CELEX: 51993PC0713
Language: en
Date: 1994-01-24
Title: Proposal for a EUROPEAN PARLIAMENT AND COUNCIL DIRECTIVE on certain methods for the quantitative analysis of binary textile fibre mixtures

No C 96/20                                   Official Journal of the European Communities                                      6 . 4 . 94
               Proposal for a European Parliament and Council Directive on certain methods for the
                                           quantitative analysis of binary textile fibre mixtures
                                                                 ( 94/C 96/02 )
                                                          ( Text with EEA relevance )
                                                             COM(93) 713 final
                                          (Submitted by the Commission on 25 January 1994).
THE EUROPEAN PARLIAMENT AND THE COUNCIL OF                                 5.    Whereas developments in technology necessitate
THE EUROPEAN UNION,                                                              frequent adaptation of the technical specifications
                                                                                 defined in the separate directives on methods of
                                                                                 textile analysis; whereas, in order to facilitate the
Having regard to the Treaty establishing the European                            implementation of measures required to that effect,
Community, and in particular Article 100a thereof.                               a procedure should be laid down establishing,
                                                                                 within a Committee for the adaptation of methods
                                                                                 of textile analysis to developments in technology,
Having regard to the proposal from the Commission,                               close cooperation between Member States and the
                                                                                 Commission;
Having regard of the opinion of the Economic and Social
Committee,                                                                 6.    Whereas, in the case of binary mixtures for which
                                                                                 there is no uniform method of analysis at
1.      Whereas Council Directive 72/276/EEC of 17 July                           Community level, the laboratory responsible for
        1972 on the approximation of the laws of the                             the test may determine the composition of such
        Member States relating to certain methods for the                        mixtures using any valid method at its disposal,
        quantitative analysis of binary textile fibre                             indicating in the analysis report the result obtained
        mixtures ( ] ), as last amended by Directive                              and, in so far as this is known, the degree of
        87/184/EEC ( 2 ) has been amended frequently and                          accuracy of the method used;
        substantially; whereas for reasons of clarity and
        rationality the said Directive should be                           7.    Whereas the provisions of this Directive are in
        consolidated;
                                                                                  accordance with the opinion of the Committee for
                                                                                  Directives relating to Textile Names and
2.      Whereas       European     Parliament        and    Council               Labelling;
        Directive .../.. ./EC of ... 19 .. on textile names
        requires labelling to indicate the nature of the
                                                                           8.     Whereas    this   Directive  must    not  affect     the
        fibres in textile products, checks on the conformity
        of these products with the indications given on the                       obligations of the Member States concerning the
        label being carried out by analysis;                                      deadlines for transposal of the Directives set out in
                                                                                  Annex III, part B,
3.      Whereas the methods used for official tests in the
        Member States to determine the fibre composition
        of textile products should be uniform, as regards                  HAVE ADOPTED THIS DIRECTIVE :
        both the pre-treatment of the sample and its
        quantitative analysis;
                                                                                                     Article 1
4.      Whereas Directive .../.. ./EC provides that the
        sampling and analysing methods to be used in all
        Member States for the purpose of determining the                   This Directive concerns methods for the quantitative
        fibre composition of products will be specified in                 analysis of certain binary textile fibre mixtures, including
        separate directives; whereas therefore Annex II of                 the preparation of test samples and test specimens .
        this Directive lays down 15 uniform methods of
        analysis for most of the textile products composed
        of binary mixtures that are on the market;                                                   Article 2
                                                                           'Test sample ' means a sample of a suitable size for
0 ) OJ No L 173 , 31 . 7 . 1972 , p . 1 .                                  analysis, taken from laboratory bulk samples in turn
(2 ) OJ No L 75, 17. 3 . 1987, p. 21 .                                     taken from a batch of articles for analysis.
 ---pagebreak--- 6 . 4 . 94                             Official Journal of the European Communities                              No C 96/21
'Test specimen' means that part of the test sample                2. The representative of the Commission shall submit to
required to give an individual test result.                       the Committee a draft of the measures to be adopted.
                                                                  The Committee shall deliver its opinion on the draft
                                                                  within a time limit set by the chairman having regard to
                                                                  the urgency of the matter. Opinions shall be delivered by
                          Article 3
                                                                  a majority of 54 votes, the votes of the Member States
                                                                  being weighted as provided in Article 148 (2 ) of the
Member States shall take all necessary steps to ensure            Treaty.
that, in accordance with the Directive             ./EC, the
provisions in Annexes I and II on methods for the                 The chairman shall not vote.
quantitative analysis of certain binary mixtures, including
the preparation of test samples and test specimens, are           3 . ( a ) The Commission shall adopt the measures
applied in all official tests to determine the composition                  envisaged where they are in accordance with the
of textile products put on the market.                                      opinion of the Committee.
                                                                       ( b) Where the measures envisaged are not in
                                                                            accordance with the opinion of the Committee, or
                          Article 4                                         if no opinion is delivered, the Commission shall
                                                                            without delay propose to the Council the
Any laboratory responsible for the testing of binary                        measures to be adopted.
mixtures for which there is no uniform method of                            The Council shall act by a qualified majority.
analysis at Community level shall determine the
                                                                       (c) If, within three months of the proposal being
composition of such mixtures by using any valid method                      submitted to it, the Council has not acted, the
at its disposal, indicating in the analysis report the result
obtained and, in so far as this is known, the degree of                     proposed measures shall be adopted by the
                                                                            Commission.
accuracy of the method used.
                                                                                             Article 7
                           Article 5
                                                                  Member States shall ensure that the texts of the main
                                                                  provisions of national law which they adopt in the field
 1 . A Committee for the adaptation of methods of textile         covered by this Directive are communicated to the
 analysis to developments in technology (hereinafter called        Commission .
the 'Committee') is hereby set up; it shall consist of
 representatives of the Member States with a
representative of the Commission as chairman.                                                Article 8
                                                                  The Directives listed in Annex III, Part A are repealed,
2. The Commission shall adopt its own rules of                    without prejudice to the obligations of the Member States
 procedure.                                                       concerning the deadlines for transposal set out in Annex
                                                                  III, Part B.
 3 . Adaptations to technological developments in the              References to the repealed Directives shall be construed
 methods of quantitative analysis provided for in Annex II         as references to this Directive and should be read in
 shall be made in accordance with the procedure laid               accordance with the correlation table set out in Annex
 down in Article 6 .                                               IV.
                                                                                             Article 9
                           Article 6
                                                                  This Directive is addressed to the Member States .
 1 . Where the procedure laid down in this Article is
 invoked matters shall be referred to the Committee by its        This Directive shall enter into force on the 20th day
 chairman, either on his own initiative or at the request of       following its publication in the Official Journal of the
 the representative of a Member State .                            European Communities.
 ---pagebreak--- No C 96/22                                    Official Journal of the European Communities                                      6 . 4 . 94
                                                                    ANNEX I
            PREPARATION OF TEST SAMPLES AND TEST SPECIMENS TO DETERMINE THE FIBRE
                                                 COMPOSITION OF TEXTILE PRODUCTS
            1 . FIELD OF APPLICATION
                  This Annex gives procedures for obtaining laboratory test samples of a suitable size for pre-treatment
                  for quantitative analysis ( i.e. of a mass not exceeding 100 g) from laboratory bulk samples, and for
                  selecting test specimens from the laboratory test samples that have been pre-treated to remove
                  non-fibrous matter (').
            2.   DEFINITIONS
                 2.1 . Bulk source — That quantitiy of material which is judged on the basis of one series of test results.
                         This may comprise, for example, all the material in one delivery of cloth; all the cloth woven from
                         a particular beam; a consignment of yarn, a bale or a group of bales of raw fibre.
                 2.2 . Laboratory bulk sample — That portion of the bulk source taken to be representative of the whole,
                         and which is available to the laboratory. The size and nature of the laboratory bulk sample should
                         be sufficient to overcome adequately the variability of the bulk source and to facilitate ease of
                         handling in the laboratory (2 ).
                 2.3. Laboratory test sample — That portion of the laboratory bulk sample that is subjected to
                        pre-treatment to remove non-fibrous matter, and from which test specimens are taken. The size and
                        nature of the laboratory test sample should be sufficient to overcome adequately the variability of
                        the laboratory bulk sample (3 ).
                 2.4. Test specimen — The portion of material required to give an individual test result, and selected
                        from the laboratory test sample.
           3.    PRINCIPLE
                 The laboratory test sample is selected so that it is representative of the laboratory bulk sample.
                 The test specimens are taken from the laboratory test sample in such a way that each of them is
                 representative of the laboratory test sample.
          4 . SAMPLING FROM LOOSE FIBRES
                 4.1 . Unorientated fibres — Obtain the laboratory test sample by selecting at random tufts from the
                        laboratory bulk sample. Mix thoroughly the whole of the laboratory test sample by means of a
                        laboratory carder (4 ). Subject the web or mixture, including loose fibres and fibres adhering to the
                        equipment used for mixing, to pre-treatment. Then select test specimens, in proportion to the
                        respective masses, from the web or mixture, from the loose fibres and from the fibres adhering to
                        the equipment.
                        If the card web remains intact after pre-treatment, select the test specimens in the manner described
                        in 4.2 . If the card web is disturbed by the pre-treatment, select each test specimen by removing at
                        random at least 16 small tufts of suitable and approximately equal size and then combine them . -
                 4.2. Orientated fibres (cards, webs, slivers, rovings ) — From randomly selected parts of the laboratory
                        bulk sample cut not less than 10 cross-sections each of mass approximately 1 g. Subject the
                        laboratory test sample so formed to the pre-treatment. Recombine the cross-sections by laying them
                        side by side and obtain the test specimen by cutting through them so as to take a portion of each of
                        the 10 lenghts.
          5.     SAMPLING YARN
                 5.1 . Yarn in packages or in hanks — Sample all the packages in the bulk laboratory sample.
          (') In some cases it is necessary to pre-treat the individual test specimen.
          ( 2 ) For made-up and finished articles see Section 7.
          ( 3 ) See 1 .
          (4 ) The laboratory carder may be replaced by a fibre blender, or the fibres may be mixed by the method of 'tufts and
                rejects '.
 ---pagebreak--- 6 . 4 . 94                                  Official Journal of the European Communities                                       No C 96/23
                      Withdraw the appropriate continuous equal lengths from each package either by winding skeins of
                      the same number of turns on a wrap-reel ('), or by some other means. Unite the lengths side by side
                      either as a single skein or as a tow to form the laboratory test sample, ensuring that there are equal
                      lenghts from each package in the skein or tow.
                      Subject the laboratory test sample to the pre-treatment.
                      Take test specimens from the laboratory test sample by cutting a bunch of threads of equal length
                      from the skein or tow, taking care to see that the bunch contains all the threads in the sample.
