Textile materials

testing I
Sampling
Moisture
Fiber mixtures
Fiber identification
Ji Militk
Technical University of Liberec
Textiles testing
The subject of textile testing can be answered by the 3w" questions:
1. Why do we test? 2. What do we test? 3.Who does the test?
(E. Booth, Principles of Textile Testing, Chemical Publishing Co.,
Inc., New York (1969), p. 1)
Goals of testing
Research and Development, Quality Control , Comparative
Testing, Analyzing Product Failure, End-Use Performance

Classification of textile test methods
(1) fiber identification, (2) fiber and yam analysis, (3) fabric
analysis, (4) physical performance tests ((4.1) aesthetic appearance,
(4.2) durability, (4.3) comfort (4.4) safety, (4.5) care, (4.6)
biological resistance, (4.7) environmental resistance), and (5)
performance to care-laundering and dry cleaning.
physical testing, chemical testing, and microscopic testing
Fibrous strand
Ideal case of layer composed from n fibers of the same length l,
with displacement d. Layer total length is L.
d is large compared with l
n is small
d is smaller than l
n is large
The fibrous strand is composed from k layers with
number of fibers n
1
, n
2
,n
k
. The total number of
fibers is n
T
= n
1
+ n
2
++n
k
and fraction of fiber in
strand is n
1
/n
T
, n
2
/n
T
,,n
k
/n
T
L
n
d
=
Picking from strand
1. Random picking
The probability of picking of fiber is l/d = l n/L
2. Random picking
The probability of picking of fiber is here greater than 1, i.e. at
least one fiber will be picked every times.

For the M attempts the number of picked fibers is in both cases
M l/d = M l n/L. Number of fibers taken randomly from strand is
then dependent on the length M l
1
n
1
/L, M l
1
n
2
/L ,, M l
k
n
k
/L

Sampling I
Randomized sampling: By this term we mean a series of
observation extracted from a population in such a way that each of
them has an equal chance of being extracted: in other words, the
probability that a given observation has a certain value is
proportional to the relative frequency of this value in the
population.
Systematic sampling; the samples are removed at constant intervals
of time ( hour, shift): this system, frequently used in quality
control, can be satisfactory in the absence of periodic variations in
the production quality, or if the period of the variations is not of the
same order of magnitude as the interval between two successive
sampling.
Sampling II
Stratified sampling: when there is reason to hold that the batch
is not homogenous in all its parts. It is divided into a number
of homogenous "layers and the sample is composed of
specimens taken from each of them in a quantity proportional
to the size of every layer.

Weighted sampling: measurements on fibers often give rise to
samples which are not random (numerical), but weighted; the
weight factor is also reflected in the value of the calculated
statistical parameters. ( see. length biased sample)
One step sampling
2
2
x
n
o
o =
( )
2 2 2
2 2
( - )
1
-
x x
N n n
for higher N
n N n n N n
o o o
o o
| |
= ~
|
\ .
x x
x t =x m o
From population of size N the n samples are selected
Sampling with replacements
Sampling without replacements
Confidence interval for
Sample size
( )
1 / 2
-1 t t n
o

Sample size
2 2
2
p
t v
n
m
=
*
x
p
m
m
x
=
v
x
o
=
( )
( )
( )
2 2
*
2 2 2
/ 1
/ 1
x
t N N
n
m t N
o
o

=
+
In practice t 2, m
P
= 0.01
v = 0.05 n*=100
v = 0.10 n*= 400
Two step
sampling I
2 2
2
1 2
1
ij
i j
a a
N N
o =

( )

1 2
1 2
N N N
n n n
=
=


2 1
1 1
i ij i
j j
a a a a
N N
= =


Population of size N is naturally divided into N
1
groups and in
each group are N
2
elements. The n samples are created from n
1

groups and n
2
elements
Population
1. Level selection of groups
2. Level selection of elements
a
ij
i . . . group, 1 . . . N
1
j . . . element, 1 . . . N
2
( )
2
2
1
1
1
i
i
a a
N
o =

2 2 2
1 2 c
o o o = +
Mean values
Variance between groups
Variance in groups
Total variance
Two step
sampling II
2 2
2
1 2
1
ij
i j
s x x
n n
=

