Research & Development (R&D)
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- Kory Wilson
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1 Research & Development (R&D) Concept Brief/ Formula direction Formulation of the Product Testing of the Product (Safety, Stability and Claims) Manufacture of the Product
2 The Metric System Scientist throughout the world use the metric system for measurement. The Metric System is based on WATER, where 1 gram (g) = 1 milliliter (ml) = 1 cubic centimeter (cc). I Kilogram = 1000grams etc.
3
4
5 Equipment used in the lab Beakers
6 Prop Mixer
7 Homogenizers: Gifford Wood- High Flow, Low Shear Pro Scientific - Low Flow, High Shear
8 Balance/ Scale
9 Ring Stand and Clamps
10 Hot Plate
11 Separatory Funnel
12 Lab Notebook
13 Heat Seal tube crimper
14 Hopper
15 Kettles Manufacturing Equipment
16 TYPES OF FORMULATIONS Aerosols & Non Aerosol sprays Emulsions Gels and Solutions Sticks Anhydrous (liquids, solids and semisolids) Powders
17 Aerosols Any product that is evacuated out of a sealed, pressurized container. EXAMPLES: Hair Spray, Spray deodorant, Continuous spray sunscreens. PRO: Fine Mist, Controllable dosage, good coverage, usually light weight and stable formulas. CON: Flammable, High MOQ s, specialty manufacturers, requires XP equipment, requires use of a PROPELLANT that can be irritating. Hard to fill in the lab. May require registration with the ATF.
18 CFC s (Chloroflurocarbons)used to be used as a Propellant, however these have since been banned due to environmental protection legislations. Propellants in cosmetics today are mostly mixtures of volatile HYDROCARBONS like propane, n-butane and isobutane.
19 Example Ingredient Listing Tresemme Extra Firm Control Hairspray alcohol denat., hydrofluorocarbon 152A, va/crotonates/vinyl neodecanoate, copolymer, octylacrylamide/ acrylates/ butylaminoethyl methacrylate copolymer, aminomethyl propsanol, dimethyl stesramine, fragrance (parfum), linalool, limonee, butylphenyl, methylpropional, amyl cinnamal, hexyl cinnamal, citronellol, geraniol.
20 Non-Aerosol Sprays Any product that is evacuated through a spray pump. Examples include pump hair spray, linen sprays and body sprays. These products typically contain high amounts of ethyl alcohol (ethanol) that might require registration with the ATF. PRO: better for the environment, easier to source components, have more control over the formula ingredients. CON: not as fine of a mist, compromise on the dosage, packaging compatibility issues.
21 Example Ingredient Listing Bumble & bumble Prep: Water\Aqua\Eau, Ascophyllum Nodosum (Algae) extract, Humulus Lupulus (Hops) extract, Macrocystis Pyrifera (Kelp) extract, Rosmarinus Officinalis (Rosemary) Leaf Extract, Tocopheryl Acetate, Biotin, Cysteine, Retinyl Palmitate, Linoleic Acid, Linolenic Acid, Amodimethicone, Distearlydimonium Chloride, Trideceth-10, Disodium EDTA, Citric Acid, Diazolidinyl Urea, Limonene, Fragrance (parfum). <ILN31468>
22 EMULSIONS A fine dispersion of one or more insoluble liquid in another. Basic Types: o/w (Oil in Water) w/o (Water in Oil) w/s & s/w (Water in Silicone & Silicone in Water) CHAPTER 13 & CHAPTER 25
23
24 Parts of an Emulsion Oil Phase (Waxes, oils, Lipophilic Ingredients, Emollients) Water Phase (Surfactants, Hydrophilic ingredients, Glycols, Emollients ) Emulsifier Preservatives Fragrance, Color or Active Ingredients
25 WATER PHASE OIL PHASE Making an Emulsion HEATING, EMULSIFYING, ADDITIONAL INGREDIENTS MIXING (Side note: SHEER v SHEAR) COOLING EVALUATION
26 o/w emulsion An emulsion in which which the dispersed phase is an oil and the external (continuous) phase is water. Most common type of emulsion Micelles --->
27 Example Ingredient Listing Bliss Fabulous Every Day Eye Cream Water (Aqua), Squalane, Glycerin, Neopentyl Glycol Dicaprylate/Dicaprate, Butylene Glycol, Cetearyl Ethylhexanoate, Steareth-21, Hydrogenated Coco-Glycerides, Vitis Vinifera Seed Oil, Glyceryl Stearate, Polymethyl Methacrylate, Prunus Armeniaca (Apricot) Kernel Oil, Macadamia Ternifolia Seed Oil, Ribes Nigrum (Black Currant) Seed Oil, Citrus Aurantium Dulcis (Orange) Peel Oil, Sodium Hyaluronate, Ceramide 2, Magnesium Ascorbyl Phosphate, Laminaria Digitata Extract, Polyacrylamide, Phenoxyethanol, Chlorphenesin, Dimethicone, Stearic Acid, Tocopheryl Acetate, Cetyl Alcohol, Ethylhexylglycerin, Stearyl Alcohol, Acrylates/C10-30 Alkyl Acrylate Crosspolymer, Sodium Hydroxide, Cholesterol, Disodium EDTA, Limonene, Benzyl Alcohol, C13-14 Isoparaffin, Citric Acid, Glyceryl Linoleate, Isopropyl Myristate, Laureth-7, Palmitic Acid, Potassium Sorbate, Sucrose Palmitate, Mica, Titanium Dioxide
28 w/o emulsion An emulsion in which the dispersed phase is a water and the external (continuous) phase is oil. These emulsion tend to feel more luxurious and heavy. They typically leave a sheen on the skin and can feel greasy. Due to the Oil being the continuous phase, these formulas do NOT have a ph specification.
