1、 ISO 2012 Nanotechnologies Nanoscale titanium dioxide in powder form Characteristics and measurement Nanotechnologies Dioxyde de titane la nano-chelle sous forme de poudre Caractristiques et mesurage TECHNICAL SPECIFICATION ISO/TS 11937 First edition 2012-12-15 Reference number ISO/TS 11937:2012(E)
2、ISO/TS 11937:2012(E)ii ISO 2012 All rights reserved 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 pe
3、rmission in writing from either ISO at the address below or ISOs 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 copyrightiso.org Web www.iso.org Published in Switzerland ISO/TS 11937:2012(E) Fore
4、word 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 techn
5、ical 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
6、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
7、 the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. In other circumstances, particularly when there is an urgent market requirement for such documents, a technical committee may decide to publish other types
8、of document:an ISO Publicly Available Specification (ISO/PAS) represents an agreement between technical experts in an ISO working group and is accepted for publication if it is approved by more than 50 % of the members of the parent committee casting a vote;an ISO Technical Specification (ISO/TS) re
9、presents an agreement between the members of a technical committee and is accepted for publication if it is approved by 2/3 of the members of the committee casting a vote. An ISO/PAS or ISO/TS is reviewed after three years in order to decide whether it will be confirmed for a further three years, re
10、vised to become an International Standard, or withdrawn. If the ISO/PAS or ISO/TS is confirmed, it is reviewed again after a further three years, at which time it must either be transformed into an International Standard or be withdrawn. Attention is drawn to the possibility that some of the element
11、s of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO/TS 11937 was prepared by Technical Committee ISO/TC 229, Nanotechnologies. ISO 2012 All rights reserved iii ISO/TS 11937:2012(E) Introduction Titanium dioxide,
12、 TiO 2 , has been used extensively for circa 90 years as the main white pigment in paints, plastics, printing inks and many other products due to its ability to scatter visible light and provide white opacity to the products in which it is used. More recently, nanoscale titanium dioxide has been dev
13、eloped, here the smaller particle size does not provide pigmentary properties but gives a transparent product which can be used in different applications such as sunscreens or catalysis where the small particle size can enhance the activity. Accordingly, there is a need to better define the characte
14、ristics of the nanoscale material providing these alternative properties. This technical specification provides the methods to evaluate mass fraction of the rutile and anatase titanium dioxide as well as to measure four key parameters: crystal structure, average crystallite size, average primary par
15、ticle size and specific surface area, which are commonly used to indicate characteristics of nanoscale materials. Most of the manufactured nanoscale titanium dioxides are synthesized by the sulfate process, the chloride process or the sol-gel process, and the crystal structures of the products are a
16、lmost entirely rutile and anatase. Therefore, brookite and amorphous forms are not specified in this Technical Specification. The X-ray diffraction (XRD) method is used to measure the crystal structure and the ratio of anatase to rutile. Commonly, some of the nanoscale titanium dioxide products are
17、coated with silica or alumina for specific applications. Alternatively, some of the nanoscale titanium dioxide products may include a dopant of another metal within their crystal lattice for other specific applications. These coatings and dopants are permanent. Buyer, seller and regulator should be
18、aware the presence of any coatings. The XRD method and transmission electron microscopy (TEM) are used to measure crystal size and primary particle size/shape, respectively. The Brunauer, Emmet and Teller (BET) method is widely used for the evaluation of specific surface area. Theoretically, XRD jus
19、t measures the core size of the coated nanoscale titanium dioxide but not the surface coating. TEM is used to measure the physical primary particle size including surface coatings. Nanotechnology is a rapidly growing and evolving field. Users of this document should maintain an awareness of the legi
