BS Quantitative Analysis of Fiber Mixtures

BRITISH STANDARD BS 4407:1988
Incorporating
Amendments No. 1
and No. 2
Methods for
Quantitative analysis of
fibre mixtures
ICS 59.060.01
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BS 4407:1988
Committees responsible for this

British Standard
The preparation of this British Standard was entrusted by the Textiles and
Clothing Standards Committee (TCM/-) to Technical Committee TCM/26, upon
which the following bodies were represented:
British Carpet Manufacturers’ Association Ltd.

Coopted members
Department of Trade and Industry (Laboratory of the Government Chemist)
International Wool Secretariat
Man-made Fibres Producers’ Committee
Ministry of Defence
Textile Research Council
This British Standard, having

been prepared under the
direction of the Textiles and
Clothing Standards Committee,
was published under the
authority of the Board of BSI
on 29 July 1988 and comes
into effect on
1 September 1988
© BSI 03-1999
First published January 1969 Amendments issued since publication

First revision November 1975
Second revision July 1988 Amd. No. Date of issue Comments
The following BSI references 6297 September

relate to the work on this 1990
standard:
Committee reference TCM/26 9438 May 1997 Indicated by a sideline in the margin
Draft for comment: Special
Announcement in BSI News,
February 1988
ISBN 0 580 16812 3

BS 4407:1988
Contents
Page
Committees responsible Inside front cover
Foreword ii
Section 1. General
1 Scope 1
2 Definitions 1
Section 2. Information common to the methods given for the quantitative
analysis of fibre mixtures
3 Apparatus 2
4 Reagents 2
5 Conditioning and testing atmosphere 2
6 Sample 2
7 Pretreatment of sample 2
8 Test procedure 2
9 Calculation and expression of results 3
10 Report 6
Section 3. Method of quantitative analysis by manual separation
11 General 7
12 Principle 7
13 Apparatus and reagents 7
14 Test procedure 7
15 Calculation and expression of results 7
Section 4. Methods of quantitative analysis by chemical procedures
16 Precision of the methods 8
17 Method 1. Binary mixtures of acetate and certain other fibres
(method using acetone) 8
18 Method 2. Binary mixtures of certain protein fibres
(wool, animal hair, silk or protein) and certain other fibres
(method using hypochlorite) 9
19 Method 3. Binary mixtures of viscose, cupro or certain types of
modal and cotton (method using formic acid and zinc chloride) 10
20 Method 4. Binary mixtures of polyamide 6 or polyamide 6.6
and certain other fibres (method using formic acid 80 % m/m) 11
21 Method 5. Binary mixtures of acetate and triacetate (method
using benzyl alcohol) 11
22 Method 6. Binary mixtures of triacetate and certain other fibres
(method using dichloromethane) 12
23 Method 7. Binary mixtures of certain cellulose fibres and
polyester (method using sulphuric acid 75 % m/m) 13
24 Method 8. Binary mixtures of acrylics, certain modacrylics or
certain chlorofibres and certain other fibres (method using
dimethylformamide) 13
25 Method 9. Binary mixtures of certain chlorofibres and certain
other fibres (method using carbon disulphide/acetone 55.5/44.5) 14
26 Method 10. Binary mixtures of acetate and certain chlorofibres
(method using glacial acetic acid) 15
27 Method 11. Binary mixtures of silk and wool or hair
(method using sulphuric acid 75 % m/m) 15
28 Method 12. Deleted 16
© BSI 03-1999 i
BS 4407:1988
Page
29 Method 13. Binary mixtures of jute and certain animal
fibres (method of determining the nitrogen content) 16
30 Method 14. Binary mixtures of flax and viscose
(method using sulphuric acid) 18
31 Method 15. Binary mixtures of polypropylene and certain other
fibres (method using xylene) 19
32 Method 16. Binary mixtures of chlorofibres (homopolymers
of vinyl chloride) and certain other fibres (method using
concentrated sulphuric acid) 20
33 Method 17. Binary mixtures of asbestos and certain fibres
(method based on heating to 450 °C) 20
34 Method 18. Binary mixtures of chlorofibres, certain
modacrylics, certain elastanes, acetates, triacetates and
certain other fibres (method using cyclohexanone) 21
Appendix A Procedures to be adopted for ternary fibre mixtures 26
Appendix B Agreed allowances for moisture and other matter to
be used in connection with the analysis of fibre mixtures as given in
Annex II of the EEC Directive on textile descriptions, 71/307/EEC, as
amended by Directive 83/623/EEC 26
Figure 1 — Hot extraction apparatus 22
Table 1 — Precision of methods for ternary mixtures 8
Table 2 — Procedures to be used for quantitative chemical analysis
of ternary fibre mixtures 24
Publications referred to Inside back cover
ii © BSI 03-1999
BS 4407:1988
Foreword
This revision of this British Standard has been prepared under the direction of
the Textiles and Clothing Standards Committee. It is anticipated that a revision
of the present UK regulations concerning the determination of the composition of
certain textile products will be made to bring them into line with
Directive 87/184/EEC amending Directive 72/276/EEC. Until that occurs, the
Textile Products (Determination of Composition) Regulations 1976 (SI 202/1976)
as amended by SI 767/1982 apply, when establishing and testing fibre
percentages of certain textile products. These regulations refer to BS 4407:1975,
which will be withdrawn and superseded by this standard on 1 September 1988
when the expected changes to the regulations come into operation.
The principal changes that have been made in this revision in the light of
experience gained by national laboratories and the results of inter-laboratory
trials carried out under the auspices of the EEC are as follows:
a) Method 2 has been redrafted to incorporate the use of a stable and easily
prepared additional reagent;
b) certain points in Method 8 have been amended to simplify the test
procedures and ensure uniform results;
c) Method 12 has been deleted because it has proved to be insufficiently
accurate;
d) a new Method 18 has been introduced which utilizes cyclohexanone.
Whenever possible, the fibre components of the textile being analysed should be
separated manually: for example, fabric in which the fibre in the warp is different
from that in the weft, or yarn consisting of elements which are composed of fibres
differing in type. When the different fibres form an intimate mixture, one of the
methods based on the selective solution of the individual components
(method 13 is an exception) should be used.
Semi-manufactured textiles and, to a lesser extent, finished textiles, may contain
fats, waxes or dressings, either occurring naturally or added to facilitate
processing. Salts and other water-soluble matter may also be present. Some or all
of these substances would be removed during analysis by a chemical method and
hence would be included in the soluble fibre component. Non-fibrous matter of
this type should therefore be removed before analysis and an appropriate method
of pretreatment for this purpose is given.
In addition, textiles may contain resins or other matter added to bond the fibres
together or to confer special properties, such as water-repellency or
crease-resistance. 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 is also
removed before the sample is analysed1). Dye in dyed fibres is considered to be an
integral part of the fibre and is not removed.
Most textile fibres contain water, the amount depending on the type of fibre and
on the relative humidity of the surrounding air. Analyses are conducted on the
basis of dry mass, and a procedure for determining the dry mass of test specimens
and residues is given. The result is therefore obtained on the basis of clean dry
fibres.
Provision is also made for recalculating the result after applying:
a) agreed allowances for moisture and other matter (see Appendix B), and also
b) allowances, where appropriate, for non-fibrous matter removed in
pretreatment.
For many fibres b) can usually be disregarded in calculation.
1)
Recommended procedures for removal of non-fibrous matter are given in ISO/TR 5090.
© BSI 03-1999 iii

BS 4407:1988
In some methods the insoluble component or components 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, it shall be allowed for
and correction factors for this purpose are given. These correction factors have
been determined in several laboratories by treating in the appropriate reagent,
as specified in the method of analysis, fibres cleaned by the pretreatment. These
correction factors apply only to undegraded fibres; different correction factors
may be necessary if the fibres have been degraded during processing.
The Directive 73/44/EEC, relating to the quantitative analysis of ternary fibre
mixtures allows a choice of methods based on procedures for binary mixtures. The
analyst is allowed to choose the variants used for analysis of any ternary fibre
mixture, but trials have shown that this is not entirely satisfactory. The UK
committee is of the opinion that it is preferable to limit the choice of variants to
those listed in Annex 3 of 73/44/EEC, and these are given in Table 2 of this
standard. Appendix A details procedures to be adopted for ternary fibre mixtures,
and refers to Table 2.
Parts of this standard include references, directly or indirectly, to the handling of
asbestos materials. Although the most hazardous types of this fibre (crocidolite)
have for some time been very carefully controlled, the potential dangers of
asbestos cannot be too strongly emphasized. Any person intending to use any of
the asbestos, involving parts of this standard listed below, should follow the
approved working practices with respect to asbestos as laid down by the Health
and Safety Executive. Details of relevant publications may be obtained from the
Health and Safety Executive’s Library and Information Services at:
St Hugh’s House
Stanley Precinct
Trinity Road
Bootle
Merseyside L20 3QY
The following clauses give references, directly or indirectly, to asbestos sheet:
17.3.2.1 and 25.3.2.1 (cross-reference to BS 509-1)
22.3.2.1 (cross-reference to BS 1994) 29.3.2.1
Clause 33 and Appendix B give references, directly or indirectly, to asbestos fibre.
A British Standard does not purport to include all the necessary provisions of a
contract. Users of British Standards are responsible for their correct application.
Compliance with a British Standard does not of itself confer immunity
from legal obligations.
Summary of pages
This document comprises a front cover, an inside front cover, pages i to iv,
pages 1 to 26, an inside back cover and a back cover.
This standard has been updated (see copyright date) and may have had
amendments incorporated. This will be indicated in the amendment table on
the inside front cover.
iv © BSI 03-1999
BS 4407:1988
Section 1. General
1 Scope
This British Standard describes methods for the
quantitative analysis of textile fibre mixtures after
identification of the fibre components of the
mixture, including the composition of the individual
yarns. Any non-fibrous matter is removed by a
suitable pretreatment. If the fibre components do
not form an intimate mixture and can be readily
separated by hand, the analysis is carried out by the
procedure given in section 3.
If part or the whole of the textile consists of an
intimate mixture of two fibre types (binary mixture)
one of the components is removed using a suitable
method2) following the appropriate procedure given
in section 4, and the proportion of this component is
calculated from the loss in mass. Wherever possible
it is preferable to remove the fibre present in greater
proportion, thus obtaining the fibre present in the
smaller proportion as residue.
If part or the whole of the textile consists of an
intimate mixture of three fibre types (ternary
mixture) the above process is repeated using a
second reagent. Suitable methods for the analysis of
specific ternary mixtures are given in Appendix A.
NOTE 1 To obtain a reliable result, at least two determination
should be made, either by manual separation or by chemical
separation, if the results of duplicate tests differ by more
than 2 %, two repeat determinations should be made.
NOTE 2 The titles of the publications referred to in this stand
are listed on the inside back cover.
2 Definitions
For the purposes of this British Standard, the
definition given in BS 4815 apply.
2)
Method 13 is an exception. It is based on a determination of the content of a constituent element of one of the two component
© BSI 03-1999 1
BS 4407:1988
Section 2. Information common to the methods given

