Scientific Soapmaking

Transcription

1 Scientific Soapmaking Kevin M. Dunn Summer 2008 $Revision: 1.1 $ 1

2 Acknowledgements Copyright 2008 Kevin M. Dunn Acknowledgements Mike Lawson/Columbus Foods 2

3 Why Teach Soapmaking? Why Teach Soapmaking? Thriving cottage industry

4 Why Teach Soapmaking? Why Teach Soapmaking? Thriving cottage industry Soapmakers generally come from a cooking/craft background

5 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

6 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

7 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

8 Let s Make Soap Let s Make Soap g Delight (an oil blend) g Lye (500 ppt NaOH)

9 Let s Make Soap Let s Make Soap g Delight (an oil blend) g Lye (500 ppt NaOH) But how are we to weigh?

10 Weighing Synthetically Weighing Synthetically Place cup of water on balance Press tare button Use pipet to transfer water to second cup What if we overshoot? What about the water in the pipet?

11 Let s Make Soap Let s Make Soap g Delight (already weighed) g Lye (weigh synthetically into oil)

12 Let s Make Soap Let s Make Soap g Delight (already weighed) g Lye (weigh synthetically into oil) Shake vigorously for 60 seconds Pour into styrofoam cup Measure temperature

13 Oil and Water Oil and Water

14 Glyceryl Trilaurate Glyceryl Trilaurate O O O O O O

15 Saponification Saponification

16 Saponification Saponification NaOH O O O O O O NaOH NaOH O Na O OH OH OH O Na O Na O O

17 Saponification Saponification Oil + 3 NaOH = Glycerol + 3 Soap Each molecule of oil requires 3 molecules of NaOH

18 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?

19 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?

20 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

21 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

22 Saponification Value Saponification Value Theoretical saponification value of glyceryl tristearate: ( )( )( ) 1 mol Oil 3 mol KOH 56 g KOH? g KOH = 1000 g Oil 890 g Oil 1 mol Oil 1 mol KOH = 189 ppt KOH Experimental saponification value of tallow: ppt

23 Saponification Value Saponification Value Theoretical sodium saponification value of glyceryl tristearate: ( )( )( ) 1 mol Oil 3 mol NaOH 40 g NaOH? g NaOH = 1000 g Oil 890 g Oil 1 mol Oil 1 mol NaOH = 135 ppt NaOH Experimental sodium saponification value of tallow: ppt

24 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

25 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 ppt KOH SSV of Delight is ppt NaOH

26 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 ppt KOH SSV of Delight is ppt NaOH Since Lye is 500 ppt NaOH, we have used an AR of 144 ppt NaOH Why?

27 Lye Discounting Lye Discounting Total Alkali (ppt NaOH) Day Old Alkali Ratio (ppt NaOH) Total Alkali (ppt NaOH) Weeks Old Alkali Ratio (ppt NaOH)

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

29 Measurable quantities Measurable Quantities Finished soap Total alkali Moisture content Hardness

30 Measurable quantities Measurable Quantities Finished soap Total alkali Moisture content Hardness Raw materials Saponification value Lye concentration Free fatty acid

31 Free Fatty Acid Free Fatty Acid Real-world oils may contain free fatty acid How can we measure it?

32 Titration Titration

33 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

34 Weighing Analytically Weighing Analytically Place coconut oil bottle on balance Press tare button Transfer drops of oil to Erlenmeyer flask Replace oil bottle on balance and read weight

35 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

36 Acid Value Acid Value ( )( ) YY.YY g Std 4.ZZ g KOH? g KOH = 1000 g Oil ( ) 1.XX g Oil 1000 g Std YY.YY = 4.ZZ ppt KOH 1.XX What is the Acid Value of your oil?

37 Acid Value Acid Value ( )( ) YY.YY g Std 4.ZZ g KOH? g KOH = 1000 g Oil ( ) 1.XX g Oil 1000 g Std YY.YY = 4.ZZ ppt KOH 1.XX What is the Acid Value of your oil? Why did we get different values?

38 Free Fatty Acid Free Fatty Acid Free Lauric Acid = AV What is the Free Lauric Acid content of your oil?

39 Free Fatty Acid Free Fatty Acid Free Lauric Acid = AV What is the Free Lauric Acid content of your oil? Which oil would saponify quicker?

