Reactive Dyes Tests

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Dye lab Quality Assurance
System Implementation Document 02/09

Standard Operating Procedure for Reactive Dyes testing

Details of the Dyes

Collected Date :

Collected By :

Drum No :

Lot No :

Date of Expiry :

REPORT SHEET

CHARACTERS TEST METHOD RESULT REQT REQT

Moisture content Internal % Nil

Strength by Reflectance for 1:1 AATCC method Integ value for 1:1 Sample tested
Standard Depth Std Depth from must have same
Supplier Integ value as
specified by
Supplier
Determination of relative colour ISO 105 – Z 10 Color strength Comply to strength
strength of dyes in solution value as per prepared
strength
Electrolyte stability of reactive dyes ISO -105 Z08 No absorbable 0 at 80 % salt No precipitation
damage to concentration
dyes
Dye Migration ( for use in CPB also ) AATCC 140- Migration Rate Depending upon
2006 dye

Dyes Accepted / Rejected :

Conclusion and Remarks :

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Standard Operating Procedure for Reactive Dyes testing

Specifications for the acceptance of the Dyes : -

Moisture content

Purpose and scope :-

Moisture content of a dye can, if high or variable ,significantly affect the performance of the
coloration process by effectively altering the amount of dye in a given recipe .

So it is essential to keep the at constant level with in the tolerance limit

Relative color strength in solutions –AATCC 182-2005

Purpose and scope: -

The method describes the strength of a dye relative to the standard by transmittance .

This method applicable to any class that can be prepared as a true solution in a suitable
solvent . The most accurate results are obtained by this method when the sample and standard
under test are chemically identical and from the same manufacturer .

Strength by Reflectance –AATCC Method

Purpose and Scope :-

The reflectance value of the standard and the batch will be carried out in a common
percentage at the same time and the same substrate

Determination of relative color strength dyes in solution ISO 105 –Z 10

Purpose and scope : -

This method is intended for the determination of the colour strength of a dye in relation to that of a
reference dye by means of Spectrophotometric absorption measurement on solution of dyes

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Standard Operating Procedure for Reactive Dyes testing

Electrolyte stability of reactive dyes – ISO 105 –ZO8

Purpose and Scope:-

Determine the solubility of reactive dyes in the presence of reactive dyes in the presence of
electrolytes . Can be assessed in aqueous media.

Dye migration – AATCC 140 -2006

Purpose and Scope:-

The test method provides a means for assessing the migration propensity of a pad liquor
system containing dyes or pigments, subsequently referred to as colorants, and which may
also contain different types and amounts of migration inhibitors.
.
Determination of application Solubility and solution stability -ISO 105 Z07

Purpose and scope :-

Checking the solubility of the dye at different concentrations at the temp where process to be
followed .

Evaluation of dye and pigment migration ISO 105 – Z06 :-

Scope :-

This method describes a method for assessing the migration propensity of a pad liquor system
containing dyes and pigments ,Subsequently referred to as colorants ,and which may also
contains different types and amounts of migration inhibitors .The degree of migration is
obtained by visual examination or by reflectance measurements .

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System Implementation Document 02/09

Standard Operating Procedure for Reactive Dyes testing

Moisture content

Purpose and scope :-

Moisture content of a dye can, if high or variable, significantly affect the performance of the
coloration process by effectively altering the amount of dye in a given recipe .

So it is essential to keep the at constant level with in the tolerance limit

Principle:-

This test method describes the weight variation between the two samples before and after
drying .

Apparatus required:-

Dessicator

Glass container

Hot air oven

Procedure:-

2.0 Gms of the dye is accurately weighed into a previously weighed glass container .The
sample is dried in an oven at 95 to 100 C , Cooled in a desiccator and reweighed . The drying ,
cooling and re weighing processes are repeated until a constant weight is obtained

Calculation:-

Moisture Content ( % ) = Original – Dry weight x 100


Original weight

MOISTURE CONTENT

WORK SHEET

Date : Time : Test done By :

Ambient Temp : Deg C

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System Implementation Document 02/09

Standard Operating Procedure for Reactive Dyes testing

Vendor : Batch No : Drying temp :

Name of the Dyes -

No of samples picked -

Wt of the weighing Bottles -

Wt of the Dyes before drying ( Original ) –

Wt of the Dyes after 1st drying – ( Oven Dry weight ) –

Wt of the Dyes after 2nd Drying - ( oven Dry Weight ) –

Wt of the Dyes after 3rd Drying - ( Oven Dry Weight ) –

Note :-

The drying , cooling and re weighing processes are repeated until a constant weight is obtained
The final reading will be taken as a dry weight ) .

Calculation :-

Moisture Content ( % ) - Original – Dry weight x 100


Original weight

Moisture Content ( % ) - - X100

Result -

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Standard Operating Procedure for Reactive Dyes testing

RELATIVE COLOR STRENGTH OF DYES IN SOLUTIONS – AATCC 182 -2005

Purpose and Scope :-

This test method to determine the color strength of a dye sample relative to a reference
dye by means of spectrometric transmittance measurements on solutions of each .It is a
comparison of the color strength of the dyes in a chosen solvent which may or may not be
correspond to strengths when applied to a textile substrate .

Principle :-

Solutions of the dye test dye and the reference dye and the reference dye are prepared in
known concentrations and their transmittance values are determined using spectrophotometer.
The relative color strength for the test dye is then calculated using absorbance and
concentration values .

Uses and Limitations :-

This method is not applicable to all dyestuffs : Eg. pigments,due to solubility and /or
limitations .Dyes that are commonly measured include acid ,basic, direct and disperse .Many
reactive dyes are not easily measured using this procedure .

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Standard Operating Procedure for Reactive Dyes testing

Relative Dye Strength by Spectrophotometric Measurement –AATCC METHOD

Purpose and Scope :-

The determination of dye strength by spectrophotometric reflectance measurement is


applicable to all dyes applied as a Single component on a textile substrate. The method is
designed to solve the problem of comparing the relative dye strength of two or more samples of
a dye.

Principle:-

Dyeing is uniform and a true representation of the dye applied to the substrate under the
specified standard conditions; that the dye applied to the substrate follows, within the
concentration difference used in the test, a linear relationship between concentration in the
dyed substrate and K/S; that the strength relationship found between the standard and sample
is not concentration-dependent.

It should be mentioned that due to factors not yet fully recognized and understood, dealing with
substrate and application process variables, the repeatability of the dye application on
substrates on small scale is not entirely satisfactory for analytical purposes, and often several
dyeings are required to obtain a representative average.

