SIST EN ISO 23674:2023
(Main)Cosmetics - Analytical methods - Direct determination of traces of mercury in cosmetics by thermal decomposition and atomic absorption spectrometry (mercury analyser) (ISO 23674:2022)
Cosmetics - Analytical methods - Direct determination of traces of mercury in cosmetics by thermal decomposition and atomic absorption spectrometry (mercury analyser) (ISO 23674:2022)
This International Standard specifies the determination of mercury in cosmetics by integrated mercury analytical systems. The purpose of this standard is :
• Description of the analytical procedure
• Validation and characterization of the method by its accuracy profile
Kosmetische Mittel - Untersuchungsverfahren - Direkte Bestimmung von Quecksilberspuren in kosmetischen Mitteln mittels thermischer Zersetzung und Atomabsorptionsspektrometrie (Quecksilber-Analysator) (ISO 23674:2022)
Dieses Dokument legt ein Untersuchungsverfahren zur direkten Bestimmung von Quecksilberspuren in kosmetischen Endprodukten mittels thermischer Zersetzung Atomabsorptionsspektrometrie (Quecksilber-Analysator) fest.
Dieses Dokument zielt darauf ab, ein Verfahren zur Quantifizierung von Quecksilberspuren in kosmetischen Mitteln bereitzustellen, denen Verbraucher bei ihrer Verwendung ausgesetzt sein können. Dieses Verfahren beschreibt die Bestimmung von Quecksilberspuren in kosmetischen Mitteln durch direkte Feststoffanalyse, ohne die Notwendigkeit eines vorherigen Aufschlusses. Das gesamte Quecksilber (sowohl anorganische als auch organische Spezies) kann entweder in festen oder flüssigen Proben quantifiziert werden.
Cosmétiques - Méthodes d’analyse - Dosage direct des traces de mercure dans les cosmétiques par décomposition thermique et spectrométrie d’absorption atomique (analyseur de mercure) (ISO 23674:2022)
Le présent document spécifie un mode opératoire d’analyse pour le dosage direct des traces de mercure dans les produits cosmétiques finis par décomposition thermique – spectrométrie d’absorption atomique (analyseur de mercure).
Le présent document a pour but de fournir un mode opératoire pour la quantification des traces de mercure dans les produits cosmétiques auxquelles les consommateurs sont susceptibles d’être exposés lors de leur utilisation. Cette méthode décrit le dosage des traces de mercure dans les cosmétiques par analyse solide directe sans nécessiter de digestion préalable. Le mercure total (à la fois les espèces inorganiques et organiques) peut être quantifié aussi bien dans des échantillons solides que liquides.
Kozmetika - Analizne metode - Neposredno določevanje živega srebra v sledovih v kozmetičnih izdelkih s termično razgradnjo in atomsko absorpcijsko spektrometrijo (analizator živega srebra) (ISO 23674:2022)
Ta mednarodni standard določa način določanja živega srebra v kozmetičnih izdelkih z integriranimi analiznimi sistemi za živo srebro. Cilj tega standarda je:
• Opis analitičnega postopka
• Validacija in karakterizacija metode s profilom točnosti
General Information
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN ISO 23674:2023
01-april-2023
Kozmetika - Analizne metode - Neposredno določevanje živega srebra v sledovih v
kozmetičnih izdelkih s termično razgradnjo in atomsko absorpcijsko
spektrometrijo (analizator živega srebra) (ISO 23674:2022)
Cosmetics - Analytical methods - Direct determination of traces of mercury in cosmetics
by thermal decomposition and atomic absorption spectrometry (mercury analyser) (ISO
23674:2022)
Kosmetische Mittel - Untersuchungsverfahren - Direkte Bestimmung von
Quecksilberspuren in kosmetischen Mitteln mittels thermischer Zersetzung und
Atomabsorptionsspektrometrie (Quecksilber-Analysator) (ISO 23674:2022)
Cosmétiques - Méthodes d’analyse - Dosage direct des traces de mercure dans les
cosmétiques par décomposition thermique et spectrométrie d’absorption atomique
(analyseur de mercure) (ISO 23674:2022)
Ta slovenski standard je istoveten z: EN ISO 23674:2022
ICS:
71.100.70 Kozmetika. Toaletni Cosmetics. Toiletries
pripomočki
SIST EN ISO 23674:2023 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST EN ISO 23674:2023
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SIST EN ISO 23674:2023
EN ISO 23674
EUROPEAN STANDARD
NORME EUROPÉENNE
September 2022
EUROPÄISCHE NORM
