1、BSI Standards PublicationBS ISO 18473-1:2015Functional pigments andextenders for specialapplicationsPart 1: Nanoscale calcium carbonate forsealant applicationBS ISO 18473-1:2015 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 18473-1:2015.The UK participation i
2、n its preparation was entrusted to TechnicalCommittee STI/1, Pigments.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does not purport to include all the necessaryprovisions of a contract. Users are responsible for its correctapplicat
3、ion. The British Standards Institution 2015. Published by BSI StandardsLimited 2015ISBN 978 0 580 86236 6ICS 87.060.10Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of theStandards Policy and Strategy Committee
4、on 31 August 2015.Amendments issued since publicationDate Text affectedBS ISO 18473-1:2015 ISO 2015Functional pigments and extenders for special applications Part 1: Nanoscale calcium carbonate for sealant applicationPigments et matires de charges fonctionnels pour applications spciales Partie 1: Ca
5、rbonate de calcium nanomtrique pour les enduitsINTERNATIONAL STANDARDISO18473-1First edition2015-08-15Reference numberISO 18473-1:2015(E)BS ISO 18473-1:2015ISO 18473-1:2015(E)ii ISO 2015 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2015, Published in SwitzerlandAll rights reserved. Unless oth
6、erwise specified, 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
7、 below or ISOs member body in the country of the requester.ISO copyright officeCh. de Blandonnet 8 CP 401CH-1214 Vernier, Geneva, SwitzerlandTel. +41 22 749 01 11Fax +41 22 749 09 47copyrightiso.orgwww.iso.orgBS ISO 18473-1:2015ISO 18473-1:2015(E)Foreword ivIntroduction v1 Scope . 12 Normative refer
8、ences 13 Terms and definitions . 14 Requirements and test methods 25 Sampling 36 Determination of whiteness . 36.1 Apparatus 36.2 Procedure 36.2.1 Sample preparation . 36.2.2 Calibration of the apparatus 46.2.3 Determination 46.2.4 Calculation of whiteness . 47 Marking and label 48 Test report . 4Bi
9、bliography 5 ISO 2015 All rights reserved iiiContents PageBS ISO 18473-1:2015ISO 18473-1:2015(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carri
10、ed 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. I
11、SO 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
12、 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
13、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).A
14、ny trade name used in this document 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
15、the Technical Barriers to Trade (TBT) see the following URL: Foreword - Supplementary informationThe committee responsible for this document is ISO/TC 256, Pigments, dyestuffs and extenders.ISO 18473 consists of the following parts, under the general title Functional pigments and extenders for speci
16、al applications: Part 1: Nanoscale calcium carbonate for sealant application Part 2: Nanoscale titanium dioxide for sunscreen applicationiv ISO 2015 All rights reservedBS ISO 18473-1:2015ISO 18473-1:2015(E)IntroductionSealants are widely used to prevent the penetration of air, gas, or liquid in many
17、 industries including construction, automobile, and electronics. Extenders are essential part of sealant formulation to reduce cost and improve their rheological and mechanical properties. Content of extenders vary significantly and can be as high as 50 % (mass fraction). The most common extender in
18、 sealants is calcium carbonate (CaCO3) because it is readily available and comes in various sizes which act as a rheological modifier, a reinforcing agent, and opacifier. Commercial calcium carbonate can be divided into ground calcium carbonate (GCC) and precipitated calcium carbonate (PCC), possess
19、es three crystal structures including calcite, aragonite, and vaterite, and exists in various morphologies such as cubic, spherical, spindle, fibrous, needle-like, etc. Calcium carbonates with calcite crystal structure and cubic or spherical morphology are most widely used in sealant applications.Na
20、noscale calcium carbonate (NCC) provides various sealants with improved performance and additional functionalities including thixotropy, flame resistance and improved durability and recyclability, and has become a major component in sealant formulation. Nanoscale calcium carbonate in the powdered fo