Limitations:-

Differences in hue between two samples to be compared reduce the degree of


confidence which can be placed on the results of the evaluation because hue differences have
an important influence on perceived strength. A defined degree of hue differences tolerable for
strength determination by the Kubelka-Munk relationship has not been established. If the
absorption maxima do not occur at the same wavelength, if absorption maxima or minima are
broadened or if there are additional absorption maxima or shoulders in the curve of one dyeing,
little confidence can be placed on the strength visually but having different spectral reflectance
curves.

General Considerations and For Accuracy Precision:-

Accuracy is defined as the magnitude of the bias between the true value and the measured
value. When we speak of the accuracy of a method or procedure, we are considering only the
bias introduced when the procedure is carried out exactly as specified. Accuracy does not
include any error introduced by failing to follow the specified procedure exactly in all details.
Thus, it is possible to have a method which is known to give accurate, that is, unbiased values,

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Standard Operating Procedure for Reactive Dyes testing

but have a particular value obtained by using this method which is in error due to some
procedural failure, or omission.

Precision may be defined as the uncertainty which is associated with any measured value as a
result of uncontrollable variations in the procedural steps. Uncontrollable variations are present
to some degree, regardless of how carefully the experimental work is carried out.

Accuracy of Strength Evaluation:-

Application of the standard dye and the sample dye to the substrate followed by visual
assessment of the strength of the dyeing is considered to be the primary method of evaluation.
The precision of this method is relatively low; due to the inability of the average observer to
detect strength difference smaller than approximately + 3% in most cases. For this reason, it is
sometimes difficult to get a meaningful assessment of the accuracy of strength evaluation by
reflectance factor measurement.

Precision of Strength Evaluation:-

In the determination of dye strength by spectrophotometric reflectance measurement of


dyeings, precision expresses the uncertainty in the final value for strength which arises due to
uncontrolled variations in all the operations of determining strength, whether it be connected
with the standard dye or the sample dye. Precision is a statistical concept and is a function of
the standard deviation of replicate determinations of dye concentrations in the dyed substrate.
If replicate determinations are carried out by one operator in one laboratory using one
instrument, the precision is frequently called repeatability. If the replication involves different
operators in different laboratories using different instruments, the precision is frequently called
reproducibility. These values are best expressed as standard deviations. For five or fewer
replicate values the range is a more convenient and equally valid expression of precision. The
precision of strength evaluations is conceptually different from specifications for dye strength
and the two should not be confused.

The degree of precision required varies with the user and depends on the available equipment
among other things. It can be said generally, however, that based on the current state of the
art, the precision attainable in determination of dye strength by reflectance factor measurement
on a textile substrate is considerably lower than that attainable by transmittance measurement
of a dye in solution.

The magnitude of the precision can be evaluated by determining or assessing the standard
deviations s in the experimental variables. The overall standard deviation s 0 is calculated as
the square root of the sum of the squares of the individual standard deviation values.

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Standard Operating Procedure for Reactive Dyes testing

As mentioned before, the precision depends on the number of replicate analyses of standard
and sample. The standard deviation is then calculated as follows:

s 0 = [(s2 /N st ) + (s2 /N sa ]1/2

where s 0 is the overall standard deviation, N st is the number of replicate standard analyses and
N sa is the number of replicate sample analyses. Any standard text on statistics (2, 3) may be
consulted for further elucidation of this technique.

Practical experience indicates that based on single dyeings of standard and sample and single
reflectance factor measurements on these, the standard deviation for strength determination is
approximately 3.5%. In order to reduce this, replicate dyeings for standard and sample and
repeat measurements are necessary.

Dye Application Variables:-

The precision of the relative strength determination, as described, depends largely on the
precision with which the dye is applied on the substrate. Great care must e taken, therefore,
that the application procedure is representative and repeatable.

Many variables affect the strength as finally determined on the dyed substrate. The following
are some of the more important variables to be taken into consideration.

Dye Sample :-

Since most dyes contain adjunct materials, a sample large enough to be representative
should be used in the preparation of a stock solution or dispersion for subsequent application of
the dye. Dye samples should be 1 g or more and weighed on an analytical balance. Volumetric
flasks and pipettes should be use in the preparation of stock solutions and dilutions.

Substrate Sample :-

The weight of the substrate sample must be accurate to + 1%. The substrate samples used
for the application of standard and lot dye must be, for all practical purposes, chemically and
physically identical.

Dye Application :-

Liquor ratios, pH and additions of necessary chemicals must be controlled closely. If the
dye is applied by padding or printing, the pickup by the substrate and the penetration and

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Standard Operating Procedure for Reactive Dyes testing

distribution of the dye liquor or print paste can considerably affect the strength determination.
Care must be taken so that, when repeated, the procedures employed yield statistically
identical results.

In exhaust dyeing, the temperature and time profile of the dye cycle must be closely controlled.
It is imperative that standard and sample be dyed at the same time under identical conditions.
Every care should be taken that the resultant dyeings are level.

Optimal Colorant Concentration:-

Ideally the strength determination should be performed at a dye concentration which is


similar to the concentration of the dye in the end product; however, this is usually employed.
Instrumental considerations pose some limitations from which an optimal concentration can be
determined.

For visual observation, the dyeing optimally should have a reflectance factor at the
measurement wavelength of between 10 & 20% (4, 5). The dye concentration should be
adjusted so that the reflectance factor will fall in this interval.

This interval is also best suited from the instrumental point of view, since for reflectance factor
values below 10% the precision of the reflectance factor measurements is reduced. The effect
on the strength determination can be considerable, e.g. an uncertainty of + 0.1% at the 5%
reflectance factor level is equal to a relative colorant concentration uncertainty of + 2.3% based
on the Kubelka- Munk function. The influence of the surface reflectance on the result also
increases sharply below the 10% reflectance factor level. Practical dye application
considerations suggest that reflectance factor values between 10 and 25% produce satisfactory
results.

If strength evaluations of samples of greater depth are unavoidable, a wavelength different


from that of minimum reflectance factor can be chosen if the standard and sample are virtually
identical in hue, since the Kubelka-Munk absorption function applies at each wavelength In
choosing an alternative wavelength, care should be taken to avoid steep slopes and areas
where the reflectance factor is insensitive to dye concentration. For precise evaluation the
relative dye concentration of standard and sample should be adjusted to be within 15% of each
other. I reflectance factor values of less than 10% must be used, it is generally necessary to
substract an empirically determined constant attributable to surface reflectance (6).

Working Procedures :-

Sample Presentation and Measuring

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Standard Operating Procedure for Reactive Dyes testing

One of the most important aspects of strength determinations by reflectance factor


measurement is the presentation of the sample. An improperly presented sample will usually
yield meaningless results. Although each material to be evaluated will have its own measuring
problems, certain problems are common to most or all of them.

