Download as pdf or txt
Download as pdf or txt
You are on page 1of 30

08/07/2021

WELCOME

FIBER ANALYSIS

1
08/07/2021

TYPES OF FIBRE

Mainly 2 types of fiber


1. Natural Fibers
- Plant (Cellulosic Fibers)
- Animal ( Hair/Protein)
- Mineral
2. Man Made Fibers.
- Synthetic fibers
- Regenerated Cellulosic fibers

Insert Footer Here 3

TYPES OF FIBER
Natural Fibers:
• Cotton
• Hair (Wool, Cashmere)
• Hemp (From Jute)
• Linen
• Ramie
• Silk
• Asbestos (Mineral fiber)

Man Made Fibers (Regenerated Cellulosic Fibers):

• Acetate & Tri acetate


• Rayon/Viscose (Regenerated Cellulose)
• Lyocell & Tencel
• Modal
4

2
08/07/2021

TYPES OF FIBRE

Man Made Fibers (Synthetic Fibers):

• Acrylic
• Mod Acrylic
• Nylon/Polyamide
• Olefin
• Polyester
• Spandex.
• Metallic fiber

FIBER ANALYSIS PROCEDURE

Two types of fiber analysis process


- Qualitative Analysis
- Quantitative Analysis

Qualitative Analysis:
• Burning Behavior Analysis
• Microscopically Analysis
(Cross Sectional & Longitudinal View)

Quantitative Analysis:
• Manual Separation Analysis
• Chemical Analysis
• Counting Analysis
6

3
08/07/2021

BURNING BEHAVIOR

Insert Footer Here 7

MICROSCOPICAL ANALYSIS

Fiber Longitudinal View


8

4
08/07/2021

MICROSCOPICAL ANALYSIS

Fiber Longitudinal View


9

MICROSCOPICAL ANALYSIS

Fiber Longitudinal View


10

10

5
08/07/2021

MICROSCOPICAL ANALYSIS

Cross Section View 11

11

MICROSCOPICAL ANALYSIS

Cross Section View 12

12

6
08/07/2021

MICROSCOPICAL ANALYSIS

Cross Section View 13

13

FIBER ANALYSIS PROCEDURE

Fiber Composition ISO 1833 Part 1-24


• For Qualitative Analysis & Quantitative Analysis

Fiber Composition AATCC 20-2013(2018)e


• For Qualitative Analysis

Fiber Composition AATCC 20A-2020


• For Quantitative Analysis

14

14

7
08/07/2021

FIBRE ANALYSIS FLOW CHART

Take the Drying & Weight the Microscopic


Pretreatment
Sample Cooling sample Analysis

Manual/Chemical Weight the


Drying & Cooling Calculation
Separation sample

15

15

01
FIBRE ANALYSIS

ISO 1833

16

8
08/07/2021

SAMPLING

Take a laboratory sample as described ISO


5089, that is representative of the laboratory
bulk sample and sufficient to provide all the
specimens, each of at least 1.00 gm that are
required.
Fabrics may contain yarns of different
composition and account should be taken of
this fact in the sampling of the fabrics.

ISO 1833 17

17

SAMPLING-FOR BLEND

Cut 3 pieces of specimens along the diagonal


of the fabric because different warp yarns and
different weft yarns can be tested so as to find
a consistent result of fabric.
For a regular pattern, repeating unit of fabric
should be cut.
For garment, specimen should be taken from
different part of the garment as front panel,
black panel, sleeves as in preliminary test.

ISO 1833 18

18

9
08/07/2021

PRETREATMENT

• There is not necessary to apply for fabric


containing one kind of fibres, e.g., cotton
only, wool only or polyester only, etc.
• There are 4 kinds of simple pre-treatments
applying to different fibre blends (fabric
contains at least 2 different fibres).
• The purpose is to remove non-fibrous
material such as resin, oil, waxy substance
or soluble matter so as not to affect the
actual percentage of fibres.

