CALCULATION OF HLB VALUES OF NON-IONIC SURFACTANTS

William C. Griffin

254 JOURNAL OF THE SOCIETY OF COSMETIC CHEMISTS TAB[oe 1--(Continued) Name Mfr. * Chemical Designation Typet HLB j'•' Atlas G-2140 1 Tetraethylene glycol mono61eate N 7.7 Atlas G-2800 1 Polyoxypropylene mannitol dioleate N 8 Atlas G-1493 1 Polyoxyethylene sorbitol lanolin oleate derivative N 8 Atlas G-1425 1 Polyoxyethylene sorbitol lanolin derivative N 8 Atlas G-3608 1 Polyoxypropylene stearate N 8 Span 20 1 Sorbitan monolaurate N 8.6 Arlacel :20 1 Sorbitan monolaurate N 8.6 Emulphor VN-430 3 Polyoxyethylene fatty acid N 9 Atlas Go1734 1 Polyoxyethylene sorbitol beeswax derivative N 9 Atlas G-2111 1 Polyoxyethylene oxypropylene ole- ate N 9 Atlas G-2125 1 Tetraethylene glycol monolaurate N 9.4 Brij 30 1 Polyoxyethylene lauryl ether N 9.5 Tween 61 1 Polyoxyethylene sorbitan monoste- arate N 9.6 Atlas G-2154 1 Hexaethylene glycol monostearate N 9.6 Tween 81 1 Polyoxyethylene sorbitan mono61e- ate N 10.0 Atlas G-1218 1 Polyoxyethylene esters of mixed fatty and resin acids N 10.2 Atlas G-3806 1 Polyoxyethylene cetyl ether N 10.3 Tween 65 1 Polyoxyethylene sorbitan tristea- rate N 10.5 Atlas G-3705 1 Polyoxyethylene lauryl ether N 10.8 Tween 85 1 Polyoxyethylene sorbitan trioleate N 11 Atlas G-2116 1 Polyoxyethylene oxypropylene ole- ate N 11 Atlas G-1790 1 Polyoxyethylene lanolin derivative N 11 Atlas G-2142 1 Polyoxyethylene mono61eate N 11.1 Myrj 45 1 Polyoxyethylene monostearate N 11.1 Atlas G-2141 1 Polyoxyethylene monobleate N 11.4 P.E.G. 400 mono- oleate 6 Polyoxyethylene mono61eate N 11.4 P.E.G. 400 mono- oleate 7 Polyoxyethylene mono61eate N 11.4 Atlas G-2076 1 Polyoxyethylene monopalmitate N 11.6 S-541 4 Polyoxyethylene monostearate N 11.6 P.E.G. 400 mono- stearate 6 Polyoxyethylene monostearate N 11.6 P.E.G. 400 mono- stearate 7 Polyoxyethylene monostearate N 11.6 Atlas G-3300 1 Alkyl aryl sulfonate A 11.7 Triethanolamine oleate A 1:2 Atlas G-2127 1 Polyoxyethylene monolaurate N 1:2.8 Igepal CA-630 3 Polyoxyethylene alkyl phenol N 12.8 Atlas G-1431 1 Poloxyethylene sorbitol lanolin de- rivative N 13 Atlas G-1690 1 Polyoxyethylene alkyl aryl ether N 13 S-307 4 Polyoxyethylene monolaurate N 13.1 P.E.G. 400 mono- laurate 6 Polyoxyethylene monolaurate N 13.1 Atlas G-2133 1 Polyoxyethylene lauryl ether N 13.1 Atlas Go1794 1 Polyoxyethylene castor oil N 13.3 Emulphor EL-719 3 Polyoxyethylene vegetable oil N 13.3 Tween 21 1 Polyoxyethylene sorbitan mono- laurate N 13.3