Representative Sample

The sample used for strength determination by reflectance factor measurement must be
uniform, evenly dyed or fabricated and clean. Although the eye tends to disregard specks,
uneven spots, impurities, and dirt, the instrument does not and will include their effect in the
measurement.

Sample Size

To measure a sample properly it should completely cover the sample port of the instrument. If
it does not, the measurement will obviously include a portion of the sample holder, black on
most instruments, resulting in a lower reflectance factor.

Sample Thickness

A sample which is of insufficient thickness will permit light to pass through it and reflect off the
sample holder. A white backing would result in a higher reflectance reading while a black one
results in a lower reading. It is essential that a sufficiently thick sample be measured. This is
determined by measuring the sample with increasing numbers of layers, until no further change
in reflectance factor is observed. The number of layers required will vary greatly with fabric
construction and depth of dyeing.

Texture

Depending on the geometry of the instrument, texture of the sample is more or less of a
problem. Integrating spheres will help reduce this effect. If there is a choice of material upon or
in which the colorant is to be applied, the one with the least texture should be chosen.
Measurements on such fabrics as corduroy, twills and carpets can pose problems with certain
instruments and should be avoided if at all possible. If such measurements are necessary and
prove to be a problem, a device providing rapid rotation of the sample during measurement
may prove useful.

Specular component

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Standard Operating Procedure for Reactive Dyes testing

Most instruments that have an integrating sphere for collecting all of the light reflected from
the sample have the capability for including or excluding that part of the light reflected in the
mirror, or specular, direction from a glossy sample. Exclusion is attained by inserting black
cups or light traps in the sphere at the specular direction from the sample and reference ports.
With the white cups in use (specular included) the total reflectance is measured. Most textile
samples have a matte surface and should be measured in this way. If the sample has
extremely high gloss, the black cups may be used to exclude the specular component.
Samples mounted behind glass should be measured this way. Most nominally glossy samples,
however, have reflecting characteristics such that the gloss reflection is spread over a range of
angles and is not totally excluded by the use of the black cups. More reliable results will be
obtained by measuring such samples with the specular component included.

Fluorescence:-

Fluorescence is the property of a substance that enables it to absorb light of one


wavelength and then re-emit it at a longer wavelength randomly in all directions. In reflectance
measurement the fluorescent substance mat be the colorant, the substrate or both. Only
instruments that have the monochromator between the sample and the detector will most
accurately describe the reflectance characteristics of fluorescent samples in the absorption
range of the dyes. The problem of measuring fluorescent colors is beyond the scope of this
report.

Calculation:-

Reflectance factor data are used to produce a numerical value that represents the
strength relationship between a standard dye and a dye sample as applied to a substrate .the
reflectance is linear with concentration with an accuracy of +/- 1% over a concentration range
of +/-15 % .It is there fore possible to use differences in reflectance factor to calculate
differences in concentration .The wave length selected is usually the wave length of maximum
absorption ( minimum reflectance factor ),but others may be used .The wave length used must
be stated .

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Standard Operating Procedure for Reactive Dyes testing

DETERMINATION OF RELATIVE COLOR STRENGTH IN SOLUTIONS – ISO 105 Z10

Scope : -
This method is intended for the determination of the colour strength of a dye in relation
to that of a reference dye by means of spectrophotometric absorption measurement on solution
of dyes.
Important notes :-
- Basic requirements for this method are that the dye solutions do not scatter light and abbey
the Baugher-Lambert-Beer law as well as identical or similar absorption curves of the samples
and the reference in the visible region of the spectrurm.
- Identical or similar absorption curves are usually obtained if the tests are carried out for the
purpose of dye production control of batches/deliveries of the same dye. This method is not
applicable for the evaluation of dyes with distinctly different adsorption curves.
- The colour strength of a dye is not a physical constant, since it is dependent, for example, on
the test medium and test method. The colour strength determined by this method therefore
may differ from those found by other determination, e.g. instrumental or visual assessments of
dyeings.

Principle:-
Solutions of dye under test and the reference dye are prepared and the absorptive or
colour strength values derived from them are determined.
The percentage relative colour strength Fs, is given by the following equation:

Fs= fk2 x100


fk1
fk1 is the colour strength value of reference dye;
fk2 is the colour strength value of dye under test.

Apparatus:-
Flasks, in accordance with ISO 1042
Pipettes, in accordance with ISO 648.
Cells.
Cuvettes or flow cells.
Analytical balance.
Spectrophotometer or filter colorimeter.
Solvents
WARNING – This part of ISO 105 cells for the use of substances and/ or procedures that
may be injurious to health if adequate precautions are not taken. It refers only to technical
suitability and does not absolve the user from legal obligation relating to health and safety
at any stage. It has been assumed in the drafting of this part of ISO 105 that the execution
of its provisions is entrusted to appropriately qualified and experienced people.

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Standard Operating Procedure for Reactive Dyes testing

NOTE- When selecting solvents the following aspects are important:

Solubility of dye;
Stability of solutions;
Reproducibility of test;
Applicability of result to other media or practical applications.

The solvent used shall be selected from the following:


(a) for water soluble dyes : water ( demineralized )
(b) for water insoluble dyes:
methanol, ethanol ;
acetone;
N-methylpyrrolidone;
Cellosolve, ethylene glycol monoethylether ;
Mixtures of the above solvents.

(a)To adjust the pH


Acids (e.g. Sulphuric acid, acetic acid);
Bases (e.g. Sodium hydroxide , sodium carbonate);
Buffer systems .
(b)To eliminate the influence of unwanted metal ions:
Sequestering agents.
(c) Agents with a deagglomerating or disaggregating action in water;
Surfactants, generally ethylene oxide adducts to alkanols.
( d) Other additives:
Dispersing agents;
Antioxidants.

Procedure :-

Preparation of solutions for measurement

Samples

Store the samples in firmly sealed containers in order to avoid erroneous results arising
from the release or uptake of moisture.

Weighing
Weighing an amount of not less than 0.5 g, to avoid errors attributable to micro in
homogeneities to the nearest 0.0005 g.

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Standard Operating Procedure for Reactive Dyes testing

NOTE- It is essential to ensure that uptake of moisture by hygroscopic dye samples does not
lead to errors weighing.

Dissolving/ dispersing :-

Transfer the weighed dye quantitatively to a graduated flask and then dissolve/disperse it.
In general, pre-dissolving/dispersing in about 20 ml of the dissolving/dispersing medium or an
additional solvent or auxiliary is advantageous. Water soluble dyes are preferably dissolved
hot.
NOTE - It is essential to ensure that the solubility limit is not exceeded during subsequent
cooling.

