1、Textiles Composition testing Identification of fibres (ISO/TR 11827:2012)PD CEN ISO/TR 11827:2016BSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06National forewordThe UK participation in its preparation was entrusted to Technical Committee TCI/100, Co-ordination of ac
2、tivities in textiles and clothing.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 application. The British Standards Instit
3、ution 2016. Published by BSI Standards Limited 2016ISBN 978 0 580 93121 5ICS 59.060.01Compliance with a British Standard cannot confer immunity from legal obligations.This Published Document was published under the authority of the Standards Policy and Strategy Committee on 30 June 2012.Amendments/c
4、orrigenda issued since publicationDate T e xt affectedPUBLISHED DOCUMENTPD CEN ISO/TR 11827:201630 June 2016 This corrigendum renumbers PD ISO/TR 11827:2012 as PD CEN ISO/TR 11827:2016This Published Document is the UK implementation of CEN ISO/TR 11827:2016. It is identical to ISO/TR 11827:2012. It
5、supersedes PD ISO/TR 11827:2012 which is withdrawn.TECHNICAL REPORT RAPPORT TECHNIQUE TECHNISCHER BERICHT CEN ISO/TR 11827 June 2016 ICS 59.060.01 English Version Textiles - Composition testing - Identification of fibres (ISO/TR 11827:2012) Textiles - Essai de composition - Identification des fibres
6、 (ISO/TR 11827:2012) This Technical Report was approved by CEN on 22 May 2016. It has been drawn up by the Technical Committee CEN/TC 248. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic
7、 of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISA
8、TION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2016 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. CEN ISO/TR 11827:2016 EEuropean foreword This document (CEN ISO/TR 11827:2016) h
9、as been prepared by Technical Committee ISO/TC 38 “Textiles” in collaboration with Technical Committee CEN/TC 248 “Textiles and textile products” the secretariat of which is held by BSI. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rig
10、hts. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. Endorsement notice The text of ISO/TR 11827:2012 has been approved by CEN as CEN ISO/TR 11827:2016 without any modification. iiPD CEN ISO/TR 11827:2016 CEN ISO/TR 11827:2016 (E)ISO/TR 11827:2012(E) I
11、SO 2012 All rights reserved iiiContents Page Foreword iv Introduction.v 1 Scope1 2 Safety note .1 3 Normative references2 4 Terms and definitions .2 5 Principle2 6 Apparatus and preparation of solutions.3 6.1 Apparatus.3 6.2 Preparation of solutions .3 7 Techniques.4 7.1 Microscopy.4 7.2 Flame tests
12、.6 7.3 Staining Tests 7 7.4 Solubility Tests 7 7.5 Infrared Spectroscopy 8 7.6 Thermal Analysis.12 7.7 Density measurement methods .14 7.8 Other Instrumental Methods.14 8 Examples of procedures.15 8.1 Procedure using microscopy, solubility tests and FT-IR tests (examples) 15 8.2 Procedure using solu
13、bility tests (examples)17 8.3 Procedure using combustion tests and melting point determination (example) .19 8.4 Procedure using microscopy, FT-IR analysis and thermal analysis, case of bicomponent fibres (examples) .19 Annex A (informative) Characteristics relative to fibre identification testing 2
14、4 Annex B (informative) Photomicrographs of Fibres (Light Microscopy) 29 Annex C (informative) Scanning Electron Micrographs of Fibres .34 Annex D (informative) Solubility of fibres 42 Annex E (informative) Examples of Infrared Spectra 45 Annex F (informative) Thermal transition temperature.50 Annex
15、 G (informative) Density.54 Annex H (informative) Alphabetical index of figures 55 Bibliography57 PD CEN ISO/TR 11827:2016ISO/TR 11827:2012(E) iv ISO 2012 All rights reservedForeword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO
16、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, govern
17、mental 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. International Standards are drafted in accordance with the rules given in the ISO/IEC Di
18、rectives, Part 2. The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member b
19、odies casting a vote. In exceptional circumstances, when a technical committee has collected data of a different kind from that which is normally published as an International Standard (“state of the art”, for example), it may decide by a simple majority vote of its participating members to publish
20、a Technical Report. A Technical Report is entirely informative in nature and does not have to be reviewed until the data it provides are considered to be no longer valid or useful. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. I
