COMMON POSITION (EC) No 25/96 adopted by the Council on 26 February 1996 with a view to adopting Directive 96/.../EC of the European Parliament and of the Council on certain methods for the quantitative analysis of binary textile fibre mixtures
Date: 1996-02-26
Institutions: Council of the European Union
Subjects: analytical chemistry, man-made fibre, natural fibre, plastics, textile fibre, textile product













EUR-Lex - 51996AG0706(02) - EN






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51996AG0706(02)

COMMON POSITION (EC) No 25/96 adopted by the Council on 26 February 1996 with a view to adopting Directive 96/.../EC of the European Parliament and of the Council on certain methods for the quantitative analysis of binary textile fibre mixtures  


Official Journal C 196 , 06/07/1996 P. 0020 





COMMON  POSITION (EC) No 25/96adopted by the Council on 26 February 1996with a view to adopting Directive  96/. . ./EC of the European Parliament and of the Council on certain methods for the quantitative  analysis of binary textile fibre mixtures(96/C 196/02)THE EUROPEAN PARLIAMENT AND  THE COUNCIL OF THE EUROPEAN UNION, Having regard to the Treaty establishing the European Community, and in particular Article 100a  thereof, Having regard to the proposal from the Commission (1), Having regard to the opinion of the Economic and Social Committee (2), Acting in accordance with the procedure laid down in Article 189b of the Treaty (3), Whereas Council Directive 72/276/EEC of 17 July 1972 on the approximation of the laws of the Member  States relating to certain methods for the quantitative analysis of binary textile fibre mixtures  (4) has been amended frequently and substantially; whereas, for reasons of clarity and rationality,  the said Directive should be consolidated; Whereas Directive 96/. . ./EC of the European Parliament and of the Council of . . . on textile  names (5) requires labelling to indicate the nature of the fibres in textile products, checks on  the conformity of these products with the indications given on the label being carried out by  analysis; Whereas the methods used for official tests in the Member States to determine the fibre composition  of textile products should be uniform, as regards both the pre-treatment of the sample and its  quantitative analysis; Whereas Directive . . ./. . ./EC provides that the sampling and analysing methods to be used in all  Member States for the purpose of determining the fibre composition of products will be specified in  separate directives; whereas therefore Annex II of this Directive lays down 15 uniform methods of  analysis for most of the textile products composed of binary mixtures that are on the market; Whereas developments in technology necessitate frequent adaptation of the technical specifications  defined in the separate directives on methods of textile analysis; whereas, in order to facilitate  the implementation of measures required to that effect, a procedure should be laid down  establishing, within a Committee for the Adaptation of Methods of Textile Analysis to Developments  in Technology, close cooperation between Member States and the Commission; Whereas, in the case of binary mixtures for which there is no uniform method of analysis at  Community level, the laboratory responsible for the test may determine the composition of such  mixtures using any valid method at its disposal, indicating in the analysis report the result  obtained and, in so far as this is known, the degree of accuracy of the method used; Whereas the provisions of this Directive are in accordance with the opinion of the Committee for  Directives relating to Textile Names and Labelling; Whereas this Directive must not affect the obligations of the Member States concerning the  deadlines for transposal of the Directives set out in Annex III, part B, HAVE ADOPTED THIS DIRECTIVE: Article 1 This Directive concerns methods for the quantitative analysis of  certain binary textile fibre mixtures, including the preparation of test samples and test  specimens. Article 2 'Test sample` means a sample of a suitable size for analysis, taken from laboratory  bulk samples in turn taken from a batch of articles for analysis. 'Test specimen` means that part of the test sample required to give an individual test result. Article 3 Member States shall take all necessary steps to ensure that, in accordance with  Directive . . ./. . ./EC, the provisions in Annexes I and II on methods for the quantitative  analysis of certain binary mixtures, including the preparation of test samples and test specimens,  are applied in all official tests to determine the composition of textile products put on the  market. Article 4 Any laboratory responsible for the testing of binary mixtures for which there is no  uniform method of analysis at Community level shall determine the composition of such mixtures by  using any valid method at its disposal, indicating in the analysis report the result obtained and,  in so far as this is known, the degree of accuracy of the method used. Article 5 1. A Committee for Directives relating to Textile Names and Labelling, hereinafter  called the 'Committee`, is hereby set up; it shall consist of representatives of the Member States  with a representative of the Commission as chairman. 