Equilibrate the solution to ambient temperature (20*C to 25*C ) Make up to the graduated
flasks to the mark and homogenize the solution/dispersion by stirring or by mixing by turning
the flask end over end.

Dilution :-

Dilute or dissolve the solution/dispersion prepared according to so that the maximum


absorption (the minimum transmittant at the lowest point) lies within the range of 10% to 60%
transmittance.

NOTE -
- To avoid errors of dilution no pipette of total volume less than 5 ml nor graduated flask
less than 100 ml should be used.
- For commercial dyes the corresponding concentrations for measurement are within the
range 10 mg/l to 100 mg/l for a 10 mm cell path length or proportionately more for shorter path
length cells.

Measurement and evaluation:-

Carry out the measurement as soon as possible after preparation of the solution , in order
to exclude the influence of changes in solution.

NOTE—When a dye is measured for the first time it is advisable to confirm the validity of
the relationship (Beer’ s low) under the conditions selected (concentration, solvent) within a
range of concentrations between one-half and twice that actually used.

Adopt appropriate techniques with light sensitive solutions e.g. using darkened flaskes ,or
working in dimly lit surroundings.

NOTE--- In certain instances the solution to be measured may be influenced adversely by


the light energy of the source in the measuring instrument.

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Standard Operating Procedure for Reactive Dyes testing

Measurement :-
Measure the absorbance of the solution in cells of identical path length (usually 5 mm or
10 mm). The difference in absorbance between the sample and the reference shall not exceed
30 % in order to minimize the influence of variations in the spectrophotometric response over a
relatively wide range of concentrations, Depending on the measuring instrument used, the
absorbance, A, of the dye solution is obtained directly as a measured result (double-beam
spectrophotometer with simultaneous measurement of an identical cell filled with the solvent
used for dilution , or a single beam instrument previously calibrated with cell containing solvent
), or is calculated as the difference between the absorbance of the dye solution Ar,and a blank
value Ab (measurement of the solvent ).
A= AR – AB
Evaluation:-

Base the evaluation on Beer’s low, using the following equation :

A= log10 (I/t) =εcd

Where
A is the absorbance:
t is the transmittance (decimal fraction, 0 to 1,0):
e is the specific extinction coefficient, in square centimetres per gram;
c is the dye concentration, in grams per cubic centimetre;
d is the cell path length, in centimetres.

Relative colour strength :-

The relative colour strength is given by the following equation:

Fs= ε 2/ε 1 x100

Or by substituting from the above equation;


Fs = A2C1 X100
A1C2
Where subscript 1 refers to the reference dye and subscript 2 refers to the dye under test
If the measured concentrations are equal the following simplified equations is obtained :
Fs = A2 x100
A1
If other colour strength values are used ,they are dealt with accordingly.

Precision:-
The coefficient of variation for determinations under the same conditions (repeated
conditions ) is approximately 0,2% to 0,5 % Hence, this gives about 0,4% to 1,0 % for the

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Standard Operating Procedure for Reactive Dyes testing

uncertainty of an individual determination with a confidence level of 95 % for the uncertainty of


determination under different conditions ( various testing locations), at least double these
values should be assumed.

Test report :-

The test report shall contain the following information:


(a) reference to this Part of ISO 105, i.e, ISO 105-Z10:1997;
(b) the type and designation of the sample tested and the reference dye;
(c) the relative colour strength
NOTE--- A full test report, as required for example in cases of dispute, may contain the
following additional details:
(a) date of test;
(b) dye mass;
(c) solvent used;
(d) dissolving conditions, (e.g. concentration, temperature);
(e) dilution factor;
(f) concentration and temperature of measured solution;
(g) measuring instrument, i.e, type and band width;
(h) cell path length;
(i) wavelength;
(j) colour strength value.

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Standard Operating Procedure for Reactive Dyes testing

ELECTROLYTE STABILITY OF REACTIVE DYES – ISO 105 ZO8

Purpose and Scope:-

This part of ISO 105 describes a method for the determination of the application
solubility of water soluble dyes in the range 40*C to 90*C and of their solution stability. The
method is not interned to measure absolute solubility.

Principle:-

Several solutions of known concentration, including the solubility limit, of the dye to be
tested are prepared at a specified temperature. The solutions are then filtered under suction at
this temperature in a heatable Nutsch filter and the application solubility limit determined by
visual assessment of the filter residues and the measured flow-through time of the filtrate.
The application solubility of dyes is normally determined at 90*C For certain classes of
dyes the solubility is determined at a lower temperature. In selecting the test temperature, the
manufacturer recommendations are followed. The temperature is indicated in the test report
(e.g. application solubility limit determined at 90*C,60*C etc).
The solution stability of dyes is determined by strong for 2 h and, as the case requires,
cooling the above mentioned solution before filtration and assessment. The dissolving and
storage temperatures are indicated in the test report (e.g. solution stability at
90*C/60*C,60*C/60*C etc.).

Apparatus and reagents:-

- Erlenmeyer flask,-capacity 500 ml

- Heating bath - Thermostatically controlled, with magnetic stirring bar 40mm long by 6 mm
diameter, speed of stirrer 500 r/min to 600 r/min.

- Water bath - with temperature regulator( heating/cooling) for adjusting the storage
temperature (e.g. 60*C,30*C or 25*C).

- Nutsch filter (Buchner funnel) - heatable, of glass, steel or porcelain, of inner diameter 70
mm, capacity at least 200 ml, having more than 100 holes with a total surface area of holes
(evenly distributed) of not less than 200 mm

- Thermostatic device - (optional), with circulation pump to adjust temperature of Nutsch filter.

- Vacuum apparatus.

- Suction bottle - Capacity 1 litre to 2 litres.

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Standard Operating Procedure for Reactive Dyes testing

- Piston or membrane pump - sufficiently high suction capacity to create a full vacuum of at
least 50 kPa under pressure.

- Apparatus - to adjust and maintain a given vacuum, preferably coupled with a manometer.

- Stopwatch- to measure flow-through time.


- Filter paper, circular, 70mm+_2 mm diameter.

NOTE ---- Filter papers of the following characteristics have been found suitable.
Property Two typical set of values
Grammage, g/m 2 12 121
Thickness, 210 330
Air resistance,Gurley,s/100ml 3,6 1
Wet burst strength, kPa >1 >4

Surface appearance smooth smooth

The type of filter paper used and the manufacturer shall be listed in the test report.
An amount of 200 ml is designated as normal. More water may be added to the solution, but
such additions shall be reported together with the dye solubility values.
No account is taken of changes in volume as a function of temperature, or those caused by the
addition of dye.