                      If the tex of the yarn is t and the number of packages selected from the laboratory bulk sample is n,
                      then to obtain a test sample of 10 g, the length of yarn to be withdrawn from each package is
                       10 6
                      ~T7~
                        Nt
                             cm -
                      If nt is high, i.e. more than 2 000, wind a heavier skein and cut it across in two places to make a
                      tow of suitable mass. The ends of any sample in the form of a tow should be securely tied before
                      pre-treatment and test specimens taken from a place remote from the tie bands .
               5.2 . Yarn on warp — Take the laboratory test sample by cutting a length from the end of the warp, not
                      less than 20 cm long and comprising all the yarns in the warp except the selvedge yarns, which are
                      rejected. Tie the bunch of threads together near one end. If the sample is too large for pre-treatment
                      as a whole divide it into two or more portions, each tied together for pre-treatment, and reunite the
                      portions after each has been pre-treated separately. Take a test specimen by cutting a suitable length
                      from the laboratory test sample from the end remote from the tie band, and comprising all the
                      threads in the warp . For warp of N threads of tex t, the length of a specimen of mass 1 g is
                       10 5
                        Nt
           6 . SAMPLING FABRIC
                6.1 . From a laboratory bulk sample consisting of a single cutting representative of the cloth
                      — Cut a diagonal strip from one corner to the other and remove the selvedges. This strip is the
                            laboratory test sample. To obtain a laboratory test sample of x g, the strip area shall be
                            x 1 04
                            ——— cm2, where G is the mass of the cloth in g/m2.
                               G
                            Subject the laboratory test sample to the pre-treatment and then cut the strip transversely into
                            four equal lengths and superimpose them.
                            Take test specimens from any part of the layered material by cutting through all the layers so
                            that each specimen contains an equal length of each layer.
                            If the fabric has a woven design, make the width of the laboratory test sample, measured
                            parallel to the warp direction, not less than one warp repeat of the design. If, with this
                            condition satisfied, the laboratory test sample is too large to be treated as a whole, cut it into
                            equal parts, pre-treat them separately, and superimpose these parts before selection of the test
                            specimen, taking care that corresponding parts of the design do not coincide.
                6.2. From a laboratory bulk sample consisting of several cuttings
                      — Treat each cutting as described in 6.1 , and give each result separately.
           7 . SAMPLING MADE-UP AND FINISHED ARTICLES
                The bulk laboratory sample is normally a complete made-up or finished article or representative fraction
                of one .
                Where appropriate determine the percentage of the various parts of the article not hiving the same fibre
                content, in order to check compliance with Article 9 of the Directive on textile names.
           (!) If the packages can be mounted in a convenient creel, a number can be wound simultaneously.
 ---pagebreak--- No C 96/24                          Official Journal of the European Communities                                      6 . 4 . 94
           Select a laboratory test sample representative of the part of the made-up or finished article, whose
           composition must be shown by the label . If the article has several labels, select laboratory test samples
           representative of each part corresponding to a given label.
           If the article whose composition is to be determined is not uniform, it may be necessary to select
           laboratory test samples from each of the parts of the article and to determine the relative proportions of
           the various parts in relation to the whole article in question.
           Then calculate the percentages taking into account the relative proportions of the sampled parts.
           Subject the laboratory test samples to the pre-treatment.
           Then select test specimens representative of the pre-treated laboratory test samples.
 ---pagebreak--- 6 . 4 . 94                               Official Journal of the European Communities                                       No C 96/25
                                                              ANNEX II
                   METHODS FOR QUANTITATIVE ANALYSIS OF CERTAIN BINARY FIBRE MIXTURES
                                                            1 . GENERAL
            Introduction
            Methods for the quantitative analysis of fibre mixtures are based on two main processes, the manual
            separation and the chemical separation of fibres.
            The method of manual separation should be used whenever possible since it generally gives more accurate
            results than the chemical method. It can be used for all textiles whose component fibres do not form an
            intimate mixture, as for example in the case of yarns composed of several elements each of which is made
            up of only one type of fibre, or fabrics in which the fibre of the warp is of a different kind to that of the
            weft, or knitted fabrics capable of being unravelled made up of yarns of different types.
            In general, the methods of chemical quantitative analysis are based on the selective solution of the individual
            components. After the removal of a component the insoluble residue is weighed, and the proportion of the
            soluble component is calculated from the loss in mass. This first part of the Annex gives the information
            common to the analyses by this method of all fibre mixtures dealt with in the Annex, whatever their
            composition. It should thus be used in conjunction with the succeeding individual sections of the Annex,
           which contain the detailed procedures applicable to particular fibre mixtures. Occasionally, an analysis is
            based on a principle other than selective solution; in such cases full details are given in the appropriate
            section .
           Mixtures of fibres during processing and, to a lesser extent, finished textiles may contain non-fibrous
           matter, such as fats, waxes or dressings, or water-soluble matter, either occurring naturally or added to
           facilitate processing. Non-fibrous matter must be removed before analysis. For this reason a method for
           removing oils, fats, waxes and water-soluble matter is also given.
           In addition, textiles may contain resins or other matter added to confer special properties. Such matter,
           including dyestuffs in exceptional cases, may interfere with the action of the reagent on the soluble
           component and/or it may be partially or completely removed by the reagent. This type of added matter may
           thus cause errors and should be removed before the sample is analysed. If it is impossible to remove such
           added matter the methods for quantitiative chemical analysis given in this Annex are no longer
           applicable.
           Dye in dyed fabrics is considered to be an integtal part of the fibre and is not removed.
           Analyses are conducted on the basis of dry mass and a procedure is given for determining dry mass.
           The result is obtained by applying to the dry mass of each fibre the recovery factors listed in Annex II to the
           Directive on textile names .
           Before proceeding with any analysis, all the fibres present in the mixture should have been identified. In
           some methods, the insoluble component of a mixture may be partially dissolved in the reagent used to
           dissolve the soluble component. Where possible, reagents have been chosen that have little or no effect on
           the insoluble fibres. If loss in mass is known to occur during the analysis, the result should be corrected;
           correction factors for this purpose are given.
           These factors have been determined in several laboratories by treating, with the appropriate reagent as
           specified in the method of analysis, fibres cleaned by the pre-treatment. These correction factors apply only
           to undegraded fibres and different correction factors may be necessary if the fibres have been degraded
           before or during processing. The procedures given apply to single determinations.
           At least two determinations on separate test specimens should be made, both in the case of manual
           separation and in the case of chemical separation. For confirmation, unless technically impossible, it is
           recommended to use alternative procedures whereby the constituent that was the residue in the standard
           method is dissolved out first .
           I.          General information on methods for the quantitative chemical analysis of textile fibre mixtures
                       Information common to the methods given for the quantitative chemical analysis of fibre
                       mixtures .
 ---pagebreak--- No C 96/26                                  Official Journal of the European Communities                                              6. 4. 94
            1. 1 .        Scope and field of application
                          The field of application for each method specifies to which fibres the method is applicable.
            1.2 .         Principle
                          After the identification of the components of a mixture, the non-fibrous material is removed by
                          suitable pre-treatment and then one of the components, usually by selective solution (!). The
                          insoluble residue is weighed and the proportion of soluble component calculated from the loss in
                         mass. Except where this presents technical difficulties, it is preferable to dissolve the fibre present
                          in the greater proportion, thus obtaining the fibre present in the smaller proportion as residue.
            1.3 .        Materials and equipment
            1.3.1 .      Apparatus
            1.3.1.1 .    Filter crucibles and weighing bottles large enough to contain such crucibles, or any other
                         apparatus giving identical results.
           1.3.1.2 .     Vacuum flask .
           1.3.1.3 .     Desiccator containing self-indicating silica gel.
           1.3.1.4.      Ventilated oven for drying specimens at 150° ± 3 °C.
           1.3.1.5 .     Analytical balance, accurate to 0,0002 g.
           1.3.1.6 .     Soxhlet extractor or other apparatus giving identical results.
           1.3.2 .       Reagents
           1.3.2.1 .     Light petroleum, redistilled, boiling range 40 to 60 °C.
           1.3.2.2 .     Other reagents are specified in the appropriate sections of each method. All reagents used should
                         be chemically pure.
           1.3.2.3 .     Distilled or deionized water .
           1.4.          Conditioning and testing atmosphere
                         Because dry masses are determined, it is unnecessary to condition the specimen or to conduct
                         analyses in a conditioned atmosphere.
           1.5 .         Laboratory test sample
                         Take a laboratory test sample that is representative of the laboratory bulk sample and sufficient
                         to provide all the specimens, each of at least 1 g, that are required.
           1.6 .         Pre-treatment of laboratory test sample
                         Where a substance not to be taken into account in the percentage calculations ( see Article 12 ( 3 ),
                         of the Directive on textile names) is present, it should first be removed by a suitable method that
                         does not affect any of the fibre constituents.
                         For this purpose, non-fibrous matter which can be extracted with light petroleum and water is
                         removed by treating the air-dry test sample in a Soxhlet extractor with light petroleum for 1 hour
                         at a minimum rate of 6 cycles per hour. Allow the light petroleum to evaporate from the sample,
           (') Method 12 is an exception . It is based on a determination of the content of a constituent substance of one of the two
                 components .
           ( 2 ) See Annex 1.1 .
 ---pagebreak--- 6 . 4 . 94                                Official Journal of the European Communities                                      No C 96/27
                      which is then extracted by direct treatment consisting in soaking the specimen in water at room
                      temperature for 1 hour and then soaking it in water at 65 ± 5 °C for a furhter hour, agitating the
                      liquor from time to time. Use a liquor: specimen ratio of 100:1 . Remove the excess water from
                      the sample by squeezing, suction, or centrifuging and then allow the sample to become air-dry.
                      Where non-fibrous matter cannot be extracted with light petroleum and water, it should be
                      removed by substituting for the water method described above a suitable method that does not
                      substantially alter any of the fibre constituents. However, for some unbleached, natural vegetable
                      fibres (e.g. jute, coir) it is to be noted that normal pre-treatment with light petroleum and water
                      does not remove all the natural non-fibrous substances; nevertheless additional pre-treatment is
                      not applied unless the sample does contain finishes insoluble in both light petroleum and
                      water .
                      Analysis reports should include full details of the methods of pre-treatment used.
           1.7.       Test procedure
           1.7.1 .    General instructions
           1.7.1.1 .  Drying
                      Conduct all drying operations for not less than 4 hours and not more than 16 hours at 105 ± 3
                      °C in a ventilated oven with the oven door closed throughout. If the drying period is less than 14
                     hours, the specimen must be weighed to check that its mass has become constant. The mass may
                      be considered to have become constant if, after a further drying period of 60 minutes, its
                     variation is less than 0,05,% .
                      Avoid handling crucibles and weighing bottles, specimens or residues with bare hands during the
                     drying, cooling and weighing operations.
                     Dry specimens in a weighing bottle with its cover beside it. After drying, stopper the weighing
                      bottle before removing it from the oven, and transfer it quickly to the desiccator.
                     Dry the filter crucible in a weighing bottle with its cover beside it in the oven. After drying, close
                     the weighing bottle and transfer it quickly to the desiccator.
