EP2629742A2

EP2629742A2 - Hair-mending compositions and associated methods

Info

Publication number: EP2629742A2
Application number: EP11834854.9A
Authority: EP
Inventors: Michael Wright; Margaret Szerszen; Jason Cohen; Dan Petroski; Deborah Eagan; Chris Felski; Gilles M. Verboom
Original assignee: Alberto Culver Co
Current assignee: Alberto Culver Co
Priority date: 2010-10-20
Filing date: 2011-10-07
Publication date: 2013-08-28
Also published as: BR112013009589A2; WO2012054243A2; CN103179943B; MX350219B; EP2629742A4; PH12013500698B1; MX2013004435A; WO2012054243A3; CA2812991C; JP2013540152A; EA201390583A1; EA024282B1; WO2012054029A1; CN103179943A; CA2812991A1; PH12013500698A1; JP5977750B2

Abstract

Disclosed herein are hair-mending compositions containing a polyelectrolyte complex. Also disclosed are methods of their use, methods of their manufacture, methods of testing their efficacy, and media methods involving hair mending.

Description

HAIR-MENDING COMPOSITIONS AND ASSOCIATED METHODS

CROSS-REFERENCE TO RELATED APPLICATIONS

[0001] This patent application claims the benefit of U.S. Provisional Patent Application No. 61/394,966, filed October 20, 2010 and International Application No. PCT/US 10/53360, filed October 20, 2010, both of which are incorporated by reference herein in their entireties.

BACKGROUND OF THE INVENTION

[0002] Hair care compositions are often formulated to have multiple properties. For example, a hair conditioner may be formulated to condition hair and also may be formulated to repair hair. Hair care compositions with multiple properties are attractive to a consumer in that fewer compositions need be applied to the hair to achieve a desired effect. However, to formulate such a hair care composition, multiple ingredients are often necessary. As the number of ingredients increases, the complexity of the composition increases. The long term stability of such a composition can become compromised due to incompatibilities among the many ingredients.

[0003] Furthermore, due to the large number of ingredients in many hair care

compositions, formulators are not only faced with the challenges of finding the proper ingredients to provide the desired cosmetic properties but are also faced with the challenge of manufacturing these complicated compositions. Such challenges include developing production protocols to produce a composition both on a small scale for initial testing and on a large scale for commercial marketing. A greater number of ingredients may translate into a greater number of manufacturing containers required, which itself translates into more time and expense to produce the composition. Cosmetic compositions thus are complicated mixtures of ingredients, and with such complexity, require careful consideration when developing production protocols.

[0004] Hair care composition ingredients include conditioning agents, which are often positively charged compounds. Hair fibers have a net negative charge. The positive charge of the conditioning agents is attracted to the overall negative charge of the hair fibers, making the positively charged conditioning agents substantive to the hair. This substantive nature allows the conditioning agent to interact with the hair in order for the conditioning agent to provide its conditioning effect. The conditioning effect can include restoring the hair fiber after damage to the hair, such as repairing split-ends.

[0005] Conditioning agents known in the art include quaternary ammonium nitrogen compounds, known as "quats," and polymers comprising moieties of such compounds, known as "polyquats." The polyquats include polyquaternium-28, a

vinylpyrrolidone/methacrylamidopropyl trimethyl ammonium chloride copolymer. It has been found that the combination of polyquat-28 and methylvinylether/maleic acid copolymer (PVMMA) at particular ratios produces a polyelectrolyte complex (PEC) that repairs split- end damage (U.S. Patent Application Publication Nos. 2005/0089494 and 2006/0251603, both assigned to ISP Investments Inc.). However, within the context of complicated hair care formulations, the stability of PECs may be compromised due to the presence of other ingredients, especially charged compounds and polymers that could disrupt the PEC structure. Thus, the usefulness of PECs may be limited by their compatibility with other ingredients that may be desirable to include in a hair care composition. Since multiple properties are often desired in hair care compositions, it would be desirable to formulate hair care compositions that include stable combinations of PECs with other hair care ingredients that provide additional desirable properties.

[0006] Also, although PVMMA:polyquat-28 PECs consist of only two component ingredients, the method of producing these PECs is described in the ISP Investments applications as comprising two or three separate containers. Such a method is cumbersome, especially in view of any additional containers required to incorporate additional ingredients. The dedication of two or three containers in a large-scale production facility for the making of one complex is inefficient and costly.

[0007] Additionally, when a consumer purchases hair care products, the consumer does so based on the properties of the hair care product. For example, a consumer with frizzy hair may purchase a product to de-frizz the hair, and a consumer with split-ends may purchase a product to repair the split-ends. Thus, consumers may purchase hair care products having properties desirable for a particular hair type or hair problem. In order for consumers to compare hair care product compositions to make a decision regarding which to purchase, the beneficial properties of the compositions should be clearly communicated to the consumers. One method is to use still photography, such as described in the ISP Investments applications. However, additional methods are needed.

[0008] It would therefore be desirable to formulate a stable hair care composition that includes intact PECs in combination with other hair benefit agents, especially charged hair benefit agents. Also, there is a need for a more efficient process for making PECs and hair care compositions containing PECs. Further, there is a need for the development of test methods that can show improved results of split-end mending of a hair care composition such that the benefits of the hair care composition can then be effectively communicated to consumers. There also is a need for the development of additional methods that can show the benefits of a hair care composition such that the benefits can then be effectively

communicated to consumers. The present invention provides these advantages. Additional advantages of the invention, as well as additional inventive features, will be apparent from the description of the invention provided herein.

BRIEF SUMMARY OF THE INVENTION

[0009] In one aspect, the present invention provides a hair care composition comprising a polyelectrolyte complex of a cationic polymer and an anionic polymer in the form of an emulsion with improved freeze-thaw stability relative to comparative compositions containing such polyelectrolyte complexes.

[0010] In another aspect, the present invention provides a hair care composition comprising a polyelectrolyte complex of a cationic polymer and an anionic polymer, wherein the viscosity of the composition is greater than 3000 cps.

[0011] In another aspect, the present invention provides a hair care composition comprising a polyelectrolyte complex of a cationic polymer and an anionic polymer; from about 1% to about 5% of a thickening agent; about 10% or greater of propylene glycol; and about 5% or greater of an emollient; wherein the percentages are based on the total weight of the composition.

[0012] In yet another aspect, the present invention provides a hair care composition comprising a polyelectrolyte complex of a cationic polymer and an anionic polymer; from about 3% to about 5% of a thickening agent; and about 2% or less of an emollient; wherein the percentages are based on the total weight of the composition.

[0013] The present invention also provides methods of using the compositions described herein, including a method of conditioning a hair fiber and a method of repairing a split-end of a hair fiber.

[0014] Furthermore, the present invention provides a method for improving the freeze- thaw stability of a hair care composition comprising a polyelectrolyte complex of a cationic polymer and an anionic polymer, the method comprising adding to the hair care composition from about 1% to about 5% of a thickening agent, wherein the percentage is based on the total weight of the composition.

[0015] Additionally, the present invention provides a method for improving the freeze- thaw stability of a hair care composition comprising a polyelectrolyte complex, the method comprising adding to the hair care composition from about 10% or greater of propylene glycol, wherein the percentage is based on the total weight of the composition.

[0016] The present invention also provides a method for thermally protecting hair by applying to the hair compositions as described herein.

[0017] Furthermore, an aspect of the present invention provides a method of producing a polyelectrolyte complex, the method comprising hydrating a methylvinylether/maleic acid copolymer having repeating units of the formula (Formula I) in a container; reacting the methylvinylether/maleic acid copolymer with a base, in the container in an amount sufficient to at least partially neutralize the acidic groups thereof, to form an intermediate mixture; heating the intermediate mixture in the container; adding to the intermediate mixture in the container a cationic copolymer of a vinylpyrrolidone of the formula (Formula II)

and a methacrylamidopropyl trimethylammonium chloride of the formula (Formula III)

and mixing the polymers in the container at high shear force and at a temperature of at least about 50-60 °C to produce the polyelectrolyte complex.

[0018] The present invention also provides a method of producing a polyelectrolyte complex, the method comprising hydrating a methylvinylether/maleic acid copolymer having repeating units of the formula I in a container; reacting the methylvinylether/maleic acid copolymer with, e.g., a 20% sodium hydroxide solution in the container, wherein the sodium hydroxide is added in an amount sufficient to achieve a pH of, e.g., from about 6.5 to about 7.5 or from about 6.9 to about 7.0, to form an intermediate mixture; heating the intermediate mixture in the container to a temperature of from about 50 °C to about 60 °C; adding to the intermediate mixture in the container a cationic copolymer of a vinylpyrrolidone of the formula II and a methacrylamidopropyl trimethyl ammonium chloride of the formula III; and mixing the polymers in the container for at least about 10 minutes at high shear force and at a temperature of at least about 50-60 °C to produce the polyelectrolyte complex. In an embodiment, the method further comprises the step of mixing the polyelectrolyte complex with one or more components selected from aqueous carriers, surfactants, fragrances, conditioning agents, emollients, emulsifiers, thickening agents, preservatives, gelling agents, silicones, hair fixatives, humectants and moisturizers to form a hair care composition. In an embodiment, the mixing is sufficient to allow adequate incorporation of the one or more components.

[0019] The present invention also provides a method of producing a hair care

composition comprising producing a polyelectrolyte complex, comprising the steps of hydrating a methylvinylether/maleic acid copolymer having repeating units of the formula I in a container; reacting the methylvinylether/maleic acid copolymer with a base, such as, e.g., 20% sodium hydroxide, in the container in an amount sufficient to at least partially neutralize the acidic groups thereof, e.g., wherein the sodium hydroxide is added in an amount sufficient to achieve a pH of, e.g., from about 6.5 to about 7.5 or from about 6.9 to about 7.0, to form an intermediate mixture; heating the intermediate mixture in the container, e.g., to a temperature of from about 50 °C to about 60 °C; adding to the intermediate mixture in the container a cationic copolymer of a vinylpyrrolidone of the formula II and a methacrylamidopropyl trimethylammonium chloride of the formula III; mixing the polymers in the container at high shear force and at a temperature of at least about 50-60 °C to produce the polyelectrolyte complex; adding to the polyelectrolyte complex in the container one or more additional components selected from aqueous carriers, surfactants, fragrances, conditioning agents, emollients, emulsifiers, thickening agents, preservatives, gelling agents, silicones, hair fixatives, humectants and moisturizers; and mixing the resulting composition in the container. In an embodiment, the method produces a hair care composition in the form of a shampoo, conditioner, leave-in treatment, creme, gel, mousse, serum, oil treatment, glaze, or spray.

[0020] The present invention also provides a method of producing a hair care

composition comprising producing a polyelectrolyte complex between a

methylvinylether/maleic acid copolymer and a cationic copolymer of a vinylpyrrolidone and a methacrylamidopropyl trimethylammonium chloride, comprising the steps of hydrating a methylvinylether/maleic acid copolymer having repeating units of the formula I in a first container; reacting the methylvinylether/maleic acid copolymer with a base, such as, e.g., 20% sodium hydroxide, in the first container in an amount sufficient to at least partially neutralize the acidic groups thereof, e.g., wherein the sodium hydroxide is added in an amount sufficient to achieve a pH of, e.g., from about 6.5 to about 7.5 or from about 6.9 to about 7.0, to form an intermediate mixture; heating the intermediate mixture in the first container, e.g., to a temperature of from about 50 °C to about 60 °C; adding to the

intermediate mixture in the first container a cationic copolymer of a vinylpyrrolidone of the formula II and a methacrylamidopropyl trimethylammonium chloride of the formula III; mixing the polymers in the first container at high shear force and at a temperature of at least about 50-60 °C to produce the polyelectrolyte complex; mixing in a second container one or more components selected from aqueous carriers, surfactants, fragrances, conditioning agents, emollients, emulsifiers, thickening agents, preservatives, gelling agents, silicones, hair fixatives, humectants and moisturizers; and mixing together in the first or second container the polyelectrolyte complex of the first container and the mixed components of the second container. In an embodiment, the method produces a hair care composition in the form of a shampoo, conditioner, leave-in treatment, creme, gel, mousse, or spray.

[0021] Furthermore, the present invention provides a method of graphically

reconstructing a repair of a split-end of a hair fiber, the method comprising securing a hair fiber to a surface, wherein the hair fiber secured to the surface has a split-end or is damaged while on the surface to produce a split-end; associating the surface with a magnifying device, wherein the split-end is positioned within the field of view of the magnifying device;

associating an image capture device with the magnifying device so as to capture an enlarged image of the field of view of the magnifying device; treating the split-end with a composition, wherein the composition repairs the split-end and wherein the split-end fuses together; and via the image capture device associated with the magnifying device, capturing an image of the repair of the split-end during treatment with the composition, and storing a representation of the captured image of the repair for subsequent retrieval. In an embodiment, the composition comprises, e.g., from about 1% to about 5% of a thickening agent, about 10% or greater of propylene glycol, and about 5% or greater of an emollient, wherein the percentages are based on the total weight of the composition. In another embodiment, the composition comprises from about 3% to about 5% of a thickening agent, and about 2% or less of an emollient, wherein the percentages are based on the total weight of the composition. In another embodiment, the degree of split-end hair fiber repair is communicated to consumers.

[0022] The present invention also provides a method of quantitatively assessing the degree of split-end hair fiber repair, the method comprising obtaining a tress of hair, wherein the hair is twice-bleached hair; combing and blow drying the tress of hair to produce at least one split-end in at least one hair fiber; removing at least one hair fiber having a split-end from the tress; optionally marking the at least one hair fiber; capturing a first image of the split-end of the at least one hair fiber and storing a representation, e.g., an electronic representation, of the image; associating the hair fiber with the tress from which the hair fiber was removed; treating the tress and the hair fiber with a composition; removing the hair fiber from the treated tress; capturing a second image of the end of the hair fiber removed from the treated tress; assigning a value of 0 for no repair of the split-end, ½ for partial repair, or 1 for complete repair with respect to the hair fiber to assess the degree of split-end repair of the hair fiber; and if more than one hair fiber is assessed, optionally determining an average value with respect to the assessed hair fibers. In an embodiment, the composition comprises, e.g., from about 1% to about 5% of a thickening agent, about 10% or greater of propylene glycol, and about 5% or greater of an emollient, wherein the percentages are based on the total weight of the composition. In another embodiment, the composition comprises from about 3% to about 5% of a thickening agent, and about 2% or less of an emollient, wherein the percentages are based on the total weight of the composition. In another embodiment, the degree of split-end hair fiber repair is communicated to consumers.

[0023] One embodiment of the present invention provides a method of quantitatively assessing the degree of split-end hair fiber repair, the method comprising obtaining a tress of hair; producing at least one hair fiber of the tress to have a spilt-end; removing at least one hair fiber having a split-end from the tress; optionally marking the at least one hair fiber; capturing a first image of the split-end of the at least one hair fiber and storing a representation, e.g., an electronic representation, of the image; associating the hair fiber with the tress from which the hair fiber was removed; treating the tress and the hair fiber with a composition, wherein the composition comprises a hair care composition comprising a polyelectrolyte complex of a cationic polymer and an anionic polymer, from about 1% to about 5% of a thickening agent, about 10% or greater of propylene glycol, and about 5% or greater of an emollient, wherein the percentages are based on the total weight of the composition; removing the hair fiber from the treated tress; capturing a second image of the end of the hair fiber removed from the treated tress; assigning a value of 0 for no repair of the split-end, ½ for partial repair, or 1 for complete repair with respect to the hair fiber to assess the degree of split-end repair of the hair fiber; and if more than one hair fiber is assessed, optionally determining an average value with respect to the assessed hair fibers.

[0024] Another embodiment of the present invention provides a method of quantitatively assessing the degree of split-end hair fiber repair, the method comprising obtaining a tress of hair; producing at least one hair fiber of the tress to have a spilt-end; removing at least one hair fiber having a split-end from the tress; optionally marking the at least one hair fiber; capturing a first image of the split-end of the at least one hair fiber and storing a

representation, e.g., an electronic representation, of the image; associating the hair fiber with the tress from which the hair fiber was removed; treating the tress and the hair fiber with a composition, wherein the composition comprises a hair care composition comprising a polyelectrolyte complex of a cationic polymer and an anionic polymer, from about 3% to about 5% of a thickening agent, and about 2% or less of an emollient, wherein the percentages are based on the total weight of the composition; removing the hair fiber from the treated tress; capturing a second image of the end of the hair fiber removed from the treated tress; assigning a value of 0 for no repair of the split-end, ½ for partial repair, or 1 for complete repair with respect to the hair fiber to assess the degree of split-end repair of the hair fiber; and if more than one hair fiber is assessed, optionally determining an average value with respect to the assessed hair fibers.

[0025] Another embodiment of the present invention provides a method of quantitatively assessing the degree of split-end hair fiber repair, the method comprising obtaining a tress of hair; producing at least one hair fiber of the tress to have a spilt-end; removing at least one hair fiber having a split-end from the tress; optionally marking the at least one hair fiber; capturing a first image of the split-end of the at least one hair fiber and storing a

representation, e.g., an electronic representation, of the image; associating the hair fiber with the tress from which the hair fiber was removed; treating the tress and the hair fiber with a composition, wherein the composition comprises a hair care composition comprising a polyelectrolyte complex of a cationic polymer and an anionic polymer, wherein the viscosity of the composition is greater than 3000 cps; removing the hair fiber from the treated tress; capturing a second image of the end of the hair fiber removed from the treated tress, ;

assigning a value of 0 for no repair of the split-end, ½ for partial repair, or 1 for complete repair with respect to the hair fiber to assess the degree of split-end repair of the hair fiber; and if more than one hair fiber is assessed, optionally determining an average value with respect to the assessed hair fibers.

[0026] Another embodiment of the present invention provides a method of quantitatively assessing the degree of split-end hair fiber repair, the method comprising obtaining a tress of hair; producing at least one hair fiber of the tress to have a spilt-end; removing at least one hair fiber having a split-end from the tress; optionally marking the at least one hair fiber; capturing a first image of the split-end of the at least one hair fiber and storing a

representation, e.g., an electronic representation, of the image; associating the hair fiber with the tress from which the hair fiber was removed; treating the tress and the hair fiber with a composition, wherein the composition comprises a hair care composition comprising a polyelectrolyte complex of a cationic polymer and an anionic polymer in the form of an emulsion with improved freeze-thaw stability relative to comparative compositions containing such polyelectrolyte complexes; removing the hair fiber from the treated tress; capturing a second image of the end of the hair fiber removed from the treated tress;

BRIEF DESCRIPTION OF THE DRAWINGS

[0027] Figure 1 is a bar graph that shows percent mending determined using a method of the present invention with rinse-off conditioners in three cycles. Numbers in parentheses are percent polyelectrolyte complex (PEC). The number of fibers tested for the various compositions were 20, 100, and/or 50. [0028] Figure 2 is a bar graph that shows percent mending determined using a method of the present invention with leave-in compositions in one treatment. Twenty fibers were tested for each composition.

[0029] Figure 3 is a drawing showing the mending of a split-end using polyelectrolyte complexes (PECs). The drawing shows a possible mechanism of split-end repair by PECs:

PECs attach to the site of the split-end, form a network with themselves and the fiber assembly, and shrink as they dry, binding the split end from within.

[0030] Figures 4A-4D show still photography of the mending of a variety of split-end types.

[0031] Figure 5 shows still photography taken from video of the mending of split-ends during the process of mending.

[0032] Figure 6 is a schematic diagram of an image data capture system in accordance with an embodiment of the invention.

[0033] Figure 7 shows a line graph comparing high humidity curl retention of exemplary compositions of the present invention.

[0034] Figure 8 shows thermal protection of hair using exemplary compositions of the present invention.

[0035] Figures 9-19 show freeze/thaw comparisons of compositions described herein.

[0036] Figure 20 shows split-ends mended by exemplary compositions of the present invention.

DETAILED DESCRIPTION OF THE INVENTION

[0037] The present invention is predicated on the surprising and unexpected discovery of stable compositions containing polyelectrolyte complexes (PECs) and other hair benefit agents, particularly charged species, wherein the PECs remain intact and exhibit hair repair efficacy. It was unexpectedly found that the PECs can be combined with other charged hair benefit agents, i.e., substances that have beneficial properties for hair or that impart beneficial properties to hair, such as, e.g., cationic conditioning agents, without disrupting the complex that defines the PEC structure. Due to this unexpected discovery, the present invention provides compositions that not only provide the hair mending effect of PECs but also provides the advantages of other hair benefit agents. Thus, the present invention provides compositions and methods that include, e.g., charged hair benefit agents, e.g., quaternary ammonium salts, cationic conditioning polymers, and the like. Suitable hair benefit agents that can be combined with PECs in accordance with the present invention include, for example, stearamidopropyl dimethylamine, cocamidopropyl betaine, polyquaternium-37, polyquaternium-7, polyquaternium-39, DC 5-71 13 (silicone quaternium- 16 and undeceth-1 1 and butyloctanol and undeceth-5), Abil^® T Quat 60 (silicone quaternium-22), quaternium-80, Merquat^® 2001 (polyquaternium ^"47), and acrylic acid/VP crosspolymer. Other suitable charged hair benefit agents are described herein.

[0038] The present invention also provides a one-container process for producing a PEC. The process of the present invention also allows for the production of PECs of the same particle size distribution as those prepared using conventional processes requiring two or more separate containers. Thus, the present invention provides a more efficient and cost effective process for manufacturing PECs and hair care compositions containing PECs.

[0039] The present invention also allows for concentrations of PECs greater than 4 wt. %, e.g., 8 wt. %.

[0040] Additionally, the present invention has the advantage of providing methods that can graphically demonstrate the benefits of a hair care composition such that the benefits can then be effectively communicated to consumers. Consumers purchase hair care products based on the properties of the hair care products. Effectively communicating to these consumers the beneficial properties of a hair care product composition, then, is very important so that the consumers can make informed purchasing decisions when comparing competing hair care products.

[0041] The present invention further has the advantage of providing a test method that allows for showing improved results of split-end mending of a hair care composition such that the benefits of the hair care composition can then be effectively communicated to consumers. Most split-end mending test methods use virgin hair where the split-ends are mechanically induced. It is likely that virgin hair is used in order for the ingredients of a split-end mending composition to act solely on the mechanically induced damage. In other words, in virgin hair, there is no other damage to the hair besides the split-ends. Therefore, the mending composition directs its mending capabilities only to the split-end damage. The mending ingredients of such a composition, then, would not be wasted on other parts of the hair. However, it has been unexpectedly found that the use of hair with additional damage, e.g., due to bleaching, can be used instead of virgin hair in a split-end mending test method. This is counterintuitive since it would be expected that any mending composition would have its mending ingredients attracted to other damage of the hair and not just the split-ends, reducing the amount of split-end repair. It has been found by Applicants that the more damaged the hair, the better the mending of split-ends. Further, it has been found that, using more damaged hair, a high mending percentage can be achieved in a rinse-out product, e.g., greater than 50%, a level achievable with leave-in products. In one aspect, the present invention provides a hair care composition comprising a polyelectrolyte complex of a cationic polymer and an anionic polymer in the form of an emulsion with improved freeze- thaw stability relative to comparative compositions, e.g., made by formulating the PECs described in U.S. Patent Application Publication Nos. 2005/0089494 and 2006/0251603 in conventional hair care base formulations. In an embodiment, the composition comprises, e.g., from about 1% to about 5% of a thickening agent, about 10% or greater of propylene glycol, and about 5% or greater of an emollient, wherein the percentages are based on the total weight of the composition. In another embodiment, the composition comprises from about 3% to about 5% of a thickening agent, and about 2% or less of an emollient, wherein the percentages are based on the total weight of the composition.

[0042] The compositions of the present invention provide unexpected freeze-thaw stability. Freeze-thaw stability is an important property of hair care compositions particularly for purposes of transport and storage which often exposes the compositions to low

temperature extremes. Freeze-thaw stability is also important for products which remain on the hair and are thus exposed to temperature extremes outdoors. A composition containing PECs is not inherently unstable under freeze/thaw conditions. However, when combined with one or more fatty alcohols (e.g., cetyl, stearyl, etc.), which have been used in the art to thicken conditioner compositions, at e.g., about 3 wt. % or higher (e.g., about 5 wt. %), the formulation will be unstable during freeze/thaw. The composition will get grainy and chunky, which is unsatisfactory to a consumer, and will likely be rejected by the consumer.

[0043] In addition to freeze/thaw instability, conventional compositions with PECs that contain about 5% fatty alcohol do not have long term high temperature stability. The viscosity of such a composition continues to increase over time (e.g., over 100,000 cps after 2-3 months at 45 °C), which is unsatisfactory to a consumer since it will be too thick and hard to spread throughout the hair, and will likely be rejected by the consumer. The present inventors have found that the addition of Salcare improves viscosity control; that is, viscosity is controlled to stay within, e.g., about 20,000-40,000 cps.

[0044] The compositions and methods of the present invention can include a thickening agent. Thickening agents add viscosity to a composition such that a composition with a greater amount of a given thickening agent has a higher viscosity. The thickening agent can be, for example a quaternary ammonium nitrogen compound or polymer, for example polyquaternium-37, and for example where polyquaternium-37 is in a mixture with propylene glycol dicaprylate/dicaprate and polypropylene glycol-1 trideceth-6. Salcare^® SC 96 from Ciba^®/BASF, Basel, Switzerland is an example of such a mixture. Salcare^® SC 96 is 65% polyquaternium-37, 25% propylene glycol dicaprylate/dicaprate, 10% PPG-1 trideceth-6. Other suitable thickening agents also can be added to the compositions of the present invention including, for example, xanthan gum, acrylic acid/VP crosspolymer (e.g.,

Ultrathix™ P-100; ISP, Wayne, NJ, USA), PVP, PVP K-90, PEG-90M, and styrene/VP copolymer.

[0045] In another aspect, the present invention provides a hair care composition comprising a polyelectrolyte complex of a cationic polymer and an anionic polymer, wherein the viscosity of the composition is greater than 3000 cps. In an embodiment, such a composition can include, e.g., from about 1 % to about 5% of a thickening agent, about 10% or greater of propylene glycol, and about 5% or greater of an emollient, wherein the percentages are based on the total weight of the composition. In another embodiment, such a composition can include, e.g., from about 3% to about 5% of a thickening agent, and about 2% or less of an emollient, wherein the percentages are based on the total weight of the composition.

[0046] The viscosity of the compositions of the present invention can be varied based on the amount of thickening agent and/or other ingredients added. The compositions of the present invention may comprise thickening agents in a concentration of from about 1 wt. % to about 10 wt. %. The thickening agent may be present in an amount in wt. %, e.g., as listed in the table below. In the table, an "X" represents the range "from [corresponding value in first row] to [corresponding value in first column]." For example, the first "X" is the range "from about 1 wt.% to about 2 wt.%." [0047] Table 1

Thus, the viscosity can have a range between any aforementioned endpoints.

[0048] The viscosity of the compositions of the present invention can range, e.g., from about 3000 cps to about 100,000 cps, or, e.g., from about 20,000 cps to about 40,000 cps, as measured by RV T-B, 10 rpm, 1 min, at 25 °C for viscosities under 50,000 cps or RV T-C, 5 rpm, 1 min, at 25 °C for viscosities above 50,000 cps, but below 100,000 cps. The viscosity of the compositions of the present invention can range, e.g., as listed in the table below. In the table, an "X" represents the range "from [corresponding value in first row] to

[corresponding value in first column]." For example, the first "X" is the range "from about 3000 cps to about 10,000 cps."

[0049] Table 2

Thus, the viscosity can have a range bounded by any two of the aforementioned endpoints.

[0050] In one aspect of the invention, the composition contains a thickening agent, propylene glycol, and a relatively high concentration of an emollient, e.g., in an amount of 5 wt. % or greater. Suitable emollients can include, e.g., one or more fatty alcohols.

Consumers may find hair care products containing 10 wt. % or more of propylene glycol to be unacceptable in that they may think such products would be heavy or sticky feeling, may notice hair taking too long to dry (due to the humectant properties of glycols), or may notice hair is hard to comb or is not shiny. Surprisingly, however, it was found that including propylene glycol at 10% or greater in accordance with the present invention not only provided acceptable freeze-thaw stability but also may provide a composition that is more likely to be found acceptable by consumers. Additionally, Applicants have found that an emulsion in such compositions can accept a high level of glycol and not be affected (e.g., viscosity change, etc.). Applicants found that other polyhydric alcohols such as sorbitol and glycerin at 5 wt. %, did not provide for acceptable freeze-thaw stability.

[0051] In some embodiments, the compositions and methods of the present invention may include propylene glycol, e.g., in concentrations of about 10 wt. % or greater, about 20 wt. % or greater, about 30 wt. % or greater, about 40 wt. % or greater, or about 50 wt. % or greater.

[0052] The present invention also provides a hair care composition comprising a polyelectrolyte complex of a cationic polymer and an anionic polymer; from about 1 % to about 5% of a thickening agent; about 10% or greater of propylene glycol; and about 5% or greater of an emollient; wherein the percentages are based on the total weight of the composition.

[0053] In another aspect, the present invention provides a hair care composition that includes a polyelectrolyte complex of a cationic polymer and an anionic polymer, in combination with from about 3% to about 5% of a thickening agent, and about 2% or less of an emollient, wherein the percentages are based on the total weight of the composition. In this aspect, the composition of the present invention is preferably substantially free of propylene glycol. As used herein, "substantially free of propylene glycol" means that the composition of the present invention contains less than about 1 wt. % propylene glycol, less than about 0.5 wt. % propylene glycol, less than about 0.1 wt. % propylene glycol, and more preferably 0 wt. % or no propylene glycol.

[0054] The compositions and methods of the present invention can include the presence of one or more emollients. Emollients can, e.g., soften and/or soothe skin. Suitable emollients can include, for example, fatty alcohols. Fatty alcohols include, e.g., cetyl alcohol, stearyl alcohol, and combinations thereof. Fatty alcohols can sometimes be used to thicken compositions as well as provide emollient properties. Applicants have surprisingly found that compositions of the present invention, e.g., 5% fatty alcohol/1% Salcare^® SC 96 and 1 % fatty alcohol/5% Salcare^® SC 96, exhibit roughly the same emulsion properties {e.g., viscosity, rheology, yield value, appearance, color). This was unexpected at cetyl alcohol concentrations down to only about 1 wt. %. Furthermore, it has been found that the emollient concentration can be reduced to about 1 wt. % or less in a composition with 2 wt. % PECs where the composition also has from about 3 wt. % to about 5 wt. % of a thickening agent. The wt. % range of fatty alcohols can be expanded when the concentration of PECs is lower. Even with a low concentration of emollient fatty alcohols, PEC compositions have been found to still provide an acceptable sensory experience. This is unexpected in that most hair care compositions, especially conditioners, have higher concentrations of emollient fatty alcohols to provide a sensory experience for the consumer. Also, coupled with the thickening agent, the PEC composition retains an acceptable viscosity. Additionally, the combination of a low concentration of emollient fatty alcohol and PECs with from about 3 wt. % to about 5 wt. % thickening agent provides for a rich, white opacity not observed with any of these ingredients individually.