for the quantitative analysis of fibre mixtures
3 Apparatus Where non-fibrous matter, e.g. size or special finish,
cannot be extracted with light petroleum and water,
3.1 Glass-filter crucibles, with sealed-in sintered
remove it by substituting for the water treatment
disc filters of porosity grade P160 complying with
described above, a suitable method that does not
BS 1752 and provided with either ground-glass
substantially alter any of the fibre constituents.
stoppers or watch glass covers. However, for some unbleached, natural vegetable
3.2 Soxhlet extractor, complying with BS 2071. fibres (e.g. jute, coir) note that normal pretreatment
3.3 Weighing bottles. with light petroleum and water does not remove all
3.4 Ventilated oven for drying specimens the natural non-fibrous substances. Do not apply
at 105 ± 3 °C. additional pretreatment unless the sample does
contain finishes insoluble in both light petroleum
3.5 Desiccator containing self-indicating silica gel. and water. Include full details of the methods of
3.6 Analytical balance, accurate to ± 0.0002 g. pretreatment used in the analysis report.
3.7 Vacuum flask.
3.8 Additional apparatus as specified in the 8 Test procedure
appropriate clauses of this standard. 8.1 General instructions
8.1.1 Drying. Conduct all drying operations for not
4 Reagents less than 4 h and not more than 16 h at 105 ± 3 °C
4.1 Light petroleum, redistilled, boiling range 40 °C in a ventilated oven with the oven door closed
to 60 °C. throughout. If the drying period is less than 14 h,
4.2 Water complying with grade 3 of BS 3978. weigh the specimen or residue to check that its mass
has become constant. The mass may be considered
4.3 Other reagents as specified in the appropriate
to have become constant if, after a further drying
clauses of this standard. of 60 min, its variation is less than 0.05 %. Where
apparatus other than a filter crucible is used,
5 Conditioning and testing conduct drying operations in the oven in such a way
atmosphere as to enable the dry mass of the fibres to be
Dry masses are determined and therefore it is determined without loss of fibre.
unnecessary to condition the specimen. The analysis 8.1.2 Drying of specimen. Dry the specimen in a
is carried out under ordinary room conditions. weighing bottle with its stopper beside it. After
drying, stopper the weighing bottle before removing
6 Sample it from the oven and transfer it quickly to a
Take a sample that is representative of the bulk and desiccator.
sufficient to provide all the specimens, each of at 8.1.3 Drying residue. Dry the residue in the filter
least 1 g, that are required. Follow the sampling crucible with its stopper or cover beside it. After
procedure as described in BS 4658. drying, close the crucible and transfer it quickly to a
desiccator.
7 Pretreatment of sample 8.1.4 Cooling. Conduct all cooling operations in the
Extract the air-dry sample in a soxhlet desiccator, the latter being placed beside the
apparatus (3.2) with light petroleum for 1 h at a balance, until complete cooling of the weighing
minimum rate of 6 cycles/hour. Allow the light bottles is attained, and in any case for not less
petroleum (4.1) to evaporate from the sample. Then than 2 h.
extract it by immersing the sample in water at room 8.1.5 Weighing. After cooling, complete the
temperature for 1 h and then immersing it in water weighing of the weighing bottle or crucible
at 65 ± 5 °C for a further hour, agitating the liquor within 2 min of its removal from the desiccator.
from time to time. Use a liquor to sample ratio NOTE Do not handle the crucibles, weighing bottles, specimens
of 100 : 1. or residues with bare hands during the drying, cooling and
weighing operations.
2 © BSI 03-1999
BS 4407:1988
8.2 Procedure 9.1.3 Determine the percentage of clean insoluble

Take from the pretreated sample a test specimen component in the mixture with agreed allowances
weighing at least 1 g. Cut yarn or dissected fabric for moisture and other matter and also allowances
into lengths of about 10 mm. Dry the specimen in a for non-fibrous matter removed in pretreatment, as
weighing bottle, cool it in a desiccator and weigh it follows:
(see 8.1.2, 8.1.4 and 8.1.5). Transfer the specimen
to the glass vessel specified in the appropriate
method, reweigh the weighing bottle immediately
and obtain the dry mass of the specimen by
difference.
Except in the case of method 13, complete the test
procedure as specified in the appropriate clause of where
the standard and examine the residue P1A is the percentage of clean insoluble
microscopically to check that the treatment has component in the mixture with agreed
completely removed the soluble fibre. allowances for moisture and other matter
and also, where appropriate, allowances
9 Calculation and expression of results for non-fibrous matter removed in the
9.1 Two-component mixtures pretreatment;
9.1.1 Express the mass of the insoluble component P1 is the percentage of clean dry insoluble
as a percentage of the total mass of fibre in the component as calculated in 9.1.2;
mixture. Calculate the results on a clean dry mass a1 is the agreed allowance added to the
basis as in 9.1.2 or on clean dry mass with agreed insoluble component for moisture and
allowances for moisture and other matter and also other matter [see Appendix B (%)];
allowances, where appropriate, for non-fibrous
matter removed in the pretreatment as in 9.1.3. a2 is the agreed allowance added to the
soluble component for moisture and other
Obtain the percentage of the soluble component by
matter [see Appendix B (%)];
difference.
b1 is the percentage loss of insoluble
9.1.2 Determine the percentage of clean dry
component caused by the pretreatment
insoluble component as follows:
(%);
100rd (%)
P 1 = ------------------ b2 is the percentage loss of soluble component
m caused by the pretreatment (%);
where The percentage of the second component (P2A is
P1 is the percentage of clean dry insoluble equal to (100 – P1A).
component; Where a special pretreatment has been used the
m is the dry mass of the specimen (g); values b1 and b2 should be determined, if possible,
by submitting each of the pure fibre constituents to
r is the dry mass of the residue (g); the pretreatment applied in the analysis. Pure
d is the correction factor for loss in mass of the fibres are those free from all non-fibrous material
insoluble component in the reagent. except those which they normally contain (either
(Suitable values of d are given in the naturally or because of the manufacturing process)
appropriate clauses of this standard.) 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, shall be adopted.
© BSI 03-1999 3
BS 4407:1988
If normal pretreatment by extraction with light d2 is the correction factor for loss in mass in
petroleum and water is applied, b1 and b2 may the first reagent, of the third component
generally be ignored except in the case of undissolved in the first specimena;
unbleached cotton, unbleached flax and unbleached d3 is the correction factor for loss in mass in
hemp where the loss due to the pretreatment is the second reagent, of the first component
usually accepted as 4 %, and in the case of undissolved in the second specimena;
polypropylene as 1 %. d4 is the correction factor for loss in mass in
In the case of other fibres, losses in the the second reagent, of the third component
pretreatment are usually disregarded in undissolved in the second specimena.
a
calculation. The values of d are indicated in the corresponding clauses of
this standard relating to the various methods of analysing
9.2 Three-component mixtures binary mixtures.
9.2.1 General. Express the mass of each component 9.2.3 Variant 2. Formulae to be applied where a
as a percentage of the total mass of the fibres in the component (a) is removed from the first test
mixture. Calculate on a clean dry mass basis as specimen leaving as residue the other two
given in 9.2.2, 9.2.3, 9.2.4, 9.2.5 (see Appendix A, components (b + c), and two components (a + b) are
variants 1 to 4) or on a clean dry mass with agreed removed from the second test specimen leaving as
allowances for moisture and other matter and also, residue the third component (c).
where appropriate, allowances for non-fibrous
matter removed in the pretreatment, as given
in 9.3.
9.2.2 Variant 1. Formulae to be applied where a
component of the mixture is removed from one
specimen and another component from a second
specimen.
where
P1 is the percentage of the first clean dry
component (component of the first specimen
soluble in the first reagent);
P2 is the percentage of the second clean dry
component (component soluble, at the same
time as the first component of the second
where specimen, in the second reagent);
P1 is the percentage of the first clean dry P3 is the percentage of the third clean dry
component (component in the first specimen component (component insoluble in both
dissolved in the first reagent); specimens);
P2 is the percentage of the second clean dry m1 is the dry mass of the first specimen after
component (component in the second pretreatment (g);
specimen dissolved in the second reagent);
P3 is the percentage of the third clean dry m2 is the dry mass of the second specimen after
component (component undissolved in both pretreatment (g);
specimens); r1 is the dry mass of the residue after removal
m1 is the dry mass of the first specimen after of the first component from the first
pretreatment (g); specimen in the first reagent (g);
m2 is the dry mass of the second specimen after
pretreatment (g); r2 is the dry mass of the residue after removal
r1 is the dry mass of the residue after removal of the first and second components from the
of the first component from the first second specimen in the second reagent (g);
specimen in the first reagent (g); d1 is the correction factor for loss in mass in
r2 is the dry mass of the residue after removal the first reagent, of the second component
of the second component from the second undissolved in the first specimena;
specimen in the second reagent (g);
d1 is the correction factor for loss in mass in d2 is the correction factor for loss in mass in
the first reagent, of the second component the first reagent, of the third component
undissolved in the first specimena; undissolved in the first specimena;
4 © BSI 03-1999
BS 4407:1988
d4 is the correction factor for loss in mass in 9.2.5 Variant 4. Formulae to be applied where two
the second reagent, of the third component components are successively removed from the
undissolved in the second specimena. mixture using the same specimen.
a
The values of d are indicated in the corresponding clauses of
binary mixtures.
9.2.4 Variant 3. Formulae to be applied where two

components (a + b) are removed from a specimen
leaving as residue the third component (c), then two
components (b + c) are removed from another where
specimen leaving as residue the first component (a). P1 is the percentage of the first clean dry
component (first soluble component);
component (second soluble component);
P3 is the percentage of the third clean dry
component (insoluble component);
m is the dry mass of the specimen after
where pretreatment (g);
P1 is the percentage of the first clean dry r1 is the dry mass of the residue after
component (component dissolved by the elimination of the first component by the
reagent); first reagent (g);
P2 is the percentage of the second clean dry r2 is the dry mass of the residue after
component (component dissolved by the elimination of the first and second
reagent); components by the first and second reagents
P3 is the percentage of the third clean dry (g);
component (component dissolved in the d1 is the correction factor for loss in mass of the
second specimen by the second reagent); second component in the first reagenta
m1 is the dry mass of the first specimen after d2 is the correction factor for loss in mass of the
pretreatment (g); third component in the first reagenta
m2 is the dry mass of the second specimen after d3 is the correction factor for loss in mass of the
pretreatment (g); third component in the first and second
r1 is the dry mass of the residue after removal reagentsa.
of the first and second components from the a
first specimen with the first reagent (g); this standard relating to the various methods of analysing
r2 is the dry mass of the residue after removal binary mixtures.
of the second and third components from the
9.3 Calculation of the percentage of each
second specimen with the second reagent
component with addition of agreed allowance
(g);
for moisture and other matter and also
d2 is the correction factor for loss in mass with allowances, where appropriate, for
the first reagent of the third component non-fibrous matter removed in the
undissolved in the first specimena; pretreatment
d3 is the correction factor for loss in mass with Given
the second reagent of the first component
undissolved in the second specimena.
a
binary mixtures.
© BSI 03-1999 5
BS 4407:1988
then Where a special pretreatment is used the values b1,