                     Where apparatus other than a filter crucible is used, drying operations in the oven should be
                     conducted in such a way as to enable the dry mass of the fibres to be determined without
                     loss .
           1.7.1.2 . Cooling
                     Conduct all cooling operations in the desiccator the latter placed beside the balance, until
                     complete cooling of the weighing bottles is attained, and in any case for not less than 2 hours.
           1.7.1.3 .  Weighing
                     After cooling, complete the weighing of the weighing bottle within 2 minutes of its removal from
                     the desiccator . Weigh to an accuracy of 0,0002 g .
           1.7.2 .   Procedure
                     Take from the pre-treated laboratory test sample a test specimen weighing at least 1 g. Cut yarn
                     or cloth into lengths of about 10 mm, dissected as much as possible. Dry the specimen in a
                     weighing bottle, cool it in the desiccator and weigh it. Transfer the specimen to the glass vessel
                     specified in the appropriate section of the relevant Community method, reweigh the weighing
                     bottle immediately and obtain the dry mass of the specimen by difference. Complete the test as
                     specified in the appropriate section of the applicable method. Examine the residue
                     microscopically to check that the treatment has in fact completely removed the soluble fibre.
           1.8 .     Calculation and expression of results
                     Express the mass of the insoluble component as a percentage of the total mass of fibre in the
                     mixture. The percentage of soluble component is obtained by difference. Calculate the results on
                     the basis of clean, dry mass, adjusted by (a ) the relevant recovery factors and ( b) the correction
                     factors necessary to take account of loss of matter during pre-treatment and analysis.
                     Calculations should be made by applying the formula given in 1.8.2 .
 ---pagebreak--- No C 96/28                                Official Journal of the European       Communities                              6 . 4 . 94
           1.8.1 .  Calculation of percentage of insoluble component on clean, dry mass basis, disregarding loss of
                    fibre mass during pre-treatment.
                    Pl% = JSlEl     m
                    where
                    P t is the percentage of clean, dry insoluble component;
                    m is the dry mass of the specimen after pre-treatment;
                    r   is the dry mass of the residue;
                    d is the correction factor for loss of mass of the insoluble component in the reagent during the
                        analysis .
                    Suitable values of d are given in the appropriate section of each method.
                    Such values of d are of course the normal values applicable to chemically undegraded fibres.
           1.8.2 .  Calculation of percentage of insoluble component on clean, dry mass basis, with adjustment by
                    conventional recovery factors and, where appropriate, correction factors for loss mass during
                    pre-treatment .
                                                ,00 P, / l + a' + bl \
                                                     1\         100   /
                    P,A % =                                                                 —
                                      p,1 (i\ ♦     100 /
                                                            ♦ (loo
                                                              v
                                                                    - p,)"I(l ♦ -2z_L^_)
                                                                                    100 /
                   where
                   P}A is the percentage of insoluble component, adjusted by conventional recovery factors and for
                         loss of mass during pre-treatment;
                   Pt    is the percentage of clean, dry insoluble component as calculated from the formula shown in
                         1.8 . 1 .;
                         is the conventional recovery factor for the insoluble component ( see Annex II to the
                         Directive on textile names );
                   a2    is the conventional recovery factor for the soluble component ( see Annex II to the Directive
                         on textile names );
                   b!    is the percentage loss of insoluble component caused by the pre-treatment;
                   b2    is the percentage loss of soluble component caused by the pre-treatment.
                   The percentage of the second component (P2 A) is equal to 100 — Pi A.
                   Where a special pre-treatment has been used, the values of b ^ and b2 should be determined, if
                   possible, by submitting each of the pure fibre constituents to the pre-treatment applied in the
                   analysis. Pure fibres are those free from all non-fibrous material except that which they normally
                   contain (either naturally or because of the manufacturing process ), in the state ( unbleached,
                   bleached) in which they are found in the material to be analysed.
                   Where no clean separate constituent fibres used in the manufacture of the material to be analysed
                   are available, average values of b ( and b2 as obtained from tests performed on clean fibres similar
                   to those in the mixture under examination, should be used .
                   If normal pre-treatment by extraction with light          petroleum and water is applied, correction
                   factors b! and b2 may generally be ignored, except        in the case of unbleached cotton, unbleached
                   flax and unbleached hemp, where the loss due to           the pre-treatment is conventionally taken as
                   4 % , and in the case of polypropylene, where it is       taken as 1 % .
                   In the case of other fibres, losses due to the pre-treatment are conventionally disregarded in
                   calculations .
 ---pagebreak--- 6 . 4 . 94                               Official Journal of the European Communities                                       No C 96/29
           II.         Method of quantitative analysis by manual separation
           II. 1 .     Field of application
                       This method is applicable to textile fibres of all types provided they do not form an intimate
                       mixture and that it is possible to separate them by hand.
           II.2 .      Principle
                       After identification of the constituents of the textile, the non-fibrous material is removed by
                       suitable pre-treatment and then the fibres are separated by hand, dried and weighed in order to
                       calculate the proportion of each fibre in the mixture.
           II . 3 .    Apparatus
           II. 3.1 .   Weighing bottle or any other apparatus giving identical results.
           II. 3.2 .   Desiccator containing self-indicating silica gel.
           11. 3 . 3 . Ventilated oven for drying specimens at 150 ± 3 °C.
           11.3.4 .    Analytical balance, accurate to 0,0002 g.
           II. 3 .5 .  Soxhlet extractor, or other apparatus giving an identical result.
           II.3.6 .    Needle .
           II.3 . 7.   Twist tester or similar apparatus.
           II.4 .      Reagents
           II.4.1 .    Light petroleum, redistilled, boiling range 40 to 60 °C.
           II.4.2 .    Distilled or deionized water.
           II.5 .      Conditioning and testing atmosphere
                       See 1.4 .
           II . 6 .    Laboratory test sample
                       See 1.5 .
           II.7.       Pre-treatment of laboratory test sample
                       See 1.6 .
           II . 8 .    Procedure
           II. 8.1 .   Analysis of yarn
                       Select from the pre-treatment laboratory test sample a specimen of mass not less than 1 g. For a
                       very fine yarn, the analysis may be made on a minimum length of 30 m, whatever its mass. Cut
                       the yarn into pieces of a suitable length and separate the fibre types by means of a needle and, if
                       necessary, a twist tester. The fibre types so obtained are placed in pre-weighed weighing bottles
                       and dried at 105 ± 3 °C until a constant rnass is obtained, as described in 1.7.1 and 1.7.2 .
           II.8.2 .    Analysis of cloth
                       Select from the pre-treated laboratory test sample, well away from all selvedges, a specimen of
                       mass not less than 1 g, with edges carefully trimmed to avoid fraying and running parallel with
                       weft or warp yarns, or in the case of knitted fabrics in the line of wales and courses. Separate the
                       different fibre types, collect them in pre-weighed weighing bottles and proceed as described in
                       II . 8.1 .
 ---pagebreak--- No C 96/30                                Official Journal of the European Communities                                      6 . 4 . 94
           II.9 .      Calculation and expression of results
                       Express the mass of each fibre constituent as a percentage of the total mass of the fibres in the
                       mixture. Calculate the results on the basis of clean, dry mass, adjusted by ( a ) the relevant
                       recovery factors and ( b) the correction factors necessary to take account of loss of matter during
                       pre-treatment.
           II.9.1 .    Calculation of percentage masses of clean, dry fibre, disregarding loss of fibre mass during
                       pre-treatment:
                           n/        100 m ,          100
                       1 ] /O =                =
                                    mi + m2       1 +
                                                        m2=—
                                                        mi
                       where
                       Pi is the percentage of the first clean, dry component;
                       ni | is the clean, dry mass of the first component;
                       m2 is the clean, dry mass of the second component.
           II.9.2 .    For calculation of the percentage of each component with adjustment by conventional recovery
                       factors and, where appropriate, by correction factors for loss of matter during pre-treatment, see
                       1.8.2 .
           III.l .     Precision of the methods
                       The precision indicated in individual methods relates to the reproducibility.
                       The reproducibility refers to the realiability, i.e. the closeness of agreement between experimental
                       values obtained by operators in different laboratories or at different times using the same method
                       and obtaining individual results, on specimens of an identical consistent mixture.
                       The reproducibility is expressed by confidence limits of the results for a confidence level of
                       95 % .
                       By this is meant that the difference between two results in a series of analysis made in different
                       laboratories would, given a normal and correct application of the method to an identical and
                       consistent mixture, be exceeded only in five cases out of a 100.
           III.2 .      Test report
           111.2.1 .    State that the analysis was conducted in accordance with this method.
            111.2.2 .   Give details of any special pre-treatment ( see 1.6 ).
            III.2 .3 .  Give the individual results and the arithmetic mean, each to an accuracy of 0,1 .
 ---pagebreak--- 6 . 4 . 94                    Official Journal of the European Communities                           No C 96/31
                                2 . SPECIAL METHODS — SUMMARY TABLE
           Method                       Field of application                        Reagent
           No 1   Acetate                           Certain other fibres  Acetone
           No 2   Certain protein fibres            Certain other fibres  Alkaline sodium
                                                                          hypochlorite
           No 3   Viscose, cupro or certain         Cotton                Zinc chloride, Formic acid
                  types of modal
           No 4   Polyamide or nylon                Certain other fibres  Formic acid, 80 % m/m
           No 5   Acetate                           Triacetate            Benzyl alcohol
           No 6   Triacetate                        Certain other fibres  Dichloromethane
           No 7   Certain cellulose fibres          Polyester             Sulphuric acid, 75 % m/m
           No 8   Acrylics, certain                 Certain other fibres  Dimethylformamide
                  modacrylics or certain
                  chlorofibres
           No 9   Certain chlorofibres              Certain other fibres  Carbon disulphide/acetone,
                                                                          55,5/44,5 v/v
           No 10  Acetate                           Certain chlorofibres  Glacial acetic acid
           No 11  Silk                              Wool or hair          Sulphuric acid, 75% m/m
           No 12  Jute                              Certain animal fibres Nitrogen content method
           No 13  Polypropylene                     Certain other fibres  Xylene
           No 14  Chlorofibres                      Certain other fibres  Concentrated sulphuric
                  (homopolymers of vinyl                                  acid method
                  chloride )
           No 15  Chlorofibres, certain             Certain other fibres  Cyclohexanone
                  modacrylics, certain
                  elastanes, acetates,
                  triacetatates
 ---pagebreak--- No C 96/32                                   Official Journal of the European Communities                                                   6 . 4 . 94
                                                                  METHOD No 1
                                              ACETATE AND CERTAIN OTHER FABRICS
                                                                 ( Acetone method )
           1.  FIELD OF APPLICATION
               This method is applicable, after removal of non-fibrous matter, to binary mixtures of:
               1 . acetate ( 19 )
                    with
               2. wool ( 1 ), animal hair (2 and 3 ), silk (4 ), cotton ( 5 ), flax ( 7 ), true hemp ( 8 ), jute ( 9 ), abaca ( 10), alfa
                    ( 11 ), coir ( 12 ), broom ( 13 ), ramie ( 14 ), sisal ( 15 ), cupro ( 21 ), modal (22 ), protein (23 ), viscose (25 ),
                    acrylic (26 ), polyamide or nylon ( 30 ) and polyester ( 31 ).