[0055] The concentration of the emollient in the compositions of the present invention desirably can be tailored based on the concentration of thickening agent. With the thickening agent at 3-5 wt. %, For example, the emollient concentration can range, e.g., as listed in the table below. In the table, an "X" represents the range "from [corresponding value in first row] to [corresponding value in first column]." For example, the first "X" is the range "from about 0 wt.% to about 0.1 wt.%."

[0056] Table 3

Thus, the concentration of emollient can have a range bounded by any two of the

aforementioned endpoints. Alternatively, with the thickening agent at 1-5 wt. %, for example, the emollient concentration can be, e.g., from about 5 wt. % or greater, about 6 wt. % or greater, about 7 wt. % or greater, about 8 wt. % or greater, about 9 wt. % or greater, about 10 wt. % or greater, about 20 wt. % or greater, about 30 wt. % or greater, about 40 wt. % or greater, or about 50 wt. % or greater.

[0057] Some PECs are described in U.S. Patent Application Publication Nos.

2005/0089494 and 2006/0251603, both of which are incorporated herein by reference in their entireties. As outlined in these publications, the formation of PECs is not simply due to the presence of oppositely charged polymers in a composition. A phase diagram may be produced to show the polymer-polymer species present when concentrations of the oppositely charged polymers are varied (thus varying the ratios of the polymers to each other). Based on the phase diagram, the ratio of polymers in terms of weight percent, moles, etc. at which PECs are formed can be determined. For PVMMA/polyquat-28 PECs, a preferred weight ratio is 1 :9 PVMMA:polyquat-28. However, PECs may exist at other weight percent ratios. For example, PVMMA/polyquat-28 PECs can be formed around the 1 :9 weight percent ratio, such that a ratio slightly higher or lower than 1 :9 will have some amount of PECs present. The weight percent ratio can range from about 1 :8 to about 1 :10 PVMMA:polyquat-28. Thus, the cationic polymer and anionic polymer in the compositions of the present invention, and used in the methods of the present invention, can be in the weight ratio of actives from about 1 :8 to about 1 : 10.

[0058] In addition to weight percent ratios, the formation of PECs may be determined based on the charge-charge ratio of polymers. PECs are usually formed when the charge- charge ratio of the polymers is 1 :1. Therefore, PECs are likely to form when, e.g., each negative charge of a polymer is balanced by a positive charge of another polymer. However, PECs may exist at other charge-charge ratios. For example, PECs can be formed around the 1 :1 charge-charge ratio, such that a ratio slightly higher or lower than 1 : 1 will have at least some amount of PECs present, for example at ratios such as 0.82 to 1.8 cationic to anionic charge. A phase diagram can be produced to determine the presence of PECs at varying charge-charge ratios.

[0059] Contemplated herein are PECs formed between polymers comprising cationic charges and polymers comprising anionic charges. However, phase diagrams may be constructed to determine the suitability of PEC formation for any polymer-polymer system, so long as the polymers interact through ionic bonds. The compositions and methods of the present invention may include a polyelectrolyte complex wherein a cationic polymer comprises one or more monomelic units with one or more quaternary ammonium nitrogen moieties, for example, vinylpyrrolidone/methacrylamidopropyl trimethylammonium chloride copolymer (polyquaternium-28). Non-limiting examples of other cationic polymers that may be used in forming PECs include other polyquat polymers such as polyquaternium-7, polyquaternium-10, or polyquaternium-1 1. The compositions and methods of the present invention may include a polyelectrolyte complex wherein an anionic polymer comprises monomelic units having ionizable carboxylic acid moieties, for example, a

methylvinylether/maleic acid copolymer. Another example of an anionic polymer that may be used in forming PECs is vinylpyrrolidone/acrylates/lauryl methacrylate copolymer.

[0060] Polymers with ionizable groups, such as carboxylic acid groups or tertiary amine groups, may require the adjustment of the pH in order for a polyelectrolyte complex to form. Adjustment of the pH alters the percent of ionizable groups that are ionized and thus adjusts the number of groups that may interact through ionic bonds. Production of phase diagrams at varying pHs can be used to determine the proper pH for PEC formation. For

PVMMA/polyquat-28 PECs, a pH range of from about 6.5 to about 7.5 may be used for PEC formation. The suitable pH can range, e.g., as listed in the table below. In the table, an "X" represents the range "from [corresponding value in first row] to [corresponding value in first column]." For example, the first "X" is the range "from about pH 6.5 to about pH 6.6."

[0061] Table 4

Thus, the pH can have a range bounded by any two of the aforementioned endpoints.

[0062] The pH of a composition may be adjusted using neutralizing/buffering agents. For acidic groups such as carboxylic acid, a basic neutralizer can be used, such as a hydroxide compound. Suitable hydroxide compounds include strong bases such as sodium hydroxide. For basic groups, an acidic neutralizer can be used, such as citric acid. Any suitable concentration of neutralizer can be used, including, e.g., those listed in the table below. In the table, an "X" represents the range "from [corresponding value in first row] to [corresponding value in first column]." For example, the first "X" is the range "from about 0.1 wt.% to about 1 wt.%."

[0063] Table 5

Thus, the concentration of neutralizer can have a range bounded by any two of the aforementioned endpoints. So long as the PECs have formed under desired pH conditions, the final pH of any resulting composition comprising the PECs may be the same or different from the pH at which the PECs were formed, so long as the PECs remain intact.

[0064] The PVMMA/polyquat-28 PECs have the ability to mend split-ends of hair fibers. Hair has a net negative charge. Without being bound to any particular theory, PECs are believed to be substantive to the hair fiber and adhere the ends of a split-end together through adhesive properties. The positive charges of the polyquat-28 polymer are attracted to the negatively charged hair fibers and are substantive to the hair. Since the negatively charged PVMMA polymer is complexed to the polyquat-28, the PVMMA also is drawn to the hair. The ends of the split-end are then adhered together through the adhesive action of multiple PECs interacting with the ends of the split-end and/or each other (e.g., in film-formation where the film contracts while drying). Additionally, the surface tension experienced by the ends of the split-end due to the interaction of water during film-formation assists in adhering the ends together.

[0065] To the extent that the PECs exist in the form of suspended or emulsified particles, the particle size of PECs should allow the PECs access to the ends of a spilt-end in order for the PECs to mend damaged hair fibers. As long as the PECs have access to the ends of a split-end, the particle size distribution can have any suitable average PEC particle size.

Suitable average PEC particle sizes can include, e.g., those listed in the table below. In the table, an "X" represents the range "from [corresponding value in first row] to [corresponding value in first column]." For example, the first "X" is the range "from about 0.5 μπι to about 1 μιη."

[0066] Table 6

Thus, the average PEC particle size distribution can have a range bounded by any two of the aforementioned endpoints. In some embodiments, the compositions and methods of the present invention includea PEC particle distribution with an average PEC particle size of about 5 micrometers, e.g., of about 5 ± 3 micrometers or about 5 ± 2 micrometers. The compositions and methods of the present invention also can include PEC particles that exist within a microgel, e.g., an interlocking microgel structure.

[0067] The compositions and methods of the present invention can incorporate PECs at higher concentrations than previously recognized as achievable in the art. For instance, the compositions of the present invention can include PECs of PVMMA/polyquat-28 at a concentration of 8 wt. %. The concentration of PECs in a hair care composition may be varied. The compositions and methods of the present invention may contain the

polyelectrolyte complex in a concentration of from about 1 % to about 8% based on the total weight of the composition. The compositions of the present invention may contain the polyelectrolyte complex in a concentration of from about 1% to about 3% or from about 2% to about 4% based on the total weight of the composition. The concentration of PECs may be, e.g., as listed in the table below. In the table, an "X" represents the range "from

[corresponding value in first row] to [corresponding value in first column]." For example, the first "X" is the range "from about 0.1% to about 0.5%." [0068] Table 7

Thus, the concentration of PECs can have a range bounded by any two of the aforementioned endpoints.

[0069] PEC formation may be confirmed using any suitable method. An example of a suitable method includes microscopy. Under a light microscope, the structure of a polymer- polymer system can be investigated, and the sizes of any particles present can be determined using sizing software. Such a method can yield the particle size distribution of PECs, provided the presence of other ingredients does not obscure the PEC structure. Another method includes determining the particle size distribution using a Malvern particle size analyzer. Also, the physical properties of a composition of only PECs in a carrier solvent can indicate the presence of the PECs. For example, as the presence of PECs increases, such a composition increases in haziness and opacity. Also, the viscosity of such a composition decreases to a minimum that corresponds to the presence of the greatest amount of PECs for a given polymer-polymer system, where the PECs are the most compact.

[0070] The compositions of the present invention may be in the form of, and the methods of the present invention can produce or use compositions in the form of, e.g., shampoos, conditioners, gels, rinses, emulsions (oil-in- water, water-in-oil or multiphase), lotions, creams, cremes, ointments, pomades, sprays (pressurized or non-pressurized), spritzes, mousses, foams, shampoos, solutions, and solids {e.g., as sticks, semisolids and the like). Thus, the compositions of the present invention may be in the form of, and the methods of the present invention can produce or use compositions in the form of, e.g., a cream, a lotion, a solution, an ointment, or a gel. Thus, the hair care compositions and methods of the present invention can include other components that may be suitable for use in these types of compositions. Preferably such components are compatible with PECs, in that the

components do not disrupt PEC structure.

[0071] Compositions can be meant for rinse-out, leave-in, and/or overnight treatments. The methods and hair care compositions of the present invention may include mixing a polyelectrolyte complex with one or more components selected from aqueous carriers, surfactants, neutralizers, fragrances, conditioning agents, emulsifiers, thickening agents, preservatives, gelling agents, silicones, hair fixatives, humectants and moisturizers to form a hair care composition. Thus, the compositions and methods of the present invention can include, e.g., a preservative, a neutralizer, a fragrance, a silicone, or a combination thereof. One of ordinary skill in the art would recognize that the ingredients identified herein may have multiple properties and thus may fit within multiple ingredient categories, especially if it is a commercially available product with multiple components.

[0072] The aqueous carrier can include any suitable quantity of water, e.g., from about 25 wt% to about 97 wt% water (e.g., from about 30% to about 95% water). The composition of the present invention can include from about 30 wt. % to about 97 wt. % water, from about 50 wt. % to about 80 wt. % water, or from about 60 wt. % to about 70 wt. % water. The water used in the composition of the present invention can be deionized water.

[0073] Suitable emulsifiers can include, for example, PPG-3 benzyl ether myristate {e.g., Crodamol STS; Croda, Inc., Edison, NJ, USA), arachidyl alcohol and behenyl alcohol and arachidyl glucoside {e.g., Montanov^® 202; SEPPIC, Paris, France), polyacrylamide and CI 3- 14 isoparaffm and laureth-7 {e.g., Sepigel™ 305; SEPPIC), glyceryl stearate, isoceteth-20, oleth-2, methoxy PEG/PPG-7/3 aminopropyl dimethicone, PEG/PPG-18/18 Dimethicone {e.g., DC- 190; Dow Corning), PEG- 12 dimethicone, PEG-40 hydrogenated castor oil, PEG-6 caprylic/capric triglyceride, aminomethyl propanol (AMP-95), and polyglyceryl-3 distearate.

[0074] Suitable surfactants, e.g., detersive and/or cleansing surfactants, may be used, including, for example, disodium laureth sulfosuccinate, sodium laureth sulfate, polysorbate 20, polysorbate 60, cocamidopropyl betaine, and stearalkonium chloride. Such surfactants may be present in a shampoo composition. A conditioner preferably is substantially free of detersive surfactants, unless the conditioner is a two-in-one combination of a shampoo and conditioner. As used herein, "substantially free of detersive surfactants" means that the composition of the present invention contains less than about 2 wt. % detersive surfactants and more preferably less than about 1 wt. %, e.g., 0 wt. % or no detersive surfactants.

[0075] Suitable conditioning agents can include, for example, tertiary or quaternary amines such as stearamidopropyl dimethylamine, polyquaternium-47 {e.g., Merquat^® 2001 ; Nalco, Naperville, IL, USA), silicone quaternium-22 {e.g., Abil^® T Quat 60; Evonik, Essen, Germany), cocamidopropyl betaine, polyquateraium-1 1 , polyquaternium-39,

polyquaternium-4 (Celquat^® H-100; Akzo Nobel, Amsterdam, Netherlands), polyquaternium- 4 (Celquat^® L-200; Akzo Nobel) to 0.5 wt. %, polyquaternium-7, polyquaternium 10, and quaternium-80. Other suitable conditioning agents include, e.g., Aqu D 4272 N-Hance SPlOO (Acrylamidopropyltrimonium Chloride/Acrylamide Copolymer), Distearoyl ethyl Dimonium Chloride; Cetearyl Alcohol (Varisoft EQ 65), Rhodia Guar S, Behenyltrimethyl Ammonium Chloride, and Behentimonium Chloride/Cetearyl Alcohol. The N-Hance SPlOO copolymer has been found to be especially beneficial. Thus, the compositions and methods of the present invention can include, e.g., acrylamidopropyltrimonium chloride/acryl amide copolymer. As is shown in Example 16 below, this copolymer provides additional split-end mending in a composition that contains PECs.

[0076] Although not essential, an effective amount of at least one preservative may be incorporated in the composition. For example, the preservative can be selected to kill bacteria that might otherwise be sustained or multiply in the composition. Suitable preservatives can include, for example, DMDM hydantoin, disodium EDTA, Kathon™ CG (actives: 5-chloro-2-methyl-4-isothiazolin-3-one and 2-methyl-4-isothiazolin-3-one) and the like, and combinations thereof.

[0077] Suitable gelling agents can be used. Suitable gelling agents can include, for example, acrylic acid/VP crosspolymer {e.g., Ultrathix™ P-100; ISP).

[0078] Suitable silicones can be added, e.g., to improve conditioning of hair. Suitable silicones can include, for example, polysiloxanes, including dimethicone, dimethiconol, cyclopentasiloxane, and cyclohexasiloxane. These include, e.g., phenyl trimethicone, Abil^® OSW 5 (84% Cyclopentasiloxane, 15% Dimethiconol, 1 % Dimethicone; Evonik, Essen, Germany), DC-200 (dimethicone; Dow Corning, Midland, MI, USA), Fluid Blend (80% cyclomethicone, 20% dimethicone), and DC- 1501 (D5/Dimethiconol; Dow Corning). Other suitable silicones include, for example, DC-556 (phenyl trimethicone; Dow Corning), and amino functional silicones, for example, DC-949 (31 % amodimethicone, 1.9% trideceth-12, 2.2% cetrimonium chloride, 55-60%) water, 2.2% cyclotetrasiloxane, 1.6%

cyclopentasiloxane, and <0.5% sodium benzoate; Dow Coming), DC-8500 (82% Bis(C13-15 Alkoxy) PG-Amodimethicone, 18% C14-15 Alcohols; Dow Corning), aminopropyl dimethicone, DC 5-71 13 Silicone Quat Microemulsion (66% Water, 25% Silicone

Quaternium-16, 7.4% Undeceth-1 1 , 4.5% Butyloctanol, 3.5% Undeceth-5; Dow Corning), DC 2-8566 (amodimethicone; Dow Corning), and amodimethicone (ADM 1 100; Wacker).

[0079] Suitable hair fixative may be used. Suitable examples include, for example VP/methacryl amide/vinyl imidazole Copolymer (e.g., LUVISET® Clear; BASF), acrylic acid/vinylpyrrolidone crosspolymer (e.g., Ultrathix™ P-100; ISP), vinyl

caprolactum/VP/dimethylaminoethyl methacrylate copolymer (Advantage® S; ISP), and VP/VA Copolymer.

[0080] Additional ingredients may be added, including, for example, Cocos nucifera (coconut) oil, mineral oil (paraffinum liquidum), sodium chloride, hydrolyzed silk, keratin amino acids, ascorbic acid, panthenol, tocopherol acetate, biotin, niacinamide,

triethanolamine, triticum vulgare (wheat) flour lipids, ceramide 3, persea gratissima

(avocado) oil, tetrahexyldecyl ascorbate, glycine soja (soybean) sterols, alpha-glucan oligosaccharide, ethylhexyl methoxycinnamate, butyl methoxydibenzoylmethane, and tocopheryl acetate. A propellant may be used, such as in a spray composition, including isobutane and propane and 152A (78.5% A46; 28.5% HFC 152A). Fatty acids can be used, such as myristic acid, palmitic acid, and stearic acid.

[0081] Additional components and/or ingredients can be provided to impart beneficial properties to the hair, e.g., components and/or ingredients for imparting softness to the hair after drying, providing moisturization to the hair, providing pleasing consistency/viscosity of the composition, and providing volume/fullness to the hair.

[0082] Fragrances can be provided in the compositions of the present invention. A non- limiting example of a fragrance is flower extract. Any particular fragrance can be used, and one of ordinary skill in the art would recognize that the particular identity of fragrance is not important. Indeed, the compositions of the present invention can be provided without fragrance.

[0083] An embodiment of a composition of the present invention can include, for example, 1 -2 wt. % PEC of PVMMA copolymer and polyquaternium-28 in a 1 :9 ratio. Such a complex can be manufactured in a side tank and added to the main batch tank after an emulsion phase is prepared and when the emulsion phase has cooled to 45-65 °C. A tertiary or quaternary amine at approximately 1 -2 wt. % can be included in the emulsion phase and neutralized to a pH of about 4.0-6.0. Fatty alcohol (e.g., cetyl and/or stearyl) can be included at approximately 3-7 wt. % in conjunction with a low-HLB co-emulsifier such as glyceryl monostearate, distearate, or the like, in a 5:1 ratio and can be included in the emulsion phase. Silicones at, e.g., 0.1-10 wt. %, or a blend of dimethicones, cylcomethi cones, phenyl and/or amino functional silicones also can be included. An emollient ester, such as PPG-3 benzyl ether myristate (e.g., Crodamol STS), at, e.g., 1-4 wt. % can be added to enhance product spreadability in addition to enhancing shine and hair feel. Propylene glycol at 10% can be included to improve freeze/thaw stability. Salcare^® SC-96 can also be included, which can be after the emulsion phase and when the batch has cooled to 45-65 °C, at, e.g., 0.1-5 wt. % to increase viscosity, improve conditioned feel in hair, and improve long term stability and viscosity control. Another embodiment of a composition of the present invention can include, for example, the same composition except with approximately 1 % fatty alcohol, no emollient ester, and Salcare^® SC 96 at, e.g., 1-7 wt. %. An embodiment of a composition with approximately 3-7 wt. % fatty alcohol can include PEC complex that has been made first in a main tank, with the rest of the composition then made in the same tank, where Salcare^® SC-96 has been increased to, e.g., 1-7 wt. %. An embodiment of a composition with approximately 1 wt. % fatty alcohol can include PEC complex that has been made first in a main tank, with the rest of the composition then made in the same tank, where Salcare^® SC- 96 has been increased to, e.g., 3-10 wt. %.

[0084] The present invention includes hair care compositions formed from any of the suitable ingredients described herein. In an embodiment, the present invention includes hair care compositions formed from polyquaternium-28 and methylvinylether/maleic acid copolymer; from about 1 % to about 5% of a thickening agent; about 10% or greater of propylene glycol; and about 5% or greater of an emollient; wherein the percentages are based on the total weight of the composition. In an embodiment, the present invention includes hair care compositions formed from polyquaternium-28 and methylvinylether/maleic acid copolymer; from about 3% to about 5% of a thickening agent; and about 2% or less of an emollient; wherein the percentages are based on the total weight of the composition. In an embodiment, the present invention includes hair care compositions formed from

polyquaternium-28 and methylvinylether/maleic acid copolymer, wherein the viscosity of the composition is greater than 3000 cps. In an embodiment, the present invention includes hair care compositions formed from polyquaternium-28 and methylvinylether/maleic acid copolymer in the form of an emulsion with improved freeze-thaw stability relative to comparative compositions containing such polyelectrolyte complexes. In an embodiment, the present invention includes hair care compositions formed from polyquaternium-28, methylvinylether/maleic acid copolymer, and polyvinylpyrrolidone.

[0085] The present invention also provides embodiments of hair care formulations and their method of use that do not: increase the force required to comb hair, as compared to untreated hair; increase the force required to separate the adhesion of two hair fibers, as compared to untreated hair; increase the "three point bending" force, as compared to untreated hair; increase Young's Modulus, as compared to untreated hair; reduce the luster/shine of hair, as compared to untreated hair; or impart other quantifiable "negative" attributes.

[0086] The compositions of the present invention may be used in any suitable method for treating hair. For example, compositions described herein may be used for conditioning a hair fiber by applying a composition to the hair fiber and rinsing the hair fiber with water. After rinsing, the hair fiber may be dried with a blow dryer, combed, and/or styled using styling products or compositions. Additionally, compositions described herein may be used to repair a split-end of a hair fiber by applying a composition to the split-end and rinsing the split-end with water. This method also may be followed by blow drying, combing, and/or styling. The compositions described herein further may be used in a method of thickening a hair fiber by applying to the hair fiber a composition of the present invention and rinsing the hair with water. In other embodiments, the compositions of the present invention can be used for hair styling, for example, when the compositions comprise a styling hair benefit agent. For example, the composition can be a styling spray (aerosol and non-aerosol). In other embodiments, the compositions of the present invention can be used for shampooing hair when formulated as a shampoo. Other styling products can include leave-in conditioners, overnight conditioning treatments, styling lotions/cremes/balms, styling gels, styling mousses, serums, oil treatments, glazes, and conditioning sprays (aerosol and non-aerosol).

[0087] The freeze-thaw stability of a hair care composition comprising a polyelectrolyte complex of a cationic polymer and an anionic polymer may be improved by adding to the hair care composition from about 1 % to about 5% of a thickening agent, wherein the percentage is based on the total weight of the composition. The thickening agent can comprise a quaternary ammonium nitrogen compound or polymer. The quaternary ammonium nitrogen compound or polymer can be, e.g., polyquaternium-37. The

polyquaternium-37 can be in a mixture with propylene glycol dicaprylate/dicaprate and polypropylene glycol- 1 trideceth-6. Alternatively, the freeze-thaw stability of a hair care composition comprising a polyelectrolyte complex of a cationic polymer and an anionic polymer may be improved by adding to the hair care composition from about 10% or greater of propylene glycol, wherein the percentage is based on the total weight of the composition.

[0088] The present invention provides for the thermal protection of hair. When a leave- on composition with PECs as described herein is applied to hair, the PECs protect the hair shaft from damage (e.g., fiber fragmentation) due to heat. The heat can be from any source, including, for example, a hair dryer, a flat iron, or a hot styling tool.

[0089] The methods of the present invention allow for the production of PECs in one container. Accordingly, one aspect of the present invention provides a method of producing a polyelectrolyte complex, the method comprising hydrating a methylvinylether/maleic acid copolymer having repeating units of the formula (Formula I)

in a container; reacting the methylvinylether/maleic acid copolymer with a base, such as, e.g.. sodium hydroxide, in the container in an amount sufficient to at least partially neutralize the acidic groups thereof, to form an intermediate mixture; heating the intermediate mixture in the container; adding to the intermediate mixture in the container a cationic copolymer of a vinylpyrrolidone of the formula (Formula II)

; and mixing the polymers in the container at high shear force and at a temperature of at least about 50-60 °C to produce the polyelectrolyte complex.

[0090] Additionally, another aspect of the present invention allows for production of a hair care composition by combining the PECs produced in accordance with the present invention with other hair benefit agents. In accordance with the process of the present invention, such hair care compositions can be prepared by combining the PECs produced in accordance with the present invention with other hair benefit agents in a single container. Accordingly, the present invention also provides a method of producing a hair care composition comprising producing a polyelectrolyte complex, comprising the steps of hydrating a methylvinylether/maleic acid copolymer having repeating units of the formula I in a container; reacting the methylvinylether/maleic acid copolymer with a base, such as, e.g., sodium hydroxide (e.g., a 20% sodium hydroxide solution, e.g., in water), in the container in an amount sufficient to at least partially neutralize the acidic groups thereof (e.g., by adding sufficient base to achieve a pH of from about 6.5 to about 7.5 or from about 6.9 to about 7.0), to form an intermediate mixture; heating the intermediate mixture in the container, e.g., to a temperature of from about 50 °C to about 60 °C; adding to the intermediate mixture in the container a cationic copolymer of a vinylpyrrolidone of the formula II and a

methacrylamidopropyl trimethylammonium chloride of the formula III; mixing the polymers in the container at high shear force, e.g., at a temperature of about 50-60 °C to produce the polyelectrolyte complex. The process of the present invention optionally includes further adding to the polyelectrolyte complex in the container one or more additional components selected from aqueous carriers, surfactants, fragrances, conditioning agents, emollients, emulsifiers, thickening agents, preservatives, gelling agents, silicones, hair fixatives, humectants and moisturizers; and mixing the resulting composition in the container.

[0091] The present invention also allows for producing a hair care composition in two containers, the PECs being produced in one container and the rest of the composition being produced in a second container, where the PECs and other ingredients are then combined. In this aspect, the present invention also provides a method of producing a hair care composition comprising producing a polyelectrolyte complex between a methylvinylether/maleic acid copolymer and a cationic copolymer of a vinylpyrrolidone and a methacrylamidopropyl trimethylammonium chloride, comprising the steps of hydrating a methylvinylether/maleic acid copolymer having repeating units of the formula I in a first container; reacting the methylvinylether/maleic acid copolymer with a base, such as, e.g., sodium hydroxide, in the first container in an amount sufficient to at least partially neutralize the acidic groups thereof, to form an intermediate mixture; heating the intermediate mixture in the first container;

adding to the intermediate mixture in the first container a cationic copolymer of a

vinylpyrrolidone of the formula II and a methacrylamidopropyl trimethyl ammonium chloride of the formula III; mixing the polymers in the first container at high shear force and at a temperature of at least about 50-60 °C to produce the polyelectrolyte complex; mixing in a second container one or more components selected from aqueous carriers, surfactants, fragrances, conditioning agents, emollients, emulsifiers, thickening agents, preservatives, gelling agents, silicones, hair fixatives, humectants and moisturizers; and mixing together in the first or second container the polyelectrolyte complex of the first container and the mixed components of the second container.

[0092] Phase diagrams, as indicated above, can be produced to determine the conditions under which PECs form, including within which polymer:polymer weight ratios and charge- charge ratios. Additional conditions may be varied as well, including temperature, solvent system, etc. Each of these conditions may be varied to determine their effects on PEC formation. Thus, due to the various conditions required to produce PECs and the vast number of variables involved, the production of PECs can be complicated and difficult. This is especially the case when a particular particle size is desired, as in producing

PVMMA/polyquat-28 PECs that can mend split-end damaged hair. In addition to the polymenpolymer weight ratios and/or charge-charge ratios, etc., the particular production method used also may impact the average particle size distribution of PECs. For example, the mixing speed and/or mixing time during the addition of one polymer to another, and the mixing speed and/or mixing time after this addition, can affect the PEC particle size distribution. Other process variables such as temperature, pH, and the presence of other charged compounds during the formation of PECs can also have an affect. The compositions of the present invention can be produced by methods that allow for production of PECs on a large scale where the proper particle size distribution for mending split-ends is achieved.

[0093] The formation of PECs may be facilitated by application of heat at a certain stage, e.g., when the anionic polymer is neutralized with a base and/or when the cationic polymer is added to the anionic polymer to produce the complex. A composition may be preheated prior to combining polymers, may be heated with one or a subset of polymers, or may be heated during or after combining all polymers for PEC formation. For PVMMA/polyquat-28 PECs, it has been found that heating neutralized PVMMA prior to addition of the polyquat-28 is advantageous, e.g., with the temperature ranging from at least 50 °C to 60 °C or greater. The temperature may range, e.g., as listed in the table below. In the table, an "X" represents the range "from [corresponding value in first row] to [corresponding value in first column]." For example, the first "X" is the range "from about 50 °C to about 51 °C."

[0094] Table 8

Thus, the temperature can have a range bounded by any two of the aforementioned endpoints.

[0095] The compositions of the present invention may be prepared in a single container or may be prepared in separate containers, e.g., by preparing the PECs separately from other components prior to combining the PECs with the other components. The methods described herein produce PECs of the same size, morphology, and stability as conventional methods, yet do so with reduced numbers of containers.

[0096] The step of adding a cationic polymer to the intermediate mixture can include adding a solution, e.g., an aqueous solution, of the cationic polymer to the intermediate mixture. The cationic polymer can be added to the intermediate mixture at any suitable rate, which can include, e.g., from about 0.3 kg/min per minute to about 1.0 kg/min per minute (e.g., if the period of addition is 10 minutes, the rates would be from about 3 kg/min to about 10 kg/min) and can include, e.g., those listed in the table below. In the table, an "X" represents the range "from [corresponding value in first row] to [corresponding value in first column]." For example, the first "X" is the range "from about 0.3 kg/min per min to about 0.4 kg/min per min."

[0097] Table 9

Thus, the addition can have a range bounded by any two of the aforementioned endpoints.

[0098] The formation of PECs depends on the mixing speed and mixing duration when one polymer is added to another. A high shear force can be used for complete mixing.

