Scientific Soap Making
description
Transcript of Scientific Soap Making
Scientific Soapmaking
Kevin M. Dunn
Summer 2010
$Revision: 1.1 $
1
Acknowledgements
Copyright © 2010 Kevin M. Dunn
Acknowledgements
• Mike Lawson/Columbus Foods
• Scientific Soapmakers
2
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, theywill 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, theywill become interested in the chemistry
• Experiments are designed to solve real-world problems
Let’s Make Soap
Let’s Make Soap
• 1000 g Delight (an oil blend)
• 288 g Lye (500 ppt NaOH)
Let’s Make Soap
Let’s 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?
Let’s Make Soap
Let’s Make Soap
• 1000 g Delight (already weighed)
• 288 g Lye (weigh synthetically into oil)
Let’s Make Soap
Let’s 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
SaponificationNaOH
O
O
O
O
O
O
NaOH NaOH
↓
ONa
O
OH
OH
OH
ONa
O
ONa
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 forcomplete saponification
Saponification Value
Saponification ValueTheoretical saponification value of glyceryl tristearate:
? g KOH = 1000 g oil(1 mol oil890 g oil
)(3 mol KOH
1 mol oil
)(56 g KOH
1 mol KOH
)= 189 ppt KOH
Experimental saponification value of tallow: 190-200 ppt
Saponification Value
Saponification ValueTheoretical sodium saponification value of glyceryl tristearate:
? g NaOH = 1000 g oil(1 mol oil890 g oil
)(3 mol NaOH
1 mol oil
)(40 g NaOH
1 mol NaOH
)= 135 ppt 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 = weight (mg) of NaOH needed to saponify 1 g of oil
• AR = 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 pptNaOH
• Why?
Lye Discounting
Lye Discounting
0 2 4 6
140 144 148 152 156
TA /
ppt N
aOH
AR / ppt NaOH
1 Day Old
0 2 4 6
140 144 148 152 156
TA /
ppt N
aOH
AR / ppt NaOH
11 Weeks Old
Checking In
Checking InWhat 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
? g KOH = 1000 g oil(YY.YY g standard
1.XX g oil
)(4.ZZ g KOH
1000 g standard
)AV =
(YY.YY1.XX
)4.ZZ ppt KOH
• What is the Acid Value of your oil?
Acid Value
Acid Value
? g KOH = 1000 g oil(YY.YY g standard
1.XX g oil
)(4.ZZ g KOH
1000 g standard
)AV =
(YY.YY1.XX
)4.ZZ ppt KOH
• What is the Acid Value of your oil?
• Why did we get different values?
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 Soapmaker’s 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 Soapmaker’s 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 Soapmaker’s 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 140◦F 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 ofsoap?
Total Alkali
Total Alkali
? g NaOH = 1000 g soap(Y.YY g acid1.XX g soap
)(5 g H3Cit
1000 g acid
)(
1 mol H3Cit192.12 g H3Cit
)(3 mol NaOH1 mol H3Cit
)(40.00 g NaOH1 mol NaOH
)TA = 3.123
(Y.YY1.XX
)ppt NaOH
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 OilBatch Code Moisture (ppt) Alkali (ppt NaOH)KMD2007.12.27 Initial Final Initial Final
Top Bottom Top BottomA Palm1000Lye286 111 54 1.8 4.9 0.3 0.9B Palm1000Lye286Aq143 200 60 1.8 1.4 -1.7 -0.2C Palm1000Lye286Aq286 273 74 0.5 0.3 -1.7 -0.1
0
100
200
300
0 30 60
ppt
Days
MoistureABC
0
5
10
0 30 60
kg/s
cm
Days
Hardness
Coconut Oil
Coconut OilBatch Code Moisture (ppt) Alkali (ppt NaOH)KMD2008.1.8 Initial Final Initial Final
Top Bottom Top BottomD Coconut1000Lye348 129 41 0.4 0.5 -0.6 -0.3E Coconut1000Lye348Aq174 229 88 -0.1 -0.2 -1.7 -1.0F Coconut1000Lye348Aq348 308 109 0.1 0.2 -1.8 -0.4
0
100
200
300
0 30 60
ppt
Days
MoistureDEF
0
5
10
0 30 60
kg/s
cm
Days
Hardness
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 OilBatch Code Moisture (ppt) Alkali (ppt NaOH)KMD2008 Initial Final Initial Final
Top Bottom Top Bottom1.7A Olive1000Lye264 104 36 0.3 0.2 -3.2 -0.43.5A Olive990Clove10Lye259 103 43 -0.4 -0.7 -0.7 -0.73.5B Olive990Clove10Lye259Aq130 187 61 -0.4 -0.4 -0.8 -0.73.5C Olive990Clove10Lye260Aq260 256 67 -0.7 6.2 -1.1 -0.2
0
100
200
300
0 30 60
ppt
Days
Moisture1.7A3.5A3.5B3.5C
0