ICS 71.100.70
English Version
Cosmetics - Analytical methods - Direct determination of
traces of mercury in cosmetics by thermal decomposition
and atomic absorption spectrometry (mercury analyser)
(ISO 23674:2022)
Cosmétiques - Méthodes d'analyse - Dosage direct des Kosmetische Mittel - Untersuchungsverfahren - Direkte
traces de mercure dans les cosmétiques par Bestimmung von Quecksilberspuren in kosmetischen
décomposition thermique et spectrométrie Mitteln mittels thermischer Zersetzung und
d'absorption atomique (analyseur de mercure) (ISO Atomabsorptionsspektrometrie (Quecksilber-
23674:2022) Analysator) (ISO 23674:2022)
This European Standard was approved by CEN on 15 August 2022.
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, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Türkiye and
United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2022 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 23674:2022 E
worldwide for CEN national Members.
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SIST EN ISO 23674:2023
EN ISO 23674:2022 (E)
Contents Page
European foreword . 3
2
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SIST EN ISO 23674:2023
EN ISO 23674:2022 (E)
European foreword
This document (EN ISO 23674:2022) 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 March 2023, and conflicting national standards shall
be withdrawn at the latest by March 2023.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN shall not be held responsible for identifying any or all such patent rights.
Any feedback and questions on this document should be directed to the users’ national standards
body/national committee. A complete listing of these bodies can be found on the CEN website.
According to the CEN-CENELEC Internal Regulations, the national standards organizations 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, Republic of
North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Türkiye and the
United Kingdom.
Endorsement notice
The text of ISO 23674:2022 has been approved by CEN as EN ISO 23674:2022 without any modification.
3
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SIST EN ISO 23674:2023
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SIST EN ISO 23674:2023
INTERNATIONAL ISO
STANDARD 23674
First edition
2022-08
Cosmetics — Analytical methods —
Direct determination of traces of
mercury in cosmetics by thermal
decomposition and atomic absorption
spectrometry (mercury analyser)
Cosmétiques — Méthodes d’analyse — Dosage direct des traces
de mercure dans les cosmétiques par décomposition thermique et
spectrométrie d’absorption atomique (analyseur de mercure)
Reference number
ISO 23674:2022(E)
© ISO 2022
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SIST EN ISO 23674:2023
ISO 23674:2022(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2022
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting on
the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address below
or ISO’s member body in the country of the requester.
ISO copyright office
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Email: copyright@iso.org
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Published in Switzerland
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SIST EN ISO 23674:2023
ISO 23674:2022(E)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 1
5 Reagents . 2
6 Apparatus and equipment . 2
7 Calibration .3
7.1 General . 3
7.2 Liquid calibration standards. 3
7.3 Solid calibration standards . 4
8 Procedure .5
8.1 General . 5
8.2 Preparation of samples . 5
8.2.1 General recommendations . 5
8.2.2 General of samples . 5
9 Instrument parameters . 5
10 Quality control of the analysis . 5
10.1 General . 5
10.2 Quality control procedure . 5
10.2.1 Analysis blanks . 5
10.2.2 Quality control samples . 6
10.2.3 Replicates . 6
11 Calculation . 6
12 Method performance .6
13 Test report . 7
Annex A (informative) Performance of the method determined by the accuracy profile
methodology . 8
Annex B (informative) ISO 23674 and ISO 23821 common ring test results .13
Bibliography .16
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SIST EN ISO 23674:2023
ISO 23674:2022(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.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).