40 Extended Investigations Extended Investigations Dreaded Orange Spots

41 Extended Investigations Extended Investigations Dreaded Orange Spots Seizing

42 Extended Investigations Extended Investigations Dreaded Orange Spots Seizing Superfatting vs Discounting

43 Extended Investigations Extended Investigations Dreaded Orange Spots Seizing Superfatting vs Discounting The Water Discount

44 Lye Concentration Lye Concentration What is the normal, correct, or standard lye concentration?

45 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

46 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

47 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

48 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

49 The Soap Formula The Soap Formula Lye = 50.00% NaOH, 50.00% distilled water Coconut 1000 Lye 348 Coconut 1000 Lye 348 Aq 174 Coconut 1000 Lye 348 Aq 348

50 The Soap Formula The Soap Formula Lye = 50.00% NaOH, 50.00% distilled water Coconut 1000 Lye 348 (50.00% NaOH Low-Water ) Coconut 1000 Lye 348 Aq 174 (33.33% NaOH Medium-Water ) Coconut 1000 Lye 348 Aq 348 (25.00% NaOH High-Water )

51 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

52 Questions Questions What do we want to know?

53 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?

54 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

55 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

56 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

57 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

58 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

59 Moisture Moisture Coconut 1000 Lye 348 Aq 348 Total weight 1696 g Water weight ( ) = 522 g Initial moisture = (522/1696) = = 30.8% = 308 ppt

60 Moisture Moisture Coconut 1000 Lye 348 Aq 348 Total weight 1696 g Water weight ( ) = 522 g Initial moisture = (522/1696) = = 30.8% = 308 ppt Initial bar weight g; Final weight g Weight loss (28.15/141.32) = = 19.9% = 199 ppt Final moisture = = 109 ppt

61 Penetrometer Penetrometer Smaller foot used for hard soaps.

62 Titration Titration How many grams of acid required to titrate a given weight of soap?

63 Total Alkali Total Alkali ( )( ) Y.YY g Acid 5 g H3 Cit? g NaOH = 1000 g Soap ( 1.XX )( g Soap 1000 )( g Acid ) 1 mol H3 Cit 3 mol NaOH g NaOH ( g H 3 ) Cit 1 mol H 3 Cit Y.YY = ppt NaOH 1.XX 1 mol NaOH

64 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

65 Palm Oil Palm Oil Batch Code Moisture/ppt Alkali/ppt NaOH KMD Initial Final Initial Final Top Bottom Top Bottom A Palm 1000 Lye B Palm 1000 Lye 286 Aq C Palm 1000 Lye 286 Aq ppt Moisture A B C kg/scm 10 5 Hardness Days Days

66 Coconut Oil Coconut Oil Batch Code Moisture/ppt Alkali/ppt NaOH KMD Initial Final Initial Final Top Bottom Top Bottom D Coconut 1000 Lye E Coconut 1000 Lye 348 Aq F Coconut 1000 Lye 348 Aq Moisture D E F 10 Hardness ppt kg/scm Days Days

67 Olive Oil Olive Oil Medium and high water soaps separated What can I do to accelerate trace?

68 Olive Oil Olive Oil Medium and high water soaps separated. What can I do to accelerate trace? Add clove oil.

69 Olive Oil Olive Oil Batch Code Moisture/ppt Alkali/ppt NaOH KMD2008 Initial Final Initial Final Top Bottom Top Bottom 1.7A Olive 1000 Lye A Olive 990 Clove 10 Lye B Olive 990 Clove 10 Lye 259 Aq C Olive 990 Clove 10 Lye 260 Aq ppt Moisture 1.7A 3.5A 3.5B 3.5C kg/scm 10 5 Hardness Days Days

70 Delight Delight Delight = Olive 390 Palm 280 Coconut 280 Castor 50

71 Delight Delight Batch Code Moisture/ppt Alkali/ppt NaOH KMD Initial Final Initial Final Top Bottom Top Bottom A Delight 1000 Lye B Delight 1000 Lye 288 Aq C Delight 1000 Lye 288 Aq ppt Moisture A B C kg/scm 10 5 Hardness Days Days

72 Delight Gel Phase Delight 1000 Lye 288 Aq 50 T max 151 F after 180 minutes Never reached gel phase Total alkali: 1.3 ppt (top), -0.2 ppt (bottom)

