prEN ISO 23674

Cosmetics - Analytical methods - Direct determination of traces of mercury in cosmetics by thermal decomposition - Atomic absorption spectrometry (mercury analyzer) (ISO/DIS 23674:2021)

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 - Bestimmung von Quecksilberspuren in kosmetischen Mitteln mit integrierten Analysesystemen (ISO/DIS 23674:2021)

Das Ziel dieses Dokuments ist es, ein Verfahren zur Quantifizierung von Quecksilberspuren in kosmetischen Mitteln bereitzustellen, denen Verbraucher bei ihrer Verwendung ausgesetzt sein könnten. Dieses Verfahren beschreibt die Bestimmung von Quecksilberspuren in kosmetischen Mitteln durch direkte Feststoffanalyse, ohne die Notwendigkeit eines externen Aufschlusses. Das gesamte Quecksilber (sowohl anorganische als auch organische Spezies) kann entweder in festen oder flüssigen Proben quantifiziert werden.
Diese Norm wurde parallel zu einem anderen Verfahren zur Bestimmung von Quecksilberspuren in kosmetischen Mitteln entwickelt: ISO 23821 Cosmetics - Analytical methods - Determination of traces of mercury in cosmetics by atomic absorption spectrometry (AAS) cold vapour technology after pressure digestion [1]. Mit diesem Wissen wurde an den gleichen individuell gefertigten kosmetischen Mitteln ein Ringversuch durchgeführt, bei dem entweder das eine oder das andere Verfahren angewendet wurde, um nachzuweisen, dass beide Verfahren die gleichen Anforderungen erfüllt haben (siehe Anhang B).

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)

Kozmetika - Analizne metode - Neposredno določevanje živega srebra v sledovih v kozmetičnih izdelkih s termično razgradnjo - Atomska absorpcijska spektrometrija (analizator Hg) (ISO/DIS 23674:2021)

General Information

• Status: Not Published
• ICS: 71.100.70 - Cosmetics. Toiletries
• Technical Committee: CEN/TC 392 - Cosmetics
• Drafting Committee: CEN/TC 392 - Cosmetics
• Current Stage: 4060 - Closure of enquiry - Enquiry
• Due Date: 17-Aug-2021
• Completion Date: 17-Aug-2021
• Ref Project: oSIST prEN ISO 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)

Standards Content (sample)

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

All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may

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Published in Switzerland
ii © ISO 2021 – All rights reserved
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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.

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.

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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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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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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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
...