( )

2 1
1 1
i ij i
j j
x x x x
n n
= =


Sample
x
ij
i . . . group, 1 . . . n
1
j . . . element, 1 . . . n
2
( )
2
2
1
1
1
i
i
s x x
n
=

2 2 2
1 2 c
s s s = +
Mean values
Variance between groups
Variance in groups
Total variance
Sampling without replacements
Two step
sampling III
Mechanical sample - in each group is
randomly selected one element
( )
2 2
1 1
1
1 1
1
x
N n
n N
o o

1 1 2
1 n n N n = = =
2
2
2
x
n
o
o =
Group sample groups are randomly selected.
In each selected group all elements are tested
1 1 2 2
n N n N s =
Worst case
Two step
sampling - example
N
1
= 100 cops. Strength testing on the N
2
= 1000 portions
Let
2 2
1 1 2 2
1 2
1 1 1 2 2
2 6.65
( 1) ( 1)
x
N n N n
m
n N n n N
o o

= + =

2
2 3.46
c
x
m
n
o
= =
2
1 1
1
1 1
2 20
( 1)
x
N n
m
n N
o

= =

( ) ( ) ( )
1 2
17.3 300 10 100 14.14 200
c
o o o = = =
2
2
1
2 2.82
x
m
n
o
= =
One step sampling (n = 100)
Two step sampling (n
1
= 10, n
2
= 10)
Mechanical sampling
(n
1
= 100, n
2
= 1)
minimum
Group sampling
(n
1
= 1, n
2
= 100)
maximum
Fibers sampling - Zoning
Zoning is a method that is used for selecting samples from raw
cotton or wool or other loose fiber where the properties may vary
considerably from place to place.
A handful of fibers is taken at random from each of at least
40 widely spaced places (zones) throughout the bulk of the
consignment (quantity of material delivered at the same time)
Each handful is divided into two parts and one half of it is discarded
at random; the retained half is again divided into two and half of
that discarded.
This process is repeated until about n/x fibers remain in the handful
(where n is the total number of fibers required in the sample and x
is the number of original handfuls).
Each handful is treated in a similar manner and the fibers that remain
are placed together to give a correctly sized test sample containing
n fibers.
Zoning
schemes
Final sample
Fibers sampling - Core
Technique that is used for assessing the proportion of grease,
vegetable matter and moisture in samples taken from unopened
bales of raw wool. A tube with a sharpened tip is forced into the bale
and a core of wool is withdrawn.

The tubes for manual coring are 600 mm long so that they can
penetrate halfway into the bale, the whole bale being sampled by
coring from both ends.

A detachable cutting tip is used whose internal diameter is slightly
smaller than that of the tube so that the cores will slide easily up the
inside of the tube.