5
10
0 30 60
kg/s
cm
Days
Hardness
Delight
Delight
• Delight = Olive390Palm280Coconut280Castor50
Delight
Delight
Batch Code Moisture (ppt) Alkali (ppt NaOH)KMD2008.2.17 Initial Final Initial Final
Top Bottom Top BottomA Delight1000Lye288 112 48 -0.2 0.2 -1.0 -0.4B Delight1000Lye288Aq144 201 89 -0.4 0.3 -3.1 -0.9C Delight1000Lye288Aq288 274 104 -0.9 0.9 -3.7 -1.3
0
100
200
300
0 30 60
ppt
Days
MoistureABC
0
5
10
0 30 60
kg/s
cm
Days
Hardness
Delight
Gel Phase
• Delight1000Lye288Aq50
Tmax 151◦F after 180 minutes
Never reached gel phase
Total alkali: 1.3 ppt (top), -0.2 ppt (bottom)
Delight
Gel Phase
• Delight1000Lye288Aq50
Tmax 151◦F after 180 minutes
Never reached gel phase
Total alkali: 1.3 ppt (top), -0.2 ppt (bottom)
• Delight1000Lye288Aq100
Tmax 156◦F after 165 minutes
“Very dry vaseline” at 145◦F after 210 minutes
Total alkali: 0.5 ppt (top), 0.1 ppt (bottom)
Delight
Gel Phase
• Delight1000Lye288Aq200
“Vaseline” with beads of oil at 151◦F after 195 minutes
Tmax 154◦F after 210 minutes
Total alkali: -0.2 ppt (top), 4.0 ppt (bottom)
Delight
Gel Phase
• Delight1000Lye288Aq200
“Vaseline” with beads of oil at 151◦F after 195 minutes
Tmax 154◦F after 210 minutes
Total alkali: -0.2 ppt (top), 4.0 ppt (bottom)
• Delight1000Lye288Aq250
Tmax 156◦F after 165 minutes
“Jello” with layer of oil at 156◦F after 180 minutes
Total alkali: -0.2 ppt (top), 8.7 ppt (bottom)
Delight
Gel Phase
0
20
40
60
80
100
Aq288Aq144Aq0
40
80
120
160
200
100 200 300Te
mpe
ratu
re (o C)
Tem
pera
ture
(o F)
Moisture Content (ppt)
curd (solid)
curd + neat
neat (gel)
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 toequilibrate.
Conclusions
Conclusions
• Does the initial water portion affect the final moisture content?Probably not, though moisture may take more than 60 days toequilibrate.
• 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 toequilibrate.
• Does it affect the curing time? Yes, more water initially length-ens 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 toequilibrate.
• Does it affect the curing time? Yes, more water initially length-ens 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 toequilibrate.
• Does it affect the curing time? Yes, more water initially length-ens the curing time.
• Does it effect the hardness of the soap? Yes, high-water soapsare softer initially, but may equilibrate to the same final hard-ness 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 toequilibrate.
• Does it affect the curing time? Yes, more water initially length-ens the curing time.
• Does it effect the hardness of the soap? Yes, high-water soapsare softer initially, but may equilibrate to the same final hard-ness 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 toequilibrate.
• Does it affect the curing time? Yes, more water initially length-ens the curing time.
• Does it effect the hardness of the soap? Yes, high-water soapsare softer initially, but may equilibrate to the same final hard-ness as low-water soaps.
• Is there a danger of separation? Yes, high-water soaps are moreprone to separation than low-water soaps.
Checking In
Checking InWhat are the temperature and consistency of your soap?
Scientific Soapmaking Class
Teaching Scientific SoapmakingEconomically
• Spring 2010, 26 students
Scientific Soapmaking Class
Teaching Scientific SoapmakingEconomically
• Spring 2010, 26 students
• Each student paid $50 fee.
Scientific Soapmaking Class
Teaching Scientific SoapmakingEconomically
• Spring 2010, 26 students
• Each student paid $50 fee
• Students self-organized into four “firms”
Scientific Soapmaking Class
Teaching Scientific SoapmakingEconomically
• 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 SoapmakingEconomically
• 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 SoapmakingEconomically
• 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 supplies—no netcost 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)