1、BSI Standards Publication PD ISO/TR 17276:2014 Cosmetics Analytical approach for screening and quantification methods for heavy metals in cosmeticsPD ISO/TR 17276:2014 BRITISH STANDARD National foreword This British Standard is the UK implementation of ISO/TR 17276:2014. The UK participation in its
2、preparation was entrusted to Technical Committee CW/217, Cosmetics. A list of organizations represented on this committee can be obtained on request to its secretary. This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct applic
3、ation. The British Standards Institution 2014. Published by BSI Standards Limited 2014 ISBN 978 0 580 83686 2 ICS 71.100.70 Compliance with a British Standard cannot confer immunity from legal obligations. This British Standard was published under the authority of the Standards Policy and Strategy C
4、ommittee on 30 June 2014. Amendments issued since publication Date Text affectedPD ISO/TR 17276:2014 ISO 2014 Cosmetics Analytical approach for screening and quantification methods for heavy metals in cosmetics Cosmtiques Approche analytique des mthodes pour lvaluation et la quantification des mtaux
5、 lourds dans les cosmtiques TECHNICAL REPORT ISO/TR 17276 First edition 2014-05-01 Reference number ISO/TR 17276:2014(E)PD ISO/TR 17276:2014ISO/TR 17276:2014(E)ii ISO 2014 All rights reserved COPYRIGHT PROTECTED DOCUMENT ISO 2014 All rights reserved. Unless otherwise specified, no part of this publi
6、cation 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 ISOs member body in the count
7、ry 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 copyrightiso.org Web www.iso.org Published in SwitzerlandPD ISO/TR 17276:2014ISO/TR 17276:2014(E) ISO 2014 All rights reserved iii Contents Page Foreword iv Introduction v
8、1 Scope . 1 2 Principles . 1 2.1 Planning 1 2.2 Selection of a test substance . 2 2.3 Preparation of samples 2 2.4 Detection tests and methods 3 Annex A (informative) Colourimetric reaction 38. 6 Annex B (informative) X-ray fluorescence .10 Annex C (informative) Quantification of elements in samples
9、 .11 Bibliography .16PD ISO/TR 17276:2014ISO/TR 17276:2014(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 comm
10、ittees. 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
11、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 th
12、e 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. I
13、SO 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 doc
14、ument is information given for the convenience of users and does not constitute an endorsement. For an explanation on the meaning of ISO specific terms and expressions related to conformity assessment, as well as information about ISOs adherence to the WTO principles in the Technical Barriers to Tra
15、de (TBT) see the following URL: Foreword - Supplementary information The committee responsible for this document is ISO/TC 217, Cosmetics.iv ISO 2014 All rights reservedPD ISO/TR 17276:2014ISO/TR 17276:2014(E) Introduction Heavy metals occur naturally in the environment. Some heavy metals are utiliz
16、ed in many industries, and some in very small amount are essential minerals to life. On the other hand, heavy metals are often a concern due to their toxicity. Even for essential minerals, they can be a concern when excess amounts are ingested, or more generally, when the human exposure is too high,
17、 independently of the route of exposure. Heavy metals are ubiquitous as they are found in nature (rocks, soil, water, amongst other sources). As such, these heavy metals can be found as impurities in raw materials, and, while not added intentionally to cosmetics, might be present as traces in finish
18、ed products. 12 The term “heavy metals” is widely used without a single definition. Commonly recognized heavy metals include, but are not limited to: lead, mercury, cadmium, arsenic, and antimony. While it is acknowledged that heavy metal traces in cosmetic products are unavoidable due to the ubiqui
19、tous nature of these elements, companies have implemented numerous measures to monitor and control the amount that might be present. This Technical Report presents the most common and typical analytical methods and tools for the detection of heavy metals in cosmetic raw materials and finished produc
20、ts. ISO 2014 All rights reserved vPD ISO/TR 17276:2014PD ISO/TR 17276:2014Cosmetics Analytical approach for screening and quantification methods for heavy metals in cosmetics 1 Scope This Technical Report introduces most common and typical analytical approaches for screening and quantification of he