To collect the sample the tube is entered in the direction
of compression of the bale so that it is perpendicular to the layers of
fleeces.
Sampling from
rovings and yarns
One of the main difficulties in sampling fibers is length biasing due
to fiber length distribution. Unless special precautions are taken, the
longer fibers in the material being sampled are more likely to be
selected by the sampling procedures, leading to a length-biased
sample.
This is particularly likely to happen in sampling material such as
sliver or yarn where the fibers are approximately parallel
The fiber extent
rather than the fiber
length determines
the likelihood of
selection.
Numerical
sample
Length bias must be avoided in the measurement of fiber length, but
any bias can also have effects when other properties such as fineness
and strength are measured since these properties often vary with the
fiber length.
Numerical ( unbiased) sample
A, B represent two planes separated
by a short distance in a sample from
parallel fibers. If all the fibers
whose left-hand ends (shown as
solid circles) lay between A and
B were selected by some means they
would constitute a numerical sample.
.
Length biased sample
Length-biased sample. In a length-biased sample the percentage of
fibers in any length group is proportional to the product of the
length and the percentage of fibers of that length in the bulk
The removal of a length-biased sample
changes the composition of the remaining
material as a higher proportion of the longer
fibres are removed from it.
Length biased sample is realized by
gripping the sample along a narrow line
of contact and then combing away any
loose fibers from either side of the grips.
This type of sample is also known as a
tuft sample.
Tuft sample
Tuft sample
Tuft sample contains more pieces of the longer fibers because they
are more likely to cross grip section.
If there are equal numbers of fibers in each length group, the total
length of the group with the longest fibers will be greater than that
of the other groups so that there will be a greater number of those
fibers in the sample (higher mean value).
Samples for the measurement of fiber diameter using the projection
microscope are prepared in this manner by sectioning a bundle of
fibers, thus giving a length-biased sample.
The use of a length-biased sample is deliberate in this case so that
the measured mean fiber diameter is then that of the total fiber
length of the whole sample. If all the fibers in the sample are
considered as being joined end to end the mean fiber diameter is
then the average thickness of that fiber.
Comparison
Histograms of length-biased and numerical samples.
Random draw
method
The sliver is parted carefully by hand and placed
over two velvet boards with the parted end near
the front of the first board.
The opposite end of the sliver is weighed down
with a glass plate to stop it moving.
A wide grip which is capable of holding
individual fibers is then used to remove and
discard a 2mm fringe of fibers from the parted
end. This procedure is repeated, removing and
discarding 2mm draws of fiber until a distance
equal to that of the longest fiber in the sliver has
been removed.
The sliver end has now been 'normalised' and any
of the succeeding draws can be used to make up a
sample as they will be representative of all fiber
lengths.
Cut square
method
A length of the yarn is cut off and the end
untwisted by hand. The end is laid on a small
velvet board and covered with a glass plate.
The untwisted end of the yarn is then cut about
5mm from the edge of the plate.
All the fibers that project in front of the glass
plate are removed one by one with a pair of
forceps and discarded.
By doing this all the cut fibers are removed,
leaving only fibers with their natural length.
The glass plate is then moved back a few
[mm], exposing more fiber ends.
These are then removed one by one and
measured. When these have all been measured
the plate is moved back again until a total of 50
fibers have been measured.
Yarn
Yarn sampling
Yarn for testing: 10 packages are selected at random
from the consignment.
If the consignment contains more than 5 containers, 5
containers are selected at random from it. The test
sample then consists of two packages selected at
random from each container.
If the consignment contains less than five containers ,
ten packages are selected at random from all the
containers with approximately equal numbers from
each containers.
The appropriate number of tests are then carried out
on each package.
Consignment = quantity of material delivered at the same time
Fabric
sampling
Rules:
1. Fabric samples are always taken
from the warp and weft separately
as the properties in each direction
generally differ.
2. The warp direction should be marked on each sample before it is
cut out.
3. No two specimens should contain the same set of warp or weft
threads. In the correct layout each sample contains a different set of
threads so that their properties are potentially different.
4. Samples should not be taken from within 50mm of the selvedge
as the fabric properties can change at the edge and they are no
longer representative of the bulk.
Correct

Moisture
Some of the important properties
of textile fibers are closely related to their
behavior in various atmospheric conditions.
Many physical properties are affected by the amount of water
absorbed such as dimensions, tensile strength, elastic recovery,
electrical resistance, and rigidity
Hygroscopic fibers are able to absorb water vapor from a moist
atmosphere.
The structure of the fabric can
modify the behavior of the fiber.
Fabrics from a hydrophobic fibers
can pick up water by a "wicking"
action along the fiber and yam
surfaces.
wool
Swelling
The swelling due to moisture absorption
B P Saville: Physical testing of textiles, 1999, Woodhead Publishing Ltd
Swelling anisotropy
Fiber
Swelling
Dimensional changes due to water sorption
Radial swelling S
D
, area swelling S
R,
axial
swelling S
A
volume swelling S
V
).
R A A R V
S S S S S * + + =
/
D
S D D = A
/
R
S A A = A
/
A
S l l = A
/
V
S V V = A
2
2
R D D
S S S = +
Area swelling
Radial swelling
Axial swelling
Volume swelling
Al
The ratio S
D
/S
A
is always
greater than 1 and can reach
very high values
Okubayashi, et. all.: Kinetic study of
moisture sorption, Carbohydrate
Polymers, 58, 293-299, (2004)
Hygral
expansion
Hygral expansion HE [%] is reversible
variation in the dimensions of a fabric
subjected to variations in humidity: it lengthens when it is more
humid and shortens as it becomes drier.
Basically, the causes of hygral expansion are due to the large
difference between longitudinal and radial swelling in a fiber when
it absorbs humidity. E.g. the diameter of wool increases by about
16% at saturation (35% regain), while the length increases by only
1%.
In a fiber subjected to bending (as in the
case of a fabric), this radial swelling tends to
cause straightening (increase of the radius of
curvature , due to the increase in the moment
of inertia I), and thus a decrease in crimp and a
lengthening of the fabric.
Electrical
resistance
The moisture content of fibers
has an important effect on their
electrical properties. The main
change is to their electrical
resistance.
resistance of nylon
The resistance decreases with increasing moisture content. For
fibers that absorb water the following approximate relation between
the electrical resistance RE and the moisture content M holds for
relative humidities between 30% and 90%
n
RE k M

