Determination of sunscreen UVA photoprotection in vitro (ISO 24443:2012)

This test method provides an in vitro procedure to characterize the UVA protection of sunscreen products. Specifications are given to enable determination of the spectral absorbance characteristics of UVA protection in a reproducible manner. In order to determine relevant UVA protection parameters the method has been created to provide a UV spectral absorbance curve from which a number of calculations and evaluations can be undertaken. Results of this measurement procedure can be used for other computations as necessary for local regulatory authorities. These include calculation of Ultraviolet-A Protection Factor (UVA-PF) (correlating with in vivo UVA-PF from Persistent Pigment Darkening testing procedure), Critical Wavelength, and UVA/UVB absorbance proportionality. These computations are optional and relate to local sunscreen product labelling requirements.

In vitro Bestimmung des UVA-Schutzes von Sonnenschutzmitteln (ISO 24443:2012)

Diese Internationale Norm stellt ein in vitro Verfahren zur Charakterisierung des UVA-Schutzes von Sonnenschutzmitteln dar. Es werden Spezifikationen angegeben, für eine reproduzierbare Bestimmung der spektralen Extinktion als Charakterisierung des UVA-Schutzes.
Zur Bestimmung der relevanten Kenngrößen für den UVA-Schutz wird die Kurve der spektralen Extinktion im UV ermittelt, auf deren Grundlage eine Reihe von Berechnungen und Bewertungen vorgenommen werden können. Ergebnisse dieses Messverfahrens können für weitere Berechnungen, wie zum Beispiel für örtliche Aufsichtsbehörden, verwendet werden. Dies beinhaltet die Berechnung des UVA-Schutzfaktors (UVAPF) [korreliert mit dem in vivo UVA-Schutzfaktor aus dem Persistent Pigment Darkening-Prüfverfahren (PPD)], der kritischen Wellenlänge und des UVA-/UVB-Extinktionsverhältnisses. Diese Berechnungen sind optional und beziehen sich auf die örtlichen Anforderungen zur Kennzeichnung von Sonnenschutzmitteln. Diese Methode basiert auf der Verwendung der in vivo SPF-Ergebnisse für die Skalierung der UV-Extinktionskurve.
Diese Internationale Norm gilt nicht für pulverförmige Produkte, die zum Beispiel gepresst oder lose vorliegen.

Détermination in vitro de la photoprotection UVA (ISO 24443:2012)

L'ISO 24443:2012 d'essai spécifie un mode opératoire in vitro pour caractériser la protection UVA apportée par des produits de protection solaire. Des spécifications sont données pour permettre de déterminer les caractéristiques d'absorbance spectrale de la protection UVA de façon reproductible.
Afin de déterminer les paramètres de protection UVA pertinents, la méthode a été mise au point pour fournir une courbe d'absorbance spectrale UV à partir de laquelle des calculs et des évaluations peuvent être effectués. Cette méthode repose sur les résultats du FPS in vivo pour élaborer la courbe d'absorbance des UV.

Kozmetika - Določevanje zaščitnega faktorja UVA in vitro (ISO 24443:2012)

Ta preizkusna metoda zagotavlja postopek in vitro za zaščito pred žarki UVA varovalnih sredstev za zaščito kože pred soncem. Podane specifikacije omogočajo določitev lastnosti spektralne absorpcije zaščite pred žarki UVA na ponovljiv način. Za določitev ustreznih parametrov zaščite pred žarki UVA je bila ustvarjena metoda za zagotovitev krivulje spektralne absorpcije UV, iz katere je mogoče izpeljati številne izračune in ocene. Rezultati tega postopka merjenja se lahko po potrebi uporabijo za druge izračune za lokalne regulativne organe. Ti vključujejo izračun ultravijoličnega A zaščitnega faktorja (UVA-PF) (ki se navezuje na UVA-PF in vivo iz preizkusnega postopka obstojne pigmentacije), kritične valovne dolžine in razmerja absorpcije žarkov UVA/UVB. Ti izračuni so izbirni in se nanašajo na zahteve glede označevanja izdelkov za zaščito kože pred soncem.