b2 and b3 should be determined, if possible, by
submitting each of the pure fibre constituents to the
pretreatment applied in the analysis. Pure fibres
are those free from all non-fibrous material except
those 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 analysed.
Where no clean separate constituent fibres used in
the manufacture of the material to be analysed are
available average values of b1, b2 and b3, as
where
obtained from tests performed on clean fibres
P1A is the percentage of the first clean dry similar to those in the mixture under examination,
component, including agreed allowance for should be used.
moisture and loss in mass during
If normal pretreatment by extraction with light
pretreatment;
petroleum and water is applied b1, b2 and b3 may
P2A is the percentage of the second clean dry generally be ignored, except in the case of
component, including agreed allowance for unbleached cotton, unbleached flax and unbleached
moisture and loss in mass during hemp where the loss due to pretreatment is usually
pretreatment; accepted as 4 % and in the case of polypropylene
P3A is the percentage of the third clean dry as 1 %.
component, including agreed allowance for In the case of other fibres, losses in the
moisture and loss in mass during pretreatment are usually disregarded in
pretreatment; calculations.
P1 is the percentage of the first clean dry
component obtained by one of the formulae
10 Report
given in 9.2; 10.1 State that the analysis was conducted in
accordance with the appropriate method(s) of this
component obtained by one of the formulae standard.
given in 9.2; 10.2 State whether the result relates to the overall
composition of the assembly or to an individual
P3 is the percentage of the third clean dry
component of the assembly.
component obtained by one of the formulae
given in 9.2; 10.3 Give details of any special treatment for the
removal of size or finish given in substitution for or
a1 is the agreed allowance for moisture of the addition to the specified pretreatment.
first component (see Appendix B) (%);
10.4 State the number of individual determinations
a2 is the agreed allowance for moisture of the made. Give the individual results and the
second component (see Appendix B) (%); arithmetic mean, each to an accuracy of 0.1 %.
a3 is the agreed allowance for moisture of the 10.5 State whether the result is based on:
third component (see Appendix B) (%); a) clean dry mass;
b1 is the percentage of loss in mass of the first b) clean dry mass with agreed allowances for
component during pretreatment; moisture and other matter and also, where
b2 is the percentage of loss in mass of the appropriate, for non-fibrous matter removed in
second component during pretreatment; the pretreatment, and state the values of the
allowances used.
b3 is the percentage of loss in mass of the
third component during pretreatment; 10.6 Whenever possible, state the precision of the
method for each component for ternary mixtures.
X, Y, Z are correction factors. Calculate the precision according to Table 1
(see clause 16).
6 © BSI 03-1999
BS 4407:1988
Section 3. Method of quantitative analysis by manual

separation
11 General 15 Calculation and expression of
This method is applicable to textile fibre mixtures of results
all types, provided that they do not contain an 15.1 General
intimate mixture of two or more different fibres,
Express the mass of each fibre constituent as a
which can be separated by hand.
percentage of the total mass of the fibres in the
mixture. Calculate the results on a clean, dry mass
12 Principle basis or on a clean dry mass with agreed allowances
After identification of the constituents of the fibre for moisture and other matter and also, where
mixture including the composition of the individual appropriate, for non-fibrous matter removed in the
yarns, the non-fibrous material is removed by pretreatment.
suitable pretreatment and then the constituents are 15.2 Method based on clean dry mass
separated by hand, dried and weighed in order to
calculate the proportion of each fibre in the mixture. 15.2.1 Binary mixtures
13 Apparatus and reagents

13.1 Apparatus
The following apparatus, together with apparatus where
specified in clause 3, is required.
P1 is the percentage of the first clean, dry
13.1.1 Needle. component;
13.1.2 Twist tester, or similar apparatus. P2 is the percentage of the second clean, dry
13.2 Reagents component;
No additional reagents are required. m1 is the clean, dry mass of the first
component (g);
14 Test procedure m2 is the clean, dry mass of the second
component (g).
14.1 Analysis of yarn
15.2.2 Ternary mixtures
Select from the pretreated sample a specimen
weighing 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 weighing
bottles and dried at a temperature of 105 ± 3 °C
until a constant mass is obtained, as described
in 8.1. Remove the fibre, re-weigh the weighing
bottle immediately and determine the mass of fibre where
by difference. P1 is the percentage of the first clean, dry
14.2 Analysis of fabric component;
Select from the pretreated sample, well away from P2 is the percentage of the second clean, dry
all selvedges, a specimen weighing not less than 1 g, component;
with edges carefully trimmed and running parallel P3 is the percentage of the third clean, dry
with weft or warp yarns, or in the case of knitted component;
fabrics in the line of wales and courses. In the case m1 is the clean, dry mass of the first
of knitted fabrics, ensure that all cut loops are component (g);
removed before selection of the specimen. Separate m2 is the clean, dry mass of the second
the different fibre types, collect them in weighing component (g);
bottles and proceed as described in 14.1. m3 is the clean, dry mass of the third
component (g).
15.3 For calculation of the percentage of each
component with adjustment for agreed allowance
for moisture and other matter and also, where
appropriate, for non-fibrous matter removed in the
pretreatment, see 9.1.3 in the case of binary
mixtures and 9.2 and 9.3 in the case of ternary
mixtures.
© BSI 03-1999 7
BS 4407:1988
Section 4. Methods of quantitative analysis by

chemical procedures
16 Precision of the methods 17 Method 1. Binary mixtures of
The precision indicated in individual methods acetate and certain other fibres
relates to the reproducibility. Reproducibility refers (method using acetone)
to the reliability, i.e. the closeness of agreement 17.1 General
between experimental values obtained by operators
in different laboratories, or at different times using This method is applicable, after removal of
the same method and obtaining individual results non-fibrous matter, to binary mixtures of acetate
on specimens of an identical homogeneous mixture. with cotton, wool, animal hair, silk, protein,
polyamide, polyester, acrylic, flax, true hemp, jute,
The reproducibility is expressed by confidence limits abaca, alfa, coir, broom, ramie, sisal, modal, cupro
of the results for a confidence level of 95 %. and viscose. It is not applicable to mixtures
By this is meant that the difference between two containing modacrylic. In no circumstances is the
results in a series of analyses made in different method applicable to acetate which has been
laboratories would, given a normal and correct deacetylated on the surface.
application of the method to an identical and
17.2 Principle
homogeneous mixture, be exceeded only in five
cases out of a hundred. The acetate is dissolved from a known dry mass of
the mixture using acetone. The residue is collected,
To determine the precision of the analysis of a
washed, dried, and weighed. Its mass is expressed
ternary mixture the values indicated in the methods
as a percentage of the dry mass of the mixture. The
for the analysis of binary mixtures which have been
percentage of acetate is found by difference.
used to analyse the ternary mixture are applied in
the usual way. 17.3 Apparatus and reagents
Given that in the four variants (see Appendix A) of The following apparatus and reagents, together
the quantitative chemical analysis of ternary with those specified in clauses 3 and 4, are required.
mixtures, provision is made for two dissolutions 17.3.1 Apparatus
(using two separate specimens for the first three
variants and a single specimen for the fourth 17.3.1.1 Conical flask, capacity 250 mL, with
variant), and assuming E1 and E2 denote the ground glass stopper.
precision of the two methods for analysing binary 17.3.2 Reagent
mixtures, the precision of the results for each 17.3.2.1 Acetone complying with BS 509-1.
component is shown in Table 1.
17.4 Test procedure
Table 1 — Precision of methods for ternary
mixtures Follow the procedure described in 8.2 and proceed
as follows.
Component Variant
fibre To the specimen contained in the stoppered conical
1 2 and 3 4 flask (17.3.1.1) add 100 mL of acetone (17.3.2.1) per
a E1 E1 E1 gram of specimen, insert the stopper, shake the
flask, and stand it for 30 min at room temperature
b E2 E1 + E2 E1 + E2 shaking it occasionally. Decant the liquid through
c E1 + E2 E2 E1 + E2 the weighed filter crucible retaining the fibres in the
flask. Repeat the treatment twice more (making
If the fourth variant is used, the degree of precision three extractions in all) but for periods of 15 min
may be found to be lower than that calculated by the only, so that the total time of treatment in acetone
method indicated above, owing to possible action of is 1 h. Wash the residue into the filter crucible with
the first reagent on the residue consisting of acetone, and drain with suction. Refill the crucible
components (b) and (c), which would be difficult to with acetone and allow it to drain under gravity.
evaluate. Finally, drain the crucible with suction, dry the
crucible and residue, and cool and weigh them
(see 8.1.3, 8.1.4 and 8.1.5).
17.5 Calculation and expression of results
Calculate the results as described in 9.1. The value
of d is 1.00.
8 © BSI 03-1999
BS 4407:1988
17.6 Precision b) sodium hypochlorite solution,

On a homogeneous mixture of textile materials, the containing 35 ± 2 g/L of active chlorine
confidence limits of results obtained by this method and 5 ± 0.5 g of sodium hydroxide, prepared as
are not greater than ± 1 for a confidence level follows.
of 95 %. Standardize iodometrically a supply of sodium
hypochlorite solution available commercially to
18 Method 2. Binary mixtures of establish its active chlorine content. Calculate
certain protein fibres (wool, animal the dilution necessary to convert it to an active
hair, silk or protein) and certain other chlorine content of 3.5 %, and therefore the
volume of concentrated hypochlorite solution
fibres (method using hypochlorite)
needed to produce 1 L of the required reagent. To
18.1 General this amount of the concentrated solution, add the
This method is applicable, after removal of whole of a solution containing 5 ± 0.5 g of sodium
non-fibrous matter, to binary mixtures of hydroxide in 200 mL of water and dilute to 1 L
with water. Mix well, and prepare freshly each
a) wool, animal hair, silk and protein based on
day
casein; with
NOTE Lithium hypochlorite is recommended in cases involving
b) cotton, cupro, elastane, modal, viscose, acrylic, a small number of analyses or for analyses conducted at fairly
chlorofibres, polyamide, polyester or nylon, lengthy intervals, because the percentage of active chlorine in
polypropylene and glass. solid lithium hypochlorite, unlike that in sodium hypochlorite, is
virtually constant.
If different protein fibres are present, the method 18.3.2.2 Acetic acid solution. Dilute 5 mL of glacial
gives the total of their amounts, but not their acetic acid (approximately 99.7 % (m/m), Ô
individual quantities. approximately 1.06 g/m mL) to 1 L with water.
18.2 Principle 18.4 Procedure
The protein fibre is dissolved out from a known dry Follow the procedure described in 8.2 and proceed
mass of the mixture, with a hypochlorite solution. as follows.
The residue is collected, washed, dried and weighed.
Its mass, corrected if necessary, is expressed as a Mix approximately 1 g of the specimen with
percentage of the dry mass of the mixture. The approximately 100 mL of the hypochlorite
percentage of dry protein fibre is found by solution (18.3.2.1) in the flask (18.3.1.1) and agitate
difference. thoroughly to wet out the specimen.
18.3 Apparatus and reagents Maintain the flask for 40 min at 20 ± 2 °C and
agitate continuously.
The following apparatus and reagents, together NOTE 1 To ensure fibres completely dissolve in 40 min, a
with those specified in clauses 3 and 4, are wetting agent may be required.
required. NOTE 2 Since the dissolution of the wool proceeds
exothermically, the heat of reaction of this method has to be
18.3.1 Apparatus distributed and removed. Otherwise, considerable errors may be
18.3.1.1 Erlenmeyer flask, capacity 250 mL, with caused by the incipient dissolution of the non-soluble fibres.
ventilated, loose fitting stopper. After 40 min, filter the flask contents through a
18.3.1.2 Means of controlling temperature weighed glass-filter crucible (3.1) and transfer any
residual fibres into the filter crucible by rinsing the
at 20 ± 2 °C.
flask with a little hypochlorite reagent. Drain the
18.3.2 Reagents crucible with suction and wash the residue
18.3.2.1 Hypochlorite reagent consisting of either successively with water, dilute acetic acid (18.3.2.2)
a) lithium hypochlorite solution. Dissolve and finally water, draining the crucible with suction
either 100 g of lithium hypochlorite after each addition. Do not apply suction until each
containing 35 % active chlorine or 115 g washing liquor has drained under gravity.
containing 30 % active chlorine in Finally, drain the crucible with suction, dry the
approximately 700 mL of water. Add 5 g of crucible and residue, and cool and weigh them
sodium hydroxide (NaOH) dissolved in (see 8.1.3, 8.1.4 and 8.1.5).
approximately 200 mL of water and dilute to 1 L 18.5 Calculation and expression of results
with water. Prepare this solution freshly each
day; or
of d is 1.00, except for cotton, viscose and modal, for
which d = 1.01, and unbleached cotton, for which
d = 1.03.
© BSI 03-1999 9
BS 4407:1988
18.6 Precision 19.3.2.2 Dilute ammonia solution. Dilute 20 mL of

