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Quality Control in Textile Chemical Processing (TTPC 430)

Course contents, course outcomes, syllabus and reference books

Only for Academic purpose during Covid time

Dr. Lalit Jajpura,


Associate Professor, Department of Textiles
Technology,
Contents

 Introduction of subject
 Course outcomes
 Syllabus
 Teaching Plan
 Reference books
TTPC- 430 Quality Control in Textile Chemical Processing [3 00 3]
Course Outcomes
CO1
Exposure on quality control and its importance in TCP
CO2 Recipe and quality control parameters of pretreatment
processing
CO3
Testing of chemicals, auxiliary and fabric quality and
properties
CO4 Printing paste recipe, different methods and style of
printing and their control parameter
CO5
Various finishes and their control parameters
Reviewing various areas of chemical processing of textiles, viz.
pretreatment, dyeing, printing and finishing.

Pretreatment: Optimized process parameters imparted to


textiles in pretreatment and quality of products obtained, viz.
singeing, desizing, scouring, bleaching, mercerization,
Assessment of quality of pretreated product after each stage.
Colouration: Optimized dyeing parameters for dyeing of
natural, manmade and blended textiles with different dyes and
quality of product, Quality printing in various styles and
methods.
Finishing: Optimized finishing parameters to impart various
finishes on different fibres. Process parameters / process
modification / any other changes. Change in quality due to
selection of impure chemicals / faulty fabric / machine handing.
Methods to assess quality of processed product after every
stage of processing and that of final product. Standardization of
instruments / machineries, analysis of colour to check impurity
percentage, evaluation of chemicals to check their efficiencies.
Sr. No. Topic covered Required Topic
Lectures covered
dated
1 Overview of the subject. Flow chart of textile wet processing. Objective of Textile 1
Chemical Processing. Overview of Preparatory wet processing, Dyeing, Printing &
finishing.
2 Pretreatment: 2
Optimized process parameters imparted to textiles in pretreatment and quality of
products obtained,
Perching
Singeing and various control parameters
Sizes, identification of sizes, desizing operation, various control parameters and 2
quality assessment of desized operation
Scouring operation, control parameters, assessment of scouring operation and fabric 2
assessment after scouring operation
Bleaching operation, control parameters, assessment of bleaching operation and fabric 2
assessment after scouring operation
Mercerisation operation, control parameters, assessment of mercerizing operation and 2
fabric assessment after this operation
Heat setting operation, control parameters, assessment of operation and fabric 2
assessment after this operation.
3 Colouration: Optimized dyeing parameters for dyeing of natural, manmade 5
and blended textiles with different dyes and quality of product.

Identification of dyes: Identification of dye on dyed natural and manmade 2


textiles. Various parameters of dyes and their purity
Pretreatment and dyeing machineries: Singeing operation and types of 3
Singeing machine and their applications. type of pretreatment and dyeing
machines. ie batch process and continuous processes, , J-box, kier,
mercerizing machine, loose fibre, yarn and package dyeing machines. Jigger,
winch, jet and HTHP beam dyeing m/cs. padding mangles.
Colour, colour attributes, computer colour matching and its application 3

Colour fastness evaluation 3


Wash, light, perspiration, sublimation, etc
4 Printing: 5
Printing paste ingredients
Quality Control in printing operation and applicable machineries.
5 Finishing:
Optimized finishing parameters to impart various finishes on different fibres.
Mechanical Finishes: 1
Calendering
Sanforizing
Process parameters, process modification, evaluation of finish and finished fabric
parameters
Functional finishes: 5
Anti crease finishe
Water repellent finishes
Soil release finish,
Flame retardant finish: Burning cycle, Limiting Oxygen Index (LOI), various proposals for
application of flame retardants on various textiles.
Softeners
Antistatic finish
Antibacterial finish
Process parameters, process modification, evaluation of finish and finished fabric
parameters
6 Change in quality due to selection of impure chemicals / faulty fabric / machine handing. 4
Methods to assess quality of processed product after every stage of processing and that of
final product.
Total Lectures 44
Scheduled classes
Recommended books

 1. Gokhale S V and Modi J R, “Process and Quality Control in Chemical


Processing of Textiles”, ATIRA, Ahmedabad, 1992.
 2. Doshi S M and Shah H A, “Quality and Process Control”, Chemical
Processing Tablet IX, The Textile Association Education System, Ed. P C Mehta,
The Textile Association (India), 1984.
 3. Karmakar S R, “Chemical Technology in the pretreatment processes of
Textiles”, Textile Science and Technology Series, Vol-12, 1st Edition, Elsevier
(1999).
 4. Peters R H, “Textile Chemistry”, Vol- III, Elsevier Scientific Publishing Co.,
New York, 1975.
 5. Datye K.V and Vaidye A.A, “Chemical Processing of Synthetic Fibres and
Blends”, John Wiley and Sons, New York, 1984.
Recommended books for preliminary pre-treatments and dyeing

 1. V A Shenai, Technology of Bleaching and Mercerising, Vol 2,


Sevak Publication, Mumbai (1991).
 2. Peters R. H, “Textile Chemistry”, Vol - II, Elsevier Publishing
Company, London (1967).
 3. Shore J, “Cellulosics dyeing”, Society of Dyers and Colourists,
Bradford, UK (1979).
 4. Mittal R M and Trivedi S S, “Chemical Processing of polyester /
cellulosic Blends”, Ahmedabad Textile Industries Research
Association, Ahmedabad, India (1983).
 5. Karmakar S R, “Chemical Technology in the pretreatment
processes of Textiles”, Textile Science and Technology Series, Vol-12,
1st Edition, Elsevier (1999).
Blends of Dyeing
 John Shore, Blends Dyeing, Society of Dyers and Colourists, 1998
Pre-Treatment and Dyeing Machines
 Chemical Processing of Textiles: Preparatory Processing and dyeing by NCUTE
Publications
Printing
 Miles L W C, “Textile Printing”, Dyers Company Publication Trust, Bradford,
England, 1981.
 Shenai V A, “Technology of Printing”, Sevak Publications, Mumbai, 1990.
 R S Prayag, Technology of Textile Printing, Jyoti Printers, Dharwad,
Finishing
• Dr Charles Toasino, Chemistry and Technology of Fabric Preparation and Finishing
• Shenai V A, “Technology of Textile Finishing”, Sevak Publications, Mumbai, 1990.
• M. Levin, Handbook of Fiber Science and Technology, Vol. II, Chemical Processing of Fibers and
Fabrics. Functional Finishes, Part B, Levin M and Sello S B (eds), New York, Marcel Dekker,
1984, 1–141.
• W. D. Schindler and P. J Hauser, “Chemical Finishing of Textiles,” Cambridge, Wood Head
Publishing Ltd., Vol. 165, 2004
• A. K. R. Choudhury, In Principles of Textile Finishing, Woodhead Publishing, 2017, 195-244
• Hall A J, “Textile Finishing”, Haywood Books, London, 1996.
• Shenai V A and Saraf, N M, “Technology of Textile Finishing”, Sevak Publications, Mumbai, 1990.
• Nunn D M, “The Dyeing of Synthetic Polymer and Acetate Fibres”, Dyers Company Publication
Trust, London, 1979.
Thank you
Quality Control in Textile Chemical Processing
(TTPC 430)

Quality control in Preparatory wet operations


Only for Academic purpose during Covid time

Dr. Lalit Jajpura,


Associate Professor, Department of Textiles
Technology,
Textile chemical processing

 Inspection
 Pretreatment:
 Colouration: Dyeing & Printing
 Finishing
Preparatory wet processing:
Inspection
Singeing
Desizing
Scouring
Bleaching
Mercertisation
Heat setting
Inspection

 Perching,
 Burling and
 Mending

Perching:
Flaws, stains or spots, yam knots and other imperfections are
marked.

Perches used for inspection of fabric


On-line system cloth inspection by the use of laser beams
 The recent innovation is the cloth inspection by the use of laser beams. Stains, holes, thick and thin places,
and warp or weft thread breaks are detected.

Such apparatus operates on three different principles, namely,


the coaxial, remission and transmission methods.
In the coaxial method the scanner light beam is reflectecd back
to its source (retroreflection) onto a receiver situated in the
optical hand.
In the remission method the emitted light beam is received at a
freely adjustable angle by a light guide system and conducted to
the signal converter.
The transmission method uses a receiver system located below
the path of the fabric which measures the light passing through
the web.

Machine has data input option, a display unit, a recorder, a


counter with acoustic alarm, a marking device, a data store
and/or a printer.
Fabric inspection system followed by garment industries
 4- point system https://textilestudycenter.com/fabric-inspection/
 7- point system
 10- Point system
 2.5- point system etc.

4- point system
General Inspection Procedures
 Fabric inspection is done in suitable and safe environment with enough ventilation and proper lighting.
 Fabric passing through the frame must be between 45-60 degree angles to inspector and must be done on
appropriate Cool White light 2 F96 fluorescent bulbs above viewing area. Back light can be used as and when
needed.
 Fabric speed on inspection machine must not be more than 15 yards per minute.
 Standard approved bulk dye lot standards for all approved lots must be available prior to inspection (if possible)
 Approved standard of bulk dye lot must be available before starting inspection for assessing color, construction,
finish and visual appearance.
 Shade continuity within a roll by checking shade variation between centre and selvage and the beginning,
middle and end of each roll must be evaluated and documented.
 Textiles like knits must be evaluated for weight against standard approved weight.
 Fabric width must be checked from selvage to selvage against standard.
 All defects must be flagged during inspection
 The length of each roll inspected must be compared to length as mentioned on supplier ticketed tag and any
deviation must be documented and reported to mill for additional replacement to avoid shortage.
 If yarn dyed or printed fabrics are being inspected the repeat measurement must be done from beginning, middle
and end of selected rolls.
Acceptable Level:
Many used to say that up to 40 points per 100 square yards is acceptable. In the apparel and
textile industry, textile mills, apparel brands and buyers set their own standards for acceptable
points. A standards level is set by ASTM.
Many mills grade fabrics as first quality and second quality instead of just Pass/Fail the fabric
roll or fabric lot. Again grading is done based number of penalty points per 100 square yards.
Singeing
 In this operation protruding fibres and hairs are burnt from the fabric
surface and improves the end use and wearing properties of the textiles.
 Produce clean fabric surface which allows the dyed fabrics appear brighter
 With no or less pilling especially in synthetics and their blends
 Less soiling
 Provide sharpen printing effect in intricate patterns

Fabric Singeing Yarn Singeing


Singeing advantages

 Singeing improves the end use and wearing properties of textiles.


 The burning-off of protruding fibres results in a clean surface which allows
the structure of the fabric more clear.
 Singeing reduces the fogginess caused by differing reflection of light by
the projecting fibre and the dyed fabrics appear brighter.
 Singeing is an effective means of reducing pilling in blended fabrics
containing synthetic fibres.
 Unsinged fabrics soil more easily than singed fabrics.
 A closely singed fabric is essential for printing fine intricate patterns.
 Singeing process facilitates and speeds up desizing, if the fabric is
impregnated with desizing liquor immediately after singeing.
Plate Singeing machine
Singeing Machines
Direct systems: Singeing of fabrics can be performed by plate,
roller and gas singeing machines.
Roller Singeing machine
Indirect systems: Thermal energy produced by the source is used for burning
the fibres and there is no contact between the heat source and fabric.
Example– Radiation Singeing: Here fire-proof ceramic blocks are heated to
a high temperature, which radiate infrared radiation. This radiation can heat
the fibres to such an extent that they can burn. The advantage of indirect Gas Singeing machine
singeing are: No Flame Contact, hence safer approach
Uniform Singeing, as radiation can be distributed uniformly around a fabric
surface.
Yarn Singeing machine Yarn Singeing
Singeing of yarns is also carried out which is called
“gassing”.
Textile yarns are singed for applications like sewing thread, where the
resistance caused by protruding fibres during high speed sewing
needs to be lowered. The high friction may lead to a lot of frictional
heat generation, leading to damage to fabric and frequent yarn
breakages.
Flame Singeing Machine
 1. Composition of flame -1 part LPG (liquid petroleum gas) -
2 parts Air
 2. Nature of flame -Use oxidizing flame because it produces
minimum amount of ash. -Temperature of the flame is about
1300°C.
 3. Distance of flame from fabric surface should be 1.5 to 4
mm.
 4. Speed of the fabric -Speed of the fabric depends upon
quality of the fabric -Speed of low quality fabric should be
120 meter per minute. -Speed of High quality fabric should
be 60 to 80 meter per minute.
 5. Angle of the flame -Perpendicular to fabric structure (for
heavy weight fabric) -Tangential to fabric structure (for light
weight fabric)

Zones of Gas Singeing Machine There are four zones of singeing Machine
Entrance Zone Brushing Zone Singeing Zone Washing Zone

Dust and gaseous combustion products are exhausted through a ventilation hood arranged above the singeing
machine. Singeing room should be well ventilated, spacious and fire-proof.
Features in modern singeing machine

Modem singeing machines include


 Pneumatic adjustable firing position,
 Ultraviolet flame scanner, built-in flame extraction system,
 Improved guiding system,
 High frequency burners and variable speed and adjustable burners.
 Meter counters, speedometer and a thermocouple with a stationary multi-voltmeter for
measuring the temperature of singed surface.
 Warning noise or fire alarm in the case of a fire.
 May have steam quenching for those sorts of fabric which are not to be wetted, e.g.
 grey mercerized fabrics.
The flame can be applied on the fabric in three different ways:
Tangential singeing
Here the fabric is exposed to the flame tangentially. Only the protruding fibres are burned-off. This
position is especially suitable for the singeing of light weight and heat sensitive fabrics.

Singeing on to a water-cooled roller


In this case the flame strikes the fabric at right angle while it is passing over a water cooled roller. The contact of
fabric with water cooled roller ensures that the temperature of the fabric does not rise alarmingly. The intense
flame quickly converts any moisture in the fabric to steam. This steam and the air in inter-fibre gaps provide a
cushion against the penetration of fabric by flame. It is suitable for synthetic and blended textiles and fabrics
with open structure.

Singeing into the fabric


Here, the flame strikes the free guided fabric at
right angles. Absence of any support means the
flame can penetrate the fabric and burn off fibres
embedded in fabric structure. This configuration
is suitable for cellulosic fibres and other heavy
technical fabrics made from fibre blends
Singeing different kinds of fibres fabrics
Cotton & Other Cellulose fibres
 Cellulosic fibres such as cotton are easily singed because the protruding fibres burn to a light
trace ash which is easily removed.
 In Grey State (Economical) - As one drying step is avoided.
 Slight Yellowing Occurs - Removed on bleaching
 Singed with maximum burner intensity.

Wool
 Poor Combustion properties.
 Heat sensitive and thus flame is not allowed to penetrate the fabric.
 It need delicate singeing or flame is restricted on only fabric surface by blowing the air from
opposite side of the fabric or passing through the fabric on water cooled roller during the
singeing
Thermoplastic fibres
 Thermoplastic fibres are harder to singe because they melt and form hard residues
on the fabric surface.
 Polyester  melt at 280-290 degree C but does not burn till about 500 degree C
 Normal flame forms fused polymer at fabric surface.
 So, powerful flame is used for quick burning or in order to avoid the polyester
starts melting before it gets ignited the energy has to be supplied in a shock form
and the pyrolysis has to be like an explosion, igniting the protruding fibre end
over all its length.

Synthetic fibres and their blends


 Singeing conditions are to be selected depending on the sensitiveness of the kinds
of fibres to heat, blend composition, weight of fabric and fabric geometry.
 i.e. singeing should be carefully conducted to avoid heat damage of the acetate
component of the accetate/viscose blended fibre fabrics.
In general Limitations of Singeing
Generated faults in singeing operation if once occurred then it can no longer be repaired.
 Uneven singeing effect can cause streaks when the fabric is dyed
 Synthetic fabrics and their blends forms small globules due to melting of thermoplastic
synthetic fibres on fabric surface. Thus if singeing is carried out before dyeing then these
small globules absorb more dyes and give speckled effect to the fabric.
 If singeing is carried out to polyester fabric after the dyeing operation then it may sublime
the disperse dye present on fabric.
 It may thermally damage the thermoplastic fibres or may change Tg.
 Stop offs of machine or crease marks produces uneven result which are generally appeared
after dyeing operation.
 Creasing produces streaks which is magnified when dyed.
 This thermal operation may bound certain sizes strongly on fabric surface
 There may be reduction of tear strength due to over singeing of the fabric.
Sizing and Desizing
Sizing
 Thickening agents:
 Starch: amylose and amylopectin- Insoluble
 Soluble starches: may be removed by boiling or hot wash
 PVA: may be removed by hot wash
 Acrylates: may be removed by hot wash
 CMC: soluble in dilute acids
 Glue
 Gelatin
 Vegetable oils:
 Tallow:
 Antibacterial
Sources of Sizing Compounds
Some of the base materials are used either alone or as additives to impart desirable properties
to other bases. When designing the desizing step, it is important to know what base size was
used. Each film-former has its own optimum conditions for effective removal. A knowledge of
the chemistry of the film-formers will make it easier for one to grasp how to best desize
specific fabrics.

Of the bases listed above, starch and polyvinyl alcohol are the polymers most often used when
sizing spun yarns. Synthetic polymers work best on filament yarns. These polymers at times are
blended with starch to improve starch's adhesion to synthetic fibres.
The size, after impregnation into the warp yams at a level of 10-15% (o.w.f.) for cotton and cotton
blends, and at a level of 3-5% on filament synthetics.
Starch

 The structure contains two secondary hydroxyls at the -2,3- positions and a primary hydroxyl at the -6- position.
 The alpha linkage is an acetal formed by the linkage of the hydroxyl at the -1-position with the -4- position of
another. This gives rise to a linear polymer called Amylose. Branching can occur when an acetal linkage
between the -1- position of one ring forms with the -6- position of another. Highly branched polymers are called
Amylopectin.
Starch Solutions
 Natural starches are not very soluble in cold water. Cooking is necessary to get the starch granules to form a
homogenous solution. Typically the starch granules are stirred in cold water and kept suspended by high
speed mixing.
 Gelatinization of starch: As the temperature is raised, water penetrates through the amylopectin membrane
solubilizing amylose. The granules swell as more and more water diffuses in enlarging to many time their
original dimensions. The viscosity of the solution increases as the granules swell, reaching a maximum at the
point where the swollen granules are crowding against each other.

