DIN EN ISO 17751-2-2016 Textiles - Quantitative analysis of cashmere wool other specialty animal fibers and their blends - Part 2 Scanning Electron Microscopy method (ISO 17751-2 2.pdf

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1、November 2016 English price group 21No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS 59.060.10www.din.deDIN EN ISO 1

2、7751-2Textiles Quantitative analysis of cashmere, wool, other specialty animal fibers and their blends Part 2: Scanning Electron Microscopy method (ISO 177512:2016);English version EN ISO 177512:2016,English translation of DIN EN ISO 17751-2:2016-11Textilien Quantitative Analyse von Kaschmir, Wolle,

3、 anderen speziellen tierischen Fasern und deren Mischungen Teil 2: RasterelektronenmikroskopieVerfahren (ISO 177512:2016);Englische Fassung EN ISO 177512:2016,Englische bersetzung von DIN EN ISO 17751-2:2016-11Textiles Analyse quantitative du cachemire, de la laine, dautres fibres animales spciales

4、et leurs mlanges Partie 2: Mthode par microscopie lectronique balayage (ISO 177512:2016);Version anglaise EN ISO 177512:2016,Traduction anglaise de DIN EN ISO 17751-2:2016-11www.beuth.deDocument comprises 55 pagesDTranslation by DIN-Sprachendienst.In case of doubt, the German-language original shall

5、 be considered authoritative.10.16!%YJ“2585439 DIN EN ISO 17751-2:2016-11 2 A comma is used as the decimal marker. National foreword This document (EN ISO 17751-2:2016) has been prepared by Technical Committee ISO/TC 38 “Textiles” in collaboration with Technical Committee CEN/TC 248 “Textiles and te

6、xtile products” (Secretariat: BSI, United Kingdom). The responsible German body involved in its preparation was DIN-Normenausschuss Materialprfung (DIN Standards Committee Materials Testing), Working Committee NA 062-05-21 AA Physikalisch-technologische Prfverfahren fr Textilien. EUROPEAN STANDARD N

7、ORME EUROPENNE EUROPISCHE NORM EN ISO 17751-2 April 2016 ICS 59.060.10 English Version Textiles - Quantitative analysis of cashmere, wool, other specialty animal fibers and their blends - Part 2: Scanning Electron Microscopy method (ISO 17751-2:2016) Textiles - Analyse quantitative du cachemire, de

8、la laine, dautres fibres animales spciales et leurs mlanges - Partie 2: Mthode par microscopie lectronique balayage (ISO 17751-2:2016) Textilien - Quantitative Analyse von Kaschmir, Wolle, anderen speziellen tierischen Fasern und deren Mischungen - Teil 2: Rasterelektronenmikroskopie-Verfahren (ISO

9、17751-2:2016) This European Standard was approved by CEN on 13 December 2015. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibl

10、iographical references concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the respon

11、sibility of a CEN member into its own language and notified to the CEN-CENELEC Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Repu

12、blic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey andUnited Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMAL

13、ISATION 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. EN ISO 17751-2:2016 EEuropean foreword .3Introduction 51 Scope . 62 Terms and

14、 definitions .63 Principle 74 Apparatus, materials, and reagents 74.1 Apparatus 74.2 Materials . 74.3 Reagents 85 Sample drawing . 86 Preparation of test specimens 86.1 Number of test specimens . 86.2 Preparation method for test specimens of various types of samples 86.2.1 Loose fibre . 86.2.2 Slive

15、r . 96.2.3 Yarn 96.2.4 Woven fabrics 106.2.5 Knitted fabrics . 106.3 Coating the specimens . 107 Test procedure . 107.1 Test on each specimen stub 107.2 Qualitative analysis (purity analysis) and determination of fibre content 108 Calculation of test result 11Annex A (informative) Drawing of lot sam

16、ple and laboratory sample 12Annex B (informative) Surface morphology of common animal fibres . 13Annex C (normative) Density of common animal fibres .52Bibliography .53Contents Page2DIN EN ISO 17751-2:2016-11 EN ISO 17751-2:2016 (E) Foreword 4European foreword This document (EN ISO 17751-2:2016) has

17、 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. This European Standard shall be given the status of a national standard, either by publication of an identical text

18、 or by endorsement, at the latest by October 2016, and conflicting national standards shall be withdrawn at the latest by October 2016. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN and/or CENELEC shall not be held responsib

19、le for identifying any or all such patent rights. According to the CEN-CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland,

20、Former Yugoslav Republic 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 the United Kingdom. Endorsement notice The text of ISO 17

21、751-2:2016 has been approved by CEN as EN ISO 17751-2:2016 without any modification. 3DIN EN ISO 17751-2:2016-11 EN ISO 17751-2:2016 (E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing I

22、nternational 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, governmental and non-governmental, in liaison

23、 with ISO, also take part in the work. ISO 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 Directi

24、ves, Part 1. In particular the different 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

25、of the elements of this document may be 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 declarati

26、ons received (see www.iso.org/patents).Any 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

27、ISOs adherence to the WTO principles in the Technical Barriers to Trade (TBT) see the following URL: Foreword - Supplementary informationThe committee responsible for this document is ISO/TC 38, Textiles.ISO 17751 consists of the following parts, under the general title Textiles Quantitative analysi

28、s of cashmere, wool, other speciality animal fibres and their blends: Part 1: Light microscopy method Part 2: Scanning electron microscopy method4DIN EN ISO 17751-2:2016-11 EN ISO 17751-2:2016 (E) IntroductionCashmere is a high value speciality animal fibre, but cashmere and other animal wool fibres