20、slative environment and latest developments in Environmental Health and Safety regarding nanotechnology. These references may be of interest 1-12 . Responsibilities of users of this document include the following: the seller is obliged to provide the buyer with such environmental health and safety i
21、nformation as required by law. If the seller or buyer wishes to assess the environmental, safety or health risks of the material, they may refer to ISO/TR 12885:2008 8for further guidance. This document may be used in conjunction with other application specific standards developed either by ISO or o
22、ther standards development bodies.iv ISO 2012 All rights reserved Nanotechnologies Nanoscale titanium dioxide in powder form Characteristics and measurement WARNING Persons using this document should be familiar with normal laboratory practice, if applicable. This document does not purport to addres
23、s all of the safety concerns, if any, associated with its use. It is the responsibility of the user to establish appropriate safety and health practices and to ensure compliance with any regulatory requirements. 1 Scope This Technical Specification provides requirements to describe the basic charact
24、eristics of titanium dioxide in powder form relevant for applications in nanotechnology. It is intended to detail the materials specification necessary to use titanium dioxide in the applications related to nanotechonology. It is limited to dry powders and does not include materials dispersed or sus
25、pended in water or solvents. It does not cover characteristics for health and safety issue, and for specific application of titanium dioxide or for surface modification, if coated. 2 Normative references The following referenced documents are indispensable for the application of this document. For d
26、ated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 591-1, Titanium dioxide pigments for paints Part 1: Specifications and methods of test ISO 9277:2010, Determination of the specific surface a
27、rea of solids by gas adsorption using the BET method ISO 13322-1, Particle size analysis Image analysis methods Part 1: Static image analysis methods ISO 14887, Sample preparation Dispersing procedures for powders in liquids ISO 14488, Particulate materials Sampling and sample splitting for the dete
28、rmination of particulate properties ISO/TS 27687, Nanotechnologies Terminology and definitions for nano-objects Nanoparticle, nanofibre and nanoplate ISO 80004-1, Nanotechnologies Vocabulary Part 1: Core terms 3 T erms an d definiti ons For the purposes of this document, the terms, definitions and a
29、bbreviated terms given in ISO 14488, ISO/TS 27687 and ISO/TS 80004-1 and the following apply. 3.1 transmission electron microscope (TEM) instrument that produces magnified images or diffraction patterns of the sample by an electron beam which passes through the sample and interacts with it ISO 29301
30、2010, definition 3.37 TECHNICAL SPECIFICATION ISO/TS 11937:2012(E) ISO 2012 All rights reserved 1 ISO/TS 11937:2012(E) 3.2 X-Ray diffraction (XRD) scattering in which the incident radiation is a beam of x-rays. The elastic scattering of the x-rays from the electron clouds of atoms in a system produ
31、ces a diffraction pattern that gives information about the crystallographic structure 3.3 s p e c i f ic s u r f ac e area absolute surface area of the sample divided by sample mass ISO 9277:2010, definition 3.11 3.4 crystal structure arrangement of a regular and repeating internal unit of atoms in
32、three dimensions in which the atoms are set in space in a fixed relation to each other 3.5 primary particle particle not formed from a collection of smaller particles Note 1 to entry: The term typically refers to particles formed through nucleation from the vapour phase before coagulation occurs. IS
33、O/TR 27628:2007, definition 2.16 4 Basic characteristics and measurement methods For titanium dioxide in powder form conforming to this Technical Specification the following basic characteristics should be measured and reported. The necessary characteristics and corresponding measurement method are
34、listed in Table 1. The requirements for magnitudes of measured characteristics shall be agreed upon between interested parties and test results should be reported complying with the requirement of Clause 6. Table 1 Basic characteristics with corresponding measurement methods Characteristics Unit mea
