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Combination Colors – Optical
Properties and Regulatory
Update
PCPC Science Symposium
October 3, 2012
2 BASF Personal Care
Outline
1 | History leading to current FDA
dialogue on Combination Pigments
2 | Optical and Physical Properties of
Combination (Effect) Pigments
3 | Next Steps and Summary
BASF Personal Care 2
3
21 CFR listing of “Mica-Based
Pearlescent Pigments”
A petition was filed and approved by FDA for the use of some combination
pigments in direct food and pharma applications
2005-’06: In the 21 CFR Part 73 listing of Mica-Based Pearlescent
Pigments for use in food and drugs, FDA:
Treated pearlescent pigments as a composite, not a mixture of color
additives and other ingredients
Established approval for this composite for food & drugs, but not
cosmetics
4
February 5, 2007 “untitled” letter by FDA
Alleges that effect pigments are adulterated in that they are unapproved
color additives for cosmetics
Contends that FDA approved similar composite pigments made from iron
oxide, titanium dioxide and mica as separate color additives for food and
drugs (but not cosmetics)
Based on Agency experience, manufacture of these pigments whereby
the color is formed in situ on a substrate results in other chemical
residues that must be assessed.
5
Industry dialogue with FDA (2007 - 2009)
BASF/Merck comments to FDA in 2007 meeting:
Effect pigments have been used safely in cosmetics for over 40 years in hundreds
of thousands of products.
Manufacturers and industry have long considered these products to be mixtures of
approved color additives (and no regulatory authority treats them otherwise).
International labeling nomenclature is based on this mixture principle.
BASF/Merck to provide a study plan to FDA that would demonstrate effect pigments
as mixtures
BASF/Merck submitted effect pigment study plan to FDA in February 2008
The “mixture” nature of effect pigments was demonstrated, but not accepted by
FDA
6
An effect pigment working group (EPWG), composed of major
effect pigment manufacturers working in conjunction with the
PCPC, was formed to discuss with FDA:
The variety and composition of effect pigments in the cosmetic marketplace
(categorization)
Manufacturing/safety information
Possible framework for proposed regulation changes
A consensus was reached that the term “combination pigments” best described
effect pigments
Dialogue with FDA (2010 - today)
7
More Recent Events (2011)
After some import detentions of cosmetic products containing effect pigments in mid-
2011, the PCPC and EPWG put together a proposed “straw” regulation and requested a
meeting with FDA. The straw regulation proposed two basic groupings of combination
pigments:
Combination pigments are formed by binding one or more safe and suitable cosmetic color
additives with…
i. a safe and suitable cosmetic color additive that serves as a base, with or without one or
more safe and suitable coloring adjuncts, or
ii. a safe and suitable cosmetic ingredient that serves as a base, with or without one or more
safe and suitable coloring adjuncts.
Note: safe and suitable is defined as color additives listed in Part 73,74, and 82
Dialogue with FDA (2010 - today)
8
Recent EPWG/PCPC/FDA Activities
PCPC March 2012 letter submitted to FDA:
Provided written responses to the October 2011 questions FDA emailed to PCPC
Proposed three 90-minute technical meetings with the agency to allow the
EPWG/PCPC an opportunity to better describe the identity and manufacture of
combination pigments
FDA answered favorably, and 3 meetings were scheduled for
April-June
9
April 13, 2012 EPWG/PCPC/FDA Meeting
The intent of the first meeting was to educate FDA on the optical and
physical properties of combination pigments
Presented by EPWG/PCPC: “Combination Pigment Optics” (with a glossary of
terms provided to FDA)
Important topics presented
Combinations of bases, color additives, and coloring adjuncts produce a wide variety of
coloring effects
Bases provide structure but not necessarily color
Mixture best describes the relationship between a base, coloring adjunct, and the color
additive coating
Bases and coloring adjuncts serve to modify the shape, structure and shading of
combination pigments while different particle sizes produce different effects. Thus one
cosmetic color additive, with or without coloring adjuncts, can generate many colors and
effects when combined with a base
10
Concepts Presented
Existing color additives develop color by physics
Combinations of bases, adjuncts, and a limited number of color
additives produce a wide variety of coloring effects
Bases provide structure but not necessarily color
“Mixture” best describes the physicochemical relationship between a
base and a coating.