=
n and k are constants

Air humidity
Absolute humidity is the weight
of water present in a unit volume of moist air [g m
-3
]

Relative humidity RH is the ratio of the absolute humidity of the
air to that of air saturated with water vapor at the same temperature
and pressure. It is also the ratio of the actual vapor pressure p
a
to
the saturated vapor pressure p
sv
at the same temperature, expressed
as a percentage.
100
a
sv
p
RH
p
=
Regain of fabrics appears to depend on the relative humidity
rather than the actual amount of water vapor present
water vapour
in the atmosphere
Air
Pressure
Dry air
Density
Thermal conductivity
The dew point is the temperature at
which the saturation state (RH =
100%) of the air and water vapor
during a cooling process is reached.
Saturated vapor pressure p
sv


Standard conditions
The standard atmosphere

temperature of 21 1C (70 2F)
relative humidity of 65 2 %
Differences in temperature of 30 C should not cause too much
variation in physical characteristics.
Humidity:
most man-made fiber fabrics, being hydrophobic, do not absorb
much moisture and so will not be greatly affected by changes in
relative humidity.
More significant differences may be evident in the results of the
tests of hydrophilic materials (e.g. rayon, cotton and wool) at
different relative humidities.
Humidity determination I
Wet and dry bulb hygrometer
If the bulb of a glass thermometer is surrounded by a wet sleeve
of muslin in an atmosphere that is not saturated, water vapor will
evaporate into the air at a rate proportional to the difference
between the actual humidity and 100% humidity. Owing to the
latent heat of evaporation, heat is drawn from the thermometer
bulb, thus cooling it.
This cooling effect has the consequence that the temperature
indicated by a wet bulb thermometer is lower than the air
temperature.
By mounting two identical thermometers together, one with a wet
sleeve and one with a normal bulb, the two temperatures can be
read directly.
Humidity determination II
The relative humidity can then be calculated from the
temperature difference between the two readings. The value
is usually read from appropriate tables.

The rate of evaporation of water is also governed by the
speed of the airflow past the wet bulb. Therefore for
accurate work the rate of airflow past the thermometer bulbs
has to be controlled as still air conditions are difficult to
achieve in practice.

The sling and the Assmann type hygrometers are two
instrument in which the flow of air is controlled.
Assmann
hygrometer
dry
wet
air
T
d
T
w
p
w
= p
S
(T=T
w
)
p
d
(T
d
>T
w
)

d
w
Amount of water evaporated at equilibrium
to the unit volume of air
m = k
1
(p
w
p
d
)

Evaporation heat
q = k
2
(T
d
T
w
) = m L
V
L
V
- latent heat of evaporation = 2.26 MJ kg
-1
.
Combination: (T
d
T
w
) = L
V
k
1
(p
w
p
d
)/k
2
Among the terms which appear in this final formula, L
V
, k
1
, k
2
and p
w

are known or can be obtained from special tables: by reading T
d
and
T
b
on the two thermometers one can thus calculate p
d
and then relative
humidity RH
Hair hygrometer
Bundle of human hair is used, which have
the property of expanding or contracting
according to an increase or a decrease in
the humidity in the air with which they are
in equilibrium.
This instrument is not as accurate as the
previously mentioned instrument (margin
of error 3-4% total).
It has the advantage that it can be read
directly and is frequently used for its
simplicity, normally coupled with a bi-
metallic thermometer and a recording
device
V . .. Hair bundle
S . .. Adjusting
Z .. . Balance weight
R . .. Indicator
Regain and
moisture content
oven dry weight = D
weight of water W = conditioned weight - dry weight
Regain R is defined as the weight of water in a material expressed as
a percentage of the oven dry weight