21、rm is readily manufactured nowadays, mostly through precipitation route to control the size and morphology. Surface treatment is crucial for utilizing NCC in sealants. Native CaCO3is hydrophilic. As a result, it tends to agglomerate in organic polymers and plasticizers. NCC, in particular, has a gre
22、ater propensity for agglomeration because of its small size and large specific surface area. NCCs are surface treated to render them hydrophobic and improve their dispersibility in hydrophobic systems. Surface treatment also improves polymer matrix compatibility, thus improving interfacial adhesion
23、between extender and polymer.It has been found that the particle size, specific surface area, mass fraction, morphology, pH value, magnesium content, oil absorption value, moisture content, and other characteristics of supplied nanoscale calcium carbonate all have impact on the performance of the se
24、alant incorporating these nanoparticles. The need to specify the characteristics of NCC which relate to sealant performance comes from the following facts. First, the agreements between customers and suppliers do not always cover all material characteristics that have influences on performance and/o
25、r processability of sealants or they have been interpreted differently by the customers and suppliers. Second, nanomaterials are relatively new. Material properties can depend on the techniques to measure them. Therefore, providing information regarding characteristics of nanoscale calcium carbonate
26、 in sealants will facilitate the communication between customers and suppliers.This part of ISO 18473 lists the properties, measurements, and characteristics of nanoscale calcium carbonate and intents to aid its acceptance and application in sealants. ISO 2015 All rights reserved vBS ISO 18473-1:201
27、5BS ISO 18473-1:2015Functional pigments and extenders for special applications Part 1: Nanoscale calcium carbonate for sealant application1 ScopeThis part of ISO 18473 specifies requirements and corresponding methods of test for surface treated nanoscale calcium carbonate in powder form for sealant
28、application.2 Normative referencesThe following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (includin
29、g any amendments) applies.ISO 787-2, General methods of test for pigments and extenders Part 2: Determination of matter volatile at 105 CISO 787-5, General methods of test for pigments and extenders Part 5: Determination of oil absorption valueISO 787-9, General methods of test for pigments and exte
30、nders Part 9: Determination of pH value of an aqueous suspensionISO 3262-1, Extenders for paints Specifications and methods of test Part 1: Introduction and general test methodsISO 3262-6, Extenders for paints Specifications and methods of test Part 6: Precipitated calcium carbonateISO 9277, Determi
31、nation of the specific surface area of solids by gas adsorption BET methodISO 15528, Paints, varnishes and raw materials for paints and varnishes Sampling3 Terms and definitionsFor the purposes of this part of ISO 18473, the following terms and definitions apply.3.1nanoscalesize range from approxima
32、tely 1 nm to 100 nmNote 1 to entry: Properties that are not extrapolations from a larger size will typically, but not exclusively, be exhibited in this size range. For such properties, the size limits are considered approximate.Note 2 to entry: The lower limit in this definition (approximately 1 nm)
33、 is introduced to avoid single and small groups of atoms from being designated as nano-objects or elements of nanostructures which can be implied by the absence of a lower limit.SOURCE: ISO/TS 80004-2:2015, 2.1INTERNATIONAL STANDARD ISO 18473-1:2015(E) ISO 2015 All rights reserved 1BS ISO 18473-1:20
34、15ISO 18473-1:2015(E)3.2precipitated calcium carbonatesynthetic calcium carbonate consisting of trigonal crystals (like those of calcite) or rhombic bipyramidal crystals (like those of aragonite)SOURCE: ISO 3262-6:1998, 3.14 Requirements and test methodsNanoscale calcium carbonate (powdered form) ap
35、plied for industrial use of sealant shall comply with the requirements specified in Table 1.Table 1 Requirements for nanoscale CaCO3used in sealantCharacteristic/Property Unit Requirement Test methodAverage crystal size, mass basedanm 100 XRDbmethodMedian particle size by mass distribution (particle