On a homogeneous mixture of textile materials, the concentrated ammonia solution
confidence limits for results obtained by this method (approximately 35 % (m/m), Ô
are not greater than ± 1 for a confidence level approximately 0.88 g/mL) to 1 L with water.
of 95 %. 19.4 Test procedure
Follow the procedure described in 8.2 and proceed
19 Method 3. Binary mixtures of as follows.
viscose, cupro or certain types of Place 100 mL of the formic acid and zinc chloride
modal and cotton (method using solution per gram of specimen in the conical flask,
formic acid and zinc chloride) heat it to a temperature of 40 °C and add the
19.1 General specimen. Insert the stopper and shake the flask
vigorously. Keep the flask and its contents at a
This method is applicable, after removal of
constant temperature of 40 ± 2 °C for 2.5 h, shaking
non-fibrous matter, to binary mixtures of viscose,
the flask at hourly intervals. Filter the contents of
cupro or certain types of modal with cotton. If modal
the flask through the weighed filter crucible and,
is found to be present, a preliminary test should be using more reagent, transfer to the crucible any
carried out to see whether it is soluble in the fibres remaining in the flask. Wash the crucible and
reagent, under the conditions of test. For certain
residue with a further 20 mL of the reagent at 40 °C
types of modal fibre which are difficult to dissolve,
and then wash the crucible and residue thoroughly
the procedure, modified as described in 19.4, may be
with water at a temperature of 40 °C. For certain
used.
modal fibres for which the method is not suitable,
This method is not applicable to mixtures in which use the same method but maintain the temperature
the cotton has suffered extensive chemical of the reagent at 70 ± 2 °C for a period
degradation, nor when the viscose, cupro or modal is of 20 ± 1 min. Rinse with a further 10 mL of reagent
rendered incompletely soluble by the presence of preheated to 70 °C and then wash the crucible and
certain dyes or finishes that cannot be removed residue thoroughly with water also at 70 °C. Rinse
completely by pretreatment. the fibrous residue with approximately 100 mL of
19.2 Principle cold ammonia solution ensuring that the residue
remains wholly immersed in solution for 10 min.
The viscose, cupro or modal is dissolved from a
NOTE To ensure that the fibrous residue is immersed
known dry mass of the mixture, using a reagent for 10 min in the ammonia solution, it is possible, for example, to
containing formic acid and zinc chloride. The add to the filtering apparatus an adaptor fitted with a tap by
residue is collected, washed, dried and weighed. Its which the flow of ammonia solution can be regulated.
corrected mass is expressed as a percentage of the Drain the crucible with suction and then rinse with
dry mass of the mixture. The percentage of dry cold water. Do not apply suction until each washing
viscose, cupro or modal is found by difference. liquor has drained under gravity. Finally, drain the
19.3 Apparatus and reagents remaining liquid with suction, dry the crucible and
residue and cool and weigh them
The following apparatus and reagents, together (see 8.1.3, 8.1.4 and 8.1.5).
with those specified in clauses 3 and 4, are
required. 19.5 Calculation and expression of results
19.3.1 Apparatus Calculate the results as described in 9.1. The value
of d is 1.02.
19.3.1.1 Conical flask, capacity 250 mL, with
ground glass stopper. If the high temperature procedure is used, the value
of d is 1.03.
19.3.1.2 Means of controlling the temperature of the
flask and contents at 40 ± 2 °C (or 70 ± 2 °C if the 19.6 Precision
high temperature method is used). On a homogeneous mixture of textile materials, the
19.3.2 Reagents confidence limits of results obtained by this method
are not greater than ± 2 for a confidence level
19.3.2.1 Formic acid/zinc chloride solution
of 95 %.
Either prepare a solution containing 20 g of
anhydrous zinc chloride and 68 g (56 mL) of formic
acid (96 % to 100 % m/m) made up to 100 g with
water or alternatively prepare a solution of 20 parts
by mass of zinc chloride to 76 parts by mass
of 90 % m/m formic acid (63 mL) plus 4 parts of
water.
10 © BSI 03-1999
BS 4407:1988
20 Method 4. Binary mixtures of 20.4 Test procedure

polyamide or nylon and certain other Follow the procedure described in 8.2 and proceed
fibres (method using formic as follows.
acid 80 % m/m) To the specimen contained in the glass-stoppered
20.1 General conical flask (20.3.1.1), add 100 mL of the formic
acid per gram of specimen, insert the stopper, shake
This method is applicable, after removal of the flask to wet out the specimen and stand it
non-fibrous matter, to binary mixtures of polyamide for 15 min, shaking it at intervals. Filter the
or nylon with cotton, animal hair, cupro, modal, contents of the flask through a weighed filter
viscose, chlorofibre, polypropylene, acrylic, crucible and transfer any residual fibres to the
polyester or glass fibre. It is applicable also to crucible by washing out the flask with more formic
mixtures with wool or animal hair, but when the acid reagent. Drain the crucible with suction and
animal fibre content exceeds 25 %, the method wash the residue on the filter successively with
described in clause 18 shall be used. formic acid reagent, hot water, dilute ammonia
NOTE This method applies to polyamide 6 or polyamide 6.6 solution, and finally cold water, draining the
and not to other polyamides.
crucible with suction after each addition. Do not
20.2 Principle apply suction until each washing liquor has drained
The polyamide is dissolved from a known dry mass under gravity. Finally, drain the crucible with
of the mixture using aqueous formic acid. The suction, dry the crucible and residue, and cool and
residue is collected, washed, dried, and weighed. Its weigh them (see 8.1.3, 8.1.4 and 8.1.5).
mass is expressed as a percentage of the dry mass of 20.5 Calculation and expression of results
the mixture. The percentage of polyamide or nylon
is found by difference.
of d is 1.00.
20.3 Apparatus and reagents
20.6 Precision
The following apparatus and reagents, together
On a homogeneous mixture of textile materials, the
with those specified in clauses 3 and 4, are required.
confidence limits of results obtained by this method
20.3.1 Apparatus are not greater than ± 1 for a confidence level
20.3.1.1 Conical flask, capacity minimum 200 mL, of 95 %.
with ground glass stopper.
21 Method 5. Binary mixtures of
20.3.2 Reagents
acetate and triacetate (method using
20.3.2.1 Formic acid solution benzyl alcohol)
(approximately 80 % (m/m), Ô
approximately 1.19 g/mL). Dilute 880 mL of formic 21.1 General
acid (approximately 90 % (m/m), Ô This method is applicable after the removal of
approximately 1.20 g/mL) to 1 L with water. non-fibrous matter, to binary mixtures of acetate
The concentration is not critical within the with triacetate.
range 77 % to 83 % m/m formic acid. 21.2 Principle
Alternatively, dilute 780 mL of 98 % to 100 % m/m The acetate is dissolved from a known dry mass of
formic acid relative density at (20 °C : 1.220) to 1 L the mixture using benzyl alcohol. The residue is
with water. collected, washed, dried and weighed. Its mass is
20.3.2.2 Dilute ammonia solution. Dilute 80 mL of expressed as a percentage of the dry mass of the
concentrated ammonia solution mixture. The percentage of acetate is found by
(approximately 35 % (m/m), Ô difference.
approximately 0.88 g/mL) to 1 L with water. 21.3 Apparatus and reagents
21.3.1 Apparatus
ground glass stopper.
21.3.1.2 Mechanical shaker.
21.3.1.3 Means of controlling the temperature of the
flask and contents at 52 ± 2 °C.
© BSI 03-1999 11
BS 4407:1988
21.3.2 Reagents 22.2 Principle

21.3.2.1 Benzyl alcohol. The triacetate is dissolved from a known dry mass of
21.3.2.2 Ethanol complying with BS 507. the mixture with dichloromethane. The residue is
collected, washed, dried, and weighed. Its mass,
21.4 Test procedure corrected if necessary, is expressed as a percentage
Follow the procedure described in 8.2 and proceed of the dry mass of the mixture. The percentage of
as follows. triacetate is found by difference.
To the specimen contained in the conical 22.3 Apparatus and reagents
flask (21.3.1.1), add 100 mL of benzyl alcohol per
The following apparatus and reagent, together with
gram of specimen. Insert the stopper, secure the
those specified in clauses 3 and 4, are required.
flask to the shaker so that it is immersed in the
water-bath, kept at a temperature of 52 ± 2 °C, and 22.3.1 Apparatus
shake for 20 min at this temperature. 22.3.1.1 Conical flask, capacity 250 mL, with
Decant the liquid through the weighed filter ground glass stopper.
crucible retaining the fibres in the flask. Add a 22.3.2 Reagent
further quantity of benzyl alcohol to the flask and
shake as before for 20 min. Decant the liquid 22.3.2.1 Dichloromethane (methylene chloride),
through the crucible retaining the fibres in the complying with BS 1994.
flask. Repeat the cycle of operations a third time. 22.4 Test procedure
Finally, pour the liquid and the residue into the Follow the procedure described in 8.2 and proceed
crucible; wash any fibres remaining in the flask into as follows.
the crucible with more benzyl alcohol at a
To the specimen contained in the glass-stoppered
temperature of 52 ± 2 °C. Drain the crucible
conical flask, add 100 mL of dichloromethane per
thoroughly. Transfer the fibres into a flask, rinse
with ethanol and, after shaking manually, decant gram of specimen, insert the stopper, shake the
through the filter crucible retaining the fibres in the flask to wet out the specimen, and allow the flask to
stand for 30 min, shaking it occasionally. Decant
flask. Repeat this rinsing operation two or three
the liquid through the weighed filter crucible
times. Transfer the residue to the crucible and drain
retaining the fibres in the flask. Add 60 mL of
thoroughly. Dry the crucible and residue and cool
dichloromethane to the residue in the flask, replace
and weigh them (see 8.1.3, 8.1.4 and 8.1.5).
the stopper, shake it by hand, and filter the contents
21.5 Calculation and expression of results of the flask through the filter crucible. Transfer any
Calculate the results as described in 9.1. The value residual fibres to the crucible by washing out the
of d is 1.00. flask with more dichloromethane. Drain the crucible
with suction, refill the crucible with
21.6 Precision
dichloromethane, and allow it to drain under
On a homogeneous mixture of textile materials, the gravity. Finally, drain the crucible with suction.
confidence limits of results obtained by this method
If the residue is glass fibre, polyamide, polyester,
protein, or acrylic, dry the crucible and residue and
of 95 %. cool and weigh them (see 8.1.3, 8.1.4 and 8.1.5).
22 Method 6. Binary mixtures of If the residue is other fibres, treat it in the following
triacetate and certain other fibres way to remove solvent that cannot be removed by
oven-drying.
(method using dichloromethane)
Transfer the residue by means of forceps to a beaker
22.1 General containing about 100 mL of boiling water. Continue
This method is applicable, after removal of boiling for 5 min, and then decant through the same
non-fibrous matter, to binary mixtures of triacetate filter crucible retaining the fibres in the beaker. Add
with wool, animal hair, silk, cotton, cupro, modal, about 100 mL of boiling water to the residue in the
viscose, polyamide, or nylon, polyester, protein, beaker, boil it for 5 min, and again decant retaining
acrylic or glass fibre. It is not applicable to triacetate the fibres in the beaker. Give a third boiling
which has received a finish leading to partial treatment and transfer the residue to the filter
hydrolysis. crucible. Allow the water to drain under gravity and
then drain with suction. Wash any residual fibres
from the beaker into the crucible with water.
Finally, drain the crucible with suction, dry the
crucible and residue and cool and weigh them
(see 8.1.3, 8.1.4 and 8.1.5).
12 © BSI 03-1999
BS 4407:1988
22.5 Calculation and expression of results 23.4 Test procedure