21、avy metals of general interest at both raw material and finished product level. This Technical Report covers techniques from traditional colourimetric reaction, which can be executed without expensive instrument to the high-end one, like that of inductively coupled plasma-mass spectrometry (ICP-MS),
22、 which allows detection of elements at g/kg level. Thus, this Technical Report covers the advantages and disadvantages of each analytical technique so that a suitable approach can be chosen. The intent of this Technical Report is not to set or suggest acceptable concentration limits of heavy metals
23、in both raw materials and finished products which have to be determined by each regulatory authority. NOTE 1 The term “heavy metals” is widely used without single definition. NOTE 2 Elements can be specified as heavy metals by one legislation, while not by others. 2 Principles 2.1 Planning First, th
24、e approach is divided into screening and quantification of total heavy metals content. Heavy metals analysis requires not only technical knowledge and experience, but often requires expensive facilities and vigorous condition of sample preparation, especially when quantification of heavy metals cont
25、ent is investigated. The screening approach can contribute to identifying whether heavy metals levels should be determined using more quantitative methods. An approach to analyse heavy metals in cosmetics products and raw materials consists of sample preparation method and detection method. Analytic
26、al testing conditions should be determined with appropriate combination of preparation method and detection method with acceptable validation data. Sample preparation methods: leaching; digestion. Detection tests and methods: colourimetric reaction; 3-8 x-ray fluorescence (XRF); atomic absorption sp
27、ectrometry (AAS); inductively coupled plasma optical emission spectroscopy (ICP-OES), which is also known as inductively coupled plasma atomic emission spectroscopy (ICP-AES); inductively coupled plasma mass spectrometry (ICP-MS). These approaches basically do not detect a difference between organic
28、 and inorganic compounds of an element. For example, they do not detect difference between metallic mercury and a phenylmercury TECHNICAL REPORT ISO/TR 17276:2014(E) ISO 2014 All rights reserved 1PD ISO/TR 17276:2014ISO/TR 17276:2014(E) compound. Also, they do not detect difference by valence state,
29、 such as, between chromium (III) and chromium (VI). If there is a specific interest in them, appropriate approaches should be taken, e.g. ICP- MS equipped with chromatography. Typical approach for the screening and quantification on both raw materials and finished products are introduced in the Anne
30、x A, Annex B, and Annex C. Approaches other than introduced in the annexes can be effective. 2.2 Selection of a test substance Screening and quantification of heavy metals can be performed on both raw materials and finished products. As heavy metals are found in nature, certain raw materials, such a
31、s, inorganic materials can naturally contain heavy metals. Knowing the source and signature of raw materials is an effective approach to control the levels of heavy metals in finished products. Monitoring at raw material level can avoid the use of heavy-metal contaminated raw materials and is an eff
32、ective way to control heavy metal concentration in finished products. 2.3 Preparation of samples 2.3.1 General In many elemental analysis techniques, samples are converted into liquid. The preparation of the samples is related to the nature of the cosmetic matrix. The sample preparation techniques a
33、re basically classified into two: leaching method and digestion method. 2.3.2 Leaching method Leaching method is a preparation method in order to determine an amount of heavy metals extracted from a sample under acidic conditions. The principle of the leaching method is modelling the conditions of a
34、 gastrointestinal fluid or sweat to liberate heavy metals that might be present in products. This allows estimating an amount of heavy metals to which users can be exposed. 2.3.3 Digestion method Digestion method is a preparation method in order to determine the total amount of heavy metals present
35、in a sample. When full digestion method is used, it reliably reveals the worst case scenario of exposure. Also, full digestion of the matrix reduces interferences in the detection, especially in ICP-MS. Samples are sometimes simply heated to ashes (dry ashing) in order to remove organic matter. Dry
