Wet Lab Manual

Laboratory Manual
Course no.: Tex 208

Course Title: Wet Processing- I Lab
2nd Year 2nd Semester
Department of Textile Engineering

Ahsanullah University of Science and Technology
Contents
General Practices and Safety Procedures in Wet Processing Laboratory …………………………………….……….1
I. Safety code for laboratories ……………………………………………………………………………….………..…….1
II. Accidents……………………………………………………………….……………………………………………………..…….1
III. Chemicals ………………………………………………………………………………………….…………………………..….1
Concentrated acids and alkalis ………………………………………………………………………………….…………….1
Flammable solvents ………………………………………………………………………… …….……………….……….…….1
Hazardous chemicals ………………………………………………………………………………………………………..…….1
General …………………………………………………………………………………………………………………………....…… 2
IV. Housekeeping ……………………………………….……………………………………………………………………..…… 2
V. Hygiene …………………………………………………………………………………….….……….……………………..…… 2
VI. Weights and volumes …………………….…………………………………….……….……………………………..…… 2
Weighing ………………………………………………………………………………………….……….……………………..…… 2
Volumetric measurement ………………………………………………………………………….……………………..…… 3
Effect of dye weighing errors …………………………………………………………………….……………………..…… 3
Effect of pipetting errors …………………………………………………………….….………………………………..…… 4
Effect of weight of specimen ………………………………………………….………………….……………………..…… 4
VII. Temperature ………………………………………….…………………………………………………………..………..…… 5
Measurement …………………………………………………………………………………………………………………..…… 5
Temperature control ……………………………………………………………………………………………….………..……5
Methods of Heating …………………………………………………………………………………………..……….……..……5
VII. pH Measurement ……………………………………………………………………………….………………………..… 6
Definition………………………………………………………………………………………………………………..…………..… 6
pH Indicators ………………………………………………………………………………………………………………..……..…7
Indicator papers …………………………………………………………………………………………………………………..…7
pH meters ……………………………………………………………………………………………………………………….…..…7
Measurement of pH using a pH meter ………………………………………………………………………………...…7
Measurement and adjustment of pH of dye liquor …………………………………………………………………8
Care of Electrodes ………………………………………………………………………………..………………………………..8
Literature Review ...........................................................................................................................10

1.1.1 Desizing ...................................................................................................................................10
1.1.2 Starch Desizing ........................................................................................................................10
1.1.3 Enzyme Steeping Method .......................................................................................................11
Standard Recipe .............................................................................................................................12
Recipe Calculation ..........................................................................................................................12
Working Procedure ........................................................................................................................13
Process curve .................................................................................................................................13
Assessment of Desizing Quality .....................................................................................................14
1.6.1 Test- 01: Calculation of weight loss in percentage .................................................................14
1.6.2 Test 02: Tegewa test (Iodine test) ..........................................................................................14
Functions of Chemicals ..................................................................................................................14
i
2.1.1 Scouring...................................................................................................................................15
2.1.2 Scouring of Cotton ..................................................................................................................15
Standard Recipe .............................................................................................................................16
Process curve .................................................................................................................................17
Assessment of Scouring Quality .....................................................................................................17
2.6.1 Test- 01: Calculation of weight loss in percentage .................................................................17
2.6.2 Test -02: Absorbency test (Drop/Spot test) ............................................................................18

3.1.1 Bleaching .................................................................................................................................20
3.1.2 Bleaching with Hydrogen Peroxide .........................................................................................21
Standard Recipe .............................................................................................................................22
Process curve .................................................................................................................................23
Assessment of Bleaching Quality ...................................................................................................24

4.1.1 Silk Degumming ......................................................................................................................25
Standard Recipe .............................................................................................................................26
Process curve .................................................................................................................................27
Assessment of Degumming Quality ...............................................................................................28
4.5.1 Test- 01: Visual Assessment ....................................................................................................28
4.5.2 Test -02: Calculation of weight loss in percentage .................................................................28
4.5.3 Test- 03: Absorbency test (Drop/Spot test) ............................................................................28
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5.1.1 Bleaching of Silk ......................................................................................................................30
Standard Recipe .............................................................................................................................31
Process curve .................................................................................................................................32
Assessment of Bleaching Quality ...................................................................................................33

6.1.1 Dyeing .....................................................................................................................................34
6.1.2 Direct Dyes ..............................................................................................................................34
6.1.3 Chemical structure ..................................................................................................................35
6.1.4 Mechanism of substantivity of direct dyes .............................................................................35
6.1.5 Properties ................................................................................................................................35
6.1.6 Effect of different variables ....................................................................................................36
6.1.7 Fastness properties .................................................................................................................36
Standard Recipe for Direct Dyeing .................................................................................................37
Preparation of Stock Dye Solutions ...............................................................................................37
Preparation of Laboratory Dye-Liquors .........................................................................................37
6.4.1 Calculation for Percentage Required ......................................................................................38
6.4.2 Calculation for g/l Required ....................................................................................................38
Process curve .................................................................................................................................39
Assessment of Dyeing Quality........................................................................................................40

7.1.1 Vat Dyeing ...............................................................................................................................41
7.1.2 Principles of application of vat dyes .......................................................................................42
Recipes and Procedures .................................................................................................................42
7.2.1 Step- 1: Vatting.......................................................................................................................42
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7.2.2 Step- 2: Dyeing .......................................................................................................................43
Process curve .................................................................................................................................43
7.3.1 Step- 3: Oxidation ...................................................................................................................44
7.3.2 Step- 4: After-treatment .........................................................................................................44

8.1.1 Silk Dyeing ...............................................................................................................................46
8.1.2 Mechanism of silk dyeing with acid dyes ................................................................................46
Standard Recipe and process parameters .....................................................................................47
Preparation of Stock Dye Solutions ...............................................................................................47
Preparation of Laboratory Dye-Liquors .........................................................................................47
Calculation .....................................................................................................................................48
Process curve .................................................................................................................................49
Functions of Chemicals ................................................................................................................50

9.1.1 Printing ....................................................................................................................................51
9.1.2 Difference between dyeing and printing ................................................................................51
9.1.3 Styles of printing .....................................................................................................................52
9.1.4 Steps of printing ......................................................................................................................52
9.1.5 The essential ingredients of a printing paste are selected from the following ......................52
Printing with Direct Dyes ...............................................................................................................53
Standard Recipe and process parameters .....................................................................................53
Preparation of Stock Paste of Thickener ........................................................................................53
Preparation of Laboratory Dye Paste.............................................................................................54
Assessment of Printing Quality ......................................................................................................54
iv
Literature Review .........................................................................................................................56
10.1.1 Printing ..................................................................................................................................56
10.1.2 Steps of printing ....................................................................................................................56
Printing with Acid Dyes ................................................................................................................56
Standard Recipe and process parameters ...................................................................................57
10.3.1 Preparation of Stock Paste of Thickener ...............................................................................57
10.3.2 Preparation of Laboratory Dye Paste....................................................................................57
Working Procedure ......................................................................................................................57
Assessment of Printing Quality ....................................................................................................58
Functions of Chemicals ................................................................................................................58
v
General Practices and Safety Procedures in
Wet Processing Laboratory
This article describes some of the principles and practices that are required in a dyeing
laboratory, such as general health and safety guidelines and other general good
housekeeping practices. It also looks at measuring weights and volumes and the problems
that can result from inaccuracies in these measurements.
I. Safety code for laboratories

In all places of work, but especially in a laboratory, it is important that each individual ensures
that he/she works safely so as not to endanger themselves or their colleagues. The
responsibility that each individual is aware of the best practices in the area that they work in
surely rests with the employer and the environment of a laboratory makes this especially
important.
II. Accidents
There should be a recognised first aider in all places of work on all shifts and they should be
known to all. If an accident does occur, no matter how small, this should be recorded and
reported to the laboratory manager. This will allow for an assessment of the accidents and if a
trend appears this can be acted upon.
III. Chemicals
i) Concentrated acids and alkalis

 Protective gloves and eye protection should be worn.
 Never pipette by mouth – always use a pipette filler.
 Always add acid or alkali to water while stirring the water, never add water to acid or
alkali.
 Bottles of concentrated acid or alkali (fuming) should be opened in an extraction fume
cupboard.
 Store concentrated acids and alkalis separately.
ii) Flammable solvents

 Do not use near a naked flame.
 Solvents with a boiling point below 80 °C must not be heated directly: use a water
bath.
 Ideally, all flammable solvents should be stored in a special solvents cupboard.
iii) Hazardous chemicals

 An experienced colleague should be made aware that a hazardous chemical is about
to be used to ensure good practice is followed and the nature of the hazard should be
shared with anyone working close by.
 Avoid skin contact by using appropriate protective equipment and use a fume
cupboard if necessary.
Tex 208: Wet Processing-I Lab Manual

Department of Textile Engineering, AUST
1
iv) General
 Avoid inhaling vapours or dust. If in doubt, wear a face mask or use a fume cupboard.
 Never pipette liquids or solutions by mouth
 Avoid skin contact: wash off any accidental contact with cold water.
 Do not lift or carry bottles by the neck, use two hands with one being the support
underneath.
 Always carry chemicals in a suitable closed container.
IV. Housekeeping
 Keep all laboratories tidy at all times. Do not leave apparatus in sinks or on the floor.
Workbenches should be uncluttered and clean.
 Make sure all containers are correctly labelled. Anything in an unlabelled container
should be disposed of safely.
 Clear up all spillages at once even if it is just a small spill down the side of the bottle.
 Do not throw chemicals down the sink unless you know it is safe to do so.
 For cleaning apparatus use available detergents.
V. Hygiene
 After handling chemicals, wash your hands before eating, drinking smoking or going to
the toilet.
 Do not smoke, drink or eat in the laboratory.
 Use appropriate protective clothing. Always fasten clothing as loose clothing can
cause accidents.
 Do not rush in a laboratory.
VI. Weights and volumes

It is important that volume or weight is measured to the appropriate degree of accuracy.
i) Weighing
Weighing is the means of measuring out a quantity of material (usually a solid), e.g. for
making up known concentration solutions or dispersions.
Units of weight are:
 Gram g (1 g = 1000 mg)

 Kilogram kg (1 kg = 1000 g)
It is essential to use calibrated balances to ensure that accuracy is maintained.

2
ii) Volumetric measurement
As with weight, volume is a means of measuring out a quantity of material (usually a liquid),
e.g. for making up known concentration solutions or dispersions or for making dyebath
additions.
Units of volume are:
Microlitre (l)
Millilitre ml or cm3 (1 ml = 1 cm3 = 1000l)
Litre L or dm (1 L = 1 dm3 = 1000 ml)
There is a variety of equipment available for volume measurement and the type used is
determined by the accuracy required.
iii) Effect of dye weighing errors
For a 0.4% stock solution or dispersion, 100 ml is normally prepared, i.e. 0.4 g in 100 ml or 2.0
g in 500 ml.
e.g. If 2.0 g was weighed out correctly for a 2% shade on a 4 g specimen:
% depth x weight of specimen

ml required =
% of stock or dispersion
2.0 × 4.0
=
0.4
= 20.0 ml
If 1.9g was weighed out, the dye dispersion would only be 0.38%
x% × 4.0
20.0 ml pipetted out =
0.38
= % applied = 𝟏. 𝟗%
If 2.1g was weighed out, the dye dispersion would be 0.42%.
x% × 4.0
20.0 ml pipetted out =
0.42
= % applied = 2.1%
The total variance in depth of shade applied could be as much as 10% which is well above the
acceptable accuracy level.
The weighing of 2.0 g dye needs to be within ± 0.020 g for acceptability.