General Information

Status
Published
Public Enquiry End Date
09-Nov-2010
Publication Date
08-Oct-2012
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
13-Sep-2012
Due Date
18-Nov-2012
Completion Date
09-Oct-2012

RELATIONS

Buy Standard

Standard
SIST EN ISO 24443:2012 - PAZI: k standardu spada tudi "ISO 24443;2012(E)-Electronic_inserts"
English language
34 pages
sale 10% off
Preview
sale 10% off
Preview
e-Library read for
1 day

Standards Content (sample)

SLOVENSKI STANDARD
SIST EN ISO 24443:2012
01-december-2012
.R]PHWLND'RORþHYDQMH]DãþLWQHJDIDNWRUMD89$LQYLWUR ,62
Determination of sunscreen UVA photoprotection in vitro (ISO 24443:2012)
In vitro Bestimmung des UVA-Schutzes von Sonnenschutzmitteln (ISO 24443:2012)
Détermination in vitro de la photoprotection UVA (ISO 24443:2012)
Ta slovenski standard je istoveten z: EN ISO 24443:2012
ICS:
71.100.70 .R]PHWLND7RDOHWQL Cosmetics. Toiletries
SULSRPRþNL
SIST EN ISO 24443:2012 en,fr,de

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

---------------------- Page: 1 ----------------------
SIST EN ISO 24443:2012
---------------------- Page: 2 ----------------------
SIST EN ISO 24443:2012
EUROPEAN STANDARD
EN ISO 24443
NORME EUROPÉENNE
EUROPÄISCHE NORM
June 2012
ICS 71.100.70
English Version
Determination of sunscreen UVA photoprotection in vitro (ISO
24443:2012)

Détermination in vitro de la photoprotection UVA (ISO In vitro Bestimmung des UVA-Schutzes von

24443:2012) Sonnenschutzmitteln (ISO 24443:2012)
This European Standard was approved by CEN on 24 May 2012.

CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European

Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national

standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member.

This European Standard exists in three official versions (English, French, German). A version in any other language made by translation

under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management Centre has the same

status as the official versions.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,

Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland,

Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom.

EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: Avenue Marnix 17, B-1000 Brussels

© 2012 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 24443:2012: E

worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
SIST EN ISO 24443:2012
EN ISO 24443:2012 (E)
Contents Page

Foreword ..............................................................................................................................................................3

---------------------- Page: 4 ----------------------
SIST EN ISO 24443:2012
EN ISO 24443:2012 (E)
Foreword

This document (EN ISO 24443:2012) has been prepared by Technical Committee ISO/TC 217 "Cosmetics" in

collaboration with Technical Committee CEN/TC 392 “Cosmetics” the secretariat of which is held by AFNOR.

This European Standard shall be given the status of a national standard, either by publication of an identical

text or by endorsement, at the latest by December 2012, and conflicting national standards shall be withdrawn

at the latest by December 2012.

Attention is drawn to the possibility that some of the elements of this document may be the subject of patent

rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights.

According to the CEN/CENELEC Internal Regulations, the national standards organisations of the following

countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech

Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia,

Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain,

Sweden, Switzerland, Turkey and the United Kingdom.
Endorsement notice

The text of ISO 24443:2012 has been approved by CEN as a EN ISO 24443:2012 without any modification.