73 Delight Gel Phase Delight 1000 Lye 288 Aq 50 T max 151 F after 180 minutes Never reached gel phase Total alkali: 1.3 ppt (top), -0.2 ppt (bottom) Delight 1000 Lye 288 Aq 100 T max 156 F after 165 minutes Very dry vaseline at 145 F after 210 minutes Total alkali: 0.5 ppt (top), 0.1 ppt (bottom)

74 Delight Gel Phase Delight 1000 Lye 288 Aq 200 Vaseline with beads of oil at 151 F after 195 minutes T max 154 F after 210 minutes Total alkali: -0.2 ppt (top), 4.0 ppt (bottom)

75 Delight Gel Phase Delight 1000 Lye 288 Aq 200 Vaseline with beads of oil at 151 F after 195 minutes T max 154 F after 210 minutes Total alkali: -0.2 ppt (top), 4.0 ppt (bottom) Delight 1000 Lye 288 Aq 250 T max 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)

76 Conclusions Conclusions I encountered no problems with lye concentrations up to 50%.

77 Conclusions Conclusions I encountered no problems with lye concentrations up to 50%. High-water Olive and Delight soaps separated.

78 Conclusions Conclusions I encountered no problems with lye concentrations up to 50%. High-water Olive and Delight soaps separated. More water delays trace.

79 Conclusions Conclusions I encountered no problems with lye concentrations up to 50%. High-water Olive and Delight soaps separated. More water delays trace. Low-water soaps start out hard; medium- and high-water soaps may or may not catch up.

80 Conclusions Conclusions I encountered no problems with lye concentrations up to 50%. High-water Olive and Delight soaps separated. More water delays trace. Low-water soaps start out hard; medium- and high-water soaps may or may not catch up. Gel phase was observed only for medium- and high-water soaps. Since all soaps were fully saponified, gel phase is not essential. In fact, when separation occurred, it always happened during gel phase.

81 Conclusions Conclusions I encountered no problems with lye concentrations up to 50%. High-water Olive and Delight soaps separated. More water delays trace. Low-water soaps start out hard; medium- and high-water soaps may or may not catch up. Gel phase was observed only for medium- and high-water soaps. Since all soaps were fully saponified, gel phase is not essential. In fact, when separation occurred, it always happened during gel phase. Saponification and curing are two separate processes.

82 Recommendations Recommendations Decide on a standard lye concentration and always use that when making soap.

83 Recommendations Recommendations Decide on a standard lye concentration and always use that when making soap. You can always add extra (water, milk, etc.) to delay trace or decrease initial hardness.

84 Recommendations Recommendations Decide on a standard lye concentration and always use that when making soap. You can always add extra (water, milk, etc.) to delay trace or decrease initial hardness. If oil separates from the soap, try decreasing the amount of (water, milk, etc.).

85 Recommendations Recommendations Decide on a standard lye concentration and always use that when making soap. You can always add extra (water, milk, etc.) to delay trace or decrease initial hardness. If oil separates from the soap, try decreasing the amount of (water, milk, etc.). Be aware that soaps may continue to lose moisture, even after 60 days.

86 Recommendations Recommendations Decide on a standard lye concentration and always use that when making soap. You can always add extra (water, milk, etc.) to delay trace or decrease initial hardness. If oil separates from the soap, try decreasing the amount of (water, milk, etc.). Be aware that soaps may continue to lose moisture, even after 60 days. Make lye only from NaOH and water.

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

88 Summary Why Am I Teaching You to Teach Soapmaking? There is a market for soapmaking instruction

89 Summary Why Am I Teaching You to Teach Soapmaking? There is a market for soapmaking instruction Soapmaking can motivate gen-ed students

90 Summary Why Am I Teaching You to Teach Soapmaking? There is a market for soapmaking instruction Soapmaking can motivate gen-ed students Online soapmaking communities are fraught with MSU

91 Summary Why Am I Teaching You to Teach Soapmaking? There is a market for soapmaking instruction Soapmaking can motivate gen-ed students Online soapmaking communities are fraught with MSU I m lonely

92 Summary Organizations The Handcrafted Soap Makers Guild ( The Saponifier ( Scientific Soapmaking (