Preparation of solutions :-
The concentrations at which the dye solutions are prepared shall be chosen considering
the expected application solubility limit of the dye.
Expected limit to fall between Stepwise increase in dye Conc. approaching limit

1g/l to 10 g/l 1 g/l


10 g/l to 50 g/l 5 g/l
50 g/l to 100 g/ 10 g/l
Above 100 g/l 20 g/l

To determine solubility at 90*C, paste a known amount of the test dye and introduce it
into the wide-mouthed Erlenmeyer flask with a portion of the 200ml water at about 60*C, but
not in excess of the dissolving temperature of the dye When the dye is completely wetted out,
add the rest of the water to the flask.
Place this solution into the heating bath maintained at 95*C Switch on the magnetic
stirrer. When the solution has attained a temperature of 95*C+_ 2*C, continue stirring at this
temperature for a further 5 min (total stirring time approximately 10 min).

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Standard Operating Procedure for Reactive Dyes testing

Then filter the solution (see clause 6) immediately to determine the solubility of the dye at
90*C. Repeat the process for each concentration of dye under test.
To determine solubility at temperatures below 90*C, paste a known graduated amount of
the test dye and introduce it into a wide-mouthed Erlenmeyer flask with a portion of the 200ml
water at the desired dissolving temperature until the dye is completely wetted out. Then add the
rest to the water to the flask. Place the solution in the heating bath maintained at the desired
dissolving temperature; stir the solution for 10 min and then filter.
Repeat the process for each concentration of dye under test.To determine the solution
stability at the desired temperature (e.g.60*C,30*C or 25*C), place the Erlenmeyer flask
with the solution prepared according to bath maintained at the desired temperature and
allow to stand for 2 h before filtration. Before filtering, mix the solution thoroughly by tilting
the flask to and fro.
Filtering the solutions :-

In order to avoid any temperature shock effects, it is essential that heated solution are
filtered through equipment already brought to the same temperature as the solution under test.
Ideally this is test done using a jacketed filter funnel, but acceptable results can also be
obtained using preheated funnels, either by immersion in a water bath or oven, or by passing
water preheated to the test temperature through the equipment immediately prior to carrying
out the test. When using this later technique, the amount of water should be determined locally
in order that the filter funnel can be heated to the same temperature irrespective of its geometry
and the ambient conditions. In all cases when using preheating techniques rather then a
jacketed funnel, the test solution should be passed through the test equipment immediately
after removing it from its heating medium.
Preheat the Nutsch filter to the test temperature and maintain at this temperature
throughout the entire filtration operation. Immediately before filtering, wet out two filter papers
in the Nutsch filter in a double layer using at least 50 ml water at the test temperature.Adjust
the vacuum to 3 kPa to 4 kPa, Which is equivalent to 300 mm to 400 mm water column
pressure. Filter the dye solution at the recommended temperature and measure the flow-
through time with a stopwatch. Visually examine the flask which contained the solution to
determine whether any residue remains. If the solution does not filter within 2 min at a
stabilized vacuum, filter for an additional maximum 2 min under full vacuum .After the solution
has flowed through, continue to extract the filter uniformly under full vacuum for 1 min .Allow
the filters to dry completely at room temperature before evaluation.

Evaluation:-

Compare visually the dried filters after filtration of the various dye solutions of known
concentrations. The application solubility limit, or the solution stability limit, is taken as that
concentration at which filter residues are seen. Residues that are difficult to see may possibly
be detected by gently rubbing the filter surface with a fingertip.Flow-through time may be used
as a further evaluation criterio. A sudden sharp increase in flow-through time when moving up

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Standard Operating Procedure for Reactive Dyes testing

the range of solution concentrations indicates that the application solubility limit has been
exceeded or that the solution is no longer stable.

Test report :-
The test report shall include the following information:
- Full identification of the dyestuff under test;
- Type of filter paper used and its manufacturer;
- Application solubility limit of the dyestuff, expressed in grams per litre, including the dissolving
temperature:
- Solution stability, expressed in grams per litre, including the dissolving and storage
temperatures;
- Flow-through time
- Any special observations during the test or evaluation procedure
- Any deviation, by agreement or otherwise, from the procedure specified (e.g. amounts of
solvent other than 200 ml, etc.).

Factors affecting results :-

This test method has given good results over several years. However, it should be pointed
out that test conditions which deviate from those specified may lead to quite different results.
For example, the results may be influenced when:
- A different filter is used. The filter selected for the test should represent a compromise with
respect to permeability and should do full justice to the practical conditions.

- Other dissolving temperatures are used. Many dyes dissolve well at temperatures appreciable
below 90*C (or the given test temperature). However there are dyes which readily dissolve at
90*C but are difficult to dissolve at 85 *C.

- Other storage temperatures and storage times are used.


- Water having different hardness or added electrolyte is used .

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Standard Operating Procedure for Reactive Dyes testing

DYE MIGRATION – AATCC 140-2006

Process and Scope :-

This test method provides a means of assessing the migration propensity of a pad
liquor system containing dyes or pigments, subsequently referred to as colorants, and
which may also contain different types and amounts of migration inhibitors.

Principle :-

Fabric impregnated with colorant alone, or with colorant and auxiliaries, is dried while
partially covered with a watch glass permitting differential drying and, therefore, migration to
occur. The degree of migration is evaluated by visual examination, or by reflectance
measurements of the covered and uncovered areas.

Uses and Limitations :-

This method offers two alternative procedures:

- Procedure A. The fabric/glass assembly is allowed to dry at room temperature. The procedure
is very simple, but time consuming (overnight).
- Procedure B. The fabric/glass assembly is dried in a laboratory dryer or oven, either with or
without air circulation. This procedure is faster, but somewhat more complicated.
The test method may be used to compare the migration propensity of dyes and the effect on
migration of different types of migration inhibitors, thickeners and electrolyte.
The test method may be used to evaluate a pad liquor with which migration has been found on
a continuous dye range. The pad liquor composition may be modified by varying the amount or
type of migration inhibitors and tested in the laboratory prior to the application on the range.
The colorant concentrations, substrate and wet pickup should be the same in the laboratory as
used on the range. It is then possible to correlate the test results with the improvement
experienced in practise.

Apparatus and Materials:-

1. Laboratory padder.
2. Glass plate, 600 ×350 mm (Procedure A).
3. Watch glasses (90 mm), 22 mm arch punch.
4. Aluminium rings: 110 mm outer diameter, 80 mm inner diameter and 1 mm thickness
(Procedure B).
5. Clips (Procedure B).
6. Laboratory dryer or oven (Procedure B).
7. Gray Scale for Color Change (for visual evaluation ) (see 13.2).
8. Spectrophotometer (for evaluation by reflectance).

