Classifications

• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K8/00—Cosmetics or similar toiletry preparations
  • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
  • A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
  • A61K8/23—Sulfur; Selenium; Tellurium; Compounds thereof
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K8/00—Cosmetics or similar toiletry preparations
  • A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
  • A61K8/04—Dispersions; Emulsions
  • A61K8/044—Suspensions
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K8/00—Cosmetics or similar toiletry preparations
  • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
  • A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
  • A61K8/20—Halogens; Compounds thereof
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K8/00—Cosmetics or similar toiletry preparations
  • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
  • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
  • A61K8/60—Sugars; Derivatives thereof
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
  • A61Q5/00—Preparations for care of the hair
  • A61Q5/006—Antidandruff preparations
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
  • A61Q5/00—Preparations for care of the hair
  • A61Q5/02—Preparations for cleaning the hair

Definitions

• the invention relates to structured aqueous shampoos having suspending properties. Formulating suspensions of water insoluble, or sparingly soluble solids and/or liquids in aqueous shampoos presents a long-standing problem.
• Formulators need to be able to suspend a variety of such ingredients.
• oils, anti-dandruff agents, such as selenium sulphide, hair conditioners including cationic polymers, and opacifiers such as mica are widely used.
• opacifiers such as mica
• the latter desirably, also comprise anionic and /or amphoteric surfactants, such as alkyl ether sulphates, or betaines, which are high foaming and mild to the skin.
• Cationic polymers such as poly(diallyldimethylammonium) chloride, referred to hereinafter as "polyquaternium", are widely used as hair conditioners. There is therefore a need to disperse them in aqueous shampoos. Cationic polymers are, however liable to interact with anionic or amphoteric surfactants. Formulators have serious problems dispersing them in shampoo active systems to form stable homogeneous dispersions.
• Selenium sulphide is widely used as an anti-dandruff agent, but presents problems of formulation. It is a dense, water-insoluble solid, with a strong, unattractive orange colour. Attempts to maintain selenium sulphide in suspension have generally involved the use of polymeric thickeners. It has also been proposed to suspend selenium sulphide in structured surfactant systems. However due to its high density, some sedimentation is usually observed. Even the most effective suspending systems have not been able to avoid an appearance of inhomogeneity.
• structured surfactant suspending systems that are capable of suspending cationic polymers and dense particles such as selenium sulphide stably, without sedimentation, using shampoo surfactants which give dense stable foams with good wetting and feel.
• structured system means a pourable composition comprising water, surfactant, any structurants, which may be required to impart suspending properties to the surfactant, and optionally other dissolved matter, which together form a mesophase, or a dispersion of a mesophase in a continuous aqueous medium, and which has the ability to immobilise non-colloidal, water- insoluble particles, while the system is at rest, thereby forming a stable, pourable suspension.
• mica can be tinted to match different hair shades, making it a positively desirable ingredient.
• Mica is used herein broadly, where the context permits, to include natural mica, artificially coated mica, and synthetic, mica-like, pearlescent, mineral flakes such as calcium aluminium borosilicate, which can be coated to give similar effects to coated mica.
• Mica is one of a large number of lamellar solids known to be capable of imparting a pearly appearance to liquids, but in practice its use in aqueous formulations has been restricted because, like selenium sulphide, it is difficult to suspend. Pearl shampoos are therefore normally formulated with glycol stearates, which are self-suspending.
• Gums and polymeric thickeners which increase the viscosity of the liquid medium, retard, but do not prevent sedimentation, and at the same time make the composition harder to pour. They do not provide stable suspensions.
• Colloidal dispersions contain particles of about 1 micron or smaller, which are prevented from sedimenting by Brownian motion. Such systems are obviously incapable of dispersing relatively coarse particles. They are moreover not fully stable, because the dispersed particles tend to grow in size, due to agglomeration and Ostwald ripening, until they are too large to be maintained in suspension.
• Structured suspending systems depend on the rheological properties of the suspending medium to immobilise the particles, irrespective of size. This requires the suspending medium to exhibit a yield point, which is higher than the sedimenting or creaming force exerted by the suspended particles, but low enough to enable the medium to flow under externally imposed stresses, such as pouring and stirring, like a normal liquid. The structure reforms sufficiently rapidly to prevent sedimentation, once the agitation caused by the external stress has ceased.