               In no circumstances is the method applicable to acetate fibres which have been deacetylated on the
               suface .
           2.  PR NCIPLE
               The acetate is dissolved out from a known dry mass of the mixture, with acetone. The residue is
               collected, washed, dried and weighed; its mass, corrected if necessary, is expressed as a percentage of the
               dry mass of the mixture. The percentage of dry acetate is found by difference.
           3 . APPARATUS AND REAGENTS ( additional to those specified in the general instructions)
               3.1 . Apparatus
                      Glass-stoppered conical flasks of at least 200 ml capacity.
               3.2 . Reagent
                      Acetone .
           4.    TEST PROCEDURE
                 Follow the procedure described in the general instructions and proceed as follows:
                 to the specimen contained in a glass-stoppered conical flask of at least 200 ml capacity, add 100 ml of
                 acetone per gram of specimen, shake the flask, stand it for 30 minutes at room temperature, stirring
                 from time to time, and then decant the liquid through the weighed filter crucible;
                 repeat the treatment twice more (making three extractions in all ), but for periods of 15 minutes only,
                 so that the total time of treatment in acetone is one hour . Transfer the residue to the filter crucible .
                 Wash the residue in the filter crucible with acetone and drain with suction . Refill the crucible with
                 acetone and allow to drain under gravity;
                 finally, drain the crucible with suction, dry the crucible and residue, and cool and weigh them .
           5.   CALCULATION AND EXPRESSION OF RESULTS
                Calculate the results as described in the general instructions. The value of 'd' is 1,00.
           6.   PRECIS ON
                On a homogeneous mixture of textile materials, the confidence limits of results obtained by this method
                are not greater than ± 1 for a confidence level of 95 % .
 ---pagebreak--- 6 . 4 . 94                                      Official Journal of the European Communities                                    No C 96/33
                                                                 METHOD No 2
                                        CERTAIN PROTEIN FIBRES AND CERTAIN OTHER FIBRES
                                                            (Method using hypochlorite)
           1.     FIELD OF APPLICATION
                  This method is applicable, after removal of non-fibrous matter, to binary mixtures of:
                   1 . certain protein fibres, namely: wool ( 1 ), animal hair (2 and 3 ), silk (4 ), protein (23 )
                         with
                  2 . cotton ( 5 ), cupro (21 ), viscose (25 ), acrylic (26 ) chlorofibres (27), polyamide or nylon ( 30 ),
                         polyester (31 ) polypropylene ( 33 ), elastane ( 39) and glass fibre (40).
                  If different protein fibres are present, the method gives the total of their amounts but not their
                  individual quantities.
           2.     PRINCIPLE
                 The protein fibre is dissolved out from a known dry mass of the mixture, with a hypochlorite solution.
                  This residue is collected, washed, dried and weighed; its mass, corrected if necessary, is expressed as a
                  percentage of the dry mass of the mixture. The percentage of dry protein fibre is found by
                  difference.
                  Either lithium hypochlorite or sodium hypochlorite can be used for the preparation of the hypochlorite
                  solution .
                  Lithium hypochlorite is recommended in cases involving a small number of analyses or for analyses
                 conducted at fairly lengthy intervals. This is because the percentage of hypochlorite in solid lithium
                 hypochlorite — unlike that in sodium hypochlorite — is virtually constant. If the percentage of
                 hypochlorite is known , hypochlorite content need not be checked iodometrically for each analysis, since
                 a constant weighed portion of lithium hypochlorite can be employed.
           3.    APPARATUS AND REAGENTS (other than those specified in the general instruction )
           3.1 . Apparatus
                  (i) Erlenmeyer flask with ground-glass stopper, 250 ml;
                 ( ii ) thermostat, adjustable to 20 (± 2 ) °C.
           3.2 . Reagents
                 ( i ) Hypochlorite reagent
                        ( a ) Lithium hypochlorite solution
                              This consists of a freshly prepared solution containing 35 (± 2 ) g/1 of active chlorine
                              ( approximately 1 M ), to which 5 (± 0,5 ) g/1 of previously dissolved sodium hydroxide is added.
                              To prepare, dissolve 100 grams of lithium hypochlorite containing 35 % active chlorine (or 115
                              grams containing 30 % active chlorine) in approximately 700 ml of distilled water, add 5 grams
                              of sodium hydroxide dissolved in approximately 200 ml of distilled water and make up to
                              1 litre with distilled water. The solution which has been freshly prepared need not be checked
                              iodometrically;
                        ( b ) Sodium hypochlorite solution
                              This consists of a freshly prepared solution containing 35 (± 2 ) g/1 of active chlorine
                              ( approximately 1 M ) to which 5 (± 0,5 ) g/1 of previously dissolved sodium hydroxide is added.
                              Check the active chlorine content of the solution iodometrically before each analysis;
                 ( ii ) Acetic acid, dilute solution
                        Dilute 5 ml of glacial acetic acid to 1 1 with water.
           4.    TEST PROCEDURE
                 Follow the procedure described in the general instructions and proceed as follows: mix approximately
                 1 gram of the sample with approximately 100 ml of the hypochlorite solution ( lithium or sodium
                 hypochlorite) in the 250 ml flask and agitate thoroughly in order to wet out the sample.
 ---pagebreak--- No C 96/34                            Official Journal of the European Communities                                         6 . 4 . 94
              Then heat the flask for 40 minutes in a thermostat at 20 °C and agitate continuously, or at least at
              regular intervals. Since the dissolution of the wool proceeds exothermically, the reaction heat of this
              method must be distributed and removed. Otherwise, considerable errors may be caused by the
              incipient dissolution of the non-soluble fibres.
              After 40 minutes, filter the flask contents through a weighed glass-filter crucible and transfer any
              residual fibres into the filter crucible by rinsing the flask with a little hypochlorite reagent. Drain the
              crucible with suction and wash the residue successively with water, dilute acetic acid, and finally water,
              draining the crucible with suction after each addition. Do not apply suction until each washing liquor
              has drained under gravity.
              Finally, drain the crucible with suction, dry the crucible with the residue, and cool and weigh them.
           5. CALCULATION AND EXPRESSION OF RESULTS
              Calculate the results as described in the general instructions. The value of 'd' is 1,00, except for cotton,
              viscose and modal, for which 'd' = 1,01 , and unbleached cotton, for which 'd' = 1,03 .
           6. PRECISION
              On homogeneous mixtures of textile materials, the confidence limits for results obtained by this
              method are not greater than ± 1 for a confidence level of 95 % .
 ---pagebreak--- 6 . 4 . 94                                    Official Journal of the European Communities                                      No C 96/35
                                                                 METHOD No 3
                                  VISCOSE, CUPRO OR CERTAIN TYPES OF MODAL AND COTTON
                                                 (Method using formic acid and zinc chloride)
            1 . FIELD OF APPLICATION
                 This method is applicable, after removal of non-fibrous matter, to binary mixtures of:
                 1 . viscose (25 ) or cupro ( 12 ), including certain types of modal fibre (22 ),
                      with
                 2 . cotton ( 5 ).
                 If a modal fibre is found to be present, a preliminary test should be carried out to see whether it is
                 soluble in the reagent.
                This method is not applicable to mixtures in which the cotton has suffered extensive chemical
                degradation nor when the viscose or cupro is rendered incompletely soluble by the presence of certain
                dyes or finishes that cannot be removed completely.
           2.   PRINCIPLE
                The viscose, cupro or modal fibre is dissolved from a known dry mass of the mixture, with a reagent
                consisting of formic acid and zinc chloride. The residue is collected, washed, dried and weighed; its
                corrected mass is expressed as a percentage of the dry mass of the mixture. The percentage of dry
                viscose, cupro or modal fibre is found by difference.
           3 . APPARATUS AND REAGENTS (other than those specified in the general instructions)
                3.1 . Apparatus
                       (i) glass-stoppered conical flasks of at least 200 ml capacity;
                       (ii ) apparatus for maintaining flasks at 40 ± 2 °C.
                3.2 . Reagents
                       (i) Solution containing 20 g of fused anhydrous zinc chloride and 68 g of anhydrous formic acid
                             made up to 100 g with water (namely 20 parts by mass of fused anhydrous zinc chloride to
                             80 parts by mass of 85 % m/m formic acid).
                             Attention is drawn, in this respect, to Annex II (1 ), pont 1.3.2.2, which lays down that all
                             reagents used should be chemically pure; in addition, it is essential to use only fused anhydrous
                             zinc chloride.
                       (ii ) Ammonium hydroxide solution : dilute 20 ml of a concentrated ammonia solution ( specific
                             gravity 0,880 g/ml)) to 1 litre with water.
           4 . TEST PROCEDURE
                Follow the procedure described in the general instructions and proceed as follows: place the specimen
                immediately in the flask, pre-heated to 40 °C. Add 100 ml of the solution of formic acid and zinc
                chloride, pre-heated to 40 °C per gram of specimen. Insert the stopper and shake the flask vigorously.
                Keep the flask and its contents at a constant temperature of 40 °C for two hours and a half, shaking the
                flask at hourly intervals. Filter the contents of the flask through the weighed filter crucible and with the
                help of the reagent transfer to the crucible any fibres remaining in the flask. Rinse with 20 ml of
                reagent .
                Wash crucible and residue thoroughly with water at 40 °C.
                Rinse the fibrous residue in approximately 100 ml of cold ammonia solution ( 3.2.ii ) ensuring that this
                residue remains wholly immersed in the solution for 10 minutes 0 ); then rinse thoroughly with cold
                water .
                Do not apply suction until each washing liquor has drained under gravity. Finally, drain the remaining
                liquid with suction, dry the crucible and residue, and cool and weigh them.
           (') To ensure that the fibrous residue is immersed in the ammonia solution for 10 minutes, one may, for example, use
               filter crucible adaptor fitted with a tap by which the flow of the ammonia solution can be regulated .
 ---pagebreak--- No C 96/36                              Official Journal of the European Communities                                   6 . 4 . 94
           5.  CALCULATION AND EXPRESSION OF RESULTS
               Calculate the results as described in the general instructions. The value of 'd' for cotton is 1,02 .
           6 . PRECISION
               On a homogeneous mixture of textile materials, the confidence limits of results obtained by this method
               are not greater than ± 2 for a confidence level of 95 % .