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Standard Operating Procedure for Reactive Dyes testing

9. Fabric swatches (see 13.3 and 8.2.1 or 8.3.1).


Test Specimen :-

1. Colorant(s) in required concentration(s).


2. Migration inhibitors, thickening agents and other auxiliaries (e.g., electrolyte for
reactive dyes) may be used as appropriate.

Procedure:-

1. Pad Bath Preparation.


a. Prepare a pad bath appropriate to the colorant(s) with or without a
migration inhibitor.
2. Procedure A: Drying in Air at Room Temperature.
a. Pad a 150 × 300 mm swatch of fabric at 20 +2◦C (68 +4◦F). Other padding
temperatures may be used, but must then be stated in the report.
Generally use a wet pickup of 60%, but adjust as necessary to simulate
wet pickup of a particular fabric to be run on a particular range
Immediately after padding place the fabric on a flat glass plate. Place the
watch glass on the fabric as , and leave the fabric to dry at room
temperature. Record the room temperature and relative humidity during
drying.
b. Remove the watch glass.

3. Procedure B: Pin Frame Oven Drying.


a. Pad a 110 × 220 mm swatch of fabric at 20 +2◦C (68 +4◦F). Other padding
temperatures may be used, but must then be stated in the report.
Generally, use a wet pickup of 60%, but adjust as necessary to simulate
wet pickup of a particular fabric to be run on a particular range.
b. Immediately after padding mount the fabric taut on a pin frame, and
sandwich it between two watch glasses, one on the fabric face and one
directly underneath on the back of the fabric. Hold the watch glasses in
place with two aluminium rings and clamps.
c. Dry the fabric horizontally at 100 +2◦C for approximately 7 min (or until dry)
in a laboratory dryer of oven, with or without air circulation.
d. Remove the watch glasses.

Evaluation:-

1. Visual Evaluation
a. Compare the depth of color of the fabric that was covered by the watch
glass(es), Area A, to the depth of color of the fabric that was not covered,

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Standard Operating Procedure for Reactive Dyes testing

Area B, by reference to the Gray Scale for Color Change and assign a
migration grade,(refer to AATCC Evaluation Procedures 1, Gray Scale for
Color Change, and 7, Instrumental Assessment of the Change in Color of
a Test Specimen).

2. Evaluation by Reflectance Measurement.

a. Determine the reflectance of the watch glass(es) covered area of the


fabric, Area A, and of uncovered area of the fabric, Area B, using a
spectrophotometer.
b. Convert the reflectance values to K/S values to 4 decimal places, using
equation (1). The percent migration is calculated to the nearest 1% from
equation (2), (refer to AATCC Evaluation Procedure 6, Instrumental Color
Measurement,4.3 and 4.5)

(1) K/S = (1- R)2 /2R

where:
R = reflectance factor at the wavelength of maximum absorption. (The wavelength
should be determined for the reference Area B and used for both measurements).

(2) %M = 100 [1- (K/S) a / (K/S) b


where:

(K/S) a = K/S value of Area A (specimen)

(K/S) b = K/S value of Area B (reference).

Report

1. Report substrate, pad liquor composition, including dyes,


chemicals, auxiliaries, etc. and wet pickup.
2. For Procedure A, report room temperature and relative humidity
during drying.
3. For Procedure B, report whether dried with or without air
circulation,
4. For visual examination, report assessment on a scale of 1-5 by
reference to the Gray Scale for Color Change:
Grade 5-no migration
Grade 4-slight migration
Grade 3-medium migration
Grade 2 – severe migration
Grade 1 –very severe migration

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Standard Operating Procedure for Reactive Dyes testing

5. For reflectance measurements, report percent migration using


the outer dyed area as reference

DYE MIGRATION – AATCC 140-2006

WORK SHEET

Date : Time : Test done By :

Ambient Temp : Deg C Drying Temp :

Vendor : Batch No : Color :

Calculation of Migration :-

%M = 100 [1- (K/S) a / (K/S) b

K/S = (1- R)2 /2R


Where ,
R = reflectance factor at the wavelength of maximum absorption. (The wavelength should be
determined for the reference Area B and used for both measurements).
K – Molar absorbtion CO efficient .
S – Scattering Co efficient
To note the value of R , the least value of the Reflectance curve starting from 360 -700

(K/S) a = K/S value of Area A (specimen covered by the Watch glass )

( K/S )a = K/S = K/S = (1- R)2 /2R =(1- )2 /2 * = / =

Wave length at which the highest ref value -

(K/S) b = K/S value of Area B (Uncovered area fo the specimen).

Wave length at which the highest ref value -

( K/S )b = K/S = K/S = (1- R)2 /2R =(1- )2 /2 * = / =

M = 100 [1- (K/S) a / (K/S) b

M = 100 ( 1 – ( - ) )

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Standard Operating Procedure for Reactive Dyes testing

M = 100 ( 1- )

M = 100 *

% of Migration =

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Standard Operating Procedure for Reactive Dyes testing

DETERMINATION OF SOLUBILITY AND SOLUTION STABILITY – ISO 105 ZO7

Purpose and Scope:-

This method describes a method for the determination of the solubility and the solution
stability of reactive dyes for use in batch wise and continuous dyeing processes in the
presence of electrolytes.

Principle:-

Several solutions of known concentrations, including the solution stability limit, of the dye to
be tested are prepared at a specified temperature in accordance with the dye manufacturers
recommendation .The dye solution is adjusted to the desired test temperature .A specified
amount of the desired electrolyte solution is added and the resultant solution either filtered
immediately or stored for a specified temperature and subsequently filtered under suction.

The solution and /or solution stability limits of the dye solution to the addition of electrolyte are
determined by visual assessment of the filter residues and the measured flow through time of
the filterate.

Apparatus and Reagents:-

-Erlen meyer Flask

-Heating bath – Thermostatically controlled ,with magnetic stirring bar40 mm long by 6 mm


diameter ,speed of stirrer 500 r /min to 600 r/min

-Water Bath ,with temperature regulator (heating/cooling for adjusting the storage temperature)

-Nutsch Filter ( Buchner funnel ),heatable , of glass .steel or porcelain ,of inner diameter 70mm.
Capacity at least 200 ml,having more than 100 holes with a total surface area of holes ( evenly
distributed ) of not less than 200 m3.
-Thermostatic device ( optional ) -,with circulation pump adjust temperature of Nutsch filter.
-Vaccum apparatus
-Suction apparatus –Capacity 1 or 2 litre bottles.
-Piston or membrane pump , of sufficeiently high suction capacity to create a full vacuum of at
least 50 KPa under pressure .
Apparatus to adjust and maintain a given vacuum,preferably coupled with a manometer .
Stop watch ,to measure flow through time
-Filter paper ,circular,70 mm +/-2 mm diameter
Filter papers of the following charteristics have been found suitable .