35、surement methods Mass fraction of titanium dioxide % (kg/kg) Aluminium reduction method/ Chromium(II) chloride reduction method (ISO 591-1) or other chemical analysis methods upon the agreement between interested parties Ratio of crystalline phases % XRD Average crystallite size nm XRD (Scherrer for
36、mula) Average primary particle size nm TEM Specific surface area m 2 /g BET method NOTE 1 The set of basic characteristics is evaluated in order to represent the nanoscale titanium dioxide in powder form in terms of nano size-related features and its main ingredient. NOTE 2 Additional characteristic
37、s relevant to specific applications may be specified depend on the intended application and other related international standards. NOTE 3 The detailed procedures for these measurement methods are not provided in this Technical Specification. In order to obtain the measurement results required by the
38、 interested parties, the measurement methods should be applied and managed under a well recognized quality system.2 ISO 2012 All rights reserved ISO/TS 11937:2012(E) 5 Sampling Take a representative sample of the product to be tested, as described in ISO 14488. 6 Reporting The test report should con
39、tain at least the following information: 6.1 A reference to this Technical Specification, i.e. ISO/TS 11937. 6.2 Identification of material tested (product name, chemical name). 6.3 Samples description (manufacturer of nanoscale titanium dioxide, batch number or lot number, country of origin). 6.4 L
40、aboratory (name of testing laboratory). 6.5 Results. 6.5.1 Measurement results of basic characteristics, and their measurement methods required in Table 1 (for TEM, also report the number of particles used in the determination of the average size, standard deviation of measurement results and detail
41、s on measurement method for TEM method). 6.5.2 Measurement uncertainty (subject to the agreement between users, suppliers and regulators). 6.6 Additional information (if any). ISO 2012 All rights reserved 3 ISO/TS 11937:2012(E) Bibliography 1 CAN/CSA-Q850-97 Risk Management: Guideline for Decision M
42、akers 2 Consumer Product Safety Commission, Handbook for Manufacturing Safer Consumer Products. July 2006, www.cpsc.gov/businfo/intl/handbookenglishaug05.pdf 3 Consumer Product Safety Commission, Recall Handbook, May 1999, www.cpsc. gov/BUSINFO/8002.html 4 EC Guidelines for the notification of Dange
43、rous Consumer Products to the Competent Authorities of the Member States by Producers and Distributors in Accordance with Article 5(3) of Directive 2001/95/EC ec.europa.eu/consumers/cons_safe/prod_safe/guidelines_documents.pdf 5 European Commission, Risk Assessment Guidelines for Non-Food Consumer P
44、roducts, Draft for Consultation, August 2008 6 http:/ /ec.europa.eu/consumers/ipm/risk_assesment_guidelines_non_food.pdf 7 IECs Advisory Committee on Safety Development of a standard for safety related risk assessment in the area of low voltage 8 ISO/TR 12885:2008, Nanotechnologies Health and safety
45、 practices in occupational settings relevant to nanotechnologies 9 ISO/IEC Guide 51 Safety aspects Guidelines for their inclusion in standards 10 ISO/IEC Guide 50 Safety aspects Guidelines for child safety 11 ISO/IEC Guide 71 Guidelines for standards developers to address the needs of older persons
46、and persons with disabilities 12 ISO Guide 73 Risk management Vocabulary 13 EN 13925-1:2003, Non-destructive testing X-ray diffraction from polycrystalline and amorphous materials Part 1: General principles 14 ISO/TS 11931, Nanotechnologies Nanoscale calcium carbonate in powder form Characteristics
47、and measurement 15 EN 13925-2:2003, Non-destructive testing X-ray diffraction from polycrystalline and amorphous materials Part 2: Procedures 16 ISO 29301:2010, Microbeam analysis Analytical transmission electron microscopy Methods for calibrating image magnification by using reference materials hav
48、ing periodic structures 17 ISO/TR 27628:2007, Workplace atmospheres Ultrafine, nanoparticle and nano-structured aerosols Inhalation exposure characterization and assessment 18 EN 13925-3:2005, Non-destructive testing X-ray diffraction from polycrystalline and amorphous materials Part 3: Instruments4 ISO 2012 All rights reserved ISO/TS 11937:2012(E) ISO 2012 All rights reserved IC S 07.030 Price based on 4 pages
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