However, depending on the polymer-polymer systems, the mixing speed may have to be adjusted for proper PEC formation. For PVMMA/polyquat-28 PECs, the polyquat-28 can be first mixed prior to addition of the PVMMA for, e.g., 5 minutes, 10 minutes, 20 minutes, 25 minutes, 30 minutes, 40 minutes, 50 minutes, or 60 minutes. The polyquat-28 can be added to the PVMMA over a period of, e.g., 5 minutes, 10 minutes, 20 minutes, 25 minutes, 30 minutes, 40 minutes, 50 minutes, or 60 minutes. The polyquat-28 can be added to the PVMMA over a period of 30 minutes. The rate of addition can be any suitable rate in which PECs are formed. The rate can be determined based on the time needed for the period of addition. For example, the rate can be based on the amount added per minute per minute of the period of addition. For PVMMA/polyquat-28 PECs, this can be from about 0.4 kg/min per minute to 1.0 kg/min per minute. Thus, if the period of addition is 10 minutes, the rates would be from about 4 kg/min to about 10 kg/min. After the addition of the polymer, mixing can occur for over a period of, e.g., 5 minutes, 10 minutes, 20 minutes, 25 minutes, 30 minutes, 40 minutes, 50 minutes, or 60 minutes. The mixing can include a combination of mixing before, during, and/or after addition of the polyquat-28. Thus, the intermediate mixture of PVMMA can be mixed for at least about 10 minutes prior to addition of the cationic polymer, at least about 10 minutes after addition of the cationic polymer, or a combination thereof.

[0099] Some embodiments of the compositions of the present invention include compositions with the formulations of PVMMA and polyquat-28 as in Table 10.

[0100] Table 10

[0101] The present invention provides for mixing in additional ingredients after PEC formation, wherein the mixing is sufficient to allow adequate incorporation of the one or more components.

[0102] The present invention provides a one-container process for producing a PEC, which is highly efficient, cost effective, and eliminates the additional time and labor required to transfer materials from one tank to another as is done in conventional PEC production processes. Accordingly the process of the present invention is particularly suitable for manufacturing PECs and hair care compositions containing PECs on a commercial scale, e.g., about 500 to about 10,000 gallons.

[0103] The process of the present invention further provides for the production of PEC compositions (e.g., at 8 wt. %) at concentrations that substantially exceed the concentration of PEC compositions which have been produced conventionally. Increasing the

concentration at which PECs are produced has several advantages. The higher concentration allows for a smaller pre-mix tank to be used in connection with combining the PECs with other ingredients to produce hair care products, e.g., conditioners. Also, PECs can be prepared and stored for future use, and less storage space is needed for a more concentrated stock. Furthermore, fewer quality control steps would be required in that one batch of PECs could be prepared and tested at a higher concentration instead of preparing multiple batches at lower concentrations, requiring additional testing. Additionally, if a PEC stock is used for preparing a hair care composition, the PEC stock will not require as much volume in a processing container, allowing for the addition of a greater volume of other ingredients and allowing for higher concentrations to be achieved for additional ingredients. For example, the Applicants have found for preparing PVMMA/polyquat-28 PECs, it is not necessary to dilute the polyquat-28 (e.g., Conditioneze NT-20 which is commercially available at a concentration of 20% actives). Rather, in accordance with the present invention,

PVMMA/polyquat-28 PECs can be prepared in a single container by directly adding

Conditioneze NT-20 at full strength to the PVMMA copolymer, which surprisingly produces a stable PEC at high concentration. Further, Applicants have found that the higher PEC concentration in the compositions produced in accordance with the present invention are substantially more likely than conventional PEC compositions of lower concentration to form stable emulsions with other ingredients used to produce hair care products such as, e.g., conditioners.

[0104] The present invention provides a method of graphically reconstructing the repair process in the mending of a split-end of a hair fiber. In one embodiment the method includes securing a hair fiber to a surface, wherein the hair fiber secured to the surface has a split-end or is damaged while on the surface to produce a split-end; associating the surface with a magnifying device, wherein the split-end is positioned within the field of view of the magnifying device; associating an image capture device with the magnifying device so as to capture an enlarged image of the field of view of the magnifying device; treating the spilt-end with a composition, wherein the composition repairs the split-end and wherein the split-end fuses together; and via the image capture device associated with the magnifying device, capturing an image of the repair of the split-end during treatment with the composition, and storing a representation of the captured image of the repair for subsequent retrieval. The method of graphically reconstructing hair mending in accordance with the present invention includes using video to record the hair mending process in real-time. Desirably the hair mending process is recorded using a video device adapted to record the reparation process, in real-time, at a magnification sufficient to visualize the reparation process with the naked eye, e.g., at 20-50X magnification. The video can be stored on a recording media, using methods that are well known to those of ordinary skill in the art, for subsequent retrieval.

[0105] Additionally, the methods of the present invention may include securing a hair fiber to a surface, wherein the hair fiber secured to the surface has a split-end or is damaged while on the surface to produce a split-end. The hair fiber, thus, may have a split-end prior to securing it to the surface, or a split-end can be induced (for example, by mechanical means) after the hair fiber is secured to the surface. The surface may be any surface that can be associated with a magnifying device. Such a surface can include, for example, a table top or a microscope slide. The properties of the surface can be determined by the type of magnifying device used. For example, if a light microscope is used wherein light is transmitted through a sample, a transparent surface, e.g. , a microscope slide, may be used. As another example, the surface may be a stage on which the hair fiber rests. As yet another example, if the magnifying device is a simple lens, such as a magnifying glass, the surface can be a table top. Nothing should interfere with the mending of the split-end. For example, cover slips for microscope slides should not be used if the slip would prevent the ends of the split-end from coming together.

[0106] The hair fiber can be secured by any suitable means, including, for example, using one or more clamps. The hair fiber can also be secured using tape, for example, when using a table top or a microscope slide. As long as the split of the hair fiber can be observed with the magnifying device, any suitable means may be used for securing (e.g., fastening) the hair fiber to the surface.

[0107] The methods of the present invention can include associating the surface with a magnifying device, wherein the split-end is positioned within the field of view of the magnifying device. The magnifying device may be, for example, a magnifying glass, a microscope (e.g., a light microscope). Each magnifying device has a field of view. "Field of view" means the image area that the magnifying devices magnifies for observation. The split-end is positioned within the field of view such that the split-end is magnified for observation.

[ 0108] The methods of the present invention can include associating an image capture device with the magnifying device so as to capture an enlarged image of the field of view of the magnifying device. The image capture device can be, for example, a digital recorder. The image capture device also can be analog. Non-limiting examples of image capture devices include still cameras, video cameras, charge-coupled device (CCD) cameras, digital cameras and/or camcorders, or any other similar recording device.

[0109] The methods of the present invention can include treating the spilt-end with a composition, wherein the composition repairs the split-end and wherein the split-end fuses together. Treatment may include, for example, massaging the composition into the hair. Treatment also may include, for example, rinsing the hair to remove the composition, such as with a rinse-off composition. The composition may be allowed to remain on the hair, for example, when using a leave-in composition. The method of treatment may be any suitable method, including methods described herein. The composition may be any suitable compositions, including compositions described herein.

[0110] The methods of the present invention can include a step where, via the image capture device associated with a magnifying device, capturing an image of the repair of the split-end during treatment with the composition, and storing a representation of the captured image of the repair for subsequent retrieval. The image capture device can capture the repair of the split-end using any suitable means. For example, if the image capture device is a digital recorder, the digital recorder may generate an electronic file. As another example, if the image capture device is a camera, the camera may capture the repair using photographic film.

[0111] Storage of a representation of a captured image of repair for subsequent retrieval may be through any suitable means. For example, this may include storing an electronic representation of the image, for example, using an electronic file accessible on a digital camera and/or computer. This may also be through the use of photographic film.

[0112] Furthermore, the present invention can be used for any method of communicating to consumers. These may include, for example, the use of still photographs {e.g., before and after photographs); diagrams, depictions, and/or drawings; computer animation; and/or in- vivolin-vitrolin-situ video using actual human hair fiber or analogues {e.g., sheep wool). Additionally, the methods of communication can be in print, on television, on the Internet, in- store, in-person {e.g., live demonstrations), and/or on social media. The methods of the present invention also can be used for the explanation of a binding mechanism {e.g., PECs shrinking to draw together two ends of a split-end).

[0113] The present invention also provides a method of quantitatively assessing the degree of split-end hair fiber repair, the method comprising obtaining a tress of hair, preferably twice-bleached hair; producing at least one spilt-end of a hair fiber in the tress {e.g., by combing and/or blow drying the tress sufficiently to produce split-ends); removing at least one hair fiber having a split-end from the tress; optionally marking the at least one removed hair fiber; capturing a first image of the split-end of the at least one removed hair fiber; associating the hair fiber with the tress from which the hair fiber was removed; treating the tress and the hair fiber with a composition; removing the hair fiber from the tress;

capturing a second image of the end of the hair fiber, wherein the end is the same end captured for the first image of the split-end of the at least one removed hair fiber; assigning a value of 0 for no repair of the split-end, ½ for partial repair, or 1 for complete repair; and summing the assigned numbers for all marked hair fibers and dividing the sum by the total number of marked hair fibers. Exemplary compositions of the present invention, when assessed according to this method can achieve an average value of, e.g., 0.85 or greater, e.g., 0.925, 0.95, and even 0.975 based on an assessment of 20 fibers.

[0114] The methods of the present invention can include producing split-ends. This may include combing and blow drying the tress of hair to produce at least one hair fiber of the tress having a spilt-end. Other methods include selecting split-ends naturally. For example, hair samples may be attained from live specimens wherein the hairs are already split. Due to variety, however, this method may cause data to have poor reproducibility.

[0115] The methods of the present invention can include marking at least one removed hair fiber of the tress of hair. The split-end can be marked right at the beginning of the split. If the mark is gone after treatment with the composition, this can indicate that the split-end broke off the hair fiber. When assigning a value to the fibers, then, this fiber can be excluded since the split-end neither remained as a split-end nor was repaired. Thus, e.g., false positives can be avoided when assessing the mending ability of a composition.

[0116] The methods of the present invention can include the capturing an image of the split-end of at least one removed hair fiber. Examples of such capturing methods are described herein. This step may include storing an electronic representation of the image, for example, using an electronic file accessible on a digital camera and/or computer.

[0117] The methods of the present invention can include associating the at least one marked hair fiber with the tress from which the hair fiber was removed. Replacing the removed hair fiber back with the tress provides a more natural environment for testing the mending ability of a composition. The hair fibers with split-ends remain with other hair fibers that may not have split-ends and remain within a larger grouping of hair fibers. This situation better simulates the environment of a normal lock of hair, e.g., on a human head. Simply removing the hair fibers with split-ends and testing compositions on these removed fibers would only provide results based on an artificial environment. Thus, when using the method to test compositions for use by consumers, the present invention allows for reporting results that are meaningful to those consumers, e.g., results that report on the mending of hair fibers that are in an environment important to the consumers.

[0118] The methods of the present invention can include treating the tress and the at least one marked hair fiber with a composition. Treatments may include, for example, massaging the composition into the hair. Treatment also may include, for example, rinsing the hair to remove the composition, such as with a rinse-off composition. The composition may be allowed to remain on the hair, for example, when using a leave-in composition. The method of treatment may be any suitable method, including methods described herein. The composition may be any suitable compositions, including compositions described herein.

[0119] The methods of the present invention can include determining parameters of hair mending. For example, the rate at which a split-end is mended can be determined under defined conditions, e.g., those described herein. Compositions can then be compared to determine which provide for faster mending of split-ends. The split-end mending efficacy of the compositions used and/or tested also can be determined, e.g., using the video methods described herein. Mending of a split-end is preferable within one hour, less than 50 minutes, less than 40 minutes, less than 30 minutes, less than 20 minutes, less than 10 minutes, less than 5 minutes, or less than 1 minute. The completion or amount of mending may be 10% or greater, 20% or greater, 30% or greater, 40% or greater, 50% or greater, 60% or greater, 70% or greater, 80% or greater, 90% or greater, or complete (e.g., aboutl00%). The mending can be measured against a negative control or no treatment, wherein the treated split-end can show a statistically significant improvement in split-end mending (e.g., faster mending and/or greater amount or completion of mending).

[0120] The methods of the present invention can include assigning a value of 0 for no repair of the split-end, ½ for partial repair, or 1 for complete repair and summing the assigned numbers for all marked hair fibers and dividing the sum by the total number of marked hair fibers. Thus, e.g., when there is an accounting for all of the split-ends of a tress, the resulting value will report on the ability of the composition to mend split-ends. A composition with poor mending ability will have a value that is low and/or approaches zero, whereas a composition with better mending ability will have a value that is higher and/or approaches one. Compositions thus may be compared using the method of the present invention where a composition that results in a higher value provides better mending than a composition that results in a lower value.

[0121] Any type of split-end can be mended by the methods of the present invention. One type of split-end includes, for example, the primary split-end. With this type of split- end, the hair fiber contains a single split along the longitudinal axis of the hair fiber, producing two ends of the hair fiber. Another example of a split-end includes the double Y split-end, which is created by an additional split along the longitudinal axis of an end of a primary split. The tree split-end is an example of a split-end where there are several double Y splits within one hair fiber. Another example of a split-end is where the end of a hair fiber has many short splits that feather out, often resulting in fiber shafts of varying thickness. Another example of a split-end is the long split-end where one side of a primary split end is significantly longer than the other (e.g., one side broke off). The taper split-end is another example of a split-end where only a portion of the hair fiber remains at the end. Split-ends also may, for example, be characterized by the number of ends, such as with the triple split- end with two splits of the hair fiber. A deep split-end is an example of a split that occurs at the mid-point of a hair shaft (not necessarily the end). A baby split-end is an example of a split-end that only has a small split in the hair fiber. The term "split-ends" as used herein also can include splits that do not extend to the end of the hair fiber. An example of such a split is an incomplete split. Figures 4A-4D show some types of split-ends.

[0122] The hair fibers used in the methods of the present invention may be of any mammalian hair. In one embodiment, the hair is human hair. Human hair of any nationality, region, or ethnicity may be used, e.g., European, Asian, African, or Caucasian. In an embodiment, the hair is European hair. The hair may have any type of damage due to, e.g., bleaching once, bleaching twice, bleaching more than twice, dyeing, or mechanical damage. The hair fibers may have no damage, for example, as with virgin hair. Additionally, the type of hair used in the methods of the present invention can be varied from one run of the method to another. This varying of the hair can correspond to the use and testing of various compositions, which can, e.g., depend on what type of results are desired to be communicated to consumers. Varying the hair type and/or composition will allow for the communication of results for any hair type and any hair care composition.

[0123] An aspect of the present invention includes selecting a hair fiber with a split end and cutting to, e.g., about 1-1.5 inch in length (measuring from the split end side). A small piece of clear tape can be used to secure the fiber on, for example, a glass slide. The glass slide can be placed under a microscope with, e.g., 50X magnification and that has an interface with a camera and computer. Lighting and focus can be adjusted accordingly. Depending on set-up, a recording can take place within the computer interface or a video camera can be set-up on, e.g., a tripod pointing at the computer screen. With the camera recording, one drop of a composition, e.g., containing 2% active complex can be applied over the split-end using a micropipette. Lighting and focus can be further adjusted accordingly. A blow drier can be turned on, e.g., medium heat and aimed toward the split end. Recording can take place during and until the split end has fully or partially mended.

[0124] An aspect of the invention includes taking human hair, preferably damaged, most preferably twice-bleached European hair, and assembling into, e.g., wax bound strips that may be, for example, 1-1.5 inches wide. These tresses are then combed many thousands of times while a blow dryer is pointed perpendicularly to brushing to form an appropriate number of split- ends. A select number (for example, 10-20) of fibers with split-ends are selected and pulled out of the fiber assembly. Pictures of each split-end are taken with the use of a microscope at 20-50X magnification. Brass ferrule tabs are clamped on the end opposite of the split-end of each fiber. These brass tabs are then labeled and placed between two pieces of masking tape. The assembly is then inserted into the middle of the hair tress and a paper clamp is affixed to keep the assembly in place. The tress is then treated with a rinse-out split-end mending composition for a series of, e.g., three cycles. After the final cycle, the clamp is removed and new pictures of the split-ends are taken. By comparing the before and after pictures, an evaluator can give a value of "0" for no mending, "1/2" for partial mending, and "1" for complete mending. Summing these numbers and dividing by the total number of fibers allows for the expression of the degree of split-end repair.

[0125] As noted above, an image capture system is used in an embodiment of the invention to produce a representation of the appearance of the split end both before and after repair or attempted repair. While various such image capture systems are possible within the scope of the teachings herein, an exemplary such system is shown in FIG. 6. In particular, FIG. 6 is a schematic diagram showing an image data capture system in which the described image capture and processing steps may be executed.

[0126] The illustrated system 600 comprises a number of interacting components, including a sample support device 601, such as a platform or surface suitable for supporting a sample 602. The sample support device 601 may be transparent to allow under-lighting, via a light source 603. The light source 603 may also be situated above the support device 601 to provide illumination via reflectance.

[0127] An electrical image capture device 604 is provided for capturing an enlarged image or video sequence of the sample 602 under treatment. In this regard, a magnification device 605 is provided adjacent the sample support device 601 , between the sample support device 601 and the image capture device 604. The image capture device 604 may be a still camera or video camera adapted to capture a sequence of images. The magnification device 605 may be an optical magnifying lens or lens arrangement such as an optical microscope, or may be an electronic magnification device such as an electron microscope or the like. In an embodiment of the invention, the image capture device 604 and/or the magnification device

605 may be scannable to capture images of different regions or segments of the sample 602.

[0128] An auxiliary computing and data capture device 606 is provided from controlling and receiving data from the image capture device 604. The auxiliary computing and data capture device 606 is a com-putting a processing device able to receive electronic image data from the image capture device 604 and send control signals to the image capture device 604 to cause image capture. The auxiliary computing and data capture device 606 may also control the illumination device 603.

[0129] In an embodiment of the invention, the auxiliary computing and data capture device 606 is communicably linked to an electronic database 607, either locally or remotely via a wired or wireless link. In this manner, the auxiliary computing and data capture device

606 is able to gather data from the image capture device 604 and to store the gathered data in the electronic database 607 for later analysis, manipulation, and/or retransmission, e.g., to a printing or publishing facility (not shown).

[0130] The auxiliary computing and data capture device 606 may be a computer such as a person computer, laptop computer, workstation or the like, and operates by the computer- execution of computer readable instructions stored on a computer-readable medium. The computer-readable medium is a tangible medium such as a magnetic or optical disc system, flash drive, PRO, etc. Thus, the steps discussed herein that involve the capture, manipulation, and/or transmission of data are executed in this manner. A user interface 608 allows a user to receive information from the auxiliary computing and data capture device 606 in human understandable form and to provide input to the device in computer understandable form. In an embodiment of the invention, the user interface 608 includes a graphical user interface on a screen and a keyboard, keypad, stylus pad, mouse, and/or other user input mechanism.

[0131] In one embodiment of the present invention, the image capture device is a video camera adapted to record reparation of one or more hair shafts, e.g., a hair shaft containing one or more split-ends, in real-time. Desirably, the video is recorded at magnification sufficient to visualize with the naked eye the hair reparation process in real-time. Suitable magnification can include, e.g., 20-50X magnification.

[0132] The following examples further illustrate the invention but, of course, should not be construed as in any way limiting its scope. EXAMPLE 1

[0133] This example demonstrates production of hair care compositions comprising a polyelectrolyte complex using a two-tank process.

[0134] Compositions 1A-1C

[0135] One of ordinary skill in the art would be able to determine the proper RPM settings for the mixers as listed in this Example and other Examples based on the identity of the particular tanks to be used in following the listed protocols.

[0136] In a suitable, stainless steel premix tank, charge water set at 1 13-131 °F (45-55 °C). Begin vigorous turbine mixing (turbine mixer at vigorous clockwise direction; side sweep mixer off). Once the batch temperature is 86 °F (30 °C) or above, and with vigorous mixing, slowly add PVMMA Copolymer (Gantrez^® S-97 BF; ISP, Wayne, NJ, USA) to the premix tank. Adjust mixing accordingly in order to achieve vigorous agitation without creating excessive foam on the liquid surface. Once all of the powder has been added, use water set at 1 13-131 °F (45-55 °C) to rinse the mixing blades and side walls. Once the rinse is completed, turn on the side sweep agitator and begin heating to 122-131 °F (50-55 °C). (The powder lumps will disperse more quickly when the premix is 1 13-131 °F (45-55 °C)). Continue heating and maintain the temperature throughout the mix time. Set the mixer (turbine mixer at vigorous counterclockwise direction; side sweep mixer at moderate clockwise direction).

[0137] Mix the batch for a minimum of 20 minutes or until no particles or lumps are present.

[0138] Once the premix is uniform and free of lumps, reduce turbine mixing to moderate. Add the sodium hydroxide to the premix tank and mix for 10 minutes. The solution will have a low viscosity and will appear slightly hazy. (Mixer settings: turbine mixer at moderate counterclockwise direction; side sweep mixer at moderate clockwise direction.) Mix the batch for a minimum of 10 minutes or until completely uniform.

[0139] Once the batch is uniform, submit a sample for an in-process pH test. Continue to retest the sample until a stable pH reading of 6.9-7.0 is achieved. If pH is low, add additional sodium hydroxide 20% to meet the specification range. Remix and resample. If pH is high, add additional aspartic acid to meet specification range. Remix and resample.

[0140] Once the Gantrez has been completely hydrated and the pH is within

specification, check that the premix temperature is 122-131 °F (50-55 °C). Heat if necessary. Once the premix is 122-131 °F (50-55 °C), turn off the side sweep agitator, reverse turbine direction and increase turbine mixing speed to create a vortex (turbine mixer at vigorous clockwise direction; side sweep mixer off).

[0141] Slowly add the polyquaternium 28 (Conditioneze^® NT-20 (20% active); ISP, Wayne, NJ, USA) to the premix vessel. Add slowly to the premix vessel for the proper polyelectrolyte complex particle size. Use a drum spout to regulate addition flow rate. Do not dump the entire open container into the premix vessel at once. During this material addition, the premix will become very viscous and begin to turn white. Once all of the material has been added, the solution will again thin out and appear milky in appearance.

[0142] Reverse turbine direction and turn on side sweep agitator. Mix vigorously for 20 minutes or until the premix is completely uniform (turbine mixer at vigorous counterclockwise direction; side sweep mixer at moderate clockwise direction). Mix the batch for a minimum of 20 minutes or until no visible particles or lumps are present.

[0143] Once the mix is complete, take a sample and visually inspect the premix. Check that it is completely white and not hazy or gray. Also check that the premix viscosity is thin and milk-like and not too viscous. If the premix is not thin and milky white, continue mixing vigorously for an additional 20 minutes and resample.

[0144] Once the premix is completely uniform, reduce agitation and begin cooling to 86- 1 13 °F (30-45 °C). Maintain mixing and temperature until the premix is ready to be added to the main compounding tank (turbine mixer at moderate counterclockwise direction; side sweep mixer at moderate clockwise direction).

[0145] Into a main stainless steel compounding tank, charge water set at 180-185 °F (82- 85 °C) with moderate mixing (turbine mixer at moderate counterclockwise direction; side sweep mixer at moderate clockwise direction). Slowly add the disodium EDTA and aspartic acid to the main compounding tank. After the items have been added, begin heating the batch to 180-185 °F (82-85 °C), as necessary (turbine mixer at moderate counterclockwise direction). Continue heating the batch to 180-185 °F (82-85 °C). Mix the batch for a minimum of 5 minutes or until the solids are completely dissolved.

[0146] Once the batch temperature is 176 °F (80 °C) or above, add the stearamidopropyl dimethylamine to the main compounding tank and mix until it is completely melted (turbine mixer at moderate counterclockwise direction; side sweep mixer at moderate clockwise direction). Continue heating the batch to 180-185 °F (82-85 °C). Mix the batch for a minimum of 5 minutes or until the solids are completely melted.

[0147] Once the batch temperature is 180- 185 °F (82-85 °C), add the following items to the main compounding tank: cetyl alcohol, stearyl alcohol, glyceryl stearate, and PPG-3 benzyl ether myri state for Composition 1A (conditioner); cetyl alcohol, glyceryl stearate, and aminopropyl dimethicone for Composition IB (overnight creme); cetyl alcohol and glyceryl stearate for Composition 1 C (leave-in creme). Once the batch temperature is again 180-185 °F (82-85 °C), maintain this temperature and mix for a minimum of 30 minutes (turbine mixer at moderate counterclockwise direction; side sweep mixer at moderate clockwise direction). Mix the batch while holding it between 180-185 °F (82-85 °C).

[0148] Take a sample from the main compounding tank and visually verify that all of the solids have been melted and that the batch is smooth and uniform. If there remains any non- dissolved materials or particles, continue vigorous mixing and resample.

[0149] Begin cooling the batch to 104-1 13 °F (40-45 °C) and reduce the turbine and side sweep agitator speeds to moderate/slow to help de-aerate the batch (turbine mixer at moderate counterclockwise direction; side sweep mixer at slow clockwise direction). While cooling and once the batch temperature is 167 °F (75 °C) or below, add the propylene glycol to the main compounding tank (turbine mixer at moderate counterclockwise direction; side sweep mixer at moderate clockwise direction). For Composition 1C (leave-in creme), also add glycerin at this mixing speed.

[0150] Once the main batch temperature is 150 °F (65 °C) or below for Composition 1 A (conditioner) or 131 °F (55 °C) or below for the cremes turn off the side sweep agitator, reverse the direction of the turbine agitator, and increase mixing to create a slight vortex (turbine mixer at moderate clockwise direction; side sweep mixer off). Add the Salcare^® SC- 96 (65% polyquaternium-37, 25% propylene glycol dicaprylate/dicaprate, 10% PPG-1 trideceth-6; Ciba/BASF, Basel, Switzerland) to the main compounding tank and continue cooling to 104-1 13 °F (40-45 °C). (Mix Salcare^® SC-96 well in its container prior to addition to the batch.)

[0151] Once all of the material has been incorporated into the batch and is no longer sitting on the surface, reverse turbine agitator and turn on side sweep agitator (turbine mixer at moderate counterclockwise direction; side sweep mixer at moderate clockwise direction).

[0152] Once the main batch temperature is 150 °F (65 °C) or below for Composition 1 A (conditioner) or 131 °F (55 °C) or below for Composition IB (overnight creme), and the premix is ready, add the premix to the main compounding tank. While the premix is being added, turn off the turbine mixer or reduce it to slow as the liquid level passes the top set of turbine blades to minimize aeration. Once the premix has been added, rinse the premix tank with water set at 77-95 °F (25-35 °C) and add it to the main compounding tank. The batch viscosity will decrease as the premix is mixed into the batch. Adjust mixer speeds accordingly to avoid splashing (turbine mixer at moderate counterclockwise direction; side sweep mixer at moderate clockwise direction).

[0153] For Composition 1 A (conditioner), mix the batch for a minimum of 15 minutes or until the batch is uniform. Once the main batch temperature is 122 °F (50 °C) or below, add the Fluid Blend directly to the main compounding tank. Mix well during addition. Increase mixing as necessary to mix in the silicone turbine mixer at vigorous counterclockwise direction; side sweep mixer at moderate clockwise direction). [0154] For the cremes, once all of the premix has been added, charge with water set at 77-95 °F (25-35 °C) below the surface of the batch, to minimize aeration, if possible. Mix the batch for a minimum of 15 minutes or until the batch is uniform. Continue cooling to 104-1 13 °F (40-45 °C). In a suitable stainless steel phase vessel or container, premix the following silicone items with vigorous agitation: Abil^® OSW 5 (84% cyclopentasiloxane, 15% dimethiconol, 1% dimethicone), and dimethicone (60,000 est) for Composition I B (overnight creme); dimethicone (60,000 est), phenyl trimethicone (DC-556; Dow Corning), and D5 dimethiconol (DC- 1501) for Composition 1C (leave-in creme). Once the silicone premix is uniform, add it to the main compounding tank and allow the silicone premix container to drain out as much as possible into the main batch tank. Increase mixing as necessary to mix in the silicones (turbine mixer at vigorous counterclockwise direction; side sweep mixer at moderate clockwise direction).

[0155] When the batch temperature is 1 13 °F (45 °C) or below, add the following ingredients to the main compounding tank: fragrance (parfum), DMDM hydantoin, cocos nucifera oil, keratin amino acids, flower/leaf extract. For the Composition IB (overnight creme), also add DC-8500 (82% Bis(C13-15 alkoxy) PG-Amodimethicone, 18% C14-15 alcohols; Dow Corning, Midland, MI, USA). Continue mixing and cooling to 95-104 °F (35- 40 °C).

[0156] Mix vigorously for a minimum of 45 minutes or until all of the lumps have been removed and the batch is smooth and uniform. The batch may be recirculated through an 80 Mesh Filter throughout this Final Mix to help break down the lumps. Although shear (increased mixing and/or recirculating) is needed to break down the lumps, minimize aeration as much as possible (turbine mixer at vigorous counterclockwise direction; side sweep mixer at moderate clockwise). Mix for a minimum of 45 minutes.

[0157] When the batch temperature is 95-104 °F (35-40 °C), analyze sample(s).

Discontinue mixing and cooling.

[0158] Adjustments that may be made are the following. If the pH is low, add sodium hydroxide (20%) at a maximum of 5% of the total batch requirement. Remix and resample. If the pH is high, add aspartic acid at a maximum of 7.5% of the total batch requirement. Remix and resample. If the viscosity is low, mix additional 60 minutes and resample. Batch may also be recirculated through an 80 Mesh Filter.

[0159] Pumps that should be used for pumping material into the tanks include air diaphragm and positive displacement. Filters that should be used include 80 mesh for all transfer operations. The fill temperature should be 90-99 °F (32-37 °C). Do not reheat batch if product temperature falls below 90 °F (32 °C).

[0160] Composition ID

[0161] Into a main stainless steel compounding tank, charge water, set at 95 - 104 °F (30 - 35 °C), and begin vigorous agitation (turbine mixer at vigorous counterclockwise direction; side sweep mixer at moderate clockwise direction, if available). Do not heat the water to maintain temperature. Slowly add the following items, in order, to the main compounding tank and mix vigorously (turbine mixer at vigorous counterclockwise direction; side sweep mixer at moderate clockwise direction, if available) for 10 minutes or until the batch is completely uniform and no lumps are present: PVM/MA copolymer (Gantrez S97BF), NaOH, Polyquaternium 28 (Conditioneze). Mix the batch for a minimum of 10 minutes or until the batch is completely uniform and no lumps are present.

[0162] With vigorous mixing (turbine mixer at vigorous counterclockwise direction; side sweep mixer at moderate clockwise direction, if available) add the following ingredients to the main compounding tank: PVP, disodium EDTA. Mix the batch for a minimum of 15 minutes or until the solids are completely dissolved and the batch is uniform.

[0163] After mixing, take a sample from the main compounding tank and verify that there are no lumps or particulates, and that the batch is smooth and uniform. If there are lumps or particulates, continue to mix and resample until the batch is smooth and uniform.