Retrograding of starch solution


The solution will remain fluid as long as it is stirred and kept hot. However if the solution becomes concentrated by
evaporation of water, and/or should the solution cool, an irreversible gel is formed which will not redisperse, no
matter how long it is heated or stirred. Materials that won't redissolve once they have been solubilized are said to
retrograde. In the case of starch, the linear amylose molecules align themselves, and through hydrogen bonding,
form 3-dimensional arrays that are difficult to break apart. This peculiarity in starch is the reason specific processing
conditions are needed to economically remove it during desizing.
Modified Starch
Thin Boiling Starch
 Thin boiling starches are made by adding a small amount of acid to a starch
suspension that is held just below its gel point. The acid cleaves the polymer at
the glucosidic linkage thereby lowering the viscosity of a solution made from it.
Their solutions still retrograde.
Dextrin
 Dextrine are made by heating dry starch with a mineral acid. White dextrin is
made by heating at moderate temperatures and yellow dextrine is made by
heating at higher temperatures with less acid. The degree of hydrolysis is higher
than for thin boiling starch so dextrine solutions have lower viscosities.
British Gum
 British gums are made by dry heating starch granules at 180 0C without acid.
Some of the 1-4 acetal linkages are broken and 1-6 are formed. A more highly
branched, lower molecular weight product is formed having more reducing end
groups. British gums are more water soluble and produce higher solution
viscosities. They are mainly used as print paste thickeners.

Oxidized Starch

Starch granules are oxidized with sodium hypochlorite which


converts the 2-3 hydroxyl into -COOH groups breaking the ring at
that point. Five to seven –COOH groups per 100 anhydroglucose
are introduced.
Some of the synthetic Sizes
Starch sizing of manmade fibres and their blends possess many problems when yarns are slashed and fabrics are
woven. Beside this, starch alone is not suitable on high speed machines thus especial synthetic polymers are
developed for these purpose which are used alone or in mixture.
 The main synthetic sizes comprise of polyvinyl alcohol (PVA), polyacrylic acid, CMC,
 Series of plasticised acidic vinyl acetate and acidic methyl acrylate polymers.
Polyacrylic based sizes
There is a very wide variety of acrylic monomers that can be synthesised by various processes to yield products of different
properties. They are derived from acrylic acid and from acrylic esters. Polyacrylic is a water soluble salt of acrylic acid and
are soluble in mildly acidic or alkaline solutions. It has excellent av,,dhesion to nylon therefore it is used to size filament
for nylon yarns. The affinity is through hydrogen bonding of the -COOH with amide and amine end groups in the nylon
polymer.
Desizing is accomplished by saturating the fabric with a caustic soda
solution which converts -COOH to -COONa making the size water
soluble. Flushing with water completes the removal of the size.
Effect of Heat- Setting on Removal
Like polyvinyl alcohol, acrylic sizes are sensitive to greige heat
setting. The carboxyl groups can split out one mole of water
between two groups on adjacent polymer chains and form an
anhydride. These anhydrides densify the polymer structure, slowing
down the penetration of water and alkali and the size will be
permanently fixed to the fiber. (Anhydride Formation)
Polyvinyl alcohol (PVA)
PVA is the oldest and best known group of synthetic sizes. Polyvinyl alcohol is manufactured by
hydrolysing polyvinyl acetate. Some of the properties of PVA size are:
• Dries to form a tough to hard film of poor flexibility.
• Dried film properties are a function of both molecular weight and the degree of hydrolysis. Super
tough films are formed from high molecular weight, fully hydrolyzed polymers. As a textile size,
the adhesiveness and toughness of the dried film are advantages which have been responsible for
its growing usage, especially on spun yarns. It doesn't retrograde.
• Because of the film properties, less add-on required to produce a good weaving warp.

Removal of PVA based sizing agent


When water soluble PVA is used as sizing agent in weaving, no desizing of synthetic fibre fabrics is
necessary. Light scouring with non-ionic surfactant (3-5 g/l) at 95-100 degree C for 20-30 min is
enough to remove the sizing material. The polymer is inert to most chemical reactions available for use
in desizing. The optimum wash temperature is a function of the grade used to size the warp yarns.
Temperatures near the boil are required for the fully hydrolyzed grades.
Effect of Heat-Setting on Removal of PVA
 Solubility is decreased by heat applied during sizing, grey fabric heat-setting or singeing. A desizing
process using neutral hydrogen peroxide in presence of metal catalysts results in easier removal of
PVA
 Greige heat-setting fabrics with PVA size may insolubilize the size. When PVA films are heated
above 120 0C, water is eliminated from the polymer backbone to form either unsaturation, or to form
ether crosslinks between polymer chains. Once unsaturation starts, the double bond activates the
splitting out of a second mole of water to form a conjugated system. Conjugation is responsible for
the darkening color of the polymer film.

Size Recovery
Since PVA's properties are not altered in desizing, the solids in the spent desizing liquor can be reused as warp
size provided the concentration can be built back up to the level used in sizing warp yarns. This can be
accomplished by passing the spent liquor through a size recovery unit. Ultrafiltration is one technique for
doing this.
Carboxy methyl Cellulose (CMC):
 Carboxymethyl cellulose is made by the reaction of sodium chloroacetate with cellulose. The degree
of substitution can be controlled up to a maximum of 3 carboxymethyl groups per anhydroglucose
unit.
 A. Synthesis

 B. Advantages and Disadvantages over Starch


 CMC is soluble in cold water and does not requiring a cooking step. Solutions remain fluid at room
temperature and don't retrograde. They can be reheated and cooled repeatedly. It is easy to remove
and redissolve CMC size in warm water. CMC like starch supports mildew on storage of fabrics. It is
more expensive than starch.
CMC and water dispensible polyester based size materials are used for sizing of synthetic fibre materials.
They are insoluble in acidic form and soluble in the presence of dilute alkali and can be removed from the
fabric at about 60 degree C. They are, however, precipitated in presence of metal ions in the washing bath
and hence the addition of chelating agent is recommended to nullify its effect. Synthetic detergents of either
anionic or non-ionic type may be used to remove the polyester size from the fabric.
The CMC can be reclaimed, recycled and reapplied from other size material.
 Removal of polyester sizing (consist PVA and CMC)
 The grey fabric is treated with a solution containing non-ionic
surfactant, 2-3 g/l; sodium hydroxide or soda-ash, 1-2 g/1 at 80-95
degree C for 20-30 min.

Desizing of polyester/cotton blended fibre


Acrylic size: removed by simply mild alkaline scour,
PVA and CMC: removed by hot water wash,
Starch and emulsifying wax: Removed by means of enzymatic desizing followed by alkaline scour.
Gelatin and dextrin: Readily soluble in hot water.
Starch with casein protein: amylase and a proteolytic enzyme should be used in the same bath.
Desizing:

Hydrolytic Method:
 Rot steeping
 Acid Steeping
 Enzymatic
Rot steeping
 Immersion of fabric in warm water at approx. 40 degree C  Squeezed the fabric
 store for 24 hours
 Thus microorganism multiply and secrete the various enzymes which may
hydrolyse the starch and other polysaccharides (cotton).
 Time consuming and uncontrolled reaction may take place
 No need of any chemical
Acid Steeping
 Treatment of sized fabric with dilute sulphuric or hydrochloric acid (0.2-1%) at room
temperature or approx. 40 degree C for 2-3 hours.
 Economical, faster than rot steeping but may also hydrolyse the cellulosic material.
 There must be no evaporation of water or drying during storage of the fabric.
Enzymatic operation:
 Amylose needs to be hydrolyse.
 Enzymes are biocatalyst work in optimum pH and Temperature range. Enzymes are complex and have high
molecular weights proteineous molecules.
 Amylase (alpha & Beta) enzymes are specific for amylose hydrolysis thus it does not harm the cellulose
substrate.
Alpha and beta amylases
 Alpha Amylases are capable of hydrolysing starch molecules at random present in the sizing preparation,
transform starch to dextrins, breaking them down to soluble sugars thus helping in eventual desizing.
 Whereas beta amylase attacks straight chains, cleaves the units and produces maltose, so that molecular chain of
starch is shortened gradually.
 Amylase enzyme of appropriate activity:
 Malt extract: 3-20 gpl, 50-60 degree Centigrade at pH 6-7.5; time approx. 1 hr
 Pancreatic: 1-3 gpl, 50-60 degree Centigrade at pH 6.5-7.5; time approx. 1 hr
 Bacterial: 0.5-2 gpl, 60-70 degree Centigrade at pH 5.5-7.5; time approx. 1 hr
 By increasing temperature time duration of the process may be shortened.
 Thermostable enzymes can be used even at 100 degree C and operation can be done in few minutes.
 Over all enzymatic operation is eco-friendly and safer for cellulosic material.
Oxidative desizing: Hydrogen peroxide
The most important aspects of oxidising agents are that they can be applicable Chlorine
to wide range of fabrics, the size content of which is often not known. The Chlorite
main limitations of oxidative desizing agents are increased pollution load, Bromite
fibre damage and inability to recover and re-use water soluble sizes. Alkaline per oxycompounds

 Hydrogen peroxide desizing: 1% at 90 degree C with presence of caustic soda for few minutes
 Bromite Desizing (suitable for P/C blends) containing starch and water soluble sizes
 Sodium bromite: 1-5-2 gpl of available bromite
 Sodium carbonate: 5 gpl
 Wetting agent: 1-2 gpl
 Temperature: Room Temp for 30-40 minutes
 Sodium chlorite: It is found that even it fixes the size material.
 In case of P/C blends or in other synthetic fibres: treatment with sodium carbonate (5 gpl) & wetting
agent/detergent (1-2 pgl) at 70 degree C for 1 hr.
Novel Desizing Technique
Solvent based desizing: May be employed for synthetics and their blends, solvent can be recovered
Plasma treatment: Low temperature plasma
Test for Starch
 A drop of iodine solution placed on a test specimen resulting in a characteristic blue color is the
universal test for identifying starch. It can be used as a qualitatively test to show whether all the
starch was removed. Absence of the blue color signifies that all the starch has been removed. The
intensity of the color is some what related to how much is left. Usually, if the color is faintly
perceptible, the remaining starch will come out in the scouring and bleaching steps that follow.
Desizing efficiency
 Conventional Method
 Tegewa rating
Conventional Method:
In this method we first take the weight of the sized fabric, let it be W1. Then desize the fabric, dry &
take the weight, let it be W2. After that the fabric is treated with 3gpl (35%) HCl at 700 C for 30 min.
dry & take the weight of the fabric. Let it be W3.
Total size = W1-W3.
Residual size = W2-W3.
Desizing Efficiency = (Total size – Residual size)/Total size X 100.
TEGEWA RATING:
TEGEWA association was established in 1951 in Wiesbaden as an association of the manufacturers of
chemicals, the name being an amalgam of these key activities: TExtilhilfsmittel” (textile auxiliaries),
“GErbstoffe” (tanning agents) and “WAschrohstoffe” (detergent raw materials).
Reagent: potassium iodide (10 gm. Of KI (100%) in 100 ml water, add 0.6358 gm of iodine (100%) stir and
shake; iodine is completely dissolved. Fill up to 800 ml with water then complete to 1000 ml with ethanol. (Shelf
life approx 6 months only).
Method:
Spot drop wise solution onto fabric.
2. Rub in gently.
3. Assess change of colour.
Assessment:
Grey fabric:
No change of colour = no starch size present.
Pale blue to bluish = presence of starch size or blend
Violet =of starch size with synthetic size
Desized fabric: Pale blue to bluish violet = refer to violet scale TEGEWA This indicates residual Starch content.

(Karmakar)
Identification of Sizes
Sizes Reagents Procedure Reaction Notes
Starch Iodine/Potassi 1. apply solution dropwise, colourless = no starch size Cool material and
um 2. rub in gently, present, test; neutralise
iodide 3. assess colour reaction. blue violet = starch present alkaline goods with
solution. brown = modified starch or acetic acid.
mixture with PVA present.
Polyvinyl Iodine/Potassi 1. apply iodine/ potassium colourless = no PVA Colour intensity
(PVA) um iodide solution dropwise present, depends on amount
alcohol iodide 2. apply boric acid solution blue = PVA present. of size
solution, boric dropwise to the same spot as
acid soln. the I2 / KI soln.
CMC + copper-II 1. cut up the sample, Clear liquor= no CMC or Add 2-3 drop of
Acrylate sulphate 2. add water at ratio 40:1, Acrylate present, acetic acid 80% to
solution. 3. boil up for 10 min, the liquor,
4. filter off liquor and cool, White turbidity /precipitation = Precipitate
5. add 5 drops solution to the CMC or Acrylate present dissolves= CMC
liquor,
6. assess reaction. Precipitate
undissolved=
Acrylate
Preparation of Test Solutions:
 Solution 1: 2.4 g of potassium iodide and 1.3 g of iodine dissolved in water and diluted to one litre.
 Solution 2: 0.13 g of iodine, 2.6 g of potassium iodide and 4.0 g of boric acid added in that order and diluted to 100 ml.
 Solution 3: 11.88 g of potassium dichromate and 25 ml of concentrated sulphuric acid diluted to 50 ml with water.
 Solution 4: 30 g of sodium hydroxide in 70 ml of water.
 Solution 5: 0.012 M ferric chloride. Steps:
 Solution 6: 0.06 M potassium thiocyanate.
 Solution 7: 0.005 M potassium ferrocyanide. Step 1: Spot fabric with one or two drops of solution 1. Formation of
a deep blue colour indicates the presence of starch or PVA.

Step 2: (Only if you know that starch is not present) Spot fabric with
one or two drops of solution 2. A purple colour indicates the presence
of PVA.

Step 3: Apply on fabric one drop of solution 3 and immediately


neutralise with 3-4 drops of solution 4. Wait for 5 seconds, and then
rub mixture with a glass rod. Formation of a brown spot indicates
presence of PVA.

Step 4: Mix thoroughly 5 drops each of solution 5 and 6. Spot the


fabric with one drop of this mixture and let stand approximately 3
minutes. Rinse in running water for 10 seconds and blot dry. Add one
drop of solution 7 and let stand 1 minute. Rinse in running water 5
seconds and blot dry. A blue or blue-green spot indicates CMC.
Degradation of Cotton during Desizing
Degradation can occur with acid or oxidative desizing if proper care is not taken during the desizing process
Acid desizing
• Insignificant degradation of cotton with dilute sulphuric acid (upto 10 gpl) at R.T.
• Degradation of cellulose can take place if the temperature increases beyond 40 deree C or the concentration
increases beyond 10 gpl
• Fluidity increases from 4 to 5.8 rhes in 4 h
• About 70% of the starch is removed
• The fabric should be washed thoroughly and traces of acid neutralized
• If fabric dries before acid is removed completely, cotton degrades as per the following equations
This results in lowering of DP of cellulose (M. Wt.)
The end –OH groups undergo tautomeric change to CHO
This –CHO (aldehyde) group has reducing power
Scouring
Scouring
 Natural impurities such as Oils, fats, waxes, proteins, pectic substances, remnants of the
added matter, adventitious dirt, motes (seed coat fragments)and other stains are removed in
scouring operation. Objective is to improve absorbability of the fabric.
Phenomenon in Scouring
 Saponification
 Emulsification
Alkali
• Caustic Soda (NaOH): Required for
saponification
• Sodium Carbonate: Required for
saponification
Surfactants
A surfactant may be defined as a substance which, when applied in low concentration, markedly
reduces the surface tension of a solvent. A good surfactant, for example, will reduce the surface tension
of water from 72 dynes/cm to 30 dynes/ cm at a concentration of less than 0.1%. A high quality
synthetic detergent provides a good balance with wetting, cleaning, emulsifying, dispersing and
foaming properties, thus providing it a good cleaning ability.
Chemically, the surfactants are long chain organic compounds containing both a
hydrophobic and a hydrophilic component. Surfactants may be classified into four groups,
viz. anionic, cationic, non-ionic and amphoteric surfactants. However, the non-ionic and
anionic detergents and blends, solvent assisted detergent blends, soaps, etc are mainly used
for scouring.

Builders
Builders are generally salts such as borates, silicates, phosphates, sodium chloride, sodium sulphate
etc. Sodium metasilicate (Na2SiO3. 5H20) also acts as a detergent and buffer and assists other
chemicals to penetrate into the lignin mass of cellulose materials. It increase the concentration of
soap on the fabric and improve efficiency of soap and detergent. Sodium Silicate also help in
Preventing iron stains, Improve whiteness of scoured cotton
Scouring of cotton
(contains approx 0.5% oils and waxes)

 Caustic soda: 1-1.5 % owf


 Sodium Silicate: 1%
 Soap: 1%
 Detergent: 1%
 MLR: 1:5
 pH: 10-11
 Temperature: 100-110 degree C
 Boiling under pressure: 1.5 to 2 kg/cm square for 6-10 hours.
Enzymatic Scouring or Bio-scouring
 Environmental friendly bio scouring using suitable enzymes is gaining more and more acceptance.
Cellulases,, lipases, pectinases and xylanases may be used for effective scouring in eco-friendly
way.
 Lipases are enzymes, which catalyze hydrolysis of triglycerides into diglycerides, monoglycerides
and free fatty acids. Lipases are enzymes with general interest within many industrial applications
such as textiles, food, detergent etc.
 In pectin chains, pectic acid are esterified with methyl alcohol and the free hydroxyl group may be
also acetylated. Pectinases have been found to be most suitable in bio-scouring as they are
capable of removing impurities from raw cotton substrate without adverse changes in the property
of the cotton substrate.
 In scouring, cellulase hydrolyzes cotton removing non-cellulosic impurities effectively but causes
damage to fabric that cannot be completely eliminated. Commercial cellulases currently used in
the textile industry are usually crude mixtures consisting of a multiple enzyme system, which
hydrolyzes cellulose.

 1,4-ß-D-glucan 4-glucanohydrolases (endoglucanases) randomly hydrolyze cellulose chain

 1,4-ß-D-glucan cellobiohydrolases (exocellulase or cellobiohydrolases) split cellobiose from the chain end

 ß-D-glucanohydrolases (cellobiases or ß- glucosidases) split cellobiose to glucose.