Insert Footer Here 19

19

PRETREATMENT

POLYESTER / CELLULOSIC FIBRES e.g. T/C, T/Ramie or T/Linen


0.1N HCl (a few drops of conc. HC1 + 150 ml water) is used to remove resin. The fabric is immersed in
0.1N HCl to boil for minutes, then rinse with water and then neutralize with dilute ammonia solution
(several drops of conc. ammonia + 150 ml water). Finally, the fabric is rinsed with water again.

FABRIC CONTAINING ANIMAL FIBRE(S) e.g. Silk Blend, Wool Blend or Angora Blend
Ether is used to remove oil or waxy substances. The fabric is put in a beaker containing ether and stir
with a glass rod for a while, then cover with a watch glass for 15 minutes. After 15 minutes, the fabric is
squeezed and place in fume cupboard to evaporate the ether.

OTHER FIBRES e.g. T/C/N, N/A, R/C, A/P, N/Sp, etc


Boiling water is used to remove soluble matter. The fabric boils with water for 5 - 10 minutes and then
dry it.

ISO 1833 20

20

10
08/07/2021

PRETREATMENT

FABRIC CONTAINING STARCH


When you feel a cellulosic fibre blend fabric being rigid, the fabric may contain starch. How to know it ?
A drop of iodine solution (brown colour) is added to the fabric. If the fabric becomes blue or dark
colour, the fabric must contain starch. If the fabric remains brown colour, the fabric will be containing
starch.
Enzyme solution is used to remove starch. How to know all starch to be removed ? First rinse the fabric
with water and then retest the fabric by addition of iodine solution.

Insert Footer Here 21

21

PRETREATMENT-STRIPPING
PRETREATMENT OF RAYON / COTTON
Sodium hypochlorite
Immerse the dried specimen for not more than 5 min in 2.5% sodium hypochlorite at 15 - 25.
Stir occasionally.
Wash thoroughly with sodium bisulfite (1.0%) followed by water &Dry at 105-110C to constant weight.
Sodium Hydroxid
Immerse the dried specimen for not more than 5 min in 5.0% sodium hydroxide at 100C.
Stir occasionally.
Rinse thoroughly with water and dry at 105-110C to constant weight.
Dimethylformamide
Immerse the dried specimen in dimethylformamide at 80C for 30 min.
Stir occasionally.
Rinse thoroughly with water and dry at 105-110C to constant weight.

Insert Footer Here 22

22

11
08/07/2021

MECHANICAL SEPARATION

Yarn:
Cut the yarn into pieces of a suitable length and
separate the fiber types by means of a needle and, if
necessary, a twister. The fiber types so obtained are
placed in pre-weighed weighing bottles and dried at
(105±3)°C until a constant mass is obtained. Conduct
all drying operations for not less than 4 hours and not
more than 16 hours at (105±3)°C in a ventilated oven
with the oven door closed throughout.

Insert Footer Here 23

23

MECHANICAL SEPARATION

Analysis of Cloth:
Select from the pre-treated laboratory test sample,
well away from selvedge. A specimen of masses not
less than 1.0 g with edges carefully trimmed to avoid
fraying and running parallel with weft or warp yarns,
or in the cases of knitted fabrics in the line of knitted
fabrics in the line of wales and courses. Separate the
different fiber types, collect them in pre-weighted
weighing bottle and proceed

Insert Footer Here 24

24

12
08/07/2021

DISSOLVING-BLEND FIBRE

We must follow the dissolving order to find


the actual percentage of each fibre. If we do
not follow the dissolving order, incorrect result
may be obtained.

