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S U M M A R Y :

T H I S D O C U M E N T D E S C R I B E S A N E W S U B S T R A T E F O R S P E C T R O P H O T O M E T R I C M E A S U R E M E N T O F S U N P R O T E C T I O N I N D E X E S . I T P R E S E N T S T H E S T A T E O F T H E A R T , T H E E X P L A N A T I O N O F A N E W M A N U F A C T U R I N G P R O C E S S , A S W E L L A S T H E M A I N C H A R A C T E R I S T I C S O F H E L I O P L A T E ™ H D , I N F O R M A T I O N A B O U T T H E I R P R O D U C T I O N A N D T H E I R Q U A L I T Y C O N T R O L .

The substrate in in vitro evaluation methods of sun products protection indexes

Since B Diffey and Robson’s recommendation, published in 1989(1), to use a new substrate, the TRANSPORE TM, the method based on the evaluation of the absorption of a spread on a substrate product layer became the starting point of most in vitro evaluation methods. Different substrates have been proposed with variable success, such as manually frosted quartz or the VITROSKIN, based on proteïnic substances. HELIOSCIENCE laboratories (HelioScreen Labs) have made available for the first time in 2000, a PMMA substrate “HELIOPLATE™ ” the roughness of which was from 5 to 10 microns. Today, PMMA as a substrate is almost universally accepted. A different quality has been introduced by DGK (2) when was published a new UVA protection evaluation method according to the DIN standard. Unlike with HELIOPLATE™ proposed by HelioScience laboratory, roughness is much lower, about 2 microns instead of 6. It has been selected as a measuring substrate in the COLIPA’s method as published in 2007, for the evaluation of the UVA protection (3).

1- A new substrate to measure sunscreen protection factors throughought the ultraviolet

spectrum J cosmet.chem-40.[1989] 127-133

2- Characterization of UVA protection of dermal suncare products by measuring the

tranmittance with regard to the sun protection factor DIN 67502 Janv 2004

3- Method for the in vitro determination of UVA protection provided by sunscreen products Edition of 2007a

Page 1

Page 2

Present Quality Control

Characteristics of the substrate “PMMA plates” The present checking of existing plates is limited to one roughness parameter (Sa) and evaluation of absorption properties as for example recommended in UVA COLIPA’s method: The mean optical transmission through the glycerine covered substrate should be (N=20):

Wavelength (nm) Minimum transmission (%)

Maximum transmission (%)

290 60 70

300 69 79

320 81 91

Micro topography measurements can be achieved to characterize the plate surface roughness. Contact or non-contact systems are available to accurately provide a surface roughness value (e.g., Sa in µm, according to EUR 15178 EN). The roughness value of the PMMA plates used for the validation of the COLIPA’s method.

Plates manufacture by sandblasting

The manufacturing principle of the « former plates » is to start from a large PMMA plate containing no UV filters. It is sandblasted according to an industrial method and then cut into 5cmx5cm plates which are right away used for in vitro measurement.

[from Colipa‘s method (3)]

Page 3 HELIOPLATE™HD : a new approach

HelioScreen labs Laboratories, already forerunners with PMMA plates proposal in 2000 (HELIOPLATE™ ), have developed, with the help of 2 partners, a new manufacturing process to offer a specifically adapted substrate, with very precise specification: > Manufacturing process by injection for an assured reproducibility. > Availability of two grades to respond to market’s need. > Setting up of a development plan, of molds design, of definition of prints topography, careful manufacture and stringent quality. > Stringent definition and validation of topographic data. > Validation of correlation of values obtained with existing plates. > Setting up of a precise control card, not solely limited to the Sa roughness parameters. The 3 first steps have been taken care of through a high level technical cooperation with LFP (1), which led molds design and is also in charge of manufacture and production follow up. The 3 last steps have been taken care of through contract cooperation with COTY Lancaster (b) which proved in a recent publication (1) its perfect control for checking topographical parameters. and is in charge of supervising production quality. (a) LFP La française des plastiques BP4 route de Vitré F35680 LOUVIGNE DE BAIS (b) Coty Lancaster 98000 Monaco

1-Importance of Substrate Roughness for In Vitro Sun Protection Assessment. L. Ferrero, M Pissavini. IFSCC Vol9 n°2 avril/juin 200 6

Page 4

Design and Manufacture

Production follow up and Quality Control

The PMMA polymer is checked according to the specifications below. The step of production by injection press strictly defined with validated parameters stick with a global quality process. Next step is a stringent checking of the plates.

HELIOPLATE™ HD manufacture by injection is done in rigorously checked conditions in accordance with the quality certification standards.