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. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www.iso.org/patents).
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and
expressions related to conformity assessment, as well as information about ISO's adherence to
the World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT), see
www.iso.org/iso/foreword.html.
This document was prepared by Technical Committee ISO/TC 217, Cosmetics, in collaboration with
the European Committee for Standardization (CEN) Technical Committee CEN/TC 392, Cosmetics, in
accordance with the Agreement on technical cooperation between ISO and CEN (Vienna Agreement).
Any feedback or questions on this document should be directed to the user’s national standards body. A
complete listing of these bodies can be found at www.iso.org/members.html.
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SIST EN ISO 23674:2023
ISO 23674:2022(E)
Introduction
[1]
This document has been developed in parallel with ISO 23821 . Knowing this, an interlaboratory test
using either one or the other method was performed on same tailor-made cosmetic products in order to
establish that both methods fulfilled the same requirements (see Annex B).
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SIST EN ISO 23674:2023
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SIST EN ISO 23674:2023
INTERNATIONAL STANDARD ISO 23674:2022(E)
Cosmetics — Analytical methods — Direct determination of
traces of mercury in cosmetics by thermal decomposition
and atomic absorption spectrometry (mercury analyser)
1 Scope
This document specifies an analytical procedure for direct determination of traces of mercury in
finished cosmetic products by thermal decomposition – atomic absorption spectrometry (mercury
analyser).
This document aims to provide a procedure of quantification of mercury traces in cosmetic products
that consumers can be exposed to in their usage. This method describes the determination of mercury
traces in cosmetics by direct solid analysis with no need of prior digestion. Total mercury (both
inorganic and organic species) can be quantified either in solid or liquid samples.
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements of this document. For dated references, only the edition cited applies. For
undated references, the latest edition of the referenced document (including any amendments) applies.
ISO 3696, Water for analytical laboratory use — Specification and test methods
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at https:// www .electropedia .org/
3.1
validation range
range from the upper to the lower concentration of samples used for the method evaluation
3.2
validated range
range of concentrations between the upper and lower levels that the method performance has been
demonstrated to be compliant with the method requirements
Note 1 to entry: The validated range shall not be confused with the validation range (3.1); it can be smaller.
4 Principle
The described method uses integrated instruments allowing mercury traces quantification. Samples
are weighed with no need of any chemical sample preparation as they are thermally decomposed in the
instrument (burned or ashed) in an oxygen flow at high temperature (between 650 °C and 900 °C). The
combustion gases travel through a catalyst tube set at about 615 °C. This step ensures conversion of
interfering components to forms that do not interfere and that are subsequently flushed. The resulting
mercury vapour is enriched on a downstream gold amalgamator and is then released as atomic
vapour by rapid heating of the amalgamator at a temperature of 800 °C to 900 °C. The atomic vapour
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SIST EN ISO 23674:2023
ISO 23674:2022(E)
is passed through a measuring cuvette system. The quantification occurs thanks to absorption at
253,7 nm. A wide dynamic range may be achieved by simultaneously passing mercury vapours through
measurement cells of different lengths.
5 Reagents
WARNING — The use of this document can involve hazardous materials, operations and
equipment. This document does not address all the safety risks associated with its use. It is the
responsibility of the analyst to take all appropriate measures for ensuring the safety and health
of the personnel prior to application of the document.
-1
5.1 Water, conforming to Grade 1 of ISO 3696 (conductivity below 0,1 μS.cm at 25 °C).
5.2 Hydrochloric acid, minimum mass fraction w = 30 %, density = 1,15 g/ml, suitable for elemental
analysis.
5.3 Diluted hydrochloric acid, produced by mixing hydrochloric acid (5.2) with ultrapure water
(5.1) at a ratio of approximately 1+9 parts, respectively.
5.4 Diluted nitric acid, prepared by diluting nitric acid of minimum mass fraction w=60 %,
density = 1,15 g/ml, suitable for ICP-MS with pure water (5.1) at a ratio of 1+9 respectively.