Moisture content MC is the weight of water in a material expressed
as a percentage of the total weight (or conditioned weight as
measured under standard conditions).
100
W
MC
W D
=
+
100
W
R
D
=
( ) ( )
and
1 100 1 100
MC R
R MC
MC R
= =
+ / /
Regain prediction
( ) ( )
4
100 R a b RH T = +
1
o
o
a b p RH
R
a p RH
=
+



Regain R is dependent on the relative humidity
RH [%] and temperature T [
o
C].
Rough estimate (40-65 % RH):
cotton a = 0.8007, b = 0.02912
Wool a = 2.8, b = 0.02938
More precisely is regain R predicted as:
where p
sv
[kg cm
-2
] is saturated water vapor pressure.
(silk: a = 5.5 , b = 0.97)
RH [%]
R

[
%
]

25
o
C
1. wool
2. jute
3. silk
4. cotton
5. acetate
Kinetic of
moisture absorption
Transfer rate in air to the fiber surface
M amount of transferred moisture till equilibrium
D* - diffusion coefficient in air (around 0.25 cm
2
s
-1

(20
o
C). Diffusion of water in fibers is slower ~ 10
-7

cm
2
s
-1

S area of absorbing surface
L distance of source from fibers
C
o
concentration of water in the source (not changed
during time)
C
1
initial concentration of water in the fiber
Transfer rate K is reciprocal value of characteristic time of sorption t
e
i.e. time when concentration of water in the fiber reaches value
(1-e
-1
) C
o
= 0.63 C
o
o e
C C 1- exp(-t/t ) = /
100g cotton in cylinder r = 2 cm
and L = 10 cm is t
e
= K
-1
= 5 hours.
Regain
measurement
Regain is based on the oven
dry mass, which for most fibres
is the constant mass obtained by
drying at a temperature of
105 2
o
C. Constant mass is
achieved by drying and weighing
repeatedly until successive
weightings differ by less than 0.05%
or at 5 min intervals
if using a forced air oven
Conditioning oven
A continual flow of air at the
correct relative humidity is
passed through the oven which
is maintained at 105
o
C.

Conditioning ovens
The ventilation must ensure an exchange of air at least 20 times
per hour, with an entrance reasonably speed of not less than 0.2
m/s. The operation can be speeded up enormously (reducing the
time required by about a half) with a forced ventilation system
(e.g. CSIRO Direct Reading) or by operating in depression, i.e.
attaching the ventilator to the air outlet e.g. Branca Regain Tester)
Branca Regain Tester
CSIRO Direct Reading
Rapid regain
dryer
The rapid regain type of dryer represents a quicker way of drying
fiber samples. The basis of this type of dryer is that the hot air is
blown directly through the sample to speed up the drying process.
The WIRA improved
rapid regain dryer,
shown in Fig., uses a
powerful
blower to force air
through the sample in
order to give more
rapid drying
The time for weighing should not
exceed 20s from removal of the
sample from the dryer
Fiber volume
Fiber packing
Temperature
Ventilation
Laboratory conditioning
cabinets
Laboratory cabinets
control the atmosphere of
a relatively small volume.
The relative humidity of a
small enclosed volume of
air, such as a desiccators,
may be controlled by the
presence of a dish
containing a saturated
solution of certain salts.
The relative humidity of air over
saturated solutions of salts at 20
o
C
Correct
invoice weight
Samples of at least 200 g are
selected according to adequate
sampling procedures and
immediately stored in airtight containers so that no moisture is lost.
The samples are weighed and then the oven dry weight is
determined as described above.