 ---pagebreak--- 6 . 4 . 94                                    Official Journal of the European Communities                                         No C 96/37
                                                                 METHOD No 4
                                         POLYAMIDE OR NYLON, AND CERTAIN OTHER FIBRES
                                                     (Method using 80 % m/m formic acid )
            1. FIELD OF APPLICATION
               This method is applicable, after removal of non-fibrous matter, to binary mixtures of:
                1 . polyamide or nylon, ( 30 ),
                    with
               2 . wool ( 1 ), animal hair (2 and 3 ), cotton ( 5 ), cupro (21 ), modal (22 ), viscose (25 ), acrylic (26 )
                    chlorofibre (27), polyester (31 ), polypropylene (33 ) and glass fibre (40).
               As mentioned above, this method is also applicable to mixtures with wool, but when the wool content
               exceeds 25 % , method No 2 should be applied (dissolving wool in a solution of alkaline sodium
               hypochlorite ).
           2 . PRINCIPLE
               The polyamide fibre is dissolved out from a known dry mass of the mixture, with formic acid. The
               residue is collected, washed, dried and weighed; its mass, corrected if necessary, is expressed as a
               percentage of the dry mass of the mixture. The percentage of polyamide or nylon is found by
               difference .
           3 . APPARATUS AND REAGENTS ( other than those specified in the general instructions)
               3.1 . Apparatus
                     Glass-stoppered conical flask of at least 200 ml capacity;
               3.2 . Reagents
                     ( i) formic acid ( 80 % m/m, relative density at 20 °C: 1,186 ). Dilute 880 ml of 90 % m/m formic
                            acid ( relative density at 20 °C: 1,204 ) to 1 litre with water. Alternatively, dilute 780 ml of 98 to
                            100 % m/m formic acid (relative density at 20 °C: 1,220 ) to 1 litre with water,
                            the concentration is not critical within the range 77 to 83 % m/m formic acid;
                     ( ii ) ammonia, dilute solution : dilute 80 ml of concentrated ammonia solution ( relative density at
                            20 °C : 0,880 ) to 1 litre with water .
           4.    TEST PROCEDURE
                 Follow the procedure described in the general instructions and proceed as follows: to the specimen
                 contained in the conical flask of at least 200 ml capacity, add 100 ml of formic acid per gram of
                 specimen . Insert the stopper, shake the flask to wet out the specimen . Stand the flask for 15 minutes at
                 room temperature, shaking it at intervals. Filter the contents of the flask through the weighed filter
                 crucible and transfer any residual fibres to the crucible by washing out the flask with a little formic
                 acid reagent. Drain the crucible with suction and wash the residue on the filter successively with formic
                 acid reagent, hot water, dilute ammonia solution, and finally cold water, draining the crucible with
                 suction after each addition . Do not apply suction until each washing liquor has drained under gravity.
                 Finally, drain the crucible with suction, dry the crucible and residue, and cool and weigh them.
           5.    CALCULATION AND EXPRESSION OF RESULTS
                 Calculate the results as described in the general instructions . The value of ' d ' is 1,00 .
           6.    PRECISION
                 On a homogeneous mixture of textile materials, the confidence limits of results obtained by this
                 method are not greater than ± 1 for a confidence level of 95 % .
 ---pagebreak--- No C 96/38                                  Official Journal of the European Communities                                  6 . 4 . 94
                                                             METHOD No 5
                                                     ACETATE AND TRIACETATE
                                                       (Method using benzyl alcohol)
            1 . FIELD OF APPLICATION
                 This method is applicable, after removal of non-fibrous matter, to binary mixtures of:
                 — acetate ( 19 )
                     with
                — triacetate ( 24 )
           2.    PRINCIPLE
                The acetate fibre is dissolved out from a known dry mass of the mixture, with benzyl alcohol at 52
                 ± 2 °C .
                The residue is collected, washed, dried and weighed; its mass is expressed as a percentage of the dry
                mass of the mixture. The percentage of dry acetate is found by difference.
           3 . APPARATUS AND REAGENTS (other than those specified in the general instructions )
                3.1 . Apparatus
                      (i)    Glass-stoppered conical flask of at least 200 ml capacity;
                      ( ii ) Mechanical shaker;
                      (iii) Thermostat or other apparaturs for keeping the flask at a temperature of 52 ± 2 °C.
                3.2 . Reagents
                      (i)    Benzyl alcohol;
                      (ii ) Ethanol .
           4 . TEST PROCEDURE
                Follow the procedure described in the general instructions and proceed as follows:
                To the specimen contained in the conical flask, add 100 ml of benzyl alcohol per gram of specimen.
                Insert the stopper, secure the flask to the shaker so that it is immersed in the water-bath, kept at 52
                ± 2 °C, and shake for 20 minutes at this temperature.
                (Instead of using a mechanical shaker, the flask may be shaken vigorously by hand.)
                Decant the liquid through the weighed filter crucible. Add a further dose of benzyl alcohol in the flask
                and shake as before at 52 ± 2 °C for 20 minutes .
                Decant the liquid through the crucible. Repeat the cycle of operations a third time.
                Finally pour the liquid and the residue into the crucible; wash any remaining fibres from the flask into
                the crucible with an extra quantity of benzyl alcohol at 52 ± 2 °C. Drain the crucible thoroughly.
                Transfer the fibres into a flask, rinse with ethanol and after shaking manually decant through the filter
                crucible .
                Repeat this rinsing operation two or three times. Transfer the residue into the crucible and drain
                thoroughly. Dry the crucible and the residue and cool and weigh them .
           5.   CALCULATION AND EXPRESSION OF RESULTS
                Calculate the results as described in the general instructions. The value of 'd' is 1,00.
           6.   PRECISION
                On a homogeneous mixture of textile materials, the confidence limits of results obtained by this method
                are not greater than ± 1 for a confidence level of 95 % .
 ---pagebreak--- 6 . 4 . 94                                Official Journal of the European Communities                                             No C 96/39
                                                             METHOD No 6
                                          TRIACETATES AND CERTAIN OTHER FIBRES
                                                     (Method using dichloromethane)
            1 . FIELD OF APPLICATION
                 This method is applicable, after removal of non-fibrous matter, to binary mixtures of:
                 1 . triacetate (24 )
                     with
                 2 . wool ( 1 ), animal hair (2 and 3 ), silk (4 ), cotton ( 5 ), cupro (21 ), modal (22 ), viscose (25 ), acrylic
                     (26 ), polyamide or nylon ( 30 ), polyester ( 31 ) and glass fibre (40 ).
                Note:
                Triacetate fibres which have received a finish leading to partial hydrolysis cease to be completely soluble
                in the reagent. In such cases, the method is not applicable.
           2 . PRINCIPLE
                The triacetate fibre is dissolved out from a known dry mass of the mixture, with dichloromethane. The
                residue is collected, washed, dried and weighed; its mass, corrected if necessary, is expressed as a
                percentage of the dry mass of the mixture. The percentage of dry acetate is found by difference.
           3 . APPARATUS AND REAGENTS (other than those specified in the general instructions)
                3.1 . Apparatus
                      Glass-stoppered conical flask of at least 200 ml capacity;
                3.2 . Reagents
                      Dichloromethane .
           4 . TEST PROCEDURE
                Follow the procedure described in the general instructions and proceed as follows:
                To the specimen contained in the 200 ml glass-stoppered conical flask, add 100 ml of dichloromethane
                per gram of specimen, insert the stopper, shake the flask every 10 minutes to wet out the specimen and
                stand for 30 minutes at room temperature, shaking the flask at regular intervals. Decant the liquid
                through the weighed filter crucible. Add 60 ml of dichloromethane to the flask containing the residue,
                shake manually and filter the contents of the flask through the filter crucible. Transfer the residual fibres
                to the crucible by washing out the flask with a little more dichloromethane. Drain the crucible with
                suction to remove excess liquid, refill the crucible with dichloromethane and allow it to drain under
                gravity.
                Finally, apply suction to eliminate excess liquid, then treat the residue with boiling water to eliminate all
                the solvent, apply suction, dry the crucible and residue, cool and weigh them.
           5 . CALCULATION AND EXPRESSION OF RESULTS
                Calculate the results as described in the general instructions. The value of 'd' is 1,00, except in the case
                of polyester, for which the value of 'd' is 1,01 .
           6.   PRECISION
                On a homogeneous mixture of textile materials, the confidence limits of results obtained by this method
                are not greater than ± 1 for a confidence level of 95 % .
 ---pagebreak--- No C 96/40                                    Official Journal of the European Communities                                 6 . 4 . 94
                                                               METHOD No 7
                                             CERTAIN CELLULOSE FIBRES AND POLYESTER
                                                   (Method using 75 % m/m sulphuric acid )
           1 . FIELD OF APPLICATION
                This method is applicable, after removal of non-fibrous matter, to binary mixtures of:
                1 . cotton (5 ), flax ( 7), true hemp ( 8 ), ramie ( 14 ), cupro (21 ), modal ( 22 ), viscose (25 )
                    with
                2 . polyester ( 31 )
           2.  PRINCIPLE
               The cellulose fibre is dissolved out from a known dry mass of the mixture, with 75 % m/m sulphuric
                acid. The residue is collected, washed, dried and weighed; its mass is expressed as a percentage of the
               dry mass of the mixture. The proportion of dry cellulose fibre is found by difference.
           3 . APPARATUS AND REAGENTS ( other than those specified in the general instructions)
               3.1 . Apparatus
                     ( i ) Glass-stoppered conical flask of at least 500 ml capacity;
                     ( ii ) Thermostat or other apparatus for maintaining the flask at 50 + 5 °C.
               3.2 . Reagents
                     (i ) Sulphuric acid, 75 ± 2 % m/m
                            Prepare by adding carefully, while cooling, 700 ml of sulphuric acid (relative density at
                            20 °C: 1,84 ) to 350 ml of distilled water. After the solution has cooled to room temperature,
                            dilute to 1 litre with water.
                     ( ii ) Ammonia, dilute solution
                            Dilute 80 ml of ammonia solution ( relative density at 20 °C: 0,88 ) to 1 litre with water.
          4 . TEST PROCEDURE
               Follow the procedure described in the general instructions and proceed as follows:
               To the specimen contained in the glass-stoppered conical flask of at least 500 ml capacity, add 200 ml
               of 75 % sulphuric acid per gram of specimen, insert the stopper and carefully shake the flask to wet out
               the specimen. Maintain the flask at 50 ± 5 °C for one hour, shaking it at regular intervals of roughly
               10 minutes. Filter the contents of the flask through the weighed filter crucible by means of suction.
               Transfer any residual fibres by washing out the flask with a little 75 % sulphuric acid. Drain the
               crucible with suction and wash the residue on the filter once by filling the crucible with a fresh portion
               of sulphuric acid. Do not apply suction until the acid has drained under gravity.
               Wash the residue successively several times with cold water, twice with dilute ammonia solution, and
               then thoroughly with cold water, draining the crucible with suction after each addition, do not apply
               suction until each washing liquor has drained under gravity. Finally, drain the remaining liquid from the
               crucible with suction, dry the crucible and residue, and cool and weigh them .
