change prices daily

No real money changed hands, 90% of soap returned

Average value of returned soap: $60/student

Scientific Soapmaking Class

Grading Scientific Soapmaking

11% Homework

11% HSMG CP/HP Level I Exam

11% HSMG CP/HP Level II Exam

22% Cumulative Exam

11% Return on Equity

11% Analytical Project Report

22% Quarterly Report for Firm

Scientific Soapmaking Class

Organizations

The Handcrafted Soap Makers Guild (www.SoapGuild.org)

The Saponifier (www.Saponifier.com)

Scientific Soapmaking (www.ScientificSoapmaking.com)