21、SO shall not be held responsible for identifying any or all such patent rights. ISO/TR 11827 was prepared by Technical Committee ISO/TC 38, Textiles. PD CEN ISO/TR 11827:2016ISO/TR 11827:2012(E) ISO 2012 All rights reserved vIntroduction The correct identification of fibres in textiles and the accur
22、ate determination of the composition of each fibre present is a legal requirement in many countries throughout the world for imported textile goods and at the point of sale to the public. Fibre identification can be carried out by a number of different techniques, e.g. microscopy, solubility, spectr
23、oscopy, melting point, pyrolysis, density, refractive index, etc. PD CEN ISO/TR 11827:2016This page deliberately left blankTECHNICAL REPORT ISO/TR 11827:2012(E) ISO 2012 All rights reserved 1Textiles Composition testing Identification of fibres IMPORTANT The electronic file of this document contains
24、 colours which are considered to be useful for the correct understanding of the document. Users should therefore consider printing this document using a colour printer. 1 Scope This Technical Report describes procedures for the identification of natural and man-made fibres, and may be used, when nec
25、essary, to coordinate with methods for the quantitative analysis of fibre blends. Textile FibresNatural fibresAnimal fibresAnimal HairsWool (Sheep)Cash me r e , M o h ai r (Goat)Alpaca, Guanaco, Vicuna (Llama)Angor a (Rabbit)Other fibresSecretion fibresSi l k Other fibresVegetable fibresFrom SeedCot
26、tonKapokOther fibresFr om St e mFl axHempRami eJu t eOther fibresFr om l eafSi salAlfaOther fibresFr o m Fr u i tCo i rOther fibresMineral fibresAsbestosMan-made fibresFr om organic chemistry Synthetic fibresAcrylic, ModacrylicCh l o r o f i b r eFl u or of i br ePolyamidePolyest erAramidPolyimidePo
27、lyethylenePolypropylenePolylactideEl ast an eElastodieneElastolefinMelaminePolycarbamideTr i vi nylEl ast o m u l t i e st e rPolypropylene/Polyamide-bicomponentOther fibresArtificial fibresFrom celluloseViscose, CuproModal, LyocellAcetate, TriacetateOther fibresOthersElastodiene(from latex)Protein
28、fibresAlginateOther fibresFr om inorganic chemistryGl assMetallic fibresCe r ami csCar b o nOther fibresFigure 1 Classification of the textile fibres in relation to their origin 2 Safety note This Technical Report calls for the use of substances/procedures that may be injurious to the health/ enviro
29、nment if appropriate conditions are not observed. It refers only to technical suitability and does not absolve the user from legal obligations relating to health and safety/environment at any stage. PD CEN ISO/TR 11827:2016ISO/TR 11827:2012(E) 2 ISO 2012 All rights reserved3 Normative references The
30、 following referenced documents are indispensable for the application 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 1833-4, Textiles Quantitative chemical analysis
31、Part 4: Mixtures of certain protein and certain other fibres (method using hypochlorite) ISO 2076, Textiles Man-made fibres Generic names ISO 6938, Textiles Natural fibres Generic names and definitions 4 Terms and definitions For the purposes of this document, the following terms and definitions giv
32、en in ISO 2076 and ISO 6938 and the following apply. 4.1 natural fibre fibre which occurs in nature: it can be categorized according to its origin into animal, vegetable and mineral fibre 4.2 man-made fibre manufactured fibre fibre obtained by a manufacturing process 4.2.1 artificial fibre manufactu
33、red fibre made by transformation of natural polymers (macromolecular material existing in nature) 4.2.2 synthetic fibre manufactured fibre made from synthetic polymers (macromolecular material which has been chemically synthesised) 4.2.3 bicomponent fibre fibre composed of two fibres forming polymer
34、 components, which are chemically or physically different or both 5 Principle Objective: identify the fibres Means: based on fibre properties (single or combination) Properties for example: Morphology Solubility Light absorption or transmission by IR Burning behaviour Thermal behaviour PD CEN ISO/TR
35、 11827:2016ISO/TR 11827:2012(E) ISO 2012 All rights reserved 3 Colouration Optical behaviour Elemental composition 6 Apparatus and preparation of solutions 6.1 Apparatus 6.1.1 Light Microscope, using transmitted light 6.1.2 Scanning Electron Microscope 6.1.3 Bunsen Burner or other flame source 6.1.4