3
iv) Effect of pipetting errors
Assuming that a 2.0% depth of shade is required on a 4 g specimen using a 0.4% dye stock
solution or dispersion: i.e.
2.0 × 4.0
0.4
= 20.0 ml of dispersion
If 20.1 ml is pipetted, the effective amount of dye used becomes:
20.1 × 2.0
= 2.01%
20.0
If 19.9ml pipetted, the effective amount of dye used becomes:

19.9 × 2.0
= 1.99%
20.0
The total variance in depth of shade applied could be as much as 1%, which is within the
limits of accuracy, but an error greater than this would be borderline.
v) Effect of weight of specimen
Assuming that a 2.0% depth of shade is required on a 4.0 g specimen, if a 3.9 g pattern is
used, the effective amount of dye used becomes:
2.0 × 4.0
= 2.05
3.9
If a 4.1 g pattern is used, the effective amount of dye used becomes
2.0 × 4.0
= 1.95
4.1
A total variance of 5% is possible from variations in weighing.
The weighing of 4.0 g patterns needs to be within ± 0.05 g for acceptability.
Thus, the weighing of dye and specimens is much more critical than pipetting, but it is
important to remember that errors in all three areas will contribute to unreproducible results.
All this occurs before we even start to consider errors introduced by variations in the dyeing
process, e.g. temperature, pH, liquor-to-goods ratio etc.

4
VIII. Temperature
i) Measurement
During many preparatory, dyeing and finishing processes, temperature control is important.
For example
 scouring is carried out at 70 °C

 dyeing is carried out at 100–130 °C
 reduction-clearing is carried out at 70 °C
Temperature measurement in °C is carried out using either
a. a ‘mercury in glass’ thermometer.

b. an electronic thermometer
A thermometer is a delicate instrument and should never be used as a stirrer. The

thermometers typically in use in a dyeing laboratory are in the range 10–100 °C or 10–250 °C.
It is a good idea to have all thermometers calibrated before use.
Warning: if you break a thermometer, seek advice on cleaning up the mercury as it is

hazardous to breathe the vapour.
ii) Temperature control

Good temperature control is important when carrying out preparatory, dyeing or finishing
processes.
In an effort to provide accurate control of temperature, the following points should be noted:
 remove or reduce the heat supply to the equipment 5–10 °C before the desired
temperature is reached. This will help to prevent over-shooting.
 keep a check on the temperature once the required temperature has been reached,
making adjustments to the heat supply as necessary to maintain the required
temperature.
 if the equipment is being heated indirectly e.g. in a water bath, it is usually necessary
to heat the heating medium (in this case, the water) to a few degrees higher than the
required temperature in order to allow for the temperature difference between the
hearing medium and the liquor being heated.
iii) Methods of Heating

Heating methods can be divided into two types:
Indirect: for example water baths. The water acts as a medium by which the heat is
transferred from the heat source to the vessel to be heated. The heat sources can be gas (e.g.
in a Bunsen burner) although water baths may be heated electrically and thermostatically
controlled and this would be the preferred method.
Indirect heating provides advantages over direct methods as it is safer and provides a more
accurate temperature control.

5
Direct: for example, Bunsen burners, gas rings, hot plates. With this type of heating, the heat
source is in direct contact with the vessel to be heated. Bunsen burners and gas rings are
prone to causing localised over-heating.
When in use, the Bunsen or gas ring should be placed on an asbestos sheet.
It is considered best practice to use a hotplate in preference to a gas flame.
Warning: a fully aerated Bunsen flame is invisible in sunlight. To avoid accidents, an orange
flame should be used when the Bunsen is not in use for a short period of time. For any longer
periods of time, the Bunsen should be shut off.
IX. pH Measurement
Definition
pH is a measure of the acidity or alkalinity of a solution and is expressed on a logarithmic
scale of 0 to 14.
pH Acidity/Alkalinity
The acidity of a solution depends upon the concentration of hydrogen icons (H +, protons) in
the solution. The pH is given by the equation:
pH = -log [H+] , H+ = Hydrogen ion concentration
In strong acid solutions where the concentration of hydrogen ions is high, the pH value is low.
As the concentration of hydrogen ions decreases, the acidity decreases and the pH value
increases. In strong alkaline solutions, the hydrogen ion concentration is very low and the pH
is therefore high.

6
pH control is important, particularly in dyeing. Certain dyes, for example disperse dyes,
require a weakly acidic dyebath of pH 4–5 for dyeing to occur, whereas reactive dyes are
applied from a bath of pH 9–10.
The pH of each dye liquor should be checked and adjusted to the required pH using the
appropriate reagent (as shown in Table 1) before the fabric to be dyed is added.
pH Indicators
pH indicators are soluble organic colouring matters which show a change in colour when the
pH of the solution in which they are dissolved is altered. Different indicators change colour
over different portions of the pH scale so it is possible to select a series of indicators to cover
the whole pH scale. Universal indicators are solutions of a number of indicators each showing
a colour change over a different portion of the pH scale from pH 3–10 with colour changes
from red at low pH, to orange, yellow and green, to blue at high pH. Examples of available pH
indicators are given in Table 2.
Indicator papers
These are produced by soaking filter paper in indicator solutions and then allowing it to dry.
The papers are usually prepared in the form of a book or reel. To measure the pH of a
solution, a small drop of the solution is placed on the paper and the colour produced is
compared with the chart on the book or reel cover. The pH is then read off the chart.
pH meters
The use of a pH meter provides a more accurate measure of pH. The pH meter depends on
the fact that when suitable electrodes are placed in a solution charged particles will flow from
one electrode to the other to produce an electro-motive force (EMF). The pH meter amplifies
and measures the EMF produced. The pH of the solution is a linear function of the EMF
produced.
Measurement of pH using a pH meter

To measure the pH of a solution, carry out the following steps:
i) Accuracy Check
This should be carried out if you are the first person to use the pH meter on a particular day:
a) Pour a small quantity of pH 4.0 buffer solution into a clean beaker.
b) Immerse the electrode and temperature probe in the beaker and shake briefly.
c) Check that the pH reading is within the tolerance set by the manufacturer. In a dyehouse
laboratory this should be at least ± 0.2 pH units of the buffer solution.
d) If the reading is out of tolerance, the pH meter should not be used until it has been fully
calibrated.
[ N.B. Refer to handbook for the particular meter in use for details of calibration method.]
e) If the reading is within tolerance, remove the electrode and temperature probe and rinse
in cold distilled or deionised water, unless the instructions supplied with the electrode state
use buffer solution.

7
ii) Measurement and adjustment of pH of dye liquor
a) Pour the dye liquor into a glass beaker.
b) Immerse the electrode and temperature probe in the dye liquor and agitate slightly.
c) Add a few drops of the required reagent (i.e. acid or alkali) agitating after each addition,
until the required pH is reached.
d) Remove the electrode and temperature probe and rinse in cold distilled or deionised
water.
e) Return dye liquor to dyeing vessel and rinse out beaker.
f) Repeat steps (a) to (e) for all other dye liquors.
g) After use, place the electrode and temperature probe into a beaker of distilled or deionised
water, unless the instructions supplied with the electrode state use buffer solution.
Care of Electrodes
i) The electrode should be kept immersed in clean distilled or deionised water between
measurements. Best practice is to prepare distilled or de-ionised water of grade 3
purity on site to ensure its quality.
ii) Avoid handling the pH sensitive membrane, any damage to its surface caused by
abrasion will lead to inaccuracy and slow response.
iii) Always clean the electrode in cold distilled or deionised water after each use.
Table-1: Suitable reagents for pH adjustments

8
Table- 2: pH ranges of some common indicators

9
Name of the Experiment: Enzymatic desizing of grey cotton fabric.
Literature Review
1.1.1 Desizing
The yarns, particularly the warps running lengthways throughout the fabric, are subjected to a
high degree of abrasion during weaving. To prevent breakage or damage of warp yarns due to
abrasion, size is imparted to the warp yarn. The presence of size on the fabric makes it stiff and
renders its treatment with different liquors used in dyeing and finishing difficult. Therefore,
one of the initial steps in wet processing is the elimination of size and water-soluble
admixtures, the operation being called desizing.
The typical sizing materials are:

 Natural starches from potatoes, maize, rice or topioca.
 Chemically modified starches (ethers or esters).
 Organic polymers e.g. polyacrylates, carboxymethylcellulose, methylcelluose,
polyesters or polyvinylalcohol.
 Solvent-soluble materials e.g. copolymers of methyl methacrylate.
1.1.2 Starch Desizing

About 75% of the sizing agents used throughout the world consists of starch and its derivatives
because of low cost and high effectiveness as a sizing material on cellulosic textiles. Starch is
difficult to remove, as it is not soluble in water or in normal scouring liquor. Removal of starch
before scouring minimises the work required in subsequent cleaning processes, hence reduced
concentrations of the chemicals are required in subsequent scouring and bleaching processes.
Chemically starch is a poly-α-glucopyranose in which straight chain amylose and branched
chain amylopectin polymers are present. Both the constituents are insoluble in water, but can
be solubilised by hydrolysis of these long chain compounds into shorter ones. Under
favourable conditions, starch can be progressively hydrolysed to the following products with
varying solubility in water: Starch (insoluble) → dextrin (insoluble) → dextrin (soluble) →
maltose (soluble) → α-glucose (soluble). In desizing, the hydrolysis reaction is carried out up
to the stage of soluble dextrin only and not up to the stage of α-glucose to avoid degradation of
cellulose.
Figure: Structures of amylase and amylopectin

10
Starch desizing methods can be classified as follows:
1. Hydrolytic methods
I. Rot steeping
II. Acid steeping
III. Enzyme steeping
2. Oxidative methods
I. Chlorine desizing
II. Chlorite desizing
III. Bromite desizing
IV. Peroxy compounds
1.1.3 Enzyme Steeping Method

The word enzyme is from Greek words for 'in yeast' and was coined in 1876 by the German
biochemist Willey Kuhne. Enzymes are organic biocatalysts highly specific both in the
reaction catalysed and their choice of reactants (substrate). Physically enzymes are colloidal
nature and chemically they are of the nature of protein. Enzymes are complex and have high
molecular weights. Today enzymes are produced by biotechnological processes in great
amount of constant quality, and are therefore applicable to large-scale processes. Advances in
the field Desizing of genetic engineering allow enzyme manufacturers to design specific
enzymes for specific processes (with regard to temperature stability or an optimum pH, for
example).
Desizing by enzymes is the safest method. Starch-degrading enzymes, which may be classified
according to their source of occurrence, are as follows:
1. Enzymes from animal sources such as slaughterhouse waste – clotted blood, pancreas,
liver, etc.
2. Enzymes from vegetable sources
I. Malt extract
II. Bacterial
The main enzymatic development within starch desizing has so far been the introduction of
amylase products (Diastafor) optimised to different temperature ranges. Malt amylases fall into
two categories and are named α (alpha) and β (beta) species which are found to be present in
the ratio of 1:5 to 1:6. α-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. β-amylase attacks straight chains, cleaves the units
and produces maltose, so that molecular chain of starch is shortened gradually. When an (α-
amylase is applied to a starch solution, it is found that viscosity of the solution decreases
rapidly, but for β-amylase the viscosity drops slowly. Thus it is clear that the proportion of α
and β-amylases in a desizing mixture determines the period (time) of effective desizing. It is
also clear that the molecular structure of cotton is unaffected by amylases.