Insert Footer Here 25

25

FIBRE ANALYSIS

01 Cotton + Elastane (ISO 1833 Part 1 & 12)

02 Cotton + Polyester (ISO 1833 Part 11)

03 Cotton + Viscose (ISO 1833 Part 6)

26

26

13
08/07/2021

QUANTITATIVE CHEMICAL ANALYSIS


GENERAL PRINCIPLES OF TESTING
ISO 1833 PART 1:2020

27

SCOPE

• This part of ISO 1833 specifies a common method


for the quantitative chemical analysis of various
binary mixtures of fibres.
• This method and the methods described in the
other parts of ISO 1833 are applicable, in general,
to fibres in any textile form.
• Where certain textile forms are excepted, these are
listed in the scope of the appropriate part.

ISO 1833 PART 1:2020 28

28

14
08/07/2021

PRINCIPLE

• After the identification of the components of a


mixture, one component is removed, usually by
selective solution,
• The insoluble residue is weighed, and the
proportions of soluble component are calculated
from the loss in mass.
• Where relevant, the fibre in the larger proportion
is removed first.

Insert Footer Here ISO 1833 PART 1:2020 29

29

APPARATUS & REAGENTS


• Light petroleum:
Re-distilled, distilling between 40°C and 60°C.
• Distilled or deionized water
• Stoppered weighing bottole
• Glass Filter Crucible:
Capacity 30 to 40 ml, with sealed-in sintered
disk filter with pore size of 90 μm to 150 μm.
The crucible shall be provided with either a
ground glass stopper or a watch-glass cover.
In place of a glass filter crucible, any other
apparatus giving identical results may be used.

Glass Filter Crucible

ISO 1833 PART 1:2020 30

30

15
08/07/2021

APPARATUS & REAGENTS

• Conical flask, minimum capacity 500 ml, glass-stoppered.


• Heating Apparatus:
Suitable for maintaining the temperature of the flask
at (50 ± 5) °C.
• Analytical Balance:
with a resolution of 0.0002g 0r better.
• Vacuum flask
• Desiccator: Containing self-indicating silica gel.
• Ventilated Oven for drying specimens at (105 ± 3) °C.
• Soxhlet Extraction:
Sufficient size to give a volume, in ml, equal to 20
times the mass, in gms, of the specimen, or any other
apparatus giving identical results.
Figure: Soxhlet Extraction

ISO 1833 PART 1:2020 31

31

SAMPLING
Extract the air-dry sample in a
Soxhlet with light petroleum for 1 h
at a minimum rate of six cycles/hr.
Take a laboratory test sample, as
described in ISO 5089, that is Allow the light petroleum to
Pretreatment

representative of the laboratory bulk evaporate from the sample. Soak the
Sampling

sample & sufficient to provide all the specimen in cold water for 1 h, and
specimens, each of at least 1 g, that then in water at (65 ± 5) °C for a
are required. Fabrics may contain further 1 h.
yarns of different composition and In both cases, use a liquor/specimen
account should be taken of this fact ratio of 100:1 and agitate the liquor
in the sampling of the fabric. from time to time.
Remove the excess water from the
sample by squeezing, suction, or
centrifuging and then allow the
sample to become air-dry.

ISO 1833 PART 1:2020 32

32

16
08/07/2021

SAMPLING

Dry the specimen for not less than 4 h After cooling, take the dry mass of the
Drying & Cooling

and not more than 16h/14h at (105 ± weighing bottle or crucible and sample

Weighing
3) °C in a weighing bottle with its within 2 min of its removal from the
stopper beside it. After drying, stopper desiccator.
the weighing bottle before removing it Weigh to an accuracy of 0.000 2 g.
from the oven, and
Transfer it quickly to a desiccator until
complete cooling is attained, and in
any case for not less than 2 h

ISO 1833 PART 1:2020 33

33

TESTING EXECUTION

• Take from the pre-treated laboratory test sample a


test specimen weighing about 1 g.
• Cut yarn or dissected cloth into lengths of about 10
mm.
• Dry the specimen in a weighing bottle, cool it in a
desiccator and weigh it.
• Transfer the specimen to the glass vessel specified
in the appropriate part of ISO 1833, reweigh the
weighing bottle immediately, and obtain the dry
mass of the specimen by the difference.
• Complete the test procedure as specified in the
appropriate part of ISO 1833, and examine the
residue microscopically, or otherwise, as
appropriate, to check that the treatment has in fact
completely removed the soluble fibre.