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Standard Operating Procedure for Reactive Dyes testing

Property Two typical sets of values

Grammage ,g/m3 92 121


Thickness ,Ym 210 330
Air resistance ,Gurley ,s/100 3.6 1
ml
Wet burst strength ,kPa >1 >4
Surface appearance Smooth smooth

-Water ,complying with grade 3 of ISO 3696 ( recommended PH 7 ),used a solvent.

Electrolyte Solution ( Stock Solution ) ,Prepared using grade 3 water according to the
concentrations given in table 1 or such that the required quantity of the desired electrolyte is
contained in 50 ml of solution .

The reproducibility of the test method depends on the quality of the electrolyte .For this reason
,chemically pure substances should be used .

Although the electrolytes used are mostly salts ,tests of the stability of their solutions ,which
need to be carried out rapidly ,often prove not very meaningful .electrolyte solutions should
there fore be discarded at the latest one week after the preparation .

Test Parameters:-
The parameters chosen for the test , including dissolving ,storage and filtration temperatures
,electrolyte chosen and its concentration, will ,depend , on the type of dyestuff being tested
.Examples of combinations of test parameters made as a table.

Preparation of Solutions:-

The concentrations at which the test dye solutions are prepared shall be chosen considering
the expected solution stability limit of the dye in the presence of electrolyte:

Expected limit fall Step wise increase in dye concentration approaching limit
between
1 g/l to 10 g/l 1 g/l
10 to 30 g/l 5 g/l
30 to 100 g/l 10 g/l

The maximum dye concentrations used for the test shall be :


30 g/l for batch wise dyeing processes;
100 g/l for continuous dyeing processes .

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Standard Operating Procedure for Reactive Dyes testing

Place a known amount of the dye to be tested in the wide – mouthed Erlenmeyer flask and add
150 ml water at about 60 c ( But not above the dissolving temperature). Swirl the flask by hand
until the dye is fully wetted out ( pre dissolving ) .
If the addition of urea is required as a dissolving agent in accordance with the
recommendations of the dye manufacturer ,reduce the amount of water by 1 Ml per gram of
urea added ,so as not to change the total volume of the test solution .

Place the solution in to the heating bath ,set at the desired dissolving temperature and stir for
10 min at 500 r/min to 600 r/min.

In order to simulate dye bath compositions used in commercial practice ,additions of other
components to the test solution at this point are permissible (see dye manufacturers
recommendations).Any such additions ,including their influence on the volume of test solution
,shall be noted in the test report.
( Change in volume attributable to changes in temperature need to be taken in to account ).

Adjust the dye solution to the desired temperature for filtration or storage using the water
bath,add 50 ml of the electrolyte solution previously adjusted to the test temperature ,and
homogenize the resulting solution .

Examples of combinations of test parameters

Dyeing Dissolving Filtration/stora Storage Electrolyte added and


Process temp of dye ge temp C Time concentration of stock solution
c min
Batchwise 90 40 120 SodiumChloride ,50 Gpl
60 25 30 Sodium Chloride ,60 Gpl
Sodium carbonate ,5 Gpl
50 50 0 Sodium chloride , 60 Gpl

80 25 60 Sodium Chloride ,50 g/l


Sodium Carbonate ,5 Gpl
Sodium Hydroxide,2 ml/lprepared
from solution containing
approx.435 g/l
90 40 90 Sodium Sulfate(anhydrous),50 g/l
Sodium carbonate ,5 g/l
Sodium Hydroxide ,2 ml/l
prepared from solution
con.app.435g/l

Storage :-

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Standard Operating Procedure for Reactive Dyes testing

Allow the final test solution to stand at constant temperature for the specified storage time .

Filtering the solutions:-


In order to avoid any temperature shock effects it is essential that heated solutions are
filtered through equipment already brought to the same temperature as the solution under test
.Ideally this is best done using a jacketed filter funnel, but acceptable results can also be
obtained using preheated funnels, either by immersion in a water bath or oven ,or by passing
water preheated to the test temperature through the equipment immediately prior to carrying
out the test .When using the later technique ,the amount of water should be determined locally
in order that the filter funnel can be heated to the same temperature irrespective of its geometry
and the ambient conditions . In all the cases when using preheating techniques rather than a
jacketed funnel ,the test solution shuld be passed through the test equipment immediately after
removing it from its heating medium .
Preheat the Nutsch Filter to the test temperature and maintain at this temperature through out
the entire filtration operation

Immediately before filtering ,wet out two filter papers and place in the nutsch filter in a double
layer using at least 50 ml water at the test temperature .

Adjust the vacuum to between 3 kPa to 4 kPa ,which is equivalent to 300 mm to 400 mm water
column pressure.
Before filtering ,homogenize the test solution by swirling it in the flask ( visual check ) .Filter the
entire test solution ( do not decant ) at the desired temperature .Measure the flow through time
with a stop watch .

If the solution does not filter with in 2 min at a stabilized vacuum ,Filter for an additional 2 min
under full vacuum .
After the solution has passed through ,continue to extract the filters uniformly under vacuum for
1 min.
Allow the filters to dry completely at room tmparature before evaluation .

Evaluation:-

Compare visually the dried filters after filtration of the various test solutions of known dyestuff
concentrations .The solubility limit ,or the solution stability limit ,in the presence of electrolyte is
taken as that concentration at which filter residues are seen .Residues that are difficult to see
may possibly be detected by gently rubbing the filter surface with a finger grip .

Flow through time may be used as a further evaluation criterion .A sudden sharp increase in
flow through time when moving up the range of solution concentrations indicates that the
solubility limit has been exceeded or that the solution is no longer stable .

Test report :-

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Standard Operating Procedure for Reactive Dyes testing

a)Number and year of this part of ISO 105 .


b)Full identification of the dye stuff under test ;
c)Full identification and amount of added electrolytes .
d)Type of Filter paper used and its manufacturer
e)Solubility limit of the dyestuff ,in the presence of electrolyte expressed in grams per litre
,including the dissolving temperature .
f)Solution in the presence of electrolyte ,expressed in grams per litre ,including the dissolving
and storage temperatures .
g)Flow –through time ,where applicable .
h)Any special observations during the test or evaluation procedure
i) Any deviation ,by agreement or other wise ,from the procedure specified ( e.g.total volume of
solution other than 200 ml ,addition of urea or other components .etc )

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Standard Operating Procedure for Reactive Dyes testing

EVALUATION OF DYES AND PIGMENT MIGRATION – ISO -105 –Z06

Purpose and Scope:-

This method describes a method for assessing the migration propensity of a pad liquor system
containing dyes and pigments ,Subsequently referred to as colorants ,and which may also
contains different types and amounts of migration inhibitors .The degree of migration is
obtained by visual examination or by reflectance measurements .