[0164] Begin heating the batch to 170 - 175 °F (76 - 79 °C) with vigorous agitation (turbine mixer at vigorous counterclockwise direction; side sweep mixer at moderate clockwise direction, if available). Once the batch temperature is 150°F (65 °C) or above, add the following ingredient to the main compounding tank: stearalkonium chloride. Mix the batch while holding it between 170 - 175°F (76 - 79°C). Mix the batch for a minimum of 60 minutes.

[0165] Take a sample from the main compounding tank and visually verify that there are no lumps or particulates, and the batch is uniform. If lumps or particulates are present, continue to mix vigorously and resample until the batch is uniform.

[0166] Reduce agitation to moderate (turbine mixer at moderate counterclockwise direction; side sweep mixer at moderate clockwise direction, if available) and begin cooling the batch to 90 - 95°F (32 - 35°C).

[0167] While cooling, add the following ingredients, in order, to the main

compounding tank. Mix well after each addition: DC 949 cationic emulsion; glycerin USP VEG; PEG- 12 dimethicone; propylene glycol; triethanolamine; citric acid.

[0168] Once the batch temperature is 113°F (45°C) or below, add the following ingredients, in order, to the main compounding tank: DMDM hydantoin; hydrolyzed silk; vitamin blend; polyglyceryl-3-distearate mixture.

[0169] Into a separate stainless steel vessel or container equipped with an electric or air mixer, premix the following ingredients: polysorbate 20; fragrance. Blend this premix vigorously until all of the fragrance is solubilized and the premix is uniform and clear. Charge this premix to the main compounding tank with moderate agitation. Rinse the premix vessel/container with cold water, set at 60 - 80°F (15 - 27°C), and add to the main compounding tank. Mix (turbine mixer at moderate counterclockwise direction; side sweep mixer at moderate clockwise direction, if available) for a minimum of 20 minutes or until the batch is completely uniform.

[0170] Adjustments that may be made are the following. If the pH is low, add triethanolamine in 0.20% solution increments. If the pH is high, add citric acid in 0.20% solution increments.

[0171] Pumps that should be used for pumping material into the tanks include air diaphragm and positive displacement. Filters that should be used include 80 mesh for all transfer operations. The fill temperature should be ambient. Batch may be cooled as necessary to facilitate filling.

[0172] Composition IE

[0173] Into a main stainless steel compounding tank, charge water, set at 68 - 86°F (20 - 30°C), where available, and begin vigorous agitation (turbine mixer at vigorous

counterclockwise direction; side sweep mixer at moderate clockwise direction). [0174] Slowly add the following items, in order, to the main compounding tank and mix vigorously (turbine mixer at vigorous counterclockwise direction; side sweep mixer at moderate clockwise direction) for 5 minutes or until the batch is completely uniform and no lumps are present: PVM/MA copolymer (Gantrez S97BF), sodium hydroxide (20%), Polyquaternium 28 (Conditioneze). Mix the batch for a minimum of 5 minutes or until the batch is completely uniform and no lumps are present.

[0175] Once the batch is uniform, slowly sprinkle the following item into the main compounding tank: Polyquaternium- 10. Use vigorous mixing to achieve a vortex, where possible. Rinse the inside of the tank and mixer blades with water (turbine mixer at vigorous counterclockwise direction; side sweep mixer at moderate clockwise direction).

[0176] Begin heating the batch to 1 13 - 122°F (45 - 50°C). While heating, mix for a minimum of 20 minutes, or until the polymer is completely hydrated and the solution is clear and uniform.

[0177] After mixing, take a sample from the main compounding tank and verify that there are no lumps or particles, and that the batch is smooth and homogeneous. If there are lumps or particles, continue to mix and resample until the batch is smooth and uniform. While continuing to heat, reduce turbine agitation (turbine mixer at moderate counterclockwise direction; side sweep mixer at moderate clockwise direction) and add the following items, in order, to the main compounding tank: cocamidopropyl betaine, disodium EDTA, citric acid, USP. Mix for a minimum of 10 minutes, or until the batch is uniform and all items are fully dissolved.

[0178] Check that the batch temperature is 1 13 - 122°F (45 - 50°C). Then, add the following items to the main compounding tank, in order, with moderate agitation (turbine mixer at moderate counterclockwise direction; side sweep mixer at moderate clockwise direction). Use caution to avoid aeration, and slow the mixing during addition if necessary: sodium laureth sulfate; disodium laureth sulfosuccinate; glycol distearate, cocamidopropyl betaine, cocamide MEA, water mixture; PEG-6 caprylic/capric glycerides. As the level in the tank increases, reduce the turbine mixer speed to SLOW when the level approaches the blades. Once the blades are completely covered by the batch, increase the turbine mixer speed back to moderate. This will help to reduce aeration of the batch. Mix the batch while holding it between 1 13 - 122°F (45 - 50°C). Mix for a minimum of 20 minutes or until the batch is smooth and completely uniform.

[0179] De-aerate the batch by reducing both turbine and sweep agitation to slow (turbine mixer at slow counterclockwise direction; side sweep mixer at slow clockwise direction) and begin cooling the batch to 95 - 104°F (35 - 40°C).

[0180] Once the batch temperature is 1 13°F (45°C) or below, increase turbine and sweep agitation to moderate (turbine mixer at moderate counterclockwise direction; side sweep mixer at moderate clockwise direction) and add the following items, in order, to the main compounding tank: fragrance; methylchloroisofhiazolinone, methylisothiazolinone, water mixture; coconut oil; keratin amino acids, flower extract.

[0181] In a separate stainless steel vessel or container, mix the sodium chloride and water, set at 95 - 104°F (35 - 40°C), until the salt is completely dispersed. The salt may not completely dissolve as there may not be enough Water available. Mix until the salt is completely dispersed and then continue.

[0182] Once the salt premix is ready, add it to the main compounding tank and mix until the batch is completely uniform (turbine mixer at moderate counterclockwise direction; side sweep mixer at moderate clockwise direction). With cold water, rinse the premix vessel or container and flush the transfer line. Add this rinse/flush water to the main compounding tank. Mix for a minimum of 30 minutes or until the batch is completely

uniform. Sample the composition. Discontinue mixing and cooling (if applicable).

[0183] Adjustments that may be made are the following. If the viscosity is low, add sodium chloride. Do not exceed a total sodium chloride level of 2.00% in this formula. If the viscosity is high, add propylene glycol. If the pH is low, add sodium hydroxide (20%). If the pH is high, add citric acid.

[0184] Aerated batch: Reheat the batch to 120 - 125°F (48 - 52°C) and mix

slowly for 20 minutes. Cool back down to 95 - 100°F (35 - 38°C), add

back 10% preservative and add back fragrance if necessary.

[0185] Pumps that should be used for pumping material into the tanks include air diaphragm and positive displacement. Filters that should be used include 80 mesh for all transfer operations. The fill temperature should be 90-100°F (32-38°C). Batch may be warmed to this temperature range to help facilitate filling.

[0186] Composition IF

[0187] Mix the Salcare SC-96 well in its container prior to being weighed and prior to addition to the batch.

[0188] In a suitable, stainless steel premix tank, charge water set at 113 - 131°F (45 - 55°C). Begin vigorous turbine mixing (turbine mixer at vigorous clockwise direction; side sweep mixer off).

[0189] Once the batch temperature is 86°F (30°C) or above, and with vigorous mixing, slowly add PVM/MA Copolymer (Gantrez S-97 BF) to the premix tank. Adjust mixing accordingly in order to achieve vigorous agitation without creating excessive foam on the liquid surface. Once all of the powder has been added, use water set at 1 13 - 131 °F (45 - 55°C) to rinse the mixing blades and side walls. Once the rinse is completed, turn on the side sweep agitator (turbine mixer at vigorous counterclockwise direction; side sweep mixer at moderate clockwise direction) and begin heating to 122 - 131 °F (50 - 55°C). The powder lumps will disperse more quickly when the premix is 1 13 - 131 °F (45 - 55°C). Continue heating and maintain the temperature throughout the mix time. Mix the batch for a minimum of 20 minutes or until no particles or lumps are present.

[0190] Once the premix is uniform and free of lumps, reduce turbine mixing to moderate (turbine mixer at moderate counterclockwise direction; side sweep mixer at moderate clockwise direction). Add the sodium hydroxide to the premix tank and mix for 10 minutes. The solution will have a low viscosity and will appear slightly hazy. Mix the batch for a minimum of 10 minutes or until completely uniform.

[0191] Once the batch is uniform, submit a sample for an in-process pH test. Continue to retest the sample until a stable pH reading is achieved. If pH is low, add additional sodium hydroxide (20%) to meet specification range. Remix and resample. If pH is high, add additional aspartic acid to meet specification range. Remix and resample.

[0192] Once the Gantrez has been completely hydrated and the pH is within

specification, check that the premix temperature is 122 - 131 °F (50 - 55°C). Heat if necessary.

[0193] Once the premix is 122 - 131 °F (50 - 55°C), turn off the side sweep agitator, reverse turbine direction and increase turbine mixing speed to create a vortex (turbine mixer at vigorous clockwise direction; side sweep mixer off). Slowly add the Polyquaternium 28 (Condi tioneze NT-20) to the premix vessel. Add slowly to the premix vessel for the proper complex particle size. This addition should take 10 - 15 minutes to be completed. Use a drum spout to regulate addition flow rate. Do not dump the entire open container into the premix vessel at once.

[0194] During this material addition, the premix will become very viscous and begin to turn white. Once all of the material has been added, the solution will again thin out and appear milky in appearance.

[0195] Reverse turbine direction and turn on side sweep agitator (turbine mixer at vigorous counterclockwise direction; side sweep mixer at moderate clockwise direction). Mix vigorously for 20 minutes or until the premix is completely uniform. Mix the batch for a minimum of 20 minutes or until no particles or lumps are present. Once the mix is complete, take a sample and visually inspect the premix. Check that it is completely white and not hazy or gray. Also check that the premix viscosity is thin and milk-like and not overly viscous. If the premix is not thin and milky white, continue mixing vigorously for an additional 20 minutes and resample.

[0196] Once the premix is completely uniform, reduce agitation (turbine mixer at moderate counterclockwise direction; side sweep mixer at moderate clockwise direction) and begin cooling to 86 - 1 13°F (30 - 45°C). Maintain mixing and temperature until the premix is ready to be added to the main compounding tank.

[0197] Into the main stainless steel compounding tank, charge water, set at 180 - 185°F (82 - 85°C), with moderate mixing (turbine mixer at moderate counterclockwise direction; side sweep mixer at moderate clockwise direction).

[0198] Slowly add the following items to the main compounding tank: disodium EDTA; aspartic acid. After the items have been added, begin heating the batch to 180 - 185°F (82 - 85°C), as necessary. (Turbine mixer at moderate counterclockwise direction; side sweep mixer at moderate clockwise direction). Continue heating the batch to 180 - 185°F (82 - 85°C). Mix the batch for a minimum of 5 minutes or until the solids are completely dissolved.

[0199] Once the batch temperature is 176°F (80°C) or above, add the stearamidopropyl dimethylamine to the main compounding tank and mix until it is completely melted (turbine mixer at moderate counterclockwise direction; side sweep mixer at moderate clockwise direction). Continue heating the batch to 180 - 185°F (82 - 85°C). Mix the batch for a minimum of 5 minutes or until the solids are completely melted.

[0200] Once the batch temperature is 180 - 185°F (82 - 85°C), add the following items to the main compounding tank: cetyl alcohol; glyceryl stearate; aminopropyl dimethicone.

[0201] Once the batch temperature is again 180 - 185°F (82 - 85°C), maintain this temperature and mix for 30 minutes (turbine mixer at moderate counterclockwise direction; side sweep mixer at moderate clockwise direction). Mix the batch while holding it between 180 - 185°F (82 - 85°C). Mix the batch for a minimum of 30 minutes.

[0202] After the hot mix, take a sample from the main compounding tank and visually verify that all of the solids have been melted and that the batch is smooth and uniform. If there remains any undissolved materials or particles, continue vigorous mixing and resample periodically until all of the waxes and particles are dissolved and the batch is uniform.

[0203] After the hot mix, begin cooling the batch to 104 - 113°F (40 - 45 °C) and reduce the turbine and side sweep agitator speeds to moderate/slow to help de-aerate the batch (turbine mixer at moderate counterclockwise direction; side sweep mixer at slow clockwise direction).

[0204] While cooling and once the batch temperature is 167°F (75°C) or below, add the propylene glycol to the main compounding tank (turbine mixer at moderate counterclockwise direction; side sweep mixer at moderate clockwise direction). [0205] Once the main batch temperature is 150°F (65°C) or below, turn off the side sweep agitator, reverse the direction of the turbine agitator and increase mixing to create a slight vortex (turbine mixer at moderate clockwise direction; side sweep mixer off). Add the Salcare^® SC-96 to the main compounding tank and continue cooling to 104 - 1 13°F (40 - 45°C).

[0206] Once all of the material has been incorporated into the batch and is no longer sitting on the surface, reverse turbine agitator and turn on side sweep agitator (turbine mixer at moderate counterclockwise direction; side sweep mixer at moderate clockwise direction).

[0207] Once the main batch temperature is 131 °F (55°C) or below, and the PEC Actives Premix is ready, add the premix to the main compounding tank. While the premix is being added, turn off the turbine mixer or reduce it to slow as the liquid level passes the top set of turbine blades to minimize aeration.

[0208] Once the premix has been added, rinse the premix tank with cold water set at 77 - 95°F (25 - 35°C) and add it to the main compounding tank. The batch viscosity will decrease as the PEC Actives Premix is mixed into the batch. Adjust mixer speeds accordingly to avoid splashing (turbine mixer at moderate counterclockwise direction; side sweep mixer at moderate clockwise direction).

[0209] Once all of the PEC Actives Premix has been added, charge cold water, set at 77 - 95°F (25 - 35°C) below the surface of the batch, to minimize aeration, if possible. Mix the batch for a minimum of 15 minutes or until the batch is uniform. Continue cooling to 104 - 113°F (40 - 45°C).

[0210] In a suitable stainless steel phase vessel or container, premix the following items with vigorous agitation: cyclopentasiloxane mixture; dimethicone. Once the premix is uniform, add it to the main compounding tank and allow the premix container to drain out as much as possible into the main batch tank (turbine mixer at vigorous counterclockwise direction; side sweep mixer at moderate clockwise direction), increase mixing as necessary to mix in the silicones.

[0211] When the batch temperature is 1 13°F (45°C) or below, add the following ingredients to the main compounding tank: DC-8500; fragrance; DMDM hydantoin, coconut oil, keratin amino acids, flower extract mixture. Continue mixing and cooling to 95 - 104°F (35 - 40°C).

[0212] Mix vigorously (turbine mixer at vigorous counterclockwise direction; side sweep mixer at moderate clockwise direction) for a minimum of 45 minutes or until all of the lumps have been removed and the batch is smooth and uniform. The batch may be recirculated through an 80 Mesh Filter throughout this Final Mix to help break down the lumps.

Although shear (increased mixing and/or recirculating) should be used to break down the lumps, minimize aeration as much as possible. Mix for a minimum of 45 minutes.

When the batch temperature is 95 - 104°F (35 - 40°C), sample composition. Discontinue mixing and cooling.

[0213] Adjustments that may be made are the following. If the pH is low, add sodium hydroxide (20%) at a maximum of 5% of the total batch requirement. Remix and resample. If the pH is high, add aspartic acid at a maximum of 7.5% of the total batch requirement. Remix and resample. If the viscosity is low, mix an additional 60 minutes and resample. Batch may also be recirculated through an 80 Mesh Filter.

[0214] Pumps that should be used for pumping material into the tanks include air diaphragm and positive displacement. Filters that should be used include 80 mesh for all transfer operations. The fill temperature should be 90-99 °F (32-37 °C). Do not reheat batch if product temperature falls below 90 °F (32 °C).

EXAMPLE 2

[0215] This example demonstrates production of hair care compositions comprising a polyelectrolyte complex using a one-tank process.

[0216] The process of Example 1 describes a two-tank process, where the polyelectrolyte complex is prepared in one tank, the remaining components are mixed in a separate tank, and the polyelectrolyte complex and the remaining components are combined. To simplify the process to one tank, the process is performed as described in Example 1 , except the polyelectrolyte complex is first prepared in the tank and the additional components are added directly to the same tank after the polyelectrolyte complex forms. The final viscosity of the composition may be lower than if prepared in two tanks. To compensate, add additional Salcare^® SC 96.

EXAMPLE 3

[0217] This example demonstrates the compatibility of polyelectrolyte complexes (PECs) with certain charged compounds and polymers.

[0218] Visual Appearance: The visual appearance of PECs in solution with charged particles was characterized. When PVMMA and polyquat-28 are individually solvated in water, the compositions are clear. When PVMMA and polyquat-28 are present as PECs solvated in water, the composition becomes hazy and/or milky in appearance. After adding to the PECs another charged species that produces a clear composition when solvated in water, the milky/hazy opacity is expected to decrease (and in some cases turn back to clear). This is a visual indication of the PEC complexation process reversing. The milky opaque appearance of 1 wt. % and 2 wt. % PVMMA/polyquat-28 PECs disappears in the presence of greater than 0.5 wt. % polyquaternium-4 (Celquat^® L-200; Akzo Nobel, Amsterdam, Netherlands). This indicates that the structure of the PECs has been disrupted. Below 0.5 wt. % Celquat^® L-200, the PECs are not disrupted. Celquat^® H-100 at 0.5 wt. % did not disrupt the PECs. Celquat^® L-200 and H-100 are similar, but L-200 has lower viscosity and higher cationic activity.

[0219] Thickening: Tinovis GTC/Acrylates/Beheneth-25 Methacrylate Copolymer (2.3%) in compositions with and without PECs was tested. The composition without PECs gave a viscosity of 40,000-60,000 cps. The composition with PECs was water thin. Since Tinovis is an associative thickener and the composition without PECs did not thicken, the Tinovis was thought to be rendered ineffective by PECs.

[0220] Split-end Mending: Table 1 1 shows charged compounds and polymers that were combined with PECs. These compositions showed no deleterious effects of split-end mending.

[0221] Table 1 1

Quaternium-80 0.5

Merquat* 2001

(Polyquaternium-47; 0.5

Nalco, Naperville, IL, USA)

Vinyl

Caprolactum/VP/Dimethyl- aminoethyl Methacrylate 0.25

Copolymer (in acid

environment)

N-Hance SP 100

(Acrylamidopropyltrimonium

0.1-0.2

Chloride/Acrylates Copolymer;

Aqualon)

Acrylic Acid/VP Crosspolymer 1

Varisoft EQ 65 (Distearoylethyl

Dimonium Chloride, Cetearyl 0.5

Alcohol; Evonik)

EXAMPLE 4

[0222] This example illustrates formulations comprising polyelectrolyte complexes and charged polymers.

[0223] All Compositions 4B-4E exhibited freeze-thaw stability. The present inventors also surprisingly found that Composition 4D, which contains Salcare^® SC 96, exhibited superior long-term controlled viscosity (wherein the viscosity remained stable long-term), relative to Compositions 4B, 4C, and 4E.

[0224] Comparative Composition 4A does not include PECs, whereas Compositions 4B- 4E comprise PVMMA:polyquat-28 PECs and charged compounds and/or polymers. All compositions are rinse-out conditioners. The sodium hydroxide/citric acid/aspartic acid are adjusted to achieve the proper pH, if necessary.

[0225] "MS" represents Match Standard.

[0226] Compositions 4A-4E

ragrance . . . . .

Target Specifications 4A

pH 4.00-5.00

Viscosity (RV T-B, 10 rpm, 1 min, 25C)

bulk 5,000-9,000 cps

w/ shear (finished goods) 10,000-30,000 cps

Color White (MS)

Odor MS

Appearance Viscous, opaque emulsion

Target Specifications 4B

pH 4.50-6.00

Viscosity (RV T-B, 10 rpm, 1 min, 25C)

bulk 7,000-15,000 cps

w/ shear (finished goods) 20,000-35,000 cps

Color White (MS)

Odor MS Appearance: Viscous, opaque emulsion

Target Specifications 4C:

pH: 4.50-6.00

Viscosity (RV T-B, 10 rpm, 1 min, 25C):

bulk: 7,000-15,000 cps

w/ shear (finished goods): 20,000-35,000 cps

Color: White (MS)

Odor: MS

Appearance: Viscous, opaque emulsion

Target Specifications 4D

pH 4.50-6.00

Viscosity (RV T-B, 10 rpm, 1 min, 25C)

bulk 7,000-15,000 cps

w/ shear (finished goods) 20,000-35,000 cps

Color White (MS)

Odor MS

Appearance Viscous, opaque emulsion

Target Specifications 4E:

pH: 4.50-6.00

Viscosity (RV T-B, 10 rpm, 1 min, 25C):

bulk: 7,000-15,000 cps

w/ shear (finished goods): 20,000-35,000 cps

Color: White (MS)

Odor: MS

Appearance: Viscous, opaque emulsion

EXAMPLE 5

[0227] This example demonstrates methods of making the compositions of Example 4.

[0228] For Comparative Composition 4A, start heating container to 80-85 °C and add the following: DI water, citric acid, and disodium EDTA. Check that that the temperature is 80- 85 °C and add the following: Quat-18/water, stearamidopropyl dimethyl amine, cetyl alcohol, and stearyl alcohol. Vigorously mix for 30 minutes at 80-85 °C. Cool the mixture. At 57-60 °C, slowly add the L-aspartic acid. At 45 °C or below, add the following:

isostearamidopropyl ethyldimonium ethosulfate/PEG-9,

cyclopentasiloxane/cyclohexasiloxane/dimethicone, fragrance, and DMDM hydantoin.

[0229] Compositions 4B, 4C, and 4E are prepared using two phases. For Composition 4B, in the Main Phase, add 52.05 wt. % (of the final total wt. % of the composition) of DI water. Start heating to 80-85 °C. Add the following one at a time and mix until fully dissolved and solution becomes clear: disodium EDTA and L-aspartic acid. Add the following one at a time at 80-85 °C and mix until melted: stearamidopropyl dimethylamine (check to make sure solution has turned clear), cetyl alcohol, and glyceryl stearate.

Vigorously mix for 30 minutes at 80-85 °C. After 30 minutes, turn off heat, slow the mixing speed, and allow the composition to slowly cool. In the Side Phase, add 15.5 wt. % (of the final total wt. % of the composition) of DI water and slowly add the following, and mix until hydrated: PVMMA Copolymer (Gantrez^® S-97 BF; ISP Corp., Wayne, NJ, USA) and sodium hydroxide (20% active). The solution will slightly thicken. The in-process pH should be 6.90-7.00. Heat the Side Phase to 50-55 °C. Slowly add the Polyquaternium-28 (Conditioneze^® NT-20; ISP Corp.) under very vigorous mixing. The solution will turn opaque and become less viscous. Cool the Side Phase, and at < 45 °C add 0.05 wt. % (of the final total wt. % of the composition) of DMDM hydantoin. Slowly add the Side Phase to the Main Phase at < 45 °C. Then add the following: Abil^® T Quat 60 (silicone quaternium-22; Evonik, Essen, Germany), propylene glycol, fragrance, and 0.15 wt. % (of the final total wt. % of the composition) of DMDM hydantoin.

[0230] For Composition 4C, in the Main Phase, add 52.45 wt. % (of the final total wt. % of the composition) of DI water. Start heating to 80-85 °C. Add the following one at a time and mix until fully dissolved and solution becomes clear: disodium EDTA and L-aspartic acid. Add the following one at a time at 80-85 °C and mix until melted: stearamidopropyl dimethylamine (check to make sure solution has turned clear), cetyl alcohol, and glyceryl stearate. Vigorously mix for 30 minutes at 80-85 °C. After 30 minutes, turn off heat, slow the mixing speed, and allow the composition to slowly cool. In the Side Phase, add 15.5 wt. % (of the final total wt. % of the composition) of DI water and slowly add the following, and mix until hydrated: PVMMA Copolymer (Gantrez^® S-97 BF; ISP Corp., Wayne, NJ, USA) and sodium hydroxide (20% active). The solution will slightly thicken. The in-process pH should be 6.90-7.00. Heat the Side Phase to 50-55 °C. Slowly add the Polyquaternium-28 (Conditioneze^® NT-20; ISP Corp.) under very vigorous mixing. The solution will turn opaque and become less viscous. Cool the Side Phase, and at < 45 °C add 0.05 wt. % (of the final total wt. % of the composition) of DMDM hydantoin. Slowly add the Side Phase to the Main Phase when at < 45 °C. Pre-mix the quaternium-80/propylene glycol and dimethicone and then add to the combined Main and Side Phase. Then add the following: DC-8500 (Bis (CI 3-15 Alkoxy) PG Amodimethicone; Dow Corning, Midland, MI, USA), propylene glycol, fragrance, and 0.15 wt. % (of the final total wt. % of the composition) of DMDM hydantoin.

[0231] For Composition 4D, add 40 wt. % (of the final total wt. % of the composition) of DI water. Slowly add the following, and mix until hydrated: PVMMA Copolymer (Gantrez^® S-97 BF (ISP)) and sodium hydroxide (20% active). The solution will slightly thicken. The in-process pH should be 6.90-7.00. Heat to 50-55 °C, and slowly add the Polyquaternium-28 (Conditioneze^® NT-20 (ISP)) under very vigorous mixing. The solution will turn opaque and become less viscous. Start heating to 80-85 °C, and add the following one at a time, mixing until fully dissolved: disodium EDTA, L-aspartic acid, and 22.95 wt. % (of the final total wt. % of the composition) of DI water. Add the following one at a time at 80-85 °C, and mix until melted: stearamidopropyl dimethylamine, cetyl alcohol, stearyl alcohol, glyceryl stearate, Crodamol STS (PPG-3 Benzyl Ether Myristate; Croda Inc., Edison, NJ, USA), Salcare^® SC 96 (65% polyquaternium-37, 25% propylene glycol dicaprylate/dicaprate, 10% PPG-1 trideceth-6; Ciba^®/BASF, Basel, Switzerland). Mix vigorously for 30 minutes at 80- 85 °C. Reduce the mixing speed and allow the composition to cool. When the temperature is <45 °C, add the following: D5/D6/Dimethicone, propylene glycol, fragrance, and DMDM hydantoin.

[0232] For Composition 4E, in the Main Phase, add 50.47 wt. % (of the final total wt. % of the composition) of DI water. Start heating to 80-85 °C. Add the following one at a time and mix until fully dissolved and solution becomes clear: disodium EDTA and L-aspartic acid. Add the following one at a time at 80-85 °C and mix until melted: stearamidopropyl dimethylamine (check to make sure solution has turned clear), cetyl alcohol, glyceryl stearate, Montanov^® 202 (arachidyl alcohol and behenyl alcohol and arachidyl glucoside; SEPPIC, Paris, France), and aminopropyl dimethicone. Vigorously mix for 30 minutes at 80- 85 °C. After 30 minutes, turn off heat, slow the mixing speed, and allow the composition to slowly cool. In the Side Phase, add 15.5 wt. % (of the final total wt. % of the composition) of DI water and slowly add the following, and mix until hydrated: PVMMA Copolymer (Gantrez^® S-97 BF; ISP Corp., Wayne, NJ, USA) and sodium hydroxide (20% active). The solution will slightly thicken. The in-process pH should be 6.90-7.00. Heat the Side Phase to 50-55 °C. Slowly add the Polyquaternium-28 (Conditioneze^® NT-20; ISP Corp.) under very vigorous mixing. The solution will turn opaque and become less viscous. Cool the Side Phase, and at < 45 °C add 0.05 wt. % (of the final total wt. % of the composition) of DMDM hydantoin. Slowly add the Side Phase to the Main Phase when at < 45 °C. At 45 °C or below, add the Merquat^® 2001 (polyquaternium-47; Nalco, Naperville, IL, USA). Pre-mix the D5/dimethiconol and dimethicone and then add to the combined Main and Side Phase. Then add the following: DC-8500 (Bis (C13-15 Alkoxy) PG Amodimethicone; Dow Corning, Midland, MI, USA), propylene glycol, fragrance, and 0.15 wt. % (of the final total wt. % of the composition) of DMDM hydantoin.

EXAMPLE 6

[0233] This example demonstrates the mending of split-ends of hair fibers using a test method of the present invention.

[0234] Below compares the compositions used in this study that are presented in Figure 1. The sodium hydroxide/aspartic acid are adjusted to achieve the proper pH, if necessary.

[0235] Compositions 6A-6D

Fragrance 0.6 0.6 0.6 0.6

[0236] Below compares compositions used in this study as presented in Figure 2. The sodium hydroxide/citric acid/aspartic acid are adjusted to achieve the proper pH, if necessary.

[0237] Compositions 6E to 6J

propane an

[0238] Figure 1 shows the results of mending for conditioners when using twice-bleached European hair with split-ends produced mechanically. The results show about 80% mending with the rinse-off conditioners in three cycles.

[0239] Figure 2 shows the results of various compositions when using twice-bleached European hair with split-ends produced mechanically. The results are based on the assumption that all formulas are left in, including Night Repair. The results show greater than 80% for all leave-in compositions in one treatment.

EXAMPLE 7

[0240] This example demonstrates the mending of split-ends of hair fibers using a test method of the present invention.

[0241] Below compares compositions used in this study. The sodium hydroxide/aspartic acid are adjusted to achieve the proper pH, if necessary. [0242] Compositions 7A-7D

sulfosuccinate (about

34% active)

Styrene/VP 0 0.75 0 0 copolymer (40%),

water

PEG-6 caprylic/capric 0 0.6 0 0 triglyceride

Kathon CG 0 0.07 0 0

Sodium chloride 0 2.5 0 0

Target Specifications 7A:

pH: 4.50-6.00

Viscosity (RV T-B, 10 rpm, 1 min, 25C): 5,000-15,000 cps

Color: White (MS)

Odor: MS

Appearance: Opaque emulsion

Target Specifications 7B:

pH 5.5-6.5

Viscosity (LVT/spindle 4/30 rpm/ 1 min, 25C) 15,000-20,000 cps

Color White/Off white (MS)

Odor MS

Appearance: Viscous, opaque liquid

Target Specifications 7C:

pH: 4.50-6.00

Viscosity (RV T-B, 10 rpm, 1 min, 25C): 15,000-25,000 cps

Color: White (MS)

Odor: MS

Appearance: Viscous, opaque emulsion

Target Specifications 7D

pH 4.50-6.00

Viscosity (RV T-B, 10 rpm, 1 min, 25C) 10,000-20,000 cps

Color White (MS)

Odor MS

Appearance Opaque emulsion

[0243] Fifty hair fibers containing split-ends were removed from hair tresses. The hair fiber samples were placed on glass slides aligned along a strip of double stick tape for optical imaging. Each fiber selected with a split-end was individually photographed and the image was stored before product application, using a WILD stereomicroscope at a magnification of about 25X with transmitted light emanating. The fibers were also rotated prior to image capture to make sure that the split-ends were in view.