ISO 1833 PART 1:2020 34

34

17
08/07/2021

CALCULATION & EXPRESSION OF RESULT

Calculate the results:


Express the mass of the insoluble component as a percentage of the total mass of fibre in the
mixture.
Calculate the result based on
01. Clean dry mass, or
02. Clean dry mass with agreed percentage additions for moisture, or
03. Clean dry mass with agreed percentage additions for moisture and percentage losses of fibrous
matter removed in the pre-treatment, and
04. Clean dry mass with agreed percentage additions for moisture and non-fibrous matter.
Obtain the percentage of the soluble component by difference. State which of the calculation
procedures has been used and, in cases 2, 3 and 4, state the values of the percentage additions.

ISO 1833 PART 1:2020 35

35

CALCULATION & EXPRESSION OF RESULT

01. Method Based on Clean dry mass:

where
P is the percentage of clean dry insoluble component;
m0 is the dry mass of the specimen;
m1 is the dry mass of the residue;
d is the correction factor of variation in mass of insoluble component in the reagent.
The value of d is 1,00 except for the propylene/polyamide bicomponent for which d is 1,01.

ISO 1833 PART 1:2020 36

36

18
08/07/2021

CALCULATION & EXPRESSION OF RESULT

02. Method based on clean dry mass with percentage additions for moisture:

where
PM is the percentage of clean insoluble component with percentage additions for moisture;
P is the percentage of clean dry insoluble component;
a1 is the percentage addition to the soluble component for moisture;
a2 is the percentage addition to the insoluble component for moisture.

ISO 1833 PART 1:2020 37

37

CALCULATION & EXPRESSION OF RESULT

03. Method based on clean dry mass with percentage additions for moisture and non-fibrous matter,
and/or percentage losses of fibrous matter by pre-treatment

where
PA is the percentage of clean insoluble component with percentage additions for moisture and
nonfibrous matter;
P is the percentage of clean dry insoluble component;
a1 is the percentage addition to the soluble component for moisture;
a2 is the percentage addition to the insoluble component for moisture;
b1 is the percentage loss of soluble fibrous matter caused by the pre-treatment, and/or the percentage
addition to the soluble component for non-fibrous matter;
b2 is the percentage loss of insoluble fibrous matter caused by the pre-treatment, and/or the
percentage addition to the insoluble component for non-fibrous matter.

ISO 1833 PART 1:2020 38

38

19
08/07/2021

COTTON + ELASTANE
ISO 1833 PART 12:2019

39

SCOPE

This part of ISO 1833 specifies method using


dimethylformamide to determine the percentage of
acrylic, modacrylic or elastane after removal of non
fibrous matter, in textiles made binary mixtures of
• Acrylic, certain modacrylics, certain elastanes and
• Animal fibres, cotton, viscose, cupro, modal,
polyamide, polyester or glass fibres.
• It is applicable for animal hair, wool and silk dyed
with pre-metalized dyes, but not to those dyed with
after-chrome dyes.

ISO 1833 PART 12:2019 40

40

20
08/07/2021

PRINCIPLE

• The acrylic, modacrylic, elastane is dissolved out


from a known dry mass of the mixture, with
dimethylformamide at 90°C to 95°C.
• The residue is collected, washed, dried and
weighed its mass
• Expressed as a percentage of the dry mass of the
mixture and the percentage of acrylic,
modacrylic, elastane is found by the difference.