The test method may be used to compare the migration propensity of dyes and the effect on
migration of different types of migration inhibitors ,Thickeners and electrolyte .The method may
also be used to evaluate a pad liquor with which migration has been found on a continuous
range .

Principle:-

Fabric impregnated with test colorant alone ,or with test colorant and migration inhibitor ,is
dried partially covered with a watch glass ,permitting differential drying and therefore ,migration
to occur .the degree of migration is evaluated by visual examination or by reflectance
measurements of the covered and uncovered areas .

Important notes
When drying conditions are not constant and/or uniform ,uneven migration may occur ,causing
shade variations during a run ,or shade differences between the face and back ,or between the
side and centre of the fabric .
The pad liquor composition may be modified by varying the amount or type of migration
inhibitor and tested in the laboratory prior to the application on the range .The colorant
concentration ,the fabric and the wet pick up should be the same in the laboratory as used on
the range .It is then possible to correlate the test results with the improvement experienced in
practice .

Two Procedures are described

Procedure A .The fabric assembly is allowed to dry at room temperature .The procedure is very
simple ,but time consuming .
Procedure B .The fabric assembly is dried in a laboratory dryer or oven ,either with or with out
air circulation .This procedure is faster but some what more complicated than procedure A.

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Epistêmê and Technê
T e c h n i c a l re s o u rc e s a n d s e r v i c e s f o r t h e T e x t i l e I n d u s t ry

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Dye lab Quality Assurance
System Implementation Document 02/09

Standard Operating Procedure for Reactive Dyes testing

Apparatus and materials :-

Fabric pieces for dyeing


- For disperse dyes ,vat dyes and pigments ,generally the preferred fabric is a blend
65%/35 %polyester ,
- For Reactive dyes the preferred fabrics is a bleached and mercerised 100% cotton.

Balance,Capacity of weighing to an accuracy of 1 mg.


Laboratory Padder.
Glass plate ,350 mmx600 mm,for procedure A
Watch glasses ,90 mm diameter with 22 arch punch
Laboratory pin frame ,For procedure B
Aluminium rings ,110 mm outer diameter ,80 mm inner diameter ,1 mm thickness ,for
procedure B.
Clips ,e.g metal binder clips for procedure B .
Laboratory dryer on oven ,for procedure B .
Grey scale for assessing change in colour ,in accordance with ISO 105 –A02.
Spectro photo meter

Test specimen:-
Colorant (s),migration inhibitor ,thickening agent and other auxiliaries ( eg.electrolyte for
reactive dyes ) in desired concentration(s) to be tested as appropriate .

Procedure A

Cut a 150 mm x 300 mm piece of fabric ,weigh it using the balance and then pad it using the
laboratory padder at 20 c +/- 2. If other padding temperatures are used ,these shall be stated in
the test report .Generally the wet pick up is 60 % by mass,but may be adjusted to simulate wet
pick up of a particular fabric to be run on a particular range . The pad bath contains colorants
and usually ,auxiliaries
Obtain the desired wet pick up by adjusting the pressure at the nip of the pad rolls .Calculate
the present wet pick up as the mass gained by the substrate after padding using the following
equation .

WP = 100x{m1/m0 -1}
Where
WP is the present mass wet pick up ;
M1 is the mass of the fabric after padding ;
M0 is the mass of the fabric before padding
Immediately after padding place the fabric on a flat glass plate .Place the watch glass on the
fabric . And leave the fabric to dry at room temperature .Remove the watch glass and
determine the degree of migration in accordance with clause 8 by covering the dye

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Epistêmê and Technê
T e c h n i c a l re s o u rc e s a n d s e r v i c e s f o r t h e T e x t i l e I n d u s t ry

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Dye lab Quality Assurance
System Implementation Document 02/09

Standard Operating Procedure for Reactive Dyes testing

concentration in the area of the fabric which was covered by the watch glass to the dye
concentration in the area of the fabric which was not covered .

Procedure 2

Proceed as described in Procedure A ,using a piece of fabric sufficeiently large ( usually about
110 mm x220 mm to fit a laboratory pin frame .Determine the degree of migarion in accordance
with clause 8 by comparing the dye concentration in the area of the fabric which was covered
by the watch glasses ,to the dye concentration in the area of the fabric which was not covered .

Evaluation:-

Compare the depth of color on the area of the fabric which was covered by the watch glass to
the depth of color on the area of the fabric which was not covered using the grey scale for
assessing the change in colour .
Asses the migration of the colorant (s) on the following scale .

- Grade 5 – No migration
- Grade 4 – Slight migration
- Grade 3 –Medium migration
- Grade 2 – severe Migration
- Grade 1 – Very severe migration .

Reflectance evaluation :-
Using a spectrophotometer determine the wave length of maximum absorption on the area of
the fabric which was not covered with the watch glass (es )This is reference area .

Measure the reflectance at the wave length of maximum absorption as determined .area of the
fabric which was not covered .convert the values to K/S using the following equation:

K/S =(1-R)2/2R

Where,
K/S is the ratio of light absorption to light scattering ( Kubelka – Munk function ):
R is the reflectance factor at the wavelength of maximum absorption of the reference area .

Calculate the colorant migration as a percentage to the percentage to the nearest 1 % from the
following equation :

M = 100 { 1- ( K/S ) a /(K/S )b)

Where

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E and T Textile Resources
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T e c h n i c a l re s o u rc e s a n d s e r v i c e s f o r t h e T e x t i l e I n d u s t ry

.
Dye lab Quality Assurance
System Implementation Document 02/09

Standard Operating Procedure for Reactive Dyes testing

M is the present migration :


( K/S )a is the K/S value calculated from the reflectance of area A ;
(K/S ) b is the K/S value calculated from the reflectance of area B ,
More accurate results may be obtained when ,prior to the evaluation or measurement , the dye
on the fabric is fixed by the appropriate conventional methods ,EG thermo fix for disperse dyes
,pad steam for vat and reactive dyes .( Resin curing of pigments does not normally change the
shade ) .

Test reports

The test report shall include the following information


a) reference of this part of ISO 105 ,
b) The pad liquor composition ,including concentration of colorant (s)and ,when used
,migration inhibitor, thickener and electrolyte .
c) The substrate used and the wet pick up ;
d) For procedure A :room temperature and relative humidity during drying
e) For procedure B : whether dried with or with out air circulation :
f) For visual examination : the grey scale grade ;
g) For reflectance measurements :the measurements colorant migration .
h) Details of any deviations from the test procedure .

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