---------------------- Page: 5 ----------------------
SIST EN ISO 24443:2012
---------------------- Page: 6 ----------------------
SIST EN ISO 24443:2012
INTERNATIONAL ISO
STANDARD 24443
First edition
2012-06-01
Determination of sunscreen UVA
photoprotection in vitro
Détermination in vitro de la photoprotection UVA
Reference number
ISO 24443:2012(E)
ISO 2012
---------------------- Page: 7 ----------------------
SIST EN ISO 24443:2012
ISO 24443:2012(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2012

All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means,

electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the address below or ISO’s

member body in the country of the requester.
ISO copyright office
Case postale 56 • CH-1211 Geneva 20
Tel. + 41 22 749 01 11
Fax + 41 22 749 09 47
E-mail copyright@iso.org
Web www.iso.org
Published in Switzerland
ii © ISO 2012 – All rights reserved
---------------------- Page: 8 ----------------------
SIST EN ISO 24443:2012
ISO 24443:2012(E)
Contents Page

Foreword ............................................................................................................................................................................iv

1 Scope ...................................................................................................................................................................... 1

2 Terms and definitions ......................................................................................................................................... 1

3 Principle ................................................................................................................................................................. 2

4 Apparatus .............................................................................................................................................................. 2

4.1 UV spectrophotometer specifications ........................................................................................................... 2

4.2 Calibration of the UV spectrophotometer ..................................................................................................... 3

4.3 Calibration of the UV exposure source ........................................................................................................ 3

4.4 Monitoring of the UV exposure source ......................................................................................................... 3

4.5 Calibration of the UVA radiometer used to monitor the test sample irradiation ................................ 4

4.6 Substrate/plate ..................................................................................................................................................... 4

5 Test method .......................................................................................................................................................... 4

5.1 Outline of the test procedure ........................................................................................................................... 4

5.2 Equipment calibration and validation of test plates .................................................................................. 4

5.3 Absorption measurements through the plate ............................................................................................. 5

5.4 Sample application ............................................................................................................................................. 5

5.5 Absorbance measurements of the product-treated plate ........................................................................ 5

5.6 Number of determinations ................................................................................................................................ 5

5.7 Determination of initial calculated SPF (SPF ), “C” value, initial UVAPF(UVAPF ), and UV

in vitro 0

exposure dose ...................................................................................................................................................... 5

5.8 UV exposure ......................................................................................................................................................... 7

5.9 Measurement of final adjusted absorbance spectrum .............................................................................. 7

5.10 Calculation of UVAPF of plates after UV exposure of the sample ......................................................... 8

6 Procedure using the spreadsheet in this International Standard .......................................................... 8

7 Reference sunscreen formula S2 .................................................................................................................... 9

8 Test report ............................................................................................................................................................. 9

Annex A (normative) Calibration of UV spectrophotometer and plate transmission test ............................10

Annex B (normative) Radiometer calibration to spectroradiometric irradiance procedure ........................14

Annex C (normative) Computation values: PPD and erythema action spectra and UVA and UV-SSR

spectral irradiances ..........................................................................................................................................16

Annex D (normative) PMMA test plate surface specifications .............................................................................19

Annex E (normative) UVA reference sunscreen S2 .................................................................................................21

Annex F (informative) Statistical calculations ..........................................................................................................25

Bibliography .....................................................................................................................................................................27

© ISO 2012 – All rights reserved iii
---------------------- Page: 9 ----------------------
SIST EN ISO 24443:2012
ISO 24443:2012(E)
Foreword

ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies

(ISO member bodies). The work of preparing International Standards is normally carried out through ISO

technical committees. Each member body interested in a subject for which a technical committee has been

established has the right to be represented on that committee. International organizations, governmental and

non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International

Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.

International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.

The main task of technical committees is to prepare International Standards. Draft International Standards

adopted by the technical committees are circulated to the member bodies for voting. Publication as an

International Standard requires approval by at least 75 % of the member bodies casting a vote.

Attention is drawn to the possibility that some of the elements of this document may be the subject of patent

rights. ISO shall not be held responsible for identifying any or all such patent rights.

iv © ISO 2012 – All rights reserved
---------------------- Page: 10 ----------------------
SIST EN ISO 24443:2012
INTERNATIONAL STANDARD ISO 24443:2012(E)
Determination of sunscreen UVA photoprotection in vitro
1 Scope

This International Standard specifies an in vitro procedure to characterize the UVA protection of sunscreen

products. Specifications are given to enable determination of the spectral absorbance characteristics of UVA

protection in a reproducible manner.