29、 such as sheeps wool, yak, camel, etc. exhibit great similarities in their physical and chemical properties so that their blends are difficult to distinguish from each other by both mechanical and chemical methods. In addition, these fibres show similar scale structures. It is very difficult to accu

30、rately determine the fibre content of such fibre blends by current testing means.Research on the accurate identification of cashmere fibres has been a long undertaking. At present, the most widely used and reliable identification techniques include the light microscopy (LM) method and the scanning e

31、lectron microscopy (SEM). The SEM method shows complementary characteristics to those of LM method. The advantage of the LM method is that the internal medullation and pigmentation of fibres can be observed; the disadvantage is that some subtle surface structures cannot be clearly displayed. A decol

32、ouring process needs to be carried out on dark samples for testing. An improper decolouring process can affect the judgment of the fibre analyst. The SEM method shows opposite characteristics to those of LM method so some types of fibres need to be identified by scanning electron microscope. The LM

33、and SEM methods need be used together to identify some difficult-to-identify samples in order to utilize the advantages of both methods.It has been proven in practice that the accuracy of a fibre analysis is highly related to the ample experience, full understanding, and extreme familiarity of the f

34、ibre analyst to the surface morphology of various types of animal fibres so besides the textual descriptions, several micrographs of different types of animal fibres are given in Annex B.5DIN EN ISO 17751-2:2016-11 EN ISO 17751-2:2016 (E)1 ScopeThis part of ISO 17751 specifies a method for the ident

35、ification, qualitative, and quantitative analysis of cashmere, wool, other speciality animal fibres, and their blends using scanning electron microscopy (SEM).This part of ISO 17751 is applicable to loose fibres, intermediate products, and final products of cashmere, wool, other speciality animal fi

36、bres, and their blends.2 Terms and definitionsFor the purposes of this document, the following terms and definitions apply.2.1specialty animal fibreany type of keratin fibre taken from animal (hairs) other than sheep2.2scanning electron microscopeintermediate type of microscopic morphology observati

37、on instrument between transmitted electron microscope and light microscope which use a focused beam of high-energy electrons to generate a variety of physical information signalsNote 1 to entry: The principle consists of scanning a primary focused electron beam over a whole area of interest on the s

38、urface of solid specimen and the signal derived from which is then received, amplified, and displayed in images for full observation of surface area topography of the specimen.Note 2 to entry: The signals obtained by a scanning electron microscope are, e.g. secondary electrons (2.3), Auger electrons

39、, characteristic X-ray, etc.2.3secondary electronlow-energy extra-nuclear electron released from and by ionization of a metal atom in the 5 nm to 10 nm scanned region of metal layer less than 10 nm thick nearest to the outermost meta-coated surface of a specimen under impact of the focused primary e

40、lectron beam of energy in units of tens of keVNote 1 to entry: Being surface sensitive because of the small mean free path of the electron to escape from deep within the specimen and, therefore, the signal of which produces the highest-resolution morphological images of the coated surface.2.4scalecu

41、ticle covering the surface of animal fibres2.5scale frequencynumber of scales (2.4) along the fibre axis per unit length6DIN EN ISO 17751-2:2016-11 EN ISO 17751-2:2016 (E) 2.6scale heightheight of the cuticle at the scales (2.4) distal edge2.7fibre surface morphologysum of the physical properties/at

42、tributes characterizing the fibre surfaceEXAMPLE The fibre surface morphology includes scale frequency (2.5), scale height (2.6), patterns of scale edge, scale surface, smoothness, fibre evenness along its axis, transparency under light microscope, etc.2.8lot sampleportion representative of the same

43、 type and same lot of material drawn according to requirements from which it is taken2.9laboratory sampleportion drawn from a lot sample (2.8) according to requirements to prepare specimens2.10test specimenportion taken from fibre snippets randomly cut from a laboratory sample (2.9) for measurement

44、purposes3 PrincipleA longitudinal view image of fibre snippets representative of a test specimen coated with a thin layer of gold is produced by a scanning electron microscope through scanning the side surface of the test specimen with a focused incident beam of high-energy electrons, detecting sign

45、als of secondary electrons emitted by the gold atoms excited when hit by the incident electron beam, and combining the beam position with the detected signals which contain information on surface topography of the test specimen.All fibre types found in the test specimen are identified by comparing t

46、hem with known fibre surface morphologies for different types of animal fibres.For each fibre type, the number and mean diameter of fibre snippets are counted and measured. The mass fraction is calculated from the data for the number of fibre snippets counted, mean value, and standard deviation of t

47、he snippet diameter and the true density of each fibre type.4 Apparatus, materials, and reagents4.1 Apparatus4.1.1 Scanning electron microscope, comprised of a vacuum system, electronic optical system, signal collecting and imaging system, display system, and measurement software.4.1.2 Sputter coate

48、r with a gold cathode.4.2 Materials4.2.1 Microtome.4.2.2 Glass tube, 10 mm to 15 mm in diameter.7DIN EN ISO 17751-2:2016-11 EN ISO 17751-2:2016 (E)4.2.3 Stainless-steel rod, approximately 1 mm in diameter.4.2.4 Glass plate, measuring approximately 150 mm 150 mm.4.2.5 Double-sided adhesive tape.4.2.6

49、 Tweezers, scissors.4.2.7 Specimen stub, aluminium or brass, 13 mm in diameter.4.2.8 Razor blade.4.3 Reagents4.3.1 Acetone (analytical grade) 4.3.2 Ethyl acetate (analytical grade).5 Sample drawingDraw the lot and laboratory samples in accordance with the sampling method given in Annex A.6 Preparation of test specimens6.1 Number of test specimensPrepare five specimen stubs. The fibre snippets on the specimen stubs shall be sufficient to ensure that at least 1