Insert Footer Here ISO 1833 PART 12:2019 41

41

APPARATUS & REAGENTS

Use the reagents & apparatus described in ISO 1833 Part1 together with that given

• Dimethylformamide, boiling point 152°C to 154°C


• Conical flask, minimum capacity 200ml, glass stopperd
• Heating apparatus, suitable to maintaining 90°C to 95°C

ISO 1833 PART 12:2019 42

42

21
08/07/2021

TESTING PROCEDURE
• Follow the general procedure ISO 1833-1
• Take specimen in a conical flask, add 150ml of
dimethylformamide per gm of specimen,
• Shake the flask to wet out the specimen and heat
the flask for 1hr at 90°C to 95°C
• Shake the flask and contents gentle 5 times by hand
• Decant the liquid through a weighed filter cruicible,
retaining the fibres in the flask
• Add a further 60 ml dimethylformamide to the flask
and heat for 30 min at 90°C to 95°C
• Filter the contents through the filter cruicible.
• Wash the residue twice with hot water.
• Take the residue in a flask take 160ml of water and
allow the flask to stand for 5 min, shaking
vigorously.
ISO 1833 PART 12:2019 43

43

TESTING PROCEDURE

• Decant the water through the cruicible and repeat this washing process for 3 times
• After the last wash filter the contents of the flask through the cruicible using
suction
• Transfer any residual fibres to the cruicible by washing out the flask with the water
• Finally, drain the cruicible using suction, dry the cruicible and residue, then cool
and weigh them.

ISO 1833 PART 12:2019 44

44

22
08/07/2021

CALCULATION & EXPRESSION

Calculate the results as described in ISO 1833-1


• The value of the d is 1.00 except the following cases
• Polyamide, Wool, Scoured bleached cotton,
Viscose, Cupro, Modal, Polyester 1.01.

ISO 1833 PART 12:2019 45

45

COTTON + POLYESTER
ISO 1833 PART 11:2017

46

23
08/07/2021

QUANTITATIVE CHEMICAL ANALYSIS


IS0 1833 PART 11-2017

Scope:
This method is to determine the mass percentage of
cellulose fibres, after removal of non-fibrous matter, in
textiles made of mixtures of
• Natural and man-made cellulose fibres, such as
cotton, flax, hemp, ramie, viscose, cupro, modal,
lyocell with
• Certain other fiber like polyester, polypropylene,
elastomultiester, elastolefin and polypropylene
/polyamide bicomponent.
• Using sulfuric acid

47

47

QUANTITATIVE CHEMICAL ANALYSIS


IS0 1833 PART 11-2017

Principle:
The cellulose fibre is dissolved out from a known dry
mass of the mixture, with 75 % (mass fraction) sulfuric
acid. The residue is collected, washed, dried and weighed;
its mass is expressed as a percentage of the dry mass of
the mixture. The proportion of cellulose fibre is found by
the difference.

Insert Footer Here 48

48

24
08/07/2021

QUANTITATIVE CHEMICAL ANALYSIS


IS0 1833 PART 11-2017
APPARATUS & REAGENTS:
Use the reagents & apparatus described in ISO 1833 Part1 together with that
given

• Sulfuric Acid, 75% mass fraction:


While cooling, 700 ml of concentrated sulfuric acid (ρ = 1,84 g/ml at
20 °C) to 350 ml of distilled water. After the solution has cooled to room
temperature, dilute it to 1L with water. The concentration is not critical within
the range 73 % to 77 % (mass fraction) sulfuric acid.
• Ammonia, dilute solution:
Dilute 80 ml of concentrated ammonia solution (ρ = 0,88 g/ml at 20
°C) to 1L with water.

• Conical flask, minimum capacity 500ml, glass stopperd


• Heating apparatus, suitable to maintaining 50°C ± 5°C

49

49

QUANTITATIVE CHEMICAL ANALYSIS


IS0 1833 PART 11-2017
Filter the contents of the flask
through the weighed filter crucible
using suction. Transfer any residual
Pretreated specimen are take into a fibres to the crucible by washing out
Testing Execution

conical flask, add 200:1 sulfuric acid. the flask with a little more sulfuric
Insert the stopper and shake the acid.
Washing

flask carefully to wet out the Drain the crucible using suction, and
specimen. wash the residue on the filter once
Maintain the flask at (50 ± 5) °C for 1 by filling the crucible with a fresh
h, shaking the flask gently at intervals portion of sulfuric acid.
of about 10 min. Wash the residue successively
several times with cold water, twice
with dilute ammonia solution, and
then thoroughly with cold water,
draining the crucible using suction
after each addition.