M = mass of consignment at time of sampling,
D = oven dry mass of sample,
S = original mass of sample
C = oven dry mass of the consignment
R
I
= commercial moisture regain
Correct invoice weight = CIW
100
100
I
R
CIW C
+
| |
=
|
\ .
M D
C
S
=


Typical Regains at 65% rh and 20
o
C
0
2
4
6
8
10
12
14
16
18
P
o
ly
p
r
o
p
.
P
E
T

A
c
r
y
lic

N
y
lo
n
6
6

T
r
ia
c
e
t
a
t
e

F
la
x

A
c
e
t
a
t
e

C
o
t
t
o
n

S
ilk

J
u
t
e

V
is
c
o
s
e

w
o
o
l
Fibre Type
R
e
g
a
i
n

(
%
)
Fibrous
mixtures I
Random bundle of nearly parallel fibers of various origin
k components
m
ti
..............(dry) mass of i-th component

i
............... density of i-th component
V
i
............... volume of i-th component
l
i
.................mean length of i-th component
n
i
............... fiber number of i-th component
m
t
= m
ti
...total (dry) mass of mixture
V = V
i
..... total volume of mixture
L
i
= n
i
l
i
..... total length of i-th component
w
i
= m
ti
/ m
t
.. mass fraction of i-th component
v
i
= V
i
/ V ....volume fraction of i-th component
From mass fraction
to volume fraction
1
i i
i
k
i i
i
w
v
w

=
=

/

/
1
i i
i
k
i i
i
v
w
v

=
=

From volume fraction
to mass fraction
Fibrous
mixtures II
Mixture density
t i t i
i
i i i
m m w
T
l n L
= =



i t i i
V m w = /
1 1
1
t
k k
i i i
i i
m
T
L w T
= =
= =


/
1 1 1
1
t t
k k k
i t i i i i
i i i
m m
V m w w

= = =
= =


/ /
Weighted harmonic mean
Mixture fineness T [tex]
i t i i
L m w T = /
Weighted harmonic mean
t i t i
i
i i
m m w
V V
= =


Fibrous
mixtures III
Mixture metric number Mn [Cm]
ui t i V i
I i
t i t i
m m m
R
m m

= =
i t i i
L m w Cm =
1
1
k
Vi
k
i
I i I i
i
t
m
R wR
m
=
=
= =

1
1
k
i
k
i t i i
i i
i
t t
L
m Cm w
Cm w Cm
m m
=
=
= =

Weighted arithmetic mean
Mixture standard moisture regain R
I
[%]
V i t i I i
m m w R =
i i
i
t i t i
L L
Cm
m m w
= =

Weighted arithmetic mean
m
Vi
... Standard moisture content of the i-th component
m
Ui
... Mass of the i-th component with moisture content m
Vi
= m
Ui
-m
t
Fibrous
mixtures IV
Corrected mass fraction w
i
*
(to the

standard regain R
I
)
1
u t
I u t I
t
m m
R m m R
m

= = + ( )
1 1
1 1
ti ui I I i
i
t u Ii Ii
m m R R w
w
m m R R
+ +
= = =
+ +
*
( ) ( )

( ) ( )
Example
1
ui t i I i
m m R = + ( )
1 1
1 1
i
ui I i t i I i i
u I t I
m R m w R w
w
m R m R
+ +
= = =
+ +
*
( ) ( )

( ) ( )
m
U
... Total fiber mass with standard moisture content

Fiber 1 Fiber 2
w
1
= 0.5, R
I1
= 0.1 w
2
= 0.5, R
I2
= 0.01
R
I
= w
1
R
I1
+ w
2
. R
I2
= 0.5 x 0.1 + 0.5 x 0.01 = 0.055
w
1
*
= (0.5 (1 + 0.1)) / (1 + 0.055) = 0.521 w
2
*
= 0.479

If R
Ii
> R
I
then w
i
*
> w
i
and If R
Ii
< R
I
then w
i
* < w
i
Fibrous
mixtures V
Utilization of the corrected mass fraction w
i
*

1
u t
I u t I
t
m m
R m m R
m

= = + ( )
1
1
1
1
1
1
1
k
k
Ii i
u
Ii ti
k
i
i Ii Ii i
I
i
t t Ii
R w
m
R m
R R w
R
m m R

=
=
=
(
| |
+
( = = =
|
+
(
\ .

