1996L0073 — EN — 20.11.2003 — 001.001 — 1
This document is meant purely as a documentation tool and the institutions do not assume any liability for its contents
►B DIRECTIVE96/73/ECOFTHEEUROPEANPARLIAMENTANDOFTHECOUNCIL
of16December 1996
oncertain methodsforthequantitativeanalysisofbinarytextile fibremixtures
(OJ L 32, 3.2.1997, p. 1)
Amended by:
Official Journal
No page date
►M1Regulation (EC) No 1882/2003 of the European Parliament and of the
Council of 29 September 2003L 284 1 31.10.2003
▼B
DIRECTIVE 96/73/EC OF THE EUROPEAN PARLIAMENT
ANDOFTHECOUNCIL
of16December 1996
on certain methods for the quantitative analysis of binary textile
fibre mixtures
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 withth e procedure laid down in Article 189b of
the Treaty (3),
Whereas Council Directive 72/276/EEC of 17 July 1972 on the approx-
imation of the laws of the Member States relating to certain methods
for the quantitative analysis of binary textile fibre mixtures (4)ha s
been amended frequently and substantially; whereas, for reasons ofclarity and rationality, the said Directive should be consolidated;
Whereas Directive 96/74/EC of the European Parliament and of the
Council of 16 December 1996 on textile names (
5) requires labelling
to indicate the fibre composition of textile products, with checks being
carried out by analysis on the conformity of these products with theindications given on the label;
Whereas the methods used for official tests carried out in the Member
States to determine the fibre composition of textile products should beuniform, as regards both the pre-treatment of the sample and its quan-
titative analysis;
Whereas Directive 96/74/EC provides that the methods for sampling
and analysis to be used in the Member States for the purpose of deter-mining the fibre composition of products will be specified in separatedirectives; whereas therefore Annex II to this Directive lays down 15uniform methods of analysis for most of the textile products composedof binary mixtures that are on the market;
Whereas technical progress necessitates frequent adaptation of the tech-
nical specifications defined by the separate directives on methods of
textile analysis; whereas, in order to facilitate the implementation ofthe measures required to that effect, a procedure should be laid downestablishing, within the Committee for Directives relating to TextileNames and Labelling, 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 forthe test may determine the composition of such mixtures using anyvalid method at its disposal, indicating in the analysis report the resultobtained and, in so far as this is known, the degree of accuracy of themethod used;1996L0073 — EN — 20.11.2003 — 001.001 — 2
(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), Council common position of 26 February 1996 (OJ No C 196,6. 7. 1996, p. 20) and Decision of the European Parliament of 18 June 1996
(OJ No C 198, 8. 7. 1996, p. 25), Council Decision of 7 October 1996.
(
4) OJ No L 173, 31. 7. 1972, p. 1. Directive as last amended by Directive 87/
184/EEC (OJ No L 75, 17. 3. 1987, p. 21).
(5) See p. 38 of this Official Journal.
▼B
Whereas the provisions of this Directive are in accordance with the
opinion of the Committee for Directives relating to Textile Names andLabelling;
Whereas this Directive must not affect the obligations of the Member
States concerning the time limits for transposition 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 samplesand 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 batchof 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 accor-
dance withDirective 96/74/EC, th e provisions in Annexes I and II on
methods for the quantitative analysis of certain binary textile fibre
mixtures, including the preparation of test samples and test specimens,are applied in all official tests to determine the composition of textileproducts 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 deter-
mine the composition of such mixtures by using any valid method at itsdisposal, indicating in the analysis report the result obtained and, in sofar as this is known, the degree of accuracy of the method used.
Article 5
1. The Commission shall be assisted by a Committee for Directives
relating to Textile Names and Labelling, hereinafter called ‘the
Committee’.
2. Adaptations to technical progress in the methods of quantitative
analysis provided for in Annex II shall be made in accordance withthe procedure laid down in Article 6.
Article 6
1. Where reference is made to this Article, Articles 5 and 7 of Deci-
sion 1999/468/EC (
1) shall apply, having regard to the provisions of
Article 8 thereof.
The period laid down in Article 5(6) of Decision 1999/468/EC shall be
set at three months.