11
Table: Optimum Conditions for Enzyme Desizing
Enzyme Types pH Temp (°C) Concentration (g/L)
Malt Extract 4.5-5.5 55-65 3-20
Pancreatic 6.5-7.5 40-55 1-3
Bacterial 6.5-7.5 65-75 0.5-1
Bacterial (Thermostable) 7-8 100-120 0.5-1
Standard Recipe
Chemicals/parameters Quantity (g/L)
Wetting Agent (Non-ionic) 1
Sequestering Agent 1
Enzyme 1-3
Salt 5
Temperature 900C
pH 6.5
Time 30 min
M:L Ratio 1:50
Recipe Calculation
Fabric weight = X g
Quantity of liquor = X * 50 = Z mL
Quantity of chemicals:
 Wetting agent 1g/L
1 L or 1000 mL of liquor contains 1 g of wetting agent
1∗Z
Z mL of liquor contains 1000 g of wetting agent
 Sequestering agent 1g/L
1 L or 1000 mL of liquor contains 1 g of sequestering agent
1∗Z
Z mL of liquor contains 1000 g of sequestering agent
 Enzyme 1g/L
1 L or 1000 mL of liquor contains 1 g of enzyme
1∗Z
Z mL of liquor contains 1000 g of enzyme
 Salt 5g/L
1 L or 1000 mL of liquor contains 5 g of salt
5∗Z
Z mL of liquor contains 1000 g of salt
Quantity of water = Quantity of liquor – (Quantity of Wetting agent + Sequestering agent +
Enzyme)

12
Working Procedure
1. Take weight of the given grey fabric on a weighing balance.
2. Using the liquor ratio, calculate the liquor required.
3. Calculate the amount of chemicals and required quantity of water according to the
recipe given to each group.
4. Prepare the desizing bath at room temperature with the appropriate quantity of water.
5. Add fabric and all the chemicals in accordance to the process diagram with constant
stirring.
6. Before adding the enzyme check and adjust the pH and then raise the temperature to
90°C and continue for 30 minutes.
7. Wash the fabric with cold water and hot water with 2 g/L detergent for 5 minutes at the
boil.
8. Dry the fabric using a hand dryer and test for desizing quality.
Process curve
Temperature rise up
Time 30 Min
to 90°C
Drain
Salt
Solution Hot wash with
5’ 5’ 5’ 2 g/L detergent
Room
at boil
temperature
Water pH Enzyme Cold wash

+ Check
Wetting agent
+ Drying
Sequestering
agent
Assessment
+
Fabric
Figure: Process Curve of cotton fabric desizing with enzyme.

13
Assessment of Desizing Quality
 Test 01. Calculation of weight loss in percentage

 Test 02. Tegewa test (Iodine test)
1.6.1 Test- 01: Calculation of weight loss in percentage

As cotton fabric contains approximately 10 to 14% sizing materials specially starch so loss in
fabric weight after desizing indicates the removal of starch. The weight loss is expressed as a
percentage and which can be calculated by the following formula.
Weight before desizing − Weight after desizing

Weight Loss (%) = × 100
Weight before desizing
Acceptable range is 10-14 %. Sometimes 9% is acceptable as well. Less than 9% means the
fabric is not well desized (unacceptable). Weight loss% higher than 14% indicates damage to
cotton fibers instead of starch removal which is unacceptable.
1.6.2 Test 02: Tegewa test (Iodine test)
Preparation of Tegewa or Iodine Solution: Dissolve 1.3 g Iodine and 2.6 g Potassium
Iodide (KI) with 200 mL of ethyl alcohol in a beaker and shake well for complete dissolution.
Then add distilled water to make a 1000 mL solution.
Application: Drop the prepared iodine solution onto the desized fabric and compare the color
with the Tegewa scale range from 1-9.
Functions of Chemicals
 Wetting agent: Used to facilitate the penetration of the liquor containing enzyme into the
size film by reducing the surface tension of water resulting in uniform desizing. Some
wetting agents (mostly anionic) reduce thermal stability of the enzyme. Nonionic
surfactants are comparatively safer.
 Sequestering agent: Used to deactivate the metallic ions present in the solution otherwise
the metallic ions may reduce the activity of enzymes.
 Enzyme: amylases types of enzymes are used which capable of hydrolyzing starch
molecules present in the sizing preparation, transform starch to dextrins, breaking them
down to soluble sugars thus helping in desizing.
 Salt: Certain compounds like sodium and calcium salts (mostly chlorides) added to
amylase solutions to improve its thermal resistance as well as solubility.

14
Name of the Experiment: Scouring of Desized cotton fabric.
Literature Review
2.1.1 Scouring
Scouring is the most important wet process applied to textile materials before dyeing or
printing. It is mostly a cleaning process in which the foreign maters or impurities are removed.
Precisely scouring is a purifying treatment of textiles. The objective of scouring is to reduce
the amount of impurities sufficiently to obtain level and reproducible results in dyeing and
finishing operations.
2.1.2 Scouring of Cotton

The loom state cotton fabric contains about 8-12% natural impurities of total weight of the
fibre. These impurities mainly consist of waxes, proteins, pectic substances and mineral
matters. In addition to this, the mechanically held impurities called ‘motes’ are present
containing seed-coat fragments, aborted seeds and leave etc. that clinge to the fibre. Apart from
these, the loom-state fabric is also contaminated with adventitious oils such as machine oils,
tars, greases etc. When the impurities are removed, the cotton becomes absorbent. In fact, the
success of a scouring process is judged by the improvement in wettability of the scoured
material. More specifically cotton scouring is done in order to remove unwanted oils, fats,
waxes, soluble impurities and any particulate or solid dirt adhering to the fibres, which
otherwise hamper dyeing, printing and finishing processes.
The process essentially consists of treatment with soap or detergent with or without addition
of alkali. Depending on the fibre type, alkali may be weak (e.g. soda ash) or strong (caustic
soda).
Since natural impurities such as wax, pectic substances and protein are associated mainly with
the cell wall within the primary wall, the scouring process aims to remove this wall. The
changes caused by the treatment with boiling alkali have been summarized as follows:
 Hemicelluloses as well as cellulose fractions with a low DP are dissolved.

 Saponifiable oils and fats are converted into soap.
 Unsaponifiable oils and waxes are melted at the scouring temperature and are
emulsified by the soap formed during saponification.
 Pectins and pectoses are converted into soluble salts of pectic acid and metapectic acid.
 Proteins are hydrolysed with the formation of soluble sodium salts of amino acids or
ammonia.
 Water-soluble mineral substances are dissolved.
 Insoluble dirt is removed and retained in suspension.
 Sizing and other added impurities, if present, are broken into soluble products.

15
Standard Recipe
Chemicals/ Parameters Quantity (g/L)

Scouring Agent (NaOH) 1
Detergent 1
Temperature Boiling
pH 10.5-11.5
Time 45 min
M:L Ratio 1:50
Recipe Calculation
Fabric weight = X g
1∗Z
1∗Z
 Sodium Hydroxide 1g/L
1 L or 1000 mL of liquor contains 1 g of sodium hydroxide
1∗Z
Z mL of liquor contains 1000 g of sodium hydroxide
 Detergent 1g/L
1 L or 1000 mL of liquor contains 15 g of detergent
1∗Z
Z mL of liquor contains 1000 g of detergent

Detergent)
Working Procedure
1. Take initial weight of the desized fabric on a weighing balance.


16
4. Prepare the scouring bath at room temperature with the appropriate quantity of water.
stirring.
6. Check and adjust the pH and then raise the temperature to the boiling and continue for
45 minutes with constant stirring.
boil.
8. Dry the fabric using a hand dryer and test for scouring quality.
Process curve
Temperature rise up
Time 45 Min
to the boil
Drain
NaOH &
Detergent Hot wash with
5’ 2 g/L detergent
Room 5’
at boil
temperature
Water pH Cold wash

+ Check
Wetting agent
+ Drying
Sequestering
agent
Assessment
+
Fabric
Figure: Process Curve of cotton fabric scouring with alkali.
Assessment of Scouring Quality
 Test 01. Calculation of weight loss in percentage

 Test 02. Absorbency test (Drop/Spot test)
2.6.1 Test- 01: Calculation of weight loss in percentage

As raw cotton fibre contains approximately 8% impurities so loss in fabric weight after
scouring indicates the removal of impurities. The weight loss is expressed as a percentage.

17
𝐖𝐞𝐢𝐠𝐡𝐭 𝐛𝐞𝐟𝐨𝐫𝐞 𝐬𝐜𝐨𝐮𝐫𝐢𝐧𝐠 − 𝐖𝐞𝐢𝐠𝐡𝐭 𝐚𝐟𝐭𝐞𝐫 𝐬𝐜𝐨𝐮𝐫𝐢𝐧𝐠
𝐖𝐞𝐢𝐠𝐡𝐭 𝐋𝐨𝐬𝐬 (%) = × 𝟏𝟎𝟎
𝐖𝐞𝐢𝐠𝐡𝐭 𝐛𝐞𝐟𝐨𝐫𝐞 𝐬𝐜𝐨𝐮𝐫𝐢𝐧𝐠
Acceptable range is 4-8 %. Sometimes 9% is acceptable as well. Less than 4% means the
fabric is not well scoured (unacceptable). Weight loss% higher than 8 – 9% indicates damage
to cotton fibers instead of impurity removal which is unacceptable
2.6.2 Test -02: Absorbency test (Drop/Spot test)

This method was designed to measure the water absorbency of textiles by the time required for
the specular reflection of the water drop to disappear is measured and recorded as wetting time.
0.1% direct red (congo red) dye solution was prepared and also dropped at the different places
of the fabric and the shape of the absorption area on the fabric was observed.
Procedure: For the drop test, the sample was placed over the top of a beaker so that the center
is unsupported. In a pipette a solution of 0.1% direct red is taken and dropped on the
unsupported part of the fabric. Then the absorption of the colored drop is observed visually.
 Wetting Time: It is the time required to absorb the water droplets completely by the
sample. Longer the time, lower the absorbency. Standard time for absorption of the
drop should be 0.5 – 0.8 second. Although less than 1 second is acceptable.
 Shape: In addition the scouring efficiency was also evaluated by assessing the
uniformity of scouring from the shape of the absorbed area on the fabric.
Table: Visual Evaluation Parameters of Drop/Spot Test

Visual assessment Drop shape Comment
The drop spot is circular but The scouring is even but
spreading over less area. incomplete.
The drop spot is circular and Scouring is even and
spreading over large area. complete.
The drop spot size is irregular in

Uneven scouring.
shape
 Wetting agent: Generally interracial tension between the textile fibre and the liquor is high,
and hence wetting of the fibre surface does not take place quickly. This is particularly true
in the case of grey cotton fabric and hydrophobic fibres. One of the main functions of the
surfactants is to reduce the surface tension of water and thereby bring about wetting of the
fabric resulting in uniform scouring.
the metallic ions may react with the scouring agent.
18
 Sodium Hydroxide: Sodium Hydroxide commercially known as caustic soda appears to be
the best scouring agent as it saponifies oils and fats to soluble soap, emulsifies waxes,
hydrolyses protein and eliminates pectin.
 Detergent: The function of the detergent is to remove the dirt and dust particles and other
constituents of the size such as china clay from the cotton fabric. The detergent keeps the
soils in dispersed or suspended form in scouring solution and prevents re-deposition on the
fabric. It also acts as an emulsifier.