[2]
If diluted nitric acid is chosen to dilute the analyte stock solutions, it is recommended to add
[3]
L-cysteine at 0,1 g/l .
5.5 Analyte standard stock solutions (mercury), 1 000 µg/ml (commercially available).
5.6 Analyte standard stock solutions (mercury), 10 µg/ml [commercially available or freshly
prepared by dilution in the same dilution medium as calibration solutions (5.3 or 5.4) of a more
concentrated solution for example at 1 000 µg/ml such as 5.5].
Analyte standard stock solutions 5.5 or 5.6 can be used for this document according to their availability
on the local market. Recommendations from the supplier of stock solutions regarding stability (expiry
date and storage conditions) shall be followed to avoid mercury loss.
6 Apparatus and equipment
All apparatus and equipment that come into direct contact with samples or solutions should be pre-
cleaned with diluted hydrochloric acid (5.3) and rinsed with ultrapure water (5.1) to ensure the lowest
analytical background. To prevent contamination and adsorption, do not use laboratory materials made
up of borosilicate glass. The use of diluted nitric acid (5.4) is also permitted. To check the efficiency of
the cleaning step, a blank measurement can be performed prior to the analytical sequence.
Elemental mercury analyser with instrument control unit and sample containers made of suitable
materials (e.g. nickel, quartz glass or ceramic) are used. The sample containers usually have a capacity
of approximately 500 mg of solid sample or 500 µl, 1 000 µl and 1 500 µl of liquids. Mercury analysers
are equipped with an element-specific lamp for mercury. The mercury line of 253,7 nm is used.
Many instruments from several brands are available on the market and often marketed as “mercury
analysers”. The list of instruments that have been used for the interlaboratory test validating this
document is given in Annex A.
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SIST EN ISO 23674:2023
ISO 23674:2022(E)
7 Calibration
7.1 General
The aim of this step is to build a calibration curve by introduction in the instrument of increasing
mercury amounts. This calibration curve allows to get instrument response as a function of mercury
amount (in ng). At least 5 calibration standards shall be used in a range including the expected amounts
of mercury in the samples. Calibration of the instrument remains stable and is not mandatory prior to
each series of analyses provided that quality control (QC) requirements are met (see 10.2).
Due to the specificity of the technique towards mercury element, measurement of traces of mercury
in samples is weakly affected by interferences and matrix effects. Since the technique is relatively
insensitive to the matrix type, calibration can be performed either using in-house liquid (see 7.2) or solid
(see 7.3) calibration standards. However, moisture and organic contents may affect quantification. Such
differences between calibration standard and cosmetic samples shall be neutralized. For differences
in moisture content, optimize the drying times. For differences in quantity of organic material to be
combusted, optimize the time and temperature of combustion. For differences in interfering element,
optimize time for the catalytic conversion of elements needing catalytic conversion into a chemical
form that does not interfere with mercury detection.
7.2 Liquid calibration standards
Calibration solutions should be prepared in either diluted hydrochloric acid (5.3) or diluted nitric acid
containing L-Cysteine (5.4) to ensure stability of mercury. For laboratory convenience, calibration
solutions may be prepared in other acid mixture solutions, provided the operator checks the stability
of the mercury in that solution. Fresh calibration solutions should be prepared each time calibration is
needed. Two solution calibration procedures are possible.
— Introduce increasing amounts of mercury in a constant volume using increasing concentrations of
standard solution (see Table 1).
— Introduce increasing amounts of mercury using increasing volumes of one or more standard
solutions with a given mercury concentration (see Table 2).
Below are examples for these two ways of performing calibration.