• L ⁇ -phases Three main types of structured system have been employed in practice, all involving an L ⁇ -phase, in which bilayers of surfactant are arranged with the hydrophobic part of the molecule on the interior and the hydrophilic part on the exterior of the bilayer (or vice versa).
• the bilayers lie side by side, e.g. in a parallel or concentric configuration, sometimes separated by aqueous layers.
• L ⁇ -phases also known as G- phases
• Such evidence may comprise first, second and sometimes third order peaks with a d-spacing (2 ⁇ /Q, where Q is the momentum transfer vector) in a simple integral ratio 1:2:3.
• Other types of symmetry give non-integral ratios.
• the d-spacing of the first peak in the series corresponds to the repeat spacing of the bilayer system.
• Most surfactants form an L ⁇ -phase either at ambient or at some higher temperature when mixed with water in certain specific proportions. However such conventional L ⁇ -phases do not usually function as structured suspending systems. Useful quantities of solid render them unpourable and smaller amounts tend to sediment.
• Dispersed lamellar phases are two phase systems, in which the surfactant bilayers are arranged as parallel plates to form domains of L ⁇ -phase, which are interspersed with an aqueous phase to form an opaque gel-like system. They are described in EP 0 086614.
• Spherulitic phases comprise well-defined spheroidal bodies, usually referred to in the art as spherulites, in which surfactant bilayers are arranged as concentric shells.
• the spherulites usually have a diameter in the range 0.1 to 15 microns and are dispersed in an aqueous phase in the manner of a classical emulsion, but interacting to form a structured system.
• Spherulitic systems are described in more detail in EP 0 151 884. Many structured systems are intermediate between dispersed lamellar and spherulitic, involving both types of structure. Usually systems having a more spherulitic character are preferred because they tend to have lower viscosity.
• a variant on the spherulitic system comprises prolate or rod shaped bodies sometimes referred to as batonettes. These are normally too viscous to be of practical interest.
• Both of the foregoing systems comprise two phases. Their stability depends on the presence of sufficient dispersed phase to pack the system so that the interaction between the spherulites or other dispersed mesophase domains prevents separation. If the amount of dispersed phase is insufficient, e.g. because there is not enough surfactant or because the surfactant is too soluble in the aqueous phase to form sufficient of a mesophase, the system will undergo separation and cannot be used to suspend solids. Such unstable systems are not "structured" for the purpose of this specification.
• a third type of structured system comprises an expanded L ⁇ -phase. It differs from the other two types of structured system in being essentially a single phase, and from conventional L ⁇ -phase in having a wider d-spacing.
• Conventional L ⁇ -phases which typically contain 60 to 75% by weight surfactant, have a d-spacing of about 4 to 7 nanometers. Attempts to suspend solids in such phases result in stiff pastes which are either non-pourable, unstable or both.
• the H-phase comprises surfactant molecules arranged to form cylindrical rods of indefinite length. It exhibits hexagonal symmetry and a distinctive texture under the polarising microscope. Typical H-phases have so high a viscosity that they appear to be curdy solids. H-phases near the lower concentration limit (the Li/H-phase boundary) may be pourable but have a very high viscosity and often a mucus-like appearance. Such systems tend to form expanded L ⁇ -phases particularly readily on addition of sufficient electrolyte.
• Expanded L ⁇ -phases are described in more detail in EP 0 530 708. In the absence of suspended matter they are generally translucent, unlike dispersed lamellar or spherulitic phases, which are normally opaque. They are optically anisotropic and have shear-dependent viscosity. In this they differ from Li -phases, which are micellar solutions or microemulsions. Li-phases are clear, optically isotropic and are usually substantially Newtonian. They are unstructured and cannot suspend solids.
• Li -phases exhibit small angle x-ray diffraction spectra, which show evidence of hexagonal symmetry and/or exhibit shear dependent viscosity.
• Such phases usually have concentrations near the Li/H-phase boundary and may form expanded L ⁇ -phases on addition of electrolyte.
• electrolyte In the absence of any such addition of electrolyte they lack the yield point required to provide suspending properties, and are not, therefore, "structured systems" for the purpose of this specification.