HLB VALUES OF NON-IONIC SURFACTANTS TaBLV- 1--(Continued) 255 Name Moer.* Chemical Designation Type t HLB t t Renex 20 1 Polyoxyethylene esters of mixed fatty and resin acids N 13.5 Atlas G-1441 1 Pol.yox.yethylene sorbitol lanolin de- rivarive N 14 Atlas G-7596J 1 Polyoxyethylene sorbitan mono- burate N 14.9 Tween 60 1 Polyoxyethylene sorbitan monoste- arate N 14.9 Tween 80 1 Polyoxyethylene sorbitan mono- oleate N 15 Myrj 49 1 Polyoxyethylene monostearate N 15.0 Atlas G-2144 1 Polyoxyethylene mono61eate N 15.1 Atlas G-3915 I Polyoxyethylene oleyl ether N 15.3 Atlas G-3720 1 Polyoxyethylene stearyl alcohol N 15.3 Atlas G-3920 1 Polyoxyethylene oleyl alcohol N 15.4 Emulphor ON.870 3 Polyoxyethylene fatty alcohol N 15.4 Atlas G-2079 1 Polyoxyethylene glycol monopal- mitate N 15.5 Tween 40 1 Poly. oxyethylene sorbitan monopal- m•tate N 15.6 Atlas G-3820 1 Polyoxyethylene cetyl alcohol N 15.7 Atlas G-2162 1 Polyoxyethylene oxypropylene ste- arate N 15.7 Atlas G-1471 1 Pol.yox.yethylene sorbitol lanolin de- nvauve N 16 Myrj 51 1 Polyoxyethylene monostearate N 16.0 Atlas G-7596P 1 Polyoxyethylene sorbitan mono- laurate N 16.3 Atlas G-2129 1 Polyoxyethylene monolaurate N 16.3 Atlas G-3930 1 Polyoxyethylene oleyl ether N 16.6 Tween 20 1 Polyoxyethylene sorbitan mono- burate N 16.7 Brij 35 1 Polyoxyethylene lauryl ether N 16.9 Myrj 52 1 Polyoxyethylene monostearate N 16.9 Myrj 53 1 Polyoxyethylene monostearate N 17.9 Sodium oleate A 18 Atlas G-2159 1 Polyoxyethylene monostearate N 18.8 Potassium oleate A 20 Atlas G-263 1 N-cetyl N-ethyl morpholinium ethosulfate C 2540 1 Pure sodium lauryl sulfate A App. 40 * 1 = Atlas Powder Company, 2 -•- Emulsol Corporation, 3 = General Aniline & Film Corporation, 4 -- Glyco Products Company, Inc.. 5 -- Goldschmidt Chemical Corporation, 6 = Kessler Chemical Company, Inc., 7 -- W. C. Hardesty Company, Inc. t A -- Artionic, C -- Cationic, N -- Non-ionic. tt HLB values, either calculated or determined, believed to be correct to 4-1. a variety of physical tests. There appears to be a correlation of required HLB value with chemical composition, though there are insufficient data to show a fixed relationship at the present time. It seems possible that, given (1) a suitable sorting-coding system for surfactants based on (a) HLB, and (b) chemical type, and (2) a more or less parallel or complementary sorting-coding system for the lipophilic ma-

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254 JOURNAL OF THE SOCIETY OF COSMETIC CHEMISTS TAB[oe 1--(Continued) Name Mfr. * Chemical Designation Typet HLB j'•' Atlas G-2140 1 Tetraethylene glycol mono61eate N 7.7 Atlas G-2800 1 Polyoxypropylene mannitol dioleate N 8 Atlas G-1493 1 Polyoxyethylene sorbitol lanolin oleate derivative N 8 Atlas G-1425 1 Polyoxyethylene sorbitol lanolin derivative N 8 Atlas G-3608 1 Polyoxypropylene stearate N 8 Span 20 1 Sorbitan monolaurate N 8.6 Arlacel :20 1 Sorbitan monolaurate N 8.6 Emulphor VN-430 3 Polyoxyethylene fatty acid N 9 Atlas Go1734 1 Polyoxyethylene sorbitol beeswax derivative N 9 Atlas G-2111 1 Polyoxyethylene oxypropylene ole- ate N 9 Atlas G-2125 1 Tetraethylene glycol monolaurate N 9.4 Brij 30 1 Polyoxyethylene lauryl ether N 9.5 Tween 61 1 Polyoxyethylene sorbitan monoste- arate N 9.6 Atlas G-2154 1 Hexaethylene glycol monostearate N 9.6 Tween 81 1 Polyoxyethylene