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