*
-1
*
( )
-
( )
1
ui t i I i
m m R = + ( )
1
1
k
Vi
k
i
I i I i
i
t
m
R wR
m
=
=
= =

For other properties use of the corrected mass fraction w
i
*
instead of w
i
Fibrous
mixtures VI
Mechanical characteristics (property P)
Individual components are homogeneous phases (properties P
i
)
1
i
i
v
P
P

=

i i
P v P =


Lowest limit
Highest limit
Example: modulus prediction
from two fiber types
Lowest limit
Reuss
Highest limit
Voight
Fiber identification
Relatively simple methods for fibers identification:
Burning test
Microscopic examination (longitudinal and cross section).
Solubility tests in various reagents.
Staining tests (fibers are dyed or stained with specific dyes).
Fiber density.
Burning tests may give a clue to fiber type, that is, whether it is
natural or man made. Microscopic examination and staining tests
may help confirm identification by burning. Solubility and fiber
density tests are particularly necessary when we want to separate the
individual fibers used in a blend. However, in some instances, the
use of the burning test, microscopic, staining, solubility, and fiber
density tests are of little value for fiber identification purposes.
Burning test
The burning test is useful to those who have no other means of
identification.
This test does have certain limitations. The burning behavior of
the fiber may be affected by the finish applied to the fabric.
Three things:
1. How it burns: Does it burn rapidly? Does it go out quickly? Does
it smolder?
2. How it smells: when the flame goes out, smell the smoke.
3. The ash: note its color and its shape. Can you crush it, or is it
hard?
Protein fibers
Cellulose fibers

Identification of Fibers by
Chemical Solubility
The sample should
remain in the solvent
for five minutes before
proceeding to next
step. Observe the
sample to determine
removal of fiber(s)
after each test.
Proceed In numerical
order given in the
table. Always rinse the
residue thoroughly
after each step.
For verification,
examine the residue
for microscopic
identification.
24
o
C
100
o
C
20
o
C
93
o
C
Density estimation

Single single fiber specimen is placed in a series of specially
prepared liquids of known density.
If the density of the fiber is greater than liquid density, the
specimen will sink in the liquid; if the density of the fiber is lower,
the specimen will float (The fiber's surface must be free of air
bubbles since they can affect the results of the test ).
Liquids are prepared by mixing, in various proportions, carbon
tetrachloride (density of 1600 kg m
-3
at room temperature) with
xylene (density of 870 kg m
-3
at room temperature).
Before using any of the liquids for fiber identification, their specific
gravity should be checked with a calibrated hydrometer
g mass
V volume
= =
The density of the fibers increases with the increase of regain, despite the fact that
water has a lower density than almost all textile fibers. This is due to the lower
increase in volume which follows the swelling, especially at the beginning (the
water molecules enter the structure and almost completely fill up the spaces which
were initially available).
Hydrostatic
density
1. Spiral (0.2-0. 3 mm) - weight g
1
in liquid
2. Fiber bundle (dry weight g
2
)
3. Liquid n heptane (density
c
= 648 kg
m
-3
)
Level of liquid (x)
Spiral and bundle weight in liquid g
3
Fiber bundle weight in liquid g
4
= g
3
g
1
, weight loss P = g
2
g
4
Archimedes law: volume of excluded water V = P/
c
Fiber density :
2 2
2 3 1
c
g g
V g g g

= =
+

The difference in weight is equal to
the weight of the liquid displaced, i.e.,
the volume of the fiber specimen x
the density of the fiber specimen x
the density of the liquid.
Displacement liquids used are n-
heptane (liquid of lower density
than the fiber)
Density
Pycnometric
Pycnometer glass container having precise volume
V (mark 1-2) with capillary 3 (volumes 25 or 50 cm
3
)
Empty pycnometer weight is g

Weight of pycnometer with liquid is g
2
Weight of pycnometer with fibers (approx. 0.3 g)
and liquid is g
1
Liquid (toluene) density
c
,
Fiber bundle dry weight is g
b
and volume

V
b



( )
1 2
b
b c
b
g
g g V
V
= = -
1 2
b c
b
g
g g g

=
+

( )
1 b c b
g g V V V = + +
g
g
2
g
b
+g
g
1

Densities and
porosity
: real = skeletal, real volume of solid (without pores) evaluated
by pycnometer filled by liquid with small molecules.