Table 1 — Example of calibration solutions using constant volumes of different standards
Mercury concen- Mercury
Part of 10 µg/g Part of dilution
tration in µg/g amount in the
stock solution solution
Liquid calibration standard
(ppm) in liquid boat (ng)
(ml) (ml)
solution
calibration stand-
(5.6) (5.3 or 5.4)
ards
Calibration blank — 10 Blank 0
Calibration solution 1 0,01 9,99 0,01 1
Calibration solution 2 0,02 9,98 0,02 2
Calibration solution 3 0,05 9,95 0,05 5
Calibration solution 4 0,1 9,9 0,1 10
Calibration solution 5 0,2 9,8 0,2 20
Calibration solution 6 0,5 9,5 0,5 50
Calibration solution 7 1 9 1 100
Calibration solution 8 2 8 2 200
Calibration solution 9 5 5 5 500
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SIST EN ISO 23674:2023
ISO 23674:2022(E)
Table 2 — Example of calibration solutions using adjusted volumes of single standards
Part of Volume Mercury
Part of
Mercury con-
10 µg/g loaded in amount in
dilution
centration in
stock solu- the boat the boat (ng)
Liquid calibration standard
solution
µg/g (ppm) in
tion (µl)
solution
(ml)
liquid calibra-
(ml)
tion standards
(5.3 or 5.4)
(5.6)
Calibration blank — 10 Blank 100 0
Calibration level 1 0,02 9,98 0,02 50 1
Calibration level 2 0,02 9,98 0,02 100 2
Calibration level 3 0,02 9,98 0,02 250 5
Calibration level 4 0,2 9,8 0,2 50 10
Calibration level 5 0,2 9,8 0,2 100 20
Calibration level 6 0,2 9,8 0,2 250 50
Calibration level 7 2 8 2 50 100
Calibration level 8 2 8 2 100 200
Calibration level 9 2 8 2 250 500
Recommendations from the supplier of standard solutions regarding stability (expiry date and storage
conditions) shall be followed to avoid mercury loss.
7.3 Solid calibration standards
Solid certified reference materials (CRM), with known concentrations of mercury can be used in order
to calibrate the instrument prior analysing the samples (see Table 3). Since the technique is relatively
insensitive to the matrix type, these CRM can be chosen among a wide variety of nature that are not
necessarily cosmetic matrices (sediments, rocks, sewage sludge, etc.).
To ensure similar analysis behaviour, CRMs with sufficient homogeneity shall be selected so that sample
sizes similar to those of test samples may be used.
Table 3 — Example of calibration using solid CRMs
Approximative Approximative
Mercury content
weigh of solid amount of mer-
in the solid sam-
standard loaded cury in the boat
Calibration standards Name
ple
in the boat
(ng)
(µg/g - ppm)
(mg)
Calibration blank Blank 0 0 0
Calibration solid 1 SRM 2685c 0,1494 13,3 2
Calibration solid 2 SRM 2685c 0,1494 33,5 5
Calibration solid 3 SRM 2685c 0,1494 66,9 10
Calibration solid 4 SRM 2702 0,4474 44,7 20
Calibration solid 5 SRM 2702 0,4474 111,8 50
Calibration solid 6 ERM-EC680m 2,56 39,1 100
Calibration solid 7 ERM-EC680m 2,56 78,1 200
Calibration solid 8 ERM-EC680m 2,56 195,3 500
Recommendations from the supplier of certified reference materials regarding stability (expiry date
and storage conditions) shall be followed to avoid mercury loss. It is advised to select CRM with low
uncertainty on the certified content.
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SIST EN ISO 23674:2023
ISO 23674:2022(E)
8 Procedure
8.1 General
During all the process steps it shall be ensured that there is no loss of mercury and that contamination
is kept as low as possible.
8.2 Preparation of samples
8.2.1 General recommendations
Homogenize the sample using a suitable device, thoroughly cleaned to avoid contamination. Ensure
that the weighed sample portion is homogeneous.
8.2.2 General of samples
Precisely weigh 0,1 g of sample (0,05 g to 0,200 g) into sample boats. Place each boat onto the
instrument’s carousel.
Some instrument suppliers recommend adding additives (e.g. activated alumina, sodium carbonate) to
the samples to avoid potential scatter.