2. The Committee shall adopt its rules of procedure.1996L0073 — EN — 20.11.2003 — 001.001 — 3
(1) Council Decision 1999/468/EC of 28 June 1999 laying down the procedures
for the exercise of implementing powers conferred on the Commission (OJ
L 184, 17.7.1999, p. 23).▼M1
▼B
Article 7
Member States shall communicate to the Commission the texts of the
main provisions of national law which they adopt in the field covered
by this Directive.
Article 8
The Directives listed in Annex III, part A, are hereby repealed, without
prejudice to the obligations of the Member States concerning the time
limits for transposition 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 correlationtable 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 .1996L0073 — EN — 20.11.2003 — 001.001 — 4
▼B
ANNEX I
PREPARATION OF TEST SAMPLES AND TEST SPECIMENS TO
DETERMINETHEFIBRECOMPOSITIONOFTEXTILEPRODUCTS
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 speci-
mens from the laboratory test samples that have been pre-treated to remove
non-fibrous matter (1).
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 facili-
tate 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 labora-
tory 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 speci-
mens in the manner described in 4.2. If the card web is disturbed by the
pre-treatment, select eachtest 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 eachof mass approximately 1 g. Subject th e 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 YARN
5.1. Yarn in packages or in banks — Sample all the packages in the bulk
laboratory sample.1996L0073 — EN — 20.11.2003 — 001.001 — 5
(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 point 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’.
▼B
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
lengthof yarn to be with drawn from eachpackage is
106
Ntcm.
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 is105
Ntcm.
6. SAMPLING FABRIC
6.1. From a laboratory bulk sample consisting of a single cutting representa-
tive 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 bex1 04
Gcm2,
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 eachlayer.
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 corre-
sponding parts of the design do not coincide.
6.2. From a laboratory bulk sample consisting of several cuttings
— Treat eachcutting as described in 6.1, and give eachresult sepa-
rately.
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 having the same fibre content, in order to check compliance with Article
9 of Directive 96/74/EC of the European Parliament and of the Council of 16
December 1996 on textile names.1996L0073 — EN — 20.11.2003 — 001.001 — 6
(1) If the packages can be mounted in a convenient creel a number can be wound simulta-
neously.
▼B
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 rela-
tion 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.1996L0073 — EN — 20.11.2003 — 001.001 — 7
▼B
ANNEX II
METHODS FOR QUANTITATIVE ANALYSIS OF CERTAIN BINARY
FIBREMIXTURES
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 unra-
velled made up of yarns of different types.
In general, the methods of chemical quantitative analysis are based on the selec-
tive 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 infor-
mation 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, suchas 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. Suchmatter, 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 agreed
allowances listed in Annex II to Directive 96/74/EC of the European Parliament
and of the Council of 16 December 1996 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 compo-
nent. 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 determina-
tions. 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 alter-
native procedures whereby the constituent that was the residue in the standard
method is dissolved out first.
I. GENERAL INFORMATION ON METHODS FOR THE QUANTITA-
TIVE CHEMICAL ANALYSIS OF TEXTILE FIBRE MIXTURES
Information common to the methods given for the quantitative chemical
analysis of fibre mixtures.1996L0073 — EN — 20.11.2003 — 001.001 — 8
▼B
I.1.Scopeandfieldofapplication
The field of application for each method specifies to which fibres the
method is applicable.
I.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 (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 andequipment
I.3.1.Apparatus
I.3.1.1. Filter crucibles and weighing bottles large enough to contain such cruci-
bles, 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 º ± 3 ºC.
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.Reagents
I.3.2.1. Light petroleum, redistilled, boiling range 40 to 60 ºC.
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.Conditioningandtestingatmosphere
Because dry masses are determined, it is unnecessary to condition the
specimen or to conduct analyses in a conditioned atmosphere.
I.5.Laboratorytestsample
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.
I.6.Pre-treatment oflaboratorytestsample (
2)
Where a substance not to be taken into account in the percentage calcu-
lations (see Article 12 (3)), of Directive 96/74/EC of the European
Parliament and of the Council of 16 December 1996 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 ºC 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 vege-
table 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.1996L0073 — EN — 20.11.2003 — 001.001 — 9
(1) Method 12 is an exception. It is based on a determination of the content of a consti-
tuent substance of one of the two components.
(2) See Annex I.1.
▼B
Analysis reports should include full details of the methods of pre-treat-
ment used.
I.7.Testprocedure
I.7.1.General instructions
I.7.1.1. Drying
Conduct all drying operations for not less than four hours and not more
than 16 hours at 105 ± 3 ºC 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. 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 two hours.