Calculate the results as described in 9.1. The value Follow the procedure described in 8.2 and proceed
of d is 1.00 except for polyester fibre, for which d as follows.
is 1.01. To the specimen contained in the glass-stoppered
22.6 Precision conical flask, add 200 mL of sulphuric
On a homogeneous mixture of textile materials, the acid (23.3.2.1) per gram of specimen, insert the
confidence limits of results obtained by this method stopper, and shake the flask carefully to wet out the
specimen. Maintain the flask at a temperature
of 50 ± 5 °C for 1 h, shaking the flask and contents
of 95 %.
gently at intervals of about 10 min. Filter the
23 Method 7. Binary mixtures of contents of the flask through a weighed filter
crucible by means of suction. Transfer any residual
certain cellulose fibres and polyester fibres to the crucible by washing out the flask with
(method using sulphuric more sulphuric acid reagent. Drain the crucible with
acid 75 % m/m) suction, and wash the residue on the filter once by
23.1 General filling the crucible with a fresh portion of sulphuric
acid reagent. Do not apply suction until this has
This method is applicable, after removal of drained under gravity or stood for 1 min. Wash the
non-fibrous matter, to binary mixtures of polyester residue successively several times with cold water,
and flax, hemp, ramie, cupro, modal, viscose or twice with dilute ammonia solution, and then
cotton. thoroughly with cold water, draining the crucible
23.2 Principle with suction after each addition. Do not apply
The cellulose fibre is dissolved from a known dry suction until each washing liquor has drained under
mass of the mixture using sulphuric acid, gravity. Finally, drain the crucible with suction, dry
approximately 75 % (m/m). the crucible and residue, and cool and weigh them
(see 8.1.3, 8.1.4 and 8.1.5).
The residue is collected, washed, dried, and
weighed; its mass is expressed as a percentage of the 23.5 Calculation and expression of results
dry mass of the mixture. The proportion of cellulose Calculate the results as described in 9.1. The value
fibre is found by difference. of d is 1.00.
23.3 Apparatus and reagents 23.6 Precision
The following apparatus and reagents, together On a homogeneous mixture of textile materials, the
with those specified in clauses 3 and 4, are required. confidence limits of results obtained by this method
of 95 %.
ground glass stopper. 24 Method 8. Binary mixtures of
23.3.1.1 Means of controlling the temperature of the acrylics, certain modacrylics or
flask and contents at 50 ± 5 °C. certain chlorofibres and certain other
23.3.2 Reagents fibres (method using
23.3.2.1 Sulphuric acid solution dimethylformamide)
(approximately 75 % m/m, Ô
24.1 General
approximately 1.67 g/mL). Prepare by adding,
carefully and slowly, while cooling, 700 mL of This method is applicable, after removal of
sulphuric acid (approximately 98 % m/m), Ô non-fibrous matter, to binary mixtures of acrylics,
approximately 1.84 g/mL) to 350 mL of water. After certain modacrylics or certain chlorofibres with
the solution has cooled to 20 °C, dilute it to 1 L with wool, animal hair, silk, cotton, cupro, modal, viscose,
water. polyamide or nylon and polyester. It is equally
applicable to acrylics and certain modacrylics, dyed
23.3.2.2 Dilute ammonia solution. Dilute 80 mL
with pre-metallized dyes, but not to those dyed with
concentrated ammonia solution
afterchrome dyes.
(approximately 35 % (m/m), Ô
approximately 0.88 g/mL) to 1 L with water.
© BSI 03-1999 13
BS 4407:1988
24.2 Principle modal d = 1.01

The acrylic, modacrylic or chlorofibre is dissolved polyester d = 1.01
from a known dry mass of the mixture using
24.6 Precision
dimethylformamide. The residue is collected,
washed, dried and weighed. Its mass, corrected if On a homogeneous mixture of textile materials, the
necessary, is expressed as a percentage of the dry confidence limits of results obtained by this method
mass of the mixture. The percentage of acrylic, are not greater than ± 1 for a confidence level
modacrylic or chlorofibre is found by difference. of 95 %.
24.3 Apparatus and reagent
The following apparatus and reagent, together with certain chlorofibres and certain other
those specified in clauses 3 and 4, are required. fibres (method using carbon
24.3.1 Apparatus disulphide/acetone 55.5/44.5)
24.3.1.1 Conical flask, capacity 200 mL (minimum), 25.1 General
with ground glass stopper.
This method is applicable, after removal of
24.3.1.2 Water bath, at boiling point. non-fibrous matter, to binary mixtures of
24.3.2 Reagent chlorofibres, namely certain polyvinyl chloride
24.3.2.1 Dimethylformamide (boiling point 152 °C fibres, whether after-chlorinated or not, with wool,
to 154 °C) containing not more than 0,1 % water. animal hair, silk, cotton, polyamide or nylon,
polyester, acrylic, glass fibre, cupro, modal and
NOTE This reagent is toxic. The use of a fume hood is essential
and protective gloves should be worn. viscose. When the wool, animal hair or silk content
of a mixture exceeds 25 % the method described in
24.4 Test procedure
clause 18 shall be used. When the polyamide or
Follow the procedure described in 8.2 and proceed nylon content of a mixture exceeds 25 %, the method
as follows. described in clause 20 shall be used.
To the specimen contained in the glass-stoppered 25.2 Principle
conical flask, add 80 mL of dimethylformamide,
preheated to 90 °C to 95 °C, per gram of specimen, The chlorofibre is dissolved from a known dry mass
insert the stopper, shake the flask to wet out the of the mixture using an azeotropic mixture of carbon
specimen and maintain the flask and contents disulphide and acetone. The residue is collected,
for 1 h at 90 °C to 95 °C. Shake the flask and washed, dried and weighed. Its mass is expressed as
contents gently by hand five times during this a percentage of the dry mass of the mixture. The
period. Decant the liquid through a weighed filter percentage of chlorofibre is found by difference.
crucible, retaining the fibres in the flask. Add a 25.3 Apparatus and reagents
further 60 mL of dimethylformamide to the flask The following apparatus and reagents, together
and heat for 30 min at 90 °C to 95 °C, shaking the with those specified in clauses 3 and 4, are required.
flask and contents gently by hand twice during this
period. Filter the contents of the flask through the 25.3.1 Apparatus
filter crucible by means of suction. Transfer any 25.3.1.1 Conical flask, capacity 250 mL, with
residual fibre to the crucible by washing out the ground glass stopper.
flask with dimethylformamide (24.3.2.1). Drain the 25.3.1.2 Mechanical shaker.
crucible with suction. Wash the residue with 1 L of
25.3.1.3 Small watch glass.
hot water at 70 °C to 80 °C, filling the crucible each
time. After each addition of water, apply suction 25.3.2 Reagents
briefly but not until the water has drained under 25.3.2.1 Azeotropic mixture of carbon disulphide
gravity. If the washing liquor drains through the complying with BS 662-1 and acetone complying
crucible too slowly apply slight suction. with BS 509-1. Mix 555 mL of carbon disulphide
Finally, dry the crucible and residue, cool and weigh with 445 mL acetone.
them (see 8.1.3, 8.1.4 and 8.1.5). NOTE The toxic effects and flammability of carbon disulphide
should be borne in mind and full precautions should be taken
24.5 Calculation and expression of results when it is used.
Calculate the results as described in 9.1. The value 25.3.2.2 Ethanol complying with BS 507.
of d is 1.00, except in the following cases:
wool d = 1.01
cotton d = 1.01
cupro d = 1.01
14 © BSI 03-1999
BS 4407:1988
25.4 Test procedure 26.3 Apparatus and reagent

Follow the procedure described in 8.2 and proceed The following apparatus and reagent, together with
as follows. those specified in clauses 3 and 4, are required.
To the specimen contained in the glass-stoppered 26.3.1 Apparatus
conical flask, add 100 mL of carbon
disulphide/acetone per gram of specimen. Insert the ground glass stopper.
stopper and shake the flask on a mechanical shaker
for 20 min, loosening the stopper once or twice at 26.3.1.2 Mechanical shaker.
the beginning of the process to release any excess 26.3.2 Reagent
pressure. Decant the supernatant liquid through 26.3.2.1 Glacial acetic acid distilling at 117 °C
the weighed filter crucible, retaining the fibres in to 119 °C.
the flask. Repeat the treatment with a
further 100 mL of fresh reagent. Continue with this 26.4 Test procedure
cycle of operations until no deposit is left on a watch Follow the procedure described in 8.2 and proceed
glass when a drop of the extraction liquor is as follows.
evaporated. To the specimen contained in the glass-stoppered
Transfer the residue from the flask to the filter conical flask add 100 mL of glacial acetic acid per
crucible using more reagent, drain with suction, and gram of specimen. Insert the stopper and shake
wash the crucible and residue three times for 20 min on a mechanical shaker. Decant the
with 20 mL of ethanol and then three times with supernatant liquid through the weighed filter
water. Do not apply suction until each washing crucible retaining the fibres in the flask. Repeat the
liquor has drained under gravity. Finally drain the treatment twice more using 100 mL of fresh reagent
crucible with suction, dry the crucible and residue each time, making three extractions in all. Transfer
and cool and weigh them (see 8.1.3, 8.1.4 and 8.1.5). the residue to the filter crucible, drain with suction,
NOTE With certain mixtures having a high polyvinyl chloride and wash the crucible and residue with 50 mL of
content there may have been substantial shrinkage of the acetic acid, and then three times with water. Do not
specimen during the initial drying procedure, as a result of which
the dissolution of polyvinyl chloride by the solvent may be
apply suction until each washing liquor has drained
retarded. This does not, however, affect the ultimate dissolution under gravity. Finally drain the crucible with
of the polyvinyl chloride by the solvent. suction, dry the crucible and residue, and cool and
25.5 Calculation and expression of results weigh them (see 8.1.3, 8.1.4 and 8.1.5).
Calculate the results as described in 9.1. The value 26.5 Calculation and expression of results
of d is 1.00. Calculate the results as described in 9.1. The value
25.6 Precision of d is 1.00.
On a homogeneous mixture of textile materials, the 26.6 Precision
confidence limits of results obtained by this method On a homogeneous mixture of textile materials, the
are not greater than ± 1 for a confidence level confidence limits of results obtained by this method
of 95 %. are not greater than ± 1 for a confidence level
of 95 %.
acetate and certain chlorofibres 27 Method 11. Binary mixtures of silk
(method using glacial acetic acid) and wool or hair (method using
26.1 General sulphuric acid 75 % m/m)
This method is applicable, after removal of 27.1 General
non-fibrous matter, to binary mixtures of acetate This method is applicable, after removal of
with certain chlorofibres namely polyvinylchloride non-fibrous matter, to binary mixtures of silk with
whether after-chlorinated or not. wool or animal hair. It is not applicable to mixtures
26.2 Principle containing wild silk, e.g. tussah.
The acetate is dissolved from a known dry mass of 27.2 Principle
the mixture using glacial acetic acid. The residue is The silk fibre is dissolved from a known dry mass of
collected, washed, dried, and weighed. Its mass is the mixture, using sulphuric acid 75 % (m/m).
expressed as a percentage of the dry mass of the The residue is collected, washed, dried and weighed.
mixture. The percentage of acetate is found by Its mass, corrected if necessary, is expressed as a
difference. percentage of the dry mass of the mixture. The
percentage of silk is found by difference.
© BSI 03-1999 15
BS 4407:1988
27.3 Apparatus and reagents 27.6 Precision