- GENERAL PROPERTIES Density ISO 1183 g/cm3 1,18 Water Absorption 23°C/50%HR ISO 62 % :0,3 Mould Shrinkage long. mm ASTM D-955 % :0,2-0,6 transv. mm :0,2-0,6 2 - RHEOLOGICAL PROPERTIES Rheology Melt Flow Index 230°C/3,8 kg ISO 1133 g/10 min :24 Process Melt Temperature mini °C :195 maxi 200 Mold Temperature mini °C :50 maxi 60 Drying Conditions time h 70 temperature °C 2-4 3 - MECHANICAL PROPERTIES Rockwell Hardness ASTM D-785 M-84 Tensile Strength 23°C ISO 527-1 Mpa :66 Elongation at break 23°C ISO 527-1 % :5 Flexural Modulus 23°C ISO 178 GPa :2,9 Flexural Strength 23°C ISO 178 Mpa :97 Compressive Strength 23°C ISO 604 Mpa :100 Impact Resistance (Charpy, Notched) 23°C ISO 179 1eU kJ/m² :2 Impact Resistance (Charpy, Unnotched) 23°C ISO 179 1eU kJ/m² :11 Impact Resistane (Izod, Notched) 23°C ISO 180/1a kJ /m² :1,8 4 - OPTICAL PROPERTIES Refractive Index B R-489 :1,49 Light Transmittance ASTM D-1003 % :92 Haze ASTM D-1003 % :0,5 5 - ELECTRICAL PROPERTIES Dielectric Strength ASTM D-149 MV/m :19,7 Dielectric Constant 60 Hz ASTM D-150 :3,7

P M M A T E C H N I C A L C H A R AC T E R I S T I C S

Page 5 CONTROL CARD

2D parameters can be respectively calculated from the untreated profile (P), or after filtration, from the roughness profile (R) or from the wave profile (W). Sometimes, the following list presents parameters with the X prefix which is to be replaced by P, R or W according to the needs. For each parameter, the kind of filter and of cut-off to be used is defined. Therefore, it’s possible to request several cases of a same parameter with different adjustments.

Standard ISO 4287 defines some parameters from a base length and some others on the evaluation length. Parameters estimated from a base length are then « averaged » from the collection of base lengths as shown in standard ISO 4288.

Ra Roughness Average (arithmetical average of devia tions from average): The result is expressed in unit length of Z axis.

Rp Largest peak height (of profile peaks within a b ase length):

The result is expressed in unit length of Z axis.

Rv Deepest pit (of profile pits, within a base leng th): The result is expressed in unit length of Z axis. Rsk Skewness factor : Moment of order 3 calculated within a base length. The result is without unit. When the Xsk is negative, it means that distribution is shifted upwards. When the Xsk is positive, distribution is shifted downwards. When the Xsk is close to 0, Distribution is symmetrical.

Rku: Kurtosis factor Moment of order 4 calculated within a base length. The result is without unit. Rdq Root Mean Square Gradient (of profile, within a base length) :

Current Parameters of ISO standards (profile)

A1 (Equivalent Triangle Area for peaks ) : Volume of running in scraps. A1 defines the volume of peaks likely to disappear during engine running in. A2 (Equivalent Triangle Area for pits ) : Volume of oil reserve. A2 defines the oil volume that surface can store for lubrication during running.

Parameters Rk (ISO 13565) (profile)

GRAPHICAL STUDY OF VOLUME PARAMETERS (SURFACE)

Class of state surface parameters defining one criteria which at the same time, depends on amplitude and space, such as slopes, curvatures, etc.

Ssc (Mean Summit Curvature): This parameter allows to know the average shape of summits, either sharp or rounded, from the average value of surface curvature at these locations.

This study is based on Abbott’s curve, calculated on the surface. Two thresholds are defined by their bearing rate (shown as vertical dotted lines). By default, these thresholds are defined at 10% and 80% of bearing rate.

The first threshold, p1 (by default, 10%) allows to define a section level c1 (and respectively, p2 defines c2).

Then, the following parameters are calculated:

Vmp : Volume of material of peaks, calculated in the above c1 portion.

Vmc : Volume of material of core, calculated in the portion located between c1 and c2.

Vvc : Volume of empty core, calculated in the portion located between c1 and c2.

Vvv : Volume of empty pits, calculated in the beneath c2 portion .

Standards References

ISO 3274:1997

Surface state : profile method, nominal characteristics of contact devices .

ISO 4287:1997

Surface state : profile method, wording, definitions and surface state parameters .

ISO 4288:1996

Surface state : profile method, rules and procedures for surface state evaluation.

ISO 11562:1997

Metrological definition of right phase filters and of transmission bands to be used with contact profilometers.

