Hygroscopicity and Hardness of Hair Spray Resins at Varying Humidities

Morris J. Root; Stanley Bohac

HAIR SPRAV RESINS 605 because it makes the films more flexible and prevents flaking since the absorbed water acts like a plasticizer.. It is to be understood from the data presented that several resins are available to give any desired hygroscopieity or hardness character- istics the data should not be construed to show relative ratings. Soft and tacky films may be desirable for such formulations in which stick- ing together of hair after combing is of prime importance. (Received June 8, 1966) REFERENCES (1) National Starch Technical Service Bulletin No. 743, Resyn oe8-1310, National Starch and Chemical Corp. (2) Reiter, R. W., and Horning, R. G., U.S. Patent 2,996,471 (August 15, 1961). (3) National Starch Technical Service Bulletin No. 406, Resyn 26'-131t., National Starch and Chemical Corp. (4) Davidson, R. L., and Sittig, M., Water Soluble Resins, Reinhold Publishing Co., 1962, p. 113. (5) Technical Service Bulletin No. 2M-9-59, Antara Chemicals, Division of General Aniline and Film Corp. (6) Private Communication, Daikin Kyogo Co., Ltd.

606 JOURNAL OF THE SOCIETY OF COSMETIC CHEMISTS CHANGE OF ADDRESS (1) Allow 6 weeks to make the change. (2) Send change to Editorial Assistant, 761 North Valley Chase Rd., Bloomfield Hills, Michigan 48013 (3) Print name and new ad- dress-including postal zone number. Give old address--if possible re- turn addressed portion of the envelope in which your last Journal was mailed.

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HAIR SPRAV RESINS 605 because it makes the films more flexible and prevents flaking since the absorbed water acts like a plasticizer.. It is to be understood from the data presented that several resins are available to give any desired hygroscopieity or hardness character- istics the data should not be construed to show relative ratings. Soft and tacky films may be desirable for such formulations in which stick- ing together of hair after combing is of prime importance. (Received June 8, 1966) REFERENCES (1) National Starch Technical Service Bulletin No. 743, Resyn oe8-1310, National Starch and Chemical Corp. (2) Reiter, R. W., and Horning, R. G., U.S. Patent 2,996,471 (August 15, 1961). (3) National Starch Technical Service Bulletin No. 406, Resyn 26'-131t., National Starch and Chemical Corp. (4) Davidson, R. L., and Sittig, M., Water Soluble Resins, Reinhold Publishing Co., 1962, p. 113. (5) Technical Service Bulletin No. 2M-9-59, Antara Chemicals, Division of General Aniline and Film Corp. (6) Private Communication, Daikin Kyogo Co., Ltd.

606 JOURNAL OF THE SOCIETY OF COSMETIC CHEMISTS CHANGE OF ADDRESS (1) Allow 6 weeks to make the change. (2) Send change to Editorial Assistant, 761 North Valley Chase Rd., Bloomfield Hills, Michigan 48013 (3) Print name and new ad- dress-including postal zone number. Give old address--if possible re- turn addressed portion of the envelope in which your last Journal was mailed.

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HAIR SPRAY RESINS 603 7O 6O • •o • •o Io N.S-7 • I I I I I I I 5O 6O 70 80 Reinfive Humidity (%) l,'i,gure 10. Sward hardness of various resin films rs. relative humidity (B()øC) 7O 6O • 40 •_ •o '• 20 m I0 0 VEM-5 • '"" • •-- VEM-O i ' I I I I I I I 50 60 70 80 Relative Humidity (%) I 9o Figure 11. Sward hardness of various resin fiHns with 3.5•0 plasticizer (Silicone oil DC 555) rs. relative humidity (30øC) well as unneutralized (VEM-0). The percentage of water absorption is based on dry resin. All tests were made with films with and without plasticizer. Whenever a plasticizer was used, it was 3.5% Silicone Oil DC 555* based on dry resin. Figure 4 shows the moisture absorption at different relative hu- midities of various resin films at equilibrium. PVP K-30 shows the greatest moisture absorption, followed by PVP/VA 735. VEM has lower humidity pick-up. As can be anticipated, unneutralized resin has lower moisture absorption than does neutralized resin because of its lower water solubility. Resyn 28-1310 has the lowest moisture absorp- tion. Figure 5 shows the results with plasticized films. There is a decrease in the water absorption of the plasticized fihns in comparison with the nonplasticized films. * Dow Corning Corp., Midland, Mich.