In order to determine relevant UVA protection parameters, the method has been created to provide a UV spectral

absorbance curve from which a number of calculations and evaluations can be undertaken. Results from

this measurement procedure can be used for other computations, as required by local regulatory authorities.

These include calculation of the Ultraviolet-A protection factor (UVAPF) [correlating with in vivo UVAPF

from the persistent pigment darkening (PPD) testing procedure], critical wavelength and UVA absorbance

proportionality. These computations are optional and relate to local sunscreen product labelling requirements.

This method relies on the use of in vivo SPF results for scaling the UV absorbance curve.

This International Standard is not applicable to powder products such as pressed powder and loose powder products.

2 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
2.1
in vitro UVA protection factor
UVAPF

in vitro UVA protection factor of a sun protection product against UVA radiation, which can be derived

mathematically with in vitro spectral modelling
2.2
in vitro calculation of SPF
SPF
in vitro

protection factor of a sun protection product against erythema-inducing radiation calculated with spectral modelling

2.3
action spectrum for erythema
E(l)

relative effects of individual spectral bands of an exposure source for an erythema response

NOTE See References [1] and [2].
2.4
action spectrum for PPD
P(l)

relative effects of individual spectral bands of an exposure source for a persistent pigment response

NOTE See References [3] and [4].
2.5
monochromatic absorbance

sunscreen absorbance at wavelength, l, related to the sunscreen transmittance, T , by

A = - log (T )
l l

where transmittance, T , is the fraction of incident irradiance transmitted by the sunscreen film

© ISO 2012 – All rights reserved 1
---------------------- Page: 11 ----------------------
SIST EN ISO 24443:2012
ISO 24443:2012(E)
2.6
irradiance

fluence rate per unit area, expressed in W/m , for a defined range of wavelengths

EXAMPLE From 290 nm to 400 nm for UVA + UVB irradiance; from 320 nm to 400 nm for UVA irradiance.

2.7
spectral irradiance for SPF testing or PPD testing
I(l)
irradiance per unit wavelength, I(l) , expressed in W/m /nm
2.8
spectrophotometer

instrument that measures absorbance (or transmission) properties of a test medium as a function of wavelength

2.9
spectroradiometer

instrument that measures spectral irradiance (intensity in watts per unit area per nanometre) of

electromagnetic sources

NOTE Limited to ultraviolet, visible and short infrared ranges in this International Standard.

2.10
radiometer

instrument that measures broad band irradiance (intensity in watts per unit area) of electromagnetic sources

NOTE Limited to ultraviolet, visible and short infrared ranges in this International Standard.

3 Principle

The test is based on the assessment of UV-transmittance through a thin film of sunscreen sample spread on a

roughened substrate, before and after exposure to a controlled dose of radiation from a defined UV exposure

source. Because of the several variables that cannot be controlled with typical thin film spectroscopic techniques,

each set of sunscreen transmission data is mathematically adjusted so that the in vitro SPF data yield the same

measured in vivo SPF value that was determined by in vivo testing. Samples are then exposed to a specific

measured dose of UV radiation to account for the photostability characteristics of the test product. The resulting

spectral absorbance data have been shown to be a useful representation of both the width and height of the UVA

protection characteristics of the sunscreen product being tested. The mathematical modelling procedure has

been empirically derived to correlate with human in vivo (persistent pigment darkening) test results.

4 Apparatus
4.1 UV spectrophotometer specifications

The UV spectrophotometer wavelength range shall span the primary waveband of 290 nm to 400 nm. The

wavelength increment step shall be 1 nm.

A UV spectrophotometer that does not have a monochromator after the test sample should employ a

fluorescence rejection filter.