50

50

25
08/07/2021

QUANTITATIVE CHEMICAL ANALYSIS


IS0 1833 PART 11-2017

Drying, Cooling & Weighing:


Finally, drain the crucible using suction, dry the
crucible and residue, then cool and weigh them.

51

51

QUANTITATIVE CHEMICAL ANALYSIS


IS0 1833 PART 11-2017

Calculate the results as described in ISO 1833-1


• The value of d is 1,00 except for the
propylene/polyamide bicomponent for which d is
1,01.

52

52

26
08/07/2021

COTTON + VISCOSE
ISO 1833 PART 6:2018

53

SCOPE & PRINCIPLE


SCOPE
• This document specifies a method, using a mixture
of formic acid and zinc chloride, to determine the
mass percentage of viscose, certain types of cupro,
modal or lyocell, after removal of nonfibrous
matter, in textiles made of mixtures of — viscose,
certain types of cupro, modal or lyocell, with —
cotton.
PRINCIPLE
• The viscose, cupro, modal or lyocell fibre is
dissolved out from a known dry mass of the
mixture.
• The residue is collected, washed, dried and
weighed; its corrected mass is expressed as a
percentage of the dry mass of the mixture. The
percentage of viscose, cupro, modal or lyocell fibre
is found by difference.
ISO 1833 PART 6:2018 54

54

27
08/07/2021

APPARATUS & REAGENTS


Use the reagents & apparatus described in ISO 1833 Part1 together with that
given
• Formic Acid/Zinc Chloride Solution:
Prepare a solution containing 20 g of anhydrous zinc chloride (minimum assay
to be ≥98 %) and 68 g of anhydrous formic acid, made up to 100 g with water.
If zinc chloride other than fused anhydrous zinc chloride is used, then the fibre
solubility shall be checked.
• Ammonia, dilute solution.
Dilute 20 ml of concentrated ammonia solution (ρ 0,880 g/ml at 20 °C) to 1 l
with water.
• Conical flask, minimum capacity 200 ml, glass-stoppered.
• Heating apparatus:
suitable for maintaining the temperature of the flask at (70 ± 2) °C.

ISO 1833 PART 6:2018 55

55

TESTING PROCEDURE

• Follow the general procedure described in ISO


1833-1, and then proceed as follows.
• Place the specimen without delay in the conical
flask preheated to 70°C. Add 100 ml of formic
acid/zinc chloride reagent per gram of specimen,
preheated to 70°C.
• Stopper the flask and shake it vigorously. Allow the
flask and contents to remain at 70°C for 20 min,
shaking it twice during this time at about 5 min and
15 min

ISO 1833 PART 6:2018 56

56

28
08/07/2021

WASHING & DRYING

• Filter the contents of the flask through the weighed


filter crucible and transfer any fibres into the
crucible by washing the flask with the reagent.
Rinse with a further 20 ml of reagent, preheated to
70 °C.
• Wash the crucible and residue thoroughly with
water at 70 °C.
• Place the crucible containing the residue in 100 ml
of cold ammonia solution in a 250 ml beaker,
ensuring that the residue remains totally immersed
in the solution for about 10 min and carefully
loosening the fibres with a glass rod.
• Rinse thoroughly with cold water. Finally, drain the
crucible using suction, dry the crucible and residue,
and cool and weigh them.

ISO 1833 PART 6:2018 57

57

THANK YOU
58

58

29
08/07/2021

MD. KHAIRUL ALAM MOJUMDER


+880 1670318931

khairul.mojumder@intertek.com

www.intertek.com

59

60

30

You might also like