[0244] The product application protocol listed below was followed. In each case, the 50 selected fibers with split-ends were placed respectively in five different tresses and then the product applied. Optical images of tip ends of the respective selected fibers were obtained again to examine and assess extent of split-end mending. The results appear in Table 12.

[0245] Table 12 shows a summary of the split-end data study comparing the total number of split-ends before treatment (50) to the number of split-ends repaired after treatment. (The split-ends for the repeat study, category 6, were prepared by a separate method).

[0246] Table 12

[0247] All categories show ability to mend split-ends in hair fibers, three of them showing improvements of 90% or more.

[0248] Product Application Protocol

[0249] Protocols are listed in the order presented in Table 12. To achieve 80% dry tresses for some compositions (as noted below), blow drying time was changed from 5 minutes to 20 minutes because of the nature of the blow dryer (mild air flow).

[0250] A. Pre-cleansing the Hair

1. Clean the wax-strip bound Platinum (2x) bleached hair by soaking in a 5% w/w solution of Sodium Lauryl Ether Sulfate (1M) solution. The solution to hair ratio is 40: 1. Soak for 30 minutes at room temperature, and then massage the hair by hand for 3 minutes before rinsing under 40°C tap water until all the bubbles are rinsed out.

2. Blot the hair dry with tissue paper or a towel, comb straight, and leave the hair to dry at ambient room temperature overnight.

[0251] B. Causing Split-Ends - Mechanically

1. The tresses are swatched by International Hair Importers in a way that the density of the hair is linear. Prepare 5 tresses that are 1.5" wide, cut and tape so that there is 6g of hair in each tress.

2. Attach each tress to the repeated combing machine and comb the tress 1500 times per side for a total of 3000 combings per tress.

3. During the combing, the blow dryer is positioned 8 inches from the tress and turned on high heat setting. The air flow is directed towards the bottom of the hair tress so that the hair is pushed towards the comb during repeated combing.

[0252] C. Selecting the Split-Ends from the Tress and Taking Initial Pictures

1. Using a magnifying glass, examine the tip of the tresses to find hair fibers with split-ends. Select and remove 50 fibers with split-ends from the tress by the root. Select 10 split-end fibers out of each tress so that 50 fibers can be pulled from the five tresses.

2. Crimp the fibers at the root end using metal crimps, and then line up the crimps to be placed on tape so that there are 10 fibers on each tape strip. Cover up the crimps using another tape so that they can be easily picked up together.

3. Number all 50 fibers and take optical images of 10 out of the 50 hair fibers for before and after pictures.

4. Using a red permanent marker, mark each of the selected 50 fibers up to the beginning of the split.

5. Take optical images of 10 split-ends by mounting the split-ends on glass slides. A stereomicroscope at a magnification of 50X with transmitted light emanating from under the stage of the microscope is used to take the pictures.

6. Examine the other 40 fibers with split-ends using the stereomicroscope, but they do not need to be photographed. 7. The strip of tape that contains split-ends is placed back in the middle 1.5" tress.

8. Clamp the tress with the split-end fibers using a large clip such as a binder clip.

[0253] D. Composition Application - Category 1

1. Wet the hair tress for 30 seconds under 35-40 °C water at 1 GPM.

2. Apply 1.5 ml of a non-conditioning shampoo to the 1.5 inch tress and massage for 1 minute.

3. Rinse the tress for 30 seconds under 35-40 °C water at 1 GPM.

4. Wring out the excess water by sliding the tress between fingers.

5. Mount the top of the tress to a stand for blow drying.

6. Clip the tress at ¾ of its length with a hair clip to avoid flyway hair.

7. Blow dry the tress at medium heat with the dryer being 2 ft away from the tress for about 3 minutes.

8. Apply 1.5 ml of Composition 7 A, leave in treatment, to the 1.5 inch damp tress evenly on both sides. Massage for 1 minute focusing to the ends and split-end prone areas.

9. Comb once on each side of the tress.

10. Mount the top of the tress to a stand for blow drying.

1 1. Clip the tress at ¾ of its length with a hair clip to avoid flyway hair.

12. Blow dry the tress at medium heat (mild air flow) with the dryer being 2 ft away from the tress until it is 80% dry for about 20 minutes.

13. After blow drying, comb the tress once on each side.

[0254] D. Composition Application - Category 2

1. Wet the hair tress for 30 seconds under 35-40 °C water at 1 GPM.

2. Apply 1.5 ml of Composition 7B (shampoo) to the 1.5 inch tress and massage for 1 minute.

3. Rinse the tress for 30 seconds under 35-40 °C water at 1 GPM.

4. Wring out the excess water by sliding the tress between fingers.

5. Apply 1.5 ml of Composition 7C (conditioner) to the 1.5 inch tress and stroke the tress 9 times from top to bottom and let it stand for 1 minute.

6. Rinse the tress for 30 seconds under 35-40 °C water at 1 GPM.

7. Blot dry the tress gently using Kim Wipes. 8. Mount the top of the tress to a stand for blow drying.

9. Clip the tress at ¾ of its length with a hair clip to avoid flyway hair.

10. Blow dry the tress at medium heat with the dryer being 2 ft away from the tress for 3 minutes.

1 1. Apply 1.5 ml of Composition 7A, leave in treatment, to the 1.5 inch damp tress. Massage for 1 minute focusing on the ends and split-end prone areas.

12. Comb the tress once on each side.

13. Mount the top of the tress to a stand for blow drying.

14. Clip the tress at ¾ of its length with a hair clip to avoid flyway hair.

15. Blow dry the tress at medium heat (mild air flow) with the dryer being 2 ft away from the tress until it is 80% dry for about 20 minutes.

16. After blow drying, comb through the tress twice on each side.

[0255] D. Composition Application - Category 3

1. Wet the hair tress for 30 seconds under 35-40 °C water at 1 GPM.

3. Rinse the tress for 30 seconds under 35-40 °C water at 1 GPM.

4. Wring out the excess water by sliding the tress between fingers.

5. Mount the top of the tress to a stand for blow drying.

6. Clip the tress at ¾ of its length with a hair clip to avoid flyway hair.

8. Apply 1.5 ml of Composition 7D, overnight treatment, to the damp 1.5 inch tress to both sides of the tress. Massage for 1 minute focusing on the ends and split-end prone areas.

9. Comb the tress once on each side.

10. Let the composition stand on the hair for 8 hours since this is an overnight treatment.

11. Clip the tress at ¾ of its length with a hair clip to avoid flyway hair.

[0256] D. Composition Application - Category 4

1. Wet the hair tress for 30 seconds under 35-40 °C water at 1 GPM.

2. Apply 1.5 ml of a non-conditioning shampoo to the 1.5 inch tress and massage for 1 minute. 3. Rinse the tress for 30 seconds under 35-40 °C water at 1 GPM.

4. Wring out the excess water by sliding the tress between fingers.

5. Apply 1.5 ml of Composition 7C to the 1.5 inch tress and stroke the tress 9 times from top to bottom and let it stand for 1 minute.

6. Rinse the tress for 30 seconds under 35-40 °C water at 1 GPM.

7. Blot dry the tress gently using Kim Wipes.

8. Mount the top of the tress to a stand for blow drying.

9. Clip the tress at ¾ of its length with a hair clip to avoid flyway hair.

10. Blow dry the tress at medium heat with the dryer being 2 ft away from the tress until it is 80% dry for about 5 minutes.

11. Comb through the tress twice on each side.

12. Reapply the red markings on the fiber after blow drying

13. Repeat steps 1 to 12 for an additional 2 more cycles, so there is total of three treatments.

[0257] D. Composition Application - Category 5

1. Wet the hair tress for 30 seconds under 35-40 °C water at 1 GPM.

3. Rinse the tress for 30 seconds under 35-40 °C water at 1 GPM.

4. Wring out the excess water by sliding the tress between fingers.

6. Rinse the tress for 30 seconds under 35-40 °C water at 1 GPM.

7. Blot dry the tress gently using Kim Wipes.

8. Comb through the tress once on each side.

9. Mount the top of the tress to a stand for blow drying.

10. Clip the tress at ¾ of its length with a hair clip to avoid flyway hair.

1 1. Blow dry the tress at medium heat (mild air flow) with the dryer being 2 ft away from the tress until it is 80% dry for about 20 minutes.

12. Comb through twice on each side.

13. Repeat steps 1 to 12 for an additional 2 more cycles, so there is a total of three treatments.

[0258] E. Selecting the Split-ends from the Tress and Taking Final Pictures 1. Remove the strip of tape that contains split-ends from the middle of the 1.5" tress.

2. Using the stereomicroscope, take the after treatment optical images of the 10 hair fibers with split-ends by mounting the split-ends on glass slides.

3. Examine the other 40 fibers with split-ends using the stereomicroscope.

4. Count the number of fibers that have been mended to determine % mending.

EXAMPLE 8

[0259] This example demonstrates methods of communicating split-end mending to consumers.

[0260] Figure 3 is a schematic showing the mending of a split-end using polyelectrolyte complexes (PECs). The PECs are shown here in a possible mechanism of action where they attach to the site of the split-end, form a network with themselves and the fiber assembly, and shrink as they dry binding the split end from within.

[0261] Figures 4A-4D show still photography of the mending of a variety of split-end types using methods as described herein with compositions as described herein.

[0262] Figure 5 shows still frames from a video of the mending of split-ends through the process of mending method as described herein.

EXAMPLE 9

[0263] This example demonstrates additional compositions of the present invention.

[0264] Composition 9A

Main Phase wt%

DI Water 45.0397

Aminomethyl Propanol (AMP-95) 0.02

Add the following under very vigorous mixing for 30 mins.

"Ultrathix P-100" (Acrylic Acid/VP Crosspolymer) 1

Add the following and mix until uniform

Aminomethyl Propanol (AMP-95) 0.44

Side Phase 1

DI Water 20

Sprinkle in the following and mix until clear

Polyquaternium-4 (Celquat H-100) 0.5

Disodium EDTA 0.05

Liquid Additions:

PVP K-90 (20% active) 1 VP/Methacrylamide/Vinyl Imidazole Copolymer ("Luviset

Clear" (BASF)) - 20% active 3.5

Polyquaternium-39 (8.5% active) 0.5

Propylene Glycol 1

Sorbitol (70%) 0.5

Add Side Phase 1 to main tank and mix until uniform

Side Phase 2

DI Water 15.5

Slowly add the following, mix until hydrated

PVM/MA Copolymer (Gantrez S-97 BF (ISP)) 0.2

Sodium Hydroxide (20% active) 0.25

(solution will slightly thicken)

In-process pH specification: 6.90-7.00

Heat Side Phase to 50-55C

Slowly add the following under very vigorous mixing

Polyquaternium-28 (Conditioneze NT-20 (ISP), 20% active) 9

(solution will turn opaque and become less viscous)

DMDM Hydantoin 0.05

Slowly add Side Phase 2 to main tank and mix until uniform

< 45C

Pre-mix next two and fragrance

PEG-40 Hydrogenated Castor Oil 0.6

PEG/PPG-18/18 Dimethicone (DC- 190) 0.1

Fragrance 0.6

Cocos Nucifera (Coconut) Oil 0.0001

Keratin Amino Acids 0.0001

Flower/Leaf Extract 0.0001

DMDM Hydantoin 0.15

Target Specifications 9A:

pH: 6.0-7.0

Viscosity (RV T-C, 5 rpm, 1

min, 25C) 40,000-80,000

Color White (MS)

Odor MS

Appearance: Viscous, opaque (hazy)

gel ompositions 9B-1 and 9B-2

9B-1 9B-2

Main Phase wt% wt%

64.755325 59.5249

Target Specifications 9B:

(Bulk) (Finished Goods) pH 5.0-6.5 5.0-6.5

Color off white (MS) white (ms)

Odor MS MS

Appearance: hazy liquid dense foam, non-watery, non-runny Non-Volatiles:

Foam Stability: 200 seconds min.

Vacuum: 16-18 in.

Vapor Pressure at 70F: 69-74 psig Vapor Pressure at 13 OF: 140-145 psig Spray Pattern/Diameter: Foam Composition 9C-1

Item wt%

Main Phase

DI Water 93.33163

PVM/MA Copolymer (Gantrez S-97 BF (ISP)) 0.001

NaOH, 20% 0.00125

Add the following and mix vigorously

Polyquaternium-28 (Conditioneze NT-20 (ISP), 20%

active) 0.045

Disodium EDTA 0.02

PVP 0.45

Stearalkonium Chloride 1

Heat to 170-175F and mix for 30 min

Cool the batch down to 90-95F

Glycerin 1

[DC-949]

60% Amodimethicone, 5% Trideceth-12, 5% Cetrimonium

Chloride, 30% Water 2

PEG- 12 Dimethicone 0.5

Propylene Glycol 0.5

Triethanolamine 0.00001

Citric Acid 0.00001

DMDM Hydantoin 0.3

Hydrolyzed Silk 0.05

Water, Polysorbate20, Ascorbic Acid, Panthenol,

Tocopherol Acetate, Biotin, Niacinamide 0.001

Water, Polyglyceryl-3 Distearate, Polysorbate 60, Myristic

Acid, Palmitic Acid, Stearic Acid, Guar

Hydroxypropyltrimonium Chloride, Triticum Vulgare

(Wheat) Flour Lipids, Ceramide 3, Persea Gratissima

(Avocado) Oil, Tetrahexyldecyl Ascorbate, Glycine Soja

(Soybean) Sterols, Alpha-Glucan Oligosaccharide,

Ethylhexyl Methoxycinnamate, Butyl

Methoxydibenzoylmethane, Tocopheryl Acetate 0.0001

Premix the following and add to the batch

Polysorbate20 0.4

Fragrance 0.4 Target Specification 9C-1 :

pH: 4.0-5.0

Color: Cloudy/Pale white Odor: To match reference Appearance: Milky liquid mposition 9C-2

Target Specification 9C:

pH: 4.5-6

Color: White

Odor: To match reference Appearance: Milky liquid 68] Compositions 9D-1 and 9D-2

Target Specifications 9D: Bulk

Color off white (MS)

Odor MS

Appearance hazy liquid

pH 5.0-6.5

Specific

Gravity: * 0.986

Non-Volatiles: 4.4-4.9%

(T=4.66)

Finished Product

Color: white (MS)

Odor: MS

Appearance: dense foam, non- watery, non- runny

pH: 5.0-6.5

Foam Stability: 200 seconds min

Foam Density: * 0.039 g/mL

Specific

Gravity: * 0.941

4.3-4.8%

Non-Volatiles: (T=4.58)

* for reference omposition 9E

Main Phase t%

DI Water 57.5647

Aminomethyl Propanol (AMP-95) 0.02

Add the following under very vigorous mixing for 30 mins.

"Ultrathix P-100" (Acrylic Acid/VP Crosspolymer) 1

Add the following and mix until uniform

Aminomethyl Propanol (AMP-95) 0.44

Side Phase 1

DI Water 20

Sprinkle in the following and mix until clear

Polyquaternium-4 (Celquat H-100) 0.5

Liquid Additions:

PVP K-90 (20% active) 1

VP/Methacrylamide/Vinyl Imidazole Copolymer ("Luviset

Clear" (BASF)) - 20% active 3.5

Polyquaternium-39 (8.5% active) 0.5

Propylene Glycol 1

Sorbitol (70%) 0.5 Add Side Phase 1 to main tank and mix until uniform

Side Phase 2

DI Water 7.75

Slowly add the following, mix until hydrated

PVM/MA Copolymer (Gantrez S-97 BF (ISP)) 0.1

Sodium Hydroxide (20% active) 0.125

(solution will slightly thicken)

In-process pH specification: 6.90-7.00

Heat Side Phase to 50-55C

Slowly add the following under very vigorous mixing

Polyquaternium-28 (Conditioneze NT-20 (ISP), 20% active) 4.5

(solution will turn opaque and become less viscous)

Add the following at < 45C

DMDM Hydantoin 0.025

Slowly add Side Phase 2 to main tank and mix until uniform

< 45C

Pre-mix next two and fragrance

PEG-40 Hydrogenated Castor Oil 0.6

PEG/PPG-18/18 Dimethicone (DC-190) 0.1

Fragrance 0.6

Cocos Nucifera (Coconut) Oil 0.0001

Keratin Amino Acids 0.0001

Flower/Leaf Extract 0.0001

DMDM Hydantoin 0.175

Target Specifications 9E:

pH: 6.0-7.0

Viscosity (RV T-C, 5 rpm, 1 min, 25C): 40,000-80,000

Color: White (MS)

Odor: MS

Appearance: Viscous, opaque (hazy)

gel

[0270] Compositions 9F-1 through 9F-4

9F-1 9F-2 9F-3 9F-4

Item wt% wt% wt% wt%

Main Phase

DI Water 74.2247 73.2247 71.2247 69.2247

Sprinkle in the following and mix until clear

Polyquaternium-4 (Celquat H-100) 0.5 0.5 0.5 0.5

Vinyl Caprolactum/VP/Dimethylaminoethyl

Methacrylate Copolymer ("Advantage S" (ISP)) 0.5 0.25 1 0.5 Liquid Additions

POLYQUATERNIUM-1 1 , WATER (20% active) 2.5 2.5 2.5 5

VP/Methacrylamide/Vinyl Imidazole Copolymer

("Luviset Clear" (BASF)) - 20% active 2.5 3.75 5 5

Polyquatemium-39 (8.5% active) 0.5 0.5 0.5 0.5

Propylene Glycol 1 1 1 1

Sorbitol (70%) 0.5 0.5 0.5 0.5

Side Phase

DI Water 7.75 7.75 7.75 7.75

Slowly add the following, mix until hydrated

PVM/MA Copolymer (Gantrez S-97 BF (ISP)) 0.1 0.1 0.10 0.1

Sodium Hydroxide (20% active) 0.125 0.125 0.125 0.125

(solution will slightly thicken)

In-process pH specification: 6.90-7.00

Heat Side Phase to 50-55C

Slowly add the following under very vigorous

mixing

Polyquaternium-28 (Conditioneze NT-20 (ISP),

20% active) 4.5 4.5 4.5 4.5

(solution will turn opaque and become less

viscous)

(mix for ~10 minutes)

Add the following at < 45C

DMDM Hydantoin 0.025 0.025 0.025 0.025

Slowly add side phase to main phase at < 45C

< 45C

Pre-mix next two and fragrance

PEG-40 Hydrogenated Castor Oil 0.5 0.5 0.5 0.5

PEG/PPG-18/18 Dimethicone (DC- 190) 0.1 0.1 0.1 0.1

Fragrance 0.5 0.5 0.5 0.5

DMDM Hydantoin 0.175 0.175 0.175 0.175

Cocos Nucifera (Coconut) Oil 0.0001 0.0001 0.0001 0.0001

Keratin Amino Acids 0.0001 0.0001 0.0001 0.0001

Flower/Leaf Extract 0.0001 0.0001 0.0001 0.0001

Add the following and mix until uniform

"Sepigel 305" 4 4 4 4

Mix until uniform

Target Specifications 9F

pH 7.00-7.50

Viscosity (RV T-C, 5 rpm, 1 min, 25C) 50,000-100,000 cps

Color clear-semi white

Odor MS

Appearance thick gel [0271] Compositions 9G-1 through 9G-4

Target Specifications 9G:

pH: Viscosity (RV T-B, 10 rpm, 1 rain, 25C) 20,000-40,000 cps

Color Semi-Translucent - white (MS)

Odor MS

Appearance Viscous, opaque gel Compositions 9H-1 and 9H-2

9H-1 9H-2

Item wt% wt%

Main Phase

DI Water 75.625 74.125

Sprinkle in the following and mix until clear

Polyquaternium-4 (Celquat H-100) 0.5 0.5

Vinyl Caprolactum/VP/Dimethylaminoethyl Methacrylate

Copolymer ("Advantage S" (ISP)) 0 0.25

POLYQUATERNIUM-11 , WATER (20% active) 2.5 1.25

VP/Methacrylamide/Vinyl Imidazole Copolymer

("Luviset Clear" (BASF)) - 20% active 0 2.5

PEC Pre-mix

DI Water 7.75 7.75

Slowly add the following, mix until hydrated

PVM/MA Copolymer (Gantrez S-97 BF (ISP)) 0.1 0.1

Sodium Hydroxide (20% active) 0.125 0.125

(solution will slightly thicken)

In-process pH specification: 6.90-7.00

Heat to 50-55C

Slowly add the following under very vigorous mixing

Polyquaternium-28 (Conditioneze NT-20 (ISP)) 4.5 4.5

(solution will turn opaque and become less viscous)

mix for 10 minutes

Add the following at < 45C

DMDM Hydantoin 0.025 0.025

Slowly add side phase to main phase at < 45C

< 45C

Silicone Premix

Dimethicone (60,000 est) 2 2

Phenyl Trimethicone (DC-556) 2 2

Cyclopentasiloxane, Dimethiconol 1 1

Glycerin 1 1

Propylene Glycol 0.5 0.5

Fragrance 0.2 0.2

DMDM Hydantoin 0.175 0.175 "Salcare^® SC-96" - Ciba/BASF (65% Polyquatemium-37,

25% Propylene Glycol Dicaprylate Dicaprate, 10% PPG-1

Trideceth-6) 2 2

Mix until uniform

Target Specifications 9H

pH 5.00-6.50

Viscosity (RV T-B, 10 rpm, 1 min, 25C) 5,000-15,000 cps

Color: Semi-Translucent white (MS)

Odor MS

Appearance Viscous, milky liquid

[0273] Compositions 91-1 through 91-3

91-1 91-2 91-3

Item wt% wt% wt%

Main Phase

DI Water 51.3247 62.3247 68.3247

Sprinkle in the following and mix until clear

Polyquaternium-4 (Celquat H-100) 0.5 0.5 0.5

Vinyl Caprolactum/VP/Dimethylaminoethyl Methacrylate

Copolymer ("Advantage S" (ISP)) 0.25 0.25 0.25

Disodium EDTA 0.05 0.05 0.05

L-Aspartic Acid 0.75 0.75 0.75

Add the following one at a time at 80-85C and mix until

melted/homogeneous

Stearamidopropyl Dimethylamine 2 2 2

Cetyl Alcohol 1 1 1

Glyceryl Stearate 0.2 0.2 0.2

Mix vigorously for 30 minutes at 80-85C

Reduce mixing speed; allow to cool and foam to reduce

Liquid Additions:

POLYQUATERNIUM-1 1 , WATER (20% active) 1.25 1.25 1.25

VP/Methacrylamide/Vinyl Imidazole Copolymer ("Luviset Clear"

(BASF)) - 20% active 2.5 2.5 2.5

Side Phase

DI Water 7.75 7.75 7.75

Slowly add the following, mix until hydrated

PVM/MA Copolymer (Gantrez S-97 BF (ISP)) 0.1 0.1 0.1

Sodium Hydroxide (20% active) 0.125 0.125 0.125

(solution will slightly thicken)

In-process pH specification: 6.90-7.00

Heat Side Phase to 50-55C

Mix until uniform

Target Specifications 91

pH 4.50-6.00

Viscosity (RV T-B, 10 rpm, 1 min, 25C) 20,000-30,000 cps

Color White (MS)

Odor MS

Appearance Viscous opaque lotion

[0274] Compositions 9J-1 through 9J-3

9J-1 9J-2 9J-3

Item wt% wt% t%

Main Phase

DI Water 25.8247 25.8247 25.8247

Glycerin 35 0 35

Propylene Glycol 0 35 0

Silicone Pre-Mix

"Abil OSW 5" - Evonik (84% Cyclopentasiloxane, 15%

Dimethiconol, 1 % Dimethicone) 22 20 20

Amodimethicone (ADM 1100 (Wacker)) 2 2 2

Phenyl Trimethicone (DC-556) 0 2 2

Fragrance 0.5 0.5 0.5 DMDM Hydantoin 0.175 0.175 0.175

Cocos Nucifera (Coconut) Oil 0.0001 0.0001 0.0001

Keratin Amino Acids 0.0001 0.0001 0.0001

Flower/Leaf Extract 0.0001 0.0001 0.0001

Sepigel 305 2 2 2

Mix moderately for ~30 minutes and until smooth

Side Phase

DI Water 7.75 7.75 7.75

Slowly add the following, mix until hydrated

PVM/MA Copolymer (Gantrez S-97 BF (ISP)) 0.1 0.1 0.1

Sodium Hydroxide (20% active) 0.125 0.125 0.125

(solution will slightly thicken)

In-process pH specification: 6.90-7.00

Heat Side Phase to 50-55C

Slowly add the following under very vigorous mixing

Polyquaternium-28 (Conditioneze NT-20 (ISP), 20% active) 4.5 4.5 4.5

(solution will turn opaque and become less viscous)

(mix for ~10 minutes)

Add the following at < 45 C

DMDM Hydantoin 0.025 0.025 0.025

Slowly add side phase to main phase at < 45C

Mix until uniform

Target Specifications 9J:

pH 7.0-8.0

Viscosity (RV T-B, 10 rpm, 1 min, 25C) 5,000-15,000 cps

Color: colorless-slightly yellow

Odor MS

Appearance slightly hazy oily liquid

[0275] Compositions 9K-1 through 9K-3

9K-1 9K-2 9K-3

Item wt% wt% wt%

Main Phase

DI Water 21.3247 31.3247 36.3247

Sprinkle in the following and mix until clear

Polyquaternium-4 (Celquat H-100) 0.5 0.5 0.5

Vinyl Caprolactum/VP/Dimethylaminoethyl Methacrylate

Copolymer ("Advantage S" (ISP))

0.25 0.25 0.25

Glycerin 35 35 35

POLYQUATERNIUM-1 1 , WATER (20% active) 1.25 1.25 1.25 VP/Methacrylamide/Vinyl Imidazole Copolymer ("Luviset Clear"

(BASF)) - 20% active 2.5 2.5 2.5

Side Phase

DI Water 7.75 7.75 7.75

Slowly add the following, mix until hydrated

PVM/MA Copolymer (Gantrez S-97 BF (ISP)) 0.1 0.1 0.1

Sodium Hydroxide (20% active) 0.125 0.125 0.125

(solution will slightly thicken)

In-process pH specification: 6.90-7.00

Heat Side Phase to 50-55C

Slowly add the following under very vigorous mixing

Polyquaternium-28 (Conditioneze NT-20 (ISP), 20% active) 4.5 4.5 4.5

(solution will turn opaque and become less viscous)

(mix for ~10 minutes)

Add the following at < 45C

DMDM Hydantoin 0.025 0.025 0.025

Slowly add side phase to main phase at < 45C

< 45C

"Abil OSW 5" - Evonik (84% Cyclopentasiloxane, 15%

Dimethiconol, 1 % Dimethicone) 20 10 5

"DC-8500" - Dow Corning (82% Bis(C13-15 Alkoxy) PG- Amodimethicone, 18%> C14-15 Alcohols) 2 1.5 1

Phenyl Trimethicone (DC-556) 2 1.5 1

Fragrance 0.5 0.5 0.5

DMDM Hydantoin 0.175 0.175 0.175

Cocos Nucifera (Coconut) Oil 0.0001 0.0001 0.0001

Keratin Amino Acids 0.0001 0.0001 0.0001

Flower/Leaf Extract 0.0001 0.0001 0.0001

Add the following and mix until uniform

"Sepigel 305" 2 3 4

Target Specifications 9K

pH 7.0-8.0

Viscosity (RV T-C, 10 rpm, 1 min, 25C) 50,000-100,000 cps

Color clear-semi white

Odor MS

Appearance thick gel-thin liquid

[0276] Composition 9L

Item wt%

Main Phase DI Water 31.325

PEG-90M 0.5

Heat to 90-95C

(glycerin can be added while heating)

Glycerin 12

Side Phase 1

Add the following in an appropriate side phase container, heat

to 90-95C, and mix under very moderate mixing

Mineral Oil (Paraffinum Liquidum) 9

Isoceteth-20 22

Oleth-2 8

After fully homogenous, add side phase to main phase

Mix vigorously for 45 mins at 90-95C, then allow to slowly

cool

Side Phase 2

DI Water 7.75

Slowly add the following, mix until hydrated

PVM/MA Copolymer (Gantrez S-97 BF (ISP)) 0.1

Sodium Hydroxide (20% active) 0.125

(solution will slightly thicken)

In-process pH specification: 6.90-7.00

Heat Side Phase to 50-55C

Slowly add the following under very vigorous mixing

Polyquaternium-28 (Conditioneze NT-20 (ISP), 20% active) 4.5

(solution will turn opaque and become less viscous)

Add the following at < 45 C

DMDM Hydantoin 0.025

Slowly add side phase to main phase at 60-70C

VP/Methacrylamide/Vinyl Imidazole Copolymer ("Luviset

Clear" (BASF)) - 20% active 0.2

VP/VA Copolymer, Water 2.8

Methoxy PEG/PPG-7/3 Aminopropyl Dimethicone 1

Add the following at 45C

DMDM Hydantoin 0.175

Fragrance 0.5

Target Specifications 9L:

pH: 3.20-4.50

Penetration (50g weight w/ cone) 18-24mm

Color: Colorless

Odor: MS

Appearance: thick gel wax [0277] Composition 9M

Target Specifications 9M

pH 5.5-6.5

Viscosity (LVT/spindle 4/ 30 rpm 1 min, 25C) 15,000-20,000 cps

Color White/Off white (MS)

Odor MS

Appearance Viscous, opaque liquid

[0278] Compositions 9N-1 and 9N-2

9N-1 9N-2

Item t% t%

Main Phase

DI Water 47.4497 60.2497

Start heat to 80-85C

Add the following one at time, mix until fully dissolved.