11
Combination Pigments
Color additives with structure
Color additives in a platy form
Thin layers on a base
Interacting with light in different ways
Infinite colors with varying color travel
Many sizes and shapes
12
Points for Discussion
Definitions
Optics
Absorption
Reflection
Interference
Diffraction
Some examples of combination pigments
13
Diffuse Reflection off rough surfaces Non-directional
Reflection Types
I = Illumination
Specular Reflection off a smooth surface
Incident = Reflection
(Directional Mirror
Reflection)
S I
I
Aspecular Reflection
(Directional)
S A I
D
14
Refractive Index
Light reflects from interfaces
according to:
%R=100 x (n1-n2)2/(n1+n2)
2
Refractive index, (n), of materials
Air 1.0
Water 1.33
Mineral Oil 1.5
SiO2 1.4
Borosilicate 1.52
Mica 1.58
Al2O3 1.73
TiO2 (Rutile, Anatase) 2.5
Fe2O3 2.9
Cr2O3 2.55
BiOCl 2.15
Bases
Media
Materials in media of similar refractive indices have no
interface and therefore disappear.
A dimensionless number that describes how light, or any other radiation,
propagates through a medium. Relates speed of light in medium to that in a
vacuum.
High RI
Materials
Mica in air
Mica in oil
15
Simple Reflection of Light
Light interacting with a smooth reflective surface
Typically a metallic cosmetic color additive like Al on a base
Total specular, mirror-like, reflection
Sizes from 6-70 microns, but thin
Bases do not impart color
Bases
Borosilicate
Mica
PET
Color Additive
Al
Ag
Reflecting Category II Combination Pigments
16
Interference Color is Defined by Thickness of
the Metal Oxide Layer ( e.g. TiO2) on the Base
40-60 nm 60-80 nm 80-100 nm 100-140 nm 120-160 nm
17
Interference Pigment A simple Category II Combination Pigment structure
Mica 50-200 nm thick TiO2
50-200 nm thick TiO2
300 nm thick mica
Typical Bases
Muscovite Mica
Fluorphlogopite
Borosilicate
Al2O3
SiO2
Cosmetic color additives layered onto a base...an example
2 microns
The base and color
additive retain
their distinct layer
structure
18
Examples of Some Common
Category II Bases
BiOCl
Borosilicate Based
Alumina Based
Mica Based
Natural
Mica
Silica Alumina Borosilicate Synthetic
Mica
19
Category II Combination Pigments
TiO2 layered onto various bases
BiOCl
Borosilicate Based
Alumina Based
Mica Based
Silica Based
20
Iron oxide coated Al Powder Category I Combination pigment
Cornflake type is less
reflective than silver
dollar type
The iron oxide
layer remains a
distinct component
on the Al particle
TEM cross-section
Iron Oxide
Al
21
Low refractive index adjunct sandwiched between high refractive index color additives
Examples
Fe2O3/SiO2/Al/SiO2/Fe2O3 Cat. I
TiO2/SiO2/TiO2 Cat. II
Color range determined by refractive index of
materials and thickness of layers
Color Variable Pigment, (CVP)
Color Shifting Combination Pigments
t = 200-400 nm
I
I
Color variable or optically
variable pigments have a high
degree of color change with
changing illumination and
viewing angles due to structure
and materials
22
Multilayer Combination Pigments
Two cosmetic color additives on one base resulting in a
mixture of colors and effects
Carmine layered onto a green combination pigment (TiO2
on mica) (Category II)
Mica acts as the base
Red absorption color with green interference reflection
color
High transparency
Many combinations are possible
23
Spatial Reflections The impact of size
Large Sizes
Large particles, (>35 microns), appear as
glints or sparkles
Pigment color blends seen as discrete pinpoints of confetti-like color
Small Sizes
More edges produce more scattering of light
Color blends seen as sum of colors
Blue + Gold = Silver (White)
Green + Red = Silver (White) Less sparkle, more uniform color
24
Conclusions
Physics Describes Optical Behavior
Interference, reflection, absorption, diffraction create different effects
Bases and adjuncts serve to modify the shape and structure of the
combination pigments
Different sizes generate additional effects
One cosmetic color additive can generate multiple colors and effects
when combined with a base and/or adjunct, i.e. TiO2 on a base
Infinite interference colors
Simple interference or color variable effects
Varying size effects
25
April 30, 2012 EPWG/PCPC/FDA Meeting
The intent of the second meeting was to describe the various
manufacturing processes used to product combination pigments,
as well as the role of adjuncts.