29 Example Ingredient Listing Pond s Cold Cream: Mineral Oil, Water, Ceresin, Beeswax, Triethanolamine, Behenic Acid, Fragrance, Ceteth 20, Cetyl Alcohol, Carbomer, DMDM Hydantoin, Iodopropynyl Butylcarbamate, Methylparaben
30 w/s & s/w emulsions An emulsion where the dispersed phase is water and the external phase (continuous) is Silicone (w/s) or the opposite for s/w These emulsions are typically made using a Separatory funnel for the transfer and use high shear to adjust viscosity. These emulsions have a wide variety of skin feels. Used for color cosmetics (foundations etc) since many SILICONE POLYMERS lend long wearing properties to the formulas. Also used for Sunless tanners since the water in the internal phase that contains DHA (dihydroxyacetone) is protected from oxidation and degradation.
31 Example Ingredient Listing Smashbox Healthy FX High Definition Foundation SPF % Octinoxate, 3.2%, Titanium Dioxide. Water (Aqua), Cyclopentasiloxane, Isododecane, Butylene Glycol, PEG/PPG-18/18 Dimethicone, Dimethicone, Polysilicone-11, Dimethylacrylamide/Acrylic Acid/Polystyrene Ethyl Methacrylate Copolymer, Coco-Caprylate/Caprate, Hexyl Laurate, Polyglyceryl-4-Isostearate, Dimethicone/Divinyl Dimethicone/Silsesquioxane Crosspolymer, Caprylyl Glycol, Cetyl PEG/PPG-10/1 Dimethicone, Quaternium-18 Hectorite, Lecithin, Magnesium Aluminum Silicate, Phenoxyethanol, Ribose, Sodium Chloride, PEG-10 Dimethicone, Stearic Acid, Propylene Glycol Stearate, Alumina, Propylene Carbonate, Disodium EDTA, Polysorbate 20, Sodium Dehydroacetate, Sorbitan Laurate, Propylene Glycol Laurate, Ascorbyl Palmitate. May Contain: Mica (CI 77019), Titanium Dioxide (CI 77891), Iron Oxides (CI 77491, CI 77492, CI 77499)
32 Emulsion Vocabulary HYDROPHILIC -Water Loving HYDROPHOBIC - Water Fearing LIPOPHILIC - Oil Loving LIPOPHOBIC - Oil Fearing HOMOGENEOUS - Uniform EMOLLIENTS - feel enhancers.
33 Gels and Solutions Gels- semi solid liquids, often clear. (Hair care, skin care, primers) Solutions - a mixture of mutually soluble compounds. Can be water thin to a lotion texture. (Toners, serums, cleansers)
34 Example Ingredient Listing Jack Black Body Building Hair Gel Water (Aqua), PVP, Propylene Glycol, VP/VA Copolymer, Citrus Paradisi (Grapefruit) Fruit Extract, Zingiber Officinale (Ginger) Root Extract, Panthenol, Pyridoxine HCL (Vitamin B6), Triethanolamine, Carbomer, Diazolidinyl Urea, Methylparaben, Polysorbate 20, Polyquaternium-11, Disodium EDTA, Propylparaben, Butylene Glycol.
35 Sticks A solid form cosmetic product. Examples include deodorants, lipsticks, concealer sticks and fragrance sticks. Formulas contain a mixture of high and low melt point waxes to balance the structural integrity of the stick with textural properties that the customer desires.