36、 Infrared Spectrometer 6.1.4.1 Attenuated Total Reflection (ATR) spectroscopy device 6.1.4.2 Fourier Transform Infrared (FT-IR) spectrometer 6.1.5 Melting Point device (heated block) 6.1.6 Differential Scanning Calorimeter (DSC) 6.1.7 Thermal Gravimetric Analysis (TGA) device (thermobalance) 6.1.8 G
37、ravimetric device (density gradient column) 6.1.9 Energy Dispersive X-ray (EDX) device 6.2 Preparation of solutions Use only reagents of recognized analytical grade. 6.2.1 Sodium hydroxide and calcium oxide Prepare a mixture of sodium hydroxide and calcium oxide (mass ratio of 1:1,4) 6.2.2 Iodine/po
38、tassium iodine solution Dissolve 20 g of potassium iodide in 20 ml to 50 ml of distilled water. In this solution dissolve 2,5 g of iodine and dilute to 100 ml 6.2.3 Zinc chloride/iodine solution Dissolve 66 g of zinc chloride, anhydrous, and 6 g of potassium iodide in 34 ml of water. Add a small amo
39、unt of iodine crystal so that the solution is saturated. 6.2.4 Chlorine bleaching solution Prepare the solution according to ISO 1833-4. 6.2.5 Zinc chloride/formic acid solution Dissolve 100 g of zinc chloride, anhydrous in 100 ml of water. PD CEN ISO/TR 11827:2016ISO/TR 11827:2012(E) 4 ISO 2012 All
40、 rights reservedSet the density of this solution to 1,566 g/ml. Add 6 ml of concentrated formic acid to 100 ml of this solution. 6.2.6 Sodium carbonate 0,25 % solution Add 0,25 g of sodium carbonate to 100 ml of distilled water and dissolve. 6.2.7 Sodium hydroxide 5 % solution Dissolve 5 g of sodium
41、 hydroxide in distilled water and dilute to 100 ml. 6.2.8 Sulphuric acid 75 % solution Add carefully, while cooling, 700 ml of concentrated sulphuric acid ( 1,84 g/ml) to 350 ml of distilled water. After the solution has cooled to room temperature, dilute to 1 l with water. 6.2.9 Chloroform/trichlor
42、oacetic acid solution Dissolve 50 g of trichloroacetic acid in 50 g of chloroform. 6.2.10 Ethanol / potassium hydroxide solution Dissolve 15 g of potassium hydroxide in 100 ml of ethanol. 7 Techniques 7.1 Microscopy 7.1.1 Light Microscopy Examine the longitudinal view and/or the cross section of a f
43、ibre sample under a light microscope (6.1.1) using transmitted light and magnification. Compare with photomicrographs in Annex B. 7.1.2 Scanning Electron Microscopy Examine the longitudinal view and/or the cross section of the surface of a fibre sample under a scanning electron microscope (6.1.2) us
44、ing magnification. Compare with photomicrographs in Annex C. 7.1.3 Refractive Index 7.1.3.1 General Refractive index governs the visibility of all colourless and transparent objects. When a fibre is examined in air (n=1,0), the relatively large difference in refractive index between the fibre and ai
45、r causes about 5 % of the incident light to be reflected and the transmitted light to be markedly refracted. These effects produce heavy shadows that obscure fine details of the fibre structure and can introduce misleading identification. To reduce the degree of contrast in the shadow regions the fi
46、bres are mounted in a medium of suitable refractive index for microscopic evaluation. PD CEN ISO/TR 11827:2016ISO/TR 11827:2012(E) ISO 2012 All rights reserved 57.1.3.2 Mounting media If fibres are mounted in a medium of similar refractive index, surface characteristics are practically invisible but
47、 internal structure and the presence of voids, or inclusions such as pigmentation, are clearly revealed. When it is desired to examine the surface details of a fibre a mounting medium of significantly different refractive index should be selected, preferably one with a much higher refractive index t
48、han that of the fibre, e.g. 1-bromonapthalene or di-iodo-methane. Mountants should be relatively stable, and should not be volatile or react with the polymer fibre. The most commonly used mountant is liquid paraffin which gives an image of satisfactory contrast for all fibres except for cellulose di
49、acetate and triacetate, for which n-decane is recommended. It is recommended that all fibres be examined as soon after mounting as possible. Some fibres if left for a period may be penetrated by the mountant, or they may swell which makes fibre diameter measurements incorrect, or the mountant may evaporate. 7.1.3.3 Factors governing refractive indices Factors governing the refractive index of fibres are the chemical nature of the molecules, the physical arrangement of these molecules, the wavelength of incident l