The following apparatus and reagents, together On a homogeneous mixture of textile materials, the
with those specified in clauses 3 and 4, are required. confidence limits of results obtained by this method
of 95 %.
ground glass stopper. 28 Method 12. Deleted
27.3.2 Reagents This method has been deleted because it has proved
27.3.2.1 Sulphuric acid solution to be insufficiently accurate.
(approximately 75 % m/m, Ô approximately 1.67).
Prepare by adding, carefully and slowly, while 29 Method 13. Binary mixtures of jute
cooling, 700 mL of sulphuric acid and certain animal fibres (method of
(approximately 98 % m/m, Ô determining the nitrogen content)
approximately 1.84 g/mL) to 350 mL of water. After
the solution has cooled to 20 °C, dilute to 1 L with 29.1 General
water. Because this method differs in principle from the
27.3.2.2 Sulphuric acid, dilute solution. general method based on selective solubility set out
Add 100 mL sulphuric acid in section 2, it is given in a form that is more
(approximately 98 % m/m, Ô detailed than other methods.
approximately 1.84 g/mL) slowly to 1 900 mL of The method is applicable, after the removal of
water. non-fibrous matter, to binary mixtures of jute and
27.3.2.3 Dilute ammonia solution. Dilute 200 mL wool or animal hair. The wool or animal hair
concentrated ammonia solution component may consist solely of wool or animal hair,
(approximately 35 % m/m, Ô or of any mixtures of the two. This method is not
approximately 0.88 g/mL) to 1 L with water. applicable to textile mixtures containing
non-fibrous matter (dyes, finishes etc.) with a
27.4 Test procedure
nitrogen base.
Follow the procedure described in 8.2 and proceed
29.2 Principle
as follows.
The nitrogen content of the mixture is determined,
To the specimen contained in the glass-stopper
and from this and the known or assumed nitrogen
conical flask, add 100 mL of sulphuric
contents of the two components, the proportion of
acid 75 % m/m (27.3.2.1) per gram of specimen and
each component is calculated.
insert the stopper. Shake the flask vigorously and
stand it for 30 min at room temperature. Shake the 29.3 Apparatus and reagents
flask again and stand it for 30 min. Shake it a last The following apparatus and reagents, together
time and filter the contents of the flask through the with those specified in clauses 3 and 4, are required.
weighed filter crucible. Wash any remaining fibres
from the flask with more 75 % sulphuric acid 29.3.1 Apparatus
reagent. Wash the residue on the crucible 29.3.1.1 Kjeldahl digestion flask, capacity 200 mL
successively with 50 mL of the dilute sulphuric acid to 300 mL.
reagent (27.3.2.2) 50 mL water and 50 mL of the 29.3.1.2 Kjeldahl distillation apparatus with steam
dilute ammonia solution (27.3.2.3). Each time injection.
ensure the fibres remain in contact with the liquid
29.3.1.3 Titration apparatus allowing precision
for at least 10 min before applying suction.
of 0.05 mL.
Finally rinse with water, leaving the fibres in
29.3.1.4 One-mark volumetric flask,
contact with the water for about 30 min. Drain the
capacity 200 mL, complying with BS 1792.
crucible with suction, dry the crucible and residue,
and cool and weigh them (see 8.1.3, 8.1.4 and 8.1.5). 29.3.1.5 Conical flask, capacity 100 mL.
27.5 Calculation and expression of results 29.3.2 Reagents
NOTE All reagents should be of a recognized analytical reagent
Calculate the results as described in 9.1. The value quality.
of d is 0.985 for wool.
29.3.2.1 Toluene complying with BS 135, BS 458,
BS 805.
29.3.2.2 Methanol complying with BS 506-1.
16 © BSI 03-1999
BS 4407:1988
29.3.2.3 Sulphuric acid, approximately 98 % m/m, To the specimen in the digestion flask add, in the
Ô approximately 1.84 g/mL. following order, 2.5 g potassium
29.3.2.4 Potassium sulphate. sulphate (29.3.2.4), 0.1 g to 0.2 g selenium
NOTE This reagent should be nitrogen free.
dioxide (29.3.2.5) and 10 mL sulphuric
acid (29.3.2.3). Heat the flask, gently at first, until
29.3.2.5 Selenium dioxide. the whole of the fibre is destroyed and then heat it
NOTE This reagent should be nitrogen free. more vigorously until the solution becomes clear
29.3.2.6 Sodium hydroxide solution 400 g/L. and almost colourless. Heat it for a further 15 min.
Dissolve 400 g of sodium hydroxide in 400 mL Allow the flask to cool, dilute the contents carefully
to 500 mL of water and dilute to 1 L with water. with 10 mL to 20 mL water, cool, transfer the
29.3.2.7 Mixed indicator. Dissolve 0.1 g of methyl contents quantitatively to a 200 mL flask (29.3.1.4)
red in 95 mL of ethanol and 5 mL of water, and mix and make up to volume with water to form the
with 0.5 g of bromocresol green dissolved in 475 mL digest solution.
of ethanol and 25 mL of water. Place about 20 mL of boric acid solution in a conical
29.3.2.8 Boric acid solution. Dissolve 20 g boric acid flask (29.3.1.5) and place the flask under the
in 1 L of water. condenser of the Kjeldahl distillation apparatus so
29.3.2.9 Sulphuric acid, c(H2SO4) = 0.01 mol/L. that the delivery tube dips just below the surface of
the boric acid solution. Transfer exactly 10 mL of
29.4 Test sample digest solution to the distillation flask, add not less
Take a sample that is representative of the bulk and than 5 mL of sodium hydroxide solution (29.3.2.6)
sufficient to provide all the specimens, each of to the funnel, lift the stopper slightly, and allow the
about 1 g, that are required. Treat the sample as sodium hydroxide solution to run slowly into the
described in 29.5. flask. In the digest solution and sodium hydroxide
solution remain as two separate layers, mix them by
29.5 Pretreatment of sample
gentle agitation.
Extract the air-dry sample in a Soxhlet apparatus
Heat the distillation flask gently and pass into it
with a mixture of 1 volume of toluene and 3 volumes
steam from the generator. Collect about 20 mL of
of methanol for 4 h at a minimum rate of 5 cycles/h.
distillate, lower the receiver so that the tip of the
Allow the solvent to evaporate from the sample in
delivery tube is about 20 mm above the surface of
air, and remove the last traces in an oven at a
the liquid, and distill for 1 min more. Rinse the tip
temperature of 105 ± 3 °C. Then extract the sample
of the delivery tube with water, catching the
in water (50 mL/g of sample) by boiling under reflux
washings in the receiver. Remove the receiver and
for 30 min. Filter, return the sample to the flask,
replace it with a second receiver containing
and repeat the extraction with a similar volume of
about 10 mL of boric acid solution, and collect
water. Filter, remove excess water from the sample
about 10 mL of distillate. Titrate the two distillates
by squeezing, suction, or centrifuging, and then
separately with sulphuric acid (29.3.2.9) using the
allow the sample to become, air-dry.
mixed indicator. Record the total titre for the two
NOTE The toxic effects of toluene and methanol should be distillates. If the titre for the second distillate is
borne in mind, and full precautions should be taken when they
are used. more than 0.2 mL repeat the test and start the
distillation again, using a fresh aliquot of digest
29.6 Test procedure
solution.
29.6.1 General instructions. Observe the general
Carry out a blank determination, i.e. digestion and
instructions given in 8.1. distillation, using the reagents only.
29.6.2 Detailed procedure. Take from the pretreated
29.7 Calculation and expression of results
sample a test specimen of mass about 1 g. Dry the
specimen in a weighing bottle, cool it in a desiccator, 29.7.1 Calculate the percentage nitrogen in the dry
and weigh it. Transfer the specimen to a dry specimen as follows:
Kjeldahl digestion flask, reweigh the weighing
bottle immediately, and obtain the dry mass of the A = 56 (V – b)M
---------------------------------- (%)
W
specimen by difference.
where
A is the percentage nitrogen in the clean dry
specimen;
V is the total titre of standard sulphuric acid
for the determination (mL);
b is the total titre of standard sulphuric acid
for the blank determination (mL);
© BSI 03-1999 17
BS 4407:1988
M is the molarity of standard sulphuric acid 30.3.2 Reagents

(mol/L); 30.3.2.1 Dilute hydrochloric acid solution.
W is the dry mass of specimen (g). Dilute 20 mL concentrated hydrochloric acid
29.7.2 Using the values of 0.22 % for the nitrogen (approximately 37 % (m/m), Ô
content of jute and 16.2 % for the nitrogen content approximately 1.18 g/mL) with 500 mL of water.
of animal fibre, both values being expressed on the 30.3.2.2 Dilute ammonia solution. Dilute 80 mL of
dry mass of the fibre, calculate the composition of concentrated ammonia solution
the mixture as follows: (approximately 35 % (m/m), Ô
approximately 0.88 g/mL) to 1 L with water.
A – 0.22 - × 100
P A = ------------------------------- (%) 30.3.2.3 Sulphuric acid, 60 % m/m. Prepare by
16.2 – 0.22
adding carefully, while cooling, 903 mL sulphuric
where acid (Ô approximately 1.84 at 20 °C) to 1 L of water.
PA is the percentage animal fibre in the clean After cooling to 20 °C, the mixture should have a
dry specimen. relative density of between 1.495 and 1.500. If
necessary, adjust it to that value by adding acid or
water as appropriate.
30 Method 14. Binary mixtures of flax
and viscose (method using sulphuric 30.4 Additional pretreatment of sample
acid) Follow the procedure described in clause 7 and
proceed as follows.
30.1 General
Take from the pretreated sample a test sample of
This method is applicable, after removal of mass approximately 2 g. Dry the test sample in a
non-fibrous matter, to binary mixtures of grey or weighing bottle, cool it in a desiccator and weigh it.
bleached flax with viscose (including many modal Transfer the test sample to a 500 mL
fibres). If modal is found to be present, a flask (30.3.1.1), reweigh the weighing bottle
preliminary test should be made to see whether it is immediately, and obtain the dry mass of the test
soluble in the reagent under the conditions of test. sample by difference. Add 200 mL of the dilute
The method is not applicable to mixtures in which hydrochloric acid solution to the test sample in the
the flax has suffered extensive chemical flask and reflux for 10 min. Filter the contents of the
degradation, nor when the viscose or modal has flask through a weighed filter crucible and transfer
been rendered incompletely soluble by the presence any residual fibres to the crucible by washing out
of certain finishes, or dyes which cannot be removed the flask with hot water. Wash the residue
completely by the pretreatment. successively with hot water, dilute ammonia
30.2 Principle solution and finally water, draining the crucible
The viscose or modal is dissolved from a known dry with suction after each addition. Do not apply
mass of the mixture using sulphuric acid, after suction until each washing liquor has drained under
preliminary treatment with dilute hydrochloric gravity. Finally, drain the crucible with suction, dry
acid. The residue is collected, washed, dried and the crucible and residue, and cool and weigh them
weighed. Its mass, corrected for loss, both in the (see 8.1.3, 8.1.4 and 8.1.5).
preliminary treatment and in the separation 30.5 Test procedure
treatment, is expressed as a percentage of the dry Follow the procedure described in 8.2 but cut the
mass of the mixture. The percentage of viscose or specimen into lengths of about 5 mm. Proceed as
modal is found by the difference. follows.
30.3 Apparatus and reagents
30.3.1 Apparatus
30.3.1.1 Flask, capacity 500 mL.
30.3.1.2 Glass-stoppered flask, capacity 250 mL.
30.3.1.3 Mechanical shaker.
18 © BSI 03-1999
BS 4407:1988
To the specimen contained in the glass-stoppered 31.2 Principle