Surface hybrid parameters

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Page 7

HELIOPLATE™ HD supply

These plates are delivered as tight heat sealed pac ks of 50 units. Their shape allows piling so as to avoid impairing their surface condi tion during transport or storage. Each delivery comes along with a certificate which allows iden tification and traceability, and is the assurance of our quality control. For HELIOPLATE™ HD, two roughness levels as well as a standard are available: HELIOPLATE™ HD 2 (50mmX50mm) about 2 microns roughness. This grade is mainly for carrying out the UVA COLIPA’s method (2007 version) . HELIOPLATE™ HD 6 (50mmX50mm) about 6 microns roughness. This grade is advisable for any other use and particularly for SPF and photo stability measurement. HELIOPLATE™ HD 00 (50mmX50mm) with UV filters, delivered with reference spectrum, allows checking the equipment before measurements.

Plates Availability

Ordering Process

Our Quality Assurance system imposes a stringent procedure for the receipt and order processing : > Ask by fax (+33 344 289 706) or e-mail <helioscience.account@free.fr>

> Our order form « HePmma 001 ».

> At reception (EXCEL format) fill up the lines regarding your company.

> Complete the index « order » by writing the grade and quantity of plates.

> Send it back by e-mail at < helioscience.account@free.fr

> You’ll get an acknowledgement of your order with a predictable delivery date within 24H.

> You’ll get the plates and the certificate within planned lead time (usually about 8/10 days).

To receive HELIOPLATE™ HD

Page 8 Batch Quality Certificate

Raw Material Control

ALTUGLAS VS UVT PMMA used has been checked as conform to technical data sheet ATOGLAS, at date _______________

Manufacture Control

The industrial production of this batch has been checked as conform to the requirements of the control range, at date________________

Control of plates roughness parameters (control equipment: Altisurf 500M (software: Mountain®))

Review of the summarizing data sheet done on the sampling according to protocol CL/HS 001 Rev 1, at date ________________

Date Ra Rp Rv Rdq Rsk Rku A1 A2 Ssc Vvv Global

31/01/2008 OK OK OK OK OK OK OK OK OK O K

Conclusions for roughness parameters

The analysis of roughness parameters and of protection indexes of our laboratory standard gives satisfactory results. Referring to the « control card », the samples of HD 2 plates received fulfil all specification criteria.

From this, we give our official agreement to this p roduction of PMMA HD 2 plates.

GENERAL CONCLUSION

Therefore, the above referenced product is conform to the standard and is guaranteed by our laboratories, Under responsibility of HelioScreen Labs.,

HelioScreen labs, Maître d’oeuvre

Grade : HELIOPLATE™ HD2

Reference : HD2 95HS625

Manufacture started on : 12/02/08 Batch N° : 4521 Mold N° : 769 Manufacture completed on : 12/02/08

Page 9

How to use HELIOPLATE™ HD

Choice of the roughness

Application

Two roughnesses are proposed for HELIOPLATE™ HD. It is worthwhile to precise from our point of view, the high roughness seems quite better to ensure a good spreading in most of the cases… Nevertheless the COLIPA proposed a method for the UVA determination in 2006/2007 with the use of plates with a roughness of 2 microns. That is the only purpose of the 2 microns roughness quality HELIOPLATE™ HD2 to keep within the adopted protocol. Any other in vitro test based on the spreading of a product on a rough plate (such as SPF, Photo stability, Boots rate system etc…) must be done on the 6 microns grade (1). Quantity applied will depend on the roughness. It is advisable to apply: Around 0.75 mg/cm² for HELIOPLATE™ HD2 Around 1.30 mg/cm² for HELIOPLATE™ HD6

Product is applied to the substrate by weight. Application rate is determined in such a way that the actual quantity of product left on the substrate before spreading is 0.75 mg/cm² for HELIOPLATE™ HD2 and around 1.3 mg/cm² for HELIOPLATE™ HD6. To ensure the correct application rate, the syringe has to be weighed before and after product application. The amount of sunscreen product in the form of a large number of small drops of equal volume is applied by pipette and distributed evenly over the whole roughened PMMA surface of the plate (50 x 50 mm).

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Page 10

Spreading

Immediately after weighing, the sunscreen product is spread over the whole surface with a finger-cot “pre-saturated” with the product using light strokes. Spreading had to be completed as quickly as possible (less than 30 seconds). Then the sample was rubbed into the rough surface using stronger pressure. This also had to take 20 to 30 seconds. The sample thus obtained was allowed to settle for 15 minutes in the dark at room temperature to ensure self-levelling of the formula.

T = 0 s t = 20 s

1 2 3 4

Measuring

A total of four to nine UV transmission spectra (from 290 to 400 nm in 1 nm increment steps) is recorded on each plate at different locations. At least three different plates have to be used for each roughness class to give an average of the UV transmission data at each wavelength. It is unadvised to clean the plate for any further re use (1) Pissavini, M., Lutz, D. and al, Determination of the in vitroSPF, Cosm. & Toil., 118 (2003) 63-71.

How to use HELIOPLATE™ HD