Solvent Scouring
Solvent scouring appears to be alternative to aqueous scouring and particularly suitable for polyester and
woollen goods. This process not only permits scouring, but also simultaneous scouring and desizing or even
partial bleaching in one step. Solvent scouring is also useful for the removal of lubricating oils from knitted
polyester, oligomer from polyester and bulking of knitted goods. Wool felts less in solvent media and is
particularly useful in wool milling and application of shrink-resist resins to wool.
Solvents should ideally be inexpensive, readily obtainable, non-toxic, non-flammable, stable to repeated
recovery, inert to textiles and non-corrosive.
 The most suitable solvents for textile processing are the chlorinated hydrocarbons, e.g.
 Tetrachloroethylene (perchloroethylene),
 Trichloroethylene
 and 1,1,1- Trichloroethane.
 The main difficulties of solvent scouring are the need for systems to recover the solvent from
fabrics after processing. Apart from this, solvent can remove binders from bowl fillings and
adhesives from laminated bowl covers and rapidly attacks conventional rubber coverings with
expensive effect.
 One important factor for solvent processing is the stability of solvents to recovery by
distillation or by adsorption process. The recovery of stabiliser in the solvents is also equally
important.
 Substituted diamines is work as stabiliser for Trichloroethylene
 Mixtures of acetonitrile and nitromethane is work as stabiliser for 1, 1, 1 - trichloroethane
 Soil removal in chlorinated hydrocarbons can be improved by the addition of solvent
detergents, e.g. monoethanolamine, alkylbenzene sulphonate, alkyl poly (glycol ether), alkyl
pyridine chloride, etc.
Emulsion Scouring
 Lubricants are applied extensively on weft knitted cotton fabrics.
 Spin finish, coning oils contains lubricants, mineral oils, fatty glycerides, silicones, etc.
 The presence of oil on the surface of the fibre reduces the scattering of incident light; impair
level dyeing properties and the fastness to washing and rubbing; and modify the structure of
polyester fibres on storage and thermal treatment. A proper selection of lubricants is
necessary so that scouring must be thorough.
 Non-scourable oils are difficult to remove from cotton giving rise to unlevel dyeings. The oil,
grease and tar stains are generally removed by spotting on stained portion with stain remover
comprising emulsified solvents in the liquid form.
 Lubricants constituents in different fabrics:
 They organic solvents containing emulsifier dissolved in them and hence become self-
emulsifiable. The solvent must be capable of dissolving the hydrocarbon impurity and the
detergent must be capable of emulsifying both the hydrocarbon and the solvent. Solvents
blended with surfactants are claimed to have superior environmental behaviour along with
excellent grease removal.

Emulsion Scouring Recipe


Scouring of synthetic fibres and their blended textiles

 Synthetic fibres generally contain negligible naturally occurring impurities in


comparison to natural fibres.
 Presence of added impurities are:
 Spin finishes,
 Processing and coning oils and
 Antistatic agents
 Sighting colours which is being added to to distinguish one kind of fibre from the other fibres
 Adhered dirt
 Object of scouring: Removal of aforesaid impurities and relaxation in the case of
texturised and knitted fabrics
Scouring of polyester
 Some types of polyester yarns may be simply rinsed with water or even be dyed directly without
scouring.
 Flat polyester filament fabrics are commonly scoured to remove sizes and lubricants, after spotting
(if necessary) to assist the removal of loom stains by following recipe:
 The preferable condition for scouring of polyester
 Alkaline reagents (caustic soda, soda-ash, ammonium hydroxide): approx. 1-2 g/1
 Time: 30-60 min
 Temperature: 75-80 degree C
 Alternatively, scouring can be carried out with anion active detergents in an amount 1-2 g/1 at 80-
95 degree C for 20-30 min. Reduction in weight of polyester on treatment with caustic soda at
100 degree C
Scouring of nylon
 Synthetic detergents along with mild alkali are generally suitable for scouring nylons.
Generally, non-ionic detergents are used in scouring of nylons as the anionic preparations
are absorbed by the same sites of the fibre similar to that of anionic dyes and
consequently reduce the exhaustion of the dyebath.
 Soda-ash: 1-3 gpl
 Non-ionic detergent: 2-3 gpl
 Temperature: 70-90 degree C
 Time: 10-30 min

For unset fabric the preferable temperature range is 70-80 degree C as in higher temperature rope
marks may form and for the set fabric it is 95-100 degree C

An acidic wash-off is necessary when cationic finish is to be removed from the fabric.
Scouring of poly acrylonitrile fibres
 Fabric dyed in dark shade may not require any Scouring operation
 Although yams which are to be dyed in pale and medium shades need scouring to avoid patches due to
presence of impurities like lubricant oils.
 Relaxation treatment
 In generally, high bulk acrylic yams on cones are relaxed in saturated steam at about 100 degree C for 20 min
or in hot water before scouring.
 Scouring:
 Scouring is carried out in a solution containing 1-2 g/1 non-ionic detergent and 1 g/1 trisodium phosphate
(Very weak alkali) at boil for 30 rain.
 If removal of oil and grease from the fibre is difficult then 1 ml/1 solvent-based detergent may be added in the
bath.

Alkali or soaps may discolourised


the acrylic fabric.
Scouring of acetate fibres

• Diacetate can be saponified under certain conditions of alkaline scouring and therefore careful
control is necessary to avoid surface modification. Thus, The scouring can be carried out in a
solution containing 3 g/1 soap and 1 g/1 of a 25% solution of ammonia (very weak alkali) for 30-35
rain at 70 degree C.
• Triacetate is not delustered by boiling or soap solutions thus slightly higher scouring temperature
may be given to triacetate.
Scouring of regenerated cellulose
Regenerated cellulose have very less inherent impurities. Rayon can be cleaned by treatment at a
temperature of 80-90 degree C with soap solution (0.3 - 0.5%) to which mild alkali like soda-ash
or trisodium phosphate may be added.

Scouring of texturized fabric (Relaxation and scouring)


The textured woven and knitted goods possess latent heat of torque which is already set during texturising
process. The warp yam is applied with a large amount of sizing and oiling agent and thus the grey fabric loses
its crimp by mechanical tension, becoming in a flat state. Therefore, it is necessary to restore the crimp of the
yarn by relaxing treatment in water under tensionless condition. Relaxing can be carried out by water, steam
and dry heat. The textured fabrics are relaxed in water at 80-95 degree C in the absence of tension for 20-30
min. For high twist yarn and fabric a longer time is required. A gradual elevation of temperature is more
favourable to relaxation. Further scouring may be carried out.
In most cases scouring is carried out in conjunction with the relaxing process on a tensionless machine. In
paddle scouring, circular knitted nylon fabrics or garments are loosely packed into polyester mesh bags and
scoured/relaxed in overhead or side-paddle machines using 1 g/1 non-ionic or anionic detergent, 0.5 g/1
sodium hexametaphosphate and 1 g/1 solvent scouring agent at 60 degree C for 30 min. The liquor is
cooled, fabric in rinsed, hydroextracted and dried without tension at 60-80 degree C.
Scouring of polyester/cotton blends

 Scouring is mainly designed to remove the natural oils and waxes from the cotton portion and the
finish oils which manufacturer add to polyester fibres when extruded.

Fabrics containing polyester fibre should not be kier-boiled. In such blends, milder conditions of
alkalinity and temperature are used to avoid detrimental effects on the polyester portion.
Scouring of polyester/wool blends
 Worsted polyester/ wool blend yams may contain 2.5 - 3% solvent extractable oil,
compared with 3.5 - 5% for similar all wool yams. The oils have much greater
affinity for polyester fibre than wool and after normal piece scouring, the blends
contain residual oil content of 0 . 6 - 1.2% compared with 0.3% for wool. The
object of scouring polyester/wool blended fabric is not only to remove spin
finishes, lubricating oils, sizes and contamination of all types, it also helps in fabric
relaxation and parting the necessary compactness.

 Scouring can be carried out either in rope form in Dolly washing machine for wool
rich blends or open width form for polyester rich blends. The spin finishes are
removed by 0.5-1% non-ionic alkyl phenol polyglycol ether type of detergent and
0.25-0.5 ml/l NH3 (25%) or 0.2-0.4 g/1 soda-ash at pH 8 to 9 for 20-30 min at 40-
50 degree C Synthetic detergent solution at pH 5 to 6 can be used to minimise
degradation.
Scouring of polyester/acrylic blends
Scouring of polyester/acrylic fibre blended fabrics can be carried out in either a weakly acid or
alkaline bath using a combination of 0.5-1 g/1 non-ionic and anionic detergents. The pH of the bath
is adjusted to 5-6 with acetic acid or 8-7 with ammonia or soda-ash and the treatment is done for
20-30 rain at 60~ (for acidic pH) and 40-50 degree C(for alkaline pH).

Scouring of acrylic/wool blends


Acrylic/wool blended fibre fabrics may be prepared according to established practice for wool, except that
precautions are taken to allow for the thermoplastic properties for the acrylic fibres. Relaxation is done to
remove the inherent strain. Worsted fabrics are crabbed and then scoured in either a Dolly at temperature not
exceeding 40 degree C or in winch.

Blend yams containing unrelaxed high bulk acrylic fibre should be completely relaxed before being dyed,
either by steaming in an autoclave at 107 degree C for 10 min after preliminary evacution of the steamer, or
by immersion in boiling water for 5 min.

For worsted yams, scouring can be conducted at a maximum temperature of 60 degree C for 30 min with 1
g/1 non-ionic detergent and 0.5 ml/1 acetic acid (80%). Woollen spun yams lubricated with oleine are
scoured at 30~ with soap or synthetic detergent and sodium carbonate.
Scouring of acetate/wool blends
Diacetate and triacetate are both used in blends with wool. Scouring and milling can be conducted with
the minimum quantity of alkali at temperatures not exceeding 50 degree C and care should be taken to
avoid excessive mechanical friction on the fabric. Fabrics made from triacetate/wool blends should be
given a crabbing treatment before dyeing.
Scouring of blends containing viscose
Scouring treatments that are suitable for
specific blends containing viscose
fibres are given in table but in practice
the precise conditions vary also with
the procedure and machineries used.
Degradation of Cotton during Scouring

 It induces fibre degradation under severe conditions by creating crevices in fibre or


dissolution of cuticle or primary wall. The main changes in cotton during scouring process
are loss in weight (about 5-10%), loss in length due to shrinkage and alteration in count
affected by both losses and changes in tensile strength (generally an increase). Since the
scouring treatment contributes to the dissolution of a portion of shorter cellulosic chains, it
bestows on cotton an average DP higher than that of native cellulose.
 The alkali treatment of scouring condition does not induce pronounced changes in the fine
structure of fibres and has a small effect on the degree of crystallinity.
 The degradation of cellulose in alkali solution depends on the concentration of alkali and on
the presence or absence of oxygen. In the absence of air cellulose is slowly attacked by hot
alkali in a stepwise fashion at the reducing end of the cellulose chain resulting in a loss of
material. The entrapped air should be sweeped out before kier boiling under pressure.
 The reaction scheme of this kind of degradation is represented in Fig. by the
formation of peeling-off centres on the cellulose i.e. aldehyde groups, by p-
alkoxy elimination reaction from the reducing ends of the chains, by the formation
ofcarbonyl groups containing coloured products and yellowing.
The reaction of oxygen with cellulose in presence of strong alkali
(above 40 g/l)
Determination of the Efficiency of Scouring
 On scouring cotton, following changes take place:
 Loss in weight (5-10%)
 Significant increase in absorbency (1-3 seconds)
 Further improvement is TEGEWA rating
 Slight increase in average DP (due to removal of low mol. wt. components)
 Shrinkage
Assessment of scouring efficiency
 Practical tests of absorbency
 Measurements of
 Weight loss
 Protein content
 Residual wax content
 Methylene blue absorption (removal of pectic substances)
https://nptel.ac.in/courses/116/102/116102016/
Practical tests of absorbency
Sinking time test (AATCC Test Method 17-1994).
 The scoured yarn is converted to a hank (18 in periphery, 5 g wt). The hank is
connected with the help of a hook (3 g) to a sinker which is a flat cylindrical
plate (25 mm diameter, 15-40 g wt). The assembly is put on 500 ml water in a
glass measuring cylinder. Initially the air entrapped in the hank causes the hank
to float but as wetting starts and the air is replaced with water, the hank starts to
sink due to attached sinker. The time required by the hank to go inside water
from floating state is known as sinking time.
 Method is also used in evaluation of wetting agents.
Drop test
 The fabric is placed flat on a table and creases are removed. A burette is placed at a certain
height from the fabric surface. Distilled water drops are allowed to fall on the fabric. The
time required for the drops to be absorbed completely is noted as wetting time. (Absorbency
of Bleached Textiles, AATCC Test Method 79-2000)
Measurements of Weight loss
 The weight of dried cotton sample before and after scouring may be used as an
indicator of scouring efficiency. This difference when expressed in % (% wt loss)
should be in the range 6-9%.
Measurements of Protein content
 The protein content is determined indirectly by analysing nitrogen content after
scouring.
Measurement of residual wax content
 A dry cotton sample is refluxed for 3 h in chloroform in the Soxhlet extractor and
(solvent). After extraction the sample is reweight and the wt. loss is determined which
is indicative of removal of fat and wax. For well scoured cotton, it should be approx.
0.2%.
 Methylene blue absorption (removal of pectic substances)
Bleaching
Classification of bleaching agent

• Calcium Hypochlorite [Ca(OC1)2.4H20 ]


• Sodium Hypochlorite [NaOC1]
• Hydrogen Peroxide
• Sodium Chlorite
Sodium Hypochlorite [NaOC1]
 Hydrolysis: NaOCl + H2O NaOH +HOCl
 Bleaching agent release: HOCl  HCl + [O]
 Max HOCl development: NaOCl + HCl  NaCl + HOCl
 Formation of free Chlorine: HOCl + HCl H2O + Cl2

Cotton bleaching with hypochlorite solution (Chemicking)


NaOCl: 1-3 g available chlorine per litre at
pH: 9.5 to 11.
Temp: Room temperature
Time: 3-5 hrs

The pH is maintained by adding 5 g/1 sodium carbonate in the bleach bath. After bleaching the cloth is
treated with dilute hydrochloric acid to neutralise any alkali (souring) present in the cloth. An antichlor
treatment with sodium thiosulphate or bisulphite is also recommended to remove any residual
chlorine from the cloth.
Hypochlorite solutions if buffered to pH 11, the rate of bleaching is increased by a factor of 2.3 times
for every 10 degree C rise in temperature. It is thus, possible to bleach at 60 degree C in 7 min, but is
difficult to control the degradation of cotton in such short period of bleaching.
Analysis of bleaching powder
We may define available chlorine to be the grams of chlorine liberated from 100 g of the bleaching
powder on treatment with dilute acid.
It is based on iodometric titration, is a volumetric chemical analysis or a redox titration where the
appearance or disappearance of elementary iodine indicates the end point.
5 g sample is made up to 500 ml in a volumetric flask. 50 ml of this solution is pipetted out to a 250
ml conical flask and 25 ml of distilled water is added followed by 20 ml of KI solution (10%) and 10
ml of glacial acetic acid.
Ca (OC1)2 + 4KI + 4CH3COOH  CaC12 + 4CH3COOK + 2I2 + 2H20
The liberated iodine is titrated against N/10 sodium thiosulphate (Na2S203) solution using starch
solution as indicator towards the end point when the blue colour will be discharged.
2I2 + 4Na2S203  2Na2S4O6 + 4NaI

B.R.= Sample- Blank

N/10 sodium thiosulphate have to be standardized by


with potassium iodate, KIO3 (primary standard) or Potassium dichromate.
Hydrogen Peroxide
 Pure hydrogen peroxide is fairly stable in presence of sulphuric acid and phosphoric acid if stored away
from sunlight in a perfectly smooth bottle. In alkaline medium it is less stable and even traces of alkali
(NaOH, Na2CO3) decompose aqueous solution of hydrogen peroxide. The addition of alcohol, glycerine or
berbituric acid also stabilise hydrogen peroxide. Hydrogen peroxide also decomposes in the presence of
finely divided heavy metals such as copper, iron, manganese, nickel, chromium etc. or their oxides with
liberation of oxygen.
 H2O2  H2O + (O) + X kcal (Autolysis)
 H2O2 H+ + HO2 – (perhydroxyl ion) (Dissolved in aqueous media)
 HO2 –  OH – + (O) Nascent oxygen (Bleaching action)
 NaHO2 Na+ + HO2 – (perhydroxyl ion) (Activated Bleaching actionin alkali)
 H2O2  H2O + O2 (Decomposition)

If the rate of decomposition is very high, the unutilised HO2- may damage the fibre. A safe and
optimum pH for cotton bleaching lies between 10.5 to 10.8 where the rate of evolution of
perhydroxyl ion is equal to the rate of consumption (for bleaching). At higher pH, hydrogen
peroxide is not stable and hence a stabiliser is frequently added in the bleaching bath.
Analysis of hydrogen peroxide
10 ml of sample solution is diluted to 1000 ml with distilled water. 10
ml of this solution is pipetted out into a conical flask and 10 ml of 10%
H2SO4 is added to it.
This solution is then titrated against 0.1 N KMnO4 till pink colour of
permanganate solution persist.
5H2O2 + 2KMnO4 + 3H2SO4  K2SO4 + 2MnSO4 + 8H2O + 5O2
1 ml of 0.1N KMnO4 = 0.0017 g H202
Relation between Volume strength and percentage H2O2

 2H202  H202 + 2 02
 Molecular Concentration 2*34  1 mol of oxygen
  22.4 litre at NTP
 2*34 gm per litre  22.4 litre oxygen
 68 gm per litre or 6.8 %  22.4 litre oxygen
 1 litre oxygen will be obtained from 6.8/22.4 % hydrogen peroxide
solution
 100 litre or 100 volume = 6.8*100/22.4 approx. 30%
 130 volume = 39%
 160 volume = 48%
Stabilisers
 The control of perhydroxyl ion to prevent rapid decomposition of bleach and to
minimise fibre degradation is described as stabilization.
They could include any of the following"
 Alkali, e.g. caustic soda/carbonate/silicate.
 Dispersant, e.g. acrylates/phosphonates.
 Sequestrants, e.g. EDTA/TPA/heptonates/gluconates.
 Inorganics, e.g. magnesium salts.
 Colloid stabilisers, e.g. acrylic polymers

Sodium silicate is the most conventional, easily available and widely used stabiliser. Sodium silicate is
mildly alkaline in nature and the commercial grade consists ofpolysilic acid and having a Na20 : SiO2
ratio 1 : 3.3.