I.7.1.3. Weighing
After 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.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.
I.8.Calculationandexpressionofresults
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 agreed allowances 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.
P1%¼100 rd
m
where
P1is the percentage of clean, dry insoluble component
m 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 eachmeth od.1996L0073 — EN — 20.11.2003 — 001.001 — 10
▼B
Such values of ‘d’ are of course the normal values applicable to chemi-
cally undegraded fibres.
I.8.2. Calculation of percentage of insoluble component on clean, dry mass
basis, withadjustment by conventional factors and, wh ere appropriate,
correction factors for loss of mass during pre-treatment.
P1A%¼100 P11þa1þb1
100/C18/C19
P11þa1þb1
100/C18/C19
þ100/C0P1 ðÞ 1þa2þb2
100/C18/C19
where
P1Ais the percentage of insoluble component, adjusted by agreed allow-
ances and for loss of mass during pre-treatment
P1is the percentage of clean, dry insoluble component as calculated
from the formula shown in I.8.1.
a1is the agreed allowance for the insoluble component (see Annex II to
the Directive on textile names)
a2is the agreed allowance for the soluble component (see Annex II to
the Directive on textile names)
b1is the percentage loss of insoluble component caused by the pre-
treatment
b2is the percentage loss of soluble component caused by the pre-treat-
ment
The percentage of the second component (P2A%) is equal to 100 − P1A%.Where a special pre-treatment has been used, the values of b
1and b2should 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 b1and b2as obtained from tests performed on clean fibres similar to those in themixture under examination, should be used.
If normal pre-treatment by extraction withligh t petroleum and water is
applied, correction factors b
1and b2may 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 conven-
tionally disregarded in calculations.
II. METHOD OF QUANTITATIVE ANALYSIS BY MANUAL SEPARA-
TION
II.1.Fieldofapplication
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 propor-
tion of eachfibre in th e 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.II.3.3. Ventilated oven for drying specimens at 105 ± 3 ºC.II.3.4. Analytical balance, accurate to 0,0002 g.II.3.5. Soxhlet extractor, or other apparatus giving an identical result.1996L0073 — EN — 20.11.2003 — 001.001 — 11
▼B
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 ºC.II.4.2. Distilled or deionized water.II.5.Conditioningandtestingatmosphere
See I.4.
II.6.Laboratorytestsample
See I.5.
II.7.Pre-treatment oflaboratorytestsample
See I.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 lengthof 30 m, wh atever 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 ºC until a constant mass is obtained, as described in I.7.1 and
I.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 withweft or warp yarns,
or in the case of knitted fabrics in the line of wales and courses. Sepa-
rate the different fibre types, collect them in pre-weighed weighing
bottles and proceed as described in II.8.1.
II.9.Calculationandexpressionofresults
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 agreed allowances 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:
P
1%¼100 m1
m1þm2¼100
1þm2
m1
where
P1is the percentage of the first clean, dry component
m1is the clean, dry mass of the first component
m2is the clean, dry mass of the second component.
II.9.2. For calculation of the percentage of each component with adjustment by
agreed allowances and, where appropriate, by correction factors for loss
of matter during pre-treatment, see I.8.2.
III.1.Precision ofthemethods
The precision indicated in individual methods relates to the reproduci-
bility.
The reproducibility refers to the reliability, i.e. the closeness of agree-
ment 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
analyses made in different laboratories would, given a normal and1996L0073 — EN — 20.11.2003 — 001.001 — 12
▼B
correct application of the method to an identical and consistent mixture,
be exceeded only in five cases out of a 100.
III.2.Testreport
III.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 0,1.1996L0073 — EN — 20.11.2003 — 001.001 — 13
▼B
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 Hypochlorite
No 3 Viscose, cupro or certain
types of modalCotton Formic acid and zinc
chloride
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
modacrylics or certain
chlorofibresCertain other fibres Dimethylformamide
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
(homopolymers of vinyl
chloride)Certain other fibres Concentrated sulphuric
acid method
No 15 Chlorofibres, certain
modacrylics, certain
elastanes, acetates, tria-
cetatesCertain other fibres Cyclohexanone1996L0073 — EN — 20.11.2003 — 001.001 — 14
▼B
METHOD No 1
ACETATEANDCERTAINOTHERFIBRES
(Acetonemethod)
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), poly-
amide or nylon (30) and polyester (31).