2. The Commission shall adopt its own rules of procedure. 3. Adaptations to technological developments in the methods of quantitative analysis provided for  in Annex II shall be made in accordance with the procedure laid down in Article 6. Article 6 1. Where the procedure laid down in this Article is invoked, matters shall be referred  to the Committee by its chairman, either on his own initiative or at the request of the  representative of a Member State. 2. The representative of the Commission shall submit to the Committee a draft of the measures to be  taken. The Committee shall deliver its opinion on the draft within a time limit which the chairman  may lay down according to the urgency of the matter. The opinion shall be delivered by the majority  laid down in Article 148 (2) of the Treaty in the case of decisions which the Council is required  to adopt on a proposal from the Commission. The votes of the representatives of the Member States  within the Committee shall be weighted in the manner set out in that Article. The chairman shall  not vote. 3. (a) The Commission shall adopt the measures envisaged where they are in accordance with the  opinion of the Committee. (b) Where the measures envisaged are not in accordance with the opinion of the Committee, or if no  opinion is delivered, the Commission shall without delay propose to the Council the measures to be  adopted. The Council shall act by a qualified majority. (c) If, within three month of the proposal being submitted to it, the Council has not acted, the  proposed measures shall be adopted by the Commission. Article 7 Member States shall ensure that the texts of the main provisions of national law which  they adopt in the field covered by this Directive are communicated to the Commission. Article 8 The Directives listed in Annex III, part A shall be repealed, without prejudice to the  obligations of the Member States concerning the deadlines for transposal set out in Annex III, part  B. References to the repealed Directives shall be construed as references to this Directive and should  be read in accordance with the correlation table set out in Annex IV. Article 9 This Directive is addressed to the Member States. This Directive shall enter into force on the 20th day following that of its publication in the  Official Journal of the European Communities. Done at Brussels, . . . For the European ParliamentThe PresidentFor the CouncilThe President(1) OJ  No C 96, 6. 4. 1994, p. 20. (2) OJ No C 195, 18. 7. 1994, p. 20. (3) Opinion of the European Parliament of 15 February 1995 (OJ No C 56, 6. 3. 1995, p. 53), common  position of the Council of . . . (not yet published in the Official Journal) and decision of the  European Parliament of . . . (not yet published in the Official Journal). (4) OJ No L 173, 31. 7. 1972, p. 1. Directive as last amended by Directive 87/184/EEC. (5) See p. 1 of this Official Journal. ANNEX I PREPARATION OF TEST SAMPLES AND TEST SPECIMENS TO DETERMINE THE FIBRE  COMPOSITION OF TEXTILE PRODUCTS 1. FIELD OF APPLICATIONThis 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 (1). 2. DEFINITIONS2.1. 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. PRINCIPLEThe 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 FIBRES4.1. 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 lengths. 5. SAMPLING YARN5.1. Yarn in packages or in banks - Sample all the packages in the bulk laboratory  sample. Withdraw the appropriate continuous equal lengths from each package either by winding skeins of the  same number of turns on a wrap-reel (1), 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 lengths 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 is106  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 105 Nt cm. 6. SAMPLING FABRIC6.1. 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 104 G cm², where G is the mass of the cloth in g/m². 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 ARTICLESThe 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 having the same  fibre content, in order to check compliance with Article 9 of Directive 96/. . ./EC of the European  Parliament and of the Council of . . . on textile names. 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. (1) 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`. (1) If the packages can be mounted in a convenient creel a number can be wound simultaneously.  ANNEX II METHODS FOR QUANTITATIVE ANALYSIS OF CERTAIN BINARY FIBRE MIXTURES 1.  GENERALIntroductionMethods 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 integral 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 Directive 96/. . ./EC of the European Parliament and of the Council of . . . 