sorbitan mono61e- ate N 10.0 Atlas G-1218 1 Polyoxyethylene esters of mixed fatty and resin acids N 10.2 Atlas G-3806 1 Polyoxyethylene cetyl ether N 10.3 Tween 65 1 Polyoxyethylene sorbitan tristea- rate N 10.5 Atlas G-3705 1 Polyoxyethylene lauryl ether N 10.8 Tween 85 1 Polyoxyethylene sorbitan trioleate N 11 Atlas G-2116 1 Polyoxyethylene oxypropylene ole- ate N 11 Atlas G-1790 1 Polyoxyethylene lanolin derivative N 11 Atlas G-2142 1 Polyoxyethylene mono61eate N 11.1 Myrj 45 1 Polyoxyethylene monostearate N 11.1 Atlas G-2141 1 Polyoxyethylene monobleate N 11.4 P.E.G. 400 mono- oleate 6 Polyoxyethylene mono61eate N 11.4 P.E.G. 400 mono- oleate 7 Polyoxyethylene mono61eate N 11.4 Atlas G-2076 1 Polyoxyethylene monopalmitate N 11.6 S-541 4 Polyoxyethylene monostearate N 11.6 P.E.G. 400 mono- stearate 6 Polyoxyethylene monostearate N 11.6 P.E.G. 400 mono- stearate 7 Polyoxyethylene monostearate N 11.6 Atlas G-3300 1 Alkyl aryl sulfonate A 11.7 Triethanolamine oleate A 1:2 Atlas G-2127 1 Polyoxyethylene monolaurate N 1:2.8 Igepal CA-630 3 Polyoxyethylene alkyl phenol N 12.8 Atlas G-1431 1 Poloxyethylene sorbitol lanolin de- rivative N 13 Atlas G-1690 1 Polyoxyethylene alkyl aryl ether N 13 S-307 4 Polyoxyethylene monolaurate N 13.1 P.E.G. 400 mono- laurate 6 Polyoxyethylene monolaurate N 13.1 Atlas G-2133 1 Polyoxyethylene lauryl ether N 13.1 Atlas Go1794 1 Polyoxyethylene castor oil N 13.3 Emulphor EL-719 3 Polyoxyethylene vegetable oil N 13.3 Tween 21 1 Polyoxyethylene sorbitan mono- laurate N 13.3

HLB VALUES OF NON-IONIC SURFACTANTS TaBLV- 1--(Continued) 255 Name Moer.* Chemical Designation Type t HLB t t Renex 20 1 Polyoxyethylene esters of mixed fatty and resin acids N 13.5 Atlas G-1441 1 Pol.yox.yethylene sorbitol lanolin de- rivarive N 14 Atlas G-7596J 1 Polyoxyethylene sorbitan mono- burate N 14.9 Tween 60 1 Polyoxyethylene sorbitan monoste- arate N 14.9 Tween 80 1 Polyoxyethylene sorbitan mono- oleate N 15 Myrj 49 1 Polyoxyethylene monostearate N 15.0 Atlas G-2144 1 Polyoxyethylene mono61eate N 15.1 Atlas G-3915 I Polyoxyethylene oleyl ether N 15.3 Atlas G-3720 1 Polyoxyethylene stearyl alcohol N 15.3 Atlas G-3920 1 Polyoxyethylene oleyl alcohol N 15.4 Emulphor ON.870 3 Polyoxyethylene fatty alcohol N 15.4 Atlas G-2079 1 Polyoxyethylene glycol monopal- mitate N 15.5 Tween 40 1 Poly. oxyethylene sorbitan monopal- m•tate N 15.6 Atlas G-3820 1 Polyoxyethylene cetyl alcohol N 15.7 Atlas G-2162 1 Polyoxyethylene oxypropylene ste- arate N 15.7 Atlas G-1471 1 Pol.yox.yethylene sorbitol lanolin de- nvauve N 16 Myrj 51 1 Polyoxyethylene monostearate N 16.0 Atlas G-7596P 1 Polyoxyethylene sorbitan mono- laurate N 16.3 Atlas G-2129 1 Polyoxyethylene monolaurate N 16.3 Atlas G-3930 1 Polyoxyethylene oleyl ether N 16.6 Tween 20 1 Polyoxyethylene sorbitan mono- burate N 16.7 Brij 35 1 Polyoxyethylene lauryl ether N 16.9 Myrj 52 1 Polyoxyethylene monostearate N 16.9 Myrj 53 1 