• Expanded L ⁇ -phases of the above type are usually less robust than spherulitic systems. They are liable to become unstable at low temperatures. Moreover they frequently exhibit a relatively low yield stress, which may limit the maximum size of particle that can be stably suspended.
• structured surfactants require the presence of a structurant, as well as surfactant and water in order to form structured systems capable of suspending solids.
• the term "structurant” is used herein to describe any non-surfactant capable, when dissolved in water, of interacting with surfactant to form or enhance (e.g. increase the yield point of,) a structured system. It is typically a surfactant-desolubiliser, e.g. an electrolyte.
• certain relatively hydrophobic surfactants such as isopropylamine alkyl benzene sulphonate can form spherulites in water in the absence of electrolyte.
• Such surfactants are capable of suspending solids in the absence of any structurant, as described in EP 0 414 549.
• WO 01/05932 It is known from WO 01/05932 that carbohydrates can interact with surfactants to form suspending structures. Such systems generally exhibit even greater d-spacings than the electrolyte-structured expanded L ⁇ -phases, described in EP 0 530 708.
• the d- spacings of the sugar-structured systems, described in WO 01/05932 are typically greater than 15nm, and may, for example, be as high as 50nm.
• Such systems can be obtained in a clear or translucent form by suitable choice of surfactant and carbohydrate concentration.
• the structured surfactant systems available hitherto have failed to combine adequate suspending power to suspend particles such as selenium sulphide or cationic polymer, with the foaming characteristics required of a shampoo.
• the invention provides a novel aqueous suspending system, which comprises:
• the invention provides a shampoo containing suspended particle of anti-dandruff agent, such as selenium sulphide and/or of a cationic polymer.
• anti-dandruff agent such as selenium sulphide and/or of a cationic polymer.
• the invention also provides the use of mica to improve the appearance of aqueous selenium sulphide suspensions.
• the mica is coated with a metal oxide or silica.
• an anti-dandruff shampoo which comprises an aqueous suspending medium for selenium sulphide having an effective amount of selenium sulphide suspended therein, characterised in that the suspension additionally comprises sufficient suspended mica to provide a more homogeneous-looking product.
• the aforesaid aqueous suspending medium for selenium sulphide comprises a surfactant and sufficient of an electrolyte or carbohydrate structurant to form a structured surfactant suspending system.
• the invention provides a clear, transparent container, containing an anti-dandruff shampoo as aforesaid.
• an anti-dandruff shampoo as aforesaid.
• the composition of the invention is a shampoo, which preferably comprises surfactants suitable for the cleaning of hair.
• the surfactant system is typically a high foaming mild surfactant, which may be anionic, non-ionic, amphoteric, zwitterionic or cationic. Mixtures of anionic with non-ionic, zwitterionic and/or amphoteric surfactants are particularly preferred.
• the surfactant comprises at least one high HLB surfactant, which is preferably an anionic surfactant, and which has an HLB greater than 37, more preferably greater than 38, most preferably greater than 39.
• the high HLB surfactant has an HLB less than 80, more preferably less than 50, most preferably less than 45.
• the high HLB surfactant constitutes more than 50% by weight of the total surfactant, more preferably at least 60%, most preferably at least 70%.
• the surfactant preferably comprises at least one lower HLB surfactant, e.g. having an HLB less than 35, preferably less than 30, more preferably less than 20, even more preferably lower than 15.
• the lower HLB surfactant preferably has an HLB greater than 0.5, more preferably greater than 1.
• Preferred examples include surfactants having an HLB greater than 5, but less than 12 more preferably less than 10, in particular sarcosinates, alkyl sulphates, hydroxysultaines, and diethanolamides, such as coconut diethanolamide.
• the surfactant should comprise low HLB non-ionic foam boosters having an HLB between 0.5 and 5, including fatty acids such as oleic acid, fatty alcohols such as oleyl alcohol, acetylated monoglycerides, glyceryl diesters, such as glyceryl dioleate, sorbitan triesters such as sorbitan trioleate and sorbitan tristrearate.
• fatty acids such as oleic acid
• fatty alcohols such as oleyl alcohol
• acetylated monoglycerides such as glyceryl diesters, such as glyceryl dioleate
• sorbitan triesters such as sorbitan trioleate and sorbitan tristrearate.