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  mixturesInformation common to the methods given for the quantitative chemical analysis of fibre  mixtures. I.1. Scope and field of applicationThe field of application for each method specifies to which  fibres the method is applicable. I.2. PrincipleAfter 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  (1). 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. I.3. Materials and equipmentI.3.1. ApparatusI.3.1.1. Filter crucibles and weighing bottles large  enough to contain such crucibles, or any other apparatus giving identical results. I.3.1.2. Vacuum flask. I.3.1.3. Desiccator containing self-indicating silica gel. I.3.1.4. Ventilated oven for drying specimens at 150 ° ± 3 °C. I.3.1.5. Analytical balance, accurate to 0,0002 g. I.3.1.6. Soxhlet extractor or other apparatus giving identical results. I.3.2. ReagentsI.3.2.1. Light petroleum, redistilled, boiling range 40 to 60 °C. I.3.2.2. Other reagents are specified in the appropriate sections of each method. All reagents used  should be chemically pure. I.3.2.3. Distilled or deionized water. I.4. Conditioning and testing atmosphereBecause dry masses are determined, it is unnecessary to  condition the specimen or to conduct analyses in a conditioned atmosphere. I.5. Laboratory test sampleTake 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. I.6. Pre-treatment of laboratory test sample (2)Where a substance not to be taken into account in  the percentage calculations (see Article 12 (3)), of Directive 96/. . ./EC of the European  Parliament and of the Council of . . . 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 one  hour at a minimum rate of six cycles per hour. Allow the light petroleum to evaporate from  thesample, which is then extracted by direct treatment consisting in soaking the specimen in water  at room temperature for one hour and then soaking it in water at 65 ± 5 °C for a further 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. I.7. Test procedureI.7.1. General instructionsI.7.1.1. DryingConduct all drying operations for  not less than four 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. I.7.1.2. CoolingConduct 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 two hours. I.7.1.3. WeighingAfter cooling, complete the weighing of the weighing bottle within two minutes of  its removal from the desiccator. Weigh to an accuracy of 0,0002 g. I.7.2. ProcedureTake 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. I.8. Calculation and expression of resultsExpress 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 I.8.2. I.8.1. Calculation of percentage of insoluble component on clean, dry mass basis, disregarding loss  of fibre mass during pre-treatment. 100 rdP1 % =mwhereP1 is the percentage of clean, dry insoluble componentm is the dry mass of  the specimen after pre-treatmentr is the dry mass of the residued 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. I.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. 100 P1 (1 +a1 + b1100)P1A % =P1 (1 +a1 + b1100) + (100 - P1) (1 +a2 + b2100)whereP1A  is the percentage of insoluble component, adjusted by conventional recovery factors and for loss of  mass during pre-treatmentP1 is the percentage of clean, dry insoluble component as calculated from  the formula shown in I.8.1. a1 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)b1 is the percentage loss of insoluble component caused by the  pre-treatmentb2 is the percentage loss of soluble component caused by the pre-treatmentThe  percentage of the second component (P2A %) is equal to 100 - P1A %. Where a special pre-treatment has been used, the values of b1 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 b1 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  b1 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. II. Method of quantitative analysis by manual separationII.1. Field of applicationThis 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. PrincipleAfter 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. ApparatusII.3.1. Weighing bottle or any other apparatus giving identical results. II.3.2. Desiccator containing self-indicating silica gel. II.3.3. Ventilated oven for drying specimens at 105 ± 3 °C. II.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. ReagentsII.4.1. Light petroleum, redistilled, boiling range 40 to 60 °C. II.4.2. Distilled or deionized water. II.5. Conditioning and testing atmosphereSee I.4. II.6. Laboratory test sampleSee I.5. II.7. Pre-treatment of laboratory test sampleSee I.6. II.8. ProcedureII.8.1. Analysis of yarnSelect 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 mass is obtained, as described in I.7.1 and  I.7.2. II.8.2. Analysis of clothSelect 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. II.9. Calculation and expression of resultsExpress 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: P1 % = 100 m1m1 + m2= 1001 + m2m1whereP1 is the percentage of the first clean, dry  componentm1 is the clean, dry mass of the first componentm2 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 I.8.2. III.1. Precision of the methodsThe 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 reportIII.2.1. State that the analysis was conducted in accordance with this method. III.2.2. Give details of any special pre-treatment (see I.6). III.2.3. Give the individual results and the arithmetic mean, each to an accuracy of 0,1. >TABLE>METHOD No 1ACETATE AND CERTAIN OTHER  FABRICS(Acetone method)1. FIELD OF APPLICATIONThis method is applicable, after removal of  non-fibrous matter, to binary mixtures of: 1. acetate (19)with2. 