Polyoxyethylene monostearate N 17.9 Sodium oleate A 18 Atlas G-2159 1 Polyoxyethylene monostearate N 18.8 Potassium oleate A 20 Atlas G-263 1 N-cetyl N-ethyl morpholinium ethosulfate C 2540 1 Pure sodium lauryl sulfate A App. 40 * 1 = Atlas Powder Company, 2 -•- Emulsol Corporation, 3 = General Aniline & Film Corporation, 4 -- Glyco Products Company, Inc.. 5 -- Goldschmidt Chemical Corporation, 6 = Kessler Chemical Company, Inc., 7 -- W. C. Hardesty Company, Inc. t A -- Artionic, C -- Cationic, N -- Non-ionic. tt HLB values, either calculated or determined, believed to be correct to 4-1. a variety of physical tests. There appears to be a correlation of required HLB value with chemical composition, though there are insufficient data to show a fixed relationship at the present time. It seems possible that, given (1) a suitable sorting-coding system for surfactants based on (a) HLB, and (b) chemical type, and (2) a more or less parallel or complementary sorting-coding system for the lipophilic ma-

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256 JOURNAL OF THE SOCIETY OF COSMETIC CHEMISTS T.•SLZ 2--"REo. ux•-ED HLB" VALVES w/o o/w Emulsion Emulsion Solubilizing* Acid, stearic .. 17 Alcohol, cetyl 13 Lanolin, anhydrous }' 15 Oil Cottonseed .. 7.5 Essential Mineral, heavy ¾ 1•)'. • Mineral, light 4 10-12 Vitamin (with fats or oils) ..... Vitamin (fat free) Petrolatum ¾ lb'.'5 Vitamins Esters ..... Oils (see "Oils" above) Wax Beeswax 5 10-16 Microcrystalline 9.5 Paraffin (household) ¾ 9 1• '.• 1¾.5 15 16.5 * O/W, i.e., solubilizing in water. terials used with surfactants, a cross relationship could be set up. With such a system, it should be possible to screen all the available surfactants in a few minutes and select a few that are worthy of extensive study. In summary, two conditions usually must be satisfied in choosing a sur- factant for any desired formulation. First, the proper HLB or hydrophilic content of the surfactant must be used, and second the proper chemical type of the surfactant must be chosen. Random choice, i.e., the old trial- and-error method, can lead to many selections that are wrong in two ways that is, both by chemical type and HLB. By first determining the optimum HLB value and then selecting and testing a variety of chemical types at this particular value a large number of wrong trials can be eliminated. The HLB method permits a more systematized trial than possible previously. HLB values may be calculated from analytical or composition data or the system may be used without calculating or determining exact value since it is a method of operation that has some correlation with water solubility of the surfactants. There is need for further work in this field to establish a rapid, more exact experimental procedure for observing HLB values, for de- termining "required HLB's," and for classifying and correlating chemical types of surfactants.

