EN ISO 17751-2-2016 en Textiles - Quantitative analysis of cashmere wool other specialty animal fibers and their blends - Part 2 Scanning Electron Microscopy method《纺织品-羊绒 羊毛的定量分析 .pdf

1、BSI Standards PublicationBS EN ISO 17751-2:2016T e x t i l e s Q u a n t i t a t i v eanalysis of cashmere, wool,other specialty animal fibersand their blendsPart 2: Scanning Electron MicroscopymethodBS EN ISO 17751-2:2016 BRITISH STANDARDNational forewordThis British Standard is the UK implementati

2、on of EN ISO17751-2:2016.The UK participation in its preparation was entrusted to TechnicalCommittee TCI/80, Chemical testing of textiles.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does not purport to include all the necessarypro

3、visions of a contract. Users are responsible for its correctapplication. The British Standards Institution 2016.Published by BSI Standards Limited 2016ISBN 978 0 580 82618 4ICS 59.060.10Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was publishe

4、d under the authority of theStandards Policy and Strategy Committee on 30 April 2016.Amendments issued since publicationDate T e x t a f f e c t e dEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 17751-2 April 2016 ICS 59.060.10 English Version Textiles - Quantitative analysis of cashmere,

5、wool, other specialty animal fibers and their blends - Part 2: Scanning Electron Microscopy method (ISO 17751-2:2016) Textiles - Analyse quantitative du cachemire, de la laine, dautres fibres animales spciales et leurs mlanges - Partie 2: Mthode par microscopie lectronique balayage (ISO 17751-2:2016

6、) Textilien - Quantitative Analyse von Kaschmir, Wolle, anderen speziellen tierischen Fasern und deren Mischungen - Teil 2: Rasterelektronenmikroskopie-Verfahren (ISO 17751-2:2016) This European Standard was approved by CEN on 13 December 2015. CEN members are bound to comply with the CEN/CENELEC In

7、ternal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to a

8、ny CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management Centre has the same status as the official

9、versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norw

10、ay, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey andUnited Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2016 CEN All rights of exploi

11、tation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 17751-2:2016 EBS EN ISO 17751-2:2016EN ISO 17751-2:2016 (E) 3 European foreword This document (EN ISO 17751-2:2016) has been prepared by Technical Committee ISO/TC 38 “Textiles“ in collaboration with Tec

12、hnical 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 or by endorsement, at the latest by October 2016, and conflicting national standard

13、s 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 responsible for identifying any or all such patent rights. According to the CEN-CENELEC Inter

14、nal 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, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ir

15、eland, 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 17751-2:2016 has been approved by CEN as EN ISO 17751-2:2016 without any modification.

16、 BS EN ISO 17751-2:2016ISO 17751-2:2016(E)Foreword ivIntroduction v1 Scope . 12 Terms and definitions . 13 Principle 24 Apparatus, materials, and reagents 24.1 Apparatus 24.2 Materials . 24.3 Reagents 35 Sample drawing . 36 Preparation of test specimens 36.1 Number of test specimens . 36.2 Preparati

17、on method for test specimens of various types of samples 36.2.1 Loose fibre . 36.2.2 Sliver . 46.2.3 Yarn 46.2.4 Woven fabrics . 56.2.5 Knitted fabrics 56.3 Coating the specimens 57 Test procedure 57.1 Test on each specimen stub . 57.2 Qualitative analysis (purity analysis) and determination of fibr

18、e content . 58 Calculation of test result . 6Annex A (informative) Drawing of lot sample and laboratory sample . 7Annex B (informative) Surface morphology of common animal fibres 8Annex C (normative) Density of common animal fibres .47Bibliography .48 ISO 2016 All rights reserved iiiContents PageBS

19、EN ISO 17751-2:2016ISO 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 International Standards is normally carried out through ISO technical committees. Each member body

20、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. ISO collaborates closely with the International Electrotech

21、nical 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 approval criteria needed for the different types of ISO d

22、ocuments 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 the subject of patent rights. ISO shall not be held respon

23、sible 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).Any trade name used in this document is information given f

24、or 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 the Technical Barriers to Trade (TBT) see the following UR

25、L: 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 analysis of cashmere, wool, other speciality animal fibres and their blends: Part 1: Light microscopy met