I
: intrinsic = mercury, volume of solid with pores evaluated by
pycnometer filled by liquid with no wetting liquid (mercury)
Pore volume: (cm
3
/g) V
p
= 1/
I
- 1/
Porosity: (-) P = 1 - (
I
/)
Specific area (m
2
/g) :
S = a
m
A g
a
m
maximum amount of gas (mol gas/g)
g...area of one gas molecule
A = 6.022 10
23
(molecules/mol) Avogadro number
Nitrogen g = 0,162 nm
2
/molecule
Sorption
and porosity
p/p
0
n
1 0
p/p
0
n
1 0
p/p
0
n
1 0
p/p
0
n
1 0
p/p
0
n
1 0
p/p
0
n
1 0
Common
adsorbates
Gas Temp.
K
Area per molecule
(nm
2
)
Notes
Nitrogen 77 0.162 Most of materials can be
analyzed in these conditions
except very low surfaces and
some micropores
Argon 87, 77 0.142 Specially used for some
microporous zeolites that
cannot be measured by
nitrogen
Krypton 77 0.21
(other values are also
reported)
Used for extremely low
surfaces. Difficult analysis
due to saturation and
expensive
II
B
I III
V
VI
IV
B
IUPAC
Pores
Pores dimensions: IUPAC classification
Ultramicropores
micropores < 2 nm
supermicropores
mesopores 2-50 nm
macropores >50 nm
Based on the various mechanisms of gases physical adsorption:
micropores : volume filling
supermicropores : volume filling + multiple layer
adsorption
mesopores : multiple layer adsorption + capillary
condensation
Pores are cylindrical
Pore
size
The intrusion of a non wetting liquid (often mercury) at high pressure
into a material through the use of a porosimeter. The pore size can be
determined based on the external pressure needed to force the liquid
into a pore against the opposing force of the liquid's surface tension.
Washburn relation for the material having cylindrical pores :
Since the technique is usually done under
vacuum, the gas pressure begins at zero.
The mean contact angle of mercury is
140. The surface tension of mercury at 20
C under vacuum is 480 mN/m. Then:
P
L
= pressure of liquid [MPa]
P
G
= pressure of gas
= surface tension of liquid
= contact angle of intrusion
liquid
D
P
= pore diameter [nm]
evacuation filling pressure
Mercury
porosimery
pore
mercury
Cumulative
pore distribution
pore
distribution
Intrusion
vs. pressure
Infrared
spectroscopy I
When infrared radiation is passed through
a substance, certain frequencies are
absorbed and others are transmitted. Infrared spectroscopy,
therefore, consists of determining the frequencies at which absorption
occurs.
The absorption in the infrared region is associated with molecular
vibration. The vibrational modes involve localized motions of small
groups of atoms and emit absorption bands at frequencies characteristic
of these groups and the type of motion they undergo.
Most infrared spectrophotometers use a glowing light source to provide
electromagnetic radiation from 2.5 to about 15 microns
In practice, the usual absorption spectrum in the infrared region is
shown as a plot of absorption versus the wavelength or absorption
versus wave number (cm
-1
). The wave number is defined as the
reciprocal of the wavelength.
Infrared
spectroscopy II
PAD 6
PAD 6,6
Thermal
Analysis

DTA - the difference in temperature between a sample and an inert
reference material is recorded as a function of temperature.
This difference is recorded by the instrument as a function of
temperature.( thermogram).
Changes detected may include the glass transition, desorption of
moisture, polymer crystallization or fusion, and irreversible
decomposition processes.

Differential Thermal Analysis
Undrawn polyester fiber
Thermal analysis is the
measurement of changes in
physical or chemical
properties of materials as a
function of temperature
DSC
scheme
N
2
flow
Pt thermopile
Sample
Reference
Pt thermopile
T
1

T
2

heater
heater
Low mass
1 gram
AW
Differential Scanning Calorimetry
(DSC). Measure heat absorbed or
liberated during heating or cooling
DSC
thermogram
Temperature, K
Thermogram
d
H
/
d
t
,

m
J
/
s

Glass transition
crystallization
melting
exo
endo
dq
p
/dt = heat flow
dT/dt = heating rate
(dq
p
/dt) / (dT/dt) = dq
p
/dT = c
p
Heat Capacity
T(t) = T
0
+ a t