Sodium silicate, however, has a greater stabilising action in the presence of calcium and magnesium
salts so that water with hardness between 2 degree and 5 degree is recommended or, if water of zero
hardness be used, 0.06 g/1 magnesium sulphate may be added.
Suitable sequestering agents from following may also added in bleaching bath
 Polyphosphonates,
 Polyhydroxy-carboxylic acids,
 Aminopolycarboxylic acids,
 Polyacrylic acids
Organic stabilisers such as amino polycarboxylate, protein degradation products and selected
surfactant

General recipe for cotton bleaching:


Hydrogen peroxide: 2-8% (owf)
Sodium silicate (Stabilizer): 3%
NaOH: 0.8-6%
Soda Ash: 3%
pH: 10.3-12
Temperature: 90-100 degree C ( upto 120 degree C in case of pressurised bleaching)
Time: 4-6 hours
Bleaching of Synthetic Fibres with Hydrogen Peroxide

 Viscose:
 It can be Bleached with similar chemical agents required to bleach linen and cotton fabrics. For very
good whiteness, rayon may be bleached on a jigger with alkaline hypochlorite or combined scour
and bleach using hydrogen peroxide (up to 1 vol. strength) containing sodium silicate and alkaline
detergents-at a temperature of about 70 degree C.
 Bleaching of acetate fibres
 The whiteness of the fabric made of acetate may be improved by treatment with hydrogen peroxide
(30%), 1-3 g/1 in presence of sodium silicate, 0.3 g/1. During this treatment the alkalinity of the
bath and the required temperature should be carefully maintained. The pH of the bleach bath should
not be greater than 9 and treatment for 1 h at 45 degree C gives combined scour and bleaching with
the addition of non-ionic detergent.
 Bleaching of acrylic fibres
 Certain acrylic fibres should not be chlorite bleached because of their tendency to yellow/or
loose stability to light. Such fibres can be bleached with hydrogen peroxide or hydrosulphites.
Bleaching with Sodium Chlorite (textone)
 Sodium chlorite (NaC1O2) in its white crystalline form is highly hygroscopic in nature. Solid sodium
chlorite is stable at room temperature for a longer time when it is mixed with small quantity of alkali
(Soda ash).
 Sodium chlorite on decomposition produces a strong oxidising gas known as chlorine dioxide. The
lower the pH values and higher the temperature (above 70 degree C of bleach bath, the greater is the
speed of decomposition.

 Chlorous acid (HC1O2) that is formed is unstable and decomposes to chlorine dioxide (C1O2) which is
the acitve species so far as bleaching is concerned. Maximum chlorine dioxide is formed between pH
2.5 and 3.0. Recipe:
Sodium chlorite: 1-2%
pH: approx. 4.0 (acetic or formic acid)
Wetting agent: 2 gpl
Sodium Nitrate: 1-2 gpl (corrosion inhibitor)
Temp: 85-90 degree C
Time: 1-3 hours
Analysis of sodium chlorite
2 g sample is made up to 500 ml in a volumetric flask. 25 ml of solution is pipetted
out and then 25 ml of 10% KI solution and of 10% H2SO 4 are added. The content is
titrated against 0.1N Na2S203 solution using starch as an indicator till blue colour
disappears completely.

 2NaC1O2 + 8KI + H2SO4  2NaC1 + K2SO4 + 8I + H2O


 1 ml of 0.1N Na2S2O3 = 0.00226 g NaC1O2
Bleaching of polyester with sodium chlorite
 The polyester is generally bleached with sodium chlorite in a bath containing:
Sodium chlorite (50%): 3-5 g/l,
Formic acid to get pH: 3.0
Time: 1-2 h
Temperature: 95 degree C

A small quantity of wetting agent can be added in the bleaching bath. Bleaching is followed by anti-chlorination
with thiosulphate (2-3 g/l) at 60 degree C for 20 min. Finally, warm and cold rinses are given for 10 minutes.

Bleaching of nylon with sodium chlorite


Bleaching of nylon is normally carried out where the nylon has been discoloured by heat-setting treatment.
Neither sodium hypochlorite nor hydrogen peroxide is recommended for bleaching of nylon. When
hypochlorite is used, there is a tendency for chlorine to combine with secondary amino groups, causing
decrease in tensile strength.
Nylon can be bleached in a bath containing sodium chlorite (80%), 1-2 g/l, sodium nitrate, 1-3 g/l, formic acid
(85%), 2 ml/1 for 1 h at 80-85 degree C. Acetic acid is preferred to formic acid for adjusting the pH (3.5 to 4)
because it has a buffering action on sodium chlorite solution in the required region.
Merits and demerits of chlorite bleaching
 Sodium chlorite is a versatile bleaching agent. It can be used for cotton and synthetic fibres and their
mixtures. Man-made fibres which are sensitive to alkali can be safely bleached with sodium chlorite.
 Sodium chlorite bleaching will give permanent white coupled with excellent mote removal on cotton which
has not been kier boiled. There is little or no tendency to degrade cellulose.
 Sodium chlorite is ideally suitable for bleaching of cotton/polyester blended fabrics since both fibre
components respond to acidic chlorite bleaching. However, hydrogen peroxide is also found equally
satisfactory for this fibre blend.
 Under the acid conditions of chlorite bleaching, hardness of water has little harmful effect. Sodium
chlorite is rather insensitive to the presence of metal ions as iron with peroxide.
 Drawbacks as follows
 Sodium chlorite is more expensive than hydrogen peroxide.
 It is not useful for the bleaching of silk and wool, since it gives pink colouration which, however, can
be removed with treatment of soidum bisulphite solution.
 Even at pH 4-5 certain amount of chlorine dioxide is evolved, and the bleaching action is extremely
corrosive to metals including stainless steel.
 Neutral and alkaline pH may tender the cotton.
 Chlorine dioxide is a very toxic gas because it can decompose into both hydrochloric acid and chlorine
gases.
 Physical testing
 Tensile strength, bursting strength and abrasion resistance, Tear strength can be
measured
 The results are influenced by both fabric structure and chemical damage.
 Tear strength is also influenced by residual natural lubricants.

 Staining tests
 Carboxyl groups in oxidized cellulose resist staining with C.I. Direct Blue 1 or give
increased uptake of C.I. Basic Blue 9.

 Harrison test
 The oxycellulose test sample is immersed in a boiling alkaline silver nitrate solution.
 Brown to black deposits of silver are produced on the substrate where there are reducing
aldehyde groups.
 Assessment of the degradation can be done by either assessing the
aldehyde/carboxylic group content of cellulose, measurement of fluidity or
loss in tensile strength.
Following are some of the methods for assessment of cotton cellulose
degradation:
 1. Copper number, a measure of the reducing groups present in cellulose.
 2. Carboxyl group content by methylene blue absorption
 3. Cuprammonium fluidity, which is a measure of molecular chain length of
cellulose.
 4. Tensile strength of the cotton material before and after scouring.
Copper number  The first stage of cellulose oxidation during cotton souring results in formation of –CHO groups
from –OH groups. These aldehyde groups have a reducing tendency and can reduce alkaline
solution of copper sulphate, resulting in formation of insoluble cuprous oxide which
precipitates on the cotton cellulose. The amount of cuprous oxide formed is proportional to the
amount of reducing groups which is expressed as Copper Number.

A solution is prepared by dissolving 100g copper sulphate in 1 litre of water. Another solution is prepared by
dissolving 350 g sodium carbonate and 50 g sodium bi carbonate in another 1 litre of water. These two solutions are
mixed just before use to form Fehling’s solution.
Three groups of cotton cellulose is boiled in a solution containing 100 ml of Fehling’s solution and 200 ml of water
under reflux for 15 min. during the boiling process some copper sulphate is reduced to cuprous oxide which gets
deposited on cellulose.
This mass of cellulose is filtered & washed with water. The cellulose is then transferred to a beaker containing 1-2
gm fabric alum dissolved in dilute sulphuric acid. The cuprous oxide present in cellulose reduces ferric sulphate
and forms equivalent amount of ferrous sulphate. This is titrated against N/100 ceric sulphate solution by
dissolving the ferrous sulphate in sulphuric acid. Ortho ferrous phenathroline (ferroin) is used as an indicator.

Thus copper number is defined as grams of cupric copper reduced to cuprous oxide by 100 g of cellulose under
standard treatment conditions.

Cu + + Fe 3+  Cu 2+ + Fe 2+
 The copper number is thus the weight of copper from Cu 2+ to Cu + state by 100 g dry
cellulose and is a measure of its inter and intra chain break down.
Four solutions are prepared as follows :
 Solution A : 100 g pure CuSO4 dissolved in 1 litre H2O.
 Solution B 95 0 g NaHCO3 and 350 g Na2CO3 dissolved in 1 litre H2O.
 Solution C : 100 g ferric alum and 140 ml pure concentrated H2SO4 dissolved in 1 litre
H2O.
 Solution D : N/100 cerric sulphate.

The copper number is determined by the following formula:


Where V = ml of ceric solution - blank reading
N is the normality of ceric sulphate solution
W is the weight of the bone dry cellulose sample (it depends on type of sample; for normal samples it is
0.25 g and for highly degraded samples 0.1 g is taken

Copper number for pure cellulose is 0.2-0.3 & for viscose less than 1.2.
Copper number of Fully Degraded cotton may be as high as 14
Methylene blue absorption method
 Normal cellulose generally has no affinity for methylene blue, a basic dye. When cellulose in
oxidized, -OH groups convert to aldehyde group. But when the oxidation is more severe, these
aldehyde groups can oxidize to carboxylic groups. In degraded cellulose, both –CHO & -COOH
groups may be present. Hence there is a need to determine the degree of cellulose oxidation in
terms of –COOH groups content.
 Methylene blue absorption method is based on the principle that the carboxyl groups present in
cellulose are able to absorb methylene blue dye cations quantitatively from a solution of
methylene blue dye. The scheme is shown below:

The amount of dye absorbed can be


determined by analyzing the drop in
concentration of methylene blue in treatment
solution using calorimetric methods.

Scoured and bleached American cotton have


carboxyl contents of 0.8-0.9;
Egyptian cotton: 1.16-1.74.
Cuprammonium fluidity
 Fluidity is the inverse of viscosity of cellulose solution and is measured as rhes (poise-1).
 The degradation of a polymer results in reduction of degree of polymerization. At same concentration,
the degree of polymerization is related to the viscosity of its solution. Fluidity (ease of flow) is a
property inversely related to viscosity (resistance to flow). Thus the degradation resulting in reduction
of the DP can also be assessed by measuring fluidity.
 In this test, the conditioned cotton sample required to make 0.5% solution is exactly weighed and
dissolve in cuprammonium hydroxide solution. The flow time of this solution between two fixed marks
on a calibrated viscometer (fluidity tube) is measured at specific temperature. The fluidity value "F" is
then calculated from the flow time "t" and the viscometer constant "C" by using the fomula F=C/t.
 In the table given below, fluidity values of various forms of cellulosic textiles are given.
Type of cellulose Fluidity values
Unbleached cotton ~2
Bleached cotton <5
Degraded cotton showing
>10
loss in tensile strength

standard unbleached viscose ~10


Silver nitrate test

This qualitative test is also referred to as Harrison's test since he was the first
to describe it in 1912.
The test specimen is either boiled or padded with a reagent containing a mixture
of silver nitrate (1%), sodium thiosulphate (4%) and sodium hydroxide (4%)
and then steamed.
Those parts where degradation takes place due to oxycellulose or hydrocellulose
in a fabric will be stained black or dark grey due to the formation of silver by
reduction.
Whiteness

 White is colour of purity, freshness and cleanliness.


 In physical terms, a white surface is one which reflects strongly (>50%) throughout
the visible spectrum.
 Geometrically, a white surface reflect diffusively in all direction.
 Mirror: reflect strongly in one direction.

Improvement in whiteness
 By removing blue absorbing yellowing contaminants in bleaching
 Blueing to give additional whitening by applying blue or violet dye ie ultramarine
blue (CI pigment blue 29/770077). Water soluble dyes such as blue or violet acid
dyes.
 By applying the fluorescent brightening agents (FBAs)
 FBA absorb light in the invisible UV region (300-400nm) and remit violet to blue
fluorescent light.
Reflectance curves of cotton cloth at various stages of processing
Instrumental assessment of whiteness
 Reflectance or emission at particular or a range of wavelength
W=R (Reflectance value)
SCAN (Scandinavia) and TAPPI (USA, known as paper brightness) is
recommend to measure whiteness at 457 nm. Where 457 nm special filter is
not available then the reflectance at 460 nm may be considered as
whiteness.
Whiteness
 Unbleached cotton: about 55%
 Acceptable Bleached fabric for subsequent dyeing: 78-82%
 Fully bleached: 83-85%
Harisson and Stephansen whiteness
 These calculations are based on measuring the reflectance at two wavelength- one at the short
wavelength for blueness and another at long wavelength for redness.

Hunter and Stensby whiteness

CIE whiteness Index


Whiteness of samples evaluated for CIE standard Illuminant D65. In the formula, xn, yn are the chromaticity
coordinates of the perfect reflecting diffuser, for which the value of the index will be 100. in case of FBA treated
sample value will be greater than 100.

Taube, Berger, Ganz whiteness indexes


Concentration or purity of
chemical based on specific gravity
Twaddell scale

Hydrometer
 A hydrometer is an instrument used for measuring the relative density of liquids based
on the concept of buoyancy . They are typically calibrated and graduated with one or
more scales such as specific gravity.
Twaddell scale
 The Twaddell scale is a hydrometer scale for reporting the measured specific
gravity of a liquid relative to water. The scale is named after the scientific instrument
manufacturer W. Twaddell of Glasgow, who first developed hydrometers on this scale
at the start of the 19th century.
 On this scale, a specific gravity of 1.000 is reported as 0, and 2.000 reports as
200. Concentrated sulfuric acid with a specific gravity of 1.8 has a Twaddell scale
measurement of 160 (as per the linear relationship between readings and sp. gravity).
The Twaddell scale is only used for liquids with specific gravity greater than that of
water. The scale was used in the British dye and bleach manufacturing industries.

0Tw=200(specific gravity-1) or specific gravity =0.0050Tw + 1


Baumé scale
While the Baumé scale was adopted throughout England, the Twaddell scale was used in England and Scotland.
0Be=145 (1- 1/specific gravity) or specific gravity= 145/(145-0Be)
NaOH Concentration

 For specific gravity 1.2 or 17.81% (v/v) or [21.37 (wt/v) or


213.7gpl] NaOH,
 0Tw reading will be=200(specific gravity-1) = 200(1.2-1)=
40 0Tw

 Or 52 0Tw=200(specific gravity-1) or Specific gravity
=52/200+1= 1.26
 Thus, NaOH, Specific gravity 1.26 stands for 23.5%
Specific gravity of Sulphuric acid
Mercerisation
Mercerization
 John Mercer in England: 1850
 Mercerization gives cotton woven cloth a silky lustre, and is the foundation of many improved and
beautiful finishes.
conditions:
 Application of caustic soda solution around 55-60 0Tw ( 31 to 35% v/v) at a temperature of 15 to 18
degree C
 A dwell period of 55 sec on an average, so as to permit diffusion of alkali into the fibre.
 Warp tension during alkali treatment and stretching the weft (width) of the fabric during washing
are necessary to prevent shrinkage.
 Finally, washing-off of the traces of alkali from the treated fibres.
Process parameters:
•Lye (Sodium hydroxide) temperature
•Lye concentration
•Lye reaction time 0Tw=200(specific gravity-1)
•Fabric lengthwise and crosswise tension Sp gravity = 1+ 60/200=1.30
AT WHICH STAGE CELLULOSE CAN BE
MERCERIZED?

 Mercerization is possible
 On greige goods
 After desizing
 After desizing and scouring
 After bleaching
 After dyeing
Need of wetting agent

 The wetting agents should be selected so that it should have good solubility and
high wetting ability in the alkaline bath, should have no affinity to fibre, low
foaming power, good efficiency at low concentration and stability under
conditions of sodium hydroxide recovery by centrifuge or vacuum evaporation
technique etc.

 Cryslic acid derivatives coupled with selected solvents such as triethyl or tributyl
phosphate and the other type is non-cryslic type.

 Mixtures of ortho, meta and para cresols (also called cryslic acid ), CH3-C6H4-
OH
Changes in the Properties of Cellulose Due to Mereerization
Dependence of swelling on
temperature and concentration of
alkali
 Swelling and shrinkage of eellulose
 Under optimum conditions each cotton fibre may contract nearly 9%
in length and swell nearly 150%.

 For small concentration of alkali, the diameter of the hydrated ions is


too large to penetrate into the macromolecular structure of cotton, but
as the concentration increases, the number of water molecules
available for the formation of hydrates decreases
Tyrone L. Vigo
Structural modification

 Because of the distortion of polymer network and changes in crystalline


structure, the process of mercerizaation is irreversible.
 The shape of native cellulose crystal (Cellulose I) is monoclinic and
the dimensions of monoclinic unit cells may have various crystalline
forms (Cell I to Cell X).
 Out of various Celluloses, Cellulose II is most stable and the other
Celluloses may be reconverted into each other.
 Mercerization without tension allows total conversion of Cellulose I to
Cellulose II to take place, whereas when mercerizing with tension,
mixtures of the two are formed.

Schematic lattice structures of


(A) cellulose I (native cellulose)
and (B) cellulose II.
Lustre
Increased lustre
 When a cotton hair is brought into an aqueous solution of sodium hydroxide of
18% (40 degree Tw cellulose begins to swell immediately, the hair is elliptical in
section in a few seconds, and on further swelling becomes circular and the lumen
is practically eliminated. The untwisting of the fibre takes place under effect of
swelling and increased alignment and packing of the fibres in the yam also take
place.
 Lustre increases as the tension applied to the fibre during mercerization is
increased

•Increase transparency and reduce surface roughness.


Strength
 Mercerization increases the tensile strength of cotton fibres by eliminating the
weakest points in the fibre. Mercerization increases the cohesion between
individual cotton hairs and this closer embedding of the hairs in the yam not only
increases the strength but makes it more uniform in strength and less in diameter.
 The increase in orientation of the crystallites with respect to fibre axis can be
attributed to increase strength.
 When cotton fibre, yarn or cloth is mercerized, its strength increased by 10-50%.
The tensile strength increase depends on various factors, such as temperature of
impregnation, concentration of alkali in impregnating bath, construction of yarn
etc.
 Orientation: Increases
 Elongation: Decreases
Removal of immature cotton:

 Mercerization has been recognized as a method for removing immature (dead)


fibers to obtain level dyeing effect on cotton fabrics.
 The dead fibers are underdeveloped and appear as flat or slightly twisted tapes.
They are non-crystalline, convolutions are sometimes absent, cell walls are
extremely thin and the lumen is collapsed and hence do not contain dye to same
extent as matured fibers.
Moisture absorption, dye uptake & reactivity
 At Molecular level, It will have Hydrogen bond readjustment, Orientation (parallelization) of
molecular chains in amorphous region along the direction of fibre length and Orientation of the
crystallinity in the direction of the fibre length. On the other hand it facilitates Chemical Changes
like, Increased rate of reaction on hydrolysis and oxidation; Liberation of heat during the caustic
treatment (heat of sorption and heat of reaction; Increase in the alkali absorption and Increase in
the absorption of iodine.)
 Mercerized celluloses absorb more water, have higher regains and more easily wet out than
unmercerized fibres.
 Standard cotton has moisture content of about 7%, mercerized cotton with tension has about 9%
and that of without tension about 11%.
 Mercerization, thus decreases the amount of crystalline part or increases the amorphous content
of the fibre.
 It is estimated that the number of available, hydroxyl groups are increased by about 25%.
 There is approx. 20-30% dye and chemical saving while dyeing after mercerizing.
Determination of Degree of Mercerization
Determination of deconvolution count
 Under this mercerised fibres are cut down (hair fragments 0.2 mm long)and then
mounted in liquid paraffin on a microscopic slide. Further, examine under
microscope and fibre with and without convolution are counted.
 The numbers of fibres without convolution per 100 fibres is called
"Deconvolution Count" Generally percent unconvoluted fibres are measured.
Generally the unconvoluted fibre(%) in the unmercerized cotton is around 5 to 15
%, while in fully mercerized it become upto 80%.
 The disadvantage of this method is that the extent of deconvolution is influenced
by the maturity of cotton and by the structure of material that is twist of the yam
or weave of cloth.
Cross-section of cotton fibre before and after mercerization.

