1、 ISO 2012 Nanotechnologies Nanoscale calcium carbonate in powder form Characteristics and measurement Nanotechnologies Carbonate de calcium la nano-chelle sous forme de poudre Caractristiques et mesurage TECHNICAL SPECIFICATION ISO/TS 11931 First edition 2012-12-15 Reference number ISO/TS 11931:2012
2、(E) ISO/TS 11931:2012(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, withou
3、t permission 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 11931:2012(E)
4、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 t
5、echnical 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
6、 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 circulate
7、d to 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 ty
8、pes 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
9、) represents 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
10、, revised 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 ele
11、ments 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 11931 was prepared by Technical Committee ISO/TC 229, Nanotechnologies. ISO 2012 All rights reserved iii ISO/TS 11931:2012(E) Introduction Calcium carbo
12、nate, CaCO 3 , i s w idel y u s e d i n t he p a i nt , i n k , bu i ld i n g , p ap er, ph a r m ac eu t ic a l a nd f o o d i ndu s t r ie s . The applications of this material are expected to increase with the development of nanoscale calcium car b o na te. A c c o rdin gl y , th e re is a n eed
13、to b ette r d e fin e th e c hara cte risti cs o f this ma te ri al c o n tri b u tin g to its performance. This Technical Specification provides methods to determine chemical composition of nanoscale calcium carbonate and three key parameters commonly used to characterize nanoscale calcium carbonat
14、e: average crystallite size, average primary particle size and specific surface area. Calcium carbonate has crystalline structures: calcite, aragonite and vaterite. However, only calcite is widely used in commercial applications. Thus nanoscale calcium carbonate described in this Technical Specifica
15、tion has the calcite crystal structure. There are two kinds of commercial nanoscale calcium carbonate: ground calcium carbonate (GCC) and precipitated calcium carbonate (PCC). These two products have different characteristics such as particle shape and particle size distribution. The buyer and selle
16、r should be aware of the different characteristics required for different applications. X-ray diffraction (XRD) and transmission electron microscopy (TEM) methods are used to measure crystallite size and primary particle size, respectively. The Brunauer, Emmet and Teller (BET) method is used to meas
17、ure specific surface area. Nanotechnology is a rapidly growing and evolving field. Users of this document should maintain an awareness of the legislative environment and latest developments in Environmental Health and Safety regarding nanotechnology. These references may be of interest 1-12 . Respon
18、sibilities of users of this document include the following: the seller is obliged to provide the buyer with such environmental, health and safety information as required by law. If the seller or buyer wish to assess the environmental, safety or health risks of the material, they may refer to ISO/TR
19、12885:2008 7for further guidance. This document may be used in conjunction with other application specific standards developed either by ISO or other standards development bodies.iv ISO 2012 All rights reserved Nanotechnologies Nanoscale calcium carbonate in powder form Characteristics and measureme
20、nt WARNING Persons using this document should be familiar with normal laboratory practice, if applicable. This document does not purport to address 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 a
21、nd to ensure compliance with any regulatory requirements. 1 Scope This Technical Specification provides requirements to describe the basic characteristics of nanoscale calcium carbonate in powder form relevant for applications in nanotechnology. It is intended to detail the material specification ne
22、cessary to use CaCO 3in the applications related to nanotechnology. It does not cover characteristics specific for health and safety issues, and for specific applications of nanoscale CaCO 3 . 2 Normative references The following referenced documents are indispensable for the application of this doc
23、ument. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 3262-1, Extenders for paints Specifications and methods of test Part 1: Introduction and general test methods ISO 9277:2010, Dete
24、rmination of the specific surface area 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 14488, Particulate materials Sampling and sample split ting for the determination of particulate properties ISO
25、 14887, Sample preparation Dispersing procedures for powders in liquids 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, d efinitions and abbr e viat ed t erms For t
26、he purposes of this document, the terms, definitions and abbreviated terms given in ISO/TS 27687, 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 throug
27、h the sample and interacts with it ISO 29301:2010, definition 3.37 TECHNICAL SPECIFICATION ISO/TS 11931:2012(E) ISO 2012 All rights reserved 1 ISO/TS 11931:2012(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 th
28、e electron clouds of atoms in a system produces 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 precipitated calcium carbonate (PCC) a