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  surface. 2. PRINCIPLEThe 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.  ApparatusGlass-stoppered conical flasks of at least 200 ml capacity. 3.2. ReagentAcetone. 4. TEST PROCEDUREFollow 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 RESULTSCalculate the results as described in the general  instructions. The value of 'd` is 1,00. 6. PRECISIONOn 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 %. METHOD No 2CERTAIN PROTEIN FIBRES AND CERTAIN OTHER FIBRES(Method using  hypochlorite)1. FIELD OF APPLICATIONThis 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)with2.  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. PRINCIPLEThe 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 solutionThis consists of a freshly  prepared solution containing 35 (± 2) g/l of active chlorine (approximately 1 M), to which 5 (±  0,5) g/l 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 solutionThis consists of a freshly prepared solution containing 35 (± 2)  g/l of active chlorine (approximately 1 M) to which 5 (± 0,5) g/l of previously dissolved sodium  hydroxide is added. Check the active chlorine content of the solution iodometrically before each analysis. (ii) Acetic acid, dilute solutionDilute 5 ml of glacial acetic acid to 1 l with water. 4. TEST PROCEDUREFollow 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. 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 RESULTSCalculate 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. PRECISIONOn 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 %. METHOD No 3VISCOSE, CUPRO OR CERTAIN TYPES OF MODAL AND COTTON(Method using  formic acid and zinc chloride)1. FIELD OF APPLICATIONThis 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), with2. 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. PRINCIPLEThe 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 point I.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 PROCEDUREFollow 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 (1); 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. 5. CALCULATION AND EXPRESSION OF RESULTSCalculate the results as described in the general  instructions. The value of 'd` for cotton is 1,02. 6. PRECISIONOn 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 %. METHOD No 4POLYAMIDE OR NYLON, AND CERTAIN OTHER FIBRES(Method using 80 % m/m  formic acid)1. FIELD OF APPLICATIONThis method is applicable, after removal of non-fibrous  matter, to binary mixtures of: 1. polyamide or nylon, (30), with2. 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. PRINCIPLEThe 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.  ApparatusGlass-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 PROCEDUREFollow 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 RESULTSCalculate the results as described in the general  instructions. The value of 'd` is 1,00. 6. PRECISIONOn 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 %. METHOD No 5ACETATE AND TRIACETATE(Method using benzyl alcohol)1. FIELD OF  APPLICATIONThis method is applicable, after removal of non-fibrous matter, to binary mixtures of: - acetate (19)with- triacetate (24)2. PRINCIPLEThe 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 apparatus for keeping the flask at a temperature of 52 ± 2 °C. 3.2. Reagents(i) Benzyl alcohol, (ii) Ethanol. 4. TEST PROCEDUREFollow 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 RESULTSCalculate the results as described in the general  instructions. The value of 'd` is 1,00. 6. PRECISIONOn 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 %. METHOD No 6TRIACETATES AND CERTAIN OTHER FIBRES(Method using  dichloromethane)1. FIELD OF APPLICATIONThis method is applicable, after removal of non-fibrous  matter, to binary mixtures of: 1. triacetate (24)with2. 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. PRINCIPLEThe 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.  ApparatusGlass-stoppered conical flask of at least 200 ml capacity. 3.2. ReagentDichloromethane. 4. TEST PROCEDUREFollow 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 RESULTSCalculate 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. PRECISIONOn 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 %. METHOD No 7CERTAIN CELLULOSE FIBRES AND POLYESTER(Method using 75 % m/m  sulphuric acid)1. FIELD OF APPLICATIONThis 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)with2.  polyester (31). 2. PRINCIPLEThe 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/mPrepare 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 solutionDilute 80 ml of ammonia solution (relative density at 20 °C: 0,88) to  1 litre with water. 