The UV spectrophotometer input optics should be designed for diffuse illumination and/or diffuse collection

of the transmitted irradiance through the roughened polymethylmethacrylate (PMMA) substrate, with and

without the sunscreen layer spread on its surface. The size of the diameter of the entrance port of the UV

spectrophotometer probe shall be smaller than the size of the light spot to be measured at the sample level (in

order to account for stray light). The area of each reading site should be at least 0,5 cm in order to reduce the

variability between readings and to compensate for the lack of uniformity in the product layer. The wavelength

should be accurate to within 1 nm, as checked using a holmium-doped filter (see Annex A). The ability of an

instrument to accurately measure absorbance is limited by the sensitivity of the instrument. The minimum

2 © ISO 2012 – All rights reserved
---------------------- Page: 12 ----------------------
SIST EN ISO 24443:2012
ISO 24443:2012(E)

required dynamic range for this methodology is 2,2 absorbance units as determined according to Annex A.

The maximum measured absorbance should be within the dynamic range of the device used. If the test

measurements yield absorbance curves that exceed the determined upper limit of the UV spectrophotometer,

the product should be re-tested using an instrument with increased sensitivity and dynamic range.

The lamp in the UV spectrophotometer that is used to measure the transmittance shall emit continuous

radiation over the range of 290 nm to 400 nm, and the level of irradiance should be sufficiently low, so that the

photostability of the product is not unduly challenged (a xenon flash lamp is a convenient solution). Therefore

the UV dose during one measurement cycle should not exceed 0,2 J/cm .

NOTE A UV spectrophotometer is used to measure the absorbance properties of the sunscreen on the test plates. A

spectroradiometer is used to measure the spectral energy distribution and intensity of the UV exposure source or the UV

spectrophotometer during the absorbance measurement of the sunscreen on the test plate.

4.2 Calibration of the UV spectrophotometer

The UV spectrophotometer shall be validated at regular intervals (recommended at least every month) by

measurements of reference materials.
A three-fold test is required, as described in Annex A:
— dynamic range of the UV spectrophotometer;
— linearity test of the UV spectrophotometer;
— wavelength accuracy test.
4.3 Calibration of the UV exposure source

The spectral irradiance at the exposure plane of the UV exposure source that is used for irradiation (to take into

account any photoinstability) shall be as similar as possible to the irradiance at ground level under a standard

[5] [6] [7]

zenith sun as defined by COLIPA or in DIN 67501 . The UV irradiance shall be within the following

acceptance limits (measured at sample distance).
Table 1 — UV exposure source specifications
UV exposure source specifications as measured with a spectroradiometer
2 2
Total UV irradiance (290 nm to 400 nm) 40 W/m to 200 W/m
a b
Irradiance ratio of UVA to UVB 8:22
320 nm to 400 nm.
290 nm to 320 nm.

The UV exposure source device should have the ability to maintain samples within the range of 25 °C to

35 °C. It is important that the temperature of the sample itself be measured and not just the surrounding air

temperature. To maintain samples at a temperature less than or equal to 35 °C, a filter system that particularly

reduces IR radiation should be used to achieve the specified temperature range. Cooling trays for the sample

plates or ventilators should be used to maintain a temperature below 35 °C and warming devices to maintain

samples at or above 25 °C.
4.4 Monitoring of the UV exposure source

The emission of the UV exposure source used for exposure shall be checked for compliance with the given

acceptance limits by a suitably qualified expert (at least) every 18 months, or after 3 000 hours of lamp running

time. The inspection should be conducted with a spectroradiometer that has been calibrated against a standard

lamp that is traceable to a national or an international calibration standard. In addition to the spectroradiometric

inspection, the intensity of the UV exposure source used for exposure shall be checked prior to each use. This

can be done using either a spectroradiometer or a radiometer with sensitivity in the UVA, calibrated for the

© ISO 2012 – All rights reserved 3
---------------------- Page: 13 ----------------------
SIST EN ISO 24443:2012
ISO 24443:2012(E)

same UV exposure source spectrum used for the exposure step of the procedure, applying the coefficient of

calibration to adjust for variance between the UVA radiometer and the reference spectroradiometer.