36、ashing can be carried out with magnesium nitrate as ashing aids. 910Other ashing aids might be applicable such as magnesium sulfate with sulphuric acid. 8Since cosmetic matrix is complex, insoluble matter often remains after ashing and further digestion is often conducted. Samples are digested by he
37、ating, usually with a single acid, sometimes with multiple acids (wet digestion), rarely with alkali (fusion), in open or closed vessels and are fully or almost entirely dissolved. It often requires vigorous conditions and cautions concerning possible volatilisation for some metals (such as cadmium,
38、 arsenic, or mercury) to obtain acceptable recovery. 811 Recent trends are for closed vessel digestion with microwave assistance which can reduce losses of volatile elements and also improve efficiency in routine analysis. Choice of acids is the important factor to fully digest samples. For cosmetic
39、 products, the usage of hydrofluoric acid (HF) can be considered highly effective in digestion of silica compounds. The treatment with hydrofluoric acid needs a post- treatment with boric acid in order to mask remaining HF. Nitric acid, hydrochloric acid, sulphuric acid, and other acids are also sel
40、ected to digest samples. Each acid, including HF, has their own advantage and therefore often used by combination to effect full digestion. There are many publications for heavy metals analysis, including assessments of sample digestion methods. There is a digestion method recently published with in
41、ter-laboratory results for lead, cadmium, and mercury on different finished 2 ISO 2014 All rights reservedPD ISO/TR 17276:2014ISO/TR 17276:2014(E) products containing inorganic materials. This method describes a digestion process using nitric acid with hydrochloric acid in a closed vessel under high
42、 pressure heat to around 200 C. The method specifies the detailed conditions in order to get reproducible results. 12The study by the authority reports that analytical results obtained by nitric acid and those by nitric acid with HF, in comparison. Nitric acid digestion gave lower results than nitri
43、c acid with HF on some cosmetic products. 13Nevertheless, if possible, it is recommended to avoid the use of hydrofluoric acid for safety and hygiene reasons, within the digestion. 2.4 Detection tests and methods 2.4.1 Colourimetric reaction This technique has been described as detection test, mostl
44、y for raw materials, for heavy metals which form yellow to dark brown-coloured insoluble sulphide under pH 3,0 to 3,5 condition. Elements which can be detected by this technique are for instance, lead, bismuth, copper, cadmium, antimony, tin, and mercury. 8The insoluble sulphide produced in the reac
45、tion shows dark colour in diluted solutions due to its colloidal dispersion. As the source of sulphide ion, either sodium sulphide or thioacetamide is normally used. The density of colour is increased in proportion to the concentration of heavy metals. The quantity of heavy metals is expressed in te
46、rms of concentration of lead, in comparison with a lead reference solution. The advantage of the technique is that it can be performed without expensive instruments. The colourimetric test is only applicable for sample solutions which are uncoloured and free from insoluble matter. Recovery should be
47、 determined in an accurate and suitable way, especially if dry-ashing is used to obtain such solutions. This technique cannot detect selenium and chromium. Also, zinc produces white precipitate which can cause interference. For this reason, it is important to confirm the reliability of the test by a
48、ppropriate validation. When difference in the hue of the developed colour is observed between samples solution and standard solution, other techniques should be explored. NOTE Applications of colourimetric tests are found in several compendia for cosmetics and pharmaceuticals 3-7such as Japanese Sta
49、ndards of Quasi-drug Ingredients (JSQI) 3and European Pharmacopoeia. 4Also, the Japanese Standards of Cosmetics Ingredients 5and Japanese Cosmetics Ingredients Codex 6can still be referred for actual applications, especially for English description, although they are not active compendia anymore as they have basically been consolidated to JSQI. 2.4.2 X-ray fluorescence 2.4.2.1 General When a sample is irradiated with X-rays which have energy above a certain level, core electrons in atoms are exci
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