• the low HLB surfactant should preferably be present in a sufficient proportion to the higher HLB surfactant to provide a mean HLB between 13 and 36.5, more preferably above 15, still more preferably above 20, even more preferably above 25, most preferably above 27, but preferably less than 36, more preferably less than 35, most preferably less than 34.
• the preferred high HLB anionic surfactants comprise alkyl ether sulphates.
• the latter are preferably the products obtained by:
• Suitable alkyl ether sulphates also include alkyl glyceryl sulphates, and random- or block-copolymerised alkyl ethoxy/propoxy sulphates.
• Other anionic surfactants typically of lower HLB, which may be present include, for example: Gio-jo e.g.
• aliphatic ester sulphonates e.g. alkyl glyceryl sulphonates
• a mixture of alkyl ether sulphate and sarcosinate is particularly preferred.
• the cation of the anionic surfactant is typically sodium and/or ammonium. However it may alternatively or additionally comprise potassium, lithium, calcium, magnesium, ammonium, or an alkyl or hydroxyalkyl ammonium having up to 6 aliphatic carbon atoms including ethylammonium, isopropylammonium, monoethanolammonium, diethanolammonium, and triethanolammonium, or a mixture of any of the foregoing.
• the surfactant may optionally comprise non-ionic surfactants such as amine oxides, polyglyceryl fatty esters, fatty acid ethoxylates, fatty acid monoalkanolamides, fatty acid dialkanolamides, fatty acid alkanolamide ethoxylates, propylene glycol monoesters, fatty alcohol propoxylates, alcohol ethoxylates, alkyl phenol ethoxylates, fatty amine alkoxylates and fatty acid glyceryl ester ethoxylates.
• non-ionic surfactants such as amine oxides, polyglyceryl fatty esters, fatty acid ethoxylates, fatty acid monoalkanolamides, fatty acid dialkanolamides, fatty acid alkanolamide ethoxylates, propylene glycol monoesters, fatty alcohol propoxylates, alcohol ethoxylates, alkyl phenol ethoxylates, fatty
• non-ionic compounds suitable for inclusion in compositions of the present invention include mixed ethylene oxide/ propylene oxide block copolymers, ethylene glycol monoesters, alkyl polyglycosides, alkyl sugar esters including alkyl sucrose esters and alkyl oligosaccharide esters, sorbitan esters, ethoxylated sorbitan esters, alkyl capped polyvinyl alcohol and alkyl capped polyvinyl pyrrolidone.
• the surfactant may comprise an amphoteric or zwitterionic surfactant.
• the former may comprise so-called imidazoline betaines, also called amphoacetates, which were traditionally ascribed the zwitterionic formula:
• R preferably has at least 8, more preferably at least 10 carbon atoms but less than 25, more preferably less than 22, even more preferably less than 20, most preferably less than 18.
• R represents a mixture of alkyl and alkenyl groups, obtained, for example, from coconut or palm oil, and having sizes ranging from 8 to 18 carbon atoms, with 12 predominating, or a fraction of such a feedstock, such as lauryl (>90%C 12 ).
• the zwitterionic surfactant is preferably a betaine or sulphobetaine, e.g.
• R' is an aliphatic group having 1 to 4 carbon atoms and R" is an aliphatic group having from 8 to 25 carbon atoms, preferably a straight or branched chain alkyl or alkenyl group, or more preferably a group of the formula RCONR' (CH 2 ) ni where R and R' have the same significance as before, and n is an integer from 2 to 4.
• R' is a methyl, carboxymethyl, ethyl, hydroxyethyl, carboxyethyl, propyl, isopropyl, hydroxypropyl, carboxypropyl, butyl, isobutyl or hydroxybutyl group.
• the surfactant may comprise cationic surfactants such as fatty alkyl trimethylammonium or benzalkonium salts, amidoamines or imidazolines.
• the total surfactant is present in a proportion of at least 2, more preferably at least 7, still more preferably at least 9, most preferably at least 10% by weight based on the total weight of the formulation, but less than 30, more preferably less than 25, most preferably less than 23% by weight.
• the surfactant comprises A. an ether sulphate and B. a sarcosinate, betaine or sulphobetaine in a ratio of A:B from 1:1 to 4:1, preferably 1.5:1 to 3:1.