9 Instrument parameters
Operators shall follow recommendations on technical parameters and maintenance guidelines from
instrument supplier. The procedure can be divided in four major steps; drying, decomposition, purge
and amalgam step, for which parameters can be controlled.
Instrument parameters can be adjusted by the operator in order to maximize intensity and stability of
the signal. To adjust instrument parameters, it is recommended to use samples of known concentrations
of traces of mercury and similar physicochemical nature as the sample that will be further analysed.
Drying and decomposition parameters, such as time and temperature, can be adapted according to the
nature of the sample, as long as they are included in the range of experimental conditions validated by
the laboratory.
Because instrument parameters are linked, according to the instrument, several conditions can be
used to perform an accurate mercury quantification. Experimental conditions reported by laboratories
participating to the interlaboratory test have proven to be suitable for mercury traces quantification in
cosmetic products and are reported in Table A.4.
10 Quality control of the analysis
10.1 General
Recovery and relative standard deviation (RSD) mentioned in 10.2 are acceptance criteria obtained
by a single laboratory and enabling to assess the quality of the measurement. This intralaboratory
variability shall be lower than the total error (see Claus
...
SLOVENSKI STANDARD
oSIST prEN ISO 23674:2021
01-julij-2021
Kozmetika - Analizne metode - Neposredno določevanje živega srebra v sledovih v
kozmetičnih izdelkih s termično razgradnjo - Atomska absorpcijska spektrometrija
(analizator Hg) (ISO/DIS 23674:2021)
Cosmetics - Analytical methods - Direct determination of traces of mercury in cosmetics
by thermal decomposition - Atomic absorption spectrometry (mercury analyzer) (ISO/DIS
23674:2021)
Kosmetische Mittel - Untersuchungsverfahren - Bestimmung von Quecksilberspuren in
kosmetischen Mitteln mit integrierten Analysesystemen (ISO/DIS 23674:2021)
Cosmétiques - Méthodes d’analyse - Dosage direct des traces de mercure dans les
cosmétiques par décomposition thermique - Spectrométrie d’absorption atomique
(analyseur de mercure) (ISO/DIS 23674:2021)
Ta slovenski standard je istoveten z: prEN ISO 23674
ICS:
71.100.70 Kozmetika. Toaletni Cosmetics. Toiletries
pripomočki
oSIST prEN ISO 23674:2021 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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oSIST prEN ISO 23674:2021
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oSIST prEN ISO 23674:2021
DRAFT INTERNATIONAL STANDARD
ISO/DIS 23674
ISO/TC 217 Secretariat: ISIRI
Voting begins on: Voting terminates on:
2021-05-25 2021-08-17
Cosmetics — Analytical methods – Direct determination of
traces of mercury in cosmetics by thermal decomposition
— Atomic absorption spectrometry (mercury analyzer)
ICS: 71.100.70
THIS DOCUMENT IS A DRAFT CIRCULATED
This document is circulated as received from the committee secretariat.
FOR COMMENT AND APPROVAL. IT IS
THEREFORE SUBJECT TO CHANGE AND MAY
NOT BE REFERRED TO AS AN INTERNATIONAL
STANDARD UNTIL PUBLISHED AS SUCH.
IN ADDITION TO THEIR EVALUATION AS
ISO/CEN PARALLEL PROCESSING
BEING ACCEPTABLE FOR INDUSTRIAL,
TECHNOLOGICAL, COMMERCIAL AND
USER PURPOSES, DRAFT INTERNATIONAL
STANDARDS MAY ON OCCASION HAVE TO
BE CONSIDERED IN THE LIGHT OF THEIR
POTENTIAL TO BECOME STANDARDS TO
WHICH REFERENCE MAY BE MADE IN
Reference number
NATIONAL REGULATIONS.