In no circumstances is the method applicable to acetate fibres which have
been deacetylated on the surface.
2. PRINCIPLE
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 withacetone and drain withsuction. Refill th e crucible with
acetone and allow to drain under gravity.
Finally, drain the crucible with suction, dry the crucible and residue, and cool
and weighth em.
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 %.1996L0073 — EN — 20.11.2003 — 001.001 — 15
▼B
METHOD No 2
CERTAINPROTEINFIBRESANDCERTAINOTHERFIBRES
(Methodusinghypochlorite)
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), poly-
amide 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. 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 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 percen-
tage of hypochlorite is known, hypochlorite content need not be checked
iodometrically for eachanalysis, since a constant weigh ed portion of
lithium hypochlorite can be employed.
3. APPARATUS AND REAGENTS (other than those specified in the general
instructions)
3.1.Apparatus
(i) Erlenmeyer flask withground-glass stopper, 250 ml;
(ii) thermostat, adjustable to 20 (± 2) ºC.
3.2.Reagents
(i)Hypochlorite reagent
(a) Lithium hypochlorite solution
This 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 solution
This 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 eachanalysis.
(ii)Acetic acid, dilute solution
Dilute 5 ml of glacial acetic acid to 1 litre withwater.
4. TEST PROCEDURE
Follow the procedure described in the general instructions and proceed as
follows: mix approximately 1 gram of the sample with approximately1996L0073 — EN — 20.11.2003 — 001.001 — 16
▼B
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 ºC 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 washth e residue successively withwater, 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 weighth em.
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 %.1996L0073 — EN — 20.11.2003 — 001.001 — 17
▼B
METHOD No 3
VISCOSE,CUPROORCERTAINTYPESOFMODALANDCOTTON
(Methodusingformicacidandzincchloride)
1. FIELD OF APPLICATION
This method is applicable, after removal of non-fibrous matter, to binary
mixtures of:
1. viscose (25) or cupro (21), 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) ºC.
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).
NB:
Attention is drawn, in this respect, to point I.3.2.2, which lays
down that all reagents used should be chemically pure; in addi-
tion, 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 ºC. Add 100 ml of the solution of formic acid and zinc chloride,
pre-heated to 40 ºC per gram of specimen. Insert the stopper and shake
the flask vigorously. Keep the flask and its contents at a constant
temperature of 40 ºC 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 ºC. Rinse the
fibrous residue in approximately 100 ml of cold ammonia solution
(3.2.ii) ensuring that this residue remains wholly immersed in the solu-
tion 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 weighth em.1996L0073 — EN — 20.11.2003 — 001.001 — 18
(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.
▼B
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 %.1996L0073 — EN — 20.11.2003 — 001.001 — 19
▼B
METHOD No 4
POLYAMIDEORNYLON,ANDCERTAINOTHERFIBRES
(Methodusing80%m/mformic 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), polypropy-
lene (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 hypo-
chlorite).
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 dry 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 ºC: 1,186).
Dilute 880 ml of 90 % m/m formic acid (relative density at
20 ºC: 1,204) to 1 litre withwater. Alternatively, dilute 780 ml
of 98 to 100 % m/m formic acid (relative density at 20 ºC:
1,220) to 1 litre withwater.
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 ºC: 0,880) to 1 litre
withwater.
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
withsuction after eachaddition. 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 %.1996L0073 — EN — 20.11.2003 — 001.001 — 20
▼B
METHOD No 5
ACETATEANDTRIACETATE
(Methodusingbenzylalcohol)
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, withbenzyl alcoh ol at 52 ± 2 ºC.
The residue is collected, washed, dried and weighed; its mass is
expressed as a percentage of the dry mass of the mixture. The percen-
tage 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 ºC.
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 ºC,and shake for 20 minutes at this temperature.
(Instead of using a mechanical shaker, the flask may be shaken vigor-
ously 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 ºC 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 ºC. 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 weighth em.
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 %.1996L0073 — EN — 20.11.2003 — 001.001 — 21
▼B
METHOD No 6
TRIACETATESANDCERTAINOTHERFIBRES
(Methodusingdichloromethane)
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 hydro-
lysis 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 percen-
tage of the dry mass of the mixture. The percentage of dry triacetate 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.Reagent
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 weighth em.