• the anti-dandruff shampoo of the invention has suspending properties, sufficient to suspend an anti-dandruff agent such as selenium sulphide. It should be capable of maintaining at least the major portion of the solid in suspension for at least three months. This may be achieved by the conventional method of adding thickening polymers, such as xanthan gum or ethylene glycol stearates. However we prefer suspending systems that give no sedimentation after three months. To achieve this, it is generally necessary to use a structured suspending system, and in particular a novel suspending system as herein described. We particularly prefer the use of sugar structured surfactant systems in the present invention. We have also found that use of clear suspending systems, such as those of WO 01/05932 or WO 00/63079, provide mica suspensions, which are particularly attractive, visually.
• the sugar is preferably a mono or, more preferably, disaccharide sugar, most preferably sucrose, but could for example be fructose, maltose, glucose or invert sugar.
• Other sugars which can be used, include, for example, mannose, ribose, galactose, lactose, allose, altrose, talose, gulose, idose, arabinose, xylose, lyxose, erythrose, threose, acrose, rhamnose, fucose, glyceraldehyde, stachyose, agavose and cellobiose or a tri- or tetra-saccharide.
• the composition may contain an electrolyte as structurant.
• concentration of electrolyte and/or sugar is preferably sufficient to provide a structured suspending system.
• the amount required depends on the nature and concentration of the surfactant. Typically, in the case of electrolyte alone, this is greater than 4, preferably greater than 5, more preferably greater than 6, most preferably greater than 7% by weight, based on the weight of the formulation, but less than 20, more preferably less than 15, most preferably less than 12%.
• the amount required is typically greater than 20%, preferably more than 30% most preferably more than 40%, but preferably less than 60% by weight.
• the electrolyte is typically sodium and/or ammonium chloride, but could, for example, alternatively or additionally be or comprise, sodium carbonate, potassium chloride, sodium, phosphate, or sodium citrate.
• compositions of the invention are preferably substantially free from electrolyte.
• substantially free means that they do not contain electrolyte in quantities sufficient to confer a suspending structure on the shampoo surfactant in the absence of the low HLB surfactant. Generally the lower the electrolyte content, the better the foaming properties. We prefer that the concentration of electrolyte is less than 7%, more preferably less than 5%, still more preferably less than 3%, even more preferably less than 1%, most preferably less than 0.1% by weight of the composition.
• our invention therefore provides a substantially electrolyte-free structured aqueous shampoo composition comprising:
• a high foaming anionic, amphoteric and/or zwitterionic shampoo surfactant (1) A high foaming anionic, amphoteric and/or zwitterionic shampoo surfactant.
• the low HLB surfactant comprises a non-ionic surfactant, which is preferably a low HLB foam booster having an HLB less than 5.
• the optimum amount of electrolyte and/or low HLB surfactant can be determined by making incremental additions and measuring the yield point, e.g. using a rheometer, to determine where the maximum yield point is obtained.
• a quick indication of the optimum amount is obtained by measuring conductivity. This falls with the addition of electrolyte or low HLB surfactant, to a minimum, located within a shallow trough, and then rises to a peak.
• the preferred range is usually within +/-2%, preferably +1-1%, of the first such minimum.
• Another quick indication of the formation of a structured system is to shake air into the composition and observe the bubbles, which show no tendency to rise in a structured system.
• the shampoo preferably contains a cationic polymer, which may for example comprise a polyquaternium polymer, present in an amount effective for hair treatment. Typically this requires at least 0.01%, preferably at least 0.05%, more preferably at least 0.1%, most preferably at least 0.2% by weight of the polymer. While it is technically possible to suspend much larger concentrations of polymer, e.g. more than 10%, for reasons of cost effectiveness we prefer to use less than 5%, more preferably less than 2%, still more preferably less than 1%, most preferably less than 0.5% by weight of the polymer.
• the anti-dandruff shampoo of the invention preferably contains at least an effective amount, preferably more than 0.05, more preferably more than 0.1, most preferably more than 0.5%, by weight, based on the total weight of the composition, of selenium sulphide.
• the upper limit technically, is largely dependant upon what viscosity can be tolerated, however the more selenium there is present, the more mica will be required to mask it. This, as well as economic considerations, dictates a practical concentration less than 7%, preferably less than 5%, more preferably less than 3%, most preferably less than 2% by weight of the composition.