19
Name of the Experiment: Bleaching of Scoured Cotton Fabric with
Hydrogen Peroxide.
Literature Review
3.1.1 Bleaching
The natural fibre and fabrics even after scouring still contain naturally occurring colouring
matter. This yellowish and brown discolouration may be related to flavones pigments of the
cotton flower. The climate, soil, drought and frost can also cause various degrees of
yellowness. Tips of leaves or stalks coming in contact with the moist ball after opening will
cause dark spots and discolouration. Discolouration may also come from dirt, dust, and insects
or from harvesting or processing equipment in the form of oils and greases.
The object of bleaching is to produce white fabrics by destroying the colouring matter with the
help of bleaching agents with minimum degradation of the fibre. The bleaching agents either
oxidize or reduce the colouring matter which is washed out and whiteness thus obtained is of
permanent nature. Chemical bleaching of textile fibres is further aided by addition of optical
brighteners.
Almost invariably the oxidizing agents give a more permanent white. When the color is acted
upon by a reducing agent, there is always the possibility that the oxygen in the air may re-
oxidize it to its original state. The natural color is only present in very small amounts and its
chemical nature is not known. For the production of high quality fabrics and for those that will
be dyed in pale or a medium, bright shade, bleaching is essential. It is not necessary for dull or
dark shade provided the fabric is already of adequate and uniform absorbency.
A general classification of bleaching agents is shown below:
Figure: Classification of bleaching agents

20
3.1.2 Bleaching with Hydrogen Peroxide
Hydrogen peroxide was discovered in 1818 and its use in bleaching textiles was first suggested
in 1866. However, its high cost limited its use in cotton bleaching until 1935. The problem was
partially solved by the process using barium peroxide and phosphoric acid. In 1926 hydrogen
peroxide was manufactured by an electrolytic process based on the decomposition of
persulphuric acid (H2SO5).
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 stabilize 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.
2H2O2 → 2H2O + O2
Advantages of hydrogen peroxide bleaching

 Hydrogen peroxide is a universal bleaching agent and can be used for bleaching cotton,
silk, wool, jute etc. (hypochlorites should not be used for bleaching protein fibres).
 There is less manipulation of the fabric in peroxide bleaching so that the labor cost
involved is less, even though the chemical cost may be higher.
 The loss suffered by the fabric during peroxide bleaching is less than in the case of
hypochlorite bleaching.
 Less water is required in peroxide bleaching.
 There is no necessity for scouring as in the case of hypochlorite bleaching.
 Superior fastness can be achieved in finished products bleached with hydrogen
peroxide (knitted goods and towels).
 Goods bleached with hydrogen peroxide are more absorbent than hypochlorite bleached
goods.
 Peroxide bleaching is much safer from the point of chemical degradation of cotton
during bleaching.
 There is less tendency of after yellowing of white goods bleached with hydrogen
peroxide than with hypochlorite.
Mechanism of peroxide bleaching

Though hydrogen peroxide is stable in acidic medium, but bleaching occurs by the addition of
alkali or by increased temperature. Hydrogen peroxide liberates per-hydroxyl ion (HO2-) in
aqueous medium and chemically behaves like a weak dibasic acid. The per-hydroxyl ion is
highly unstable and in the presence of oxidisable substance (coloured impurities in cotton), it is
decomposed and thus bleaching action takes place. Sodium hydroxide activates hydrogen
peroxide because H+ ion is neutralized by alkali which is favourable for liberation of HO2-.
H202 → H+ + HO2-
H2O2 → H+ + HO2- OH-

HO2- + H2O

21
However, at higher pH (above 10.8) the liberation of HO2- ion is so rapid that it becomes
unstable with the formation of oxygen gas which has no bleaching property. If the rate of
decomposition is very high, the unutilized 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 per-hydroxyl ion
is equal to the rate of consumption (for bleaching). At higher pH, hydrogen peroxide is not
stable and hence a stabilizer is frequently added in the bleaching bath.
Stabilizers for peroxide bleaching

The process of regulation or control of per-hydroxyl ion to prevent rapid decomposition of
bleach and to minimize fibre degradation is described as stabilization. Stabilizers for peroxide
normally function by controlling the formation of free radicals. These are compex blends of a
selection of materials serving a number of functions.
Sodium silicate is the most conventional, easily available and widely used stabilizer. Sodium
silicate, however, has a greater stabilizing action in the presence of calcium and magnesium
salts so that water with hardness between 2° and 5° is recommended or, if water of zero
hardness be used, 0.06 g/1 magnesium sulphate may be added.
Standard Recipe
Hydrogen Peroxide (50%) 2-5
Sodium Hydroxide 1
Sodium Silicate (Stabilizer) 1/3 of H2O2
Temperature Boiling
pH 10.5-11.5
Time 45 min
M:L Ratio 1:50
Recipe Calculation
Fabric weight = X g
1∗Z
1∗Z
 Sodium Hydroxide 1g/L
22
1∗Z
Z mL of liquor contains g of sodium hydroxide
1000
 Hydrogen Peroxide 2 g/L
1 L or 1000 mL of liquor contains 2 g of hydrogen peroxide
2∗Z
Z mL of liquor contains 1000 g of hydrogen peroxide
 Sodium Silicate 1/3 of hydrogen peroxide
hydrogen peroxide)
Working Procedure
1. Take initial weight of the scoured fabric on a weighing balance.
4. Prepare the bleaching bath at room temperature with the appropriate quantity of water.
stirring.
6. Check and adjust the pH and then raise the temperature to 60 °C.
7. Add hydrogen peroxide and again rise the temperature to the boil and continue for 45
minutes with constant stirring.
boil.
9. Dry the fabric using a hand dryer and test for bleaching quality.
Process curve
Temperature rise
up to the boil Time 45 Min
Drain
NaOH & 60
Stabilizer °C
Hot wash
Room 5 5’ with 2 g/L
H2O2
temperatur ’ detergent at
e boil
Water pH Cold wash
+ Check
Wetting Drying
agent
+
Sequesterin Assessmen
g agent t
+
Figure: Process Curve of cotton fabric bleaching with hydrogen peroxide.
Fabric

23
Assessment of Bleaching Quality
Visual Assessment
Compare visually the whiteness of bleached sample with un-bleached sample as well as the
bleached samples of other groups.
 Wetting agent: Used to facilitate the penetration of the bleach liquor into the fibre by
reducing the surface tension of water resulting in uniform bleaching.
the metallic ions may decompose the bleach bath.
 Hydrogen Peroxide: Used as bleaching agent. Hydrogen peroxide liberates per-hydroxyl

ion (HO2-) in aqueous medium which is highly unstable and in the presence of oxidisable
substance (coloured impurities in cotton), it is decomposed and thus bleaching action takes
place.
 Sodium Hydroxide: Acts as activator of hydrogen peroxide bleaching. Sodium hydroxide

activates hydrogen peroxide because H+ ion is neutralized by alkali which is favourable for
liberation of HO2-.
 Stabilizer (Sodium Silicate): The process of regulation or control of per-hydroxyl ion to

prevent rapid decomposition of bleach and to minimize fibre degradation is described as
stabilization. Stabilizers for peroxide normally function by controlling the formation of free
radicals.

24
Name of the Experiment: Degumming of Raw Silk Fabric.
Literature Review
4.1.1 Silk Degumming

Scouring is a purifying treatment of textiles. The objective of scouring is to reduce the amount
of impurities sufficiently to obtain level and reproducible results in dyeing and finishing
operations.
Raw silk possesses neither luster nor the softness commonly associated with silk; these
properties so not appear until the raw material has been scoured. The scouring process is
generally referred to as degumming, boiling off and occasionally as stripping. The process
employed to remove the silk gum (sericin) enveloping the two raw silk threads (fibrion).
During the spinning process of silk by silkworms the two filaments are made into one by
means of proteinious gummy substance called sericin.
Figure: The microphotograph of raw silk.
Apart from sericin, other impurities present in silk are lubricants and softeners added during
throwing or in preparation for weaving or knitting, dirt and oils picked up incidentally during
processing and undesirable natural colours. The component of fats and oils is around 0.5-1%
and that of natural pigments 1.0-1.4%. During the degumming process, soil, stain, oil and fats
sticking to the material will also be removed. Thus degumming is synonymous with the
scouring process normally used for the purification of cotton and wool.
Degumming is effected by careful boiling-off in soap baths which should be slightly alkaline.
The fibre is treated with soap solution to give a pH around 10.0 at 90-95 °C for 1.5-2 hours in
order to avoid lien soap deposits and resulting stains, the water should be properly softened.
Sequestering agent may be added in the bath to correct the hardness of water. In case of white
and delicate varieties a two bath method may be employed. The second degumming bath will
consist of 50% quantity of soap taken for the first degumming bath and the duration of
treatment may be divided equally between 40-45 min for each bath.
25
Degumming with synthetic detergent is increasingly replacing soap. The main drawbacks are
soap is expensive, great quantity of soap is required and longer treatment time. A large number
of synthetic detergents are available in the market and their selection is very important
particularly on the requirement of soft feel as that achieved with soap. Non-ionic product like
nonyl phenol ethoxylated compound in the pH range of 11.2-11.5 for a treatment time of 40
min at 95 °C is found to remove the gum and maintain the strength of the yarn.
Standard Recipe
Chemicals/Parameters Quantity (g/L)

Degumming agent
 Soap or 12 – 20 or
 Detergent 5–8
pH (adjusted by acid or alkali) 10
Temperature Boiling
Time 90 min
M:L Ratio 1:100
Recipe Calculation
Fabric weight = X g
 Wetting agent 2 g/L
2∗Z
 Sequestering agent 1 g/L
1∗Z
 Soap 15 g/L
15 ∗ Z
Z mL of liquor contains g of sodium hydroxide
1000
hydrogen peroxide)

26
Working Procedure
1. Take initial weight of the raw silk fabric on a weighing balance.

4. Prepare the degumming bath at room temperature with the appropriate quantity of
water.
stirring for 5 minutes.
6. Dissolve the calculated amount of soap in a beaker with warm water and then add the
solution in the main bath.
7. Continue stirring for another 5 minutes.
8. Check and adjust the pH and then raise the temperature to the boiling and continue for
90 minutes with constant stirring.
boil.
10. Dry the fabric using a hand dryer and test for degumming quality.
Process curve
Temperature rise up
Time 90 Min
to the boil
Drain
Soap or
Detergent Hot wash with
5’ 2 g/L detergent
Room 5’
at boil
temperature
Water pH Cold wash

+ Check
Wetting agent
+ Drying
Sequestering
agent
Assessment
+
Fabric
Figure: Process Curve of silk degumming with soap or detergent

27
Assessment of Degumming Quality
 Test 01. Visual Assessment

 Test 02. Calculation of weight loss in percentage
 Test 03. Absorbency test (Drop/Spot test)
4.5.1 Test- 01: Visual Assessment

Visually assess softness and whiteness of the degummed sample with raw sample.
4.5.2 Test -02: Calculation of weight loss in percentage

As raw silk fibre contains approximately 20 – 25% impurities so loss in fabric weight after
degumming indicates the removal of impurities. The weight loss is expressed as a percentage.
Weight before degumming − Weight after degumming

Weight Loss (%) = × 100
Weight before degumming
Acceptable range is 20 - 25%. Less than 20% means the fabric is not well degummed. Weight
loss% higher than 25% indicates damage to silk fibers instead of impurity removal which is
unacceptable.
4.5.3 Test- 03: Absorbency test (Drop/Spot test)

This method was designed to measure the water absorbency of textiles by the time required for
the specular reflection of the water drop to disappear is measured and recorded as wetting time.
0.1% direct red (Congo Red) dye solution was prepared and also dropped at the different
places of the fabric and the shape of the absorption area on the fabric was observed.
Procedure: For the drop test, the sample was placed over the top of a beaker so that the center
is unsupported. In a pipette a solution of 0.1% direct red is taken and dropped on the
unsupported part of the fabric. Then the absorption of the colored drop is observed visually.
 Wetting Time: It is the time required to absorb the water droplets completely by the
sample. Longer the time, lower the absorbency. Standard time for absorption of the
drop should be 0.5 – 0.8 second. Although less than 1 second is acceptable.
 Shape: In addition the degumming efficiency was also evaluated by assessing the
uniformity of degumming from the shape of the absorbed area on the fabric.
Table: Visual Evaluation Parameters of Drop/Spot Test

Visual assessment Drop shape Comment
The drop spot is circular but spreading The scouring is even but
over less area. incomplete.
The drop spot is circular and spreading
Scouring is even and complete.
over large area.