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 %.1996L0073 — EN — 20.11.2003 — 001.001 — 22
▼B
METHOD No 7
CERTAINCELLULOSEFIBRESANDPOLYESTER
(Methodusing75%m/msulphuricacid)
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 ºC.
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 ºC: 1,84) to 350 ml of distilled
water. After the solution has cooled to room temperature, dilute
to 1 litre withwater.
(ii) Ammonia, dilute solution
Dilute 80 ml of ammonia solution (relative density at 20 ºC:
0,88) to 1 litre withwater.
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 ºC 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.
Washth e residue successively several times withcold 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 weighth em.
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 %.1996L0073 — EN — 20.11.2003 — 001.001 — 23
▼B
METHOD No 8
ACRYLICS, CERTAIN MODACRYLICS OR CERTAIN CHLOROFI-
BRESANDCERTAINOTHERFIBRES
(Methodusingdimethylformamide)
1. FIELD OF APPLICATION
This method is applicable, after removal of non-fibrous matter, to binary
mixtures of:
1. acrylics (26), certain modacrylics (29), or certain chlorofibres (27) (1)
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 necessary, 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 bathat boiling point.
3.2.Reagent
Dimethylformamide (boiling point 153 ± 1 ºC) 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 dimethylfor-
mamide, 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 ºC, filling the crucible
eachtime. After eachaddition 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 RESULTS
Calculate the results as described in the general instructions. The value
of ‘d’ is 1,00 except in the following cases:
wool 1,011996L0073 — EN — 20.11.2003 — 001.001 — 24
(1) The solubility of such modacrylics or chlorofibres in the reagent should be checked
before carrying out the analysis.
▼B
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 %.1996L0073 — EN — 20.11.2003 — 001.001 — 25
▼B
METHOD No 9
CERTAINCHLOROFIBRESANDCERTAINOTHERFIBRES
(Methodusing55,5/44,5mixtureofcarbondisulphideandacetone)
1. FIELD OF APPLICATION
This method is applicable, after removal of non-fibrous matter, to binary
mixtures of:
1. certain chlorofibres (27), namely certain polyvinyl 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 mechan-
ical 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 watchglass wh en 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 withsuction. Dry th e 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 1,00.1996L0073 — EN — 20.11.2003 — 001.001 — 26
(1) Before carrying out the analysis, the solubility of the polyvinyl chloride fibres in the
reagent should be checked.
▼B
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 confi-
dence level of 95 %.1996L0073 — EN — 20.11.2003 — 001.001 — 27
▼B
METHOD No 10
ACETATEANDCERTAINCHLOROFIBRES
(Methodusingglacial acetic acid)
1. FIELD OF APPLICATION
This method is applicable, after removal of non-fibrous matter, to binary
mixtures of:
1. acetate (19)
with
2. certain chlorofibres (27) namely polyvinyl chloride fibres, 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 percen-
tage 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 treat-
ment twice, using 100 ml of freshreagent eachtime, making th ree
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
the results obtained by this method are not greater than ± 1 for a confi-
dence level of 95 %.1996L0073 — EN — 20.11.2003 — 001.001 — 28
▼B
METHOD No 11
SILKANDWOOLORHAIR
(Methodusing75%m/msulphuricacid)
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,
with75 % m/m sulph uric 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.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 ºC: 1,84) to 350 ml distilled water.
After cooling to room temperature, dilute the solution to 1 litre
withwater.
(ii) Sulphuric acid, dilute solution: add 100 ml sulphuric acid
(density at 20 ºC: 1,84) slowly to 1 900 ml distilled water.
(iii) Ammonia, dilute solution: dilute 200 ml concentrated
ammonia (density at 20 ºC: 0,880) to 1 000 ml withwater.
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 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 withth e 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 weighth em.
5. CALCULATION AND EXPRESSION OF RESULTS
Calculate the results as described in the general instructions. The value
of ‘d’ is 0,985 for wool (1).
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 %.1996L0073 — EN — 20.11.2003 — 001.001 — 29
(1) Wild silks, suchas tussahsilk, are not completely soluble in 75 % m/m sulph uric acid.
▼B
METHOD No 12
JUTEANDCERTAINANIMALFIBRES(Methodbydeterminingnitrogencontent)
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.)
witha 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 propor-
tion of eachcomponent 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 ºC: 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 withwater.
(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 bromo-
cresol 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 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 four 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 ºC. 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 centrifu-
ging 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.1996L0073 — EN — 20.11.2003 — 001.001 — 30
(1) These reagents should be nitrogen-free.