4.5 Calibration of the UVA radiometer used to monitor the test sample irradiation

If a UVA radiometer is used, this device shall have been suitably calibrated. This requires that it be calibrated

to the spectroradiometer used to measure the exposure source (as during annual solar simulator calibration).

Calibration shall be conducted in terms of UVA irradiance (320 nm to 400 nm) and shall be at the same level

at which the test plates are exposed. Once calibrated with the spectroradiometer, the UVA radiometer may be

used to determine the UV doses to be used during the exposure procedure on a day-to-day basis. Annex B

provides the step-by-step calibration procedure.
4.6 Substrate/plate

The substrate/plate is the material to which the test product is to be applied. For this method, PMMA plates

with one rough side of the substrate are to be used and are commercially available. One specific plate has

[9]

been validated for this test method; the specifications and preparation of this type of plate are described in

Annex D. The size of the substrate should be chosen such that the application area is not less than 16 cm .

5 Test method
5.1 Outline of the test procedure

5.1.1 Conduct the calibration and validation of the test equipment, including the UV spectrophotometer

used for transmission/absorbance measurements and the UVA radiometer (or spectroradiometer)

used to measure the UV exposure source, and verify the transmission properties of the test plates

as described in Annex D.

5.1.2 Conduct blank measurements of a glycerin-treated plate for the reference “blank”, which will be

used in the subsequent absorbance measurements.

5.1.3 Conduct in vitro absorbance measurements of the sunscreen product spread on a PMMA plate,

prior to any UV irradiation. Acquire the initial UV absorbance spectrum with A (l) data.

5.1.4 Conduct the mathematical adjustment of the initial UV absorbance spectrum using coefficient “C”

(see the calculation in 5.7.2) to achieve an in vitro SPF (no UV dose) equal to the in vivo SPF. Initial

UVAPF is calculated using A (l) and C.
0 0

5.1.5 A single UV exposure dose, D, is calculated, equal to 1,2 × UVAPF in J/cm .

5.1.6 Conduct UV exposure of the same sample as in 5.1.3, according to the calculated UV exposure

dose D.

5.1.7 Measure the in vitro absorbance of the sunscreen product after UV exposure. Acquire the second

UV spectrum with A(l) data.

5.1.8 Conduct the mathematical adjustment of the second absorbance spectrum (following UV

exposure) by multiplying with the same “C” coefficient, previously determined in 5.1.4. The resulting

absorbance curve is the final adjusted absorbance values.
NOTE For calculations, UV absorbance values shall be used.
5.2 Equipment calibration and validation of test plates

Test procedures as described in Annex A are to be completed to validate the wavelength accuracy, linearity and

absorbance limits of the UV spectrophotometer/spectroradiometer to be used for the test procedure. Validation

of the UV properties of the test PMMA plates shall also be conducted as described in Annex D.

4 © ISO 2012 – All rights reserved
---------------------- Page: 14 ----------------------
SIST EN ISO 24443:2012
ISO 24443:2012(E)
5.3 Absorption measurements through the plate

It is necessary to first determine the absorbance of UV radiation through a “blank” PMMA plate. Prepare a

“blank” plate by spreading a few microlitres of glycerin on the roughened side of the plate. Choose the amount

of glycerin such that the entire surface is just completely covered (approximately 15 µl for a 50 × 50 mm plate).

Any excess of glycerin should be avoided. Measure the absorbance through this “blank” plate and use this as

the baseline measurement for subsequent absorbance measurements.