28
The drop spot size is irregular in shape Uneven scouring.
 Wetting agent: Generally interracial tension between the textile fibre and the liquor is high,
and hence wetting of the fibre surface does not take place quickly. This is particularly true
in the case of raw fabric and hydrophobic fibres. One of the main functions of the
surfactants is to reduce the surface tension of water and thereby bring about wetting of the
fabric resulting in uniform degumming.
the metallic ions may react with the degumming agent.
 Degumming agent (Soap/Detergent): The function of degumming agent is to dissolve the

sericin.

29
Name of the Experiment: Bleaching of Degummed Silk Fabric with
Hydrogen Peroxide.
Literature Review
5.1.1 Bleaching of Silk

Scouring generally removes all impurities except the natural colouring matters which have to
be broken down by bleaching, either with an oxidizing or a reducing bleaching agent. Almost
invariably the oxidizing agents give a more permanent white.
The natural colour of silk thread differs depending upon the type of silkworm and its feeding
habit. Although the bulk of the natural dyestuff such as chlorophil, xanthophil and carotin are
to be found in the silk gum, the degummed mulbery silk also has strong yellowish inherent
colour. Since some of the sericin is tenaciously held by fibrion, complete elimination of colour
by degumming is not achieved. Thus, the fabrics manufactured from yellow raw silk retain a
yellowish tint after boiling-off. This natural yellowish tint on silk is desired by some fashion
designers as a 'soft white' or natural shade.
The silk may be bleached by oxidative as well as reduction methods. If a very high degree of
whiteness is required, a combination of both methods in the form of double bleach is applied.
The best method of bleaching silk is the use of hydrogen peroxide in a separate bath. The
perhydroxyl ion or even atomic oxygen is responsible for the oxidation effect on the organic
colouring matter present in silk and thus for bleaching effect.
As silk fibre is sensitive to alkali, the alkali necessary for activation of hydrogen peroxide must
be added to the bleaching bath should be ammonia or tetrasodium pyrophosphate. The pH
value of the bleaching liquors should lie between pH 8.5-9.
Stabilisers are added to the bath to achieve a slow seperation of the oxygen needed for the
bleaching effect. Water glass, which is often used as a stabiliser, should not be used for
bleaching silk, because owing to the precipitation of silicic acid the silk can get a hard, brittle
handle. In this case, tetrasodium pyrophosphate and fatty protein condensates are the ideal
choice. The mixtures of sodium silicate and trisodium phosphate or organophosphates exert a
great stabilising effect on peroxide and help to control bleaching action.
The bath is gradually raised to required temperature in 1 h and bleaching is done at this
temperature for specified time. The silk after bleaching is thoroughly rinsed first with warm
water and then with cold water, hydroextracted and dried. Standing baths of peroxide can be
used by replenishing the bath with 1/3rd the quantity of hydrogen peroxide and 1/4th the
quantity of stabiliser originally taken for bleaching.

30
Standard Recipe

Hydrogen Peroxide (50%) 6-15
Stabilizer (TSP) 2
Temperature 60-65 °C
pH 8-9
Time 90 min
M:L Ratio 1:100
Recipe Calculation
Fabric weight = X g
1∗Z
1∗Z
 Hydrogen Peroxide 10 g/L
1 L or 1000 mL of liquor contains 10 g of hydrogen peroxide
10 ∗ Z
Z mL of liquor contains g of hydrogen peroxide
1000
 Stabilizer 2g/L
2∗Z
Z mL of liquor contains 1000 g of sodium hydroxide

hydrogen peroxide)

31
Working Procedure
1. Take initial weight of the degummed silk fabric on a weighing balance.

4. Prepare the bleaching bath at room temperature with the appropriate quantity of water.
stirring.
6. Check and adjust the pH and then raise the temperature to 60 °C.
7. Add hydrogen peroxide and again rise the temperature to the boil and continue for 45
minutes with constant stirring.
boil.
9. Dry the fabric using a hand dryer and test for bleaching quality.
Process curve
Temperature rise up
to 60-65 °C Time 90 Min
Drain
Stabilizer Hot wash with

5’ 2’
2 g/L detergent
Room 5’
at boil for 5 min
temperature
Water pH Hydrogen Cold wash

+ Check Peroxide
Wetting agent
+ Drying
Sequestering
agent
Assessment
+
Fabric
Figure: Process Curve of silk fabric bleaching with hydrogen peroxide

32
Assessment of Bleaching Quality
Visual Assessment
Compare the whiteness and softness of bleached sample with un-bleached sample as well as
with the bleached samples of other groups.
 Wetting agent: Used to facilitate the penetration of the bleach liquor into the fibre by
reducing the surface tension of water resulting in uniform bleaching.
the metallic ions may decompose the bleach bath.
 Hydrogen Peroxide: Used as bleaching agent. Hydrogen peroxide liberates per-hydroxyl

ion (HO2-) in aqueous medium which is highly unstable and in the presence of oxidisable
substance (coloured impurities in silk), it is decomposed and thus bleaching action takes
place.
 Stabilizer: Stabilizers are added to the bath to achieve a slow separation of the oxygen
needed for the bleaching effect.

33
Name of the Experiment: Dyeing of Cotton Fabric with Direct Dyes.
Literature Review
6.1.1 Dyeing
Dyeing is the process of adding color to textile products like fibers, yarns, and fabrics. Dyeing
is normally done in a special solution containing dyes and particular chemical material. After
dyeing, dye molecules have uncut Chemical bond with fiber molecules. The temperature and
time controlling are two key factors in dyeing. There are mainly two classes of dye, natural and
man-made.
For most of the thousands of years in which dyeing has been used by humans to decorate
clothing, or fabrics for other uses, the primary source of dye has been nature, with the dyes
being extracted from animals or plants. In the last 150 years, humans have produced artificial
dyes to achieve a broader range of colors, and to render the dyes more stable to resist washing
and general use. Different classes of dyes are used for different types of fiber and at different
stages of the textile production process, from loose fibers through yarn and cloth to completed
garments.
The dyeing process consists of three stages which are:

1. Migration of the dye from the solution to the interface accompanied by adsorption on
the surface of the fibre.
2. Diffusion of the dye from the surface towards the centre of the fibre.
3. The anchoring of the dye molecules by covalent or hydrogen bonds, or other forces of a
physical nature.
6.1.2 Direct Dyes

Direct dyes are defined as anionic dyes with substantivity for cellulosic fibres, normally
applied from an aqueous dyebath containing an electrolyte. Their most attractive feature is the
essential simplicity of the dyeing process, but a separate after-treatment to enhance wet
fastness has been necessary for most direct dyeing.
The standard of wet fastness, particularly to washing, of direct dyeings, even when given a
conventional cationic after-treatment, does not meet the more demanding end uses in cellulosic
apparel and furnishing materials. Consequently, direct dyes have been replaced to a great
extent by reactive dyes, which have better wet fastness and exceptional brightness in many
hues. Nevertheless, there are still many applications in the textile industry for goods dyed with
direct dyes, particularly where a high standard of wet fastness is not required.
Direct dyes are used in low-priced viscose or blended curtain fabrics, furnishings and carpets,
where good light fastness and moderate fastness to washing are usually adequate. Cheap cotton
34
dressing gowns and bedspreads that may be washed infrequently, viscose ribbons and linings,
as well as dischargeable ground shades for low quality prints are often dyed with direct dyes.
6.1.3 Chemical structure

Direct dyes can be roughly represented as R-SO3Na (Dye-SO3Na). Direct dyes are mostly
derivatives of benzene and naphthalene and are alkali salts of aromatic sulphonic acid. They
dissolve in water. The more the sulphonate group, the greater is the solubility of the dyes.
Approximately 50% of all direct dyes are disazo structures; a typical example is CI Direct
Blue1
Figure: Structure of CI Direct Blue 1
6.1.4 Mechanism of substantivity of direct dyes

Hydrogen bonding and Vander Waal’s force play dominant roles in fixation of direct dyes on
cellulosic fibre. Hydrophobic interaction may also contribute to the attachment of dye. The
bonding is only physical and not chemical.
6.1.5 Properties
 Direct dyes are capable of dyeing cellulose, protein and polyamide fibre without
preliminary mordanting. However, the application in cotton is most wide.
 They are available in full range of hue but do not have color brilliance.
 All direct dyes are soluble in water, but some of them are more soluble in a weak
alkaline medium.
 The solubility of the dyes depends greatly on the chemical nature. Solubility is greatly
influenced by the sulphonic group in the dye molecule. Thus, for instance, direct
brilliant blue containing four sulphonic group is much more soluble than Congo red
containing only two.
 Their solubility also increases considerably with liquor temperature.
 A considerable member of direct dyes forms precipitate with Mg and Ca salts. So,
either dyeing should be done with softened water or sodium hexa-meta-phosphate or
sequestering agent should be added to the dye bath.
 Direct dyes on cotton have poor wash fastness, this can somewhat be improved by
various after treatments on the fibre.
 Their light fastness on cellulosic fibres varies from poor to fairly good, though some
copper complex dyes have very good light fastness.
 They provide wide range of hues- yellow, orange, red, violet, blue, green, brown, black.

35
6.1.6 Effect of different variables
 Effect of electrolyte
The addition of electrolytes to the dye liquor tends to promote exhaustion of direct dyes,
although the effect varies considerably with different dyestuffs.
Cellulose fibres assume a negative charge when immersed in water. This has the effect of
repelling the similarly charged ion of the dye. Electrolytes reduce or extinguish the charge on
the fibre surface, thus facilitating the approach of the dye ion to within the range at which
hydrogen bonding and Vander Waal’s forces can become effective.
 Effect of temperature
Increase of temperature decreases the amount of dye absorbed by the fibre at equilibrium. By
increasing the kinetic energy of the molecules it does, however, hasten the speed at which
equilibrium is attained at the temperature in question.
 Effect of liquor ratio

Percent exhaustion continues to increase as the concentration of the dye in the liquor becomes
greater. This means that dyeing at low liquor ratio decreases the amount of dye wastage. It also
consumes less water and steam, and allows a given salt concentration with less added salt.
Dyeing in short liquor ratio is an important factor in economizing in dyestuff consumption.
When producing heavy shades the amount of dye which is necessary can become very great if
the machine is one which requires a high ratio of liquor to goods.
 Effect of pH value
Direct dyes are almost invariably applied from a neutral solution. No advantage is gained by
the addition of acid and there is a possibility that it may alter the shade. Mild alkali has a
retarding effect upon the rate of absorption. Up to 3% sodium carbonate is sometimes added
either to counteract the hardness of water or in few cases such as with Benzopurine 4B (CI
Direct Red 2) and Chlorazol Orange PO (CI Direct Orange 1) to improve the solubility.
6.1.7 Fastness properties

Direct dyes do not possess good fastness to washing nor to other wet processes such as
scouring. They cannot be used on yarns incorporated in wool goods which are to be cross-
dyed. The light fastness of some can only be rated as moderate, but many are quite good.