conical flask, add 100 mL of the sulphuric acid The polypropylene fibre is dissolved from a known
reagent per gram of specimen. Insert the stopper dry mass of the mixture with boiling xylene. The
and shake the flask vigorously on a mechanical residue is collected, washed, dried and weighed; its
shaker for 30 ± 1 min. Filter the contents of the mass, corrected if necessary, is expressed as a
flask through a weighed filter crucible and transfer percentage of the dry mass of the mixture. The
any residual fibres to the crucible by washing out percentage of polypropylene is found by difference.
the flask with a small amount of the sulphuric acid
reagent. Drain the crucible with suction and wash 31.3 Apparatus and reagents
the residue on the filter successively three times The following apparatus and reagents, together
with water, dilute ammonia solution, and finally with those specified in clauses 3 and 4, are required.
cold water, draining the crucible with suction after 31.3.1 Apparatus
each addition. Do not apply suction until each
washing liquor has drained under gravity. Finally, 31.3.1.1 Conical flask, capacity 200 mL, with
drain the crucible with suction, dry the crucible and ground glass stopper.
residue and cool and weigh them 31.3.1.2 Reflux condenser (suitable for liquids of
(see 8.1.3, 8.1.4 and 8.1.5). high boiling point) fitting the conical flask.
If the results of duplicate tests differ by more 31.3.2 Reagent
than 2 % make two repeat determinations.
31.3.2.1 Xylene, distilling between 137 °C
30.6 Calculation and expression of results and 142 °C.
Calculate the percentage of clean dry flax as follows: NOTE The harmful effects of this reagent should be borne in
mind, and full precautions should be taken when it is used.
100dbM 31.4 Test procedure
p = ----------------------------2-
aM 1 Follow the procedure described in 8.2 and proceed
as follows.
where
To the specimen contained in the conical flask
P is the percentage of clean dry flax; add 100 mL of the xylene per gram of specimen.
a is the mass of the oven-dry sample before Attach the condenser and boil the contents
pretreatment with hydrochloric acid (g); for 3 min. Decant the hot liquid through the
weighed filter crucible. Repeat this treatment twice
b is the mass of the oven-dry sample after more, each time using a fresh 50 mL of solvent.
pretreatment with hydrochloric acid (g);
Wash the residue remaining in the flask
M1 is the oven-dry mass of the test specimen successively with 30 mL of boiling xylene (twice)
after pretreatment with hydrochloric acid then with 75 mL of the light petroleum (twice).
(g); After the second wash with light petroleum, filter
M2 is the oven-dry mass of the flax residue (g); the residue through the filter crucible and allow it to
drain. Dry the crucible and residue, cool and weigh
d is the correction factor for loss in mass of the them (see 8.1.3, 8.1.4 and 8.1.5).
flax component in the reagent.
Hot extraction apparatus using the appropriate
The value of d for bleached flax is 1.16 and for grey procedure, giving identical results, may be used3).
flax is 1.22. NOTE 1 Preheat the filter crucible through which the xylene is
to be filtered.
NOTE 2 After the treatment with boiling xylene, ensure that
31 Method 15. Binary mixtures of the flask containing the residue is cooled sufficiently before the
polypropylene and certain other light petroleum is introduced.
fibres (method using xylene) 31.5 Calculation and expression of results
31.1 General Calculate the results as described in 9.1. The value
This method is applicable, after removal of of d is 1.00.
non-fibrous matter, to binary mixtures of 31.6 Precision
polypropylene fibres with wool, silk, cotton, viscose, On a homogeneous mixture of textile materials, the
cupro, modal, acetate, triacetate, polyamide, confidence limits of results obtained by this method
polyester, acrylic, and glass fibres. are not greater than ± 1 % for the confidence level
of 95 %.
3)
See, for example, the apparatus described in Melliand Textilberichte, 56 (1975) 643–645.
© BSI 03-1999 19
BS 4407:1988
32 Method 16. Binary mixtures of 32.4 Test procedure

chlorofibres (homopolymers of vinyl Follow the procedure described in 8.2 and proceed
chloride) and certain other fibres as follows.
(method using concentrated sulphuric To the specimen contained in the conical flask,
acid) add 100 mL of the concentrated sulphuric
acid (32.3.2.1) per gram of specimen.
32.1 General
Allow the contents of the flask to remain at room
This method is applicable, after removal of temperature for 10 min, and during that time stir
non-fibrous material, to binary mixtures of the test specimen occasionally by means of the glass
chlorofibres based on homopolymers of vinyl
rod. If a woven or knitted fabric is being treated,
chloride (after-chlorinated or not) with cotton,
wedge it between the wall of the flask and the glass
viscose, cupro, modal, acetate, triacetate,
rod and exert a light pressure in order to separate
polyamide, polyester and certain acrylic and certain
the material dissolved by the sulphuric acid.
modacrylic fibres. (The modacrylics concerned are
those which give a limpid solution when immersed Decant the liquid through the weighed filter
in concentrated sulphuric crucible. Add to the flask a fresh portion of 100 mL
acid Ô approximately 1.84.) of the concentrated sulphuric acid and repeat the
same operation. Transfer the contents of the flask to
It can be used particularly in place of
the filter crucible and transfer the fibrous residue
methods 8 and 9 in all cases where a preliminary
there with the aid of the glass rod. If necessary, add
test shows that the chlorofibres do not dissolve a little concentrated sulphuric acid to the flask in
completely either in dimethylformamide or in the order to remove any fibres adhering to the wall.
azeotropic mixture of carbon disulphide and
Drain the filter crucible with suction. After
acetone.
emptying or changing the filter-flask, wash the
32.2 Principle residue in the crucible successively with
The constituent other than the chlorofibre is the 50 % sulphuric acid solution (32.3.2.2), water,
dissolved from a known dry mass of the mixture the ammonia solution and finally with water,
with concentrated sulphuric acid. The residue, draining the crucible with suction after each
consisting of the chlorofibre, is collected, washed, addition until the water drained from the crucible is
dried and weighed; its mass, corrected if necessary, neutral to litmus. (Do not apply suction during the
is expressed as a percentage of the dry mass of the washing operation, but only after the liquid has
mixture. The percentage of the second constituent is drained through the crucible.)
obtained by difference. Dry the crucible and residue, cool and weigh them
32.3 Apparatus and reagents (see 8.1.3, 8.1.4 and 8.1.5).
The following apparatus and reagents, together 32.5 Calculation and expression of results
with those specified in clauses 3 and 4, are required. Calculate the results as described in 9.1. The value
32.3.1 Apparatus of d is 1.00.
32.3.1.1 Conical flask, capacity 200 mL, with 32.6 Precision
ground glass stopper. On a homogeneous mixture of textile materials, the
32.3.1.2 Glass rod with flattened end. confidence limits of results obtained by this method
are not greater than ± 1 % for the confidence level
32.3.2 Reagents of 95 %.
32.3.2.1 Sulphuric acid, concentrated,
approximately 98 % m/m, Ô 33 Method 17. Binary mixtures of
approximately 1.84 g/mL. asbestos and certain fibres (method
NOTE Concentrated sulphuric acid is highly corrosive and based on heating to 450 °C)
appropriate safety precautions should be taken when it is used.
NOTE This method differs in principle from the general method
32.3.2.2 Sulphuric acid, 50 % (m/m) aqueous based on selective solubility set out in clause 1.
solution.
33.1 General
32.3.2.3 Ammonia, dilute solution.
This method is applicable to binary mixtures of
Dilute 60 mL of concentrated ammonia solution cotton, viscose, acetate, triacetate, modal, cupro,
(approximately 35 % m/m, Ô polyester, or polyamide (excluding aramid) and
approximately 0.88 g/mL) to 1 L with water. chrysotile or crocidolite asbestos.
“WARNING Asbestos health hazard
20 © BSI 03-1999
BS 4407:1988
NOTE Full precautions should be taken to avoid inhalation of b) wool, animal hair, silk, cotton, cupro, modal,
asbestos at all stages of this method. For further details see the viscose, polyamide, acrylic and glass fibre.
foreword.
Where modacrylics or elastanes are present a
33.2 Principle
preliminary test should be carried out to determine
The constituent other than the asbestos is removed whether the fibre is completely soluble in the
from a known dry mass of the mixture by heating reagent.
at 450 ± 10 °C for 1 h. The residue consisting of
It is also possible to analyse mixtures containing
asbestos is weighed; its corrected mass is expressed
chlorofibres by using method 9 or method 16.
as a percentage of the dry mass of the mixture. The
percentage of the second constituent is calculated by 34.2 Principle
difference. The acetate and triacetate fibres, chlorofibres,
33.3 Apparatus certain modacrylics, and certain elastanes are
dissolved out from a known dry mass with
The following apparatus, together with that
cyclohexanone at a temperature close to boiling
specified in clause 3, is required.
point. The residue is collected, washed, dried and
33.3.1 Electric furnace, with automatic temperature weighed. Its mass, corrected if necessary, is
control at 450 ± 10 °C. expressed as a percentage of the dry mass of the
33.3.2 Silica or metal crucible. mixture.
33.4 Sampling The percentage of chlorofibre, modacrylic, elastane,
acetate and triacetate is found by difference.
Take a laboratory test sample that is representative
of the laboratory bulk sample and sufficient to 34.3 Apparatus and reagents
provide all the specimens, each about 5 g, that are The following apparatus and reagents, together
required. with those specified in clauses 3 and 4, are required.
NOTE Pretreatment of the laboratory test sample described in
clause 7 is not applicable to the analysis of this mixture.
34.3.1 Apparatus
33.5 Test procedure 34.3.1.1 Hot extraction apparatus (see Figure 1).
NOTE This is a variant of the apparatus used in Melliand
33.5.1 General instructions. Observe the general Textilberichte, 56 (1975) 643–645.
instructions given in 8.1.
34.3.1.2 Filter crucible.
33.5.2 Detailed procedure. Take from the laboratory
34.3.1.3 Porous baffle.
test sample a test specimen weighing about 5 g.
Determine the dry mass of the test specimen 34.3.1.4 Reflux condenser.
accurately in a weighing bottle, transfer it to a 34.3.1.5 Source of heat.
crucible of known mass and heat it in the electric 34.3.2 Reagents
furnace with automatic temperature control
34.3.2.1 Cyclohexanone, boiling point 156 °C.
at 450 ± 10 °C for 1 h.
NOTE Cyclohexanone is flammable and toxic. Suitable
Cool the crucible and its contents to room precautions should be taken when it is used.
temperature in a desiccator. Determine the mass of 34.3.2.2 Ethanol, 50 % V/V.
the crucible and residue within 2 min of its removal
from the desiccator. 34.4 Procedure
33.6 Calculation and expression of results Follow the procedure described in 8.2 and proceed
as follows.
of d is 1.02. Pour 100 mL of cyclohexanone (34.3.2.1) per gram
of specimen into the distillation flask (34.3.1.1).
34 Method 18. Binary mixtures of Insert the extraction container in which the filter
crucible, containing the specimen and the porous
chlorofibres, certain modacrylics, baffle (34.3.1.3), slightly inclined, have previously
certain elastanes, acetates, triacetates been placed. Insert the reflux condenser (34.3.1.4).
and certain other fibres (method using Bring to the boil and continue extraction for 1 h at a
cyclohexanone) minimum rate of 12 cycles/h. After extraction and
34.1 General cooling, remove the extraction container, take out
the filter crucible and remove the porous baffle.
This method is applicable, after removal of Wash the contents of the filter crucible three or four
non-fibrous matter, to binary mixtures of times with ethanol (34.3.2.2) heated to
a) acetate, triacetate, chlorofibre, certain approximately 60 °C and subsequently with 1 L of
modacrylics and certain elastanes with water at 60 °C.
© BSI 03-1999 21
BS 4407:1988
Do not apply suction during or between the washing acrylic d = 0.98.