Disodium EDTA 0.05 0.05

L-Aspartic Acid 0.75 0.75

Add the following one at a time at 80-85C and mix until melted Stearamidopropyl Dimethylamine 2 2

Cetyl Alcohol 4 1

Stearyl Alcohol 1 0

Glyceryl Stearate 1 0.2

"Crodamol STS" (100% PPG-3 Benzyl Ether Myristate) 2 0

Mix vigorously for 30 minutes at 80-85C

Reduce mixing speed and allow to cool

Add the following at 65-70C

Propylene Glycol 10 0

Side Phase

DI Water 15.5 15.5

Slowly add the following, mix until hydrated

PVM/MA Copolymer (Gantrez S-97 BF (ISP)) 0.2 0.2

Sodium Hydroxide (20% active) 0.25 0.25

(solution will slightly thicken)

In-process pH specification: 6.90-7.00

Heat Side Phase to 50-55C

Slowly add the following under very vigorous mixing

Polyquaternium-28 (Conditioneze NT-20 (ISP), 20% active) 9 9

(solution will turn opaque and become less viscous)

(mix for -10 minutes)

Add the following at < 45C

DMDM Hydantoin 0.05 0.05

Slowly add side phase to main phase at < 45C

< 45C

Fluid Blend 5 5

Fragrance 0.6 0.6

Cocos Nucifera (Coconut) Oil 0.0001 0.0001

Keratin Amino Acids 0.0001 0.0001

Flower/Leaf Extract 0.0001 0.0001

DMDM Hydantoin 0.15 0.15

Add the following and mix until uniform

"Salcare^® SC-96" - Ciba/BASF (65% Polyquaternium-37, 25%

Propylene Glycol Dicaprylate Dicaprate, 10% PPG-1 Trideceth-6) 1 5

Target Specifications 9N

pH 4.50-6.00

Viscosity (RV T-B, 10 rpm, 1 min, 25C) 15,000-25,000 cps

Color: White (MS)

Odor MS

Appearance Viscous, opaque emul Composition 90

Item wt%

Main Phase

DI Water 60.8497

Disodium EDTA 0.05

L-Aspartic Acid 0.75

Add the following one at a time at 80-85C and mix until

melted/homogeneous

Stearamidopropyl Dimethylamine 2

Cetyl Alcohol 1

Glyceryl Stearate 0.2

Mix vigorously for 30 minutes at 80-85C

Reduce mixing speed; allow to cool and foam to reduce

Side Phase

DI Water 15.5

Slowly add the following, mix until hydrated

PVM/MA Copolymer (Gantrez S-97 BF (ISP)) 0.2

Sodium Hydroxide (20% active) 0.25

(solution will slightly thicken)

In-process pH specification: 6.90-7.00

Heat Side Phase to 50-55C

Slowly add the following under very vigorous mixing

Polyquaternium-28 (Conditioneze NT-20 (ISP), 20% active) 9

(solution will turn opaque and become less viscous)

(mix for -10 minutes)

Add the following at < 45C

DMDM Hydantoin 0.05

Slowly add side phase to main phase at < 45C

< 45C

Silicone Pre-Mix

Dimethicone (60,000 est) 2

Phenyl Trimethicone (DC-556) 2

D5, Dimethiconol (DC- 1501) 1

Glycerin 1

Propylene Glycol 0.5

Fragrance 0.5

DMDM Hydantoin 0.15

Cocos Nucifera (Coconut) Oil 0.0001

Keratin Amino Acids 0.0001

Flower/Leaf Extract 0.0001

Add the following and mix until uniform

"Salcare^® SC-96" - Ciba/BASF (65% Polyquaternium-37, 25%

Propylene Glycol Dicaprylate Dicaprate, 10% PPG-1 Trideceth- 6) 3 Target Specifications 90

pH 4.50-6.00

Viscosity (RV T-B, 10 rpm, 1 min, 25C) 5,000-15,000 cps

Color White (MS)

Odor MS

Appearance opaque emulsion Composition 9P

Item wt%

Main Phase

DI Water 52.8497

Disodium EDTA 0.05

L-Aspartic Acid 0.75

Add the following one at a time at 80-85C and mix until

melted/homogeneous

Stearamidopropyl Dimethylamine 2

Cetyl Alcohol 1

Glyceryl Stearate 0.2

Aminopropyl Dimethicone 0.5

Mix vigorously for 30 minutes at 80-85C

Reduce mixing speed; allow to cool and foam to reduce

Side Phase

DI Water 15.5

Slowly add the following, mix until hydrated

PVM/MA Copolymer (Gantrez S-97 BF (ISP)) 0.2

Sodium Hydroxide (20% active) 0.25

(solution will slightly thicken)

In-process pH specification: 6.90-7.00

Heat Side Phase to 50-55C

Slowly add the following under very vigorous mixing

Polyquaternium-28 (Conditioneze NT-20 (ISP), 20% active) 9

(solution will turn opaque and become less viscous)

(mix for ~10 minutes)

Add the following at < 45C

DMDM Hydantoin 0.05

Slowly add side phase to main phase at < 45C

< 45C

Silicone Pre-Mix

"Abil OSW 5" - Evonik (84% Cyclopentasiloxane, 15%

Dimethiconol, 1 % Dimethicone) 2

Dimethicone (60,000 est) 1 "DC-8500" - Dow Corning (82% Bis(C13-15 Alkoxy) PG- Amodimethicone, 18% CI 4-15 Alcohols) 1

Propylene Glycol 10

Fragrance 0.5

DMDM Hydantoin 0.15

Cocos Nucifera (Coconut) Oil 0.0001

Keratin Amino Acids 0.0001

Flower/Leaf Extract 0.0001

Add the following and mix until uniform

"Salcare^® SC-96" - Ciba/BASF (65% Polyquaternium-37, 25%

Propylene Glycol Dicaprylate Dicaprate, 10%> PPG-1 Trideceth- 6) 3

Target Specifications 9P

pH 4.50-6.00

Viscosity (RV T-B, 10 rpm, 1 min, 25C) 10,000-20,000 cps

Color: White (MS)

Odor MS

Appearance opaque emulsion Composition 9Q

Item wt%

Main Phase

DI Water 52.8

Disodium EDTA 0.05

L-Aspartic Acid 0.75

Add the following one at a time at 80-85C and mix until

melted/homogenous

Stearamidopropyl Dimethylamine 2

Cetyl Alcohol 1

Glyceryl Stearate 0.2

Aminopropyl Dimethicone 0.5

Mix Vigorously for 30 minutes at 80-85C

Reduce mixing speed and allow to cool

Side Phase

DI Water 15.5

Slowly add the following, mix until hydrated

PVM/MA Copolymer (Gantrez S-97 BS (ISP)) 0.2

Sodium Hydroxide (20% Active) 0.25

(solution will slightly thicken)

In-process pH specification: 6.90-7.00

Heat side Phase to 50-55C

Slowly add the following under very rigorous mixing

Polyquaternium-28 (Conditioneze NT-20 (ISP), 20% Active) 9 (solution will turn opaque and become less viscous)

Add the following at < 45C

DMDM Hydantoin 0.05

Slowly add side phase to main phase at <45C

< 45C

Pre-mix next two

DS, Dimethiconol 2

Dimethicone 1

DC-8500 1

Propylene Glycol 10

Fragrance 0.5

DMDM Hydantoin 0.2

Salcare^® SC-96 3

Target Specifications 90:

pH 4.50-6.00

Viscosity (RV T-8, 10 rpm, 1 min, 25C)

bulk 7,000-15,0000 cps

Color White (MS)

Odor MS

Appearance opaque emulsion

Composition 9R

Item wt%

Main Phase

DI Water 40.55

Slowly add the following, mix until hydrated

PVM/MA Copolymer (Gantrez S-97 BS (ISP)) 0.2

Sodium Hydroxide (20% Active) 0.25

(solution will slightly thicken)

In-process pH specification: 6.90-7.00

Heat to 50-55C

Slowly add the following under very rigorous mixing

Polyquaternium-28 (Conditioneze NT-20 (ISP), 20% Active) 9

(solution will turn opaque and become less viscous)

Start heat to 80-85C

Add the following one at a time, mix until fully dissolved.

Disodium EDTA 0.05

L-Aspartic Acid 0.75

DI Water 20.27 Add the following one at a time at 80-85C and mix until

melted/homogenous

Stearamidopropyl Dimethylamine 2

Cetyl Alcohol 4

"Montanov 202" 1.18

Glyceryl Stearate 0.80

"Crodamol STS" (Benzyl Ether Myristate) 2

Salcare^® SC-96 1

Aminopropyl Dimethicone 0.75

Mix vigorously for 30 minutes at 80-85C

Reduce mixing speed and allow to cool.

< 45C

Pre-mix next two

DS, Dimethiconol 3

Dimethicone 1.5

DC 2-8566 (Amodimethicone) 2

Propylene Glycol 10

Fragrance 0.5

DMDM Hydantoin 0.2

Target Specifications 9R:

pH: 4.50-6.00

Viscosity (RV T-8, 10 rpm, 1 min,

25C)

bulk 15,0000-25,000 cps

Color: White (MS)

Odor MS

Appearance opaque emulsion

[0283] Compositions 9S-1 through 9S-6

9S-1 9S-2 9S-3 9S-4 9S-5 9S-6

Main Phase wt% wt% wt% wt% wt% wt%

DI Water 64.75565217 59.5252 64.86434783 59.6252 64.75565217 59.5252

Add the following under

vigorous mixing, mix

until hydrated (clear)

Polyquaternium-4

(Celquat L-200) 0.5 0.46 0.5 0.46 0.5 0.46

"Advantage S" (ISP) 0.25 0.23 0.25 0.23 0.25 0.23

Citric Acid 0.02 0.0184 0.02 0.0184 0.02 0.0184

Liquid Additions:

POLYQUATERNIUM- 1 1 , WATER (AQUA) 1.57 1.4444 1.57 1.4444 1.57 1.4444

POLYQU ATERNIUM -7 1 0.92 1 0.92 1 0.92 DC S-71 13 Silicone

Quat Microemulsion

(Dow Corning) 1 0.92 1 0.92 1 0.92

PROPYLENE

GLYCOL, USP 2.25 2.07 2.25 2.07 2.25 2.07

COCAMIDOPROPYL

BETAINE, WATER,

SODRJM CHLORIDE 0.4 0.368 0.4 0.368 0.4 0.368

Side Phase

DI Water 16.84782609 15.55 16.84782609 15.55 16.84782609 15.55

Slowly add the

following, mix until

hydrated.

PVM/MA Copolymer

(Gantrez S-97 BS (ISP)) 0.2173913 0.2 0.2173913 0.2 0.2173913 0.2

Sodium Hydroxide (20%

Active) 0.27173913 0.25 0.27173913 0.25 0.27173913 0.25

(solution will slightly

thicken)

In-process pH

specification: 6.90-7.00

Heat to 50-55C

Slowly add the following

under very rigorous

mixing

Poly quat ernium-28

(Conditioneze NT-20

(ISP)) 9.7826087 9 9.7826087 9 9.7826087 9

(solution will turn

opaque and become less

viscous)

Slowly add side phase to

main phase.

Pre-mix next and

Fragrance

POLYSORBATE 20,

WATER 0.70 0.644 0.70 0.644 0.7 0.644

Fragrance 0.43478261 0.4 0.32608696 0.3 0.43478261 0.4

Propellant Charge

Isobutane and Propane

and 152A 0 8 0 8 0 8

Target Specifications 9S (also for Composition 6J):

(Bulk) (Finished Goods)

pH: 5.0-6.5 5.0-6.5

color: off white (MS) white (ms)

odor: MS MS

appearance: hazy milky liquid dense foam, non-watery, non-runny Composition 9T

Target Specifications 9T:

pH 5.00-6.50

Viscosity (RV T-B, 10 rpm, 1 min, 25C)

Bulk: 7,000-15,000 cps

Color Semi-Translucent white (MS) Odor MS

Appearance Viscous, milky fluid

Composition 9U

Item wt%

Main Phase

DI Water 60.85

Disodium EDTA 0.05

L-Aspartic Acid 0.75

Add the following one at a time at 80-85C and mix until

melted/homogenous Stearamidopropyl Dimethylamine 2

Cetyl Alcohol 1

Glycerol Stearate 0.2

Mix vigorously for 30 minutes at 80-85C

Reduce mixing speed; allow to cool and foam to reduce

Side Phase

DI Water 15.50

Slowly add the following; mix until hydrated

PVM/MA Copolymer (Gantrez S-97)BF (ISP)) 0.2

Sodium Hydroxide (20% active) 0.25

(solution will slightly thicken)

In-process pH specification 6.90-7.00

Heat Side Phase to 50-55C

Slowly add the following under very vigorous mixing

Polyquaternium-28 (Conditioneze NT-20 (ISP)) 9

(solution will turn opaque and become less viscous)

(mix for -10 minutes)

add the following at <45C

DMDM Hydantoin 0.05

Slowly add side phase to main phase at <45C

<45C

Silicone Pre-Mix

Dimethicone (60,000 est) 2

Phenyl Trimethicone (Dc-556) 2

DS, Dimethiconol (DC- 1501) 1

Glycerin 1

Propylene Glycol 0.5

Fragrance 0.5

DMDM Hydantoin 0.15

Salcare^® SC-96 3

Target Specifications 9U:

pH 4.5-6.50

Viscosity (RV T-B, 10 rpm, 1 min, 25C)

Bulk: 8,000-16,000 cps

Color White (MS)

Odor MS

Appearance opaque emulsion Compositions 9V-1 through 9V-3

9V-1 9V-2 9V-3

Item wt% wt% wt%

Main Phase

24.99 24.99 24.99

Target Specifications 9V

pH 6.5-7.5

Viscosity (RV T-C, 5 rpm, 1 min, 25C)

bulk: 40,000-90,000 Color: White (MS) Odor: MS

Appearance: Viscous, opaque gel

[0287] Compositions 9W-1 through 9W-3

9W-1 9W-2 9W-3

Item wt% wt% wt%

Main Phase

DI Water 47.4497 60.2497 60.25

Start heat to 80-85C

Add the following one at a time, mix until fully dissolved

Disodium EDTA 0.05 0.05 0.05

L-Aspartic Acid 0.75 0.75 0.75

Add the following one at a time at 80-85C and mix until

melted

Stearamidopropyl Dimet ylamine 2 2 2

Cetyl Alcohol 4 1 1

Stearyl Alcohol 1 0 0

Glyceryl Stearate 1 0.2 0.2

"Crodamol STS" (100% PPG-3 Benzyl Ether Myristate) 2 0 0

Mix Vigorously for 30 minutes at 80-85C

Reduce mixing speed and allow to cool

Add the following at 65-70C

Propylene Glycol 10 0 0

Side Phase

DI Water 15.5 15.5 15.5

Slowly add the following, mix until hydrated

PVM/MA Copolymer (Gantrez S-97 BS (ISP)) 0.2 0.2 0.2

Sodium Hydroxide (20% Active) 0.25 0.25 0.25

(solution will slightly thicken)

In-process pH specification: 6.90-7.00

Heat side Phase to 50-55C

Slowly add the following under very rigorous mixing

Polyquaternium-28 (Conditioneze NT-20 (ISP), 20%

Active) 9 9 9

(solution will turn opaque and become less viscous)

(mix for " 10 minutes)

Add the following at < 45 C

DMDM Hydantoin 0.05 0.05 0.05

Slowly add side phase to main phase at <43C

< 45C

Fluid Blend 5 5 5

Fragrance 0.6 0.6 0.6

Coco Nucifera (Coconut) Oil 0.0001 0.0001 0 Keratin Amino Acids 0.0001 0.0001 0

Flower/Leaf Extract 0.0001 0.0001 0

DMDM Hydantoin 0.15 0.15 0.15

Add the following and mix until uniform

Salcare^® SC-96 - Ciba/BASF (65% Polyquaternium-37,

25% Propylene Glycol Dicaprylate Dicaprate, 10% PPG-1

Trideceth-6) 1 5 5

Target Specifications 9W:

pH 4.5-6.00

Viscosity (RV T-8, 10 rpm, 1 min, 25C) 15,000-25,000 cps

Color White (MS)

Odor MS

Appearance Viscous, opaque emulsion

[0288] Compositions 9X-1 and 9X-2

9X-1 9X-2

Item wt% wt%

Main Phase

DI Water 54.45 52.05

Start heat to 80-85C

Add the following one at a time, mix until fully dissolved and

solution becomes clear

Disodium EDTA- 0.05 0.05

L-Aspartic Acid 0.75 0.75

Add the following one at a time at 80-85C and mix until melted

Stearamidopropyl Dimethylamine 2 2

Check to make sure solution has turned clear

Cetyl Alcohol 5 7

Glyceryl Stearate 1 1.4

Vigorously mix for 30 minutes at 80-85C

After 30 minutes, turn off heat, slow mixing speed and

allow to slowly cool

Side Phase

DI Water 15.5 15.5

Slowly add the following, mix until hydrated

PVM/MA Copolymer (Gantrez S-97 BF (ISP)) 0.2 0.2

Sodium Hydroxide (20% active) 0.25 0.25

(solution will slightly thicken)

In-process pH specification: 6.90-7.00

Heat Side Phase to 50-55C

Slowly add the following under very vigorous mixing

Polyquaternium-28 (Conditioneze NT-20 (ISP)) 9 9

(solution will turn opaque and become less viscous)

Add the following at <45C DMDM Hydantoin 0.05 0.05

Slowly add side phase to main phase at <45C

Abil T Quat 60 (Evonik) - Silicone Quaternium - 22 1 1

Propylene Glycol 10 10

Fragrance 0.6 0.6

DMDM Hydantoin 0.15 0.15

Target Specifications 9X:

pH:

Viscosity (RV T-B, 10 rpm, 1

min, 25C)

Bulk 7,000-15,000 cps

w/ shear (finished goods) 20,000-35,000 cps

Color White (MS)

Odor MS

Appearance Viscous, opaque emulsion

EXAMPLE 10

[0289] This example demonstrates exemplary addition rates, addition times,

temperatures, mixing speeds, and mixing times for producing PECs.

Water Densities: Perry's Chemical Engineer's Handbook,

densities for NaOH 20% = 1.2191 kg/L and Conditioneze

[0292] One 270-kg batch

the PEC Complex in 113-liter / 30-gallon premix vessel with center turbine agitator only main batch in 227-liter / 60-gallon mixing vessel with center turbine and side sweep agitators

Processing Parameters for PEC Complex:

[0293] Initial Water Char e = 42.02 L (41.85 kg)

Addition Rate = 28 L/min (28 kg/min)

Total Addition Time = 1.5 minutes

Initial Water Temperature = 29°C

Center Turbine Agitator = Moderate (RPM) clockwise direction

Side Sweep Agitator = None in Pilot Premix Tank [0294] PVM/MA Copolymer (Gantrez S-97 BF) = 0.54 kg (solid)

Addition Rate = 0.6 kg/min

Total Addition Time = 1 minute

Temperature = 30°C

Center Turbine Agitator = Moderate (RPM) clockwise direction

Side Sweep Agitator = None in Pilot Premix Tank

Dispersion Mix Time = 30 minutes

[0295] Sodium Hydroxide, 20% = 0.55 L (0.675 kg)

Addition Rate = 0.6 L/min (0.7 kg/min)

Total Addition Time = 1 minute

Temperature = 30°C

Center Turbine Agitator = Slow (RPM) clockwise direction

Side Sweep Agitator = None in Pilot Premix Tank

Hydration Mix Time = 20 minutes

In-Process pH Check = 6.90

Heat Premix for 10 minutes to 51°C

[0296] Polyquatemium 28 (Conditioneze NT-20) = 23.32 L (24.30 kg)

Addition Rate = 3.33 L/min (3.47 kg/min)

Total Addition Time = 7 minutes

Temperature = 49°C

Center Turbine Agitator = Moderate/High (RPM) clockwise direction

Side Sweep Agitator = None in Pilot Premix Tank

Complex Mix Time = 40 minutes

[0297] Premix Cool Down

Cool to 29°C

Center Turbine Agitator = Very Slow (RPM) clockwise direction

Side Sweep Agitator = None in Pilot Premix Tank

Cool Down Mix Time = 60 minutes*

(*Note: Mix time reflects time required to get main batch to addition point for PEC Premix) [0298] One 1 1 , 800-kg batch

The PEC Complex in 5,678-liter / 1 ,500-gallon premix vessel with center turbine and side sweep agitators

main batch in MOl 12,1 13-liter / 3,200-gallon mixing vessel with center turbine and side sweep agitators

Processing Parameters for PEC Complex:

[0299] Initial Water Charge = 1840.9 L (1835 kg)

Addition Rate = 526 L/min (524 kg/min)

Total Addition Time = 3.5 minutes

Temperature = 26°C

Center Turbine Agitator = 25 RPM counter-clockwise direction

Side Sweep Agitator = 7 RPM clockwise direction

[0300] PVM/MA Copolymer (Gantrez S-97 BF) = 23.6 kg (solid)

Addition Rate = 7.87 kg/min

Total Addition Time = 3 minutes

Temperature = 27°C

Center Turbine Agitator = 20 RPM counter-clockwise direction

Side Sweep Agitator = 7 RPM clockwise direction

Dispersion Mix Time = 30 minutes

[0301] Sodium Hydroxide, 20% = 24.2 L (29.5kg)

Addition Rate = 12.1 L/min (14.75 kg/min)

Total Addition Time = 2 minute

Temperature = 27°C

Center Turbine Agitator = 20 RPM counter-clockwise direction

Side Sweep Agitator = 7 RPM clockwise direction

Hydration Mix Time = 10 minutes

In-Process pH Check = 6.72. Add additional 118 grams (0.001 wt%) of NaOH and pH = 6.80. Add additional 1 18 grams (0.001 wt%) of NaOH and pH = 6.90. Total of 29.736 kg of NaOH Heat Premix for 18 minutes to 55°C

[0302] Polyquaternium 28 (Conditioneze NT-20) = 1019 L (1062 kg)

Addition Rate = 29.1 L/min (30.3 kg/min)

Total Addition Time = 35 minutes

Temperature = 54°C

Center Turbine Agitator = 28 RPM counter-clockwise direction

Side Sweep Agitator = 7 RPM clockwise direction

Complex Mix Time = 30 minutes

[0303] Premix Cool Down

Cool to 35°C

Center Turbine Agitator = 18 RPM counter-clockwise direction

Side Sweep Agitator = 7 RPM clockwise direction

Cool Down Mix Time = 240 minutes*

(*Note: Mix time reflects time required to get main batch to addition point for PEC Premix) [0304] One 270-kg batch

The PEC Complex in 113-liter / 30-gallon premix vessel with center turbine agitator only the main batch in 227-liter / 60-gallon mixing vessel with center turbine and side sweep agitators

Processing Parameters for PEC Complex:

[0305] Initial Water Charge = 42.04 L (41.84 kg)

Addition Rate = 28 L/min (28 kg/min)

Total Addition Time = 1.5 minutes

Initial Water Temperature = 31 °C

Center Turbine Agitator = Moderate (RPM) clockwise direction

Side Sweep Agitator = None in Pilot Premix Tank

Heat Premix for 10 minutes to 52°C [0306] PVM/MA Copolymer (Gantrez S-97 BF) = 0.54 kg (solid)

Addition Rate = 0.6 kg/min

Total Addition Time = 1 minute

Temperature = 52°C

Center Turbine Agitator = Moderate (RPM) clockwise direction

Side Sweep Agitator = None in Pilot Premix Tank

Dispersion Mix Time = 25 minutes

[0307] Sodium Hydroxide, 20% = 0.56 L (0.688 kg)

Addition Rate = 0.6 L/min (0.7 kg/min)

Total Addition Time = 1 minute

Temperature = 52°C

Center Turbine Agitator = Slow (RPM) clockwise direction

Side Sweep Agitator = None in Pilot Premix Tank

Hydration Mix Time = 15 minutes

In-Process pH Check = 6.93

[0308] Polvquaternium 28 (Conditioneze NT-20) = 23.32 L (24.30 kg)

Addition Rate =4.66 L/min (4.86 kg/min)

Total Addition Time = 5 minutes

Temperature = 53°C

Center Turbine Agitator = Moderate/High (RPM) clockwise direction

Side Sweep Agitator = None in Pilot Premix Tank

Complex Mix Time = 40 minutes

[0309] Premix Cool Down

Cool to 29°C

Center Turbine Agitator = Very Slow (RPM) clockwise direction

Side Sweep Agitator = None in Pilot Premix Tank

Cool Down Mix Time = 100 minutes*

(*Note: Mix time reflects time required to get main batch to addition point for PEC Premix) [0310] One 270-kg batch

The PEC Complex in 1 13-liter / 30-gallon premix vessel with center turbine agitator only) the main batch in 227-liter / 60-gallon mixing vessel with center turbine and side sweep agitators

Processing Parameters for PEC Complex:

[0311] Initial Water Charge = 42.03 L (41.85 kg)

Addition Rate = 28 L/min (28 kg/min)

Total Addition Time = 1.5 minutes

Initial Water Temperature = 30°C

Center Turbine Agitator = Moderate (RPM) clockwise direction

Side Sweep Agitator = None in Pilot Premix Tank

[0312] PVM/MA Copolymer (Gantrez S-97 BF) = 0.54 kg (solid)

Addition Rate = 0.6 kg/min

Total Addition Time = 1 minute

Temperature = 30°C

Center Turbine Agitator = Moderate (RPM) clockwise direction

Side Sweep Agitator = None in Pilot Premix Tank

Dispersion Mix Time = 30 minutes

[0313] Sodium Hydroxide, 20% = 0.56 L (0.68 kg)

Addition Rate = 0.6 L/min (0.7 kg/min)

Total Addition Time = 1 minute

Temperature = 31 °C

Center Turbine Agitator = Slow (RPM) clockwise direction

Side Sweep Agitator = None in Pilot Premix Tank

Hydration Mix Time = 6 minutes

In-Process pH Check = Original 6.83. Add additional 2.7 grams (0.001 wt%) of NaOH and pH = 6.95. Total of 682.7 g of NaOH

Heat Premix for 10 minutes to 57°C [0314] Polvquaternium 28 (Conditioneze NT-20) = 23.32 L (24.30 kg) Addition Rate = 3.33 L/min (3.47 kg/min)

Total Addition Time = 7 minutes

Temperature = 56°C

Center Turbine Agitator = Moderate/High (RPM) clockwise direction

Side Sweep Agitator = None in Pilot Premix Tank

Complex Mix Time = 30 minutes

[0315] Premix Cool Down

Cool to 27°C

Center Turbine Agitator = Very Slow (RPM) clockwise direction

Side Sweep Agitator = None in Pilot Premix Tank

Cool Down Mix Time = 120 minutes*

(*Note: Mix time reflects time required to get main batch to addition point for PEC Premix) [0316] One 1 ,250-kg batch

The PEC Complex in 379-liter / 100-gallon premix vessel with center turbine and side sweep agitators

the main batch in 1,893-liter / 500-gallon mixing vessel with center turbine and side sweep agitators

Processing Parameters for PEC Complex:

[0317] Initial Water Charge = 195.2 L (194.4 kg)

Addition Rate = 97.6 L/min (97.2 kg/min)

Total Addition Time = 2 minutes

Temperature = 29°C

Center Turbine Agitator = 60 RPM counter-clockwise direction

Side Sweep Agitator = 10 RPM clockwise direction

[0318] PVM/MA Copolymer (Gantrez S-97 BF) = 2.5 kg (solid)

Addition Rate = 1.3 kg/min

Total Addition Time = 2 minutes Temperature = 31°C

Center Turbine Agitator = 60 RPM counter-clockwise direction

Side Sweep Agitator = 10 RPM clockwise direction

Dispersion Mix Time = 26 minutes

[0319] Sodium Hydroxide, 20% = 2.56 L (3.125 kg)

Addition Rate = 3 L/min (4 kg/min)

Total Addition Time = 1 minute

Temperature = 33°C

Center Turbine Agitator = 20 RPM counter-clockwise direction

Side Sweep Agitator = 10 RPM clockwise direction

Hydration Mix Time = 11 minutes

In-Process pH Check = 6.90

Heat Premix for 10 minutes to 52°C

[0320] Polyquaternium 28 (Conditioneze NT-20) = 108.0 L (112.5 kg)

Addition Rate = 9.0 L/min (9.4 kg/min)

Total Addition Time = 12 minutes

Temperature = 54°C

Center Turbine Agitator = 58 RPM counter-clockwise direction

Side Sweep Agitator = 15 RPM clockwise direction

Complex Mix Time = 31 minutes

[0321] Premix Cool Down

Cool to 35°C

Center Turbine Agitator = 18 RPM counter-clockwise direction

Side Sweep Agitator = 8 RPM clockwise direction

Cool Down Mix Time = 135 minutes*

(*Note: Mix time reflects time required to get main batch to addition point for PEC Premix) [0322] One 270-kg batch

The PEC Complex in 1 13-liter / 30-gallon premix vessel with center turbine agitator only the main batch in 227-liter / 60-gallon mixing vessel with center turbine and side sweep agitators

Processing Parameters for PEC Complex:

[0323] Initial Water Charge = 42.01 L (41.84 kg)

Addition Rate = 28 L/min (28 kg/min)

Total Addition Time = 1.5 minutes

Initial Water Temperature = 29°C

Center Turbine Agitator = Moderate (RPM) clockwise direction

Side Sweep Agitator = None in Pilot Premix Tank

Heat Premix for 10 minutes to 52°C

[0324] PVM/MA Copolymer (Gantrez S-97 BF) = 0.54 kg (solid) Addition Rate = 0.6 kg/min

Total Addition Time = 1 minute

Temperature = 52°C

Center Turbine Agitator = Moderate (RPM) clockwise direction

Side Sweep Agitator = None in Pilot Premix Tank

Dispersion Mix Time = 25 minutes

[0325] Sodium Hydroxide, 20% = 0.57 L (0.69 kg)

Addition Rate = 0.6 L/min (0.7 kg/min)

Total Addition Time = 1 minute

Temperature = 53°C

Center Turbine Agitator = Slow (RPM) clockwise direction

Side Sweep Agitator = None in Pilot Premix Tank

Hydration Mix Time = 5 minutes

In-Process pH Check = 6.95

[0326] Polyquatemium 28 (Conditioneze NT-20) = 23.32 L (24.30 kg) Addition Rate = 4.66 L/min (4.86 kg/min)

Total Addition Time = 5 minutes

Temperature = 53°C Center Turbine Agitator = Moderate/High (RPM) clockwise direction

Side Sweep Agitator = None in Pilot Premix Tank

Complex Mix Time = 35 minutes

[0327] Premix Cool Down

Cool to 30°C

Center Turbine Agitator = Very Slow (RPM) clockwise direction

Side Sweep Agitator = None in Pilot Premix Tank

Cool Down Mix Time = 90 minutes*

(*Note: Mix time reflects time required to get main batch to addition point for PEC Premix) [0328] One 270-kg batch