 Mercerization increase the lustre and reduces the axial ratio. Microscopic
examination shows that the corss-section of the cotton fibre changes from eliptical
to circular form due to mercerization. This can be measured as a ratio of two axes
'a' and 'b'. The axial ratio (a/b) of unmercerized cotton is about 2.2 to 2.6,
whereas that of mercerized cotton is about 1.5 to 1.6.
 Caustic mercerized samples appear to give superior lustre than ammonia treated
fibre.
Lustre, %

The mercerized sample is illuminated at an angle of incidence of 45 degree with the


help of filament lamp. Light reflected at 45 degree and 90 degree is measured by
photo electric cell. Lustre is defind by the contrast ratio of specular to diffuse
reflectance. The specular reflectance measurement method is considered as an
accurate evaluation of lustre.

Lustre = contrast ratio of specular to diffuse reflectance

Lustre= Light reflected at 45 degree/ light reflected at 90 degree


Benzopurpurine test (C.I. Direct Red 2)

In this method mercerized and unmercerized cotton samples are treated in a


0.5% solution of Benzopurpurine (Azo dye) for 30 min at boiling
temperature. The treated samples are then washed, dried and compared
visually or spectrophotometrically. The mercerized sample is always more
deeply dyed than the unmercerized. However, it is recommended that a
standard swatch be calibrated so that the actual degree of mercerization can
be assured.
Sodium hydroxide spotting test
In this method the undyed fabric is spotted with 30% solution of
caustic soda and then both mercerized and undyed spotted fabric
samples are dyed by using Benzopurpurine. If the fabric is fully
mercerized, the spots will not be evident after dyeing. On the other
hand, if the fabric is not mercerized or semi-mercerized, dark spots will
be evident and the degree of mercerization can be evaluated on
comparing the spots.
Barium Activity Number
 Mercerized cotton fibre is highly absorptive. It absorbs more iodine, dyes, moisture and alkalis
and undergoes oxidation or hydrolysis at increased rates compared to unmercerized cotton.
 BAN method is based on preferential absorption of barium hydroxide from its dilute solution by
mercerized cotton as compared to unmercerized cotton under the same conditions.
 In the test, the mercerized and unmerserized samples weighing 1 g were treated with 30 ml of
0.25 N Barium hydroxide solution for 2 hours. Then 10 ml of solution (with few drops of
phenolphthalein indicator) from that was titrated against 0.1 N hydrochloric acid (pink colour to
colourless). A blank was also run without any fibre sample. The barium activity number is
measured by using following formula:

Barium activity number = {(B-M)X100}/ (B-U)


 Where B is the titration reading for blank, M for mercerised and U for unmercerized.
 BAN of Unmercerized cotton - 100
 Semi-mercerized cotton - 115 to 130
 Completely mercerized cotton ~ 155 .
Recommended books for preliminary pre-treatments
and dyeing
 1. Bird C L and Boston W S, “The theory of coloration of textiles”, Dyers Company Publication Trust,
Bradford, England, 1975.
 2. Manivaskaram N, “Treatment of Textile Processing Effluent”, Sakthi Publications, Coimbatore, 1995.
 3. Peters R H, “Textile Chemistry”, Vol- III, Elsevier Scientific Publishing Co., New York, 1975,
 4. Smethwurst G, “Basic water Treatment”, IBT Publications, Delhi, 1989.

 5. Sule A D , “Computer colour analysis”, New Age International (P) Ltd., New Delhi, 1997.
 V A Shenai, Technology of Bleaching and Mercerising, Vol 2, Sevak Publication, Mumbai (1991).
 Peters R. H, “Textile Chemistry”, Vol - II, Elsevier Publishing Company, London (1967).
 Shore J, “Cellulosics dyeing”, Society of Dyers and Colourists, Bradford, UK (1979).
 Mittal R M and Trivedi S S, “Chemical Processing of polyester / cellulosic Blends”, Ahmedabad Textile
Industries Research Association, Ahmedabad, India (1983).
 Karmakar S R, “Chemical Technology in the pretreatment processes of Textiles”, Textile Science and
Technology Series, Vol-12, 1st Edition, Elsevier (1999).
Thank you
Chemical processing of manmade fibres and blended
textiles (TTCP 327)

Heat setting
(Only for Academic purpose during Covid time)
Dr. Lalit Jajpura,
Associate Professor, Department of Textiles
Technology,
Introduction
 It is stabilisation treatment to thermoplastic fibres.
 Heat-setting is a heat treatment by which shape retention, crease resistance, resilience and
elasticity are imparted to the fibres. It also brings changes in strength, stretchability,
softness, dyeability and sometimes on the colour of the material. All these changes are
connected with the structural and chemical modifications occuring in the fibre.
 An unset polyester filament yam shrinks about 7% when allowed to relax in boiling
water. This shrinkage is about 10% in the presence of carrier at boil.

Drawing 
 The H-bonds are formed at random and there are strains between the chains. The single
chains are, however, not yet completely stretched out and are still kinked having a zigzag
configuration. If energy in the form of heat is supplied, the chain molecules starts
vibrating, some of these interchain bonds break and some parts of the molecular chains
have a greater freedom and relax. The temperature at which there is certain increase in
molecular vibration of polymer molecules depends on Tg of the particular fibre. The
higher the temperature the more interchain bond breaks and greater the relaxation, but
care has to be taken not to heat the fibre so as to damage it.

 The newly formed bonds are more difficult to break and the fibres are dimensionally
stable and will not shrink at approximately 10 degree C below the temperature of setting.
At this juncture the process temperature commences to produce a new heat memory and
Tg is changed.
The process of thermosetting in stenter can be broken down into four
distinct phases:

 i) The goods are run wet or dry into the machine and heated
superficially to the heating temperature (heating phase).
 ii) The heat penetrates the fibres untill all points, inside and out, are
at the same temperature (penetration phase).
 iii) Heating of the fabric to a temperature which is specific for each
fibre, ensuring breakage of intermolecular bonds and equalising
internal stresses (transition and stretch phase).
 iv) Cooling the fibre resulting in the restoration of intermolecular
bonds which are free from internal stresses (cooling phase).
Stages of Heat Setting
 In grey condition
 After scouring
 After dyeing.

In grey condition
 If heat-setting is carried out in the loom state, mineral oils and non-ionic emulsifiers
can modify the fibre structure and rubbing and perspiration fastness may be reduced
due to the solubility of disperse dye in the coning oil.
 PVA size above 135 degree C looses its Tg which is followed by becoming crystallized
and melts and becomes difficult to remove from the fabric.
 However, grey heat-setting is useful in the warp knitting industry for materials that can
carry only small amount of lubricants and for goods that are to be scoured and dyed on
beam machines. The other advantages of grey heat-setting are : yellow colour due to
heat-setting can be removed by bleaching, fabric is less sensitive to crease formation
during subsequent processing.
Heat-setting after scouring
 Heat-setting can be carried out after scouring if it is suspected that the
goods will shrink or for the cloth in which 'stretch' or other properties are
developed during a carefully controlled scouring process. However, this
stage requires drying the cloth twice.

Heat-setting after dyeing


 Heat-setting can be carried out after dyeing also. Post set fabrics show
considerable resistance to stripping compared with the same dyeing on
unset fabric. The disadvantages of post setting are : yellow colour
developed cannot be removed any more by bleaching, handle of the cloth
may get altered and there is a risk of colours or optical brighteners be faded
somewhat. Heat setting after dyeing usually involves lower setting
temperatures and care in dye selection to ensure that the non-ionic disperse
dyes do not vaporise from the fibre surface.
Methods of Heat-Setting

Contact method
 Fabric is pass through metal rollers having gas fired cores and are filled with a
liquid known as diathermy or steam to uniformly distribute the heat. This method
is mainly used for heat-setting of polyester/cotton blended fibre fabrics.
 Though heat is used efficiently in this method, the width of the fabrics cannot be
controlled while fabrics run against the roller surfaces, apart from variation in
degree of setting caused by variation in tension.
Steam-setting method
 Short staple polyester yarns including polyester/cotton blends are normally set by relaxation in
saturated steam. The most effective means of stabilising these materials are to steam at 107
degree C on the ring spinners tube and soft dyeing packages (perforated packages) under
minimum tension. Steaming is carried out in an autoclave fitted with vacuum pump, e.g. two
times 15 min at 125-135 degree C with intermediate evacuation or alternatively, for 60 min with
saturated steam.
 Sewing threads receive special setting treatments, designed to confer stability whilst preserving
their high tensile properties.
 Polyester garments, garment lengths and hosiery are also stabilised by steaming in much the
same way as for yams.
 Nylon can be set in saturated steam at temperatures above 100°C in an autoclave by batch wise
process.
 Typical steam setting conditions are 115 OC (10 lb per in sq) to 130°C (25 lb/in2) for nylon 6,6
and 108 °C (5 Ib/in2) to 121°C (15 lb/in2) for nylon 6.
 Steam setting increases the build up of acid dyes and unlevel dyeings will result if the
temperature varies throughout the batch.
http://www.kd-biella.com/en

Karl Mayer made its HKS 2-3 E tricot machine for warp knits
Hydro-setting method

 The hydro-setting or aqueous heat-setting of polyester is done with hot water in


a high temperature liquor circulating machine at about 130°C. A typical cycle
may require 30 min. Water (or steam) promote swelling of fibre and may cause
some hydrolysis in the ester groups in polyester chain.

 Nylon fabric can be hydro-set in hot water since the swelling action assists in
weakening or breaking intermolecular bonds. The fabric in flat form is batched
onto a perforated metal cylinder and immersed in hot or boiling water for a
short period of time. Hydrosetting at boil is roughly equivalent to dry setting
at 1850C.
Stenter
 Drying
 Heat setting
 Curing and fixing of chemical finishes
 Development of dyes of dyed and printed
fabrics
 Brukner
 Monfort Fongs’
 Krantz
 Dilmenler
 Yamuna
 Swastik Textile engineers Pvt Ltd
Stenter
FEEDING ZONE
 Pneumatic padding mangle: Stenter Machine, the main structure is fabricated out of heavy duty M.S. –plate
and incorporates with entry device, rubber and ebonite squeezing rolls SS. Tank fitted with SS. Guide rolls
and pneumatic pressure system.
 Pre dryer & compensator : The system consists of 20`-30` Dia. S.S. cylinder of required with total 4“ NOs.
dynamically balanced and gas heated system. Cylinders are mounted on heavy channel structure frame with
complete accessories guide roll proved for maximum contact of fabrics the compensator unit ensuring, proper
speed synchronization of the Stenter and mangle.
 Bow & weft straightener : The precise bow & weft strengthener having two curved rubber sleeve expander
rolls & two ebonite coated rolls are provided for fully straightening of the fabric the auto feeding device
fitted at the entry of the Stenter.

Scroll roll
 MAIN HEATING OR SETTING ZONE
 STENTER (STENTER MACHINE): The main Stenter Machine stands on C.I. cast legs which ensuring the
vibration free movement of the machine precisely machined C.I. cast rails fitted on the structure for smooth & the
accurate running of the clips.
 The clips are S.G. iron casted which gives long & sturdy life and special without damaging the fabric clips
openers are provided at both the entry and delivery end of the Stenter.
 The stenter is driven heavy sprockets fully motorized & a complete system of width adjustment is fitted on the
machine.
 DRYING CHAMBERS: The main structure fabricated out of M.S. angles & covered with fibre glass wool, pad
insulated panels, which ensuring & keeping the temperature inside the chamber. The chamber covered the
complete length of the Stenter.
 SELVEDGE DRYING & PLATING UNIT : The main structure fabricated from heavy M.S. plates and 3 Nos.
stainless steel cylinders with the heating system which gives the quick drying for the selvage of the fabric.
 HEATING SYSTEM: The heating system will be gas fired heating in drawing chambers is possible with
infrared radiant burner fitted with the copper connection. Regulating valves & needle & V type burners are fitted
with required accessories.
COOLING ZONE:
• Cooling arrangement
• The complete plating down unit at the end of
the machine.
http://textilescommittee.nic.in/writereaddata/files/publication/Pro8.pdf
Heat-setting using stenter frame
 Stenters that are used for setting only have a light pin chains whereas stenters used for both drying
and setting (finishing) are provided with a heavy combined pin and clip chain. For knit goods
vertically running pin stenter chains are particularly suitable. In order to be suitable for drying and
setting purposes, the stenter rails are divided into three sections and can be moved laterally about
the centre line. The entry section consists feeding in, with padding mangle, selvedge uncurler (for
knitted goods), shrinkage apparatus (up to 30%), selvedge feeler for automatic correction of width
and instrument panel with all switches.
 The stenter frame is usually 80-100 feet long and 70-100 inches wide. The speed ranges from 10-
45 m/min with a maximum setting time in the setting zone 30 sec at temperature ranging from 175
to 250 degree C depending upon the thickness and type of the material.
 The shrinkage in length and width may be as much as 10% and this must be taken into
consideration in determining the overfeed and the adjustment of the width. Most of the stenters
make provision for overfeeds- 5% to + 40%.
 An overfeed of up to 20% (generally 6-10 %) is commonly used in knit goods or texturized
fabrics in order to level out variations in tensions caused by knitting. For woven goods an overfeed
of 5 to 7% is generally sufficient. The overfeed device mechanism varies from make to make of
stenter.
Multilayer stenter
The multi-layer stenter is available in versions with 3 or 5 fabric passes (layers).

Selective infra-red emitters method


Polyester can be heat-set by exposing the material under selected areas of magnetic spectrum of infra-
red rays. The wavelength of the radiation source must be chosen with respect to the absorption band
of the fibre i.e. a particular infra-red wavelength is chosen for a particular fibre. For example, in the
case of polyester the selective infra-red radiation wavelength is the region of 1 to 4 micro meter. The
radiations of wavelength of 1 to 2 micro meter passes freely through the polyester fabric and that of 3
to 3.5 micro meter are practically completely absorbed by polyester.
Heat-setting Conditions for Different Kinds of Fibres
Polyester fabrics
 Polyester piece goods are pre-set with hot air on pin stenters for 20-40 sec at 180-210 degree C according to
the type, density and weight of the material, with minimum tension on the goods to control the dry heat
stability to less than the accepted 1% shrinkage.
Heavier fabrics like suiting's require more time as fabric heating time is more. Plain fabrics, woven from unset
yams may be expected to shrink by approximately 5% in warp and weft during scouring process and their
residual potential shrinkage range from 4.5% to about 11% over the temperature range of 150 to 220 degree C.
Polyester fabrics are effectively dimensionally stable if it is set at a temperature of 30 to 40 degree C higher than
the temperature to which the fibre is subjected to expose during subsequent processes.
Nylon fabrics
An overfeed of 2-3% is normally required but this has to be determined before-hand depending upon the handle
and structure required. On steam injection stenters the heating medium is a mixture of super-heated steam and
air. The superheated steam required for the purpose can be generated inside the chamber by injection of
saturated steam. In this mixture total heat capacity of the medium is increased considerably because the specific
heat of steam-air mixture is almost twice the air alone and the fabric can be set at a running speed of 60-70
yds/min.
Texturised polyester and nylon fabrics
 The heat-setting temperature is always kept below the temperature of texturisation. Nylon can
be heat-set only once and differs in this respect from polyester fibres, which can be repeatedly
heat-set at progressively higher temperatures. This is of particular importance in the
processing of knitted fabrics produced from textured yarns since such yams have already been
permanently heat-set.
 Texturised polyester yams: Woven fabrics made from texturised polyester yams should be
heat-set for 20-30 sec at 160 degree C with slight width extension to remove creases, but
without true overfeed so as to avoid the production of rippled selvedges. Higher setting
temperatures (e.g. 165-170 degree may be required to control the tendency of some fabrics of
tighter construction to crease during jet dyeing, but these temperatures can cause some loss of
yarn bulk and tend to give a modified, leaner handle.
 Texturised nylon yarns: For texturised nylon, after relaxing heat-setting is normally done at
150-160 degree C for 30 sec in a hot air stenter with an overfeed of 10-15%. The overfeed can
be increased to 15-20% depending upon the type of stretch.
Acrylic and modacrylic fabrics
 These fibres cannot be heat-set in the conventional sense since the fibres are readily stretched
or deformed at temperatures above 75 degree The degree of stability, however, can be obtained
by passing these fabrics through a hot air stenter at about 120 degree C Temperatures above
120 degree C may cause discolouration of the fabrics. For blended fabrics containing acrylic
and modacrylic fibres higher heat-setting temperatures may be required. Knitted fabrics
produced from a feeder blend of acrylic and textured polyester fibres, are heat-set at about 160
degree for 30 sec.