29、synthetic calcium carbonate, consisting of trigonal crystals (like those of calcite) or rhombic bipyramidal crystals (like those of aragonite) ISO 3262-6:1998, definition 3.1 3.5 ground calcium carbonate (GCC) calcium carbonate produced by grinding (attrition) natural calcium carbonate 3.6 primary p
30、article 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. ISO/TR 27628:2007, definition 2.16 4 Basic characteristics and measurement methods For calcium carbona
31、te 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 listed in Table 1. The requirements for magnitudes of measured characteristics should be agreed up
32、on between interested parties and the test results should be reported complying with the requirement of Clause 6. Table 1 Basic characteristics with corresponding measurement methods Characteristics Unit Measurement methods Mass fraction of calcium carbonate % (kg/kg) Titration method (ISO 3262-1) o
33、r other chemical analysis methods upon the agreement between interested parties Average crystallite size nm XRD (Scherrer formula) 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 cal
34、cium carbonate in powder form in terms of nano size-related features and its main ingredient. NOTE 2 Additional characteristics relevant to specific applications may be specified depending on the intended application and other related international standards.2 ISO 2012 All rights reserved ISO/TS 119
35、31:2012(E) 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 interested parties, the measurement methods should be applied and managed under a well recognized quality system. 5 Sam
36、pling Take a representative sample of the product to be tested, as described in ISO 14488. 6 Reporting The test report shall contain at least the following information: 6.1 Reference to this Technical Specification, i.e. ISO/TS 11931. 6.2 Identification (product name, chemical name). 6.3 Samples des
37、cription (source of nanoscale calcium carbonate, batch number or lot number, country of origin). 6.4 Laboratory (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 particl
38、es used in the determination of the average size, standard deviation of measurement results and details 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 re
39、served 3 ISO/TS 11931:2012(E) Bibliography 1 CAN/CSA-Q850-97 Risk Management: Guideline for Decision makers 2 Consumer Product Safety Commission. Handbook for Manufacturing Safer Consumer Products. July2006, www.cpsc.gov/businfo/intl/handbookenglishaug05.pdf 3 C o n s u m e r P r o d u c t S a f e t
40、 y C o m m i s s i o n . R e c a l l h a n d b o o k , M a y 1 9 9 9 , w w w . c p s c . gov/BUSINFO/8002.html 4 EC. Guidelines for the notification of Dangerous Consumer Products to the Competent Authorities of the Member States by Producers and Distributors in Accordance with Article 5(3) of Direc
41、tive 2001/95/EC ec.europa.eu/consumers/cons_safe/prod_safe/guidelines_documents.pdf 5 European Commission. Risk Assessment Guidelines for non-food Consumer Products, Draft for Consultation, August 2008. http:/ /ec.europa.eu/consumers/ ipm/risk_assesment_guidelines_non_food.pdf 6 IECs Advisory Commit
42、tee on Safety Development of a standard for safety related risk assessment in the area of low voltage 7 ISO/TR 12885:2008, Nanotechnologies Health and safety practices in occupational settings relevant to nanotechnologies 8 ISO/IEC Guide 51 Safety aspects Guidelines for their inclusion in standards
43、9 ISO/IEC Guide 50 Safety aspects Guidelines for child safety 10 ISO/IEC Guide 71 Guidelines for standards developers to address the needs of older persons and persons with disabilities 11 ISO Guide 73 Risk management Vocabulary 12 Stancert, Product Safety Framework, 13 EN 13925-1:2003, Non-destruc
44、tive testing X-ray diffraction from polycrystalline and amorphous materials Part 1:General principles 14 EN 13925-2:2003, Non-destructive testing X-ray diffraction from polycrystalline and amorphous materials Part 2:Procedures 15 EN 13925-3:2005, Non destructive testing X ray diffraction from polycr
45、ystalline and amorphous materials Part 3:Instruments 16 Savitzky A.,Golay M., Smoothing and differentiation data by simplified least squares procedures. Analytical Chemistry, 36(8), 1964, pp. 16271639 17 Rachinger W . A . A C o r r e c t i o n f o r t h e 1 2Doublet in the Measurement of Widths of X
46、-ray Diffraction Lines. J. Sci. Instrum., 25 (7), 1948, pp. 254259 18 Jones, F.W. The Measurement of Particle Size by the X-Ray Method, Proc. Roy. Soc. London, Series A, 166(924), 1938, pp. 1648 19 Taurozzi J . S . , H ackley V . A . , W iesner M.R. Ultrasonic dispersion of nanoparticles for environ
47、mental, health and safety assessment-issues and recommendations. Nanotoxicology, 5(4), 2011, pp. 711729 20 ISO 3262-6:1998, Extenders for paints Specifications and methods of test Part 6: Precipitated calcium carbonate4 ISO 2012 All rights reserved ISO/TS 11931:2012(E) 21 ISO 18757:2003, Fine cerami
48、cs (advanced ceramics, advanced technical ceramics) Determination of specific surface area of ceramic powders by gas adsorption using the BET method 22 ISO/TR 27628:2007, Workplace atmospheres Ultrafine, nanoparticle and nano-structured aerosols Inhalation exposure characterization and assessment 23
49、 ISO/TS 11937, Nanotechnologies Nanoscale titanium dioxide in powder form Characteristics and measurement 24 ISO 29301:2010, Microbeam analysis Analytical transmission electron microscopy Methods for calibrating image magnification by using reference materials having periodic structures ISO 2012 All rights reserved 5 ISO/TS 11931:2012(E) ISO 2012 All rights reserved IC S 07.03