6{)4 JOURNAL OF THE SOCIETY OF COSMETIC CHEMISTS Figure 6 shows the moisture absorption rate of these films conditioned at $0% relative humidity and then exposed to 90% RH. Both ear- boxylie types of resin have a much faster conditioning rate than PVP/VA 735 and finally PVP K-30. Plastieized films have approximately the same conditioning rate (Fig. 7), except that the initial and final ab- sorptions are lower than those of unplastieized films. The drying rate of films conditioned at 90% RH and then exposed to 50% RH is shown in Fig. $. Equilibrium is reached by all the films in two to four hours except PVP/VA 735 and PVP K-30. Figure 9 gives the results with films that have been plastieized. The drying rate curves of plastieized films are all displaced downward due to the hydrophobic character of the plastieizer. Figure 10 shows the variation of Sward Hardness with relative humidities from 50 to 90% at equilibrium. It can be seen that the unneutralized VEM-0 and 50% neutralized VEM-5 give the hardest films. These are followed by 90% neutralized VEM-9, except beyond 61% RH where the hardness is surpassed by the unneutralized Resyn 28-1310. It can be seen that the hardness of both the PVP K-30 and PVP/VA 735 decrease more rapidly. Figure 11 gives similar data using plasticized films. Hardness obtained with plastieized films with sili- cone oil could, of course, be affected by at least three factors: (a) plastieizer decreases the moisture pick-up which results in harder film (b) plastieizer itself decreases the hardness and (e) plastieizer lubri- cates the surface between the film and the Sward Hardness rocker, thereby increasing the Sward Hardness reading. Each of these factors may produce different effects, even on the same plastieized film at different humidities. CONCLUSIONS In conclusion, it can be seen from the foregoing that the greater the degree of neutralization the greater the hygroscopicity of the films of carboxylic types of resins. PVP/VA 735 and PVP K-30 films are more hygroscopic than any of the films made with VEM or the Resyn 28-1310 resins. Although moisture pick-up by the VEM resin is greater than that of Resyn 28-1310, the hardness of the former at any given humidity is greater. Greater hardness at high humidity means less tack. A hard film on the hair will break more easily when the comb is passed through, whereas a soft, tacky film will put drag on the comb. Soft, tacky films will also result in hair snagging with resultant difficulty in combing. A certain degree of moisture pick-up is perhaps desirable

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HAIR SPRAY RESINS 603 7O 6O • •o • •o Io N.S-7 • I I I I I I I 5O 6O 70 80 Reinfive Humidity (%) l,'i,gure 10. Sward hardness of various resin films rs. relative humidity (B()øC) 7O 6O • 40 •_ •o '• 20 m I0 0 VEM-5 • '"" • •-- VEM-O i ' I I I I I I I 50 60 70 80 Relative Humidity (%) I 9o Figure 11. Sward hardness of various resin fiHns with 3.5•0 plasticizer (Silicone oil DC 555) rs. relative humidity (30øC) well as unneutralized (VEM-0). The percentage of water absorption is based on dry resin. All tests were made with films with and without plasticizer. Whenever a plasticizer was used, it was 3.5% Silicone Oil DC 555* based on dry resin. Figure 4 shows the moisture absorption at different relative hu- midities of various resin films at equilibrium. PVP K-30 shows the greatest moisture absorption, followed by PVP/VA 735. VEM has lower humidity pick-up. As can be anticipated, unneutralized resin has lower moisture absorption than does neutralized resin because of its lower water solubility. Resyn 28-1310 has the lowest moisture absorp- tion. Figure 5 shows the results with plasticized films. There is a decrease in the water absorption of the plasticized fihns in comparison with the nonplasticized films. * Dow Corning Corp., Midland, Mich.

6{)4 JOURNAL OF THE SOCIETY OF COSMETIC CHEMISTS Figure 6 shows the moisture absorption rate of these films conditioned at $0% relative humidity and then exposed to 90% RH. Both ear- boxylie types of resin have a much faster conditioning rate than PVP/VA 735 and finally PVP K-30. Plastieized films have approximately the same conditioning rate (Fig. 7), except that the initial and final ab- sorptions are lower than those of unplastieized films. The drying rate of films conditioned at 90% RH and then exposed to 50% RH is shown in Fig. $. Equilibrium is reached by all the films in two to four hours except PVP/VA 735 and PVP K-30. Figure 9 gives the results with films that have been plastieized. The drying rate curves of plastieized films are all displaced downward due to the hydrophobic character of the plastieizer. Figure 10 shows the variation of Sward Hardness with relative humidities from 50 to 90% at equilibrium. It can be seen that the unneutralized VEM-0 and 50% neutralized VEM-5 give the hardest films. These are followed by 90% neutralized VEM-9, except beyond 61% RH where the hardness is surpassed by the unneutralized Resyn 28-1310. It can be seen that the hardness of both the PVP K-30 and PVP/VA 735 decrease more rapidly. Figure 11 gives similar data using plasticized films. Hardness obtained with plastieized films with sili- cone oil could, of course, be affected by at least three factors: (a) plastieizer decreases the moisture pick-up which results in harder film (b) plastieizer itself decreases the hardness and (e) plastieizer lubri- cates the surface between the film and the Sward Hardness rocker, thereby increasing the Sward Hardness reading. Each of these factors may produce different effects, even on the same plastieized film at different humidities. CONCLUSIONS In conclusion, it can be seen from the foregoing that the greater the degree of neutralization the greater the hygroscopicity of the films of carboxylic types of resins. PVP/VA 735 and PVP K-30 films are more hygroscopic than any of the films made with VEM or the Resyn 28-1310 resins. Although moisture pick-up by the VEM resin is greater than that of Resyn 28-1310, the hardness of the former at any given humidity is greater. Greater hardness at high humidity means less tack. A hard film on the hair will break more easily when the comb is passed through, whereas a soft, tacky film will put drag on the comb. Soft, tacky films will also result in hair snagging with resultant difficulty in combing. A certain degree of moisture pick-up is perhaps desirable