Cationic dyeable polyester fibre fabrics


 Generally, CDPET has a slightly lower heat resistance than the regular PET, so that heat-
setting temperature for CDPET is kept slightly lower than that of normal PET.
Triacetate fibres
 An important property of triacetate fibres is the ability to undergo structural changes under the
influence of heat. Triacetate is not effected by dry heat up to 150 degree C.
 The fibre becomes increasingly less plastic between 150 to 190 degree C and at still higher
temperatures up to 220 degree C molecular reorientation occurs to an increasing extent
accompanied by increase in crystallinity and thus reduction in absorption and desorption of
dyes. A permanent change in thermoplastic behaviour takes place and the fibre becomes
increasingly less plastic.
Heat setting of blended textiles
Polyester / cotton blends
 Higher temperatures may discolour the cellulosic portion of the material. Normally heat-
setting in stenter with hot air is carried out at 180 degree C for 30 secs.
 For increased stability, setting may be carried out even at 200 degree C for 30 secs without
serious risk of damaging the cellulose.
 Approx 1-2% residual shrinkage is allowed.
Polyester/ wool blends
 Polyester/wool blended fabrics are normally heat-set before dyeing. Similar effect is
obtained on the wool component on the blend by crabbing. Polyester/ wool blended fabrics
can be heat-set in a hot air stenter for 30 secs at 180 + 10 degree C.
 For worsted-spun goods 3-5% relaxation shrinkage is allowed both warp and weft and for
woollen-spun materials 1-2% is allowed.
 Fabrics having wool content above 67% need not be heat-set as adequate dimensional
stability can be imparted by autoclave decatising popularly known as K.D.Finish.
Effect of Heat-setting on Various Properties of Synthetic Fibres
Polyester
The following changes take place as a function of
increasing temperature in polyester when heat-set
under free to relax conditions (i.e. free annealing)
and when held taut at constant length (i.e.taut
annealing) :
 Crystallinity increases with increasing
temperature in both the cases, but is more for
free or slack annealed samples at all
temperatures.
 Crystal size increases in both the cases.
 Crystallite orientation and birefringence increase
in case of taut annealed samples, but decrease in
case of free annealed samples.
 Amorphous orientation decreases in both the cases. In free annealed sample the
decrease is greater due to shrinkage allowed.
 The number of crystals in the fibre increases but at higher temperatures, the
crystals fuse together and their total number decreases and crystals become
perfect.
 Amorphous volume per crystals first decreases and then increases in both the
cases. This change affects the dye ability of heat set polyester.
Nylon
 Heat -setting processes result in inner changes in the amine end group content of nylon
fibres and such changes will only slightly modify the uptake of acid dyes. The density
and crystallinity of nylon increase on setting both in dry heat and in saturated steam.
Application of tension assists in the development of crystallinity.
 When heated under tension orientation increases. The increased orientation is lost,
however, by allowing the stress in the fibres maintained under tension to relax.
 Crystallinity and crystal size increase more readily at a lower temperature for steam set
sample compared to dry set samples.
 The orientation of the crystalline regions resulting from both types of heat-setting show
similar trend whereas the orientation of amorphous regions of the wet set material
increase rapidly with the setting temperature.
Dimensional stability

The higher the temperature to which the yarn or fabric is exposed, the higher the resultant
shrinkage over the temperature range of 100-200 degree C. As the result of shrinkage, the
mechanical properties of the fibre change so that its extensibility increases and breaking load
diminishes without appreciably changing the work of rupture.
Stiffness
 The setting process stiffens the fabric, which is undesirable. Higher the
setting temperature, more is the stiffening. A fairly linear correlation exists
between the stiffness and setting temperature

Crease recovery
 One of the purpose of heat-setting is to reduce the extent of creasing on
subsequent dyeing and washing processes. The higher the setting
temperature the less is the wet creasing. The degree of wet creasing, is
however also related to fabric construction, for example, open or loose
construction fabrics show better crease recovery than dense fabrics. High
setting temperature which creates a degree of stiffness in the fabric
does not recover well from creasing of dry polyester fabrics.
Dyeability

The effect of heat-setting temperature on dye uptake


when polyester is dyed with C.I.Disperse Red 1 at boil after the heat setting treatment
Test for heat setting
 Shrinkage test
Normally a square area is drawn on the heat-set material and measured. The
marked cloth is boiled in soft water in the washing wheel for 30 min,
centrifuged and air dried. The dimensions of the square are measured without
ironing the dried fabric and the shrinkage is determined. A well set fabric
should not show more than 1% residual shrinkage.

 Crease-recovery angle
The determination of crease recovery angle before and after heat-setting of
the fabric is done. The extent of crease-recovery of heat-set fabric before and
after setting at and above 170-175~ will give idea of the degree of heat-
setting.
 Iodine absorption method
The degree of heat-setting of polyester fabrics can be correlated with their
iodine absorption value. Heat-setting under industrial conditions in a taut
form reduces the amorphous content of synthetic fibres. So, there will be a
decrease in iodine sorption and increase in critical dissolution value.

 Assessment of handle
Assessment of handle before and after setting gives an idea of the degree of
heat-setting. In general, fabric becomes stiff after heat-setting. Stiffness is
measured by bending length and compared with that of the unset fabric. The
narrower the difference of bending length between the set and unset fabrics,
the better the Setting.
Books Recommended:
 1. Nunn D. M, “The Dyeing of Synthetic Polymer and Acetate Fibres”,
Dyers Company Publication Trust, London, 1979.
 2. Shore J, “Colorants and Auxiliaries”, Vol- I and II, Society of Dyers
and Colorists, Bradford, England, 1990
 3. Gulrajani M.L, “Polyester Textiles”, Book of papers: 37th National
Textile Conference, The Textile Association (India), Mumbai, 1980.
 4. Gulrajani M.L, “Blended Textiles”, Book of papers: 38th National
Textile Conference, The Textile Association (India), Mumbai, 1981.
 5. Datye K.V and Vaidye A.A, “Chemical Processing of Synthetic
Fibres and Blends”, John Wiley and Sons, New York, 1984
books for preliminary pre-treatments and dyeing

 V A Shenai, Technology of Bleaching and Mercerising, Vol 2, Sevak Publication,


Mumbai (1991).
 Peters R. H, “Textile Chemistry”, Vol - II, Elsevier Publishing Company, London
(1967).
 Shore J, “Cellulosics dyeing”, Society of Dyers and Colourists, Bradford, UK (1979).
 Mittal R M and Trivedi S S, “Chemical Processing of polyester / cellulosic Blends”,
Ahmedabad Textile Industries Research Association, Ahmedabad, India (1983).
 Karmakar S R, “Chemical Technology in the pretreatment processes of Textiles”,
Textile Science and Technology Series, Vol-12, 1st Edition, Elsevier (1999).
Books Recommended for Printing and Finishing:

Blends of Dyeing
 John Shore, Blends Dyeing, Society of Dyers and Colourists, 1998
Pre-Treatment and Dyeing Machines
 Chemical Processing of Textiles: Preparatory Processing and dyeing by NCUTE
Publications
Printing
 Miles L W C, “Textile Printing”, Dyers Company Publication Trust, Bradford,
England, 1981.
 Shenai V A, “Technology of Printing”, Sevak Publications, Mumbai, 1990.
 R S Prayag, Technology of Textile Printing, Jyoti Printers, Dharwad,
References
Finishing
• Dr Charles Toasino, Chemistry and Technology of Fabric Preparation and Finishing
• Shenai V A, “Technology of Textile Finishing”, Sevak Publications, Mumbai, 1990.
• M. Levin, Handbook of Fiber Science and Technology, Vol. II, Chemical Processing of Fibers and
Fabrics. Functional Finishes, Part B, Levin M and Sello S B (eds), New York, Marcel Dekker,
1984, 1–141.
• W. D. Schindler and P. J Hauser, “Chemical Finishing of Textiles,” Cambridge, Wood Head
Publishing Ltd., Vol. 165, 2004
• A. K. R. Choudhury, In Principles of Textile Finishing, Woodhead Publishing, 2017, 195-244
• Hall A J, “Textile Finishing”, Haywood Books, London, 1996.
• Shenai V A and Saraf, N M, “Technology of Textile Finishing”, Sevak Publications, Mumbai,
1990.
• Nunn D M, “The Dyeing of Synthetic Polymer and Acetate Fibres”, Dyers Company
Publication Trust, London, 1979.
Thank you
Colour Measurement in Textiles
Specifically for academic purpose during the Covid 19

Dr. Lalit Jajpura,


Associate Professor, Department of Textiles Technology,
Contents
 Introduction
 Electromagnetic spectrum
 Visible light
 Interaction of incident light on object
 Perception of colour
 Colour mixing or colour theories
 Colour specifying systems
 Munsell colour system
 CIE colour system
 Details of standard primaries, light sources, observer and viewing conditions
 Concept of colour measurement
 Tristimulus values (R, G and B)
 CIE imaginary primaries [X], [Y] AND [Z],
 CIE chromaticity diagram
 The CIELab, 1976
 Colour Matching System
 Applications of CCM software
Colour
 Plays important role in Aesthetics
 Textile
 Fibre, yarn, fabric and Garment

 Textile wet processing


 Preparatory wet processing, dyeing, printing &
Finishing

 Paints, plastics, paper printing, foods,


cosmetics, etc
 Electrical gadgets i.e. camera, colour
printers, LED TVs, mobiles
Visible light is the region of the electromagnetic spectrum to which
our eyes are sensitive. It corresponds to wavelength range from
360 to780 nm, or more commonly, 380 - 720 nm. The ultraviolet
region is below 360 nm and the infrared region is above 780 nm.
Visible light
Sir Isaac Newton in 1660 split white light into its component colour.
Interaction of Incident light on object
When light falls on an object, one or more of the following can
take place:
i) Transmission ii) Absorption iii) Scattering.

Object may be transparent and colourless, or it may be opaque.


If light is pass through the object it is known as colourless.
If part of light is absorbed, then the object looks coloured but transparent. If all
light is absorbed, then the object is black and opaque. Scattering is caused by
light falling on small particles within the object and having refractive index (RI)
different than that of the object.
Perception of colour
Colour is basically sensation (similar to touch, taste, odour) phenomen which
occurs when light is enters the eye. A photochemical reaction occur in side
the eys which results in impulses that are transmitted along the optic nerve to
the brain.

The perception of colours involves the interaction of three elements.


• Source of light
• An object
• Human eye

Dye stuffs give colour to the substrate or object by selectively retaining some
of the wavelengths out of the light falling upon the surface via absorption. i.e.
if dye absorb light in cyan region (between blue and green wavelength) of
visible light then resultant light that is reflected will be of a reddish hue.
Perception of colour
The retina in human eye has two distinct types of
nerve cells as follows:
• Cones: Cones nerve cells are capable to sense
the colour to the brain. Although it is able to
respond only in bright daylight or strong
artificial light. As per most acceptable Young
–Helmholtz theory, there are three types of
cones which sense the red, green and blue
wavelength of light and send the signal in
terms of electrical impulse via optic nerve to
the brain where it is perceived as colour.

• Rods: They play their efficient role in low


illumination light (i.e. in dusk, evening or in
night vision) when cones are not able to
stimulate photochemical reaction to perceive
the colour. They perceive the objects as greys
and black.
Subjective nature of colour vision

The human eye is unable to view colours consistently


due to certain reasons. The colour vision of human eyes
are dependent on following factors:
• Tiredness of the eyes
• Emotional sate of the observer
• Type of the illumination
• Contrast
• Age of the observer
• Defective colour vision
Tiredness of the eyes
• Positive after image: A prolong exposure to a coloured
substrate may result in the colours being seen for a few
seconds even after the objects have been removed from
view.
• Successive contrast: This occurs when, having
concentrated upon a coloured object, the eyes are turned
away and see the complementary colour(s) of the colour
just viewed. Successive contrast is the commonest type of
the after vision.

• Simultaneous contrast: Sometimes an object being


observed appears to be surrounded by a halo, or tinged
with its complementary colours. This effect is known as
simultaneous contrast.
Type of illumination
• Poor illumination or intensity of
illumination
• Direct sunlight: It has slight yellow tinge.

• Indirect sunlight: It is also known as


southlight or northlight. It has slight blue
tinge as blue light waves of indirect
sunlight are scattered more from molecule
of the air than waves of the other colours.

• Incandescent light: An electric bulb emit


incandescent light with excess of yellow
and red light energy.

• Fluorescent light: It has excess blue and


green light with deficiency of red.
Although, eye perceive blue colour light as
white light.
Defective colour vision
As per estimation around 8% male and 2 % female population
have defective colour vision in one or more forms. This is due
to inefficient red, green and blue cones receptors in eyes.
Colour Mixing or colour theories
Fundamental to the specification of colours is an understanding
of the laws of colour mixing, the processes by which two or
more colours are combined to ‘synthesise’ new colours.

There are two fundamentally different ways in which this may


be achieved:
1. Additive colour mixing (Light colour theory)
2. Subtractive colour mixing (Pigment colour theory).
Additive colour mixing (light colour theory)
Combinations of the primary colours (RED, GREEN & BLUE) produce a
diversified range of colours.
The appropriate combinations of all primary colours is white light.
Applications: Television, mobile screens, LED, etc

Primary colours are: Red, green and blue

Red + green + blue = white

Secondary colours are: yellow, cyan and magenta


Red + green = yellow

Green + blue = cyan

Blue + red = magenta

No light = black
Subtractive colour mixing or pigment colour theory
The mixing of dyes, pigments, printing paste, etc is called subtractive colour mixing.
The subtractive term define that when visible light falls on any object (dyes, pigment
or textile) then colour is subtracted from the light. In fact, perceived colour of the
object is complementary colour of subtracted colour by the object.

The primary colours in pigment theory are: Cyan, magenta & yellow
The secondary colours in pigment theory are: Red, green & blue

If object has all these dyes (Cyan, magenta & yellow) in appropriate proportion then
whole visible light is absorbed. Thus, combination of three primary colour in
appropriate proportion in pigment colour mixing theory is black.

Cyan + magenta = blue ;

magenta + yellow = red

yellow + cyan = green ;

cyan + magenta + yellow = black


Specifying colour
• Main Colour Coordinates are Hue, Value, and Chroma.
• Hue is the common name of the colour; ie red, pink, tan, blue,
red, etc. or it shows the tone; i.e., redder, bluer, brownish,
greenish, etc.

• Chroma or saturation of colour shows its depth, strength,


brightness, intensity, vividness or purity of colour. i.e., stronger
or weaker. Intense or dull colour

• Value is lightness; i.e., black to white through shades of grey


Appearance of colour changes when either source or observer
is changed.
Colour specifying systems
It is necessary to specify colour accurately to identify and reproduce it
correctly. Some of the well known colour system are Ostwald, Munsell
and CIE.
• Ostwald colour system: German physical chemist Wilhelm Ostwald
developed colour system in 1920 which enjoy some early success but
it was unable to add new or different colours to those on which it is
based. Thus it supressed by the Munsell system.

• Munsell colour system: Most of the todays’ colour atlases of the dye,
pigment and paint manufactures, colour codes, etc are based on
Munsell colour system. This colour system illustrate colours using
charts by displaying a large range of hues, ordered according to
value and chroma.

• Commission Internationale de L’Eclairage (CIE) system: It is


extensively used colour system based on numeric colour specification.
Munsell colour system
Albert Munsell an American
scieintist developed munsell colour
system in 1915. The position of any
colour can be defined in this system
in a spherical space by three
cylindrical coordinates namely, hue,
value and chroma.
Munsell hue defines the colour. It has
total hues including five principal and
five intermediate munsell colours.
Five principal colours namely, yellow,
red, green, blue and purple which form
a complete circle and five intermediate
hues namely, yellow-red, green-
yellow, blue-green, purple-blue and
red-purple are described. Each of the
ten hues are further sub-divided into
ten equal parts ( 1 to 10).
Munsell colour system
Munsell chroma is expressed as strength or weakness of a colour which can be recognised by
considering a single plane of constant value, one containing light grey at the centre. This is
surrounded by colours forming the complete hue circle. Along any radius, colours will have
the same perceived hue moving outward from the achromatic centre (grey), these colours
increase in chroma. This variable is also called saturation or purity. A colour is
described as weak, moderate or strong in terms of chroma. The chroma scale is from 2 to 16
with 2 interval.
Munsell value gives lightness or darkness of any hue and is expressed vertically from black to
white in terms of number 0 to 10 with a light grey at centre.
CIE SYSTEM OF COLOUR
MEASUREMENT
CIE SYSTEM OF COLOUR MEASUREMENT

• Most of modern colour measurement systems work on the Commission


Internationale De l‘Eclairage (C.I.E.) System of colour specification, agreed in
1931. CIE is an organisation devoted to international cooperation and exchange of
information among its member countries on all matters relating to the art and
science of lighting.

• Colour space is an abstract mathematical solid, describing colour in terms of


values that can be calculated such as, CIE tristimulus values x, y, z or CIE
l*a*b* (1976) which is based on additive colour mixing in which the colour of a
sample is matched by mixing of primary coloured lights.
Details of standard primaries, light sources, observer and viewing conditions

STANDARD ILLUMINANTS:
Three standard illuminants A, B and C together with their spectral power distribution were
defined. Later in 1967, more Illuminants such as D6500, D6700, Illuminants F were standardised to
accommodate increasing use of fluorescent lamps.
• ILLUMINANT_A: It represents a black body radiator at an absolute temperature of
2856ok and is similar in spectral power distribution to the light emitted from a tungsten
filament lamp. It is used to compute metameric index between the standard and the sample.

• ILLUMINANT_B_AND C: Correspond to different phases of daylight, the former represents


noon daylight with colour temperature of 48740K and the latter represents average daylight
with a colour temperature of 67740K. It has been replaced by the illuminant D6500.

• ILLUMINANT D6500 : In 1967, CIE adopted illuminant D6500 as being more representative of
natural daylight which is based on measurements of the total daylight, sun plus sky).

• ILLUMINANT F (COOL WHITE FLUORESCENT LIGHT CWF): Various fluorescent


lights have been standardised by CIE by tabulating their spectral power distribution.
Fluorescent sources consist of a mercury discharge tube, the inside of which is lined with
powder of fluoresce.
https://www.standardpro.com/guide-colour-temperature/

https://en.wikipedia.org/wiki/Color_temperature
SPECTRAL ENERGY DISTRIBUTION OF
VARIOUS ILLUMINANTS
Spectral energy distribution of average day light Vs Special energy distribution of CIE Standard
Illuminants 1. D7500 ; 2. D6500 ; 3. D5500; 4. D5000
Tungsten Light

Spectral energy distribution of fluorescent source


STANDARD OBSERVER

The original 1931 CIE standard observer was based on experiments using a 2o field
of observer. This was a much narrower field of view than that normally used for
critical colour appraisal. A much wider field of 10o was adopted later on by CIE in
1964.
STANDARD ILLUMINATING AND VIEWING CONDITIONS

The original CIE recommendation was that the sample should be illuminated at 45o to the

surface and the light viewed at right angles to the surface which is (45/0). It was

assumed that the opposite mode (0/45) would give the same result which is not the case if

the incident light is polarised. Four possible sets of conditions, are now recommended as 45/0,

0/45, d/0 and 0/d. In the third case, the sample is illuminated by diffused light, while in the

last case the light reflected at all angles is collected (by using an integrating sphere).

(Shah H. S., Gandhi R. S., 1990)


CONCEPT OF COLOUR MEASUREMENT

This concept of colour measurement is based on theory that all the


perceived colours can be formed by mixing of additive primary
colours (red, green & blue). In experiment it is observed that a wide
variety of coloured lamps can be matched by adjusting the proportions
of the red, green and blue lights in the mixture as shown in following
figure:

A colour matching equation to represent this Wright used [R], [G] and [B] (red: 700.0 nm,
green: 546.1 nm and blue:436.8).
situation can be written as
C [C] = R [R] + G [G] + B [B]
The primary colours (red, green and blue) of
particular wave length are presented the
symbols [R], [G] and [B]. The amounts of
these primaries colours required in the
match, R, G and B, are called tristimulus
values.
To over come negative tristimulus value CIE adopted imaginary primaries [X], [Y] AND [Z], which may be
considered to be very saturated red, green and blue primaries, respectively. Being imaginary primary they
may defined mathematically interms of real primaries [R], [G] and [B] used by wright (red: 700.0 nm, green:
546.1 nm and blue:436.8).