• the particle size of the selenium sulphide is preferably greater than 0.1 ⁇ m, more preferably greater than 1 ⁇ m, more preferably still, greater than 10 ⁇ m.
• the particles are preferably less than lmm, more preferably less than 0.75mm, still more preferably less than 0.5mm, most preferably less than 0.1mm.
• the proportion of mica required to give a homogeneous appearance will depend on the amount of selenium sulphide, but is typically at least 0.01, preferably at least 0.05, more preferably at least 0.1, most preferably at least 0.2% by weight of the composition. To avoid excessive cost, and also viscosity, it is preferred that the concentration of mica is less than 5, more preferably less than 2, still more preferably less than 1, most preferably less than 0.5% by weight of the composition.
• the mica preferably has a particle size greater than l ⁇ m, more preferably greater than 5 ⁇ m, most preferably greater than 10 ⁇ m, but less than 200 ⁇ m, more preferably less than 100 ⁇ m, most preferably less than 50 ⁇ m.
• the composition preferably contains effective amounts of hair conditioners such as oleyl alcohol, ethyl oleate, oleyl ethoxylate or glycerol, e.g. in proportions greater than 0.05, preferably greater than 0.1, more preferably greater than 0.5, most preferably greater than 0.7 % by weight of the composition, but less than 10, preferably less than 5, more preferably less than 3, most preferably less than 2%.
• the product preferably contains a buffer, such as a citrate/ citric acid buffer.
• a buffer such as a citrate/ citric acid buffer.
• the pH is preferably greater than 4, more preferably greater than 5. Where the ingredients are sufficiently stable, the pH is still more preferably greater than 6, most preferably greater than 6.5, but less than 9, more preferably less than 8, most preferably less than 7.5. In the case of selenium sulphide the Ph needs to be lower to ensure stability, e.g. below 6.
• the product may optionally contain other common ingredients of shampoos, such as, essential oils, fragrances, pigments, dyes, antiseptics and topical medicaments.
• the product is suitable for marketing in clear containers, such as glass or plastic bottles, or plastic tubes or sachets.
• the above composition was a stable, mild, high foaming structured liquid.
• the mean HLB of the surfactants was 33.
• the suspending system, in the absence of solid was clear.
• the suspension was stable after two months and had a particularly desirable golden lustre. It was especially suitable for washing blond hair.
• the following formulation was prepared by adding the following ingredients to water in the order shown, with gentle stirring, to avoid air entrainment.
• the ether sulphate and alkyl sulphate were each added as a 28% w/w aqueous solution.
• the surfactants had a mean HLB of 28.
• Samples were prepared using three different tints of oxide-coated mica to give shampoo formulations suitable for blond, brunette and red hair respectively.
• the shampoos were stable, pourable and had a particularly fine pearly lustre, compared with conventional pearl shampoo based on ethylene glycol stearates as the pearlising agent. The presence of the selenium sulphide was not detectable.
• the above composition was a stable, mild, high foaming structured liquid.
• the surfactant had a mean HLB of 33.
• 1% of micronized selenium sulphate (median particle size 5 ⁇ m)
• a suspension was obtained, which showed no separation after six months storage at laboratory ambient temperature.
• Small angle X- ray diffraction and electron microscopy confirmed a spherulitic structure.
• the formulation had an unattractive mottled appearance.
• the above composition was a fully stable, homogeneous-looking, spherulitic liquid, with an attractive metallic gold sheen.
• the surfactant had a mean HLB of 32. No sedimentation was observed after six months storage.
• a cationic polymer formulation was prepared by adding the following ingredients, except the ammonium chloride, to water in the order shown, with gentle stirring, and then blending with a high shear mixer. The mixture was allowed to deaerate for two hours. Finally the ammonium chloride was added with gentle stirring to avoid excessive air entrainment. The ether sulphate and alkyl sulphate were each added as a 28% w/w aqueous solution.
• Electrolyte-free formulations were prepared by adding the following ingredients to water in the order shown, with gentle stirring at room temperature until homogeneous.
• the formulations were buffered to pH 5.5 with a citrate buffer. They formed suspensions with 10% coated mica, which were stable at room temperature and at 45 ° C after two months.
• the Examples had a viscosity of approximately 3 Ps at 21s "1 shear.

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