ISO/DIS 23674:2021(E)
RECIPIENTS OF THIS DRAFT ARE INVITED
TO SUBMIT, WITH THEIR COMMENTS,
NOTIFICATION OF ANY RELEVANT PATENT
RIGHTS OF WHICH THEY ARE AWARE AND TO
©
PROVIDE SUPPORTING DOCUMENTATION. ISO 2021
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oSIST prEN ISO 23674:2021
ISO/DIS 23674:2021(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2021
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oSIST prEN ISO 23674:2021
ISO/DIS 23674:2021(E)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 1
5 Reagents . 2
6 Apparatus and equipment . 2
7 Calibration . 2
7.1 General . 2
7.2 Liquid calibration standards . 3
7.3 Solid calibration standards . 4
8 Procedure. 5
8.1 General . 5
8.2 Preparation of samples . 5
8.2.1 General recommendations . 5
8.2.2 General of samples . 5
9 Instrument parameters . 5
10 Quality control of the analysis . 5
10.1 General . 5
10.2 Quality control procedure . 5
10.2.1 Analysis blanks . 5
10.2.2 Quality control samples . 6
10.2.3 Replicates . 6
11 Calculation . 6
12 Method performance . 6
13 Test report . 7
Annex A (informative) Results of interlaboratory tests. 8
Annex B (informative) ISO 23674 and ISO 23821 common ring test results.11
Bibliography .13
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oSIST prEN ISO 23674:2021
ISO/DIS 23674:2021(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.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www .iso .org/ directives).
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. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www .iso .org/ patents).
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
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expressions related to conformity assessment, as well as information about ISO's adherence to the
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iso/ foreword .html.
This document was prepared by Technical Committee ISO/TC 217 Cosmetics.
Any feedback or questions on this document should be directed to the user’s national standards body. A
complete listing of these bodies can be found at www .iso .org/ members .html.
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oSIST prEN ISO 23674:2021
ISO/DIS 23674:2021(E)
Introduction
This standard specifies an analytical procedure for direct determination of traces of mercury in finished
cosmetic products by thermal decomposition – atomic absorption spectrometry (mercury analyser).
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oSIST prEN ISO 23674:2021
DRAFT INTERNATIONAL STANDARD ISO/DIS 23674:2021(E)
Cosmetics — Analytical methods – Direct determination of
traces of mercury in cosmetics by thermal decomposition
— Atomic absorption spectrometry (mercury analyzer)
1 Scope
The aim of this document is to provide a procedure of quantification of mercury traces in cosmetic
products that consumers might be exposed to in their usage. This method describes the determination
of mercury traces in cosmetics by direct solid analysis with no need of external digestion. Total mercury
(both inorganic and organic species) can be quantified either in solid or liquid samples.
This standard has been developed in parallel with another method of determination of traces of
mercury in cosmetics: ISO 23821 Cosmetics – Analytical methods – Determination of traces of mercury
in cosmetics by atomic absorption spectrometry (AAS) cold vapour technology after pressure digestion
[1]
. Knowing this, an interlaboratory test using either one or the other method was performed on same
tailor-made cosmetic products in order to establish that both methods fulfilled the same requirements
(see Annex B).
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements of this document. For dated references, only the edition cited applies. For
undated references, the latest edition of the referenced document (including any amendments) applies.
ISO 3696, Water for analytical laboratory use — Specification and test methods
3 Terms and definitions
Validation range: range of concentrations used for the method evaluation. It starts from the lowest
concentration of the validation samples and ends at the highest concentration of the validation samples
Validated range: range of concentrations inside which the method performances are compliant with the
method requirements, i.e. range of concentrations where the tolerance intervals are located inside the
acceptance limits.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at https:// www .electropedia .org/
4 Principle
The described method uses integrated instruments allowing mercury traces determination and
quantification. Samples are weighed with no need of any chemical sample preparation as they are
thermally decomposed in the instrument (burned or ashed) in an oxygen flow at high temperature
(between 650°C and 900°C). The combustion gases travel through a catalyst tube set at about 615°C.