Processing Parameters for PEC Complex:

[0329] Initial Water Charge = 42.01 L (41.84 kg)

Addition Rate = 28 L/min (28 kg/min)

Total Addition Time = 1.5 minutes

Initial Water Temperature = 29°C

Center Turbine Agitator = Moderate (RPM) clockwise direction

Side Sweep Agitator = None in Pilot Premix Tank

[0330] PVM/MA Copolymer (Gantrez S-97 BF) = 0.54 kg (solid)

Addition Rate = 0.6 kg/min

Total Addition Time = 1 minute

Temperature = 30°C

Center Turbine Agitator = Moderate (RPM) clockwise direction

Side Sweep Agitator = None in Pilot Premix Tank

Dispersion Mix Time = 30 minutes [0331] Sodium Hydroxide, 20% = 0.56 L (0.68 kg)

Addition Rate = 0.6 L/min (0.7 kg/min)

Total Addition Time = 1 minute

Temperature = 30°C

Center Turbine Agitator = Slow (RPM) clockwise direction

Side Sweep Agitator = None in Pilot Premix Tank

Hydration Mix Time = 20 minutes

In-Process pH Check = Original 6.81. Add additional 3.4 grams (0.00126 wt%) of NaOH and pH = 6.92. Total of 683.4 g of NaOH

Heat Premix for 10 minutes to 54°C

[0332] Polyquaternium 28 (Conditioneze NT-20) = 23.32 L (24.30 kg)

Addition Rate = 3.33 L/min (3.47 kg/min)

Total Addition Time = 7 minutes

Temperature = 54°C

Center Turbine Agitator = Moderate/High (RPM) clockwise direction

Side Sweep Agitator = None in Pilot Premix Tank

Complex Mix Time = 35 minutes

[0333] Premix Cool Down

Cool to 35°C

Center Turbine Agitator = Very Slow (RPM) clockwise direction

Side Sweep Agitator = None in Pilot Premix Tank

Cool Down Mix Time = 260 minutes*

(*Note: Mix time reflects time required to get main batch to addition point for PEC Premix) [0334] One 3,772-kg batch

The PEC Complex in 1 ,893-liter / 500-gallon premix vessel with center turbine and side sweep agitators

the main batch in 3,785-liter / 1000-gallon mixing vessel with center turbine and side sweep agitators)

Processing Parameters for PEC Complex: [0335] Initial Water Charge = 588.93 L (586.546 kg Addition Rate = 392.6 L/min (391 kg/min)

Total Addition Time = 1.5 minutes

Temperature = 29°C

Center Turbine Agitator = 46 RPM counter-clockwise direction

Side Sweep Agitator = 10 RPM clockwise direction

[0336] PVM/MA Copolymer (Gantrez S-97 BP = 7.544 kg (solid) Addition Rate = 3.77 kg/min

Total Addition Time = 2 minutes

Temperature = 29°C

Center Turbine Agitator = 46 RPM counter-clockwise direction

Side Sweep Agitator = 10 RPM clockwise direction

Dispersion Mix Time = 60 minutes

[0337] Sodium Hydroxide, 20% = 7.735 L (9.430 kg)

Addition Rate = 3.9 L/min (4.7 kg/min)

Total Addition Time = 2 minute

Temperature = 30°C

Center Turbine Agitator = 25 RPM counter-clockwise direction

Side Sweep Agitator = 10 RPM clockwise direction

Hydration Mix Time = 10 minutes

In-Process pH Check = 6.91

Heat Premix for 10 minutes to 52°C

[0338] Polyquaternium 28 (Conditioneze NT-20) = 325.80 L (339.48 kg Addition Rate = 16.3 L/min (17.0 kg/min)

Total Addition Time = 20 minutes

Temperature = 50°C

Center Turbine Agitator = 35 RPM counter-clockwise direction

Side Sweep Agitator = 6 RPM clockwise direction

Complex Mix Time = 40 minutes [0339] Premix Cool Down

Cool to 40°C

Center Turbine Agitator = 14 RPM counter-clockwise direction

Side Sweep Agitator = 6 RPM clockwise direction

Cool Down Mix Time = 55 minutes*

(*Note: Mix time reflects time required to get main batch to addition point for PEC Premix) [0340] One 270-kg batch

Processing Parameters for PEC Complex:

[0341] Initial Water Charge = 42.01 L (41.84 kg)

Addition Rate = 28 L/min (28 kg/min)

Total Addition Time = 1.5 minutes

Initial Water Temperature = 29°C

Center Turbine Agitator = Moderate (RPM) clockwise direction

Side Sweep Agitator = None in Pilot Premix Tank

Heat Premix for 10 minutes to 52°C

[0342] PVM/MA Copolymer (Gantrez S-97 BF) = 0.54 kg (solid)

Addition Rate = 0.6 kg/min

Total Addition Time = 1 minute

Temperature = 52°C

Center Turbine Agitator = Moderate (RPM) clockwise direction

Side Sweep Agitator = None in Pilot Premix Tank

Dispersion Mix Time = 20 minutes

[0343] Sodium Hydroxide, 20% = 0.57 L (0.69 kg)

Addition Rate = 0.6 L/min (0.7 kg/min) Total Addition Time = 1 minute

Temperature = 53°C

Center Turbine Agitator = Slow (RPM) clockwise direction

Side Sweep Agitator = None in Pilot Premix Tank

Hydration Mix Time = 6 minutes

In-Process pH Check = 6.98

[0344] Polyquaternium 28 (Conditioneze NT-20) = 23.32 L (24.30 kg)

Addition Rate = 4.66 L/min (4.86 kg/min)

Total Addition Time = 5 minutes

Temperature = 53°C

Center Turbine Agitator = Moderate/High (RPM) clockwise direction

Side Sweep Agitator = None in Pilot Premix Tank

Complex Mix Time = 35 minutes

[0345] Premix Cool Down

Cool to 29°C

Center Turbine Agitator = Very Slow (RPM) clockwise direction

Side Sweep Agitator = None in Pilot Premix Tank

Cool Down Mix Time = 100 minutes*

(*Note: Mix time reflects time required to get main batch to addition point for PEC Premix)

EXAMPLE 11

[0346] This example describes exemplary compositions of the present invention (Compositions 1 1A-1 1G).

[0347] The hair mending efficacy of some of these compositions (with Composition 1C) is summarized in Tables 13 and 14. The high humidity curl retention of some of these compositions is shown in Figure 7.

[0348] Composition 1 1A

Item wt%

Main Phase

DI Water 66.525

Sprinkle in the following and mix until clear Polyquaternium-4 (Celquat H-100) 0.5

Vinyl Caprolactum/VP/Dimethylaminoethyl

Methacrylate Copolymer ("Advantage S" (ISP)) 0.5

Liquid Additions:

POLYQUATERNIUM-1 1, WATER (20%

active) 5

VP/Methacrylamide/Vinyl Imidazole Copolymer

("Luviset Clear" (BASF)) - 20% active 5

Side Phase

DI Water 7.75

Slowly add the following, mix until hydrated

PVM/MA Copolymer (Gantrez S-97 BF (ISP)) 0.1

Sodium Hydroxide (20%> active) 0.125

(solution will slightly thicken)

In-process pH specification: 6.90-7.00

Heat to 50-55C

Slowly add the following under very vigorous

mixing

Polyquaternium-28 (Conditioneze NT-20 (ISP)) 4.5

(solution will turn opaque and become less

viscous)

DMDM Hydantoin 0.025

Slowly add side phase to main phase at < 45C

"Salcare^® SC-96" - Ciba/BASF (65%

Polyquaternium-37, 25% Propylene Glycol

Dicaprylate Dicaprate, 10% PPG-1 Trideceth-6) 3

Mix until uniform

< 45C

Silicone Premix

Dimethicone (60,000 est) 2

Phenyl Trimethicone (DC-556) 2

Cyclopentasiloxane, Dimethiconol 1

Glycerin 1

Propylene Glycol 0.5

Fragrance 0.3

DMDM Hydantoin 0.175

Target Specifications 11 A

pH 5.00-6.50

Viscosity (RV T-B, 10 rpm, 1 min, 25C) 20,000-40,000 cps

Color: Semi-white (MS) Odor MS

Appearance Viscous, opaque gelposition 1 IB Add the following and mix until uniform

Polyacrylamide, C13-14 Isoparaffin, Laureth-7

("Sepigel 305") 4

Target Specifications 11B

pH 6.0-7.5

Viscosity (RV T-C, 5 rpm, 1 min, 25C) 50,000-100,000 cps

Color Semi-white

Odor MS

Appearance Thick gel mposition 1 1 C

Item wt%

Main Phase

DI Water 75.725

Sprinkle in the following and mix until clear

Polyquaternium-4 (Celquat H-100) 0.5

POLYQUATERNIUM-1 1, WATER (20% active) 2.5

PEC Pre-mix

DI Water 7.75

Slowly add the following, mix until hydrated

PVM/MA Copolymer (Gantrez S-97 BF (ISP)) 0.1

Sodium Hydroxide (20% active) 0.125

(solution will slightly thicken)

In-process pH specification: 6.90-7.00

Heat to 50-55C

Slowly add the following under very vigorous

mixing

Polyquaternium-28 (Condi tioneze NT-20 (ISP)) 4.5

(solution will turn opaque and become less viscous)

mix for 10 minutes

Add the following at < 45 C

DMDM Hydantoin 0.025

Slowly add side phase to main phase at < 45C

< 45C

Silicone Premix

Dimethicone (60,000 est) 2

Phenyl Trimethicone (DC-556) 2

Cyclopentasiloxane, Dimethiconol 1

Glycerin 1

Propylene Glycol 0.5

Fragrance 0.1

DMDM Hydantoin 0.175 "Salcare^® SC-96" - Ciba/BASF (65% Polyquaternium- 37, 25% Propylene Glycol Dicaprylate Dicaprate,

10% PPG- 1 Trideceth-6) 2

Mix until uniform

Target Specifications 1 1C:

pH: 5.00-6.50

Viscosity (RV T-B, 10 rpm, 1 min, 25C): 5,000-15,000 cps

Color: Semi-translucent white (MS) Odor: MS

Appearance: Viscous, milky liquid 1] Composition 1 ID

l lD-1 11D-2

Item wt% wt%

Main Phase

DI Water 67.5247 55.0497

Sprinkle in the following and mix until clear

Polyquaternium-4 (Celquat H-100) 0.5 0.5

Vinyl Caprolactum/VP/Dimethylaminoethyl Methacrylate

Copolymer ("Advantage S" (ISP)) 0.25 0.25

Disodium EDTA 0.05 0.05

L-Aspartic Acid 0.75 0.75

Add the following one at a time at 80-85C and mix until

melted/homogeneous

Stearamidopropyl Dimethylamine 2 2

Cetyl Alcohol 1 1

Glyceryl Stearate 0.2 0.2

Mix vigorously for 30 minutes at 80-85C

Reduce mixing speed; allow to cool and foam to reduce

Liquid Additions:

POLYQUATERNIUM-1 1, WATER (20% active) 1.25 1.25

VP/Methacrylamide/Vinyl Imidazole Copolymer ("Luviset

Clear" (BASF)) - 20% active 2.5 2.5

Side Phase

DI Water 7.75 15.5

Slowly add the following, mix until hydrated

PVM/MA Copolymer (Gantrez S-97 BF (ISP)) 0.1 0.2

Sodium Hydroxide (20% active) 0.125 0.25

(solution will slightly thicken)

In-process pH specification: 6.90-7.00

Heat Side Phase to 50-55C Slowly add the following under very vigorous mixing

Polyquaternium-28 (Conditioneze NT-20 (ISP), 20% active) 4.5 9

(solution will turn opaque and become less viscous)

(mix for -10 minutes)

Add the following at < 45 C

DMDM Hydantoin 0.025 0.05

Slowly add side phase to main phase at < 45C

< 45C

"Abil OSW 5" - Evonik (84% Cyclopentasiloxane, 15%

Dimethiconol, 1 % Dimethicone) 3 3

"DC-8500" - Dow Corning (82% Bis(C13-15 Alkoxy) PG-

1 1 Amodimethicone, 18% CI 4- 15 Alcohols)

Phenyl Trimethicone (DC-556) 2 2

Fragrance 0.3 0.3

DMDM Hydantoin 0.175 0.15

Cocos Nucifera (Coconut) Oil 0.0001 0.0001

Keratin Amino Acids 0.0001 0.0001

Flower/Leaf Extract 0.0001 0.0001

Add the following and mix until uniform

"Salcare^® SC-96" - Ciba/BASF (65% Polyquaternium-37,

25% Propylene Glycol Dicaprylate Dicaprate, 10% PPG-1

Trideceth-6) 5 5

Mix until uniform

Target Specifications I IP

pH 4.50-6.00

Viscosity (RV T-B, 10 rpm, 1 min, 25C) 20,000-30,000 cps

Color White (MS)

Odor MS

Appearance Viscous opaque lotion 2] Composition HE

Item wt%

Main Phase

DI Water 26.2247

Propylene Glycol 35

Silicone Pre-Mix

"Abil OSW 5" - Evonik (84% Cyclopentasiloxane, 15%

Dimethiconol, 1 % Dimethicone) 20

Amodimethicone (ADM 1 100 (Wacker)) (~$10.50/kg) 2

Phenyl Trimethicone (DC-556) 2

Fragrance 0.1

DMDM Hydantoin 0.175

Target Specifications HE

pH 6.5-7.5

Viscosity (RV T-B, 10 rpm, 1 min, 25C) 5,000-15,000 cps

Color: Colorless-slightly yellow Odor: MS

Appearance Slightly hazy oily liquid Composition 1 IF

Item wt%

Main Phase

DI Water 17.7747

Propylene Glycol 35

VP/Methacrylamide/Vinyl Imidazole Copolymer ("Luviset

Clear" (BASF)) - 20% active 3.75

VP/VA Copolymer, Water 1.5

Silicone Pre-Mix

"Abil OSW 5" - Evonik (84% Cyclopentasiloxane, 15%

Dimethiconol, 1% Dimethicone) 22

Target Specifications 1 IF

pH 6.5-7.5

Viscosity (RV T-C, 5 rpm, 1 min, 25C) 50,000-100,000 cps

Color Colorless-slightly yellow

Odor MS

Appearance Slightly hazy viscous wax

[0354] Compositions 1 1 G- 1 through 11 G-4

l lG-1 1 1G-2 1 1G-3 1 1 G-4

Main Phase wt% wt% wt% wt%

DI Water 76.803586 70.6593 76.803586 70.6593

Add the following under vigorous mixing,

mix until hydrated (clear)

Polyquaternium-4 (Celquat H-100) 0.543478 0.5 0.543478 0.5

Vinyl Caprolactum/VP/Dimethylaminoethyl

Methacrylate Copolymer ("Advantage S"

(ISP)) 0.543478 0.5 0.543478 0.5 Citric Acid 0.02 0.0184 0.02 0.0184

Liquid Additions:

POLYQUATERNIUM- 1 1 , WATER (21.5%

active) 2.717391 2.5 2.717391 2.5

POLYQUATERNIUM-7 (8.5% active) 1 0.92 1 0.92

DC 5-7113 Silicone Quat Microemulsion - Dow Corning (66% Water, 25% Silicone

Quaternium-16, 7.4% Undeceth-1 1 , 4.5%

Butyloctanol, 3.5% Undeceth-5) 1 0.92 1 0.92

PROPYLENE GLYCOL, USP 2.25 2.07 2.25 2.07

COCAMIDOPROPYL BETAINE (-30%

active), WATER, SODIUM CHLORIDE 0.4 0.368 0.4 0.368

Side Phase

DI Water 8.423913 7.75 8.423913 7.75

Slowly add the following, mix until

hydrated

PVM/MA Copolymer (Gantrez S-97 BF

(ISP)) 0.108696 0.1 0.108696 0.1

Sodium Hydroxide (20% active) 0.13587 0.125 0.13587 0.125

(solution will slightly thicken)

In-process pH specification: 6.90-7.00

Heat Side Phase to 50-55C

Slowly add the following under very

vigorous mixing

Polyquaternium-28 (Conditioneze NT-20

(ISP), 20% active) 4.891304 4.5 4.891304 4.5

(solution will turn opaque and become less

viscous)

Add the following at < 45C

DMDM Hydantoin 0.027174 0.025 0.027174 0.025

Slowly add side phase to main phase

Pre-Mix next and Fragrance

POLYSORBATE 20 0.7 0.644 0.7 0.644

Fragrance 0.434783 0.4 0.434783 0.4

Cocos Nucifera (Coconut) Oil 0.000109 0.0001 0.000109 0.0001

Keratin Amino Acids 0.000109 0.0001 0.000109 0.0001

Flower/Leaf Extract 0.000109 0.0001 0.000109 0.0001

Propellant Charge

Isobutane and Propane and 152A (78.5%

A46; 28.5% HFC 152A) 0 8 0 8

Target Specifications Bulk:

pH: 5.0-6.5

Color: Off white (MS)

Odor: MS

Appearance: Hazy liquid Target Specifications Finished Product:

pH: 5.0-6.5

Color: White (MS)

Odor: MS

Appearance: Dense foam, non-watery, non-runny Foam stability: 200 seconds min

Spray diameter (at 8"): foam

Spray pattern (at 8"): foam

[0355] Table 13

[0356] Table 14

This example demonstrates alleviation of weakening of hair, due to hot flat g, by compositions of the present invention.

Comparative Composition 12A

Main Phase wt%

DI Water 69.9897

Aminomethyl Propanol (AMP-95) 0.02

Add the following under very vigorous mixing for 30

mins.

"Ultrathix P-100" (Acrylic Acid/VP Crosspolymer) 1

Add the following and mix until uniform

Aminomethyl Propanol (AMP-95) 0.44

Side Phase 1

DI Water 20

Sprinkle in the following and mix until clear

Polyquaternium-4 (Celquat H-100) 0.5

Disodium EDTA 0.05

Liquid Additions:

PVP K-90 (20% active) 1

VP/Methacrylamide/Vinyl Imidazole Copolymer

("Luviset Clear" (BASF)) - 20% active 3.5

Polyquaternium-39 (8.5% active) 0.5

Propylene Glycol 1

Sorbitol (70%) 0.5

Add Side Phase 1 to main tank and mix until uniform < 45C

Pre-mix next three

PEG-40 Hydrogenated Castor Oil 0.6

PEG/PPG-18/18 Dimethicone (DC-190) 0.1

Fragrance 0.6

Cocos Nucifera (Coconut) Oil 0.0001

Keratin Amino Acids 0.0001

Flower/Leaf Extract 0.0001

DMDM Hydantoin 0.2

Specifications 12A:

pH 6.0-7.0

Viscosity (RV T-C, 5 rpm, 1 min, 25C) 40,000-80,000

Color: White (MS)

Odor MS

Viscous, opaque (hazy)

Appearance: gel

[0359] Comparative Composition 12B

[0360] Into a main stainless steel compounding tank, charge cold water, set at 68 - 86°F (20 - 86°C) with vigorous mixing (turbine mixer at vigorous counterclockwise direction; side sweep mixer at moderate clockwise direction).

[0361] Add the first Aminomethyl Propanol (AMP-95) addition to the main

compounding tank and mix until completely dispersed.

[0362] Next, slowly sprinkle the acrylic acid/VP crosspolymer powder into the main compounding tank with vigorous agitation (vortex where possible; turbine mixer at vigorous counterclockwise direction; side sweep mixer at moderate clockwise direction). An eductor or any other in-line disperser may be used for this addition. Use caution during addition of the powder, as it will clump if added too quickly. Mix the batch for a minimum of 45 minutes or until the polymer is completely dispersed and no particles or lumps are present. While mixing, begin preparing the Celquat Premix.

[0363] Take a sample from the main compounding tank and visually verify that all of the polymer has been dispersed and there are no particles or lumps. If particles or lumps remain, continue vigorous mixing and resample periodically until the batch is uniform.

[0364] Next, after the dispersion has been visually approved, charge DI water to the main compounding tank with moderate agitation (turbine mixer at moderate counterclockwise direction; side sweep mixer at slow clockwise direction). Use care when charging the water, and reduce the mixing to avoid aeration. This water charge should bring the batch level above the top blades to avoid splashing and aeration during the neutralization step. Mix the batch for a minimum of 15 minutes or until the batch is smooth and homogeneous.

[0365] Once the batch is uniform after the DI water charge, continue to mix moderately (turbine mixer at moderate counterclockwise direction; side sweep mixer at moderate clockwise direction) and add the second Aminomethyl Propanol (AMP-95) addition to the main compounding tank to neutralize the polymer. The solution will eventually turn clear and the viscosity will increase dramatically. Mix the batch for a minimum of 20 minutes or until the batch is uniform.

[0366] In a suitable, stainless steel premix tank, charge the following cold Water set at 68 - 86°F (20 - 30°C). Begin vigorous mixing (turbine mixer at vigorous counterclockwise direction; side sweep mixer at moderate clockwise direction, if available).

[0367] In a suitable stainless steel container, premix dye in warm water, set at 104 - 1 13°F (40 - 45°C), where available. Mix until the dye is completely dissolved and uniform. Mix until the premix is uniform and free of any undissolved particles. Once the Dye Premix is ready, add this solution to the phase tank. [0368] Next, slowly sprinkle the Polyquaternium-4 powder into the phase tank with vigorous agitation (vortex where possible; turbine mixer at vigorous counterclockwise direction; side sweep mixer at moderate clockwise direction, if available). An eductor or any other in-line disperser may be used for this addition. Use caution during addition of the powder, as it will clump if added too quickly. Mix the batch for a minimum of 30 minutes or until there are no particles or lumps.

[0369] Take a sample from the phase tank and visually verify that all of the polymer has been dispersed and there are no particles or lumps. If particles or lumps remain, continue vigorous mixing and resample periodically until the batch is uniform.

[0370] Once the phase is clear and uniform, add the following items to the premix tank (turbine mixer at vigorous counterclockwise direction; side sweep mixer at moderate clockwise direction, if available): disodium EDTA; PVP K-90 (20% solution);

VP/Methacrylamide/Vinyl Imidazole Copolymer; polyquaternium-39; propylene glycol; sorbitol; aminomethyl propanol.

[0371] Once the premix is ready, add it to the main compounding tank. Rinse the premix tank with cold water set at 68 - 86°F (20 - 30°C) and add it to the main compounding tank (turbine mixer at moderate counterclockwise direction; side sweep mixer at moderate clockwise direction, if available). Mix the batch for a minimum of 20 minutes or until the batch is uniform.

[0372] Prepare the following fragrance premix in a suitable, sanitized container equipped with an electric or air mixer: oleth-20; fragrance. Oleth-20 should be pre-melted at 95 - 104°F (35 - 40°C) for homogeneity and ease of handling. Do not mix this ingredient with fragrance if it is above 1 10°f (43°c) or the fragrance will flash off. Mix this premix vigorously until it is clear and free of any undissolved material. Visually verify that it is clear and free of particles and then add it to the main compounding tank with moderate agitation.

[0373] Check that the batch temperature is 104°F (40°C) or below (cool the batch if necessary), and then add the DMDM hydantoin to the main compounding tank with moderate agitation (turbine mixer at moderate counterclockwise direction; side sweep mixer at moderate clockwise direction). Mix for a minimum of 30 minutes or until the batch is completely uniform. Sample the composition. Discontinue mixing and cooling (if applicable).

[0374] Adjustments that may be made are the following. If the pH is low, add aminomethyl propanol at a maximum of 5% of the total batch requirement. If the pH is high, add citric acid at a maximum of 0.1% of the total batch size, premixing in water first (20% solution). If the viscosity is low, mix an additional 60 minutes and resample. Pumps that should be used for pumping material into the tanks include air diaphragm and positive displacement. Filters that should be used include 80 mesh for all transfer operations. The fill temperature should be 68-95 °F (20-35 °C).

[0375] Composition 12C

Main Phase wt%

DI Water 45.0397

Aminomethyl Propanol (AMP-95) 0.02

Add the following under very vigorous mixing for

30 mins.

Ultrathix P-100" (Acrylic Acid/VP Crosspolymer) 1

Add the following and mix until uniform

Aminomethyl Propanol (AMP-95) 0.44

Side Phase 1

DI Water 20

Sprinkle in the following and mix until clear

Polyquaternium-4 (Celquat H-100) 0.5

Disodium EDTA 0.05

Liquid Additions:

PVP K-90 (20% active) 1

VP/Methacrylamide/Vinyl Imidazole Copolymer

("Luviset Clear" (BASF)) - 20% active 3.5

Polyquaternium-39 (8.5% active) 0.5

Propylene Glycol 1

Sorbitol (70%) 0.5

Add Side Phase 1 to main tank and mix until

uniform

Side Phase 2

DI Water 15.5

Slowly add the following, mix until hydrated

PVM/MA Copolymer (Gantrez S-97 BF (ISP)) 0.2

Sodium Hydroxide (20% active) 0.25

(solution will slightly thicken)

In-process pH specification: 6.90-7.00

Heat Side Phase to 50-55C

Slowly add the following under very vigorous

mixing

Polyquaternium-28 (Conditioneze NT-20 (ISP), 20%

active) 9 (solution will turn opaque and become less viscous)

Slowly add Side Phase 2 to main tank and mix until

uniform

< 45C

Pre-mix next three

PEG-40 Hydrogenated Castor Oil 0.6

PEG/PPG-18/18 Dimethicone (DC- 190) 0.1

Fragrance 0.6

Cocos Nucifera (Coconut) Oil 0.0001

Keratin Amino Acids 0.0001

Flower/Leaf Extract 0.0001

DMDM Hydantoin 0.2

Specifications 12C

pH 6.0-7.0

Viscosity (RV T-C, 5 rpm, 1 min, 25C) 40,000-80,000

Color White (MS)

Odor MS

Viscous, opaque (hazy)

Appearance: gel

[0376] Comparative Composition 12D: Rhodapex ES-2 (sodium laureth sulfate) from Rhodia, diluted with water to 12% active.

[0377] Quantification of Fiber Fragmentation:

Shampoo tress with sodium lauryl ether sulfate.

Apply a set quantity of test material to damp hair and distribute uniformly.

Blow dry tress without combing.

Flat Iron at 205 °C. Pull the flat iron from the top to the bottom of the tress in approximately 12 seconds; repeat 5 times for a total of one minute. Let tress cool. Repeat thermal process for another 3 minutes (total of 4 minutes).

Repeat all of the above three times.

Shampoo tress with sodium lauryl ether sulfate.

Blow Dry w/o combing

Place translucent plastic under tress.

Comb 100 times with fine teeth of comb (realistic strokes, i.e. rate of stroking).

Tape over plastic to secure fragments.

Number all collected hair fragments.

Calculate percent reduction in hair breakage (protection): % hair breakage reduction =[(C - T)/C] x 100

C = # of hair pieces collected for the control

T = # of hair pieces collected for the test

[0378] Equipment used for spectrofluorimetry-tryptophan degradation is a

Spectrofluorimeter-Horiba Jobin Yvon FluoroMax 4. Measurements are taken on five different locations in a window 2.3 cm in width and 1.7 cm in height located in the upper part or root section of the tress which is 2 inches from the bottom of the binding of the tress to the mid-point of the window. Settings of the equipment during measurements are:

Excitation: 290 nm wavelength; 5mm slit

Emission: from 300-400 nm; 5 mm slit; lnm increments

Measurements of the emission spectra from 300-400 nm are recorded in increments of 1 nm. Five measurements at 336 nm (the maximum point for tryptophan emission) are then averaged. This is done for the initial reading as well as after the hot ironing process. Percent degradation is calculated as follows:

i(Ave,S effiinissi is f 336 nm before trea tement -Ave.5 emmissicm readings at 336»rai after treatment^ X Awe.5 emmissions at 336 nm before tr atm ent

Percent protection is calculated as:

f(% Degradation of control— % degradation of experimental)

[0379] Humidity conditions: Hair tresses are stored overnight at 22% RH (76 °C dry bulb; 54 °C wet bulb). Combing tests are conducted at 30% RH (75 °C dry bulb; 56 °C wet bulb).

[00100] Tables 15 and 16 show the anti-breakage data. Table 15 shows the number of hair pieces. Table 16 shows percent reduction in breakage versus Composition 12D.

[00101] Table 15

Regimen Tress 1 Tress 2 Tress 3 Tress 4 Tress 5

12A 352 338 408 202 140

12B 327 294 241 272 172

12C 154 82 157 121 128

12C 412 503 234 289 342 [0380] Table 16

[0381] Figure 8 shows percent thermal protection via tryptophan measurements.

Composition 12C significantly decreases tryptophan degradation. Also, the trend in percent tryptophan loss correlates well with quantification of fiber fragmentation.

[0382] This examples shows that the gel with PEC significantly reduced fiber

fragmentation from combing and percent tryptophan loss.

EXAMPLE 13

[0383] This example demonstrates freeze-thaw stability of exemplary compositions of the present invention.

[0384] Compositions 13A-13D

Composition Composition Composition Composition 13A 13B 13C 13D

Item wt% wt% wt% wt%

Main Phase

DI Water 69.9497 64.9497 59.9497 64.9497

Start heat to 80-85C

Add the following one at time, mix until

fully dissolved.

Disodium EDTA 0.05 0.05 0.05 0.05

L-Aspartic Acid 0.75 0.75 0.75 0.75

Add the following one at a time at 80-85C

and mix until melted

Stearamidopropyl Dimethylamine 2 2 2 2

Cetyl Alcohol 4 4 4 4

Stearyl Alcohol 1 1 1 1

Glyceryl Stearate 1 1 1 1

"Crodamol STS" (100% PPG-3 Benzyl

Ether Myristate) 2 2 2 2

Mix vigorously for 30 minutes at 80-85C

Reduce mixing speed and allow to cool

Trideceth-6) 1 1 1 1

[0385] Compositions 13 E- 13 G

Composition Composition Composition

13E 13F 13G

Item wt% wt% wt%

Main Phase

DI Water 59.9497 62.8097 55.6697

Start heat to 80-85C

Add the following one at time, mix until fully dissolved.