Presented by EPWG/PCPC: “Combination Pigment Manufacturing Processes”
and “Role of Adjuncts”
Some of the topics presented:
Four general types of manufacturing processes are used to produce combination pigments
Combination pigments are prepared by layering the various components to create the
desired optical properties. They may be as simple as 2 layers (color additive on a base) or
several layers with adjuncts
The layers of a combination pigment are not bonded together by covalent bonding, but are
better characterized as attraction of physisorption
Tin oxide is a common coloring adjunct, used primarily as a color enhancer and stabilizer
26
Types of Manufacturing Processes
Aqueous deposition of layers
Calcined
Non-calcined
Gas Phase deposition of layers
Physical Vapor Deposition (PVD)
Chemical Vapor Deposition
27
June 5, 2012 EPWG/PCPC/FDA Meeting
The intent of the third meeting was to cover current combination
pigment specifications and control points.
Presented by EPWG/PCPC: “Current Industry Specifications for Combination
Pigments” and “Analytics of Combination Pigments”
Some of the topics presented:
Combination pigment manufacturers, through the use of the qualified raw materials of
appropriate composition, manufacture safe and suitable cosmetic ingredients.
QA/QC requirements are established to ensure combination pigments meet the applicable
21 CFR requirements for the color additives used (i.e. heavy metal purity)
A variety of physical, optical, and elemental analytical instrumentation are used by
combination pigment manufacturers in the analysis and characterization of these pigments
28
Analytical Methods for Combination Pigments
-Particle size distribution Laser beam diffraction
-Particle size and shape Scanning Electron Microscope
-Particle size and shape Transmission Electron
Microscopy
-Color Multi-angle color measurement
-Crystallographic phases Powder X-ray diffraction
-Chemical composition X-ray fluorescence
-Element analysis (heavy metal) ICP-OES, GF-AAS, HR-ICP-MS
-Density Pycnometer method
-Loss of drying ASTM D 280
-Microbiologics Microbiological examination
29
Next Planned Meeting with FDA
Discussion of EPWG/PCPC’s proposed regulation for “combination pigments” (originally submitted to FDA on September 2011)
Combination pigments are formed by binding one or more safe and suitable cosmetic color additives with:
A safe and suitable cosmetic color additive that serves as a base, with or without one or more safe and suitable coloring adjuncts, or
A safe and suitable cosmetic ingredient that serves as a base, with or without more or more safe and suitable coloring adjuncts
Safe and suitable cosmetic color additives - A color additive that is listed in parts 73,74, or 82 for use in cosmetics, is either exempt from certification or is from a batch that has previously been certified.
A color additive must conform to applicable specifications in parts 73, 74, and 82.
30
Next Planned Meeting with FDA (cont.)
Discussion of EPWG/PCPC’s proposed regulation for “combination pigments”
Safe and suitable cosmetic ingredients provide safe and suitable functional components to facilitate use of the combination pigments to color the human body.
Safe and suitable cosmetic coloring adjuncts are substances used to preserve or enhance the color or shading of combination pigments.
Examples include, but are not limited to, color stabilizers, fixatives, retention agents, and synergists
Labeling: Each ingredient comprising the combination pigment shall be declared on the label of the finished cosmetic product.
Solicit FDA acceptance of proposed regulation and define path forward
31
Summary
Three technical meetings were held with FDA during the first half of 2012.
The meetings covered three aspects of combination pigments:
1. physical and optical properties
2. manufacturing processes and role of adjuncts
3. analytical methods and specifications
The information presented supports the position that combination pigments
should continue to be considered mixtures.
32 BASF Personal Care
DISCLAIMER
This document, or any answers or information provided herein by BASF, does not constitute a legally binding
obligation of BASF. While the descriptions, designs, data and information contained herein are presented in good
faith and believed to be accurate, they are provided for your guidance only. Because many factors may affect
processing or application/use, we recommend that you make tests to determine the suitability of a product for your
particular purpose prior to use. It does not relieve our customers of the obligation to perform a full inspection of the
products upon delivery or any other obligation. The claims and supporting data provided in this publication have not
been evaluated for compliance with any jurisdiction’s regulatory requirements and the results reported may not be
generally true under other conditions or in other matrices. Users must evaluate what claims and information are
appropriate and comply with a jurisdiction’s regulatory requirements. NO WARRANTIES OF ANY KIND, EITHER
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