36
Standard Recipe for Direct Dyeing
Chemicals/ Parameters Quantity

Shade % 0.5-3 % OWF
Wetting Agent (Non-ionic) 1 g/L
Sequestering Agent 1 g/L
Glauber’s Salt 10-25 g/L
1 (or as required
Sodium Carbonate (Soda ash)
to adjust the pH)
Temperature 85 °C
pH 9
Time 45 min
M:L Ratio 1:50
Preparation of Stock Dye Solutions

In all cases the preparation method for stock dye solutions should aim at producing a stable
solution with the dye fully dissolved or dispersed. Use of modern electronic balances reduces
the possibility of weighing error. Weighing directly into a beaker, in which the initial
dissolving or dispersion can be carried out, eliminates the possibility of loss on transfer.
Dissolving or dispersing methods should be based on those recommended in the dye

manufacturers’ pattern cards. The dye solution is then made up to volume in a volumetric
flask. Hot water should be used to prevent solid dye separating out, and the solution finally
made up to the mark only when it has been cooled. The water used throughout must be
representative of that used in the dye-house, as many dyes are sensitive to calcium, magnesium
and heavy-metals ions.
The strength of the stock solution is inevitably a compromise between convenience and
stability, but 0.25% (2.5 g of dye in 1 L) is suitable for most classes of dye.
Preparation of Laboratory Dye-Liquors

It has been traditional to measure stock dye and chemical solutions with graduated pipettes,
using either top zero or bottom zero types. The full range of graduated pipettes , 0.5, 1, 2, 5, 10
and 25 ml, should be available, and the smallest convenient pipette used for the calculated
amount of dye solution. It is essential to prepare a more dilute stock solution for use when less
than 0.5 ml of solution of the usual concentration is required.
Stock solutions of dyes and chemicals are described according to conventional laboratory uses,
i.e. grams per 100 ml of solution.

37
6.4.1 Calculation for Percentage Required
A 2% dyeing, however, means that 2 g of dye are applied to 100 g of fibre, and amounts of
dyes and chemicals required in a dye-liquor are calculated on this basis. The amount of stock
solution is calculated as follows:
Percentage required × Weight of fibre

Amount of stock solution (ml) =
Concentration (%)of stock solution
The weight of dye-liquor in relation to the weight of fibre is the liquor ratio, thus with 5 g of
fibre in 100 g of dye-liquor the liquor ratio is 20:1.
6.4.2 Calculation for g/l Required

Sometimes amount of dyes and chemicals are specified in relation to the total quantity of dye-
liquor (g/l), and calculation of the amount of stock solution, if the liquor ratio is known, is:
g/l required × Weight of fibre × liquor ratio

10 × Concentration (%)of stock solution
Recipe Calculation
Fabric weight = X g
Say for 2% shade and 1% stock solution
𝐒𝐡𝐚𝐝𝐞 𝐏𝐞𝐫𝐜𝐞𝐧𝐭𝐚𝐠𝐞 𝐫𝐞𝐪𝐮𝐢𝐫𝐞𝐝 × 𝐖𝐞𝐢𝐠𝐡𝐭 𝐨𝐟 𝐟𝐢𝐛𝐫𝐞
Amount of dye solution (ml) =
𝐂𝐨𝐧𝐜𝐞𝐧𝐭𝐫𝐚𝐭𝐢𝐨𝐧 (%)𝐨𝐟 𝐬𝐭𝐨𝐜𝐤 𝐬𝐨𝐥𝐮𝐭𝐢𝐨𝐧
𝟐 ×𝐗
= = 2X
𝟏
Amount of chemicals
(The auxiliaries chemicals required in g/l can be calculated by using the following formula)
Say for Wetting agent
𝐠/𝐥 𝐫𝐞𝐪𝐮𝐢𝐫𝐞𝐝 × 𝐖𝐞𝐢𝐠𝐡𝐭 𝐨𝐟 𝐟𝐢𝐛𝐫𝐞 × 𝐥𝐢𝐪𝐮𝐨𝐫 𝐫𝐚𝐭𝐢𝐨

𝐀𝐦𝐨𝐮𝐧𝐭 𝐨𝐟 𝐰𝐞𝐭𝐭𝐢𝐧𝐠 𝐚𝐠𝐞𝐧𝐭 (𝐠/𝐦𝐥) =
𝟏𝟎 × 𝐂𝐨𝐧𝐜𝐞𝐧𝐭𝐫𝐚𝐭𝐢𝐨𝐧 (%)𝐨𝐟 𝐬𝐭𝐨𝐜𝐤 𝐬𝐨𝐥𝐮𝐭𝐢𝐨𝐧
Quantity of water = Quantity of liquor – (Quantity of dye and chemicals solution)

38
Working Procedure
1. Cut a sample from the bleached fabric and weight on a weighing machine.
3. Prepare the stock solution of dyes and chemicals.
4. Calculate the amount of dyes, chemicals and required quantity of water according to the
5. Prepare the dye bath at room temperature with the appropriate quantity of water.
stirring.
7. Check the pH of the bath and if adjusted then add dye solution.
8. Separate the salt solution in two equal parts and add in accordance to the process
diagram.
9. Raise the temperature up to 85 °C and continue dyeing for 45 minutes.
10. Wash the fabric with cold water and hot water with 2 g/L soaping agent for 5 minutes
at the boil.
11. Dry the fabric using a hand dryer and test for dyeing quality.
Process curve
Temperature rise up
to 85 °C Time 45 Min
Drain
½ Salt
Alkali Solution Hot wash with
s 2 g/L detergent
Room 5’ 5’ 5’ 5’
at boil for 5 min
temperature
Water pH Check if ½ Salt Cold wash

+ adjusted add Solution
Wetting agent dye solution s
+ Drying
Sequestering
agent
Assessment
+
Fabric
Figure: Process Curve of cotton dyeing with direct dyes

39
Assessment of Dyeing Quality
Visual Assessment
Assess visually the evenness of dyed sample and compare the depths of dyed samples with the
samples dyed by other groups.
 Wetting agent: Used to facilitate the penetration of the dye-liquor into the fibre by
reducing the surface tension of water resulting in uniform dyeing.
the metallic ions may react with the dyes and other chemicals.
 Sodium Carbonate: Direct dyes are almost invariably applied from a neutral solution. But
acid may convert the direct dyes to leuco form which is insoluble in water and there is a
possibility that it may alter the shade. Mild alkali has a retarding effect upon the rate of
absorption. Up to 3% sodium carbonate is sometimes added either to counteract the
hardness of water or in few cases to improve the solubility.
 Glauber’s Salt: The addition of electrolytes such as salt to the dye liquor tends to promote
exhaustion of direct dyes. Electrolytes reduce or extinguish the charge on the fibre surface,
thus facilitating the approach of the dye ion to within the range at which hydrogen bonding
and Vander Waal’s forces can become effective.

40
Name of the Experiment: Dyeing of Cotton Fabric with Vat Dyes.
Literature Review
7.1.1 Vat Dyeing

Vat dyes are water insoluble colored compounds. As such they cannot be directly applied on
cotton or other fibres as direct dyes are dyed. They have to be converted into their water
soluble forms. During the dyeing process, it is this soluble form of the dye that is applied on
cotton, followed by re-conversion of the soluble form into their original insoluble form. As a
result, the insoluble dye is trapped in the fibre and cannot come out during or other wet
treatments, thereby ensuring excellent fastness to washing and wet treatments.
As vat dyes are all insoluble in water and so cannot be used for dyeing without modification.
When treated with a reducing agent they are converted into leuco compounds, all of which are
soluble in water in the presence of alkalis. These leuco compounds are substantive towards
cellulose and re-oxidize to the insoluble colored pigment within the fibre when exposed to air
or treated with an oxidizing agent. The leuco compounds are often colorless or of quite a
different color (lemon yellow) from the actual dye.
The vat dyes consists of one or more carbonyl group (>C:O) which, when treated with a
reducing agent, combine with hydrogen to form leuco compounds containing (>C.OH) groups.
These secondary alcohols do not dissolve in water but form soluble sodium derivatives
(>C.ONa) in the presence of alkalis. On exposure to air or any chemical oxidizing agent the
sodium compound is converted to the insoluble colored derivative through the following
reactions:
>C=O + Hydrose (Na2S2O4)  >C.OH + NaOH  >C.ONa

Insoluble Reducing agent leuco vat alkali sodium salt of leuco vat dyes
Vat dyes (soluble in water)
C.ONa + H2O  C.OH + 2NaOH
C.OH + Oxidation [O]  >C= O + H2O

Reconverted into
Original insoluble Vat dyes

41
7.1.2 Principles of application of vat dyes
Generally, the application of vat dyes to textile materials involves four distinct steps –
1. Vatting, in which the insoluble commercial dye is reduced and solubilised (vatted) by
using sodium hydrosulphite and sodium hydroxide.
2. Dyeing in which the soluble sodium salt of the leuco vat dye is absorbed by the textile
material from an alkaline reducing medium in the presence of either a retarding agent
or an exhausting agent depending on the rate of dyeing.
3. Oxidation, in which the soluble form of the dye absorbed by the fibre is reconverted
into the original insoluble dye by atmospheric oxygen (airing) or by ‘chemical
oxidation’ (i.e. involving the use of chemical like sodium perborate, potassium
dichromate etc.) and
4. After treatment, in which the dyed material is subjected to boiling soap or other
detergent solutions in order to get the proper tone by the way of aggregation of smaller
dye particles in to bigger ones also to get the optimum fastness especially rubbing
fastness by removing the surface deposited dye particles.
Recipes and Procedures
7.2.1 Step- 1: Vatting

 Recipe and process parameters for vatting and Dyeing
Vat Dyes 10
Dispersing Agent 5-8
Caustic Soda (NaOH) 20-30

Sodium Hydrosulphite
20
(Na2S2O4)
Temperature 60 °C
Time 20 min
M:L Ratio 1:50

42
 Calculation
Calculate the amount of dyes and chemicals required by using the following formula

𝐀𝐦𝐨𝐮𝐧𝐭 𝐨𝐟 𝐜𝐡𝐞𝐦𝐢𝐜𝐚𝐥𝐬 (𝐦𝐥) =
 Procedure
i) Set the bath at room temperature with appropriate amount of water and add the chemicals
in accordance with process diagram. Stir well for a complete dissolution.
ii) Add sodium hydroxide and raise the temperature to 60 °C and add hydrose. Stir for 5
minutes minutes.
iii) Prepare the dye solution in a separate beaker with dyes, hot water (600C) and dispersing
agent and add to the dye bath.
iv) Stir the mixture, cover with a lid and keep for 15-20 minutes at 600C for the vatting to be
completed.
7.2.2 Step- 2: Dyeing

i) Place the cotton fabric into the vatted solution. If required additional sodium hydroxide and
hydrose mixed with hot water may be added but make sure to maintain a M:L ratio= 1: 50
and a pH of 10-12. [To make additional solution: NaOH=4g/l + hydrose = 3 g/l + hot
water]
ii) Continue dyeing at 70-800C for 30-45 min. Keep the bath closed all the time. If necessary
salt 3-5 g/l may also be added.
Process curve
Time 30 Min
80 °C
Drain
Time 20 Min
60 °C
Rinsing
Room 5’
Hydroze
temperature
Water NaOH
+ solution
Wetting agent
+
Sequestering
agent
Figure: Process Curve of cotton dyeing with Vat dyes

43
7.3.1 Step- 3: Oxidation
After dyeing the reduced dyes are penetrated and distributed into the fibre. The exhausted dyes
are then oxidized to convert it to original insoluble form inside the fibre. Before oxidation a
light rinsing may be carried out.
Oxidation may be carried out by exposing the dyed fabric in air or immersing in a bath with the
following recipe:
Hydrogen Peroxide (H2O2) 2
Temperature 40 °C
Time 20 min
7.3.2 Step- 4: After-treatment

The unfixed dyes from the surface are removed in after-treatment process which can be carried
out by the following recipe and parameters.