ACCELERATED STORAGE TESTS* By F. GROSSMITH, B.Sc., F.R.I.C. Macleans, Ltd., Brentford, Middlesex, England Is SPEAKING of accelerated storage tests one has in mind procedures which w•11 give a rapid indication of the shelf life characteristics of cosmetic preparations. Possible types of deterioration cover a wide field, and in- formation may be required covering some, or all of the following character- istics: emulsion stability freedom from phase separation or other change in structure of the prod- uct colour stability freedom from clouding and deposition resistance to spoilage by microbiological or oxidative processes avoidance of drying out freedom from undesirable corrosive action between product and con- tainer etc., etc. AVAILABLE TECHNIQUES--ACCELERATED SHELF TESTS At the outset let it be said that there is no complete substitute for the long term shelf test under practical conditions through a range of seasons, and for the new product, whenever the possibility exists, such tests should be carried out. Next to long term shelf tests are shelf tests involving an intensification of the environmental factor of interest, for example, high humidity, ultraviolet radiation, exposure of the unit pack to the vapour of odorous materials, and, perhaps most important of all, testing the stability of the preparation when exposed to variations of temperature. During practical conditions of transit and storage, products are exposed to temperatures which are rarely static for long, and so temperature tests should include alternating temperatures. It is usually accepted that twelve-hour cycles alternating between -3-2 and 50øC. duplicate the effects of most temperature extremes. For the home market 30øC. alternating * Presented at the April 9, 1954, Meeting, London, England. 257

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252 JOURNAL OF THE SOCIETY OF COSMETIC CHEMISTS HLB values for a wide variety of surfactants have been calculated or observed and are listed in Table 1. As with any system that deals with surfactants, there are occasional side effects which seem to alter the estab- lished value. These are often unique to the test that is being run and there is no explanation for them at the present time. Because of the difficulty, time, and expense involved in carrying out the experimental procedure, relatively few of the host of available surfactants have had their HLB values determined. However, this is not the disad- vantage that it first appears to be, since a rough estimate of the HLB can be made from the degree of water solubility and in many instances this is adequate for screening work. In its present form, the HLB system lacks exactness. A suitable simple laboratory method of measuring HLB values of surfactants accurately is needed. We have tried a variety of methods including solubility in water, or various solvents, ratio solubility in two solvents, solubilization behavior both for oils and dyes, surface and interfacial tension data, cloud point behavior, and many other properties. Of these the most promising is the determination of the cloud point of an aqueous sol'ution of the surfactant. However, this test still possesses severe limitations. In addition to hydrophile-lipophile balance, it is believed that surfactants possess a second property which is related to their behavior. We call it chemical type. For example, we may find that esters of a particular fatty acid provide better emulsification in a given system than any other fatty acid esters or polyoxyalkylene fatty alcohols may give better performance than esters. In all probability, chemical type is related to the attraction of the lipophilic group in the surfactant for the lipophilic material with which