▼B
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.Detailedprocedure
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 solutionbecomes 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 withwater 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 solu-
tion 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 distil-
late, 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 withanoth er conical flask containing
roughly 10 ml of boric acid solution and collect about 10 ml distil-
late.
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 solu-
tion.
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:
A%¼28 V /C0bðÞN
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 compo-
sition of the mixture as follows:
PA % ¼A/C00;22
16;2/C00;22/C2100
where
PA % = percentage of animal fibre in the clean dry specimen.1996L0073 — EN — 20.11.2003 — 001.001 — 31
▼B
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 %.1996L0073 — EN — 20.11.2003 — 001.001 — 32
▼B
METHOD No 13
POLYPROPYLENEFIBRESANDCERTAINOTHERFIBRES
(Xylenemethod)
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), modal (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 polypro-
pylene 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 ºC.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 conical flask (3.1 (i)), add 100 ml of
xylene (3.2) per gram of specimen. Attachth e 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 fresh50 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 petro-
leum, 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 weighth em.
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 petro-
leum 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 RESULTS
Calculate the results as described in the general instructions. The value
of ‘d’ is 1,00.1996L0073 — EN — 20.11.2003 — 001.001 — 33
(1) See for example the apparatus described in Melliand Textilberichte 56 (1975), pp. 643-
645.
▼B
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 confi-
dence level of 95 %.1996L0073 — EN — 20.11.2003 — 001.001 — 34
▼B
METHOD No 14
CHLOROFIBRES (HOMOPOLYMERS OF VINYL CHLORIDE) AND
CERTAINOTHERFIBRES
(Concentratedsulphuricacidmethod)
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 whether
after-chlorinated or not
with
2. cotton (5), acetate (19), cupro (21), modal (22), triacetate (24),
viscose (25), certain acrylics (26), certain modacrylics (29), polya-
mide 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 ºC).
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 paragraph1) is dissolved out from a known dry mass
of the mixture with concentrated sulphuric acid (relative density 1,84 at
20 ºC). 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 withflattened end.
3.2.Reagents
(i) Sulphuric acid, concentrated (relative density 1,84 at 20 ºC).
(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 ºC) to 500 ml of
distilled or de-ionized water. After cooling to room tempera-
ture, 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 ºC) to one litre withdistilled 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 neces-
sary, 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-ionizedwater (I.3.2.3 of the
general instructions, ammonia solution (3.2 (iii)) and finally washth or-
oughly with distilled or de-ionized water, draining the crucible with1996L0073 — EN — 20.11.2003 — 001.001 — 35
▼B
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 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 %.1996L0073 — EN — 20.11.2003 — 001.001 — 36
▼B
METHOD No 15
CHLOROFIBRES,CERTAINMODACRYLICS,CERTAINELASTANES,
ACETATES,TRIACETATESANDCERTAINOTHERFIBRES
(Methodusingcyclohexanone)
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 withcyclo-
hexanone 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 percen-
tage 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 ºC.
(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 of the filter crucible three or four times with 50 % ethyl
alcohol heated to about 60 ºC and subsequently with 1 litre of water at
60 ºC.
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.1996L0073 — EN — 20.11.2003 — 001.001 — 37
▼B
5. CALCULATION AND EXPRESSION OF RESULTS
Calculate the results as described in the general instructions. The value
of ‘d’ is 1,00 withth e 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 %.1996L0073 — EN — 20.11.2003 — 001.001 — 38
▼B
Figurereferred toinpoint3.1(i)ofmethodNo15
1996L0073 — EN — 20.11.2003 — 001.001 — 39
▼B
ANNEX III
PART A
REPEALEDDIRECTIVES
(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. 17)
— 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
TIMELIMITSFORTRANSPOSITION
Directive Time limits for transposition
72/276/EEC 18 January 1974
79/76/EEC 28 June 1979
81/75/EEC 27 February 1982
87/184/EEC 1 September 19881996L0073 — EN — 20.11.2003 — 001.001 — 40
▼B
ANNEX IV
CORRELATIONTABLE
This Directive Directive 72/276/EEC
Article 1 Article 1
Article 2 Article 2
Article 3 Article 3
Article 4 Article 4Article 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 11Annex 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 —1996L0073 — EN — 20.11.2003 — 001.001 — 41