J. Soc. Cosmetic Chemists, 17, 607-621 (1966) Evaluation of Certain Factors Influencing Oil Deposition on Skin After Immersion in an Oil Bath M. E. STOLAR, Ph.D.* Presented May 10, lb66, New York City Synopsis--Previously developed methods for determining quantitatively the amount of oil and recording the oil film deposited on the skin after immersion in oil baths were utilized to evaluate various oils of potential use in bath oil formulations. The effect of the presence of various surfactants in mineral oil on the amount and skin coverage of the deposited oil film was determined. The existence of a relationship between spreading coefficient values and the amount or skin coverage of the deposited oil film was investigated. The use of bath oils in the treatment of dry scaly skin has gained favor in the last few years. Originally, dry skin was explained on the assumption that the surface lubricating lipid film was qualitatively or quantitatively modified or even missing (1). Blank (2) and Borota (3) demonstrated that cornified material obtained from callus remained soft and pliable as long as it retained moisture. To extend the duration of moisture retention, as indicated by softness and pliability, the tissues were coated with oil and placed on a wet surface. Normal baths are frequently contraindicated due to their degreasing and drying effects on the skin (4). Pillsbury et al. (5) claimed that im- mersion of the skin in water followed by topical application of grease demonstrated beneficial effects. These may be attributed to hydration of the stratum corneum due to a decrease in the rate of moisture loss * Dome Laboratories, Div. Miles Chemicals, Inc, 125 West End Ave, New York• N. Y, 10023. 607

608 JOURNAL OF THE SOCIETY OF COSMETIC CHEMISTS Table I Effect of Grade of Mineral Oil (0.02%) Dispersed in Water (40øC) on Oil Deposition on Skin aft(r 15 Minutes of hnmersion Amount Amount Con-Fosition in of Oil •" Specific Saybolt Added Grade of Naph- Paraf- Gravity Viscosity to Bath Oil thehie fiuic at g0øF at 100øF (g) Mineral oil USP'* 40 () 6(/. 0 0.88,5 850 0. 200 Mineral oil NF •' 37.0 ( •1.0 0. 852 88 0. 200 Mineral oil technical" 30.0 70. f) 0. 882 55 0. 200 of Oil •/• of Eluted Oil De- from posited Skin (g) on Skin 0. 044 •' 22.2 O. 06? 81.0 0. 080 • 40.0 Supplied by Sonnenborn Chemical and Refining Company, New York, N.Y. Average of six determinations. Table II Spreading Coefficient Values for Various Grades of Mineral Oil Surface Specific Tension Interfacial Spreading Grade of Gravity at 25 øC Tension Coefficient Oil • at 60øF (dynes/era) at 25øC at 25øC Mineral oil USP 0. 885 •2.2 44.6 -- 4.8 Mineral oil NF 0. 852 33.4 41.9 -- 8.8 Mineral oil technical 0. 832 81.4 41.8 0 Supplied by Sonnenborn Chemical and Refining Company, New York, N.Y. from the skin without affecting the rate of moisture diffusion from the underlying tissues (1). Clinical studies attesting to the beneficial effects of bath oils have been reported in medical literature (6-9). Commercially available bath oils may be classified as either spreading or dispersible types. The spreading type tends to form a surface film of oil on the water, while the dispersible type forms a dispersion of fine droplets of oil throughout the water. Both types are claimed to deposit an oil film on the immersed skin. Knox (10) described the development of a water dispersible oil bath which is deposited on skin surfaces. Taylor (11) reported that about twice as much oil is deposited from aqueous dispersions of mineral oil as from vegetable oil. Similar conclusions were reached by Knox (12). Taylor's results are based on the difference between the initial amount of oil present in an immersion cylinder and the residual amount after immersion for a specified period of time. This difference is indicative of the amount of oil deposited on the treated skin surface. Stolar (13) recently developed a method for determining the actual amount of oil deposited on the skin after immersion in an oil bath and

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