Disodium EDTA 0.05 0.05 0.05

L-Aspartic Acid 0.75 0.75 0.75

Add the following one at a time at 80-85C

and mix until melted

Stearamidopropyl Dimethylamine 2 2 2

Cetyl Alcohol 4 4 4

Stearyl Alcohol 1 1 1

Glyceryl Stearate 1 1 1

"Crodamol STS" (100% PPG-3 Benzyl

Ether Myristate) 2 2 2

Mix vigorously for 30 minutes at 80-85C

Reduce mixing speed and allow to cool

Add the following at 65-70C

Propylene Glycol 0 0 0

Glycerin 10 0 0

Sorbitol (70%) 0 7.14 14.28

Side Phase

DI Water 7.75 7.75 7.75

Slowly add the following, mix until

hydrated

PVM/MA Copolymer (Gantrez S-97 BF

(ISP)) 0.1 0.1 0.1

Sodium Hydroxide (20% active) 0.125 0.125 0.125

(solution will slightly thicken)

In-process pH specification: 6.90-7.00

Heat Side Phase to 50-55C

Slowly add the following under very

vigorous mixing

Polyquaternium-28 (Conditioneze NT-20

(ISP), 20% active) 4.5 4.5 4.5

(solution will turn opaque and become less

viscous)

(mix for -10 minutes)

Add the following at < 45C

DMDM Hydantoin 0.025 0.025 0.025

Slowly add side phase to main phase at <

45-65C

< 45C

"Fluid Blend" 5 5 5

Fragrance 0.6 0.6 0.6

Cocos Nucifera (Coconut) Oil 0.0001 0.0001 0.0001

Keratin Amino Acids 0.0001 0.0001 0.0001

Flower/Leaf Extract 0.0001 0.0001 0.0001

DMDM Hydantoin 0.15 0.15 0.15

Add the following and mix until uniform "Salcare^® SC-96" - Ciba/BASF (65%

Polyquaternium-37, 25% Propylene Glycol

Dicaprylate Dicaprate, 10% PPG-1

Trideceth-6) 1 1 1

Specifications 13C-13I 24 hour specifications 13C-13I:

_PH 4.50-6.00 4.50-6.00

Viscosity (RV T-B, 10 rpm, 1 min, 25C) 15,000-25,000 cps 20,000-30,000cps

Color White (MS) White (MS)

Odor MS MS

Appearance Viscous, opaque emulsion Viscous, opaque emulsion

[0386] Compositions 13H-13K

In-process pH specification: 6.90-7.00

Heat Side Phase to 50-55C

Slowly add the following under very

vigorous mixing

Polyquaternium-28 (Conditioneze NT-20

(ISP), 20% active) 9 9 9 9

(solution will turn opaque and become less

viscous)

(mix for -10 minutes)

Add the following at < 45C

DMDM Hydantoin 0.05 0.05 0.05 0.05

Slowly add side phase to main phase at <

45-65C

< 45C

" Fluid Blend" 5 5 5 5

Fragrance 0.6 0.6 0.6 0.6

Cocos Nucifera (Coconut) Oil 0.0001 0.0001 0.0001 0.0001

Keratin Amino Acids 0.0001 0.0001 0.0001 0.0001

Flower/Leaf Extract 0.0001 0.0001 0.0001 0.0001

DMDM Hydantoin 0.15 0.15 0.15 0.15

Add the following and mix until uniform

"Salcare^® SC-96" - Ciba/BASF (65%

Polyquaternium-37, 25% Propylene Glycol

Dicaprylate Dicaprate, 10% PPG-1

Trideceth-6) 1 1 1 1

[0387] Compositions 13L-13N

Composition Composition Composition

13L 13M 13N

Item wt% wt% wt%

Main Phase

DI Water 47.4497 50.3097 43.1697

Start heat to 80-85C

Add the following one at time, mix until

fully dissolved.

Disodium EDTA 0.05 0.05 0.05

L-Aspartic Acid 0.75 0.75 0.75

Add the following one at a time at 80-85C

and mix until melted

Stearamidopropyl Dimethylamine 2 2 2

Cetyl Alcohol 4 4 4

Stearyl Alcohol 1 1 1

Glyceryl Stearate 1 1 1

"Crodamol STS" (100% PPG-3 Benzyl

Ether Myristate) 2 2 2

Mix vigorously for 30 minutes at 80-85C

Specifications 13J-13P: 24 hour specifications 13J-13P:

pH: 4.50-6.00 4.50-6.00

Viscosity (RV T-B, 10 rpm, 1 min,

25C) 15,000-25,000 cps 20,000-30,000cps

Color: White (MS) White (MS)

Odor MS MS

Appearance Viscous, opaque emulsion Viscous, opaque emulsion [0388] Compositions 130-13R

Flower/Leaf Extract 0.0001 0.0001 0.0001 0.0001

DMDM Hydantoin 0.2 0.2 0.2 0.2

Add the following and mix until uniform

Notes: Leave 10% hole. Post add

Water/Salcare^® SC-96 for varying levels of

Salcare (1 -10%) to achieve final viscosity

spec. 10 10 10 10

DI Water

"Salcare^® SC-96" - Ciba/BASF (65%

Polyquaternium-37, 25% Propylene Glycol

Dicaprylate Dicaprate, 10% PPG-1

Trideceth-6)

Initial Specifications 130- 24 hour specifications

13T: 13Q-13T:

pH: 4.50-6.00 4.50-6.00

Viscosity (RV T-B, 10 rpm, 1 min,

25C): 15,000-25,000 cps 20,000-30,000cps

Color White (MS) White (MS)

Odor MS MS

Appearance Viscous, opaque emulsion Viscous, opaque emulsion

[0389] Compositions 13S-13V

Add the following one at time, mix until

"Salcare^® SC-96" - Ciba/BASF (65%

Polyquatemium-37, 25% Propylene Glycol

Dicaprylate Dicaprate, 10% PPG-1

Trideceth-6) 0 0 0 0

[0390] Compositions 13W-13Z

Reduce mixing speed and allow to cool

Trideceth-6) 0 0 1 1

[0391] Compositions 13 AA-13CC

Composition Composition Composition

13AA 13BB 13CC

Item wt% wt% wt%

Main Phase

DI Water 59.3997 57.3997 49.3997

Side Phase

DI Water 0 0 0

Slowly add the following, mix until

hydrated

PVM/MA Copolymer (Gantrez S-97 BF

(ISP)) 0 0 0

Slowly add side phase to main phase at <

45-65C

< 45C

"Fluid Blend" 5 5 5

Fragrance 0.6 0.6 0.6

Cocos Nucifera (Coconut) Oil 0.0001 0.0001 0.0001

Keratin Amino Acids 0.0001 0.0001 0.0001

Flower/Leaf Extract 0.0001 0.0001 0.0001

DMDM Hydantoin 0.2 0.2 0.2

Add the following and mix until uniform

"Salcare^® SC-96" - Ciba/BASF (65%

Polyquaternium-37, 25% Propylene Glycol

Dicaprylate Dicaprate, 10% PPG-1

Trideceth-6) 1 1 1 ] Compositions 13DD and 13EE

Trideceth-6) 1 5

Initial Specifications 24 hour specifications 13U-13GG: 13U-13GG:

4.50-6.00 4.50-6.00

Viscosity (RV T-B, 10 rpm, 1

min, 25C): 15,000-25,000 cps 20,000-30,000cps

Color: White (MS) White (MS)

Odor: MS MS

Appearance: Viscous, opaque emulsion Viscous, opaque emulsion 93] Compositions 13FF-13HH

] Compositions 13II- 13LL

Comparative

Composition Composition Composition Composition

1311 13JJ 13KK 13LL

Item wt% wt% wt% wt%

Main Phase

er 72.3997 47.3997 47.3997 61.4997

Side Phase Slowly add the following under very

vigorous mixing

Polyquaternium-28 (Conditioneze NT-20

(ISP), 20% active) 0 0 9 9

(solution will turn opaque and become less

viscous)

(mix for ~10 minutes)

Slowly add side phase to main phase at <

45-65C

< 45C

"Fluid Blend" 5 5 5 5

Fragrance 0.6 0.6 0.6 0.6

Cocos Nucifera (Coconut) Oil 0.0001 0.0001 0.0001 0.0001

Keratin Amino Acids 0.0001 0.0001 0.0001 0.0001

Flower/Leaf Extract 0.0001 0.0001 0.0001 0.0001

DMDM Hydantoin 0.2 0.2 0.2 0.15

Add the following and mix until uniform

"Salcare^® SC-96" - Ciba/BASF (65%

Polyquaternium-37, 25% Propylene Glycol

Dicaprylate Dicaprate, 10% PPG-1

Trideceth-6) 1 1 1 5

Initial Specifications 13HH- 24 hour specifications

13MM: 13HH-13MM:

pH: 4.50-6.00 4.50-6.00

Viscosity (RV T-B, 10 rpm, 1

min, 25C) 15,000-25,000 cps 20,000-30,000cps

Color: White (MS) White (MS)

Odor MS MS

Appearance Viscous, opaque emulsion Viscous, opaque emulsion

[0395] The procedure for the freeze/thaw stability studies is as follows:

1. Fill the finished product in a glass jar. If running package stability, fill product in a

container of appropriate packaging.

2. After jar and package have been filled, label each. Tape around the labels to ensure they stay in place throughout the stability study.

Record an initial pH, viscosity, appearance, color and odor for the batch before placing into freezer.

3. Place all of the jars/packages into a freezer for a period of 24 hours.

4. After a period of 24 hours take samples out of the freezer and set them on a bench either in a plastic bin or on a paper towel. Let the samples thaw for 24 hours. 5. After another period of 24 hours check the appearance, color and odor of the sample. If applicable, measure pH and viscosity. Record results.

[0396] Measuring the viscosity uses the following parameters: RV, T-bar B, 1 Orpm, 60 sec, 25°C (except when over 40,000 cps, where the method was RV, T-bar C, 5 rpms, 60 sec, 25°C).

[0397] Tables 17-20 show viscosity (cps) and pH readings of several of the compositions described above.

[0398] Table 17

[0399] Table 18

[0400] Table 19

n a = greater than 1 MM [0401] Table 20

[0402] Salcare^® SC-96 recommendations regarding Compositions 130-13R: use 1-5% for 130, 0.5-3% for 13P, 2-10% for 13Q, 2-12% for 13R.

[0403] Figure 9 shows a comparison of Compositions 13H-13J and 13EE for evaluation of the effectiveness of varying glycols on freeze/thaw stability. Composition 13H does not exhibit freeze thaw stability. Adding 5% propylene glycol (Composition 131) does not greatly improve freeze/thaw stability. Adding 10% propylene glycol (Composition 13J) or lowering cetyl alcohol to 1% with Salcare^® SC 96 (Composition 13EE) shows freeze/thaw stability.

[0404] Figure 10 shows a comparison of Compositions 13K-13N. Different glycols, such as glycerin and sorbitol, are not as effective as propylene glycol in improving freeze/thaw stability.

[0405] Figure 1 1 shows a comparison of Compositions 13A-13C. Lowering the

Polyelectrolyte Complex to 1% shows less severe freeze/thaw instability, but freeze/thaw stability is not optimal (13A vs. 13H). Five percent propylene glycol (13B) shows some improvement; 10% (13C) shows positive results.

[0406] Figure 12 shows a comparison of Compositions 13D-13G. Glycerin and sorbitol do not show freeze/thaw stability, even when Polyelectrolyte Complex is lowered to 1%.

[0407] Figure 13 shows a comparison of Compositions 13S-13U. Adding Polyelectrolyte Complex to emulsion "crashes" the viscosity (13S (no PEC) vs. 13T (with PEC) vs. 13U (with PEC)). Adding Polyelectrolyte Complex after emulsion phase is complete (13U) has slightly less effect than adding it before (13T).

[0408] Figure 14 shows a comparison of Compositions 13V-13X. Adding Salcare^® SC-96 before the emulsion phase can be used to thicken an emulsion, when the Polyelectrolyte Complex is added before or after the emulsion (13W and 13X vs. 13T and 13U). However, initial viscosity is low and final viscosity takes about 72 hours to build, which is not preferred in a production environment. Also, 13X is not preferred in a production environment because the batch is too thick and hard to mix during the emulsion phase (does not have the additional water and PEC to lower viscosity in the batch). Freeze/thaw stability and spreadability can be improved by the addition of propylene glycol or Crodamol STS.

[0409] Figure 15 shows a comparison of Compositions 13FF-13HH. Adding propylene glycol and Crodamol STS does not negatively affect emulsion viscosity (similar results to 13V, 13W, 13X, except viscosity is thicker initially). 13GG is a possible candidate for a one tank process, however, its final viscosity is lower than 13DD/13KK. 13HH is still not preferred in production because the batch is too thick during emulsion phase.

[0410] Figure 16 shows a comparison of Compositions 13Y-13AA. Adding Salcare^® SC- 96 after the emulsion phase also can be used to thicken an emulsion when Polyelectrolyte Complex is added before or after the emulsion (13Z and 13AA vs. 13T and 13U). 13AA is preferred over 13X from a production standpoint because the batch is not too thick and can be properly mixed. The Polyelectrolyte Complex can be added after the emulsion for a thick final product (13AA vs. 13Z). Like 13W and 13X, the Freeze/Thaw stability and

spreadability can be improved with the addition of propylene glycol or Crodamol STS.

[0411] Figure 17 shows a comparison of Compositions 13II-13KK. Adding propylene glycol and Crodamol STS improves initial and final emulsion viscosity (13JJ and 13KK vs. 13Z and 13AA). Complex addition before the emulsion is not preferred because viscosity is thin (13JJ vs. 13KK).

[0412] Figure 18 shows a comparison of compositions 13BB-13DD. Both propylene glycol and Crodamol STS increase viscosity individually, as well as collectively.

[0413] Figure 19 shows a comparison of compositions 13EE and 13LL. Crodamol STS and propylene glycol can be removed if cetyl alcohol is lowered to 1 % and Salcare^® SC-96 is increased to 5% (13EE). Not including cetyl alcohol yields a product that lacks fundamental "conditioner characteristics" (opaqueness, emulsion body) (13LL). EXAMPLE 14

[0414] This example demonstrates split-end mending of exemplary compositions of the invention.

[0415] Composition 14A

I. Prepare 2% active PVM/MA copolymer

Part A

DESCRIPTION %

DEIONIZED WATER 94.4

20% NaOH 3.6

GANTREZ S-97 BF Polymer 2

Adjust pH to 6.95+/- 0.05 with NaOH if

necessary

II. Prepare 2% active Polyquat-28

Part B

DESCRIPTION %

DEIONIZED WATER 90.25

CONDITIONEZE NT-20 9.755

III. Combine A&B (Complex Concentrate)

Part C

DESCRIPTION %

Part A 5

Part B 45

IV. Prepare conditioner formulation

Part D

DESCRIPTION %

Start heating to 75-80C

DEIONIZED WATER 39.67

L-ASPARTIC ACID 0.8

HYDROXYETHYL CELLULOSE 0.5

XANTHAN GUM 0.05

DISODIUM EDTA 0.03

Complex Concentrate (*Part C) 50.1

Heat ff in separate container to

80C

CETYL ALCOHOL 5

STEARAMIDOPROPYL DIMETHYLAMINE 2

GLYCERYL STEARATE 0.2

then add back to water phase and

[0416] The "without complex" composition was prepared as above but with water in place of Part C. The control was Tresemme Anti-Breakage Conditioner.

[0417] Methodology: Use five, 1 " wide bleached, damaged tresses (from Int'l Hair Importers), tag 10 fibers from each swatch with split ends and label appropriately. Take initial photos under microscope. Shampoo using standard procedure (1 mL on 1 " tress, lmin contact time, 10 strokes on each side, 20 sec rinses, 35-40C water temp at rate of 2 gal/min). Condition (1 mL on 1 " tress, lmin contact time, 10 strokes on each side, 20 sec rinses, 35- 40C water temp at rate of 2 gal/min). Comb through wet hair once with wide-tooth end another time using narrow-end. Blow-dry at high heat until fully dry then comb through again twice, once with wide tooth end and another with narrow end. Count the number of fibers mended after the third and sixth treatments. Take final photos.

[0418] Calculations:

% mended = [(total number of tagged fibers before treatment - number of fibers broken off after treatment) - number of split ends after treatment] / (total number of tagged fibers before treatment - number of fibers broken off after treatment)

% breakage = 100 X (number of fibers broken off/ total number of tagged fibers before

treatment)

[0419] Table 21 shows the results.

[0420] Table 21

% MENDING % BREAKAGE

after 3 after 6 after 3 after 6 treatments treatments treatments treatments

Composition 14A 36 48 Composition 14 A 10 16

Control Conditioner 6 14 Control Conditioner 22 22

Without complex 30 18 Without complex 36 42 EXAMPLE 15

[0421] This example demonstrates split-end mending of exemplary compositions of the invention.

[0422] Compositions 15A-15D

Prepare conditioner formulation

Part D

DESCRIPTION

Start heating to 75-80C

DEIONIZED WATER 40.22

L-ASPARTIC ACID 0.4

HYDROXYETHYL CELLULOSE 0.5

XANTHAN GUM 0.05

DISODIUM EDTA 0.03

Complex Concentrate (*Part C) 50.1

Heat ff in separate container to 80C

CETYL ALCOHOL 5

STEARAMIDOPROPYL DIEMTHYLAMINE 2

GLYCERYL STEARATE 0.2

then add back to water phase and mix for 15 minutes

at 75-80C, add;

COCO-BETAINE

cool down to 45C then add rest of the ingredients

DMDM HYDANTOIN 0.2

FRAGRANCE 0.3 adjust with Citric Acid to around pH=5

pH 7.8 7.98 8.07

% L-ASPARTIC ACID ADDITION 0.5 0.4 0.4 0.5 pH 5.50 5.10 4.83 4.85

[0423] Composition 15E

I. Prepare 4% active PVM/MA copolymer

Part A

DESCRIPTION %

DEIONIZED WATER 84.73

10% NaOH 1 1.27

GANTREZ S-97 BF Polymer 4.00

Adjust pH to 6.95+/- 0.05 with NaOH if necessary

pH 7.2

II. Prepare 4% active Polyquat-28

Part B

DESCRIPTION %

DEIONIZED WATER 80.49

CONDITIONEZE NT-20 19.51

III. Combine A&B (Complex Concentrate)

Part C

DESCRIPTION %

Part A 5

Part B 45

IV. Prepare conditioner formulation

Part D

DESCRIPTION %

Start heating to 75-80C

DEIONIZED WATER 39.62

L-ASPARTIC ACID 0.7

HYDROXYETHYL CELLULOSE 0.50

XANTHAN GUM 0.05

DISODIUM EDTA 0.03

Complex Concentrate (*Part C) 50.1

Heat ff in separate container to 80C

CETYL ALCOHOL 5

STEARAMIDOPROPYL DIMETHYLAMINE 2

GLYCERYL STEARATE 0.2

DIMETHICONE 0.3

then add back to water phase and mix for 15 minutes at 75-80C

add;

COCO-BET AINE 1

cool down to 45C then add rest of the ingredients DMDM 0.2

FRAGRANCE 0.3

adjust with Citric Acid to around pH=5

pH 5.54

Vis (RVT-B, lO rpm, 1 min, 25C) 10,000

[0424] Test 1

[0425] From a 1 " wide brown tress, tag fibers with split ends and take initial photos. Separately shampoo tresses with control shampoo (Alberto V05 Normal shampoo) followed by corresponding conditioner treatment. Repeat wash at least twice. Blow dry tresses and air-dry for 24 hours. Take final photos of each tagged fiber.

[0426] The Test 1 results are shown in Figure 20 where the following treatments are shown:

Fiber 1 on Tress 1 : Treated with water

Fiber 2 on Tress 2: Control Shampoo - Control V05 Extra Body Conditioner Fiber 3 on Tress 3: Control Shampoo - Composition 15C

Fiber 4 on Tress 3: Control Shampoo - Composition 15C

[0427] Test 2

[0428] From a 1 " wide brown tress, tag five fibers with split ends and take initial photos. Shampoo tress with control shampoo followed by corresponding conditioner treatment.

(Follow standard washing procedure: lmL, lmin contact time, 20 sec rinse, 35-40°C water temperature). Use one tress for Composition 15E and another with Composition 15C at rate of 2 gal/min. Repeat wash at least twice. Blow dry tresses and air-dry for 24 hours. Take final photos of each tagged fiber.

[0429] Not much conditioning benefit is provided by adding silicone but mending of split-ends is still apparent.

[0430] Test 3

[0431] Use three 1 " wide brown tress, tag 10 fibers from each swatch with split ends and label appropriately. Shampoo using standard procedure (1 mL on 1 " tress, lmin contact time, 10 strokes on each side, 20 sec rinses, 35-40C water temperature at a rate of 2 gal/min).

Condition with Composition 15C (1 mL on 1 " tress, lmin contact time, 10 strokes on each side, 20 sec rinses, 35-40C water temperature at a rate of 2 gal/min). Comb through wet hair once with the wide-tooth end and another time using the narrow-end. Blow-dry then comb through again twice, once with the wide tooth end and another with the narrow end. Repeat above steps as needed. Count the number of fibers mended after each treatment. [0432] The results are shown in Table 22.

[0433] Table 22

[0434] Test 4

[0435] Use five, 1 " wide bleached, damaged tresses (from Int'l Hair Importers), tag 10 fibers from each swatch with split ends and label appropriately. Take initial photos under microscope. Shampoo using standard procedure (1 mL on 1 " tress, lmin contact time, 10 strokes on each side, 20 sec rinses, 35-40C water temp at rate of 2 gal/min). Condition (1 mL on 1 " tress, lmin contact time, 10 strokes on each side, 20 sec rinses, 35-40C water temp at rate of 2 gal/min). Comb through wet hair once with wide-tooth end another time using narrow-end. Blow-dry at high heat until fully dry then comb through again twice, once with wide tooth end and another with narrow end. Count the number of fibers mended after the third, sixth and tenth treatment. Take final photos.

[0436] Calculations

% mended = 100* number of split ends after treatment /

initial number of tagged split end fibers

% breakage = 100* number of fibers broken off / initial number of tagged split end fibers before treatment

[0437] The results are in Table 23.

[0438] Table 23

[0439] Composition 15C provides excellent conditioning on bleached tresses with easy wet combing.

[0440] Test 5

[0441] Use two, 1 " wide bleached, damaged tresses per treatment. Tag 10 fibers from each swatch with split ends and label appropriately. Take initial photos under microscope. Separately shampoo tresses using standard procedure (1 mL on 1 " tress, lmin contact time, 10 strokes on each side, 20 sec rinses, 35-40C water temperature at a rate of 2 gal/min).

Separately condition tresses with Composition 15B, 15C, or 15D (1 mL on 1 " tress, lmin contact time, 10 strokes on each side, 20 sec rinses, 35-40C water temperature at rate of 2 gal/min). Comb through wet hair once with the wide- tooth end and another time using the narrow-end. Blow-dry at high heat until fully dry, then comb through again twice, once with the wide tooth end and another with the narrow end. Count the number of fibers mended after the appropriate number of treatments. Take final photos.

[0442] The results are shown in Table 24.

[0443] Table 24

[0444] Test 6

[0445] Use three 1 " wide brown tresses, tag 10 fibers from each swatch with split ends and label appropriately. Separately shampoo tresses using standard procedure (1 mL on 1 " tress, lmin contact time, 10 strokes on each side, 20 sec rinses, 35-40C water temperature at a rate of 2 gal/min). Separately condition tresses using Control 1 (Nexxus commercial formulation), Control 2, Composition 15A, 15B, 15C, or 15D (1 mL on 1 " tress, lmin contact time, 10 strokes on each side, 20 sec rinses, 35-40C water temp at rate of 2 gal/min). Comb through wet hair once with the wide-tooth end another time using the narrow-end. Blow-dry then comb through again twice, once with the wide tooth end and another with the narrow end. Repeat above steps as needed. Count the number of fibers mended after each treatment. Count the number of broken fibers after each treatment.

[0446] Control 2 composition

DESCRIPTION %

Start heating to 75-80C

DEIONIZED WATER 89.77

L-ASPARTIC ACID 0.8

HYDROXYETHYL CELLULOSE 0.5

XANTHAN GUM 0.05

DISODIUM EDTA 0.03

Heat ff in separate container to

80C CETYL ALCOHOL 5

STEARAMIDOPROPYL DIMETHYLAMINE 2

GLYCERYL STEARATE 0.2

then add back to water phase and mix for 15 minutes at 75-80C

add:

Mackam CB35 (Coco Betaine) 1

cool down to 45 C then add rest

of the ingredients

DMD 0.2

FRAGRANCE 0.45

adjust with Citric Acid to around pH=5

Specifications

pH 4.35

Vis (RVT-B, 10 rpm, 1 min,

25C) 4,800

[0447] The results are shown in Tables 25 and 26.

[0448] Table 25

% Breakage

3 6 treatments treatments

Control 1 42 52

Control 2 (0% PEC) 30 50

Composition 15A (0.5% PEC) 20 40

Composition 15B (1% PEC) 10 15

Composition 15C (2% PEC) 22 28

Composition 15D (3% PEC) 15 25

Table 26

% Mending

3 6 treatments treatments

Control 1 8 10

Control 2 (0% PEC) 25 30

Composition 15A (0.5% PEC) 25 25

Composition 15B (1% PEC) 55 45

Composition 15C (2% PEC) 42 52

Composition 15D (3% PEC) 50 30 EXAMPLE 16

[0450] This example demonstrates split-end mending of exemplary compositions of the present invention.

[0451] Composition 16A

[0452] Mixing Procedure:

1. Premix - Added item #1-2 and mixed until hydrated

2. Used item #3 to adjust pH to 6.9-7, then heated 50-55C

3. Slowly added item #4 under very vigorous mixing, mix for -l Omin

4. In main vessel, added item #5 and began heating to 80-85C

5. Added items #6-7. When batch reached 80C, added #8-10 and mixed for 30 min.

6. Began cooling batch, when below 45C, added premix from step 1 -3 and remaining ingredients

[0453] Target Specifications:

Appearance - opaque, viscous liquid

Odor - to match standard

pH - 4.5-5.5

Viscosity - 10,000-15,000 cps RVT-B 10 rpm, 60 sec [0454] Comparative Composition 16B

[0455] Mixing Procedures:

1. In main vessel, added item #1-2 and began heating to 80-85C

2. Added item #3 when no lumps present

3. When 1-3 had no lumps, continued heating to 80-85C

4. When batch reached 80-85C, added items #4-17 and mixed for 30 minutes

5. Began cooling batch, when below 45C, added 11 -18

[0456] Target Specifications:

Appearance - opaque, viscous liquid

Odor - to match standard

pH - 4.5-5.5

Viscosity - 10,000-15,000 cps RVT-8 10 rpm, 60 sec

[0457] Composition 16A had a pH of 4.92 and a viscosity of 10,800 cps. Composition 16B had a pH of 4.95 and a viscosity of 7,200 cps.

[0458] Composition 16A had much better wet and dry combing when compared to control.

[0459] Double bleached hair tresses were flogged with addition of blow drying to create split ends. Ten splits were tagged in each of four 1 ½ inch wide tresses. Two tresses were then washed with Alberto V05 Normal shampoo and conditioned with Composition 16A. Two tresses were washed with Alberto V05 Normal shampoo and conditioned with

Comparative Composition 16B.

[0460] Composition 16A gave 90% mending of split ends, and Comparative Composition 16B gave 63% mending of split ends. The addition of N-Hance SP-100 to formula improves mending ability of the final formulation.

All references, including publications, patent applications, and patents, cited herein are hereby incorporated by reference to the same extent as if each reference were individually and specifically indicated to be incorporated by reference and were set forth in its entirety herein.

[0461] The use of the terms "a" and "an" and "the" and similar referents in the context of describing the invention (especially in the context of the following claims) are to be construed to cover both the singular and the plural, unless otherwise indicated herein or clearly contradicted by context. The terms "comprising," "having," "including," and

"containing" are to be construed as open-ended terms (i.e., meaning "including, but not limited to,") unless otherwise noted. Recitation of ranges of values herein are merely intended to serve as a shorthand method of referring individually to each separate value falling within the range, unless otherwise indicated herein, and each separate value is incorporated into the specification as if it were individually recited herein. All methods described herein can be performed in any suitable order unless otherwise indicated herein or otherwise clearly contradicted by context. The use of any and all examples, or exemplary language (e.g., "such as") provided herein, is intended merely to better illuminate the invention and does not pose a limitation on the scope of the invention unless otherwise claimed. No language in the specification should be construed as indicating any non-claimed element as essential to the practice of the invention.

[0462] Preferred embodiments of this invention are described herein, including the best mode known to the inventors for carrying out the invention. Variations of those preferred embodiments may become apparent to those of ordinary skill in the art upon reading the foregoing description. The inventors expect skilled artisans to employ such variations as appropriate, and the inventors intend for the invention to be practiced otherwise than as specifically described herein. Accordingly, this invention includes all modifications and equivalents of the subject matter recited in the claims appended hereto as pennitted by applicable law. Moreover, any combination of the above-described elements in all possible variations thereof is encompassed by the invention unless otherwise indicated herein or otherwise clearly contradicted by context.

Claims

CLAIMS:

1. A hair care composition comprising:

a polyelectrolyte complex comprising a cationic polymer and an anionic polymer; from about 3% to about 5% of a thickening agent; and

about 2% or less of an emollient;

wherein the percentages are based on the total weight of the composition.

2. The composition of claim 1, wherein the thickening agent comprises a quaternary ammonium nitrogen compound or polymer.

3. The composition of claim 2, wherein the quaternary ammonium nitrogen polymer is polyquaternium-37.

4. The composition of claim 3, wherein the polyquaternium-37 is in a mixture with propylene glycol dicaprylate/dicaprate and polypropylene glycol- 1 trideceth-6.

5. The composition of claim 1 , wherein the emollient is a fatty alcohol.

6. The composition of claim 5, wherein the fatty alcohol is cetyl alcohol, stearyl alcohol, or a combination thereof.

7. The composition of claim 1 , wherein the polyelectrolyte complex is in an amount of from about 1 % to about 8% based on the total weight of the composition.

8. The composition of claim 7, wherein the polyelectrolyte complex is in an amount of from about 1 % to about 3% based on the total weight of the composition.

9. The composition of claim 1 , wherein the cationic polymer comprises one or more monomeric units with one or more quaternary ammonium nitrogen moieties.

10. The composition of claim 9, wherein the cationic polymer is polyquateraium-

28.

1 1. The composition of claim 1 , wherein the anionic polymer comprises monomeric units having ionizable carboxylic acid moieties.

12. The composition of claim 1 1, wherein the anionic polymer is a methylvinylether/maleic acid copolymer.