36 Example Ingredient Listing Make Up Forever - Rouge Artist Intense Ricinus Communis Oil (Ricinus Communis (Castor) Seed Oil), Candelilla Cera (Euphorbia Cerifera (Candelilla) Wax), Hydrogenated Polyisobutene, Methyl Methacrylate Crosspolymer, Diisostearyl Malate, Caprylic/Capric/Succinic Triglyceride, C10-30 Cholesterol/Lanosterol Esters, Cetyl Ricinoleate, Oryza Sativa Cera (Oryza Sativa (Rice) Bran Wax), Nylon-12, Polyglyceryl-3 Polyricinoleate, Parfum (Fragrance), Lauryl Methacrylate/Glycol Dimethacrylate Crosspolymer, Stearalkonium Hectorite, Propylene Carbonate, Stearyl Glycyrrhetinate, Propyl Gallate, Trihydroxypalmitamidohydroxypropyl Myristyl Ether, BHT, [+/- CI (Red 36, Red 36 Lake), CI (Red 6, Red 7, Red 7 Lake), CI (Yellow 6, Yellow 6 Lake), CI (Yellow 5, Yellow 5 Lake), CI (Blue 1 Lake), CI (Orange 5, Orange 5 Lake), CI (Red 21, Red 21 Lake, Red 22 Lake), CI (Red 27 Lake, Red 28 Lake), CI (Yellow 10, Yellow 10 Lake), CI (Red 30, Red 30 Lake), CI (Titanium Dioxide), CI (Aluminum Hydroxide), CI (Iron Oxides), CI (Iron Oxides), CI (Iron Oxides), CI (Manganese Violet)]
37 Anhydrous Any formulation that does not contain water. Examples include: Lip glosses, Lip sticks, cream eye shadows, poured concealers, etc.
38 Sample Ingredient Listing Laura Mercier Lip Glace Hydrogenated Polyisobutene, Lanolin Oil, Polyethylene, Hydrogenated Castor Oil, Calcium Sodium Borosilicate, Aroma (Flavor), Silica, Disteardimonium Hectoriete, Simmondsia, Chinensis (Jojoba) Seed Oil, Calcium Aluminum Borosilicate, Propylene Carbonate, Boron Nitride, Butyrospermum Parkii (Shea Butter), Retinyl Palmitate, Oenothera Biennis (Evening Primrose) Oil, Vitis Vinifera (Grape) Seed Oil, Tocopheryl Acetate, Glycine Soja (Soybean) Oil, Carthamus Tinctorius (Safflower) Seed Oil, Ethylhexyl Palmitate, Aloe Barbadensis Leaf Extract, Tribehenin, Sorbitan Isostearate, Camellia SInensis Leaf Extract, Palmitoyl Oligopeptide. [+/-]: CI (Mica), CI (Titanium Dioxide), Tin Oxide, CI (Iron Oxides), CI (Iron Oxides), CI (Iron Oxides), CI (Red 6), CI (Yellow 5 Lake), CI (Red 7 Lake), CI (Carmine), CI (Red 28 Lake), CI (Yellow 6 Lake), CI (Blue 1 Lake).
39 Powders Any formula where the final product is in powder form, pressed or loose. PRESSED POWDERS: Require a BINDER. Usually liquids, sometimes waxes that help the powder stay pressed into a pan. (EX: Eye shadow, foundation powder etc.) LOOSE POWDERS: Require spherical silicas for slip to help keep the powder from agglomerating or clumping. (Loose eye shadows, loose face powder)
40 Example Ingredient Listing Stila Eye Shadow: Talc, Triethylhexanoin, Zinc Stearate, Lauroyl Lysine, Nylon-12, Magnesium Carbonate, Boron Nitride, Silica, Tocopheryl Acetate, Caprylyl Glycol, Hexylene Glycol, Phenoxyethanol, May Contain (+/-) Mica,Titanium Dioxide (CI 77891), Iron Oxides (CI 77491, CI 77492, CI 77499), Carmine (CI 75470), Ultramarines (CI 77007), Blue 1 Lake (CI 42090), Ferric Ferrocyanide (CI 77510), Manganese Violet (CI 77742), Chromium Oxide Greens (CI 77288), Yellow 5 Lake (CI 19140), Bismuth Oxychloride (CI 77163)
41 Example of Loose Powder Ingredient Listing Laura Mercier Secret Brightening Powder Talc, Silica, Dimethicone/Vinyl Dimethicone Crosspolymer, Dimethicone, Ethylene/Methacrylate Copolymer, Zeolite, Trimethylsiloxysilicate, Sorbic Acid, Methylparaben Phenoxyethanol, Propylparaben Tetrasodium EDTA, Butylparaben, Orchis Maculata Flower Extract, BHT. +/- [May Contain]: MICA (CI 77019), Titanium dioxide (CI 77891), Iron Oxides (CI 77491, CI 77492, CI 77499), Ferric Ferrocyanide (CI 77510), Carmine (CI 75470), Ultramarines (CI 77007), Red 7 Lake (CI 15850), Red 6 (CI 15850), Red 30 (CI 73360), Yellow 5 Lake (CI 19140), Yellow 6 Lake (CI 15985).