operations. Allow the liquid to drain under gravity
and then apply suction. 34.6 Precision
Finally dry the crucible and residue, cool and weigh On a homogeneous mixture of textile fibres, the
them (see 8.1.3, 8.1.4 and 8.1.5). confidence limits of results obtained by this method
are not greater than ± 1 % for a confidence level
34.5 Calculation and expression of results of 95 %.
of d is 1.00 with the following exceptions:
silk d = 1.01
Figure 1 — Hot extraction apparatus
22 © BSI 03-1999
BS 4407:1988
Appendix A Procedures to be adopted Variant 1. Component (a) is removed from the first
for ternary fibre mixtures test specimen and component (b) is removed from
the second test specimen, component (c) is found by
NOTE The Directive 73/44/EEC relating to the quantitative difference.
analysis of ternary fibre mixtures allows the use of a choice of
methods based on the procedures for binary fibre mixtures. Variant 2. Component (a) is removed from the first
test specimen, leaving as a residue the other two
The Directive 73/44/EEC allows the analyst to
components (b + c), and two components (a + b) are
choose the variants used for analysis of any ternary
removed from the second test specimen, leaving as
fibre mixture, but trials have shown that this is not
residue the third component (c).
entirely satisfactory. Although there is insufficient
information on the validity of the individual Variant 3. Components (a + b) are removed from the
variants for specific ternary fibre mixtures it is first test specimen, leaving as a residue the third
preferable to limit the choice of variants to those component (c), then two components (b + c) are
listed in annex 3 of 73/44/EEC and given in Table 2 removed from the second test specimen, leaving as a
of this standard. residue the first component (a).
Four variants may be adopted for analysis of Variant 4. Two components are successively
ternary fibre mixtures. removed from a single test specimen.
Table 2 — Procedures to be used for quantitative chemical analysis of
ternary fibre mixtures
Mixture Component fibres Varianta Number of method for binary mixtures
No. and reagent
1st component 2nd component 3rd component
(a) (b) (c)
1 wool or hair viscose, cupro cotton 1 and/or 4 2 (alkaline hypochlorite) and
or certain 3 (zinc chloride/formic acid)
types of
modal
2 wool or hair polyamide 6 cotton, viscose, 1 and/or 4 2 (alkaline hypochlorite) and
or 6.6 cupro or modal 4 (formic acid)
3 wool, hair or silk certain viscose, cupro, 1 and/or 4 2 (alkaline hypochlorite) and
chlorofibres modal or 9 (carbon disulphide/acetone)
cotton
4 wool or hair polyamide 6 polyester, 1 and/or 4 2 (alkaline hypochlorite) and
or 6.6 polypropylene, 4 (formic acid)
acrylic or glass
fibre
5 wool, hair or silk certain polyester, 1 and/or 4 2 (alkaline hypochlorite) and
chlorofibres acrylic, 4 (carbon disulphide/acetone)
polyamide or
glass fibre
6 silk wool or hair polyester 2 11 (sulphuric acid) and
2 (alkaline hypochlorite)
7 polyamide 6 acrylic cotton, viscose, 1 and/or 4 4 (formic acid) and
or 6.6 cupro or modal 8 (dimethylformamide)
8 certain polyamide 6 cotton, viscose, 1 and/or 4 8 (dimethylformamide) and
chlorofibres or 6.6 cupro or modal 4 (formic acid)
9 (carbon disulphide/acetone) and
4 (formic acid)
9 acrylic polyamide 6 polyester 1 and/or 4 8 (dimethylformamide) and
or 6.6 4 (formic acid)
10 acetate polyamide 6 viscose, cotton, 4 1 (acetone) and
11 certain acrylic polyamide 2 and/or 4 9 (carbon disulphide/acetone) and
chlorofibres 8 (dimethylformamide)
12 certain polyamide 6 acrylic 1 and/or 4 9 (carbon disulphide/acetone) and
chlorofibres or 6.6 4 (formic acid)
a
When variant 4 is used, first remove the first component using the first reagent.
© BSI 03-1999 23
BS 4407:1988

No. 1st component 2nd component 3rd component and reagent
(a) (b) (c)
13 polyamide 6 viscose, cupro, polyester 4 4 (formic acid) and
or 6.6 modal or 7 (sulphuric acid)
cotton
14 acetate viscose, cupro, polyester 4 1 (acetone) and
modal or 7 (sulphuric acid)
cotton
15 acrylic viscose, cupro, polyester 4 8 (dimethylformamide) and
modal or 7 (sulphuric acid)
cotton
16 acetate wool, hair or cotton, viscose, 4 1 (acetone) and
silk cupro, modal, 2 (alkaline hypochlorite)
polyamide,
polyester or
acrylic
17 triacetate wool, hair or cotton, viscose, 4 6 (dichloromethane) and
silk cupro, modal, 2 (alkaline hypochlorite)
polyamide,
polyester or
acrylic
18 acrylic wool, hair or polyester 1 and/or 4
8 (dimethylformamide) and
silk 2 (alkaline hypochlorite)
19 acrylic silk wool or hair 4 8 (dimethylformamide) and
11 (sulphuric acid)
20 acrylic wool, hair or cotton, viscose, 1 and/or 4 8 (dimethylformamide) and
silk cupro or modal 2 (alkaline hypochlorite)
21 wool, hair or silk cotton, polyester 4 2 (alkaline hypochlorite) and
viscose, modal 7 (sulphuric acid)
or cupro
22 viscose, cupro or cotton polyester 2 and/or 4 3 (zinc chloride/formic acid) and
certain types of 7 (sulphuric acid)
modal
23 acrylic viscose, cupro cotton 4 8 (dimethylformamide) and
types of
modal
24 certain viscose, cupro cotton 1 and/or 4 9 (carbon disulphide/acetone) and
chlorofibres or certain 3 (zinc chloride/formic acid)
types of or
modal 8 (dimethylformamide) and
3 (zinc chloride/formic acid)
25 acetate viscose, cupro cotton 4 1 (acetone) and
types of
modal
26 triacetate viscose, cupro cotton 4 6 (dichloromethane) and
types of
modal
27 acetate silk wool or hair 4 1 (acetone) and
11 (sulphuric acid)
28 triacetate silk wool or hair 4 6 (dichloromethane) and
11 (sulphuric acid)
a
When variant 4 is used, first remove the first component using the first reagent.
24 © BSI 03-1999
BS 4407:1988

No. 1st component 2nd component 3rd component and reagent
(a) (b) (c)
29 acetate acrylic cotton, viscose, 4 1 (acetone) and
cupro or modal 8 (dimethylformamide)
30 triacetate acrylic cotton, viscose 4 6 (dichloromethane) and
cupro or modal 8 (dimethylformamide)
31 triacetate polyamide 6 cotton, viscose, 4 6 (dichloromethane) and
32 triacetate cotton, polyester 4 6 (dichloromethane) and
viscose, cupro 7 (sulphuric acid)
or modal
33 acetate polyamide 6 polyester or 4 1 (acetone) and
or 6.6 acrylic 4 (formic acid)
34 acetate acrylic polyester 4 1 (acetone) and
8 (dimethylformamide)
35 certain cotton, polyester 4 8 (dimethylformamide) and
chlorofibres viscose, cupro 7 (sulphuric acid)
or modal or
9 (carbon disulphide/acetone) and
7 (sulphuric acid)
a When variant 4 is used, first remove the first component using the first reagent.
© BSI 03-1999 25
BS 4407:1988
Appendix B Agreed allowances for moisture and other matter to be used in

connection with the analysis of fibre mixtures as given in Annex II of the EEC
Directive on textile descriptions, 71/307/EEC, as amended by
Directive 83/623/EEC
Fibres Percentages Fibres Percentages

Wool and animal hair: Fluorofibre 0.00
combed fibres 18.25 Modacrylic 2.00
carded fibres 17.00 Polyamide or nylon:
Animal hair:
combed fibres 18.25 discontinuous fibre 6.25
carded fibres 17.00 filament 5.75
Horsehair:
combed fibres 16.00
carded fibres 15.00
Silk 11.00
Cotton:
normal fibres 8.50
mercerized fibres 10.50
Kapok 10.90 Polyester:
Flax 12.00 discontinuous fibre 1.50
Hemp 12.00 filament 1.50
Jute 17.00 Polyethylene 1.50
Abaca 14.00 Polypropylene 2.00
Alfa 14.00 Polycarbamide 2.00
Coir 13.00 Polyurethane:
Broom 14.00 discontinuous fibre 3.50
Ramie (bleached fibre) 8.50 filament 3.00
Sisal 14.00 Vinylal 5.00
Sunn 12.00 Trivinyl 3.00
Henequen 14.00 Elastodiene 1.00
Maguey 14.00 Elastane 1.50
Acetate 9.00 Glass fibre:
Alginate 20.00 filament with a diameter
Cupro 13.00 of over 5 4m 2.00
Modal 13.00 filament with a diameter
Protein 17.00 of 5 4m or less 3.00
Triacetate 7.00 Metal fibre 2.00
Viscose 13.00 Metallized fibre 2.00
Acrylic 2.00 Asbestos 2.00
Chlorofibre 2.00 Paper yarn 13.75
26 © BSI 03-1999
BS 4407:1988
Publications referred to
BS 135, Specifications for benzene, xylenes and toluenes.

BS 506, Methanol for industrial use.
BS 506-1, Specification for methanol.
BS 507, Specification for ethanol for industrial use.
BS 509, Acetone for industrial use.
BS 509-1, Specification for acetone.
BS 662, Carbon disulphide for industrial use.
BS 662-1, Specification.
BS 1752, Specification for laboratory sintered or fritted filters including porosity grading.
BS 1792, Specification for one-mark volumetric flasks.
BS 1994, Specification for dichloromethane (methylene chloride).
BS 2071, Specification for Soxhlet extractors.
BS 3978, Specification for water for laboratory use.
BS 4658, Methods of test for textiles — preparation of laboratory test samples and test specimens for
chemical testing.
BS 4815, Glossary of generic names for man-made fibres.
ISO/TR 5090, Textiles — Methods for the removal of non-fibrous matter prior to quantitative analysis of
fibres mixtures4).
4) Mentioned in the foreword only.
© BSI 03-1999
BS 4407:1988
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BRITISH STANDARD BS 4407:1988

Committees responsible for this

British Carpet Manufacturers’ Association Ltd.

This British Standard, having

First published January 1969 Amendments issued since publication

The following BSI references 6297 September

ISBN 0 580 16812 3

© BSI 03-1999 iii

In some methods the insoluble component or components of a mixture may be

Section 2. Information common to the methods given

8.2 Procedure 9.1.3 Determine the percentage of clean insoluble

9.2.4 Variant 3. Formulae to be applied where two

then Where a special pretreatment is used the values b1,

Section 3. Method of quantitative analysis by manual

13 Apparatus and reagents

Section 4. Methods of quantitative analysis by

17.6 Precision b) sodium hypochlorite solution,

18.6 Precision 19.3.2.2 Dilute ammonia solution. Dilute 20 mL of

20 Method 4. Binary mixtures of 20.4 Test procedure

21.3.2 Reagents 22.2 Principle

22.5 Calculation and expression of results 23.4 Test procedure

24.2 Principle modal d = 1.01

25.4 Test procedure 26.3 Apparatus and reagent

27.3 Apparatus and reagents 27.6 Precision

M is the molarity of standard sulphuric acid 30.3.2 Reagents

To the specimen contained in the glass-stoppered 31.2 Principle

32 Method 16. Binary mixtures of 32.4 Test procedure

Do not apply suction during or between the washing acrylic d = 0.98.

Figure 1 — Hot extraction apparatus

Table 2 — Procedures to be used for quantitative chemical analysis of

Table 2 — Procedures to be used for quantitative chemical analysis of

Appendix B Agreed allowances for moisture and other matter to be used in

Fibres Percentages Fibres Percentages

BS 135, Specifications for benzene, xylenes and toluenes.

4) Mentioned in the foreword only.

BSI — British Standards Institution

British Standards are updated by amendment or revision. Users of

In response to orders for international standards, it is BSI policy to supply the

BSI provides a wide range of information on national, European and

Subscribing members of BSI are kept up to date with standards developments

If permission is granted, the terms may include royalty payments or a licensing

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