NOTE Many spectrophotometers have “baseline” functions to automatically incorporate this baseline measurement

into the calculations of subsequent absorbance measurements.
5.4 Sample application

The sunscreen product is applied to a new untreated roughened PMMA plate (with the roughened side

uppermost) by mass, at an application rate of 1,3 mg/cm . To ensure dose accuracy and repeatability, the

application area should be not less than 16 cm . The application dose may be determined by measuring the

mass loss of the pipette before and after application of the product; alternatively, it may be applied based

on volumetric measurements with consideration of the specific gravity of the test sample. Where possible, a

positive-displacement automatic pipette should be used for this purpose.

The sunscreen is applied as a large number of small droplets of approximate equal volume, distributed evenly

over the whole surface of the plate. Finger cots should not be used to spread the product on the plate. The

fingertip used for spreading should be dipped into the test product and then wiped to remove excess product

before spreading the test product applied to the plate. The fingertip used to spread the product shall be cleaned

between applications of different test products.

After the sunscreen product is deposited on the surface of the plate, it shall be spread immediately over the

whole surface using light strokes with a fingertip (without finger cot). Spreading should be completed in a

two-phase process. First, the product should be distributed over the whole area as quickly as possible (less

than 30 seconds) using small circular motions with minimal pressure. Then the sample should be rubbed on the

plate surface using alternating horizontal and vertical strokes with increased moderate pressure. The second

phase should take 20 to 30 s.

This treated sample shall be allowed to dry for at least 30 min in the dark at the same temperature that will be

experienced under the UV exposure conditions (i.e. if UV source exposure conditions will be 35 °C, then the

drying conditions should also be at 35 °C; or if the UV source exposure conditions will be 25 °C, then the drying

conditions should also be 25 °C).
5.5 Absorbance measurements of the product-treated plate

The product-treated plate is placed in the light-path of the UV spectrophotometer and the absorbance of UV

radiation through the sample is determined for each wavelength, from 290 nm to 400 nm, in 1 nm steps. One or

more observations of absorbance may be made per plate and the mean value shall be determined for each plate.

5.6 Number of determinations

At least four plates prepared with the test sunscreen shall be used to establish the protection aspects of the

test sample. Additional plates shall be added to the sampling if the 95 % confidence interval (CI) is greater than

17 % of the mean value of the UVAPF value, until the 95 % CI is less than 17 % of the mean UVAPF value.

Calculation procedures for this are described in Annex F.

5.7 Determination of initial calculated SPF (SPF ), “C” value, initial UVAPF(UVAPF ),

in vitro 0
and UV exposure dose
5.7.1 Determination of SPF
in vitro

The UV solar simulator radiation (UV-SSR) source spectrum, I(l), (see Annex C) is multiplied with the corresponding

erythema action spectrum sensitivity value, E(l), (see Annex C) at that wavelength to yield the sunburning effective

energy at that wavelength. The resulting sunburning effective irradiance is integrated over the 290 nm to 400 nm

© ISO 2012 – All rights reserved 5
---------------------- Page: 15 ----------------------
SIST EN ISO 24443:2012
ISO 24443:2012(E)

range. The sunscreen transmission values at each wavelength are multiplied with the erythemal effective energy

at that wavelength and integrated over the same interval to yield the effective sunburning energy transmitted

through the test product. The ratio of these two integrals is the in vitro calculated SPF value.

Calculation of SPF is shown in Equation (1):
in vitro
λ = 400
EI()λλ××() dλ
λ =290
SPF = (1)
in vitro
λ = 400
−A ()λ
EI()λλ××() 10 ×dλ
λ =2990
where
[1]
E(l) is the erythema action spectrum (see Annex C);

I(l) is the spectral irradiance received from the UV source (SSR for SPF testing) (see Annex C);

A (l) is the mean monochromatic absorbance of the test product layer before UV exposure;

dl is the wavelength step (1 nm).
NOTE This calculated SPF value cannot be used as an SPF result.
in vitro
5.7.2 Determination of “C” value

The initial absorbance curve values are multiplied by a scalar value “C” until the in vitro calculated SPF values

are equal to the in vivo measured SPF. This is accompli
...

Questions, Comments and Discussion

Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.