Scientific Soap Making

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?
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
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
What happens if you provide only 2 molecules of NaOH?
Saponification
Saponification
What happens if you provide 4 molecules of NaOH?
Saponification
Saponification
We measure oil and NaOH by weight, not by molecules
Saponification
Saponification
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
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
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
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
SV
SSV
AR
SV
of Delight is 211.5 ppt KOH
SSV
of Delight is 150.8 ppt NaOH
SV
SSV
AR
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
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
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
Dreaded Orange Spots
Seizing
Seizing
Superfatting vs Discounting
Seizing
Superfatting vs Discounting
The Water Discount
Lye Concentration
Lye Concentration
What is the normal, correct, or standard lye concentration?
Lye Concentration
Lye Concentration
Ann Bramson, Soap: Making it, Enjoying it (1972)

25-27%, 26% average
Lye Concentration
Lye Concentration

25-27%, 26% average
Susan Cavitch, The Soapmakers Companion (1997)

26-29%, 27% average
Lye Concentration
Lye Concentration

25-27%, 26% average

26-29%, 27% average
Robert McDaniel, Essentially Soap (2000)

33-38%, 34% average
Lye Concentration
Lye Concentration

25-27%, 26% average

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
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?
Moisture content of soap over time
Hardness of soap over time
Alkalinity of soap over time
Separation of soap

Initially from formula, follow weight loss over time
Separation of soap


Soil penetrometer
Separation of soap


Soil penetrometer

Titration with 5 ppt citric acid
Separation of soap


Soil penetrometer

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
Total weight 1696 g
Water weight (174 + 348) = 522 g
Initial moisture = (522/1696) = 0.308 = 30.8% = 308 ppt
Moisture
Moisture
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
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
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
-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
Never reached gel phase
Total alkali: 1.3 ppt (top), -0.2 ppt (bottom)
Very dry vaseline at 145F after 210 minutes
Total alkali: 0.5 ppt (top), 0.1 ppt (bottom)
Delight
Gel Phase
Vaseline with beads of oil at 151F after 195 minutes
Total alkali: -0.2 ppt (top), 4.0 ppt (bottom)
Delight
Gel Phase
Vaseline with beads of oil at 151F after 195 minutes
Jello with layer of oil at 156F after 180 minutes
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
Conclusions
Conclusions
Probably not, though moisture may take more than 60 days to
equilibrate.
Conclusions
Conclusions
equilibrate.
Does it affect the curing time?
Conclusions
Conclusions
equilibrate.
Does it affect the curing time? Yes, more water initially lengthens the curing time.
Conclusions
Conclusions
equilibrate.
Does it effect the hardness of the soap?
Conclusions
Conclusions
equilibrate.
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
equilibrate.

Is there a danger of separation?
Conclusions
Conclusions
equilibrate.

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

Economically
Each student paid $50 fee.

Economically
Each student paid $50 fee
Students self-organized into four firms

Economically
Firms bought all equipment and supplies at list price

Economically
Students kept 90% of the soap produced

Economically
Each student kept more than $50 worth of soap
Department kept all equipment and leftover suppliesno net

cost to the Department
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
495 bars produced, 382 bars sold for $1746
Return on Equity: 47%, 88%, 102%, 118%
Juried Soap Sale
Rack used for curing, then displaying production soap
Juried Soap Sale
Each firm set up a display of products with prices
Juried Soap Sale
Each juror had $30 to spend
Juried Soap Sale
Jurors kept the soaps they selected
Juried Soap Sale
For each soap selected, 9 more sold at the same price
Juried Soap Sale
Firms were allowed to change prices daily
Juried Soap Sale
No real money changed hands, 90% of soap returned
Juried Soap Sale
No real money changed hands, 90% of soap returned
Average value of returned soap: $60/student
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
Organizations
The Handcrafted Soap Makers Guild (www.SoapGuild.org)
The Saponifier (www.Saponifier.com)
Scientific Soapmaking (www.ScientificSoapmaking.com)

Scientific Soap Making

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Scientific Soapmaking

Mike Lawson/Columbus Foods

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

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

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?

Place bottle of lye on balance

Press tare button

Use cup to transfer lye to jug of oil

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

Oil and Water

Oil and Water

Oil + 3 NaOH = Glycerol + 3 Soap

Each molecule of oil requires 3 molecules of NaOH

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?

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?

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?