26、hod Part 2: Scanning electron microscopy methodiv ISO 2016 All rights reservedBS EN ISO 17751-2:2016ISO 17751-2:2016(E)IntroductionCashmere is a high value speciality animal fibre, but cashmere and other animal wool fibres such as sheeps wool, yak, camel, etc. exhibit great similarities in their phy

27、sical 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 accurately determine the fibre content of such fibre blends by current testing mea

28、ns.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 electron microscopy (SEM). The SEM method shows complementary characteristics t

29、o 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 decolouring process needs to be carried out on dark samples for testing. An imprope

30、r 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 and SEM methods need be used together to identify some difficult-to-identify s

31、amples 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 fibre analyst to the surface morphology of various types of animal fibres so be

32、sides the textual descriptions, several micrographs of different types of animal fibres are given in Annex B. ISO 2016 All rights reserved vBS EN ISO 17751-2:2016BS EN ISO 17751-2:2016Textiles Quantitative analysis of cashmere, wool, other specialty animal fibers and their blends Part 2: Scanning el

33、ectron microscopy method1 ScopeThis part of ISO 17751 specifies a method for the identification, 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, i

34、ntermediate products, and final products of cashmere, wool, other speciality animal fibres, 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 she

35、ep2.2scanning electron microscopeintermediate type of microscopic morphology observation 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 consi

36、sts of scanning a primary focused electron beam over a whole area of interest on the surface 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

37、by a scanning electron microscope are, e.g. secondary electrons (2.3), Auger electrons, 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

38、 the outermost meta-coated surface of a specimen under impact of the focused primary electron 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

39、 produces the highest-resolution morphological images of the coated surface.2.4scalecuticle covering the surface of animal fibres2.5scale frequencynumber of scales (2.4) along the fibre axis per unit lengthINTERNATIONAL STANDARD ISO 17751-2:2016(E) ISO 2016 All rights reserved 1BS EN ISO 17751-2:201

40、6ISO 17751-2:2016(E)2.6scale heightheight of the cuticle at the scales (2.4) distal edge2.7fibre surface morphologysum of the physical properties/attributes characterizing the fibre surfaceEXAMPLE The fibre surface morphology includes scale frequency (2.5), scale height (2.6), patterns of scale edge

41、, scale surface, smoothness, fibre evenness along its axis, transparency under light microscope, etc.2.8lot sampleportion representative of the same 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

42、 to requirements to prepare specimens2.10test specimenportion taken from fibre snippets randomly cut from a laboratory sample (2.9) for measurement purposes3 PrincipleA longitudinal view image of fibre snippets representative of a test specimen coated with a thin layer of gold is produced by a scann

43、ing electron microscope through scanning the side surface of the test specimen with a focused incident beam of high-energy electrons, detecting signals of secondary electrons emitted by the gold atoms excited when hit by the incident electron beam, and combining the beam position with the detected s

44、ignals which contain information on surface topography of the test specimen.All fibre types found in the test specimen are identified by comparing them with known fibre surface morphologies for different types of animal fibres.For each fibre type, the number and mean diameter of fibre snippets are c

45、ounted and measured. The mass fraction is calculated from the data for the number of fibre snippets counted, mean value, and standard deviation of the snippet diameter and the true density of each fibre type.4 Apparatus, materials, and reagents4.1 Apparatus4.1.1 Scanning electron microscope, compris

46、ed of a vacuum system, electronic optical system, signal collecting and imaging system, display system, and measurement software.4.1.2 Sputter coater with a gold cathode.4.2 Materials4.2.1 Microtome.4.2.2 Glass tube, 10 mm to 15 mm in diameter.2 ISO 2016 All rights reservedBS EN ISO 17751-2:2016ISO

47、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 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 (analytic

48、al 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 suffi

49、cient to ensure that at least 1 000 fibres are examined.6.2 Preparation method for test specimens of various types of samples6.2.1 Loose fibre6.2.1.1 Place the laboratory sample flat on the test table, pick up approximately 500 mg of fibres randomly on not less than 20 spots with tweezers (4.2.6) from the top and bottom sides of the sample. Blend them homogeneously, and divide them into three equal portions. Sort those drawn fibres into basically parallel fibre bundles.6.2.1.2 Cut the fibre bundle in the middle with a microtome (4.2.1) to get