          5.   CALCULATION AND EXPRESSION OF RESULTS
               Calculate the results as described in the general instructions . The value of 'd ' is 1,00 .
          6.   PRECISION
               On a homogeneous mixture of textile materials, the confidence limits of results obtained by this method
               are not greater than ± 1 for a confidence level of 95 % .
 ---pagebreak--- 6 . 4 . 94                                     Official Journal of the European Communities                                            No C 96/41
                                                                  METHOD No 8
            ACRYLICS, CERTAIN MODACRYLICS OR CERTAIN CHLOROFIBRES AND CERTAIN OTHER
                                                                       FIBRES
                                                       (Method using dimethylformamide)
             1 . FIELD OF APPLICATION
                  This method is applicable, after removal of non-fibrous matter, to binary mixtures of:
                   1 . acrylics (26 ), certain modacrylics (27), or certain chlorofibres (29 ) ( ! )
                       with
                  2. wool ( 1 ), animal hair (2 and 3 ), silk (4 ), cotton ( 5 ), cupro ( 21 ), modal (22 ), viscose (25 ), polyamide
                       or nylon ( 30) and polyester ( 31 ).
                       It is equally applicable to acrylics, and certain modacrylics, treated with pre-metallized dyes, but not
                       to those dyed with afterchrome dyes .
            2 . PRINCIPLE
                  The acrylic, modacrylic or chlorofibre is dissolved out from a known dry mass of the mixture, with
                  dimethylformamide heated in a water-bath at boiling-point. The residue is collected, washed, dried and
                  weighed. Its mass, corrected if necesary, is expressed as a percentage of the dry mass of the mixture and
                  the percentage of dry acrylic, modacrylic or chlorofibre is found by difference.
           3 . APPARATUS AND REAGENTS (other than those specified in the general instructions)
                  3.1 . Apparatus
                         ( i ) Glass-stoppered conical flask of at least 200 ml capacity;
                         ( ii ) Water bath at boiling point.
                  3.2 . Reagent
                        Dimethylformamide ( boiling point 153 ± 1 °C ) not containing more than 0,1 % water.
                        This reagent is toxic and the use of a hood is thus recommended.
           4 . TEST PROCEDURE
                  Follow the procedure described in the general instructions and proceed as follows:
                 To the specimen contained in the glass-stoppered conical flask of at least 200 ml capacity, add per gram
                  of specimen 80 ml of dimethylformamide, pre-heated in the water-bath at boiling point, insert the
                  stopper, shake the flask to wet out the specimen and heat in the water-bath at boiling point for one
                 hour. Shake the flask and its contents gently by hand five times during this period.
                 Decant the liquid through the weighed filter crucible, retaining the fibres in the flask. Add a further 60
                 ml of dimethylformamide to the flask and heat for a further 30 minutes, shaking the flask and contents
                 gently by hand twice during this period.
                 Filter the contents of the flask through the filter crucible by means of suction.
                 Transfer any residual fibre to the crucible by washing out the beaker with dimethylformamide. Drain the
                 crucible with suction. Wash the residue with about 1 litre of hot water at 70 — 80 °C, filling the
                 crucible each time. After each addition of water, apply suction briefly but not until the water has
                 drained under gravity. If the washing liquor drains through the crucible too slowly slight suction may be
                 applied.
                 Finally dry the crucible with the residue, cool and weigh them .
           ( ] ) The solubility of such modacrylics or chlorofibres in the reagent should be checked before carrying out the analysis.
 ---pagebreak--- No C 96/42                             Official Journal of the European Communities                                    6 . 4 . 94
           5 . CALCULATION AND EXPRESSION OF RESULTS
               Calculate the results as described in the general instructions. The value of 'd' is 1,00 except in the
               following cases:
               wool                    1,01
               cotton                  1,01
               cupro                   1,01
               modal                   1,01
               polyester               1,01
           6.  PRECISION
               On a homogeneous mixture of textile materials, the confidence limits of results obtained by this method
               are not greater than ± 1 for a confidence level of 95 % .
 ---pagebreak--- 6 . 4 . 94                                         Official Journal of the European Communities                                      No C 96/43
                                                                       METHOD No 9
                                             CERTAIN CHLOROFIBRES AND CERTAIN OTHER FIBRES
                                           (Method using 55,5/44,5 mixture of carbon disulphide and acetone)
                 1 . FIELD OF APPLICATION
                      This method is applicable, after removal of non-fibrous matter, to binary mixtures of:
                      1 . certain chlorofibres (27), namely certain polyvinal chloride fibres, whether after-chlorinated or
                           not ( 1 )
                           with
                      2 . wool ( 1 ), animal hair (2 and 3 ), silk (4), cotton (5 ), cupro (21 ), modal (22), viscose (25 ), acrylic
                           (26 ), polyamide or nylon ( 30), polyester ( 31 ), glass fibre (40).
                      When the wool or silk content of the mixture exceeds 25 %, method No 2 should be used.
                      When the polyamide or nylon, content of the mixture exceeds 25 % , method No 4 should be used.
                 2 . PRINCIPLE
                      The chlorofibre is dissolved out from a known dry mass of the mixture, with an azeotropic mixture of
                      carbon disulphide and acetone. The residue is collected, washed, dried and weighed; its mass, corrected
                      if necessary, is expressed as a percentage of the dry mass of the mixture. The percentage of dry polyvinyl
                      chloride fibre is found by difference.
                  3 . APPARATUS AND REAGENTS (other than those specified in the general instructions)
                      3.1 . Apparatus
                            (i) Glass-stoppered conical flask of at least 200 ml capacity;
                             ( ii ) Mechanical shaker.
                      3.2 . Reagents
                             (i) Azeotropic mixture of carbon disulphide and acetone (55,5 % by volume carbon disulphide to
                                    44,5 % acetone );
                                    As this reagent is toxic, the use of a hood is recommended.
                             (ii) Ethanol ( 92 % by volume) or methanol.
                  4. TEST PROCEDURE
                      Follow the procedure described in the general instructions and proceed as follows:
                      To the specimen contained in the glass-stoppered conical flask of at least 200 ml capacity, add 100 ml
                      of the azeotropic mixture per gram of specimen. Seal the flask securely, and shake the flask on a
                      mechanical shaker, or vigorously by hand, for 20 minutes at room temperature. Decant the supernatant
                      liquid through the weighed filter crucible.
                      Repeat the treatment with 100 ml of fresh reagent. Continue this cycle of operations until no polymer
                      deposit is left on a watch glass when a drop of the extraction liquid is evaporated. Transfer the residue
                      to the filter crucible using more reagent, apply suction to remove the liquid, and rinse the crucible and
                      residue with 20 ml of alcohol and then three times with water. Allow the washing liquor to drain under
                      gravity before draining with suction. Dry the crucible and residue and cool and weigh them.
                      Note:
                      With certain mixtures having a high chlorofibre content there may be substantial shrinkage of the
                      specimen during the drying procedure, as a result of which the dissolution of chlorofibre by the solvent
                      is retarded. This does not, however, affect the ultimate dissolution of the chlorofibre in the solvent.
                  5 . CALCULATION AND EXPRESSION OF RESULTS
                      Calculate the results as described in the general instructions. The value of 'd' is 1,00.
                  6 . PRECISION
                      On a homogeneous mixture of textile materials, the confidence limits of the results obtained by this
                      method are not greater than ± 1 for a confidence level of 95 % .
 (>) Before carrying out the analysis, the solubility of the chlorofibres in the reagent should be checked.
 ---pagebreak--- No C 96/44                                Official Journal of the European Communities                                     6 . 4 . 94
                                                           METHOD No 10
                                            ACETATE AND CERTAIN CHLOROFIBRES
                                                   (Method using glacial acetic acid)
           1 . FIELD- OF APPLICATION
               This method is applicable, after elemination of non-fibrous matter, to binary mixtures of:
               1 . acetate ( 19 )
                    with
               2 . certain chlorofibres (27) namely polyvinyl chloride, whether after-chlorinated or not.
           2.  PRINCIPLE
               The acetate fibre is dissolved out from a known dry mass of the mixture, with glacial acetic acid. The
               residue is collected, washed, dried and weighed; its mass, corrected if necessary, is expressed as a
               percentage of the dry mass of the mixture. The percentage of dry acetate is found by difference.
           3 . APPARATUS AND REAGENTS ( other than those specified in the general instructions )
               3.1 . Apparatus
                     (i ) Glass-stoppered conical flask of at least 200 ml capacity;
                     ( ii ) Mechanical shaker.
               3.2 . Reagent
                     Glacial acetic acid ( over 99 % ). This reagent should be handled with care since it is highly
                     caustic .
           4.   TEST PROCEDURE
                Follow the procedure described in the general instructions and proceed as follows:
                To the specimen contained in the glass-stoppered conical flask of at least 200 ml capacity, add 100 ml
                glacial acetic acid per gram of specimen . Seal the flask securely and shake on the mechanical shaker, or
                vigorously by hand, for 20 minutes at room temperature . Decant the supernatant liquid through the
                weighed filter crucible. Repeat this treatment twice, using 100 ml of fresh reagent each time, making
                three extractions in all . Transfer the residue to the filter crucible, drain with suction to remove the
                liquid and rinse the crucible and the residue with 50 ml of glacial acetic acid, and then three times with
                water. After each rinse, allow the liquid to drain under gravity before applying suction. Dry the
                crucible and residue, and cool and weigh them .
           5.  CALCULATION AND EXPRESSION OF RESULTS
               Calculate the results as described in the general instructions. The value of 'd' is 1,00 .
           6.  PRECISION
               On a homogeneous mixture of textile materials, the confidence limits of results obtained by this method
               are not greater than ± 1 for a confidence level of 95 % .
 ---pagebreak--- 6 . 4. 94                                  Official Journal of the European Communities                                   No C 96/45
                                                             METHOD No 11
                                                       SILK AND WOOL OR HAIR
                                                ( Method using 75 % m/m sulphuric acid)
          1 . FIELD OF APPLICATION
              This method is applicable, after removal of non-fibrous matter, to binary mixtures of:
              1 . silk (4 )
                    with
              2 . wool ( 1 ) or animal hair (2 and 3 ).
          2 . PRINCIPLE
              The silk fibre is dissolved out from a known dry mass of the mixture, with 75 % m/m sulphuric
              acid 0 )
              The residue is collected, washed, dried and weighed: Its mass, corrected if necessary, is expressed as a
              percentage of the dry mass of the mixture. The percentage of dry silk is found by difference.
          3 . APPARATUS AND REAGENTS (other than those specified in the general instructions)
              3.1 . Apparatus
                     Glass-stoppered conical flask of at least 200 ml capacity.
              3.2 . Reagents
                     (i) Sulphuric acid (75 ±2% m/m)
                           Prepare by adding carefully, while cooling, 700 ml sulphuric acid (density at 20 °C: 1,84) to
                           350 ml distilled water .
                           After cooling to room temperature, dilute the solution to 1 litre with water.