the surfactant is being used. This, we believe, governs the efficiency of a surfactant, provided it is of the proper HLB. This second characteris- tic point, the nature of the hydrophilic and lipophilic groups, also requires further study. To select a surfactant properly for any application, we believe that one must first have the optimum HLB value and secondly have the correct chemical type. Since, at the moment we have correlation only for the HLB value our procedure is to establish the required HLB and then try a variety of chemical types at that optimum HLB. This procedure eliminates trial of all surfactants that are of the wrong HLB and, thus, reduces the time and effort required to solve a problem. Just as each surfactant or surfactant blend exhibits an HLB value each lipophilic material or blend of lipophilic materials with which surfactants are used exhibits an optimum required HLB value for any specific formula- tion or application, 'Fable 2. The determination of required HLB values has also been studied both from the standpoint of calculation and

HLB VALUES OF NON-IONIC SURFACTANTS 253 TAn•.E 1--CA•.CV•.ATEr) Ant) DETm•mn•r) HLB V^Lv•s Name Mfr.* Chemical Designation Typet HI,Bt•' Span 85 1 Arlacel 85 1 Atlas G-1706 1 Span 65 l Arlacel 65 1 Atlas G-1050 1 Eracol EO-50 2 Emcol ES-50 2 Atlas G-1704 1 Eracol PO-50 2 Atlas G-922 1 "Pure" 6 Atlas G-2158 1 Emcol PS-50 2 Emcol EL-50 2 Era col PP-50 2 Arlacel C 1 Arlacel 83 Atlas G-2859 1 Atmul 67 1 Atmul 84 1 Tegin 515 5 Aldo 33 4 "Pure" 6 Atlas G-1727 1 Emcol PM-50 2 Span 80 Arlacel 80 1 Atlas G-917 1 Atlas G-3851 1 Eracol PL-50 2 Span 60 Arlacel 60 1 Atlas G-2139 1 Emcol DO-50 2 Atlas G-2146 1 Emcol DS-50 2 Atlas G-1702 1 Emcol DP-50 2 Aldo 28 4 Tegin 5 Emcol DM-50 2 Atlas G-1725 1 Atlas G-2124 1 Emcol DL-50 2 Glaurin 4 Span 40 1 Ariaeel 40 1 Atlas G-2242 1 Atlas G-2147 1 Sorbitan trioleate N 1.8 Sorbitan trioleate N 1.8 Polyoxyethylene sorbitol beeswax derivative N 2 Sorbitan tristearate N 2.1 Sorbitan tristearate N 2.1 Polyoxyethylene sorbitol hexastea- rate N 2.6 Ethvlene glycol fatty acid ester N 2.7 Eth3, lene glycol fatty acid ester N 2.7 Polyoxyethylene sorbitol beeswax derivative N 3 Propylene glycol fatty acid ester N 3.4 Propylene glycol monostearate N 3.4 Propylene glycol monostearate N 3.4 Propylene glycol monostearate N 3.4 Propylene glycol fatty acid ester N 3.4 Ethylene glycol fatty acid ester N 3.6 Propylene glycol fatty acid ester N 3.7 Sorbitan sesquioleate N 3.7 Sorbitan sesquioleate N 3.7 Polyoxyethylene sorbitol 4.5 oleate N 3.7 Glycerol monosrearate N 3.8 Glycerol monostearate N 3.8 Glycerol monostearate N 3.8 Glycerol monostearate N 3.8 Glycerol monostearate N 3.8 Polyoxyethylene sorbitol beeswax derivative N 4 Propylene glycol fatty acid ester N 4.1 Sorbitan mono61eate N 4.3 Sorbitan mono61eate N 4.3 Propylene glycol monolaurate N 4.5 Propylene glycol monolaurate N 4.5 Propylene glycol fatty acid ester N 4.5 Sorbitan monostearate N 4.7 Sorbitan monostearate N 4.7 Diethylene glycol mono61eate N 4.7 Diethylene glycol fatty acid ester N 4.7 Diethylene glycol monostearate N 4.7 Diethylene glycol fatty acid ester N 4.7 Polyoxyethylene sorbitol beeswax derivative N 5 Diethylene glycol fatty acid ester N 5.1 Glycerol monostearate (self-emulsi- fying) A 5.5 Glycerol monostearate (self-emulsi- fying) A 5.5 Diethylene glycol fatty acid ester N 5.6 Polyoxyethylene sorbitol beeswax derivative N 6 Diethylene glycol monolaurate (soap free) N 6.1 Diethylene glycol fatty acid ester N 6.1 Diethylene glycol monolaurate (soap free) N 6.5 Sorbitan monopahnitate N 6.7 Sorbitan monopahnitate N 6.7 Polyoxyethylene dioleate N 7.5 Tetraethylene glycol monostearate N 7.7

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