Detergent 2
Sodium Carbonate 1
Temperature Boiling
Time 10 min
The after-treatment process is followed by rinsing in cold and hot water.
Visual Assessment

44
 Sodium Hydrosulphite: Sodium hydrosulphite (Na2S2O4) commercially known as Hydros
is a strong reducing agent, which is used in the vatting process of vat dyes to reduce the
insoluble commercial dye in the form of leuco vat dyes.
 Sodium hydroxide: Sodium hydroxide is a strong alkali used in the vatting process to
convert the reduced leuco vat dyes into water soluble salts.
 Glauber’s Salt: Salts are generally added in the dye bath as a exhausting agent. They
increase the exhaustion rate of dyes in the fibre. The use of exhausting agents such as
common salts, Glauber’s salt (Na2SO4 .10H2O), anhydrous sodium sulphate etc. becomes
necessary for the dyes, which are characterized by low rates of uptake by the fibre.

45
Name of the Experiment: Dyeing of Silk Fabric with Acid Dyes.
Literature Review
8.1.1 Silk Dyeing
Silk retains –NH2 and –COOH groups at either ends of its chemical structure and can be dyed
with acid, basic, metal-complex, mordant, natural, reactive dyes. The dye–silk interaction
occurs through ionic or covalent bonding.
Acid dyestuffs are so called because the substances were originally applied in a bath containing
mineral or organic acid. Most acid dyes are sodium salts of organic suphonic acids. They
consist of an aromatic structure containing a chromogen and a solubilizing group, which is
almost always a sulphonic acid salt (D-SO3Na). The acid dyes are soluble ionic compounds
where the color is contained in the anionic portion.
The acid dyes have a great affinity towards protein fibres and are main class used in wool
dyeing. Most of them will not dye cellulosic fibres but, since they resemble direct dyes in
chemical constitution, there are some which will dye cellulose well. Polyamide fibres also have
an affinity for acid dye.
8.1.2 Mechanism of silk dyeing with acid dyes

The structure of silk can be represented in its simplest form as
When dipped in water, the H+ from carboxylic ion is transferred to the amino group at the other
end so that the two ends become electrically charged, as indicated as below:
When a fibre containing such electrically-charged molecular ends is entered in a solution of an

acid, say CH3COOH, some of the negatively charged carboxylate group take up H+ ions from
the solution and become electrically neutral and the CH3COO- anions from the acid are
absorbed by the positively charged amino end groups in the protein:
Thus, when silk is entered in a solution of acid, the concentration of acid decreases with the
formation of positive sites in the protein macromolecules. An acid dye, designated as D-
SO3Na, splits into its ions when dissolves in water. The dye anion then replaces the acid anion
and form salt-linkage with the fibre.

46
Standard Recipe and process parameters

Acid Dyes 0.5-4 % OWF
Acetic Acid (80%) 2
Glauber’s Salt 10-25
Temperature 85 °C
pH 5
Time 45 min
M:L Ratio 1:100
Preparation of Stock Dye Solutions

In all cases the preparation method for stock dye solutions should aim at producing a stable
solution with the dye fully dissolved or dispersed. Use of modern electronic balances reduces
the possibility of weighing error. Weighing directly into a beaker, in which the initial
dissolving or dispersion can be carried out, eliminates the possibility of loss on transfer.
Dissolving or dispersing methods should be based on those recommended in the dye

manufacturers’ pattern cards. The dye solution is then made up to volume in a volumetric
flask. Hot water should be used to prevent solid dye separating out, and the solution finally
made up to the mark only when it has been cooled. The water used throughout must be
The strength of the stock solution is inevitably a compromise between convenience and
stability, but 0.25% (2.5 g of dye in 1 L) is suitable for most classes of dye.
Preparation of Laboratory Dye-Liquors

It has been traditional to measure stock dye and chemical solutions with graduated pipettes,
using either top zero or bottom zero types. The full range of graduated pipettes , 0.5, 1, 2, 5, 10
and 25 ml, should be available, and the smallest convenient pipette used for the calculated
amount of dye solution. It is essential to prepare a more dilute stock solution for use when less
than 0.5 ml of solution of the usual concentration is required.
Stock solutions of dyes and chemicals are described according to conventional laboratory uses,
i.e. grams per 100 ml of solution.

47
Calculation
Calculation for Percentage Required
A 2% dyeing, however, means that 2 g of dye are applied to 100 g of fibre, and amounts of
dyes and chemicals required in a dye-liquor are calculated on this basis. The amount of stock
solution is calculated as follows:
Percentage required × Weight of fibre
Concentration (%)of stock solution
The weight of dye-liquor in relation to the weight of fibre is the liquor ratio, thus with 5 g of
fibre in 100 g of dye-liquor the liquor ratio is 20:1.
Calculation for g/l Required

Sometimes amount of dyes and chemicals are specified in relation to the total quantity of dye-
liquor (g/l), and calculation of the amount of stock solution, if the liquor ratio is known, is:
g/l required × Weight of fibre × liquor ratio

10 × Concentration (%)of stock solution
Recipe Calculation
Fabric weight = X g
Say for 2% shade and 1% stock solution
𝐒𝐡𝐚𝐝𝐞 𝐏𝐞𝐫𝐜𝐞𝐧𝐭𝐚𝐠𝐞 𝐫𝐞𝐪𝐮𝐢𝐫𝐞𝐝 × 𝐖𝐞𝐢𝐠𝐡𝐭 𝐨𝐟 𝐟𝐢𝐛𝐫𝐞
Amount of dye solution (ml) =
𝐂𝐨𝐧𝐜𝐞𝐧𝐭𝐫𝐚𝐭𝐢𝐨𝐧 (%)𝐨𝐟 𝐬𝐭𝐨𝐜𝐤 𝐬𝐨𝐥𝐮𝐭𝐢𝐨𝐧
𝟐 ×𝐗
= = 2X
𝟏
Amount of chemicals
(The auxiliaries chemicals required in g/l can be calculated by using the following formula)
Say for Wetting agent,

𝐀𝐦𝐨𝐮𝐧𝐭 𝐨𝐟 𝐰𝐞𝐭𝐭𝐢𝐧𝐠 𝐚𝐠𝐞𝐧𝐭 (𝐠/𝐦𝐥) =
Quantity of water = Quantity of liquor – (Quantity of dye and chemicals solution)

48
Working Procedure
1. Cut a sample from the bleached fabric and weight on a weighing machine.
3. Prepare the stock solution of dyes and chemicals.
4. Calculate the amount of dyes, chemicals and required quantity of water according to the
5. Prepare the dye bath at room temperature with the appropriate quantity of water.
stirring.
7. Check the pH of the bath and if adjusted then add dye solution.
8. Separate the salt solution in two equal parts and add in accordance to the process
diagram.
9. Raise the temperature up to 85 °C and continue dyeing for 45 minutes.
10. Wash the fabric with cold water and hot water with 2 g/L soaping agent for 5 minutes
at the boil.
11. Dry the fabric using a hand dryer and test for dyeing quality.
Process curve
Temperature rise up Time 45 Min

to 90-95°C
60 °C’ 5’ Drain
Acetic
Acid
Dye Hot wash with
½ Salt Solution 2 g/L detergent
Room 5’ 5’ 5’
Solution s at boil for 5 min
temperature s
Water pH ½ Salt Cold wash

+ Check Solution
Wetting agent s
+ Drying
Sequestering
agent
Assessment
+
Fabric
Figure: Process Curve of silk dyeing with acid dyes.

49
Visual Assessment
 Acetic Acid: When a fibre containing electrically-charged molecular ends is entered in a

solution of an acid, say CH3COOH, some of the negatively charged carboxylate group take
up H+ ions from the solution and become electrically neutral and the CH3COO- anions from
the acid are absorbed by the positively charged amino end groups in the protein. Thus acids
active the positive sites present in the silk fibre.
 Glauber’s Salt: The addition of electrolytes such as salt to the acid dye liquor tends to
retard the reaction rate. The anionic part of salt temporarily neutralized the activated
positive group of silk fibre thus the reaction rate between dyes and fibre is slowing down.

50
Name of the Experiment: Printing of Cotton Fabric with Direct Dyes
Literature Review
9.1.1 Printing
Textile printing is the most versatile and important of the methods used for introducing colour
and design to textile fabrics. In other words, the main object of printing is the production of
attractive designs with well-defined boundaries in one or more colours. Therefore, unlike
dyeing printing generally involves the application of dyes or pigments locally from a thickened
solution commonly known as printing paste to produce various designs.
9.1.2 Difference between dyeing and printing

Features of Dyeing
 Production of even dyeing by using a fairly large volume of dyestuff solution.
 Fairly low concentration of dyestuffs
 Dyeing is carried out for a prolonged period
 The exhaustion of the bath is controlled by the manipulation of temperature of the bath,
use of retarding/leveling agents or exhausting agents.
 Produce slow dyeing in the initial stages of dyeing and rapid dyeing subsequently so
that uniform dyeing results
 The dyestuff molecules have to travel a fairly long distance before they are absorbed by
the fibre surface from the solution.
Features of Printing
 Deposition of a viscous paste containing dyestuffs, a thickening agent and a small
amount of water on the surface of the fabric.
 Immediately dried to prevent any spreading beyond the boundaries of the design.
 A fairly concentrated dye solution is used.
 After drying, the entire amount of dye is present on the dried up thickener film and can
be washed away more or less completely from the fabric by either a light rinsing or a
thorough soaping.
 The actual transfer of the dye from the thickener film to the fabric is carried out
subsequently in a hot and humid atmosphere with or without pressure in a short time.
 This is done by subjecting the printed goods to steam at 1000 to 1020C for 3-5min.
 The dye molecules have to travel a short distance
 The very high dye concentration in the thickener during steaming, the thickener film
moistened by absorption of very little amount of condensed steam, as well as high
temperature facilitates quick transfer of dye to fabric.
 Since the paste is made with very little amount of water and the small amount supplied
in steaming, special printing auxiliaries have to be used in the paste.

51
9.1.3 Styles of printing
A colored design on a white or a differently colored background can be produced on fabrics by
using different styles of printing such as –
 Direct style of printing.

 Discharge style
 Resist style
 Dyed style
 Raised style
 Azoic style
 Metal style
 Flock style
 Crimp/crepe style
 Burn out style
9.1.4 Steps of printing

The various steps of printing are as follows:
Preparation of the fabric
Preparation of the printing paste
Making an impression of the paste on the fabric
Drying of the printed fabric
Steaming of the printed fabric
After treatment
9.1.5 The essential ingredients of a printing paste are selected from the following
 Dyestuffs, pigments or dyestuff precursors (dyestuff formers)
 Wetting agents
 Solvents, solution aids, dispersing agents and humectants
 Thickeners
 Defoaming agents
 Oxidizing and reducing agents
 Catalysts and oxygen carriers
 Acids and alkalis
 Carriers and swelling agents
 Miscellaneous agents.