                     (ii ) Sulphuric acid, dilute solution: add 100 ml sulphuric acid (density at 20 °C: 1,84 ) slowly to
                           1 900 m distilled water.
                     (iii) Ammonia, dilute solution: dilute 200 ml concentrated ammonia (density at 20 °C: 0,880) to
                           1 000 ml with water.
          4.    TEST PROCEDURE
                Follow the procedure described in the general instruction and proceed as follows:
                To the specimen contained in a glass-stoppered conical flask of at least 200 ml capacity, add 100 ml of
                75 % m/m sulphuric acid per gram of specimen and insert the stopper. Shake vigorously and stand for
                 30 minutes at room temperature. Shake again and stand for 30 minutes. Shake a last time and filter the
                contents of the flask through the weighed filter crucible. Wash any remaining fibres from the flask with
                the 75 % sulphuric acid reagent. Wash the residue on the crucible successively with 50 ml of the dilute
                sulphuric acid reagent, 50 ml water and 50 ml of the dilute ammonia solution. Each time allow the
                 fibres to remain in contact with the liquid for about 10 minutes before applying suction. Finally rinse
                 with water, leaving the fibres in contact with the water for about 30 minutes. Drain the crucible with
                 suction, dry the crucible and residue, and cool and weigh them.
          5 . CALCULATION AND EXPRESSION OF RESULTS
              Calculate the results as described in the general instructions. The value of 'd' is 0,985 for wool ( J ).
          6 . PRECISION
              On a homogeneous mixture of textile materials, the confidence limits of results obtained by this method
              are not greater than ± 1 for a confidence level of 95 % .
              Wild silks, such as tussah silk, are not completely soluble in 75 % m/m sulphuric acid.
 ---pagebreak--- No C 96/46                                  Official Journal of the European Communities                                   6 . 4 . 94
                                                               METHOD No 12
                                                 JUTE AND CERTAIN ANIMAL FIRBRES
                                                  (Method by determining nitrogen content)
           1.  FIELD OF APPLICATION
               This method is applicable, after removal of non-fibrous matter, to binary mixtures of:
                1 . jute ( 9 )
                    with
               2 . certain animal fibres .
               The animal-fibre component may consist solely of hair (2 and 3 ) or wool ( 1 ) or of any mixture of the
               two. This method is not applicable to textile mixtures containing non-fibrous matter (dyes, finishes, etc.)
               with a nitrogen base.
           2.  PRINCIPLE
               The nitrogen content of the mixture is determined and from this and the known or assumed nitrogen
               contents of the two components, the proportin of each component is calculated.
           3 . APPARATUS AND REAGENTS ( other than those specified in the general instructions )
               3.1 . Apparatus
                     ( i) Kjeldahl digestion flask, 200—300 ml capacity;
                     ( ii) Kjeldahl distillation apparatus with steam injection;
                     ( iii) Titration apparatus, allowing precision of 0,05 ml.
               3.2 . Reagents
                     (i)      Toluene;
                      ( ii )   Methanol;
                      (iii )   Sulphuric acid, relative density at 20 °C: 1,84 0 );
                      ( iv )   Potassium sulphate t 1 );
                      (v)      Selenium dioxide ( ] );
                      (vi )    Sodium hydroxide solution (400 g/litre ). Dissolve 400 g of sodium hydroxide in 400—500 ml
                               of water and dilute to 1 litre with water;
                      (vii ) Mixed indicator. Dissolve 0,1 g of methyl red in 95 ml of ethanol and 5 ml of water, and mix
                               with 0,5 g of bromocresol green dissolved in 475 ml of ethanol and 25 ml of water;
                      (viii ) Boric acid solution . Dissolve 20 g boric acid in 1 litre of water;
                      (ix)     Sulphuric acid, 0,02N ( standard volumetric solution ).
           4.  PRE-TREATMENT OF TEST SAMPLE
               The following pre-treatment is substituted for the pre-treatment described in the general instructions:
               Extract the air-dry sample in a Soxhlet apparatus with a mixture of 1 volume of toluene and 3 volumes
               of methanol for 4 hours at a minimum rate of 5 cycles per hour. Allow the solvent to evaporate from
               the sample in air, and remove the last traces in an oven at 105 ± 3 °C. Then extract the sample in water
               ( 50 ml per g of sample) by boiling under reflux for 30 minutes. Filter, return the sample to the flask,
               and repeat the extraction with an identical volume of water. Filter, remove excess water from the sample
               by squeezing, suction, or centrifuging and then allow the sample to become air-dry.
           (•) These reagents should be nitrogen-free
 ---pagebreak--- 6 . 4 . 94                                 Official Journal of the European Communities                                          No C 96/47
               Note:
               The toxic effects of toluene and methanol should be borne in mind and full precautions should be taken
               in their use .
           5 . TEST PROCEDURE
               5.1 . General instructions
                     Follow the procedure described in the general instructions as regards the selection, drying and
                     weighing of the specimen.
               5.2 . Detailed procedure
                     Transfer the specimen to a Kjeldahl digestion flask. To the specimen weighing at least 1 g contained
                     in the digestion flask, add, in the following order, 2,5 g potassium sulphate, 0,1 —0,2 g selenium
                     dioxide and 10 ml sulphuric acid ( relative density 1,84 ). Heat the flask, gently at first, until the
                     whole of the fibre is destroyed, and then heat it more vigorously until the solution becomes clear
                     and almost colourless . Heat it for a further 15 minutes . Allow the flask to cool, dilute the contents
                     carefully with 10—20 ml water, cool, transfer the contents quantitatively to a 200 ml graduated
                     flask and make up to volume with water to form the digest solution.
                     Place about 20 ml of boric acid solution in a 100 ml conical flask and place the flask under the
                     condenser of the Kjeldahl distillation apparatus so that the delivery tube dips just below the surface
                     of the boric acid solution. Transfer exactly 10 ml of digest solution to the distillation flask, add not
                     less than 5 ml of sodium hydroxide solution to the funnel, lift the stopper slightly and allow the
                     sodium hydroxide solution to run slowly into the flask. If the digest solution and sodium hydroxide
                     solution remain as two separate layers, mix them by gentle agitation. Heat the distillation flask
                     gently and pass it into steam from the generator. Collect about 20 ml of distillate, lower the conical
                     flask so that the tip of the delivery tube of the condenser is about 20 mm above the surface of the
                     liquid and distil for 1 minute more. Rinse the tip of the delivery tube with water, catching the
                     washings in the conical flask. Remove the conical flask and replace it with another conical flask
                     containing roughly 10 ml of boric acid solution and collect about 10 ml distillate.
                     Titrate the two distillates separately with 0,02N sulphuric acid, use the mixed indicator. Record the
                     total titre for the two distillates. If the titre for the second distillate is more than 0,2 ml, repeat the
                     test and start the distillation again using a fresh aliquot of digest solution.
                     Carry out a blank determination, i.e. digestion and distillation using the reagents only.
           6.  CALCULATION AND EXPRESSION OF RESULTS
               6.1 . Calculate the percentage nitrogen content in the dry specimen as follows:
                                  28 (V - b ) N
                     A /o "              W
                     where
                     A = percentage nitrogen in the clean dry specimen,
                     V = total volume in ml of standard sulphuric acid used in the determination,
                     b = total volume in ml of standard sulphuric acid used in the blank determination,
                     N =      normality of standard sulphuric acid,
                     W =      dry mass ( g ) of specimen .
               6.2 . Using the values of 0,22 % for the nitrogen content of jute and 16,2 % for the nitrogen content of
                     animal fibre, both percentages being expressed on the dry mass of the fibre, calculate the
                     composition of the mixture as follows :
                     PA % =                       x 100;
                                 16,2 — 0,22
                     where
                     PA     = percentage of animal fibre in the clean dry specimen.
           7.  PRECISION
               On a homogeneous mixture of textile materials, the confidence limits of results obtained by this method
               are not greater than ± 1 for a confidence level of 95 % .
 ---pagebreak--- No C 96/48                                   Official Journal of the European Communities                                           6 . 4 . 94
                                                               METHOD No 13
                                      POLYPROPYLENE FIBRES AND CERTAIN OTHER FIBRES
                                                                (Xylene method)
            1.  FIELD OF APPLICATION
                This method is applicable, after removal of non-fibrous matter, to binary mixtures of:
                 1 . polypropylene fibres ( 33 )
                     with
                2. wool ( 1 ), animal hair (2 and 3 ), silk (4 ), cotton (5 ), acetate ( 19 ), cupro (21 ), mooal (22 ), triacetate
                     (24 ), viscose (25 ), acrylic (26 ), polyamide or nylon ( 30), polyester ( 31 ) and glass fibre (40 ).
           2.   PRINCIPLE
                The polypropylene fibre is dissolved out from a known dry mass of the mixture with boiling xylene. The
                residue is collected, washed, dried and weighed; its mass, corrected if necessary, is expressed as a
                percentage of the dry mass of the mixture. The percentage of polypropylene is found by difference.
           3 . APPARATUS AND REAGENTS ( other than those specified in the general instructions )
                3.1 . Apparatus
                       (i) Glass-stoppered conical flask of at least 200 ml capacity;
                      ( ii ) Reflux condenser (suitable for liquids of high boiling point), fitting the conical flask (i ).
                3.2 . Reagent
                      Xylene distilling between 137 and 142 °C.
                      Note:
                      This reagent is highly flammable and has a toxic vapour. Suitable precautions must be taken in its
                      use .
           4.  TEST PROCEDURE
                Follow the procedure described in the general instructions then proceed as follows:
                To the specimen contained in the concical flask. ( 3.1 . ( i)), add 100 ml of xylene ( 3.2 ) per gram of
                specimen. Attach the condenser ( 3.1 (ii )), bring the contents to the boil and maintain at boiling point for
                three minutes. Immediately decant the hot liquid through the weighed filter crucible (see Note 1 ). Repeat
               this treatment twice more, each time using a fresh 50 ml portion of solvent.
               Wash the residue remaining in the flask successively with 30 ml of boiling xylene (twice), then with 75
               ml of light petroleum (1.3.2.1 of general instructions) (twice). After the second wash with light
               petroleum, filter the contents of the flask through the crucible, transfer any residual fibres to the crucible
               with the aid of a small quantitiy of light petroleum and allow the solvent to evaporate. Dry the crucible
               and residue, cool and weigh them .
               Notes:
                1 . The filter crucible through which the xylene is to be decanted must be pre-heated.
               2 . After the treatment with boiling xylene, ensure that the flask containing the residue is cooled
                     sufficiently before the light petroleum is introduced.
               3 . In order to reduce the fire and toxicity hazards to the operator, a hot extraction apparatus using the
                     appropriate procedures, giving identical results, may be used ( 1 ).
           (!) See for example the apparatus described in 'Melliand Textilberichte' 56 ( 1975 ). p. 643 .