This step ensures conversion of interfering components to forms that do not interfere and that are
subsequently flushed. The resulting mercury vapour is enriched on a downstream gold amalgamator
and is then released as atomic vapour by rapid heating of the amalgamator at a temperature of 800°C
to 900°C. The atomic vapour is passed into a measuring cuvette system and quantified by means of the
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oSIST prEN ISO 23674:2021
ISO/DIS 23674:2021(E)
absorption at 253,7 nm. A wide dynamic range may be achieved by simultaneously passing mercury
vapors through measurement cells of different lengths.
5 Reagents
WARNING — The use of this standard can involve hazardous materials, operations and
equipment. This standard does not purport to address all the safety problems associated with
its use. It is the responsibility of the user of this standard to take appropriate measures for
ensuring the safety and health of the operator prior to application of the standard and to fulfil
local requirements for this purpose.
5.1 Ultrapure water, conductivity below 0,1µS/cm at 25°C according to Type 1 water specifications
defined in ISO 3696 standard.
5.2 Hydrochloric acid, minimum w = 30 %, density = 1,15 g/mL
5.3 Diluted hydrochloric acid, produced by mixing hydrochloric acid (5.2) with ultrapure water (5.1)
at a ratio of approximately 1+9 parts respectively.
5.4 Diluted nitric acid (0,1 mol/L).
[2]
NOTE If diluted nitric acid is chosen to dilute the analyte stock solutions, it is recommended to add
[3]
L-cysteine at 0,1 g/L .
5.5 Analyte standard stock solutions (Mercury), 1000 µg (Hg)/mL (commercially available)
5.6 Analyte standard stock solutions (Mercury), 10 µg(Hg)/mL (commercially available or freshly
prepared by dilution in the same dilution medium as calibration solutions (5.3 or 5.4) of a more
concentrated solution for example at 1000 µg/mL such as 5.5)
5.5 or 5.6 analyte standard solutions can be used for this standard according to their availability on the
local market. Recommendations from the supplier of stock solutions regarding stability (expiry date
and storage conditions) shall be carefully followed to avoid mercury loss.
6 Apparatus and equipment
WARNING — - All apparatus and equipment that come into direct contact with sample or solutions
should be pre-cleaned with diluted hydrochloric acid (5.3) and rinsed with ultrapure water (5.1)
to ensure the lowest analytical background. To prevent contamination and adsorption, do not
use lab materials made with borosilicate glass.
Many instruments from several brands are available on the market and often marketed as “mercury
analysers”. List of instruments that have been used for interlaboratory test in order to validate this
standard is available on Annex A.
7 Calibration
7.1 General
The aim of this step is to build a calibration curve by introduction in the instrument of increasing
mercury amounts. This calibration curve allows to get instrument response as a function of mercury
amount (in ng). At least 5 calibration standards shall be used in a range including the expected amounts
of mercury in the samples. Calibration of the instrument remains stable and is not mandatory prior to
each series of analyses provided that QC requirements are met (10.2).
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oSIST prEN ISO 23674:2021
ISO/DIS 23674:2021(E)
Due to the specificity of the technique towards mercury element, measurement of traces of mercury
in samples is weakly affected by interferences and matrix effects. Since the technique is relatively
insensitive to the matrix type, calibration can be performed either using in-house liquid (7.2) or solid
(7.3) calibration standards. However, moisture and organic contents may affect quantification. Such
differences between calibration standard and cosmetic samples shall be neutralized by optimizing
drying times for moisture content, and combustion times and temperatures for quantity of organic
material to be combusted or amount of interfering element needing catalytic conversion to a chemical
form that does not interfere with mercury detection.
7.2 Liquid calibration standards
Calibration solutions should be prepared in either diluted hydrochloric acid (5.3) or diluted nitric acid
containing L-Cysteine (5.4) to ensure stability of mercury. For laboratory convenience, calibration
solutions may be prepared in other acid mixture solutions, provided the operator checks the stability
of the mercury in that solution. Fresh calibration solutions should be prepared each time calibration is
needed. Two solution calibration procedures are possible:
— Introduce increasing amounts of mercury i
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