52
All these constituents are not used simultaneously in any particular printing paste. Depending
on the class of dyestuff used and style of printing employed, suitable components are selected
in making the printing paste. A variety of chemicals (auxiliaries) are available in each group of
the ingredients mentioned and a particular compound used for one class of dye may not be
suitable for use with another class of dye. The choice of a component depends on its
compatibility with other ingredients of the printing paste.
Printing with Direct Dyes

Direct dyes are characterized by their affinity for cellulose (arising from their chemical
structure) and their solubility in water (the result of the presence of sulpho-groups). This means
it is possible to dye them easily and with some degree of fastness, even if limited. In printing
practice, the direct dye in a thickened solution is printed on to the fabric and then dried. During
subsequent steaming in saturated steam the thickened paste and the fibres swell, and the dye
dissolves again and diffuses from the film of paste into the fibres. Here the dye is held fast on
the fibril surfaces by Vander Waals forces and hydrogen bonds. After an adequate steaming
time equilibrium is established between dye in the fibre and dye in the paste. During the final
washing of the print, however, the unfixed dye together with the thickening paste are rinsed off
and can stain the un-dyed parts of the cellulose. At the same time the equilibrium, which has
been established at this stage, can be disturbed by the dye migrating from the fibre into the
washing liquor. For both these reasons, textile printing using direct dyes gives good results
only if a special fixing agent is employed.
Recipe for 1 kg paste:
Chemicals/ Parameters Quantity (g)

Direct Dyes 20
Dispersing Agent (TRO) 10
Thickener (Natural Gum), 10% Stock Paste 500
Hygroscopic Agent (Glycerin) 50
Alkali (TSP) 20
Water Rest to make 1 kg paste
Preparation of Stock Paste of Thickener

The stock paste is the solid content of thickener. For 10% stock paste, take 10 g of solid
thickener into a 500 ml of plastic beaker. Add 100 ml of distilled water and mix well. Agitate
the solution vigorously by a mechanical agitator until thick and stable paste is formed.

53
Preparation of Laboratory Dye Paste
The preparation method for stock dye paste should aim at producing a well dispersed stable
solution of the dye. The required amount of dye is mixed with chemicals except thickener in
beaker. In case of dye, use of modern electronic balances reduces the possibility of weighing
error. Weighing directly into a beaker, in which the initial dissolving or dispersion can be
carried out, eliminates the possibility of loss on transfer. The water used throughout must be
Working Procedure
1. Only 100 g printing paste is enough for each group. So, calculate the necessary
chemicals for 100 g paste.
2. 10% thickener need to be prepared first in a plastic beaker. Use mechanical stirrer for
the preparation of smooth paste in the presence of lab attendant. [100 ml water + 10 g
thickener]
3. Prepare the dye paste with the all other chemicals listed in the recipe only taking half
water first in a separate glass beaker.
4. Pour and combine the colored solution from glass beaker into the plastic beaker
containing thickener and mix very well.
5. If the printing paste is too viscous then add the rest amount of water and again mix
well.
6. Print the bleached cotton fabric on the printing table by using table screen. Make sure
that while printing there is no crease in the fabric.
7. After printing dry the cloth immediately in an oven and steamed for about 1 hr in a
cottage steamer, followed by light soaping and then by washing.
8. Finally dry the printed sample and test for printing quality.
Assessment of Printing Quality
Visual Assessment
Assess visually the evenness of printed sample and compare with the samples printed by other
groups.
 Thickener
Thickeners used in textile printing are high molecular weight compounds giving viscous pastes
in water. These imparts stickiness and plasticity to the printing paste so that it can be applied to
a fabric surface without spreading and be capable of maintaining the design outlines even
under high pressure. The main function is to hold or adhere the dye particles in the desired
place on the fabric until the transfer of the dye into the fabric and its fixation are complete.

54
 Hygroscopic Agent:
Over drying of applied print paste often cause cracking and poor adhesion of paste film
fixation failure of print. Hygroscopic agents are used in print paste to prevent over drying of
the printed paste during steaming by absorbing moisture readily as well as to accelerate the
dyestuff fixation. Example: Urea, Glycerine.
 Dispersing Agent
To improve the dye dissolution or dispersibility and to avoid dye aggregation. Example:
Turkey Red Oil.
 Alkali (TSP)
Direct dyes are stable in alkaline pH in this regard mild/weak alkali is used.

55
Name of the Experiment: Printing of Silk Fabric with Acid Dyes
Literature Review
10.1.1 Printing
Textile printing is the most versatile and important of the methods used for introducing colour
and design to textile fabrics. In other words, the main object of printing is the production of
attractive designs with well-defined boundaries in one or more colours. Therefore, unlike
dyeing printing generally involves the application of dyes or pigments locally from a thickened
solution commonly known as printing paste to produce various designs.
10.1.2 Steps of printing

The various steps of printing are as follows:
Preparation of the fabric
Preparation of the printing paste
Making an impression of the paste on the fabric
Drying of the printed fabric
Steaming of the printed fabric
After treatment
Printing with Acid Dyes

Acid dye is practically important for printing silk fabric. Easily soluble thickeners of high
solids content are used for fine effects and outlines, whereas products of low solids content are
preferred for larger areas because of their better levelling effect and the reduced possibility of
crack marks occurring after printing. The printing pastes contain an acid donor for fixation of
the dye. This may be ammonium sulphate, ammonium tartrate, oxalate, acetic acid or tartaric
acid. When printing protein fibres, glycerol may be used to reduce the adverse effect of
superheat in the steam during fixation; with silk, however, the addition of glycerol can cause
‘flushing’ problems. Relatively long steaming times of 30–60 min are usually needed to fix
acid dyes on wool or silk. The most brilliant and fast prints can only be obtained in saturated
steam fixation at 100–102 °C.

56
Recipe for 1 kg paste:
Chemicals/Parameters Quantity (g)

Acid Dyes 30
Thickener (Natural Gum), 10% Stock Paste 500
Hygroscopic Agent (Glycerin) 50
Acetic Acid (40%) 50
Tartaric Acid (40%) 50
Water Rest to make 1 kg paste
10.3.1 Preparation of Stock Paste of Thickener

The stock paste is the solid content of thickener. For 10% stock paste, take 10 g of solid
thickener into a 500 ml of plastic beaker. Add 100 ml of distilled water and mix well. Agitate
the solution vigorously by a mechanical agitator until thick and stable paste is formed.
10.3.2 Preparation of Laboratory Dye Paste

The preparation method for stock dye paste should aim at producing a well dispersed stable
solution of the dye. The required amount of dye is mixed with chemicals except thickener in
beaker. In case of dye, use of modern electronic balances reduces the possibility of weighing
error. Weighing directly into a beaker, in which the initial dissolving or dispersion can be
carried out, eliminates the possibility of loss on transfer. The water used throughout must be
Working Procedure
1. Only 100 g printing paste is enough for each group. So, calculate the necessary
chemicals for 100 g paste.
2. 10% thickener need to be prepared first in a plastic beaker. Use mechanical stirrer for
the preparation of smooth paste in the presence of lab attendant. [100 ml water + 10 g
thickener]
3. Prepare the dye paste with the all other chemicals listed in the recipe only taking half
water first in a separate glass beaker.
4. Pour and combine the colored solution from glass beaker into the plastic beaker
containing thickener and mix very well.
5. If the printing paste is too viscous then add the rest amount of water and again mix
well.
6. Print the bleached cotton fabric on the printing table by using table screen. Make sure
that while printing there is no crease in the fabric.

57
7. After printing dry the cloth immediately in an oven and steamed for about 1 hr in a
cottage steamer at atmospheric conditions, followed by light soaping and then by
washing.
8. Finally dry the printed sample and test for printing quality.
Assessment of Printing Quality
Visual Assessment
Assess visually the evenness of printed sample and compare with the samples printed by other
groups.
 Thickener
Thickeners used in textile printing are high molecular weight compounds giving viscous
pastes in water. These imparts stickiness and plasticity to the printing paste so that it can be
applied to a fabric surface without spreading and be capable of maintaining the design
outlines even under high pressure. The main function is to hold or adhere the dye particles
in the desired place on the fabric until the transfer of the dye into the fabric and its fixation
are complete.
 Hygroscopic Agent
Over drying of applied print paste often cause cracking and poor adhesion of paste film
fixation failure of print. Hygroscopic agents are used in print paste to prevent over drying
of the printed paste during steaming by absorbing moisture readily as well as to accelerate
the dyestuff fixation. Example: Urea, Glycerine.
 Acid
Acid dyes form ionic bond with silk fibre in acidic medium.

58

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Laboratory Manual

Course no.: Tex 208

Department of Textile Engineering

Literature Review ...........................................................................................................................10

Literature Review ...........................................................................................................................20

Literature Review ...........................................................................................................................25

Literature Review ...........................................................................................................................34

Literature Review ...........................................................................................................................41

Literature Review ...........................................................................................................................46

Literature Review ...........................................................................................................................51

I. Safety code for laboratories

i) Concentrated acids and alkalis

ii) Flammable solvents

iii) Hazardous chemicals

Tex 208: Wet Processing-I Lab Manual

VI. Weights and volumes

Units of weight are:

 Gram g (1 g = 1000 mg)

It is essential to use calibrated balances to ensure that accuracy is maintained.

Tex 208: Wet Processing-I Lab Manual

Units of volume are:

iii) Effect of dye weighing errors

e.g. If 2.0 g was weighed out correctly for a 2% shade on a 4 g specimen:

% depth x weight of specimen

If 2.1g was weighed out, the dye dispersion would be 0.42%.

The weighing of 2.0 g dye needs to be within ± 0.020 g for acceptability.

Tex 208: Wet Processing-I Lab Manual

If 20.1 ml is pipetted, the effective amount of dye used becomes:

If 19.9ml pipetted, the effective amount of dye used becomes:

v) Effect of weight of specimen

The weighing of 4.0 g patterns needs to be within ± 0.05 g for acceptability.

Tex 208: Wet Processing-I Lab Manual

 scouring is carried out at 70 °C

Temperature measurement in °C is carried out using either

a. a ‘mercury in glass’ thermometer.

A thermometer is a delicate instrument and should never be used as a stirrer. The

It is a good idea to have all thermometers calibrated before use.

Warning: if you break a thermometer, seek advice on cleaning up the mercury as it is

ii) Temperature control

iii) Methods of Heating

Tex 208: Wet Processing-I Lab Manual

It is considered best practice to use a hotplate in preference to a gas flame.

pH = -log [H+] , H+ = Hydrogen ion concentration

Tex 208: Wet Processing-I Lab Manual

Measurement of pH using a pH meter

Tex 208: Wet Processing-I Lab Manual

Table-1: Suitable reagents for pH adjustments

Tex 208: Wet Processing-I Lab Manual

Tex 208: Wet Processing-I Lab Manual

The typical sizing materials are:

1.1.2 Starch Desizing

Figure: Structures of amylase and amylopectin

1.1.3 Enzyme Steeping Method

Tex 208: Wet Processing-I Lab Manual

Tex 208: Wet Processing-I Lab Manual

Water pH Enzyme Cold wash

Figure: Process Curve of cotton fabric desizing with enzyme.

Tex 208: Wet Processing-I Lab Manual

 Test 01. Calculation of weight loss in percentage

1.6.1 Test- 01: Calculation of weight loss in percentage

Weight before desizing − Weight after desizing

1.6.2 Test 02: Tegewa test (Iodine test)

Tex 208: Wet Processing-I Lab Manual