4. TEST PROCEDUREFollow 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 RESULTSCalculate the results as described in the general  instructions. The value of 'd` is 1,00. 6. PRECISIONOn 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 %. METHOD No 8ACRYLICS, CERTAIN MODACRYLICS OR CERTAIN CHLOROFIBRES AND CERTAIN  OTHER FIBRES(Method using dimethylformamide)1. FIELD OF APPLICATIONThis method is applicable,  after removal of non-fibrous matter, to binary mixtures of: 1. acrylics (26), certain modacrylics (27), or certain chlorofibres (29) (1)with2. 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. PRINCIPLEThe 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. ReagentDimethylformamide (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 PROCEDUREFollow 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. 5. CALCULATION AND EXPRESSION OF RESULTSCalculate the results as described in the general  instructions. The value of 'd` is 1,00 except in the following cases: wool 1,01cotton 1,01cupro 1,01modal 1,01polyester 1,016. PRECISIONOn 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 %. METHOD No 9CERTAIN CHLOROFIBRES AND CERTAIN OTHER FIBRES(Method using 55,5/44,5  mixture of carbon disulphide and acetone)1. FIELD OF APPLICATIONThis 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)with2. 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. PRINCIPLEThe 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 PROCEDUREFollow 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 RESULTSCalculate the results as described in the general  instructions. The value of 'd` is 1,00. 6. PRECISIONOn 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 %. METHOD No 10ACETATE AND CERTAIN CHLOROFIBRES(Method using glacial acetic  acid)1. FIELD OF APPLICATIONThis method is applicable, after elemination of non-fibrous matter,  to binary mixtures of: 1. acetate (19)with2. certain chlorofibres (27) namely polyvinyl chloride, whether  after-chlorinated or not. 2. PRINCIPLEThe 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. ReagentGlacial acetic acid (over 99 %). This reagent should be handled with care since it is  highly caustic. 4. TEST PROCEDUREFollow 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 RESULTSCalculate the results as described in the general  instructions. The value of 'd` is 1,00. 6. PRECISIONOn 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 %. METHOD No 11SILK AND WOOL OR HAIR(Method using 75 % m/m sulphuric acid)1.  FIELD OF APPLICATIONThis method is applicable, after removal of non-fibrous matter, to binary  mixtures of: 1. silk (4)with2. wool (1) or animal hair (2 and 3). 2. PRINCIPLEThe silk fibre is dissolved out from a known dry mass of the mixture, with 75 % m/m  sulphuric acid (1). 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.  ApparatusGlass-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 ml 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 PROCEDUREFollow 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 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 RESULTSCalculate the results as described in the general  instructions. The value of 'd` is 0,985 for wool (1). 6. PRECISIONOn 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 %. METHOD No 12JUTE AND CERTAIN ANIMAL FIBRES(Method by determining nitrogen  content)1. FIELD OF APPLICATIONThis method is applicable, after removal of non-fibrous matter, to  binary mixtures of: 1. jute (9)with2. 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. PRINCIPLEThe nitrogen content of the mixture is determined, and from this and the known or  assumed nitrogen contents of the two components, the proportion 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 (1). (iv) Potassium sulphate (1). (v) Selenium dioxide (1). (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 of boric acid in 1 litre of water. (ix) Sulphuric acid, 0,02N (standard volumetric solution). 4. PRE-TREATMENT OF TEST SAMPLEThe 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. Note: The toxic effects of toluene and methanol should be borne in mind and full precautions should be  taken in their use. 5. TEST PROCEDURE5.1. General instructionsFollow the procedure described in the general  instructions as regards the selection, drying and weighing of the specimen. 5.2. Detailed procedureTransfer 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 RESULTS6.1. Calculate the percentage nitrogen content in the dry  specimen as follows: A % =28 (V - b) NWwhereA = 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 % =A - 0,2216,2 - 0,22× 100; wherePA = percentage of animal fibre in the clean dry specimen. 7. PRECISIONOn 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 %. METHOD No 13POLYPROPYLENE FIBRES AND CERTAIN OTHER FIBRES(Xylene method)1.  FIELD OF APPLICATIONThis method is applicable, after removal of non-fibrous matter, to binary  mixtures of: 1. polypropylene fibres (33)with2. wool (1), animal hair (2 and 3), silk (4), cotton (5), acetate  (19), cupro (21), modal (22), triacetate (24), viscose (25), acrylic (26), polyamide or nylon (30),  polyester (31) and glass fibre (40). 