42 How a chemist evaluates a product During development, the formulating chemist needs to determine the SPECIFICATIONS for the product. They are a list of physical and chemical parameters of the formula. Once the product is manufactured these specifications will be checked to determine if the product matches what the customer approved (the product Standard)
43 Typical Product Specifications Color, Odor, Appearance TMS = Too Match Standard Viscosity (in-situ, initial, 24hr) ph Bulk Density/ SPG (Specific Gravity) Drop point or Melt point % Actives (for OTC, Sunscreens etc.) Microbiological Specifications
44 Color, Odor, Appearance Color - description of the final color and visual characteristics of the final product along with TMS. Test Method = Visual Odor - description of the odor of the final product. Unfragranced products are typically written as characteristic along with TMS. Test Method = Olfactory Appearance - description of the final product texture and visual appearance. Examples: Powder; semi-solid gel; whipped/aerated cream;; etc along with TMS. Test Method = Visual
45 Why is this important?
46 Viscosity Viscosity is the measurement of a fluids resistance to flow. A thin product will have a low viscosity A thick product will have a high viscosity Viscosity can be taken at several intervals depending on the formulation type. Viscosity is typically measured in centipois (cp)
47 Viscosity is measured with a VISCOMETER
48 Why is this important?
49 ph ph is the measurement of how acidic or alkaline (basic) a product is. Water needs to be present to take a ph measurement. (o/w emulsions and water based products) ph range is 0-14, where 0 is most acidic and 14 is most alkaline. Neutral ph is 7 (example: Water). Anything with a ph below 7 is considered Acidic, anything with a ph above 7 is considered Alkaline or Basic.
50 Chemists take ph readings using a ph METER. The part of the meter that goes into the product is called a CATHODE
51 Most products are formulated to have a ph somewhere in the range of The ph of your skin is roughly 5.4 Exceptions are for Acne products, which are typically more acidic and Cleansers which are typically more basic.
52 Why is this important?
53 Bulk Density and SPG Bulk Density is the measurement of density of powder formulations. It is typically measured in g/cubic inch, although some companies use g/cubic centimeter.
54 Bulk Density is measured using a Sergeant Welch. The product is sifted through the layers to fill the cube.
55 SPG (Specific Gravity) Is the measurement of the density of all liquid, cream and non- powder formulas. SPG is measured in g/cubic centimeter. SPG of water = 1
56 SPG is measured using a Pycnometer
57 Why is this important?
58 Drop Point/ Melt Point Used for non-volatile, solid anhydrous products. Melt Point or Drop Point is the point at which the product changes phase from Solid to Liquid (Melts). Measured in degrees C.
59 Why is this important?
60 % Actives For OTC products, the FDA requires that manufacturers test each batch for the concentration of active ingredients. Sunscreens comprise the majority of OTC cosmetic products on the market. The acceptable range is -10% to +20% of the formula amount
61 Examples of Sunscreens Physical Sunscreens: Zinc Oxide (ZnO) Titanium Dioxide (TiO2) Chemical Sunscreens: Avobenzone Oxybenzone Octisalate Octinoxate Octylcrylene Homosalate
62 % Actives is determined by Gas Chromatography and NMR (Nuclear Magnetic Resonance)
63 Why is this important?
64 Microbiology Every batch of product manufactured needs to be tested to make sure it is free of contaminates and can adequately kill of any bacteria that is introduced. a PLATE COUNT is performed to see if any yeast, mold or bacteria is present in the product. a STANDARD CHALLENGE is performed to make sure that the preservatives in the formula are working and can kill of any yeast, mold or bacteria that is introduced into the product.
65 Microbiologists use PETRI DISHES to test the product.
66 Why is this important?
67 MID TERM STUDY TIPS The Mid Term will cover material from the first 2 Lectures AND the Reading - CHAPTERS 1, 2, 13, 24 & 25 Pay Attention to all the vocabulary in the book and in the lecture notes. Chapter 1: Everything EXCLUDING, Table 1.1 and the section on Ingredients suppliers Chapter 2: The vocabulary!! Chapter 13, 24 and 25 - All.
68 Extra Credit Bring in your study notes (not in a notebook), flash cards, etc. for an extra 5 points on the exam!!
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