36、 size distribution is optional)anmcCentrifuge methoddMedian particle size by number distribution (particle size distribution is optional)anmcTEMemethodSpecific surface area (BET)fm2/g 16 ISO 9277Mass fraction of calcium carbonate% (mass fraction) 85 ISO 3262-1Insoluble residue in hydrochloric acid%
37、(mass fraction) 0,5gISO 3262-6MgCO3content % (mass fraction)To be agreed between the interested parties (if there is no agreement, it is not necessary to measure)ISO 3262-1DINPdor linseed oil absorptionml/100 g 23 ISO 787-5Moisture % (mass fraction)To be agreed between the interested partiesISO 787-
38、2Whiteness To be agreed between the interested partiesClause 6pH value To be agreed between the interested partiesISO 787-9aCharacteristic for particle size to be agreed between the interested parties.bXRD X-ray diffraction.cA requirement can only be fixed as soon as a standardized test method is av
39、ailable.dStandard under development.eTEM Transmission electron microscopy.fBET Brunauer-Emmett-Teller.gThe insoluble residue content is measured with the untreated CaCO3.2 ISO 2015 All rights reservedBS ISO 18473-1:2015ISO 18473-1:2015(E)Characteristic/Property Unit Requirement Test methodAmount of
40、organic treatment and general chemical type (surface treatment)% (mass fraction)To be agreed between the interested partiesTo be agreed between the interested partiesaCharacteristic for particle size to be agreed between the interested parties.bXRD X-ray diffraction.cA requirement can only be fixed
41、as soon as a standardized test method is available.dStandard under development.eTEM Transmission electron microscopy.fBET Brunauer-Emmett-Teller.gThe insoluble residue content is measured with the untreated CaCO3.NOTE The crystal type and particle shape are important, but not required for decision f
42、or a nanoscale material or not.5 SamplingTake a representative sample of the product to be tested as described in ISO 15528. Sample preparation shall always be carried out consistently so that repeated preparations based on replicate samples of a batch of powder (which was carefully mixed before bei
43、ng sampled or subdivided into samples) give closely comparable results.6 Determination of whiteness6.1 ApparatusUse ordinary laboratory apparatus and glassware together with the following.6.1.1 Whiteness photometer or colour photometer.The apparatus shall have the following characteristics:a) wavele
44、ngth range from 380 nm to 780 nm, shall not exceed the range of 400 nm to 700 nm;b) halfwidth of wavelength: the half-width of wave emitted from exit slit of the photometer shall be in the range of 10 nm;c) luminous accuracy shall be in the 0,5 % of the full-scale luminous range;d) deviation between
45、 the nominal wavelength and actual wavelength shall not exceed 0,5 nm.6.1.2 Powder sample press.6.2 Procedure6.2.1 Sample preparationPlace a quantity of sample into the pressing sampling implement and press it into a surfacing sample board without veining, staining, and spotting. Three sample boards
46、 shall be pressed for each batch of products.Table 1 (continued) ISO 2015 All rights reserved 3BS ISO 18473-1:2015ISO 18473-1:2015(E)6.2.2 Calibration of the apparatusCalibrate with a date transfer standard white plate as a working standard white plate (use MgO as white plate), then preheat the appa
47、ratus according to the operating instruction manual. Zero and calibrate the apparatus with the working standard white plate.6.2.3 DeterminationPlace three sample boards on the measured hole and measure the tristimulus value X10, Y10, Z10for each board. Take the mean of determinations for the three s
48、ample boards as the result.6.2.4 Calculation of whitenessThe whiteness (R457) is given by the following formulae:xXXYZ101010 10 10=+(1)yYXYZ101010 10 10=+(2)zxyZXYZ10 10 101010 10 101= =+(3)whereX10, Y10, Z10are the tristimulus values for the 10 observer;x10, y10, z10are the chromaticity coordinates
49、 of the sample.Take the mean of parallel determinations as the result and make sure the absolute dispersion of parallel determinations is less than 0,5.7 Marking and labelThe outer packing shall clearly mark in a visible location the manufacturer name and address, product name, type, brand, net weight and batch number or production date, this ISO standard number, and a “store dry” mark.8 Test reportThe test report shall contain at least the following information:a) all information necessary to completely
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