2. PRINCIPLEThe 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. ReagentXylene 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 PROCEDUREFollow the procedure described in the general instructions then proceed as  follows: To the specimen contained in the conical 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 (I.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 quantity 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). 5. CALCULATION AND EXPRESSION OF RESULTSCalculate the results as described in the general  instructions. The value of 'd` is 1,00. 6. PRECISIONOn 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 %. METHOD No 14CHLOROFIBRES (HOMOPOLYMERS OF VINYL CHLORIDE) AND CERTAIN OTHER  FIBRES(Concentrated sulphuric acid method)1. FIELD OF APPLICATIONThis 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)with2.  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. PRINCIPLEThe 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 PROCEDUREFollow 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 water (I.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. 5. CALCULATION AND EXPRESSION OF RESULTSCalculate the results as described in the general  instructions. The value of 'd` is 1,00. 6. PRECISIONOn 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 %. METHOD No 15CHLOROFIBRES, CERTAIN MODACRYLICS, CERTAIN ELASTANES, ACETATES,  TRIACETATES AND CERTAIN OTHER FIBRES(Method using cyclohexanone)1. FIELD OF APPLICATIONThis  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)with2. 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. PRINCIPLEThe 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 PROCEDUREFollow 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 of 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. 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 RESULTSCalculate the results as described in the general  instructions. The value of 'd` is 1,00 with the following exceptions: silk1,01acrylic0,98. 6. PRECISIONOn 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 %. Sketch referred to in point 3.1 (i) of method No 15 >START OF GRAPHIC>>END OF GRAPHIC> (1) 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 I.1.(1) To ensure that the fibrous residue is immersed in the ammonia solution for 10 minutes, one may,  for example, use a filter crucible adaptor fitted with a tap by which the flow of the ammonia  solution can be regulated. (1) The solubility of such modacrylics or chlorofibres in the reagent should be checked before  carrying out the analysis. (1) Before carrying out the analysis, the solubility of the chlorofibres in the reagent should be  checked. (1) Wild silks, such as tussah silk, are not completely soluble in 75 % m/m sulphuric acid. (1) These reagents should be nitrogen-free. (1) See for example the apparatus described in 'Melliand Textilberichte` 56 (1975), pp. 643-645.  ANNEX III PART A REPEALED DIRECTIVES (referred to in Article 8)- Council  Directive 72/276/EEC (OJ No L 173, 31. 7. 1972, p. 1) and its successive amendments: - Commission Directive 79/76/EEC (OJ No L 17, 24. 1. 1979, p. 1)- Council Directive 81/75/EEC (OJ  No L 57, 4. 3. 1981, p. 23)- Commission Directive 87/184/EEC (OJ No L 75, 17. 3. 1987, p.  21)PART B TIME LIMITS FOR TRANSPOSAL >TABLE> ANNEX IV CORRELATION TABLE >TABLE> STATEMENT OF THE COUNCIL'S REASONS I. INTRODUCTION 1. On 25 January 1994 the  Commission submitted a proposal based on Article 100a of the EC Treaty relating to certain methods  for the quantitative analysis of binary textile fibre mixtures (1). 2. The European Parliament and the Economic and Social Committee delivered their opinions on 15  February 1995 (2) and 27 April 1994 (3) respectively. 3. On 26 February 1996 the Council adopted its common position in accordance with Article 189b of  the Treaty. II. OBJECTIVE 4. The purpose of the Commission proposal is the official  consolidation of the rules in force relating to certain methods of quantitative analysis of binary  textile fibre mixtures, with the new Directive replacing the various Directives covered by the  consolidation operation. III. ANALYSIS OF THE COMMON POSITION 5. As this is an official consolidation  within the meaning of the Interinstitutional Agreement of 20 December 1994, i.e. pure and simple  consolidation of the existing texts without substantive amendment, the Council has not, in  accordance with that Agreement, altered the substance of the Commission proposal. 6. The consolidation entails changing the legal basis from Article 100 to Article 100a of the  Treaty. For the Council and the Commission the Directive consolidates the existing legislation  without in any way amending the substance. This consolidation does not in any way change the  situation existing heretofore. (1) OJ No C 96, 6. 4. 1994, p. 20. (2) OJ No C 56, 6. 3. 1995, p. 53. (3) OJ No C 195, 18. 7. 1994, p. 10.