• SE = 0.333 [X] + 0.333 [Y] + 0.333 [Z]

The amounts of the imaginary primaries (x, y, z) required to match unit energy of light at each
wavelength of the spectrum can be calculated. These amounts are all positive and are called the C.I.E. 1931
standard observer colour matching functions as shown in following figure. The values of x, y, z for
measurement of each wavelength are published by CIE.
CALCULATION OF TRISTIMULUS VALUES OF SURFACE COLOURS

• If all the wave lengths of white light are viewed simultaneously, then the total
amount of primary (x, y, z) required will be given by their sum
throughout the spectrum. These sums are known as tristimulus values and
denoted by X, Y & Z.
• It is pertinent to mention that there may be variation in light source which emits
different amount of light at each wave length (across the whole visible range) &
• Surface may reflect only proportion of the light incident on it at each
wavelength. The proportion of reflection also varies at each wavelength.
Thus, the tristimulus values of reflected light by some object under the standard observer, (x, y, z) are
represented as:

780

X =  EX R
360

780

Y =  E Y R
360

780

Z =  E Z R Special energy distribution of CIE Standard


360 Illuminants 1. D7500 ; 2. D6500 ; 3. D5500; 4. D5000

HERE,
E= spectral power distribution of standard source

R = spectral reflectance factor of the object

X, Y, Z are colour matching functions of the standard observer.
• WRIGHT AND GUILD carried out experiment using a
colorimeter constructed having 20 field of view of standard
observer on which CIE 1931 standard observer is defined.
Although this 20 field of view of standard observer is very
narrower than the normal viewing condition.

• Thus new colour matching experiments were carried out by


Special energy distribution of CIE Standard
Stiles and Birch using a colorimeter constructed having 100
Illuminants 1. D7500 ; 2. D6500 ; 3. D5500; 4. D5000

field of view standard observer. The weighting values of X,


Y and Z for illuminant D65, 100 observer is shown in
following table:

There is need to match amount of standard red, green and blue


(x, y, z) for reflected light of each wave length of
standard illuminant.
The reflectance (R ) may be 0 to 1 for each individual
wavelength. In case of perfect white object R is 1 for each
individual wavelength. Thus the perfect white object will
reflect illuminant D65 light and give.

X=94.8272 ; Y=100.00 & Y=107.3906 as shown in


aforesaid table.

It is pertinent to mention that in perfect white under equi-


energy light source (perfect white) these value would be
X= 100.00 ; Y=100.00 & Y=100.00.

If reflectance of the any object can be determined in

standard experimental condition then tristimulus X,


Y & Z value can be determined as mentioned in
aforesaid table.
The summation is done over a visible range (400-700 nm).
The weighting values for illuminant D65, 10° observer for
CIE 1931 or 1964 standard observer can be obtained
from literature. Where, R is measured by a
spectrophotometer.
RELATIONSHIP BETWEEN
TRISTIMULUS VALUES AND COLOUR APPEARANCE

The three-dimensional nature of colour makes determining relationships difficult and it is usual to
simplify any relationship involving colour by considering only one or two dimensions at a time.
The higher the Y value, the lighter the sample appears. Thus, colour can be specified in terms
of hue and purity on a two- dimensional CIE chromaticity diagram obtained by plotting
chromaticity co-ordinates x and y which are determined from tristimulus values, X, Y, Z
under different illuminating conditions.
As the Y value quantifies the lightness of a surface colour x, y, Y values are, therefore, much
more suitable than X, Y, Z values for quantifying appearance and, in consequence, they
are widely used as shown in figure. Thus,

X Y Z
x = --------------, y= --------------, z= --------------, and x + y + z = 1.
X+Y+Z X+Y+Z X+Y+Z
CIE CHROMATICITY DIAGRAM
LIMITATIONS OF THE CIE SYSTEM
The chief limitation of the CIE system is its non uniformity. Equal changes in
x, y or Y do not correspond to the same perceived difference. Many attempts
have been made to provide more uniform system. In each case, the basic
approach has been to start with the tristimulus values or chromaticity
coordinates from the CIE system and to transform these in some way to give
a more uniform system.
The end result is a colour difference formula which, for a pair of samples
gives a number that is intended to be proportional to the difference seen.
MANY COLOUR DIFFERENCE FORMULAE HAVE BEEN
PROPOSED, SUCH AS:

• ANLAB (1950-52)

• CIELAB COLOUR SPACE (1976),

• CIELUV,

• FMC-1,

• FMC-2,

• HUNTER LAB COLOUR SCALE (1958),

• CMC, ETC.
THE CIELAB, 1976

Out of these, the CIELab formula was recommended by the Colour


Measurement Committee of the Society of Dyers and Colourists in
1976. One of the features of the formula that has proved to be most
useful has been the associated colour space. This is obtained by
using L*, a* and b* as mutually perpendicular axes where L*, a* and
b* are defined by
L* = 116 (Y/Yn) 1/3 16;
a* = 500 (X/Xn)1/3  (Y/Yn)1/3;
b* = 200 (Y/Yn)1/3  (Z/Zn)1/3
where, X/Xn, Y/Yn, Z/Zn  0.01

Where, Xn, Yn, Zn are the tristimulus values for a particular


standard illuminant and observer, for a sample reflecting 100 % of
the light at all the wavelengths. The lightness of the sample is
represented by L* on a scale- zero for black to 100 for white. The
other attributes can be represented on a plot of b* against a*. Neutral
colours lie close to the origin for any illuminant (a* = b* = 0).
COLOUR MATCHING SYSTEM

• The spectrophotometers are the most fundamental instrument for colour measurement, but it does

not measure the colour of a material directly. It measures the light reflected (or transmitted)

from the material, and these values are used to compute the tristimulus values.

• The standard colour matching system consists of spectrophotometer. It enables measurement

of reflectance values since colour is defined in terms of its tristimulus values obtained

from reflectance measurements.


Single beam Spectrophotometer
• The common components of a spectrophotometer are:-

• a) Light source of continuous radiant energy;

• b) Monochromator;

• c) A detector; and

• d) An integration sphere.
APPLICATIONS OF CCM SOFTWARE

COLOURANT STRENGTH & COLOUR MEASUREMENT


Reflectance values measured with the help of A spectrophotometer are converted into additive kubelka-munk (k/s) function which is valid
for a mixture.

K (1 - R)2

S = 2R = C

Where, K = coefficient of absorption; S = coefficient of scattering;

 = optical constant at a wavelength for the dye, called alpha value;

 R = reflectance in fraction at wavelength; and C = concentration of dye.

(K/S)MIXTURE = (K/S)BLANK SUBSTRATE + (K/S)1 + (K/S)2 + (K/S)3 + ------

= (K/S)BLANK SUBSTRATE + C1 1 + C2 2 + C3 3 + ------

Where, C1, C2, C3 are the concentrations of the dyes in mixture, 1, 2, 3 are the corresponding alpha values
of the dyes mixed. It is possible to calculate unknown concentrations C1, C2, C3 to match the standard
shade. The entire process involves the complicated procedure and hence, a digital computer is used to arrive
at the results.
APPLICATIONS OF COLOUR MEASUREMENT IN CCM

• K/S measurement

• Recipe formulation

• Reformulation

• Batch correction

• Synthesise colour

• Shade search programme

• Colour matching

• Colour fastness determination by measuring fading and staining

• Determination of whiteness, yellowness, opacity, fluorescence, etc


REFERENCES

• GOHL E.P.G. & VILENSKY L.D., TEXTILE SCIENCE, CBS PUBLISHERS & DISTRIBUTORS, DELHI-
110032 (REPRINT 1999).

• CHRISTIE R.M. , MATHER R.R. & WARDMAN R.H., THE CHEMISTRY OF COLOUR APPLICATIONS,
BLACKWELL SCIENCE, INC., 2000

• CHOUDHURY A.K. ROY , TEXTILE PREPARATION AND DYEING, SCIENCE PUBLISHERS, 2006.

• SHAH H. S., GANDHI R. S., INSTRUMENTAL COLOUR MEASUREMENT & COMPUTER AIDED
COLOUR MATCHING FOR TEXTILES, MAHAJAN BOOK DISTRIBUTERS, AHMEDABAD, INDIA,
1990.

• HTTP://WWW.PREMIERCOLORSCAN.COM/COLOR_THEORY/MAIN.HTML
Thank you
Colour fastness of textiles
Only for Academic purpose during Covid time

Dr. Lalit Jajpura,


Associate Professor, Department of Textiles
Technology,
Contents
 Introduction
 Factor affecting colour fastness
 The agencies that affect coloured materials include:
 Light Fastness
 Washing Fastness
 Dry-cleaning Fastness
 Perspiration and ironing Fastness
 Chlorine Fastness
 Sea water Fastness
Factor affecting the colour fastness
The fastness properties of a dyeing are a characteristic of the particular dye–fibre combination. They are a
complex function of many variables including:
(1) the molecular structure of the dye;
(2) the manner in which the dye is bound to the fibre, or the physical form present;
(3) the amount of dye present in the fibre;
(4) the chemical nature of the fibre;
(5) the presence of other chemicals in the material;
(6) the actual conditions prevailing during exposure.

Standard depths of shade

The fastness of a dyeing to a given agency such as washing or light normally depends on the depth of shade. We have
already seen that light fastness is higher for deeper rather than paler shades. This is so because the effect on the colour
of photochemical fading of a given number of dye molecules is more pronounced the fewer the initial number of
molecules. On the other hand, washing fastness is usually inferior for deeper shades since the concentration gradients
driving diffusion between the fibre and the washing solution are much higher when more dye is present in the fibres.
Since dyeings vary in depth, it is common practice to determine a fastness property at a standard colour depth.

Arthur D Broadbent, Basic Principles of Textile Coloration, SDC, 2001


The chemical breakdown of dye molecules is most likely to occur when the coloured material is exposed to
agents capable of reacting chemically with it, such as the oxidizing agents contained in detergent powders and
nitrogen dioxides in the atmosphere, or even to the presence of foreign substances in the textile. In the
production of man‐made fibres, titanium dioxide pigment is often incorporated into the polymer mass to
render the resulting fibres opaque (dull fibres), and this can reduce their fastness to light as compared with the
corresponding unpigmented material (bright fibres).

 Residual auxiliary chemicals from the dyeing process, if not thoroughly removed, may also influence fastness. The significant
influence of moisture content on the fastness to light of dyed fibres is also well known. Singlet oxygen, formed by the action of light
in the presence of moisture, is a highly reactive attacking species.
 Fastness assessments are also affected by the fineness of fibres, simply because a given amount of dye on a fine fibre, in contrast to
coarse fibre, is spread over a larger surface area. The compactness of the yarn or fabric structure also affect the fastness. The nature of
the fibre itself can also markedly affect fastness ie fastness to light of basic dyes, for example, is very poor on cotton and wool, but
excellent on acrylic fibres.
 Crease‐resist finishes or dye‐fixing agents applied to some dyed cotton also adversely affect the fastness to light of some dyes.
 Further influences originate from the state of the dye in the fibre. Insoluble pigments trapped mechanically inside the fibre, or dyes
that have formed a strong chemical linkage with the fibre, will obviously be more resistant to removal by wet treatments than dyes
that are more loosely attached.
 The crystallinity and state of aggregation of the dye will also influence its fastness. In general, the deeper the shade, the better the
fastness properties, although a deep dyeing of a dye with poor wash fastness will release more dye into the water than a paler dyeing.

. (Roger H Wardman)
Standard Depths (RH Wardman)

 When evaluating the colour fastness properties of a dye


manufacturer’s dye prior to it being used commercially,
the dyes are measured at standard depths of shade, so
that dyers can compare the performances of dyes from
the different manufacturers on the same basis. These
standard depths of shade were developed during the
1920s by German and Swiss dye manufacturers at the
time. In ISO 105 (Part A01: General Principles of
Fastness Testing), it is stipulated that dye manufacturers
should publish fastness data obtained by testing
specimens at 1/1 standard depth wherever possible,
supplemented by data for one or more of the other ratios
as required.
Introduction

 Test standards
 Dyers and Colourists (SDC)
 The American Association of Textile Chemists and Colorists (AATCC)
 International Organisation for Standardisation (ISO). The International Standards Organisation (ISO)
was formed in 1947 and has a membership of 163 national standards bodies.
 The International Standards Organisation (ISO) was formed in 1947 and has a membership of 163
national standards bodies. It has developed standards covering all aspects of the properties of textiles.
 the International Wool Textile Organisation (IWTO).
 In the United Kingdom the British Standards Institution (BSI) began to formulate standards
relevant to consumer goods during the early 1940s.
 There are some country-based standard organisations, such as the British Standard (BS), American
Standard Test Method (ASTM) and Australian Standard (AS), Bureau of Indian standards (BIS).
These are generally based on the ISO, SDC or AATCC test method with slight changes made to
account for cultural or environmental differences.
 In the field of textiles, all of the ISO standards are adopted as CEN and UK standards. It is not uncommon for
Europe to lead the way in the development of tests and for these tests to become adopted later by ISO. It is
therefore quite common to see standard names with the letters BS EN, BS EN ISO or even BS ISO preceding the
actual title of the standard. The EN prefix indicates that the standard has been adopted by all the member states
 of the EU. The BS prefix is the UK’s national prefix: in other countries the BS prefix is replaced by the relevant
national prefix (e.g. DIN in Germany, NF in France). (Roger H Wardman)

The SDC continues its role in this area, since


writing the first BSI standards for colour
fastness in 1939, by holding the secretariat for
both the BSI and ISO committees. For ISO, the
standards are all in the 105 series and they are
coded by a letter, followed by a two‐digit
number and finally the year of introduction, for
example, ISO 105‐B02:2013. This particular
example is also a British and EN standard, so is
labelled BS EN ISO 105‐B02:2013. The letter
code (in the example given, ‘B’) indicates the
type of agency (light and weathering), of which
there are eleven as shown in Table 8.1. (Roger H
Wardman)
Grey Scales

Colour fastness is usually assessed separately with respect to:


1 changes in the colour of the specimen being tested, that is colour fading; When there is no change in the
colour of a test specimen it would be classified as '5'; if there is a change it is then classified with the number of
the scale that shows the same contrast as that between the treated and untreated specimens.
2 staining of undyed material which is in contact with the specimen during the test, that is bleeding of colour.
Fastness rating 5 is shown by two identical white samples (that is no staining) and rating 1 shows a white and a
grey sample.

Grey scales: The scale used for the assessment of colour change Grey scales: the scale used to assess staining
in the sample
Arthur D Broadbent, Basic Principles of Textile Coloration, SDC, 2001

Arthur D Broadbent, Basic Principles of Textile Coloration, SDC, 2001


Conditions of Viewing

 The source under which the


comparison is made can be-
D65 - daylight

 The specimen should be


placed on a flat, uniform
surface having no
distortions.The surrounding
field shall be uniform grey.
Fastness to washing
There is a variety of testing procedures. To some extent, these have arisen because:
(1) washing conditions vary from one country to another;
(2) the method depends upon the use of the material being washed;
(3) to evaluate repeated washing, accelerated test methods are used.
The situation becomes even more complicated when one considers that the degree of fading of a dyeing on
washing depends upon the following factors, all of which must be standardised:
1) the temperature. This may range from 20 to as high as 95 °C;
(2) the type and amount of detergent that is added to the washing bath. This may or may not include alkalis,
phosphates, silicates, optical brightener, chlorine or peroxide bleach. In many testing procedures, a standard
detergent formulation is required;
(3) the extent of mechanical action. This can be varied by changing the agitation speed in a washing machine
or by adding steel ball bearings to the revolving test bath;
(4) the washing liquor-to-goods ratio and the hardness of the washing water;
(5) the rinsing, drying or pressing methods used to restore the sample after the test.

Arthur D Broadbent, Basic Principles of Textile Coloration, SDC, 2001


Sample Preparation
 Fabric is usually tested in the form of a composite specimen (at least 10cm X 4cm), made up of the test
specimen placed in contact with undyed fabric, usually in the form of multifibre strip, of the same size.
 There are two types of multifibre adjacent fabric, one with wool which is type DW and one without wool
which is type TV. The specification of each is given in
Washing Fastness Tests
 Domestic and commercial washing
conditions are covered by a number of
ISO wash tests, which are directed
towards simulation of the conditions
likely to be encountered in normal use.
The most commonly used of which is
ISO 105‐C06.

Fastness to washing C01-C06


BS EN 20105 Textiles.
Tests for colour fastness.

The conditions for the ISO test for colour fastness to


domestic washing and commercial laundering are given in
Table 24.4. These tests are carried out using a wash wheel
with a 5 g l–1 standard soap solution at a liquor ratio of 50:1.

Arthur D Broadbent, Basic Principles of Textile Coloration, SDC, 2001


Wash fastness testing
Colour fastness to Washing

Application:

This test evaluates the color fastness to laundering of


textiles which are expected to withstand frequent home or
commercial launderings.

The fabric color loss & surface changes resulting from


detergent solution & abrasive action of typical hand,
home or commercial laundering , is roughly
approximated.
General Method

The composite sample is made up of the coloured


material under test plus the undyed material made from
the same fibre, and material composed of another fibre,
as specified

Level 3-4 is acceptable for colour change, but should be 4


for staining.
Machine and Material used

 Laundering machine : Launder-


Ometer
 Stainless steel canister
 Stainless steel balls
 Teflon fluorocarbon gaskets
 Detergents
 Multifibre strip/ Cotton adjacent
fabric
 Scales for rating test results
Equipment - Launderometer
Procedure

 Cut the sample & multifibre as per the standard & stitch
them together along one shorter side

 Adjust the laundering machine to maintain the designated


bath temperature.

 Prepare detergent solution and add it to canister.

 Add stainless steel balls to canister and preheat the


canister to the test temperature.

 Add test specimen to canister.


Procedure

 Load canister in the machine and run the machine.