 ---pagebreak--- 6 . 4 . 94                              Official Journal of the European Communities                                   No C 96/49
           5 . CALCULATION AND EXPRESSION OF RESULTS
               Calculate the results as described in the general instructions. The value of 'd' is 1,00.
           6 . PRECISION
               On a homogeneous mixture of textile materials, the confidence limits of results obtained by this method
               are not greater than ± 1 for a confidence level of 95 % .
 ---pagebreak--- No C 96/50                                   Official Journal of the European Communities                                           6 . 4 . 94
                                                               METHOD No 14
               CHLOROFIBRES ( HOMOPOLYMERS OF VINYL CHLORIDE ) AND CERTAIN OTHER FIBRES
                                                     (Concentrated sulphuric acid method)
           1.   FIELD OF APPLICATION
                This method is applicable, after removal of non-fibrous matter, to binary mixtures of:
                1 . chlorofibres ( 27) based on homopolymers of vinyl chloride (after-chlorinated or not)
                    with
                2. cotton ( 5 ), acetate ( 19 ), cupro (21 ), modal (22 ), triacetate (24 ), viscose (25 ), certain acrylics (26 ),
                    certain modacrylics (29 ), plyamide or nylon ( 30) and polyester ( 31 ).
                    The modacrylics concerned are those which give a limpid solution when immersed in concentrated
                    sulphuric acid ( relative density 1,84 at 20 °C).
                    This method can be used in place of method Nos 8 and 9 .
           2.  PRINCIPLE
               The constituent other than the chlorofibre (i.e. the fibres mentioned under point 2 of paragraph 1 ) is
                dissolved out from a known dry mass of the mixture with concentrated sulphuric acid ( relative density
                1,84 at 20 °C). The residue, consisting of the chlorofibre, is collected, washed, dried and weighed; its
               mass, corrected if necessary, is expressed as a percentage of the dry mass of the mixture. The percentage
               of the second constituent is obtained by difference.
           3 . APPARATUS AND REAGENTS ( other than those specified in the general instructions )
               3.1 . Apparatus
                     ( i ) Glass-stoppered conical flask of at least 200 ml capacity;
                     ( ii ) Glass rod with flattened end .
               3.2 . Reagents
                     ( i ) Sulphuric acid, concentrated ( relative density 1,84 at 20 °C );
                     (ii ) Sulphuric acid, approximately 50 % ( m/m) aqueous solution.
                             Prepare by adding carefully, while cooling, 400 ml of sulphuric acid ( relative density 1,84 at
                             20 °C) to 500 ml of distilled or de-ionized water. After cooling to room temperature, dilute the
                             solution to one litre with water;
                     ( iii ) Ammonia , dilute solution .
                             Dilute 60 ml of concentrated ammonia solution ( relative density 0,880 at 20 °C ) to one litre
                             with distilled water .
           4 . TEST PROCEDURE
               Follow the procedure described in the general instructions, then proceed as follows:
               To the specimen contained in the flask ( 3.1.(i )) add 100 ml of sulphuric acid ( 3.2. (i )) per gram of
               specimen.
               Allow the contents of the flask to remain at room temperature for 10 minutes and during that time stir
               the test specimen occasionally by means of the glass rod. If a woven or knitted fabric is being treated,
               wedge it between the wall of the flask and the glass rod and exert a light pressure in order to separate
               the material dissolved by the sulphuric acid.
               Decant the liquid through the weighed filter crucible. Add to the flask a fresh portion of 100 ml of
               sulphuric acid ( 3.2. ( i )) and repeat the same operation . Transfer the contents of the flask to the filter
               crucible and transfer the fibrous residue there with the aid of the glass rod. If necessary, add a little
               concentrated sulphuric acid ( 3.2 . (i )) to the flask in order to remove any fibres adhering to the wall.
               Drain the filter crucible with suction; remove the filtrate by emptying or changing the filter-flask, wash
               the residue in the crucible successively with 50 % sulphuric acid solution ( 3.2.(ii )), distilled or de-ionized
 ---pagebreak--- 6 . 4 . 94                              Official Journal of the European Communities                                           No C 96/51
               water (1.3.2.3 of the general instructions, ammonia solution ( 3.2 . ( iii ) ) and finally wash thoroughly with
               distilled or de-ionized water, draining the crucible with suction after each addition. (Do not apply
               suction during the washing operation, but only after the liquid has drained off by gravity.)
               Dry the crucible and residue, cool and weigh them .
               Do not apply suction during or between the washing operations. Allow the liquid to drain under gravity
               and then apply suction.
               Finally dry the crucible with the residue, cool and weigh them .
           5 . CALCULATION AND EXPRESSION OF RESULTS
               Calculate the results as described in the general instructions. The value of 'd' is 1,00 with the following
               exceptions :
               silk     1,01
               acrylic 0,98 .
           6.  PRECISION
               On homogeneous mixtures of textile fibres, the confidence limits of results obtained by this method are
               not greater than ± 1 for a confidence level of 95 % .
 ---pagebreak--- No C 96/52                                    Official Journal of the European Communities                                         6 . 4 . 94
                                                                METHOD No 15
           CHLOROFIBRES, CERTAIN MODACRYLICS, CERTAIN ELASTANES, ACETATES, TRIACETATES
                                                        AND CERTAIN OTHER FIBRES
                                                          (Method using cyclohexanone)
            1.   FIELD OF APPLICATION
                This method is applicable, after removal of non-fibrous matter, to binary mixtures of:
                 1 . acetate ( 19 ), triacetate (24 ), chlorofibre (27), certain modacrylics (29 ), certain elastanes ( 39 )
                        with
                2 . wool ( 1 ), animal hair (2 and 3 ), silk (4 ), cotton (5 ), cupro (21 ), modal (22 ), viscose (25 ), polyamide
                        or nylon ( 30), acrylic (26 ) and glass fibre (40).
                Where modacrylics or elastanes are present a preliminary test must first be carried out to determine
                whether the fibre is completely soluble in the reagent.
                It is also possible to analyse mixtures containing chlorofibres by using method No 9 or 14.
           2.   PRINCIPLE
                The acetate and triacetate fibres, chlorofibres, certain modacrylics, and certain elastanes are dissolved
                out from a known dry mass with cyclohexanone at a temperature close to boiling point. The residue is
                collected, washed, dried and weighed; its mass, corrected if necessary, is expressed as a percentage of the
                dry mass of the mixture. The percentage of chlorofibre, modacrylic, elastane, acetate and triacetate is
                found by difference.
           3 . APPARATUS AND REAGENTS (other than those specified in the general instructions)
           3.1 . Apparatus
                  ( i)    Hot extraction apparatus suitable for use in the test procedure in section 4. ( See figure: this is a
                          variant of the apparatus described in Melliand Textilberichte 56 ( 1975 ) 643—645 );
                  ( ii ) Filter crucible to contain the specimen .
                  ( iii ) Porous baffle (porosity grade 1 );
                  (iv) Reflux condenser that can be adapted to the distillation flask;
                  ( v ) Heating device .
                3.2 . Reagents
                  (i)     Cyclohexanone, boiling point 156 °C;
                  ( ii) Ethyl alcohol, 50 % by volume.
                  NB:        Cyclohexanone is flammable and toxic. Suitable precautions must be taken in its use.
          4 . TEST PROCEDURE
                Follow the procedure described in the general instructions and then proceed as follows: "
                Pour into the distillation flask 100 ml of cyclohexanone per gram of material, insert the extraction
               container in which the filter crucible, containing the specimen and the porous baffle slightly inclined,
               have previously been placed. Insert the reflux condenser. Bring to the boil and continue extraction for
                60 minutes at a minimum rate of 12 cycles per hour. After extraction and cooling remove the extraction
               container, take out the filter crucible and remove the porous baffle. Wash the contents fo the filter
               crucible three or four times with 50 % ethyl alcohol heated to about 60 °C and subsequently with 1 litre
               of water at 60 °C .
 ---pagebreak--- 6 . 4 . 94                             Official Journal of the European Communities                                   No C 96/53
           5. CALCULATION AND EXPRESSION OF RESULTS
              Calculate the results as described in the general instructions. The value of 'd' is 1,00.
           6. PRECISION
              On a homogeneous mixture of textile materials, the confidence limits of results obtained by this method
              are not greater than ± 1 for a confidence level of 95 % .
 ---pagebreak--- No L 86/54 Official Journal of the European Communities          31 . 3 . 94
           Sketch referred to in point 3.1 .(i ) of method No 15
 ---pagebreak--- 6 . 4 . 94                          Official Journal of the European Communities                              No C 96/55
                                                             ANNEX III
                                                               PART A
                                                    REPEALED DIRECTIVES
                                                     ( referred to in Article 8 )
           — Directive 72/276/EEC and its successive amendments :
             — Directive 79/76/EEC,
             — Directive 81 /75/EEC,
             — Directive 87/ 184/EEC .
                                                               PART B
                                              TIME LIMITS FOR TRANSPOSAL
                                 Directive                                        Deadline for implementation
           — 72/276/EEG ( OJ No L 173 , 31 . 7 . 1972 , p. 1 )          18 January 1974
           — 79/76/EEC ( OJ No L 17, 24 . 1 . 1979 , p. 17 )            28 June 1979
           — 81 /75/EEC ( OJ No L 57, 4 . 3 . 1981 , p. 23 )            27 February 1982
           — 87/184/EEC ( OJ No L 75 , 17. 3 . 1987, p. 21 )            1 September 1988
 ---pagebreak--- No C 96/56                             Official Journal of the European Communities                    6 . 4 . 94
                                                         ANNEX IV
                                                   CORRELATION TABLE
                                This Directive                                    Directive 72/276/EEC
           Article 1                                              Article 1
           Article 2                                              Article 2
           Article 3                                              Article 3
           Article 4                                              Article 4
           Article 5                                              Article 5
           Article 6                                              Article 6
           Article 7                                              Article 7 ( 2 )
           Article 8                                             —
           Article 9                                              Article 8
           Annex I                                                Annex I
           Annex II ( 1 )                                         Annex II ( 1 )
           Annex II ( 2 )                                         Annex II ( 2 )
           Annex   II  method No 1                                Annex   II method    No   1
           Annex   II  method No 2                                Annex   II method    No   2
           Annex   II  method No 3                                Annex   II method    No   3
           Annex   II  method No 4                                Annex   II method    No   4
           Annex   II  method No 5                                Annex   II method    No   5
           Annex   II  method No 6                                Annex   II method    No   6
           Annex   II  method No 7                                Annex   II method    No   7
           Annex   II  method No 8                                Annex   II method    No   8
           Annex II method No 9                                   Annex II, method No 9
           Annex II method No 10                                  Annex   II method    No   10
           Annex   II method  No  11                              Annex   II method    No   11
           Annex   II method  No  12                              Annex   II method    No   13
           Annex   II method  No  13                              Annex   II method    No   14
           Annex   II method  No  14                              Annex   II method    No   15
           Annex   II method  No  15                              Annex   II method    No   16
           Annex   III                                            —
           Annex   IV                                             —