 Remove canister after test cycle is completed.
 Remove sample and rinse it with distilled water in separate
beakers.
 Remove the excess water from the specimen and dry in air or
oven.
ISO - WASH FASTNESS TESTS
Machine: Launder-O-meter
Liquor ratio: 50:1
Steel beaker: 550 ml volume

Test Method Abbreviatio Temperatu Additives Time Steel balls Drying


n re

WASH ISO 105/C01 400 C 5 g/l soap 30min - RT


FASTNESS 1
WASH ISO 105/C02 500 C 5 g/l soap 45 min - RT
FASTNESS 2
WASH ISO 105/C03 600 C 5 g/l soap, 30 min - RT
FASTNESS 3 2-g/l soda ash

WASH ISO 105/C04 950 C 5-g/l soap, 30 min 10 RT


FASTNESS 4 2-g/l soda ash

WASH ISO 105/C05 950 C 5-g/l soap, 4 hr 10 RT


FASTNESS 5 2-g/l soda ash
Colour fastness to light
 The evaluation of fastness to light exposure represents a special case,
since eight rather than the usual five graduations are used. Fading from
indoor light sources, which have negligible emission in the near
ultraviolet, is much less of a problem and testing of light fastness usually
refers to fastness to daylight or an equivalent artificial light source.
 The rate of fading on exposure of a dyeing is sensitive to the spectral
composition of the light from the source, especially the amount of
ultraviolet light present, and also to the temperature and humidity of the
air in contact with the samples. There are also problems with light
fastness being affected by the presence of any residual chemicals in the
fibre and by chemicals in the surrounding air.
 Humidity is another important factor, which shows its impact on fastness
grades because the test is performed over a considerable length of time.
Colour fastness to light
 Curtains, upholstery, carpets, awnings and coatings
LIGHT SOURCES
 The British Standard allows either daylight or xenon arc light to be used for the test.
 Daylight B0l
 To test the resistance of a material to fading in daylight a sample of it is exposed facing due
south (in the northern hemisphere), sloping at an angle from the horizontal which is
approximately equal to the test site latitude. The sample is covered with glass and provision is
made for it to be ventilated.
 Xenon arc B02
 The xenon arc is a much more intense source of light which has a very similar spectral content to
that of daylight so that the test is speeded up considerably. An efficient heat filter has to be
placed between the lamp and specimen and the temperature monitored. This is in addition to a
glass filter as above to remove ultra-violet radiation.
 Mercury-blended tungsten fluorescent lamp (MBTF)
 This is a source found in certain commercial light fastness testers. It provides a less intense light
(J. N. CHAKRABORTY, 2011) source than the xenon arc but will still give a faster test result than using daylight. One
advantage of it is that the bulbs are cheaper and last longer than do xenon ones.
 The shorter the wavelength of the selected light source, the higher the energy output and the
faster the rate of fading. To get more accurate information of light fastness grades, heat
developed on coloured samples is removed by a cooling attachment.
Reference standards
 There are eight blue wool reference standards. A rating is given to the sample which is the
number of the reference standard which shows a similar visual contrast between the exposed
and unexposed portions as the specimen. This means that the specimen will be given a grade
between one (poor light fastness) and eight (highly resistant to fading).
 Those used in Europe are identified by the numerical designation 1 to 8. They range from 1
(very low light fastness) to 8 (very high light fastness) so that each higher numbered
reference is approximately twice as fast as the preceding one. These eight blue woollen controls
are produced by dyeing scoured and bleached woollen fabric with blue dyes of known light fastness
graded in ascending order as C.I. Acid Blue 104, C.I. Acid Blue 109, C.I. Acid Blue 83, C.I. Acid Blue
121, C.I. Acid Blue 47, C.I. Acid Blue 23, C.I. Soluble Vat Blue 5 and C.I. Soluble Vat Blue 8
respectively.
 The blue wool references used in America are identified by the letter L followed by the
numerical designation 2 to 9. The two sets of references are not interchangeable. The
standard method for light fastness recommended by the AATCC involves eight blue wool
standards called ‘L2’ to ‘L9’. These eight standards consist of blue wool yarn dyed with CI
Mordant Blue 1 (Grade L2, very poor light fastness) or CI Solubilised Vat Blue 8 (Grade
L9, excellent fastness). The intermediate blue standards from L3 to L8 are mixtures of blue
yarns dyed with these two dyes, the higher grades having a greater proportion of the vat dyed
yarn so that each grade is about twice as fast as the previous one.
Arthur D Broadbent, Basic Principles of Textile Coloration, SDC, 2001
Blue wool Scale

Consist of eight pairs of wool strips dyed with different dyes having
different light fastness properties
Light Fastness Tester- Xenon Arc

Frame & rack


Some Important Machineries ……….

LAUNDER-O-METER : KSL 300 XENO TEST 150 S


XENOTEST 450
Some Important Machineries ……….

PERSPIRO METER THERMAPLATE: Colour fastness


to heat

RUBBING TESTER
Procedure of light fastness testing
 The samples (1 cm × 4.5 cm each) and blue wool standards are partly covered with a card or metal sheet
and simultaneously and continuously exposed to daylight under glass but allowing good ventilation. The
frame holding the samples faces due south in the northern hemisphere and is inclined at an angle to the
horizontal about equal to the latitude of the test location. The exposure is usually continued until the
tested and unexposed original samples show a colour contrast equivalent to Grade 4 on the Grey Scale
for colour loss. This is roughly the light fastness rating of the specimen. Part of the exposed portions of
the dyeings may then be covered and exposure continued until a colour contrast equivalent to grade 3 on
the Grey Scale is reached.
 For samples of very high light fastness, testing is stopped if the Grade 7 blue standard has faded to a
colour contrast of 4 before the sample exhibits obvious fading, in which case its fastness is graded as 8.
The light fastness of a dyed sample is the number of the blue wool standard that has faded to the same
extent as the exposed area of the sample. It is also common practice to evaluate the light fastness
relative to the blue wool standards for the condition of a just perceivable colour difference between the
exposed and original dyed samples. (Arthur D Broadbent, 2001)
 The specimen and the controls now have three clear zones, i.e. a completely shielded area in the middle,
a permanently exposed area at the right side of AB and a partially exposed area at the left; the zones are
compared with the control and if the two degrees of fading on the specimen do not correspond with the
control, the fastness should be the mean of the two. (M. Clark, 2011)
Arthur D Broadbent, Basic Principles of Textile Coloration, SDC, 2001
Sample for light fastness test. (Savile)
Assessment without woollen standards
 Light fastness can also be assessed without using blue woollen controls. Incident light on the specimen
generates heat, which needs to be removed from the light fastness tester to maintain test conditions, as
produced heat shows a synergistic effect enhancing fading. Generated heat is directly proportional to the
extent of fading which is added to the effect of incident light (ATIRA, 1996 ). If the temperature inside the
light fastness tester is maintained at 42±1°C (the sunlight temperature), the times required for the fading of
eight known 1–8 blue controls are 5–6, 10–12, 22–24, 75–80, 155–160, 250–270, 380–400 and beyond 400 h
respectively.
 If the temperature is 50 ± 1°C, these values are changed to 3–4, 5–6, 16–18, 50–55, 110–120, 200–210, 325–
350 and beyond 350 h respectively.
 If the temperature inside the light fastness tester differs from these temperatures, the same should be
calibrated using eight blue woollen controls. The timings are for a contrast on grey scale ‘change in colour’
three grade, when the test is terminated. However, the source of light must remain identical to maintain
fading with time.

(J. N. Chakraborty, 2011)


Photochromism
Some dyes change colour rapidly on exposure to a strong light but on being put
in the dark the original colour returns to a greater or less extent. This is known as
photochromism. To avoid any error due to this effect samples should be conditioned
for 24 h in the dark before assessment.

Change in hue
Certain dyed materials change hue on prolonged exposure to light, for instance
a yellow may become brown or a purple may become blue. The rating for colour
fastness concerns only change in contrast of the dyed material which in such cases
may not have altered. In such cases the change in hue is included as part of the
rating depending on the blue dyeing which has changed at the same time. A rating
of '5 bluer' would be used for a sample which changed from green to blue at the
same rate as the reference sample 5.
Color Fastness To Perspiration

 Purpose & Scope: This method is used to determine the fastness of colored textiles to the effects of
acid perspiration and / or alkaline solution.

 Principle: A specimen of colored textile in contact with other fiber materials is wet out in simulated
acid perspiration solution,subjected to a fixed mechanical pressure and temperature.The specimen is
evaluated for color change & staining.

 Equipments: AATCC Perspiration Tester,Perspirometer or equivalent device, Multifibre Test


fabric(0.8cm,unfused), Balance with weighing accuracy +/- 0.001 g, Wringer,Drying Oven, 9 Step
AATCC Chromatic Transference scale & Grey scale for staining, Grey scale for color change, Acid
Perspiration solution (for TM 15), pH meter , White AATCC Blotting paper,Acid perspiration
solution & Alkaline perspiration solution.
AATCC 15

 Fill a volumetric flask with 500ml distilled water


 Weigh the following & place in the flask to make 1L of solution with distilled water.
10 g Sodium Chloride ,1 g Lactic acid (USP 85%) ,1 g sodium
phosphate,dibasic,anhydrous,0.25g l-histidine monohydrochloride
 Measure pH with accurate pH meter (4.3 +/-0.2)
 Do not use perspiration solution more than 3 days old,fungus will begin to grow & the pH
will rise.
 Cut specimens & multifibre fabric (unfused) 6X6 +/-2 cm
 Sew or lay the Multifibre fabric to the test specimen
Procedure

Place specimen in a petridish (9 cm dia. & 2 cm deep)


 Add solution to a depth of 1.5cm
 Soak for 30 +/- 2 min(for perspiration) ,agitate & squeeze.
 Pass through the wringer to remove excess solution , weigh 2.25 +/- 0.05 times its dry weight.

 Place specimen between plexiglass plates with the multifiber stripes running perpendicular to the long
dimension of the plate.
 Place in a test unit. Insert all 21 plates regardless of the no. of specimens being tested.
 Place the 8 lb weight on top to give a total 10 lb pressure on the specimen.
Lock the specimen unit with a set screw,Remove the weight
Place the unit on its side in the oven (38+/-1 C),Time : 6 hrs +/-5 min
Remove the specimen from oven, separate the multifibre fabric, condition overnight & assess.
ISO 105-E04

 Preparation of Alkaline solution (per litre) :0.5 g L-histidine monohydrochloride

monohydrate , 5 g of Sodium chloride, 5 g of disodium hydrogen orthophosphate

dodecahydrate (pH = 8.0 ).

 Preparation of Acid solution (per litre): 0.5 g of L-histidine monohydrochloride

monohydrate , 5 g of sodium chloride, 2.2 g of sodium dihydrogen orthophosphate

dihydrate (pH = 5.5)


Rubbing fastness
 The problem arises mainly from the presence of superfi cial dyes, which may be due to
development of heavy shades, inadequate washing at the end of dyeing, formation of
few coloured molecules at the textile–air interface, water solubility of dyes or weak
dye–fibre attachment on the surface layer.

Weight

Rubbing peg

Rubbing area

Clamp

Crockmeter
“ A transfer of colorant from the surface of a coloured yarn or fabric to
another surface or adjacent area of the same fabric principally by
rubbing.”

International Standards

 AATCC 8
 ISO 105 X12

Machine and Material Used

 Motorized or manual crockmeter


 Crock cloth
 Distilled water, Blotting paper
 Grey Scales (Staining)
 Colour matching cabinet.
Standard Specifications
AATCC - 8
 Wet pick-up : 65% +/- 2% ,Specimen size atleast 50 x 130 mm
 Vertical Load : 9 N +/- 10% ,Finger Diameter : 16 +/- 0.3 mm
 Position long dimension oblique to warp and filling or wales and
courses.

ISO 105 X12


 Wet pick-up : 95 - 100%
 Specimen size atleast 50 x 140 mm
 Vertical Load - 9 +/- 0.2 N ,Finger Diameter - 16 mm
 Position warp parallel to long dimension for one specimen and weft
parallel to long dimension for other specimen or diagonally.
 Rubbing distance : 104 +/- 3mm
Procedure
 Prior to testing, condition the test sample and crocksquare in the
standard conditions for specified time.
Dry Rub :
Fasten each test specimen by means of clamps to the baseboard of the
testing device.
 When testing multicoloured sample, care should be taken to position
the specimen in such a way that all colours of design are rubbed in the
test.
Mount crocksquare on finger such that warp of crocksquare parallel
to direction of rubbing and loops of spiral clips to face upwards.
Lower finger to front end of the machine.
Turn crank handle 10 turns at a rate 1 turn/sec.
Procedure

Wet Rub :
To be performed on fresh specimen in consequence with dry
rub and with a rubbing cloth that has been wetted with water to
ensure required pickup.
After each test remove crock square from finger
Air dry the test specimen, then condition before evaluating.
In the case of napped, brushed or sanded material, remove
extraneous fibrous material by pressing lightly on the crock
circle with the sticky side of cellophane tape before evaluating,
As these loose fibres might interfere with the rating.
Evaluate the specimen using Gray scale for staining.
Potential Problems

Surface of crocking finger - leads to poor circular image

Loose clip - leads to double, elongated image

 Incorrect mounting of crock square - If mounted diagonally


leads to stretched and streaked image

Loops to wire clip positioned downward - Leads to scuff


marks

Wet pick-up not maintained - Can lead to difference in results


Fastness to Heat Treatments
Steam fastness under excess pressure
(ISO 105/P02)

 To determine the resistance of the colour of textiles to steam pleating.

 A composite sample made up of the coloured material sandwiched


between undyed cloths is mounted on a copper cylinder (copper tube,
8cm, 0.15 cm wall thickness with 6 layers of bleached cotton fabric
wound round it) and steamed inside either a jacketed steamer or a
domestic pressure cooker.

 Three steaming conditions are specified, ranging from 5 min at 135 kPa
(108°C) to 20 min at 270 kPa (130°C).

 Change in colour and staining are assessed using the Grey Scales.

 Release steam pressure (max. 2 min), dry in warm air at max. 60°C and
condition for 4 h at 20°C and 65% relative humidity.
Dry heat fastness (ISO 105/P01)

A sample of the textile in contact with specified undyed cloths is


heated using either an electrically heated precision press, or a molten
metal bath in which a holder containing the specimen is immersed.

 The change in colour and the staining of the undyed cloths are
assessed using the Grey Scales.

 Treat the test sample and adjacent fabrics for 30 s in a drying oven
under pressure of 4 kPa (40 kp/cm2) at one of the following
temperatures:
1500C
1800C
2100C

 Remove the test sample and hang for 4 h in a normal climate ( 200C,
65% relative humidity).
Hot pressing fastness (ISO 105/X11)

 To determine the resistance of the colour of textiles to ironing and to


processing on heated cylinders.

 A heating device of the type used in the dry-heat pleating test, e.g. a
precision heating press, is specified.

 Heat must be applied only to the upper side of the material, a sheet of
asbestos is placed between the composite sample and the bottom plate of
the press.

 The use of a hand iron is considered to be less satisfactory since


unavoidable temperature fluctuations limit the accuracy and reproducibility
of the test.

 When a hand iron is used, it must be stated in the report.


Temperatures: 110°C, 150°C, 200°C. Testing can also be carried out at other
temperatures.

Pressure : 4 kPa
Time : 15s

Dry: Place the dry test sample on dry cotton fabric and press with the
heated Plate.

Moist: Place the dry test sample on dry cotton fabric and on top a sample
of cotton fabric Soaked in demineralized water and squeezed to
100% pickup and press with the heated plate.

Wet : Soak the test sample and cotton fabric separately with
demineralized water and Squeeze to 100% pickup. Place the wet
test sample and the wet cotton fabric on Dry cotton fabric and
press with the heated plate.
Fastness to Dry Cleaning Using Perchloroethylene Solvent

Dry cleaning involves the use of an organic solvent rather than water. The solvent most used is
perchloroethylene (tetrachloroethylene) and this solvent is used in the standard test BS EN
ISO 105‐D01:2010.

The sample under test is attached to a piece of multifibre strip and the composite placed in a
cotton bag, together with twelve stainless steel discs. The bag is placed in a sealed container
containing perchloroethylene solvent. The container is rotated in a water bath at 40 rev/min, at
30 °C for 30 minutes. After this treatment the composite sample is removed from the bag in
the container, excess solvent removed and then the sample and multifibre strip dried. The
change in colour of the sample and staining of the multifibre strip is assessed using the grey
scales.
Fastness to Chlorinated Water (Swimming Pool Water)
The main issue in swimming pool water is the action of chlorine on the dyes used in swimwear. The
test BS EN ISO 105‐E03:2010 assesses the change in colour (using the grey scale for colour change
or instrumental colour measurement) when pieces of the sample are treated in three solutions of
sodium hypochlorite of 20, 50 and 100 mg active chlorine per litre, at pH 7.5.

The pieces of sample being tested are placed in sealed containers, one for each concentration of
sodium hypochlorite, which are rotated in a water bath in about 40 rev/min, at 27 °C for 1 hour. The
samples are then squeezed and dried before being assessed for colour change.

 Wet out the test sample in sodium hypochlorite solution


 liquor ratio 100:1
 Treat with:
- 20, mg/l available chlorine at 270C for 1h, pH 7.5
- 50 mg/l available chlorine at 270C for 1h, pH 7.5
- 100 mg/l available chlorine at 270C for 1h, pH 7.5
 Squeeze and hang to dry at room temperature .
Water fastness (M&S C6)

 Wet out the test sample and adjacent fabric with


Demineralized water

 MLR – 1:15

 cover with a glass plate of 50 g

 Leave it for 15 mins

 Keep in drying oven for 4 h at370C

 Dry in warm air at max. 600C .


Seawater fastness (ISO 105/E02)

 Wet out the test sample with 30 g/l sodium chloride solution
 Cover with a acrylic plastic plates under a pressure of 12.5 kPa
 Keep in drying oven for 4 h at 370C
 Dry in warm air at max. 600C .
Chlorinated water fastness
(M&S C12),(M&S C37)
 Wet out the test sample in sodium hypochlorite solution
 liquor ratio 100:1
 Treat with:
C12 - 20 mg/l available chlorine at 200Cfor 4 hr at pH 8.5
C37 - 100 mg/l available chlorine at 270C for 1 hr at pH 7.5
(id. E03)
 Squeeze and hang to dry at room temperature .

Hot water fastness (ISO 105/E08)

 Roll the test sample and adjacent fabrics round a glass rod
 Treat for 30 min at 700C in slightly acid water
 Liquor ratio 30:1
 Remove test sample from glass rod
 Squeeze and hang to dry in warm air at max. 600C.
 Hypochlorite bleach fastness (ISO 105/N01)
 Sodium chlorite bleach fastness: mild (ISO 105/N03)
 Sodium chlorite bleach fastness: severe (ISO 105/N04)
 Mercerizing fastness (ISO 105 /X04)
 Per borate fastness (M&S C10)
 Fastness to burnt gases
 Colour Fastness to Nitrogen Oxides (G01 : 1978)
 Formaldehyde fastness (ISO 105/X10)
 Domestic laundering 50- 60-950C (M&S C4A X0C)
Thank You

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